WO2016171245A1 - 積層体 - Google Patents
積層体 Download PDFInfo
- Publication number
- WO2016171245A1 WO2016171245A1 PCT/JP2016/062734 JP2016062734W WO2016171245A1 WO 2016171245 A1 WO2016171245 A1 WO 2016171245A1 JP 2016062734 W JP2016062734 W JP 2016062734W WO 2016171245 A1 WO2016171245 A1 WO 2016171245A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- adhesive layer
- temporary adhesive
- molding
- layer
- mass
- Prior art date
Links
- 239000012790 adhesive layer Substances 0.000 claims abstract description 180
- 239000010410 layer Substances 0.000 claims abstract description 165
- 238000000465 moulding Methods 0.000 claims abstract description 146
- 239000000758 substrate Substances 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 35
- 230000003746 surface roughness Effects 0.000 claims abstract description 18
- 230000003287 optical effect Effects 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims description 72
- 239000011347 resin Substances 0.000 claims description 72
- 239000007788 liquid Substances 0.000 claims description 47
- 239000012778 molding material Substances 0.000 claims description 47
- 238000011282 treatment Methods 0.000 claims description 31
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- 239000003960 organic solvent Substances 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 20
- 238000004380 ashing Methods 0.000 claims description 18
- 230000009467 reduction Effects 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000000748 compression moulding Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 2
- 229920001971 elastomer Polymers 0.000 description 120
- 239000000806 elastomer Substances 0.000 description 114
- 235000012431 wafers Nutrition 0.000 description 111
- -1 acryl Chemical group 0.000 description 110
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 40
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- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 12
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 12
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- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 12
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 11
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- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 9
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- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 8
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- VSVVZZQIUJXYQA-UHFFFAOYSA-N [3-(3-dodecylsulfanylpropanoyloxy)-2,2-bis(3-dodecylsulfanylpropanoyloxymethyl)propyl] 3-dodecylsulfanylpropanoate Chemical compound CCCCCCCCCCCCSCCC(=O)OCC(COC(=O)CCSCCCCCCCCCCCC)(COC(=O)CCSCCCCCCCCCCCC)COC(=O)CCSCCCCCCCCCCCC VSVVZZQIUJXYQA-UHFFFAOYSA-N 0.000 description 7
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- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
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- USFPINLPPFWTJW-UHFFFAOYSA-N tetraphenylphosphonium Chemical compound C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 USFPINLPPFWTJW-UHFFFAOYSA-N 0.000 description 5
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- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
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- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 125000006551 perfluoro alkylene group Chemical group 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
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- 229920001568 phenolic resin Polymers 0.000 description 1
- 229950000688 phenothiazine Drugs 0.000 description 1
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- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 150000003003 phosphines Chemical class 0.000 description 1
- 150000004714 phosphonium salts Chemical class 0.000 description 1
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- CLYVDMAATCIVBF-UHFFFAOYSA-N pigment red 224 Chemical compound C=12C3=CC=C(C(OC4=O)=O)C2=C4C=CC=1C1=CC=C2C(=O)OC(=O)C4=CC=C3C1=C42 CLYVDMAATCIVBF-UHFFFAOYSA-N 0.000 description 1
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- 239000011736 potassium bicarbonate Substances 0.000 description 1
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- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- ILPVOWZUBFRIAX-UHFFFAOYSA-N propyl 2-oxopropanoate Chemical compound CCCOC(=O)C(C)=O ILPVOWZUBFRIAX-UHFFFAOYSA-N 0.000 description 1
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- 238000010298 pulverizing process Methods 0.000 description 1
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- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 1
- 229960001755 resorcinol Drugs 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
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- 238000007650 screen-printing Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
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- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- IYMSIPPWHNIMGE-UHFFFAOYSA-N silylurea Chemical compound NC(=O)N[SiH3] IYMSIPPWHNIMGE-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
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- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- LVEOKSIILWWVEO-UHFFFAOYSA-N tetradecyl 3-(3-oxo-3-tetradecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCC LVEOKSIILWWVEO-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- GVIJJXMXTUZIOD-UHFFFAOYSA-N thianthrene Chemical compound C1=CC=C2SC3=CC=CC=C3SC2=C1 GVIJJXMXTUZIOD-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 description 1
- 229940062627 tribasic potassium phosphate Drugs 0.000 description 1
- 229940001496 tribasic sodium phosphate Drugs 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- VLCLHFYFMCKBRP-UHFFFAOYSA-N tricalcium;diborate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]B([O-])[O-].[O-]B([O-])[O-] VLCLHFYFMCKBRP-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- RKBCYCFRFCNLTO-UHFFFAOYSA-N triisopropylamine Chemical compound CC(C)N(C(C)C)C(C)C RKBCYCFRFCNLTO-UHFFFAOYSA-N 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- KLNPWTHGTVSSEU-UHFFFAOYSA-N undecane-1,11-diamine Chemical compound NCCCCCCCCCCCN KLNPWTHGTVSSEU-UHFFFAOYSA-N 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
Definitions
- the present invention relates to a laminate.
- the present invention relates to a laminate used for processing a wafer device using a carrier substrate.
- a large number of IC chips are formed on a device wafer and separated into pieces by dicing.
- IC integrated circuit
- LSI large-scale integrated circuit
- a wire bonding method As an electrical connection method from an integrated circuit in an IC chip to an external terminal of the IC chip, a wire bonding method has been widely known.
- a device wafer In order to reduce the size of an IC chip, a device wafer is used.
- a method is known in which a through-hole is provided in the semiconductor device and a metal plug as an external terminal is connected to an integrated circuit so as to pass through the through-hole (so-called silicon through electrode (TSV) forming method).
- TSV silicon through electrode
- a technique for improving the degree of integration per unit area of a device wafer by multilayering integrated circuits in an IC chip is known.
- the multilayered integrated circuit increases the thickness of the IC chip, it is necessary to reduce the thickness of the members constituting the IC chip.
- thinning of a device wafer is being considered as a thinning of such a member, which not only leads to the miniaturization of an IC chip, but also saves the manufacturing process of a through hole of a device wafer in the production of a silicon through electrode. Promising because it can be done.
- thinning of semiconductor devices such as power devices and image sensors has been attempted from the viewpoint of improving the degree of integration and improving the degree of freedom of the device structure.
- a device wafer having a thickness of about 700 to 900 ⁇ m is widely known, but in recent years, for the purpose of reducing the size of an IC chip, the thickness of the device wafer has been reduced to 200 ⁇ m or less. Has been tried. However, since a device wafer having a thickness of 200 ⁇ m or less is very thin and a semiconductor device manufacturing member based on the device wafer is also very thin, such a member may be further processed, or When the member is simply moved, it is difficult to support the member stably and without damage.
- Patent Document 1 discloses a peeling method in which a support attached to a wafer via an adhesive layer is peeled off from the wafer.
- a peeling method comprising: a solvent supplying step for supplying a solvent to be lowered to the temporary adhesive layer; and a peeling step for peeling the swollen temporary adhesive layer from the wafer. Yes.
- Patent Document 1 discloses a substrate, a semiconductor element provided on at least one side of the substrate, and a first filling between the substrate, the semiconductor element, and the semiconductor element. It is obtained by covering the first resin obtained by curing the resin composition, the substrate, and the first resin, curing the first resin composition, and then curing the second resin composition. And a second resin, wherein a bonding strength between the first resin and the second resin is 18 MPa or more at room temperature.
- Patent Document 2 after covering the circuit surface of the device wafer with a molding material, a temporary adhesive layer is provided on the surface, and bonded to the carrier base material. It turned out that workability is inferior.
- An object of the present invention is to solve such a problem. After the circuit surface of the device wafer is covered with a molding material, a temporary adhesive layer is provided on the surface, and the device wafer and the carrier substrate are bonded. Even if it combines, it aims at providing the laminated body which can achieve the workability of a favorable device wafer.
- the inventors have studied and found that the workability of a good device wafer can be achieved by setting the number of voids and the surface roughness of the temporary adhesive layer to a predetermined value or less.
- the present invention has been completed. Specifically, the above-mentioned problem has been solved by the following means ⁇ 1>, preferably ⁇ 2> to ⁇ 15>.
- a device wafer having a circuit surface, a molding layer covering the surface of the circuit surface, a laminate having a temporary adhesive layer located on the surface of the molding layer,
- the number of voids having a maximum length of 30 ⁇ m or more observed with an optical microscope from a direction perpendicular to the film surface of the temporary adhesive layer is 3 or less per 700 cm 2 of the film surface of the temporary adhesive layer.
- Ra which is Ra ⁇ 10.0micrometer Ra which is the arithmetic mean surface roughness of an agent layer.
- ⁇ 3> The laminate according to ⁇ 1> or ⁇ 2>, wherein the molding layer is formed by baking a liquid molding material.
- ⁇ 4> The laminate according to ⁇ 1> or ⁇ 2>, wherein the molding layer is formed of a solid compression molding material.
- ⁇ 5> After the treatment is performed on the molding layer, a temporary adhesive layer is provided. When the temperature of the molding layer after the above treatment is increased from 100 ° C. to 200 ° C. at a rate of 10 ° C./min, the thermal mass reduction degree
- ⁇ 6> The laminate according to any one of ⁇ 5>, wherein a temporary adhesive layer is provided after the molding layer covering the surface of the circuit surface is heat-treated at 100 ° C. to 250 ° C.
- ⁇ 7> The laminate according to ⁇ 5> or ⁇ 6>, wherein the surface of the molding layer covering the surface of the circuit surface is washed with an organic solvent, and then a temporary adhesive layer is provided.
- ⁇ 8> The laminate according to any one of ⁇ 5> to ⁇ 7>, wherein a temporary adhesive layer is provided after ashing the surface of the molding layer covering the surface of the circuit surface.
- ⁇ 9> Heat-treating the molding layer covering the surface of the circuit surface at 100 ° C.
- ⁇ 1> to ⁇ 8> wherein a temporary adhesive layer is provided after performing two or more of ashing the surface of the molding layer covering the surface of the circuit surface.
- Laminated body ⁇ 10> The laminate according to ⁇ 8> or ⁇ 9>, wherein the ashing treatment is performed with oxygen plasma.
- the molding layer and the temporary adhesive layer each independently contain a resin.
- ⁇ 13> The laminate according to any one of ⁇ 1> to ⁇ 12>, wherein the thickness of the device wafer is 200 ⁇ m or less.
- ⁇ 14> The laminate according to any one of ⁇ 1> to ⁇ 13>, wherein the temporary adhesive layer is in contact with a carrier substrate.
- ⁇ 15> The laminate according to ⁇ 14>, wherein the temporary adhesive layer is one layer.
- a temporary adhesive layer is provided on the surface, and the device wafer and the carrier base material are bonded together to achieve good device wafer processability.
- Laminated bodies can be provided.
- substitution and non-substitution includes what does not have a substituent and what has a substituent.
- the “alkyl group” includes not only an alkyl group having no substituent (unsubstituted alkyl group) but also an alkyl group having a substituent (substituted alkyl group).
- Actinic light or “radiation” in the present specification means, for example, those including visible light, ultraviolet rays, far ultraviolet rays, electron beams, X-rays and the like.
- light means actinic rays or radiation.
- exposure means not only exposure with a mercury lamp, ultraviolet rays, far ultraviolet rays typified by an excimer laser, X-rays, extreme ultraviolet rays (EUV rays), etc., but also electron beams and ions unless otherwise specified. It also means drawing with a particle beam such as a beam.
- the total solid content refers to the total mass of the components excluding the solvent from the total composition of the composition.
- (meth) acrylate represents acrylate and methacrylate
- (meth) acryl represents acryl and methacryl
- (meth) acryloyl represents “acryloyl” and “methacryloyl”.
- the weight average molecular weight and the number average molecular weight are defined as polystyrene conversion values by gel permeation chromatography (GPC) measurement.
- the weight average molecular weight (Mw) and the number average molecular weight (Mn) are, for example, HLC-8220 (manufactured by Tosoh Corp.), and TSKgel Super AWM-H (manufactured by Tosoh Corp., inner diameter) as a column.
- ID 6.0 mm ⁇ 15.0 cm
- the lipophilic group means a functional group that does not contain a hydrophilic group.
- the “hydrophilic group” means a functional group showing affinity with water.
- the laminate of the present invention is a laminate having a device wafer having a circuit surface, a molding layer covering the surface of the circuit surface, and a temporary adhesive layer positioned on the surface of the molding layer, the film surface of the temporary adhesive layer
- the number of voids having a maximum length of 30 ⁇ m or more observed with an optical microscope from a direction perpendicular to the surface is 3 or less per 700 cm 2 of the surface of the temporary adhesive layer, and the arithmetic average surface roughness of the temporary adhesive layer Ra is Ra ⁇ 10.0 ⁇ m.
- the laminate of the present invention is effective in the manufacture of devices for fan-out applications. Although this mechanism is presumed, by providing a temporary adhesive layer on the surface of the molding layer, outgas derived from the molding layer is generated, and this outgas forms a void in the temporary adhesive layer, or the temporary adhesive layer It is thought that the surface is roughened. And it was found that the voids and surface roughness of such a temporary adhesive layer have a slight effect on the thinning of the device wafer, although they are slight. The workability of the device wafer is remarkably improved by setting the number of voids in the temporary adhesive layer to a predetermined value or less and further setting the arithmetic average surface roughness (Ra) to a predetermined value or less. is there. It is surprising that the slight voids and surface roughness of the temporary adhesive layer have a great influence on the processability of the device wafer.
- FIG. 1 is a schematic cross-sectional view showing the layer structure of a laminate 1 of the present invention, wherein 61 is a device wafer substrate (device substrate), 62 is a circuit surface located on the surface of the device wafer, and 15 is a circuit surface. , 11 is a temporary adhesive layer positioned on the surface of the molding layer, and 12 is a carrier substrate.
- the circuit surface 62 on the surface of the substrate 61 is covered with the molding layer 15, and then the carrier base material 12 on the side of the temporary adhesive layer 11 opposite to the side in contact with the molding layer 15. Is provided.
- the carrier substrate 12 is in contact with the temporary adhesive layer 11, but there may be other layers between the carrier substrate 12 and the temporary adhesive layer 11. Detailed description of each component of the laminated body 1 will be described later.
- the outgas derived from the molding layer damages the temporary adhesive layer 11 to form voids or temporary adhesion.
- the surface of the agent layer was rough. It was found that such voids and surface roughness caused damage when processing the device substrate 61 and caused cracks.
- the number of voids having a maximum length of 30 ⁇ m or more observed with an optical microscope from a direction perpendicular to the film surface of the temporary adhesive layer is 3 or less per 700 cm 2 of the film surface of the temporary adhesive layer, and This point is solved by setting Ra, which is the arithmetic average surface roughness of the surface of the temporary adhesive layer, to Ra ⁇ 10.0 ⁇ m.
- the maximum length means the length of the longest length of two points on the outer periphery of the void portion observed with an optical microscope from the direction perpendicular to the film surface of the temporary adhesive layer. For example, when the void is circular, the diameter of the circle is the maximum length.
- the void in the present invention may be formed such that the film surface of the temporary adhesive layer is depressed, or may be a void formed inside the temporary adhesive layer.
- the void formed inside the temporary adhesive layer is usually spherical. Note that “per film surface of the temporary adhesive layer of 700 cm 2 ” means the area of the film surface on the assumption that the temporary adhesive layer is a flat surface. That is, it is the number of voids relative to the area of the surface observed with an optical microscope.
- the number of voids is 3 or less, preferably 2 or less, more preferably 1 or less, and even more preferably 0.
- the yield (yield) of the number of chips per wafer can be improved.
- the method for measuring the number of voids specifically follows the method described in the examples. However, when the devices described in the embodiments are out of print and difficult to obtain, devices having other functions can be employed.
- the arithmetic average surface roughness (Ra) is Ra ⁇ 10.0 ⁇ m, preferably Ra ⁇ 5.0 ⁇ m, more preferably Ra ⁇ 3.0 ⁇ m, further preferably Ra ⁇ 2.0 ⁇ m, and Ra ⁇ 1. It can also be 4 ⁇ m.
- the aspect whose components with a molecular weight of 1000 or less in a molding layer are 5 mass% or less is illustrated.
- the generation of outgas can be effectively suppressed by reducing easily volatile components in the molding layer.
- the amount of highly volatile components may be reduced with respect to the molding material itself.
- the amount of the volatile component is more preferably 1% by mass or less with respect to the molding layer.
- the amount of the component having a molecular weight of 1000 or less is more preferably 2% by mass or less, further preferably 1.5% by mass or less, and can be 0.9% by mass or less. About a lower limit, although 0 mass% is desirable, it is 0.001 mass% or more as an example of embodiment.
- the method for measuring the amount of the component having a molecular weight of 1000 or less in the present invention follows the method described in Examples described later.
- the molding layer is formed by baking a liquid molding material.
- the low molecular component contained in the molding material can be reduced, and the low molecular component contained in the molding layer can be reduced.
- the liquid state means a fluid having a viscosity of 0.1 ⁇ 10 ⁇ 3 Pa ⁇ s to 150 Pa ⁇ s at 25 ° C., for example.
- the bake temperature may be, for example, 100 to 200 ° C., and further may be 150 to 300 ° C., depending on the type of molding material.
- a mode in which the molding layer is formed of a solid compression molding material is exemplified.
- a molding layer formed by a solid compression method in which the low-molecular component due to outgas contained in the molding material is originally low or almost zero generation of outgas in the molding layer can be suppressed.
- a temporary adhesive layer is provided, and when the temperature of the molding layer after the above processing is increased from 100 ° C. to 200 ° C. at 10 ° C./min.
- An embodiment in which the thermal mass reduction degree is 5% by mass or less is exemplified.
- the thermal mass reduction degree is preferably 3% by mass or less.
- the thermal mass reduction degree of the molding layer may be set to 5% by mass or less by implementing the means described above or below.
- the thermal mass reduction degree is preferably 3% by mass or less, more preferably 2% by mass or less, further preferably 1.5% by mass or less, and particularly preferably 1.4% by mass or less.
- the lower limit of the thermal mass reduction degree is preferably 0% by mass, but an example of the embodiment is 0.001% by mass or more.
- a mode in which a temporary adhesive layer is provided after heat-treating a molding layer covering the surface of the circuit surface at 100 ° C. to 250 ° C. is exemplified.
- the heat treatment temperature can be preferably 100 to 200 ° C.
- the heat treatment time is, for example, 1 to 15 hours, preferably 1 to 10 hours.
- a mode in which a temporary adhesive layer is provided after the molding layer covering the surface of the circuit surface is cleaned with an organic solvent is exemplified.
- an organic solvent By washing the molding layer and the like with an organic solvent, it is possible to remove low molecular components caused by outgas adhering to the surface portion of the molding layer.
- the organic solvent used here include benzene, long-chain alkane-based, petroleum-based, and ketone-based organic solvents, although depending on the molding material.
- the molding layer may be immersed in an organic solvent, or the surface of the molding layer may be rinsed with an organic solvent while the molding layer is spun.
- a mode in which a temporary adhesive layer is provided after ashing the surface of the molding layer covering the surface of the circuit surface is exemplified.
- the outgas can be reduced by removing the low molecular components due to the outgas attached to the surface of the molding layer by ashing.
- the ashing treatment include ashing treatment using ozone, ashing treatment using oxygen plasma and argon plasma, and ashing treatment using oxygen plasma, and ashing treatment using oxygen plasma is more preferable.
- the eighth embodiment is exemplified by combining the first embodiment to the seventh embodiment.
- the molding layer covering the surface of the circuit surface is heat-treated at 100 ° C. to 250 ° C., the surface of the molding layer covering the surface of the circuit surface is washed with an organic solvent,
- a mode in which a temporary adhesive layer is provided after performing two or more of ashing the surface of the molding layer covering the surface is exemplified.
- the number of voids in the temporary adhesive layer can be more effectively reduced and the surface roughness can be suppressed.
- the molding material for forming the molding layer is not particularly defined as long as it does not depart from the spirit of the present invention, but preferably contains a resin and more preferably contains a curable resin.
- the molding material preferably contains at least one of an inorganic filler and a curing agent, and may further contain other components.
- curable resin examples include novolak type phenol resins such as phenol novolak resin, cresol novolak resin, bisphenol A novolak resin, phenol resin such as resol type phenol resin, novolak type such as phenol novolak type epoxy resin and cresol novolak type epoxy resin.
- novolak type phenol resins such as phenol novolak resin, cresol novolak resin, bisphenol A novolak resin, phenol resin such as resol type phenol resin, novolak type such as phenol novolak type epoxy resin and cresol novolak type epoxy resin.
- Epoxy resin bisphenol A type epoxy resin, bisphenol type epoxy resin such as bisphenol F type epoxy resin, hydroquinone type epoxy resin, biphenyl type epoxy resin, stilbene type epoxy resin, triphenolmethane type epoxy resin, alkyl modified triphenolmethane type epoxy Resin, triazine core-containing epoxy resin, dicyclopentadiene modified phenolic epoxy resin, naphthol type epoxy resin, naphtha Type epoxy resin, phenol aralkyl type epoxy resin having phenylene and / or biphenylene skeleton, epoxy resin such as naphthol aralkyl type epoxy resin having phenylene and / or biphenylene skeleton, triazine ring such as urea (urea) resin and melamine resin Resin, unsaturated polyester resin, bismaleimide resin, polyurethane resin, diallyl phthalate resin, silicone resin, resin having a benzoxazine ring, cyanate ester resin, and the like.
- bisphenol A type epoxy resin
- the epoxy resin means all monomers, oligomers and polymers having two or more epoxy groups in one molecule.
- an epoxy resin is preferable.
- electrical characteristics can be improved.
- the fluidity that can be molded can be maintained even when a large amount of inorganic filler is added.
- the resin of the main component here means a component having the largest content among the resin components contained in the molding layer or the temporary adhesive layer, and usually 80% by mass or more of the resin component. is there.
- the content of the resin is not particularly limited, but is preferably 3 to 30% by mass, and particularly preferably 5 to 20% by mass of the entire molding material.
- the content is equal to or higher than the lower limit, the fluidity can be prevented from lowering and the semiconductor element can be sealed better. Moreover, the fall of solder heat resistance can be effectively suppressed by setting it as the said upper limit or less. Only one type of resin may be used, or two or more types of resins may be used.
- the curing agent examples include aliphatic polyamines such as diethylenetriamine (DETA), triethylenetetramine (TETA), and metaxylylenediamine (MXDA), diaminodiphenylmethane (DDM), m-phenylenediamine (MPDA), diaminodiphenylsulfone ( In addition to aromatic polyamines such as DDS), amine curing agents such as polyamine compounds containing dicyandiamide (DICY), organic acid dihydrazide, etc., phenolic curing agents such as novolac phenolic resins and phenolic polymers (curing with phenolic hydroxyl groups) Agent), cyclic fatty acid anhydrides (liquid acid anhydrides) such as hexahydrophthalic anhydride (HHPA), methyltetrahydrophthalic anhydride (MTHPA), trimellitic anhydride (TMA), pyromellitic anhydride ( MDA), acid anhydride curing agents such as aromatic acid an
- the curing agent is not particularly limited, but a curing agent having a phenolic hydroxyl group is preferably used. Since the curing agent having a phenolic hydroxyl group can easily control the reaction of the resin as compared with other curing agents, it can ensure good fluidity when manufacturing a semiconductor device. In addition, the curing agent having a phenolic hydroxyl group can be highly filled with an inorganic filler due to its easy reactivity control. Therefore, the excellent reliability of the semiconductor device can be ensured.
- the curing agent having a phenolic hydroxyl group is a monomer, oligomer or polymer in general having two or more phenolic hydroxyl groups in one molecule, and its molecular weight and molecular structure are not particularly limited. Specifically, it has a novolak type phenol resin such as phenol novolac resin and cresol novolak resin, a modified phenol resin such as triphenolmethane type phenol resin, terpene modified phenol resin and dicyclopentadiene modified phenol resin, and phenylene and / or biphenylene skeleton.
- a novolak type phenol resin such as phenol novolac resin and cresol novolak resin
- a modified phenol resin such as triphenolmethane type phenol resin, terpene modified phenol resin and dicyclopentadiene modified phenol resin
- phenylene and / or biphenylene skeleton a novolak type phenol resin such as phenol novolac resin and cresol novolak resin
- phenol aralkyl resins examples thereof include phenol aralkyl resins, aralkyl type phenol resins such as naphthol aralkyl resins having a phenylene and / or biphenylene skeleton, and bisphenol compounds. These may be used alone or in combination.
- the content of the curing agent is not particularly limited, but is preferably 2 to 10% by mass, particularly 4 to 7% by mass, based on the entire molding material. Only one type of curing agent may be used, or two or more types may be used.
- the resin is an epoxy resin
- a curing agent having a phenolic hydroxyl group is preferably used as the curing agent.
- the equivalent of the epoxy group of the epoxy resin and the phenolic hydroxyl group of the curing agent having a phenolic hydroxyl group is used.
- the ratio (epoxy group / phenolic hydroxyl group) is not particularly limited, but is preferably 0.5 to 2.0, particularly preferably 0.7 to 1.5. When the equivalent ratio is within the above range, the curability and moisture resistance reliability are particularly excellent.
- the molding material preferably contains an inorganic filler.
- the inorganic filler include silicates such as talc, calcined clay, unfired clay, mica and glass, silica powder such as titanium oxide, alumina, fused silica (fused spherical silica and fused crushed silica), and crystalline silica.
- the aforementioned inorganic fillers may be used alone or in combination.
- silica powders such as fused silica and crystalline silica are preferable, and spherical fused silica is particularly preferable.
- the shape of the inorganic filler is not particularly limited, but is preferably spherical and preferably has a broad particle size distribution. Thereby, the fluidity
- the content of the inorganic filler contained in the molding material is not particularly limited, but is preferably 20 to 95% by mass, particularly preferably 30 to 90% by mass, based on the entire molding material.
- the content is equal to or higher than the lower limit, a decrease in moisture resistance is suppressed, and when the content is equal to or lower than the upper limit, good fluidity can be maintained. Only one type of inorganic filler may be used, or two or more types may be used.
- the molding material includes diazabicycloalkenes such as 1,8-diazabicyclo [5.4.0]) undecene-7 and derivatives thereof, tributylamine, benzyldimethylamine, etc., as long as the object of the present invention is not impaired.
- Amine compounds such as 2-methylimidazole, organic phosphines such as triphenylphosphine and methyldiphenylphosphine, tetraphenylphosphonium / tetraphenylborate, tetraphenylphosphonium / tetrabenzoic acid borate, tetraphenylphosphonium / tetranaphth Tetra-substituted phosphonium tetras such as toic acid borate, tetraphenylphosphonium tetranaphthoyloxyborate, tetraphenylphosphonium tetranaphthyloxyborate
- Curing accelerators such as exchange borates, silane coupling agents such as epoxy silane, mercapto silane, amino silane, alkyl silane, ureido silane, vinyl silane, cups such as titanate coupling agent, aluminum coupling agent, aluminum / zirconium coup
- molding materials used in the present invention include G750 series, G760 series, G770 series, G790 series, Hitachi Chemical Co., Ltd. CEL-C-5020, CEL-C-5400, and CEL-C-5800 manufactured by Sumitomo Bakelite. Can be mentioned.
- the thickness of the molding layer is preferably 100 ⁇ m or more at the thinnest part, and more preferably 1000 ⁇ m or more. Moreover, as an upper limit of thickness, it is 3000 micrometers or less at the thinnest part, and it is more preferable that it is 5000 micrometers or less.
- Examples of the molding layer forming method include a method of baking a liquid molding material and a method of heating using a solid compression molding material as described above.
- pre-baking at 90 to 110 ° C for 15 to 30 minutes and then baking at 120 to 150 ° C for additional 2 to 4 hours to form a molding material film Can do.
- the viscosity of the molding material when covering the circuit surface is preferably about 3.0 to 20.0 Pa ⁇ s.
- the molding material is obtained by mixing the raw materials sufficiently uniformly using, for example, a mixer, then melt-kneading with a kneader such as a hot roll, a kneader, or an extruder, and pulverizing after cooling.
- a kneader such as a hot roll, a kneader, or an extruder
- the viscosity at the time of sealing with a molding material is not specifically limited, For example, it is 3.0 Pa.s or more, Preferably, it is 5.0 Pa.s or more.
- the viscosity is preferably 30.0 Pa ⁇ s or less, more preferably 20.0 Pa ⁇ s or less. Thereby, generation
- the viscosity can be determined by, for example, a Koka flow tester. After sealing with the molding material, the molding material is cured. Examples of the method for curing the molding material include a heating method and a light irradiation method.
- the heating condition of the heating method is not particularly limited, but is preferably 160 to 185 ° C., preferably 30 to 180 seconds, particularly preferably 170 to 185 ° C. and 50 to 120 seconds.
- the heating condition is set to be equal to or higher than the above lower limit value, it is possible to suppress the occurrence of mold release defects such as removal of runners, and by setting the heating condition to be within the above upper limit value, the molding cycle time can be shortened and the productivity is improved.
- ⁇ It may be heated using a solid compression molding material. That is, it is preferable to form a molding layer by molding a solid compression molding material in a mold by heating and pressing.
- the solid compression molding material include resin pellets obtained by melt-kneading the above-described molten resin, cooling, and pelletizing.
- the device wafer has a device substrate and a circuit surface located on the surface thereof.
- Any known device substrate can be used without limitation, and examples thereof include a silicon substrate and a compound semiconductor substrate.
- Specific examples of the compound semiconductor substrate include a SiC substrate, a SiGe substrate, a ZnS substrate, a ZnSe substrate, a GaAs substrate, an InP substrate, and a GaN substrate.
- the surface of the device wafer has a circuit surface. Examples of device wafers having a circuit surface include MEMS (Micro Electro Mechanical Systems), power devices, image sensors, microsensors, light emitting diodes (LEDs), optical devices, interposers, embedded devices, and microdevices. .
- MEMS Micro Electro Mechanical Systems
- the device wafer preferably has a structure such as a metal bump. According to the present invention, it is possible to stably temporarily bond a device wafer having a structure on the surface, and to easily release the temporary adhesion to the device wafer.
- the height of the structure is not particularly limited, but is preferably 1 to 150 ⁇ m, for example, and more preferably 5 to 100 ⁇ m.
- the thickness of the device wafer before thinning is preferably 500 ⁇ m or more, more preferably 600 ⁇ m or more, and still more preferably 700 ⁇ m or more.
- the upper limit is preferably 2000 ⁇ m or less, and more preferably 1500 ⁇ m or less.
- the thickness of the device wafer after thinning is preferably, for example, less than 500 ⁇ m, more preferably 400 ⁇ m or less, still more preferably 300 ⁇ m or less, even more preferably 200 ⁇ m or less, even more preferably 100 ⁇ m or less, and even more preferably 50 ⁇ m or less.
- the lower limit is, for example, preferably 1 ⁇ m or more, more preferably 5 ⁇ m or more, and further preferably 20 ⁇ m or more.
- Carrier substrate examples include various wafers such as silicon wafers, SiC wafers and GaN wafers, substrates of various materials such as glass and organic base materials, and those in which an organic film or an inorganic film is formed on the substrate.
- the thickness of the carrier substrate is not particularly limited, but is preferably 300 ⁇ m to 100 mm, and more preferably 300 ⁇ m to 10 mm.
- the laminate of the present invention may have another layer between the carrier substrate (12 in FIG. 1) and the temporary adhesive layer (11 in FIG. 1).
- the other layer include a layer for facilitating separation of the carrier substrate and the temporary adhesive layer (sometimes referred to as a separation layer or a release layer).
- a layer for facilitating separation of the carrier base material and the temporary adhesive layer it is modified by applying light, heat, etc., and a layer that separates the device substrate from the temporary adhesive layer or a specific solvent.
- An example is a mode in which the device substrate is easily dissolved and the device substrate of the laminate is thinned and then immersed in a specific solvent to separate the device substrate and the carrier base material.
- the temporary adhesive layer is used for bonding the molding layer and the carrier substrate together. Bonding can usually be produced by thermocompression bonding. Conventionally, outgas was generated during thermocompression bonding, causing cracks in the device wafer. However, in the present invention, the number of voids and the surface roughness of the temporary adhesive layer should be set to a predetermined value or less. This avoids this problem.
- the pressure bonding conditions are preferably, for example, a temperature of 100 to 210 ° C., a pressure of 0.01 to 1 MPa, and a time of 1 to 15 minutes.
- the material of the temporary adhesive layer in the present invention is not particularly defined as long as the various physical properties are satisfied, but the temporary adhesive layer preferably contains at least one binder.
- the means for obtaining the temporary adhesive layer satisfying the various physical properties can be determined as appropriate. For example, combining two or more specific binders is exemplified. It can also be adjusted by blending a specific kind of binder and a plasticizer.
- the temporary adhesive layer in the present invention contains a binder
- the binder is preferably contained in the total solid content of the temporary adhesive layer in a proportion of 50.00 to 99.99% by mass, and 70.00 to 99.99. 99% by mass is more preferable, and 88.00 to 99.99% by mass is particularly preferable.
- the elastomer is preferably contained in the total solid content of the temporary adhesive layer in a proportion of 50.00 to 99.99% by mass, and 70.00 to 99.99% by mass. More preferred is 88.00 to 99.99% by mass. Details of the binder will be described later.
- the temporary adhesive layer in the present invention preferably contains a fluorinated liquid compound.
- the temporary adhesive layer in the present invention preferably contains a fluorine-based liquid compound in a total solid content of the temporary adhesive layer in a proportion of 0.03% by mass or more and less than 0.5% by mass. 0.4 mass% is more preferable, and 0.05 to 0.2 mass% is still more preferable. Details of the fluorinated liquid compound will be described later.
- the temporary adhesive layer in the present invention can further contain other additives such as an antioxidant. Details of these will be described later.
- the temporary adhesive layer may be one layer or two or more layers, but one layer (for example, a single layer) is preferable.
- the temporary adhesive layer in the present invention preferably has an average film thickness of 0.1 to 500 ⁇ m.
- the lower limit is preferably 1 ⁇ m or more.
- the upper limit is preferably 200 ⁇ m or less, and more preferably 100 ⁇ m or less.
- the total thickness is preferably within the above range.
- the temporary adhesive layer is formed so as to be positioned on the surface of the molding layer.
- the temporary adhesive layer may be formed on the surface of the molding layer, or may be provided on the carrier substrate and bonded to the molding layer.
- the molding layer is formed on the surface of a separate support. It may be transferred.
- the temporary adhesive layer A may be provided on the molding layer, and the temporary adhesive layer B may be provided on the carrier substrate, and the temporary adhesive layer A and the temporary adhesive layer B may be bonded. In this case, the temporary adhesive layer A and the temporary adhesive layer B may be the same or different.
- peeling selectivity peeling selectivity between the molding layer interface and the carrier substrate interface
- the peeling force can be adjusted as appropriate.
- the manufacturing method of a temporary adhesive layer is demonstrated taking the case where it forms on the surface of another support body as an example, when forming on the surface of a molding layer and a carrier base material, it can carry out similarly.
- the method for producing a temporary adhesive layer is to apply a temporary adhesive composition containing a temporary adhesive and a solvent to the surface of the support to form a layer, and dry the solvent to produce a temporary adhesive layer.
- a temporary adhesive composition containing a temporary adhesive and a solvent
- Examples of the method for applying the temporary bonding composition include spin coating, blade coating, spraying, roller coating, flow coating, doctor coating, screen printing, dip coating, and the like. Spin coating and blade coating A coating method is preferred.
- coating the composition for temporary adhesion on a support body by extruding the composition for temporary adhesion with a pressure from slit-shaped opening may be sufficient.
- the application amount of the temporary bonding composition varies depending on the application, but for example, an application amount in which the average film thickness of the temporary adhesive layer after drying is 0.1 to 500 ⁇ m is preferable.
- the lower limit is preferably 1 ⁇ m or more.
- the upper limit is preferably 200 ⁇ m or less, and more preferably 100 ⁇ m or less.
- the average film thickness of a temporary adhesive layer is a film
- a cross section along one direction of the temporary adhesive layer is a cross section orthogonal to the long side direction when the temporary adhesive layer has a polygonal shape. Moreover, when a temporary adhesive layer is square shape, it is set as the cross section orthogonal to any one side. When the temporary adhesive layer is circular or elliptical, the cross section passes through the center of gravity. Drying conditions differ depending on the type of the temporary bonding composition and the film thickness of the temporary adhesive layer. Drying conditions are preferably 60 to 220 ° C. and 10 to 600 seconds, for example. The drying temperature is more preferably 80 to 200 ° C. The drying time is more preferably 30 to 500 seconds, and further preferably 40 to 400 seconds. Drying may be carried out by increasing the temperature stepwise in two steps. For example, after heating at 90 to 130 ° C. for 30 to 250 seconds, heating at 170 to 220 ° C. for 30 to 250 seconds can be mentioned.
- the type of the support on which the temporary adhesive layer is formed is not particularly defined, but a support having releasability is preferable in consideration of transfer onto one of the molding layer surface and the carrier substrate.
- the film-like temporary adhesive layer may be a film composed only of the temporary adhesive layer peeled off from the support or may be peeled off on one surface.
- seat may be sufficient, and the temporary adhesive layer which has a peeling sheet on both surfaces may be sufficient.
- the length of the long film is not particularly limited, but the lower limit is preferably, for example, 5000 mm or more, and more preferably 1000 mm or more.
- the upper limit is preferably 500000 mm or less, and more preferably 200000 mm or less.
- the release sheet is peeled off when used.
- a temporary adhesive layer is formed on a support, it is formed by applying a film-like temporary adhesive layer on one of the molding layer surface and the carrier substrate, and laminating by applying heat and pressure. Is preferred.
- the temporary adhesive layer when forming a temporary adhesive layer on the molding layer surface and carrier substrate instead of the support, leave the temporary adhesive layer as it is without peeling off from these substrates, and process the device wafer. It can be performed. The processing of the device wafer will be described later.
- the temporary adhesive layer when the temporary adhesive layer is directly provided on the surface of the base material, it includes a step of cleaning the excess temporary adhesive layer adhering to the back surface of the base material or the outer peripheral portion of the base material. Is preferred.
- the washing at this time is preferably washing with a solvent, and such a solvent is appropriately determined in relation to the composition of the temporary bonding composition, and mesitylene is mentioned as an example.
- the temporary bonding composition used in the present invention preferably contains at least one binder.
- the type of the binder is not particularly defined as long as the various properties of the temporary adhesive layer can be achieved.
- the binder include a block copolymer, a random copolymer, and a graft copolymer, and a block copolymer is preferable. If it is a block copolymer, the flow of the composition for temporary bonding during the heating process can be suppressed, so that the adhesion can be maintained even during the heating process, and the effect that the peelability does not change even after the heating process is expected. it can.
- the type of the binder is not particularly limited, and is a polystyrene copolymer, a polyester copolymer, a polyolefin copolymer, a polyurethane copolymer, a polyamide copolymer, a polyacrylic copolymer, or a silicone copolymer.
- Copolymers, polyimide copolymers and the like can be used.
- a polystyrene copolymer, a polyester copolymer, and a polyamide copolymer are preferable, and a polystyrene copolymer is more preferable from the viewpoint of heat resistance and peelability.
- the binder is preferably a block copolymer of styrene and another monomer, and a styrene block copolymer having a styrene block at one or both ends is particularly preferable.
- the binder is preferably a hydrogenated product of a block copolymer.
- thermal stability and storage stability are improved.
- the releasability and the removability of the temporary adhesive layer after peeling are improved.
- the hydrogenated product means a polymer having a structure in which a block copolymer is hydrogenated.
- the binder is preferably an elastomer.
- an elastomer As a binder, it is possible to follow a fine unevenness of a carrier substrate or a device wafer, and to form a temporary adhesive layer excellent in adhesiveness by an appropriate anchor effect.
- One or more types of elastomers can be used in combination.
- an elastomer represents the high molecular compound which shows elastic deformation. That is, when an external force is applied, the polymer compound is defined as a polymer compound that has the property of instantly deforming according to the external force and recovering the original shape in a short time when the external force is removed.
- the weight average molecular weight of the elastomer is preferably from 2,000 to 200,000, more preferably from 10,000 to 200,000, and even more preferably from 50,000 to 100,000.
- the solubility in the solvent is excellent. And there is an advantage that no residue remains on the carrier substrate.
- the elastomer is not particularly limited, and is an elastomer containing a repeating unit derived from styrene (polystyrene elastomer), polyester elastomer, polyolefin elastomer, polyurethane elastomer, polyamide elastomer, polyacryl elastomer, silicone elastomer.
- Polyimide elastomer can be used.
- polystyrene-based elastomers, polyester-based elastomers, and polyamide-based elastomers are preferable, and polystyrene-based elastomers are most preferable from the viewpoints of heat resistance and peelability.
- the elastomer is preferably a hydrogenated product.
- a hydrogenated product of a polystyrene-based elastomer is preferable.
- thermal stability and storage stability are improved.
- the releasability and the removability of the temporary adhesive layer after peeling are improved.
- the hydrogenated product means a polymer having a structure in which an elastomer is hydrogenated.
- the elastomer has a 5% thermal mass reduction temperature of 25 ° C. at a rate of 20 ° C./min, preferably 250 ° C. or higher, more preferably 300 ° C. or higher, and 350 ° C. or higher. More preferably, it is most preferably 400 ° C. or higher.
- an upper limit does not have limitation in particular, For example, 1000 degrees C or less is preferable and 800 degrees C or less is more preferable. According to this aspect, it is easy to form a temporary adhesive layer having excellent heat resistance.
- the elastomer used in the present invention can be deformed to 200% with a small external force at room temperature (20 ° C.) when the original size is 100%, and 130% in a short time when the external force is removed. It preferably has the property of returning to the following.
- Polystyrene Elastomer >>>>>
- a polystyrene-type elastomer According to the objective, it can select suitably.
- SBS styrene-butadiene-styrene block copolymer
- SIS styrene-isoprene-styrene block copolymer
- SEBS styrene-ethylene-butylene-styrene block copolymer
- styrene-butadiene-butylene-styrene styrene-butadiene-butylene-styrene.
- SBBS styrene-ethylene-butylene-styrene block copolymer
- SEBS styrene-ethylene-butylene-styrene block copolymer
- SEPS styrene-ethylene-propylene-styrene block copolymer
- SBBS styrene-ethylene-ethylene-propylene -Styrene block copolymers and the like.
- the content of the repeating unit derived from styrene in the polystyrene elastomer is preferably 10 to 90% by mass. From the viewpoint of peelability, the lower limit is preferably 25% by mass or more, and more preferably 51% by mass or more.
- the polystyrene-based elastomer has an elastomer A containing a repeating unit derived from styrene in a proportion of 10% by mass or more and 50% by mass or less in all repeating units, and 50% by mass of repeating units derived from styrene in all repeating units. It is also preferable to use in combination with elastomer B contained in a proportion of more than 95% and not more than 95% by mass.
- the elastomer A is a relatively soft material, it is easy to form a temporary adhesive layer having elasticity. For this reason, when manufacturing the laminated body of a base material and a support body using the composition for temporary adhesion
- the elastomer A preferably contains 13 to 45% by mass, more preferably 15 to 40% by mass, of all styrene-derived repeating units. If it is this aspect, the more excellent flat polishing property will be acquired. Furthermore, the occurrence of warping of the substrate after polishing can be effectively suppressed.
- the hardness of the elastomer A is preferably 20 to 82, more preferably 60 to 79. The hardness is a value measured with a type A durometer according to the method of JIS (Japanese Industrial Standard) K6253.
- the elastomer B preferably contains 55 to 90% by mass, more preferably 60 to 80% by mass, of all styrene-derived repeating units. According to this aspect, peelability can be improved more effectively.
- the hardness of the elastomer B is preferably 83 to 100, and more preferably 90 to 99.
- the polystyrene-based elastomer is preferably a block copolymer of styrene and another monomer, more preferably a block copolymer in which one end or both ends are styrene blocks, and both ends are styrene blocks. It is particularly preferred.
- both ends of the polystyrene-based elastomer are styrene blocks (repeating units derived from styrene)
- the heat resistance tends to be further improved. This is because a repeating unit derived from styrene having high heat resistance is present at the terminal.
- the block part of the repeating unit derived from styrene is preferably a reactive polystyrene hard block, which tends to be more excellent in heat resistance and chemical resistance.
- a reactive polystyrene hard block which tends to be more excellent in heat resistance and chemical resistance.
- phase-separation by a hard block and a soft block is performed at 200 degreeC or more.
- the shape of the phase separation is considered to contribute to the suppression of the occurrence of irregularities on the surface of the device wafer.
- such an elastomer is more preferable from the viewpoint of solubility in a solvent and resistance to a resist solvent.
- the unsaturated double bond amount of the polystyrene elastomer is preferably less than 15 mmol, more preferably less than 5 mmol, and most preferably less than 0.5 mmol per 1 g of the polystyrene elastomer from the viewpoint of peelability. preferable.
- the amount of unsaturated double bonds here does not include the unsaturated double bond in the benzene ring derived from styrene.
- the amount of unsaturated double bonds can be calculated by NMR (nuclear magnetic resonance) measurement.
- a repeating unit derived from styrene is a structural unit derived from styrene contained in a polymer when styrene or a styrene derivative is polymerized, and may have a substituent.
- the styrene derivative include ⁇ -methylstyrene, 3-methylstyrene, 4-propylstyrene, 4-cyclohexylstyrene, and the like.
- the substituent include an alkyl group having 1 to 5 carbon atoms, an alkoxy group having 1 to 5 carbon atoms, an alkoxyalkyl group having 2 to 5 carbon atoms, an acetoxy group, and a carboxyl group.
- Examples of commercially available polystyrene elastomers include Tufprene A, Tufprene 125, Tufprene 126S, Solprene T, Asaprene T-411, Asaprene T-432, Asaprene T-437, Asaprene T-438, Asaprene T-439, Tuftec H1272 Tuftec P1500, Tuftec H1052, Tuftec H1062, Tuftec M1943, Tuftec M1911, Tuftec H1041, Tuftec MP10, Tuftec M1913, Tuftech H1051, Tuftec H1053, Tuftec P2000, Tuftec H1043 (above, manufactured by Asahi Kasei 8) , Elastomer AR815C, Elastomer AR-840C, Elastomer AR-830C, Elastomer AR8 0C, Elastomer AR-875C, Elastomer AR-885C, Elastomer AR-SC-15
- Polyester elastomer >>>>>
- a polyester-type elastomer According to the objective, it can select suitably.
- the dicarboxylic acid include aromatic dicarboxylic acids such as terephthalic acid, isophthalic acid, and naphthalenedicarboxylic acid, and aromatic dicarboxylic acids in which hydrogen atoms of these aromatic rings are substituted with a methyl group, an ethyl group, a phenyl group, or the like.
- Examples thereof include aliphatic dicarboxylic acids having 2 to 20 carbon atoms such as acid, sebacic acid and dodecanedicarboxylic acid, and alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid. These may be used alone or in combination of two or more.
- Examples of the diol compound include aliphatic diols such as ethylene glycol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, 1,10-decanediol, 1,4-cyclohexanediol, Examples thereof include alicyclic diols and divalent phenols represented by the following structural formulas.
- Y DO represents any of an alkylene group having 2 to 10 carbon atoms, a cycloalkylene group having 4 to 8 carbon atoms, —O—, —S—, and —SO 2 —, or Represents a direct bond (single bond).
- R DO1 and R DO2 each independently represent a halogen atom or an alkyl group having 1 to 12 carbon atoms.
- p do1 and p do2 each independently represent an integer of 0 to 4, and n do1 represents 0 or 1.
- polyester elastomer examples include bisphenol A, bis (4-hydroxyphenyl) methane, bis (4-hydroxy-3-methylphenyl) propane, and resorcin. These may be used alone or in combination of two or more.
- a multi-block copolymer having an aromatic polyester (for example, polybutylene terephthalate) portion as a hard segment component and an aliphatic polyester (for example, polytetramethylene glycol) portion as a soft segment component should be used. You can also.
- the multi-block copolymer includes various grades depending on the kind, ratio, and molecular weight of the hard segment and the soft segment.
- Hytrel manufactured by DuPont-Toray Industries, Inc.
- Perprene manufactured by Toyobo Co., Ltd.
- Primalloy manufactured by Mitsubishi Chemical
- Nouvelan manufactured by Teijin Chemicals
- Espel 1612, 1620 Hitachi Chemical Industries, Ltd.
- Polyolefin Elastomer >>>>>
- a polyolefin-type elastomer According to the objective, it can select suitably.
- copolymers of ⁇ -olefins having 2 to 20 carbon atoms such as ethylene, propylene, 1-butene, 1-hexene and 4-methyl-pentene.
- examples thereof include ethylene-propylene copolymer (EPR) and ethylene-propylene-diene copolymer (EPDM).
- non-conjugated dienes having 2 to 20 carbon atoms such as dicyclopentadiene, 1,4-hexadiene, cyclooctadiene, methylene norbornene, ethylidene norbornene, butadiene, isoprene, and ⁇ -olefin copolymers can be used.
- a carboxy-modified nitrile rubber obtained by copolymerizing methacrylic acid with a butadiene-acrylonitrile copolymer can be mentioned.
- ethylene- ⁇ -olefin copolymer rubber ethylene- ⁇ -olefin / non-conjugated diene copolymer rubber, propylene- ⁇ -olefin copolymer rubber, butene- ⁇ -olefin copolymer rubber, etc.
- Miralastomer Mitsubishi Chemicals
- Thermoran Mitsubishi Chemical
- EXACT Exxon Chemical
- ENGAGE Low Chemical
- Espolex Espolex
- Sarlink Toyobo
- Newcon Nippon Polypro
- EXCELLINK JSR
- Polyurethane Elastomer >>>>>
- an elastomer containing structural units of a hard segment composed of low-molecular glycol and diisocyanate and a soft segment composed of a high-molecular (long-chain) diol and diisocyanate can be used.
- the polymer (long chain) diol include polypropylene glycol, polytetramethylene oxide, poly (1,4-butylene adipate), poly (ethylene / 1,4-butylene adipate), polycaprolactone, and poly (1,6-hexene).
- the number average molecular weight of the polymer (long chain) diol is preferably 500 to 10,000.
- the low molecular weight glycol short chain diols such as ethylene glycol, propylene glycol, 1,4-butanediol, and bisphenol A can be used.
- the number average molecular weight of the short chain diol is preferably 48 to 500.
- Examples of commercially available polyurethane-based elastomers include PANDEX T-2185, T-2983N (manufactured by DIC Corporation), milactolan (manufactured by Nippon Milactolan), elastollan (manufactured by BASF), rezemin (manufactured by Dainichi Seika Kogyo), peresen ( Dow Chemical), Iron Rubber (NOK), Mobilon (Nisshinbo Chemical), and the like.
- Polyamide Elastomer >>>>>
- a polyamide-type elastomer According to the objective, it can select suitably.
- an elastomer using a polyamide such as polyamide-6, 11, or 12 as a hard segment and a polyether such as polyoxyethylene, polyoxypropylene, or polytetramethylene glycol and / or polyester as a soft segment may be used.
- These elastomers are roughly classified into two types: polyether block amide type and polyether ester block amide type.
- UBE polyamide elastomer examples include UBE polyamide elastomer, UBESTA XPA (manufactured by Ube Industries), Daiamide (manufactured by Daicel Evonik), PEBAX (manufactured by ARKEMA), Grilon ELX (manufactured by Emschemy Japan Co., Ltd.), Nopamid ( Mitsubishi Chemical Co., Ltd.), Glais (Toyobo), Polyetheresteramide PA-200, PA-201, TPAE-12, TPAE-32, Polyesteramide TPAE-617, TPAE-617C (T & K TOKA) Manufactured).
- UBE polyamide elastomer examples include UBE polyamide elastomer, UBESTA XPA (manufactured by Ube Industries), Daiamide (manufactured by Daicel Evonik), PEBAX (manufactured by ARKEMA), Grilon ELX (manufactured by Emsche
- Polyacrylic elastomer >>>>>
- a polyacrylic-type elastomer According to the objective, it can select suitably.
- those based on acrylic acid esters such as ethyl acrylate, butyl acrylate, methoxyethyl acrylate, ethoxyethyl acrylate, Examples include those obtained by copolymerization of acrylic acid ester, glycidyl methacrylate, allyl glycidyl ether, and the like.
- crosslinking point monomers such as acrylonitrile and ethylene, are mentioned.
- acrylonitrile-butyl acrylate copolymer examples include acrylonitrile-butyl acrylate copolymer, acrylonitrile-butyl acrylate-ethyl acrylate copolymer, acrylonitrile-butyl acrylate-glycidyl methacrylate copolymer, and the like.
- Silicone Elastomer >>>>>
- a silicone type elastomer According to the objective, it can select suitably.
- it is mainly composed of organopolysiloxane, and examples thereof include polydimethylsiloxane, polymethylphenylsiloxane, and polydiphenylsiloxane.
- Specific examples of commercially available products include the KE series (manufactured by Shin-Etsu Chemical Co., Ltd.), the SE series, the CY series, and the SH series (manufactured by Toray Dow Corning Silicone Co., Ltd.).
- Epoxy elastomers include, for example, bisphenol F-type epoxy resins, bisphenol A-type epoxy resins, salicylaldehyde-type epoxy resins, phenol novolac-type epoxy resins or cresol novolac-type epoxy resins with a part or all of the epoxy groups at both terminal carboxylic acids. It can be obtained by modification with modified butadiene-acrylonitrile rubber, terminal amino-modified silicone rubber or the like.
- a polymer compound other than the above-described elastomer also referred to as other polymer compound
- Other polymer compounds can be used alone or in combination of two or more.
- polymer compounds include, for example, hydrocarbon resins, novolac resins, phenol resins, epoxy resins, melamine resins, urea resins, unsaturated polyester resins, alkyd resins, polyamide resins, polyimide resins, polyamideimide resins, Polybenzimidazole resin, polybenzoxazole resin, polyvinyl chloride resin, polyvinyl acetate resin, polyacetal resin, polycarbonate resin, polyphenylene ether resin, polybutylene terephthalate resin, polyethylene terephthalate resin, polyphenylene sulfide resin, polysulfone resin, polyethersulfone resin , Polyarylate resin, polyether ether ketone resin and the like.
- a binder containing a fluorine atom which will be described later, can be used as the binder.
- “Substantially free of fluorine-based binder” means that the content of fluorine-based binder is, for example, preferably 0.1% by mass or less, more preferably 0.05% by mass or less, with respect to the total mass of the binder. More preferably.
- any hydrocarbon resin can be used.
- the hydrocarbon resin basically means a resin consisting of only carbon atoms and hydrogen atoms, but if the basic skeleton is a hydrocarbon resin, it may contain other atoms as side chains. That is, when a functional group other than a hydrocarbon group is directly bonded to the main chain, such as an acrylic resin, a polyvinyl alcohol resin, a polyvinyl acetal resin, or a polyvinylpyrrolidone resin, to a hydrocarbon resin consisting of only carbon atoms and hydrogen atoms.
- the content of the repeating unit in which the hydrocarbon group is directly bonded to the main chain is 30 mol% or more based on the total repeating unit of the resin. Is preferred.
- the hydrocarbon resin meeting the above conditions include terpene resin, terpene phenol resin, modified terpene resin, hydrogenated terpene resin, hydrogenated terpene phenol resin, rosin, rosin ester, hydrogenated rosin, hydrogenated rosin ester, and polymerized rosin.
- Polymerized rosin ester Polymerized rosin ester, modified rosin, rosin modified phenolic resin, alkylphenol resin, aliphatic petroleum resin, aromatic petroleum resin, hydrogenated petroleum resin, modified petroleum resin, cycloaliphatic petroleum resin, coumarone petroleum resin, indene petroleum resin, polystyrene -Polyolefin copolymers, olefin polymers (eg methylpentene copolymer), and cycloolefin polymers (eg norbornene copolymer, dicyclopentadiene copolymer, tetracyclododecene copolymer), etc. .
- the hydrocarbon resin is preferably a terpene resin, rosin, petroleum resin, hydrogenated rosin, polymerized rosin, olefin polymer, or cycloolefin polymer, and is preferably a terpene resin, rosin, olefin polymer, or cycloolefin polymer. More preferably, it is more preferably, and a cycloolefin polymer is particularly preferable.
- cycloolefin polymers examples include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, and hydrides of these polymers.
- Preferred examples of the cycloolefin polymer include addition (co) polymers containing at least one repeating unit represented by the following general formula (II), and at least one repeating unit represented by the general formula (I).
- An addition (co) polymer further comprising a species or more is mentioned.
- Another preferred example of the cycloolefin polymer is a ring-opening (co) polymer containing at least one cyclic repeating unit represented by the general formula (III).
- m represents an integer of 0 to 4.
- R 1 to R 6 each represents a hydrogen atom or a hydrocarbon group having 1 to 10 carbon atoms
- X 1 to X 3 and Y 1 to Y 3 are each a hydrogen atom, or a carbon group having 1 to 10 carbon atoms.
- R 11 , R 12 , R 13 , R 14 , R 15 , R 16 and R 17 each represent a hydrogen atom or a hydrocarbon group (preferably a hydrocarbon group having 1 to 20 carbon atoms), Represents a hydrocarbon group or a hydrocarbon group substituted with a halogen, W represents SiR 18 p D 3-p (R 18 represents a hydrocarbon group having 1 to 10 carbon atoms, and D represents a halogen atom. , -OCOR 18 or -OR 18 , and p represents an integer of 0 to 3. n represents an integer of 0 to 10.
- Norbornene polymers are disclosed in JP-A-10-7732, JP-T 2002-504184, US2004 / 229157A1, WO2004 / 070463A1, and the like.
- the norbornene-based polymer can be obtained by addition polymerization of norbornene-based polycyclic unsaturated compounds. If necessary, a norbornene-based polycyclic unsaturated compound and ethylene, propylene, butene; conjugated dienes such as butadiene and isoprene; non-conjugated dienes such as ethylidene norbornene can also be subjected to addition polymerization.
- This norbornene polymer is marketed by Mitsui Chemicals, Inc.
- Tg glass transition temperatures
- APL8008T Tg70 ° C
- APL6013T Tg125 ° C
- APL6015T Tg145 ° C
- Pellets such as TOPAS 8007, 5013, 6013, 6015, etc. are available from Polyplastics. Further, Appear 3000 is sold by Ferrania.
- hydrides of norbornene polymers are disclosed in JP-A-1-240517, JP-A-7-196736, JP-A-60-26024, JP-A-62-19801, and JP-A-2003-1159767.
- it can be produced by subjecting a polycyclic unsaturated compound to addition polymerization or metathesis ring-opening polymerization and then hydrogenation.
- R 5 and R 6 are preferably hydrogen atoms or methyl groups
- X 3 and Y 3 are preferably hydrogen atoms, and other groups are appropriately selected.
- This norbornene polymer is sold under the trade name Arton G or Arton F by JSR Co., Ltd., and Zeonor ZF14, ZF16, Zeonex 250, Nippon Zeon Co., Ltd., These are commercially available under the trade names 280 and 480R, and these can be used.
- polyimide resin a resin obtained by subjecting tetracarboxylic dianhydride and diamine to a condensation reaction by a known method can be used.
- Known methods include, for example, a method of dehydrating and ring-closing the polyamic acid obtained by mixing approximately equimolar amounts of tetracarboxylic dianhydride and diamine in an organic solvent and reacting at a reaction temperature of 80 ° C. or lower. It is done.
- substantially equimolar means that the molar ratio of tetracarboxylic dianhydride to diamine is close to 1: 1.
- the composition ratio of tetracarboxylic dianhydride and diamine is 0.5 to 2.0 mol of diamine with respect to 1.0 mol of tetracarboxylic dianhydride in total. You may adjust as follows. By adjusting the composition ratio of tetracarboxylic dianhydride and diamine within the above range, the weight average molecular weight of the polyimide resin can be adjusted.
- the tetracarboxylic dianhydride is not particularly limited, and examples thereof include pyromellitic dianhydride, 3,3 ′, 4,4′-biphenyltetracarboxylic dianhydride, 2,2 ′, 3,3′-biphenyltetracarboxylic dianhydride, 2,2-bis (3,4-dicarboxyphenyl) propane dianhydride, 2,2-bis (2,3-dicarboxyphenyl) propane dianhydride 1,1-bis (2,3-dicarboxyphenyl) ethane dianhydride, 1,1-bis (3,4-dicarboxyphenyl) ethane dianhydride, bis (2,3-dicarboxyphenyl) methane Dianhydride, bis (3,4-dicarboxyphenyl) methane dianhydride, bis (3,4-dicarboxyphenyl) sulfone dianhydride, 3,4,9,10-perylenetetracar
- the diamine is not particularly limited and includes, for example, o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, 3,3′-diaminodiphenyl ether, 3,4′-diaminodiphenyl ether, 4,4′-diaminodiphenyl ether, 3 , 3'-diaminodiphenylmethane, 3,4'-diaminodiphenylmethane, bis (4-amino-3,5-dimethylphenyl) methane, bis (4-amino-3,5-diisopropylphenyl) methane, 3,3'- Diaminodiphenyldifluoromethane, 3,4'-diaminodiphenyldifluoromethane, 4,4'-diaminodiphenyldifluoromethane, 3,3'-diaminodiphenylsulfone, 3,4
- One or more selected from the group consisting of diamines are preferred, and 3- (4-aminophenyl) -1,1,3-trimethyl-5-aminoindane is more preferred.
- Examples of the solvent used for the reaction of the tetracarboxylic dianhydride and diamine include N, N-dimethylacetamide, N-methyl-2-pyrrolidone, and N, N-dimethylformamide.
- a nonpolar solvent for example, toluene or xylene
- the reaction temperature of the tetracarboxylic dianhydride and the diamine is preferably less than 100 ° C, more preferably less than 90 ° C.
- imidation of polyamic acid is typically performed by heat treatment under an inert atmosphere (typically a vacuum or nitrogen atmosphere).
- the heat treatment temperature is preferably 150 ° C. or higher, more preferably 180 to 450 ° C.
- the weight average molecular weight (Mw) of the polyimide resin is preferably 10,000 to 1,000,000, and more preferably 20,000 to 100,000.
- the polyimide resin is 25 to at least one solvent selected from ⁇ -butyrolactone, cyclopentanone, N-methylpyrrolidone, N-ethyl-2-pyrrolidone, cyclohexanone, glycol ether, dimethyl sulfoxide and tetramethylurea.
- a polyimide resin having a solubility at 10 ° C. of 10 g / 100 g Solvent or more is preferable.
- Polyimide resins having such solubility include, for example, 3,4,3 ′, 4′-benzophenonetetracarboxylic dianhydride and 3- (4-aminophenyl) -1,1,3-trimethyl-5- Examples thereof include a polyimide resin obtained by reacting with aminoindane. This polyimide resin is particularly excellent in heat resistance.
- a commercially available product may be used as the polyimide resin.
- Durimide registered trademark
- FUJIFILM Corporation manufactured by FUJIFILM Corporation
- GPT-LT manufactured by Gunei Chemical Co., Ltd.
- SOXR-S SOXR-M
- SOXR-U SOXR-C
- SOXR-C all of which are Nippon Advanced Paper Industries Co., Ltd.
- the polycarbonate resin preferably has a repeating unit represented by the following general formula (1).
- Ar 1 and Ar 2 each independently represent an aromatic group, and L represents a single bond or a divalent linking group.
- Ar 1 and Ar 2 in the general formula (1) each independently represent an aromatic group.
- Aromatic groups include benzene ring, naphthalene ring, pentalene ring, indene ring, azulene ring, heptalene ring, indecene ring, perylene ring, pentacene ring, acenaphthene ring, phenanthrene ring, anthracene ring, naphthacene ring, chrysene ring, triphenylene ring , Fluorene ring, biphenyl ring, pyrrole ring, furan ring, thiophene ring, imidazole ring, oxazole ring, thiazole ring, pyridine ring, pyrazine ring, pyrimidine ring, pyridazine ring, indolizine ring, indole ring, benzofuran ring, benzo
- aromatic groups may have a substituent, but preferably do not have a substituent.
- substituent that the aromatic group may have include a halogen atom, an alkyl group, an alkoxy group, and an aryl group.
- halogen atom include a fluorine atom, a chlorine atom, a bromine atom, and an iodine atom.
- alkyl group include alkyl groups having 1 to 30 carbon atoms.
- the alkyl group preferably has 1 to 20 carbon atoms, more preferably 1 to 10 carbon atoms.
- the alkyl group may be linear or branched.
- the hydrogen atoms of the alkyl group may be substituted with halogen atoms.
- the halogen atom include a fluorine atom, a chlorine atom, a bromine atom, and an iodine atom, and a fluorine atom is preferable.
- the alkoxy group an alkoxy group having 1 to 30 carbon atoms is preferable. The number of carbon atoms of the alkoxy group is more preferably 1-20, and still more preferably 1-10.
- the alkoxy group may be linear, branched or cyclic.
- the aryl group an aryl group having 6 to 30 carbon atoms is preferable, and an aryl group having 6 to 20 carbon atoms is more preferable.
- the weight average molecular weight (Mw) of the polycarbonate resin is preferably 1,000 to 1,000,000, and more preferably 10,000 to 80,000. If it is the said range, the solubility to a solvent and heat resistance are favorable.
- PCZ-200, PCZ-300, PCZ-500, PCZ-800 manufactured by Mitsubishi Gas Chemical
- APEC9379 manufactured by Bayer
- Panlite L-1225LM manufactured by Teijin
- the temporary bonding composition used in the present invention preferably contains the binder in a proportion of 50.00 to 99.99% by mass in the total solid content of the temporary bonding composition, and is 70.00 to 99.99% by mass. % Is more preferable, and 88.00 to 99.99 mass% is particularly preferable. If content of a binder is the said range, it is excellent in adhesiveness and peelability.
- the elastomer is preferably included in the total solid content of the temporary bonding composition in a proportion of 50.00 to 99.99% by mass, more preferably 70.00 to 99.99% by mass. 88.00 to 99.99% by mass is particularly preferable.
- the content of the elastomer is in the above range, the adhesiveness and peelability are excellent.
- the total is preferably in the above range.
- the content of the elastomer in the total binder mass is preferably 50 to 100% by mass, more preferably 70 to 100% by mass, further preferably 80 to 100% by mass, and 90 to 100% by mass. Is more preferable.
- the binder may be substantially only an elastomer.
- the content of the elastomer in the binder total mass is preferably 99% by mass or more, more preferably 99.9% by mass or more, and even more preferably only the elastomer is that the binder is substantially only the elastomer. .
- the composition for temporary adhesion in this invention contains a fluorine-type liquid compound.
- the liquid state means a compound having fluidity at 25 ° C. and having a viscosity of 1 to 100,000 mPa ⁇ s at 25 ° C., for example.
- the viscosity can be measured using a B-type viscometer, and as a method for measuring the viscosity, a value obtained by measuring the viscosity using a B-type viscometer (Viscoled Advance, manufactured by Fungi Lab Co., Ltd.) is used. .
- the viscosity of the fluorinated liquid compound at 25 ° C.
- the fluorinated liquid compound is more preferably, for example, 10 to 20,000 mPa ⁇ s, and further preferably 100 to 15,000 mPa ⁇ s.
- the viscosity of the fluorinated liquid compound is within the above range, the fluorinated liquid compound tends to be unevenly distributed in the surface layer of the temporary adhesive layer.
- the fluorinated liquid compound can be preferably used in any form of oligomer or polymer.
- the mixture of an oligomer and a polymer may be sufficient. Such a mixture may further comprise a monomer.
- the fluorinated liquid compound may be a monomer.
- the fluorine-based liquid compound is preferably an oligomer, a polymer, or a mixture thereof from the viewpoint of heat resistance and the like. Examples of the oligomer and polymer include a radical polymer, a cationic polymer, and an anionic polymer, and any of them can be preferably used. A vinyl polymer is particularly preferred.
- the weight average molecular weight of the fluorinated liquid compound is preferably 500 to 100,000, more preferably 1,000 to 50,000, and still more preferably 2,000 to 20,000.
- the fluorinated liquid compound is preferably a compound that does not denature during the treatment of the base material used for temporary adhesion.
- a compound that can exist in a liquid state even after heating at 250 ° C. or higher or after treating the substrate with various chemical solutions is preferable.
- the viscosity at 25 ° C. is 1 to 100,000 mPa ⁇ s after heating to 250 ° C. under a temperature rising condition of 10 ° C./min from a state of 25 ° C. It is preferably 10 to 20,000 mPa ⁇ s, more preferably 100 to 15,000 mPa ⁇ s.
- the fluorinated liquid compound having such characteristics is preferably a non-thermosetting compound having no reactive group.
- the reactive group here refers to all groups that react by heating at 250 ° C., and examples thereof include a polymerizable group and a hydrolyzable group. Specifically, for example, a meta (acrylic) group, an epoxy group, an isocyanato group, and the like can be given.
- the 10% thermal mass reduction temperature raised from 25 ° C. at 20 ° C./min is preferably 250 ° C. or more, and more preferably 280 ° C. or more.
- an upper limit does not have limitation in particular, For example, 1000 degrees C or less is preferable and 800 degrees C or less is more preferable. According to this aspect, it is easy to form a temporary adhesive layer having excellent heat resistance.
- the thermal mass decrease temperature is a value measured under the above temperature rise condition in a nitrogen stream by TG / DTA (thermal mass measuring device).
- the fluorinated liquid compound used in the present invention contains a lipophilic group.
- the lipophilic group include linear or branched alkyl groups, cycloalkyl groups, and aromatic groups.
- the number of carbon atoms in the alkyl group is preferably 2 to 30, more preferably 4 to 30, further preferably 6 to 30, and particularly preferably 12 to 20.
- Specific examples of the alkyl group include, for example, methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, dodecyl, tetradecyl, octadecyl, isopropyl Group, isobutyl group, sec-butyl group, tert-butyl group, 1-ethylpentyl group, 2-ethylhexyl group.
- the alkyl group may have a substituent.
- Examples of the substituent include a halogen atom, an alkoxy group, and an aromatic group.
- Examples of the halogen atom include a chlorine atom, a fluorine atom, a bromine atom, and an iodine atom, and a fluorine atom is preferable.
- the alkoxy group preferably has 1 to 30 carbon atoms, more preferably 1 to 20 carbon atoms, and still more preferably 1 to 10 carbon atoms.
- the alkoxy group is preferably linear or branched.
- the aromatic group may be monocyclic or polycyclic.
- the carbon number of the aromatic group is preferably 6 to 20, more preferably 6 to 14, and most preferably 6 to 10.
- the cycloalkyl group may be monocyclic or polycyclic.
- the cycloalkyl group preferably has 3 to 30 carbon atoms, more preferably 4 to 30 carbon atoms, still more preferably 6 to 30 carbon atoms, and most preferably 12 to 20 carbon atoms.
- Examples of the monocyclic cycloalkyl group include a cyclopropyl group, a cyclobutyl group, a cyclopentyl group, a cyclohexyl group, a cycloheptyl group, and a cyclooctyl group.
- Examples of the polycyclic cycloalkyl group include adamantyl group, norbornyl group, bornyl group, camphenyl group, decahydronaphthyl group, tricyclodecanyl group, tetracyclodecanyl group, camphoroyl group, dicyclohexyl group and pinenyl group. Can be mentioned.
- the cycloalkyl group may have the substituent described above.
- the aromatic group may be monocyclic or polycyclic.
- the carbon number of the aromatic group is preferably 6 to 20, more preferably 6 to 14, and most preferably 6 to 10. It is preferable that the aromatic group does not contain a hetero atom (for example, a nitrogen atom, an oxygen atom, a sulfur atom, etc.) in the elements constituting the ring.
- aromatic group examples include benzene ring, naphthalene ring, pentalene ring, indene ring, azulene ring, heptalene ring, indecene ring, perylene ring, pentacene ring, acenaphthene ring, phenanthrene ring, anthracene ring, naphthacene ring, chrysene ring , Triphenylene ring, fluorene ring, biphenyl ring, pyrrole ring, furan ring, thiophene ring, imidazole ring, thiazole ring, thiazole ring, pyridine ring, pyrazine ring, pyrimidine ring, pyridazine ring, indolizine ring, indole ring, benzofuran ring, Benzothiophene ring, isobenzofuran ring,
- the fluorinated liquid compound may be a compound containing only one kind of lipophilic group, or may contain two or more kinds.
- the lipophilic group may contain a fluorine atom. That is, the fluorinated liquid compound in the present invention may be a compound in which only the lipophilic group contains a fluorine atom.
- a compound further having a group containing a fluorine element also referred to as a fluorine group
- it is a compound containing a lipophilic group and a fluorine group.
- the fluorinated liquid compound is a compound having a lipophilic group and a fluorine group
- the lipophilic group may or may not contain a fluorine atom, but preferably does not contain it.
- the fluorinated liquid compound has at least one lipophilic group in one molecule, preferably 2 to 100, particularly preferably 6 to 80.
- the fluorine group a known fluorine group can be used. Examples thereof include a fluorine-containing alkyl group and a fluorine-containing alkylene group. Of the fluorine groups, those that function as lipophilic groups are included in the lipophilic groups.
- the fluorine-containing alkyl group preferably has 1 to 30 carbon atoms, more preferably 1 to 20 carbon atoms, and still more preferably 1 to 15 carbon atoms.
- the fluorine-containing alkyl group may be linear, branched or cyclic. Moreover, you may have an ether bond.
- the fluorine-containing alkyl group may be a perfluoroalkyl group in which all of the hydrogen atoms are substituted with fluorine atoms.
- the carbon number of the fluorine-containing alkylene group is preferably 2 to 30, more preferably 2 to 20, and further preferably 2 to 15.
- the fluorine-containing alkylene group may be linear, branched or cyclic. Moreover, you may have an ether bond.
- the fluorine-containing alkylene group may be a perfluoroalkylene group in which all of the hydrogen atoms are substituted with fluorine atoms.
- the fluorine-containing liquid compound preferably has a fluorine atom content of 1 to 90% by mass, more preferably 2 to 80% by mass, and still more preferably 5 to 70% by mass.
- the content of fluorine atoms is defined as “ ⁇ (number of fluorine atoms in one molecule ⁇ mass of fluorine atoms) / mass of all atoms in one molecule ⁇ ⁇ 100”.
- a commercially available product can be used as the fluorinated liquid compound.
- the content of the fluorinated liquid compound in the temporary bonding composition in the present invention is preferably 0.01 to 10% by mass with respect to the mass of the temporary bonding composition excluding the solvent, More preferable is 5% by mass. If content of a fluorine-type liquid compound is the said range, it is excellent in adhesiveness and peelability.
- One type of fluorine-based liquid compound may be used alone, or two or more types may be used in combination. When using 2 or more types together, it is preferable that total content is the said range.
- the composition for temporary adhesion used by this invention may contain the plasticizer as needed. By blending a plasticizer, a temporary adhesive layer satisfying the above-mentioned various performances can be obtained.
- a plasticizer phthalic acid esters, fatty acid esters, aromatic polycarboxylic acid esters, polyesters, and the like can be used.
- phthalic acid esters examples include DMP, DEP, DBP, # 10, BBP, DOP, DINP, DIDP (hereinafter referred to as Daihachi Chemical), PL-200, DOIP (hereinafter referred to as CG Esther), Sunsizer DUP (new) Nippon Rika).
- fatty acid esters examples include butyl stearate, Unistar M-9676, Unistar M-2222SL, Unistar H-476, Unistar H-476D, Panaceto 800B, Panaceto 875, Panaceto 810 (above, NOF Corporation), DBA, DIBA, DBS, DOA, DINA, DIDA, DOS, BXA, DOZ, DESU (manufactured by Daihachi Chemical Co., Ltd.) and the like.
- aromatic polycarboxylic acid ester examples include TOTM (manufactured by Daihachi Chemical), monosizer W-705 (manufactured by Daihachi Chemical), UL-80, UL-100 (manufactured by ADEKA), and the like.
- polyester examples include Polycizer TD-1720, Polycizer S-2002, Polycizer S-2010 (above, manufactured by DIC), BAA-15 (produced by Daihachi Chemical).
- plasticizers DIDP, DIDA, TOTM, Unistar M-2222SL and Polycizer TD-1720 are preferable, DIDA and TOTM are more preferable, and TOTM is particularly preferable. Only one type of plasticizer may be used, or two or more types may be combined.
- the molecular weight of the plasticizer is preferably 250 ° C. or more when the mass is reduced by 1% by mass when measured under a nitrogen stream under a constant rate temperature rising condition of 20 ° C./min. 270 ° C. or higher is more preferable, and 300 ° C. or higher is particularly preferable.
- the upper limit is not particularly defined, but can be, for example, 500 ° C. or less.
- the addition amount of the plasticizer is preferably 0.01% by mass to 5.0% by mass and more preferably 0.1% by mass to 2.0% by mass with respect to the total solid content of the temporary bonding composition. .
- the temporary bonding composition used in the present invention may contain an antioxidant.
- an antioxidant a phenol-based antioxidant, a sulfur-based antioxidant, a phosphorus-based antioxidant, a quinone-based antioxidant, an amine-based antioxidant, and the like can be used.
- phenolic antioxidants include p-methoxyphenol, 2,6-di-tert-butyl-4-methylphenol, “Irganox 1010”, “Irganox 1330”, “Irganox 3114”, “Irganox 1035” manufactured by BASF Corporation, Examples include “Sumilizer MDP-S” and “Sumilizer GA-80” manufactured by Sumitomo Chemical Co., Ltd.
- sulfur-based antioxidant examples include 3,3′-thiodipropionate distearyl, “Sumilizer TPM”, “Sumilizer TPS”, “Sumilizer TP-D” manufactured by Sumitomo Chemical Co., Ltd., and the like.
- phosphorus antioxidants include tris (2,4-di-tert-butylphenyl) phosphite, bis (2,4-di-tert-butylphenyl) pentaerythritol diphosphite, and poly (dipropylene glycol) phenyl.
- Examples thereof include phosphite, diphenylisodecyl phosphite, 2-ethylhexyl diphenyl phosphite, triphenyl phosphite, “Irgafos 168” and “Irgafos 38” manufactured by BASF Corporation.
- Examples of the quinone antioxidant include p-benzoquinone and 2-tert-butyl-1,4-benzoquinone.
- Examples of amine-based antioxidants include dimethylaniline and phenothiazine.
- Irganox 1010, Irganox 1330, 3,3′-thiodipropionate distearyl and Sumilizer TP-D are preferable, Irganox 1010 and Irganox 1330 are more preferable, and Irganox 1010 is particularly preferable.
- a polystyrene-based elastomer when used as the elastomer, it is preferable to use a phenol-based antioxidant and a sulfur-based antioxidant in combination.
- a phenol-based antioxidant and a sulfur-based antioxidant By using such a combination, it can be expected that the deterioration of the binder due to the oxidation reaction can be efficiently suppressed.
- Irganox 1010 and Sumilizer TP-D As the combination of antioxidants, Irganox 1010 and Sumilizer TP-D, Irganox 1330 and Sumilizer TP-D, and Sumilizer GA-80 and Sumilizer TP-D are preferable, Irganox 1010 and Sumilizer TP-D, 13g More preferred are Irganox 1010 and Sumilizer TP-D.
- the molecular weight of the antioxidant is preferably 400 or more, more preferably 600 or more, and particularly preferably 750 or more, from the viewpoint of preventing sublimation during heating.
- the content of the antioxidant is preferably 0.001 to 20.0% by mass with respect to the total solid content of the temporary bonding composition, 0.005 to 10.0 mass% is more preferable.
- One type of antioxidant may be sufficient and two or more types may be sufficient.
- the total is preferably within the above range.
- the temporary bonding composition used in the present invention preferably contains a solvent. Any known solvent can be used without limitation, and an organic solvent is preferred. Examples of the organic solvent used in the present invention include ethyl acetate, n-butyl acetate, isobutyl acetate, amyl formate, isoamyl acetate, isobutyl acetate, butyl propionate, isopropyl butyrate, ethyl butyrate, butyl butyrate, methyl lactate, ethyl lactate, Alkyl oxyacetates (eg, methyl oxyacetate, ethyl oxyacetate, butyl oxyacetate (eg, methyl methoxyacetate, ethyl methoxyacetate, butyl methoxyacetate, methyl ethoxyacetate, ethyl ethoxyacetate)), 3-oxypropionic acid alkyl esters (Eg, methyl 3-oxypropionic acid
- 2-oxyp Pionic acid alkyl esters eg, methyl 2-oxypropionate, ethyl 2-oxypropionate, propyl 2-oxypropionate, etc.
- solvents are preferably mixed in two or more types from the viewpoint of improving the coated surface.
- the solvent content of the temporary bonding composition is such that the total solid concentration of the temporary bonding composition is 5 to 80% by mass from the viewpoint of applicability. 5 to 70% by mass is more preferable, and 10 to 60% by mass is particularly preferable.
- One type of solvent may be sufficient and two or more types may be sufficient. When there are two or more solvents, the total is preferably in the above range.
- the temporary bonding composition used in the present invention preferably contains a surfactant.
- a surfactant any of anionic, cationic, nonionic, or amphoteric surfactants can be used, but a preferred surfactant is a nonionic surfactant.
- nonionic surfactants include polyoxyethylene higher alkyl ethers, polyoxyethylene higher alkyl phenyl ethers, higher fatty acid diesters of polyoxyethylene glycol, and silicone surfactants.
- attachment contains a silicone type surfactant as surfactant.
- a silicone type surfactant as surfactant.
- silicone surfactants include, for example, JP-A-62-36663, JP-A-61-226746, JP-A-61-226745, JP-A-62-170950, JP-A-63-34540, The surfactants described in Kaihei 7-230165, JP-A-8-62834, JP-A-9-54432, JP-A-9-5988, and JP-A-2001-330953 can be mentioned. An agent can also be used.
- examples of commercially available silicone surfactants include KP-301, KP-306, KP-109, KP-310, KP-310B, KP-323, KP-326, KP-341, KP-104, KP-110.
- the content of the surfactant is preferably 0.001 to 5% by mass with respect to the total solid content of the temporary bonding composition, from the viewpoint of applicability. 0.005 to 1% by mass is more preferable, and 0.01 to 0.5% by mass is particularly preferable. Only one type of surfactant may be used, or two or more types may be used. When two or more surfactants are used, the total is preferably in the above range.
- the composition for temporary bonding used in the present invention is various additives such as a curing agent, a curing catalyst, a silane coupling agent, a filler, an adhesion promoter, and the like, as long as the effects of the present invention are not impaired.
- An ultraviolet absorber, an aggregation inhibitor, etc. can be mix
- the total blending amount is preferably 3% by mass or less based on the total solid content of the temporary bonding composition.
- the temporary bonding composition used in the present invention preferably does not contain impurities such as metals.
- the content of impurities contained in these materials is preferably 1 mass ppm or less, more preferably 1 mass ppb or less, still more preferably 100 mass ppt or less, even more preferably 10 mass ppt or less, and substantially no inclusion. (It is below the detection limit of a measuring apparatus) is especially preferable.
- Examples of a method for removing impurities such as metals from the temporary bonding composition include filtration using a filter.
- the filter pore diameter is preferably 10 nm or less, more preferably 5 nm or less, and still more preferably 3 nm or less.
- the filter material is preferably a polytetrafluoroethylene, polyethylene, or nylon filter. You may use the filter previously wash
- a plurality of types of filters may be connected in series or in parallel. When using a plurality of types of filters, filters having different hole diameters and / or materials may be used in combination. Moreover, various materials may be filtered a plurality of times, and the step of filtering a plurality of times may be a circulating filtration step.
- a raw material constituting the temporary bonding composition is selected as a raw material constituting the temporary bonding composition, a raw material having a low metal content is selected.
- the filter may be filtered, or the inside of the apparatus may be lined with polytetrafluoroethylene or the like, and distillation may be performed under a condition in which contamination is suppressed as much as possible.
- the preferable conditions for filter filtration performed on the raw materials constituting the temporary bonding composition are the same as those described above.
- impurities may be removed with an adsorbent, or a combination of filter filtration and adsorbent may be used.
- adsorbent known adsorbents can be used.
- inorganic adsorbents such as silica gel and zeolite
- organic adsorbents such as activated carbon can be used.
- the temporary bonding composition used in the present invention can be prepared by mixing the above-described components.
- the mixing of each component is usually performed in the range of 0 ° C to 100 ° C.
- the filtered liquid can also be refiltered. Any filter can be used without particular limitation as long as it has been conventionally used for filtration.
- fluorine resins such as PTFE (polytetrafluoroethylene), polyamide resins such as nylon-6 and nylon-6,6, polyolefin resins such as polyethylene and polypropylene (PP) (including those with high density and ultra high molecular weight) ) And the like.
- PTFE polytetrafluoroethylene
- polyamide resins such as nylon-6 and nylon-6,6, polyolefin resins
- PP polypropylene
- the pore size of the filter is suitably about 0.003 to 5.0 ⁇ m, for example. By setting it within this range, it becomes possible to reliably remove fine foreign matters such as impurities and aggregates contained in the composition while suppressing filtration clogging.
- filters different filters may be combined.
- the filtering by the first filter may be performed only once or may be performed twice or more.
- the second and subsequent hole diameters are the same or smaller than the first filtering hole diameter.
- the pore diameter here can refer to the nominal value of the filter manufacturer.
- a commercially available filter for example, it can be selected from various filters provided by Nippon Pole Co., Ltd., Advantech Toyo Co., Ltd., Japan Entegris Co., Ltd. (formerly Japan Microlith Co., Ltd.) or KITZ Micro Filter Co., Ltd. .
- FIGS. 2A to 2E are schematic cross-sectional views (FIGS. 2A and 2B) illustrating temporary adhesion between a carrier substrate and a device wafer provided with a molding layer, respectively.
- the temporarily bonded device wafer provided with the molding layer is thinned (FIG. 2C), the carrier substrate and the device wafer provided with the molding layer are peeled off (FIG. 2D), the molding.
- FIG. 2C The temporarily bonded device wafer provided with the molding layer is thinned
- FIG. 2D the carrier substrate and the device wafer provided with the molding layer are peeled off
- FIG. 2D It is a schematic sectional drawing which shows the state (FIG.2 (E)) after removing a temporary adhesive layer from the device wafer which has a layer.
- the adhesive carrier base material 100 by which the temporary adhesive layer 11 is provided in the carrier base material 12 first is prepared. It is preferable that the temporary adhesive layer 11 is an aspect which does not contain a solvent substantially.
- the device wafer 60 is formed by providing a plurality of circuit surfaces 62 on a surface 61 a of a device substrate 61.
- the thickness of the device substrate 61 is preferably 200 to 1200 ⁇ m, for example.
- the circuit surface 62 is preferably a metal structure, for example, and the height is preferably 10 to 100 ⁇ m.
- a molding layer 15 is provided on the surface of the device wafer so as to cover the circuit surface.
- the molding layer is preferably a flat layer provided on the substrate surface of the device substrate so as to cover the circuit surface. Further, in the present invention, it is preferable that the relationship of “X + 100 ⁇ Y> X” is satisfied when the height of the circuit surface is X ⁇ m and the thickness of the molding layer is Y ⁇ m. Since the molding layer 15 is a flat layer, it is effective when it is desired to further reduce the TTV (Total Thickness Variation) of the thinned device wafer (that is, when the flatness of the thinned device wafer is to be further improved). .
- TTV Total Thickness Variation
- the adhesive carrier substrate 100 and the device wafer 60 provided with the molding layer 15 are pressure-bonded so that the temporary adhesive layer 11 and the molding layer 15 are in contact with each other, and the carrier substrate 12 And a molding layer are temporarily bonded.
- the back surface 61b of the device substrate 61 is subjected to mechanical or chemical treatment (though not particularly limited, for example, thinning treatment such as grinding or chemical mechanical polishing (CMP)).
- mechanical or chemical treatment though not particularly limited, for example, thinning treatment such as grinding or chemical mechanical polishing (CMP)
- CVD Chemical vapor deposition
- PVD physical vapor deposition
- other high-temperature / vacuum treatments treatments using chemicals such as organic solvents, acidic treatment solutions and basic treatment solutions, plating treatments, actinic rays 2
- the device substrate 61 is thinned (for example, thinned so as to have the above-mentioned thickness) as shown in FIG. 2C, and the thinned device wafer is formed. 60a is obtained.
- a through hole (not shown) penetrating the device substrate is formed from the back surface 61b1 of the thinned device wafer 60a after the thinning process, and a silicon through electrode is formed in the through hole. You may perform the process which forms (not shown).
- the heat treatment may be performed until the carrier wafer 12 is peeled off.
- a treatment with heating may be used when performing a mechanical or chemical treatment.
- the maximum temperature reached in the heat treatment is preferably 80 to 400 ° C, more preferably 130 ° C to 400 ° C, and still more preferably 180 ° C to 350 ° C.
- the highest temperature reached in the heat treatment is preferably lower than the decomposition temperature of the temporary adhesive layer.
- the heat treatment is preferably performed for 30 seconds to 30 minutes at the highest temperature, and more preferably for 1 minute to 10 minutes at the highest temperature.
- the carrier substrate 12 is separated from the thinned device wafer 60a provided with a molding layer.
- the separation method is not particularly limited, but without any treatment, one of the carrier base 12 and the thinned device wafer 60a is fixed and the other is fixed to the substrate surface fixed from the end. It is preferable to pull up in the direction and separate. In this embodiment, it is preferable to peel off at the interface between the carrier substrate 12 and the temporary adhesive layer 11. In addition, the temporary adhesive layer 11 is brought into contact with a later-described stripping solution, and then, if necessary, after sliding the thinned device wafer 60a provided with the molding layer 15 with respect to the carrier substrate 12, the above and It can also be separated.
- the temperature at the time of separation is preferably 40 ° C. or lower, and can also be 30 ° C. or lower.
- the lower limit of the temperature at the time of peeling is, for example, 0 ° C. or higher, and preferably 10 ° C. or higher.
- the separation can be performed at a room temperature of about 15 to 35 ° C.
- the removal method of the temporary adhesive layer 11 is, for example, a method of peeling and removing the temporary adhesive layer as it is, a method of removing the temporary adhesive layer using a peeling liquid (swelling the temporary adhesive layer with the peeling liquid)
- the actinic ray of the temporary adhesive layer For example, a method of decomposing and vaporizing and removing by irradiation with radiation or heat can be used.
- the film From the viewpoint of reducing the amount of solvent used, it is preferable to remove the film as it is. Further, from the viewpoint of reducing damage on the molding layer surface, dissolution and removal are preferable.
- the method of peeling and removing the temporary adhesive layer as it is means that the temporary adhesive layer is peeled as it is without performing chemical treatment such as using a peeling solution. A method of peeling and removing is more preferable. When peeling the temporary adhesive layer as it is, mechanical peeling is preferable.
- the adhesion strength B between the molding layer and the temporary adhesive layer 11 preferably satisfies the following formula (2).
- B ⁇ 4N / cm ⁇ ⁇ ⁇ Formula (2) When the temporary adhesive layer is removed using a stripping solution, the following stripping solution can be preferably used.
- the stripping solution water and a solvent (organic solvent) can be used.
- the organic solvent which melt
- the organic solvent include aliphatic hydrocarbons (hexane, heptane, isoper E, H, G (manufactured by Esso Chemical Co., Ltd.), limonene, p-menthane, nonane, decane, dodecane, decalin, etc.), aromatic Group hydrocarbons (toluene, xylene, anisole, mesitylene, ethylbenzene, propylbenzene, cumene, n-butylbenzene, sec-butylbenzene, isobutylbenzene, tert-butylbenzene, amylbenzene, isoamylbenzene, (2,2-dimethyl Propyl) benzene, 1-phenylene hydrocarbons (hexane, heptane,
- Polar solvents include alcohols (methanol, ethanol, propanol, isopropanol, 1-butanol, 1-pentanol, 1-hexanol, 1-heptanol, 1-octanol, 2-octanol, 2-ethyl-1-hexanol, 1 -Nonanol, 1-decanol, benzyl alcohol, ethylene glycol monomethyl ether, 2-ethoxyethanol, diethylene glycol monoethyl ether, diethylene glycol monohexyl ether, triethylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monomethyl ether, polyethylene glycol monomethyl Ether, polypropylene glycol, tetraethylene glycol, ethylene glycol monobutyl ether Ter, ethylene glycol monobenzyl ether, ethylene glycol monophenyl ether, propylene glycol monophenyl ether, methylphenyl carbinol,
- the stripping solution may contain an alkali, an acid, and a surfactant.
- the blending amount is preferably 0.1 to 5.0% by mass of the stripping solution.
- a form in which two or more organic solvents and water, two or more alkalis, an acid, and a surfactant are mixed is also preferable.
- alkali examples include tribasic sodium phosphate, tribasic potassium phosphate, tribasic ammonium phosphate, dibasic sodium phosphate, dibasic potassium phosphate, dibasic ammonium phosphate, sodium carbonate, potassium carbonate, and ammonium carbonate.
- Inorganic alkali agents such as sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate, sodium borate, potassium borate, ammonium borate, sodium hydroxide, ammonium hydroxide, potassium hydroxide and lithium hydroxide, monomethylamine, Dimethylamine, trimethylamine, monoethylamine, diethylamine, triethylamine, monoisopropylamine, diisopropylamine, triisopropylamine, n-butylamine, monoethanolamine, diethanolamine, triethanol Min, monoisopropanolamine, diisopropanolamine, ethyleneimine, ethylenediamine, pyridine, may be used an organic alkali agent such as tetramethylammonium hydroxide. These alkali agents can be used alone or in combination of two or more.
- Acids include inorganic acids such as hydrogen halide, sulfuric acid, nitric acid, phosphoric acid, boric acid, methanesulfonic acid, ethanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid, trifluoromethanesulfonic acid, acetic acid, citric acid
- Organic acids such as formic acid, gluconic acid, lactic acid, oxalic acid and tartaric acid can be used.
- an anionic, cationic, nonionic or zwitterionic surfactant can be used as the surfactant.
- the content of the surfactant is preferably 1 to 20% by mass and more preferably 1 to 10% by mass with respect to the total amount of the alkaline aqueous solution.
- anionic surfactant examples include, but are not limited to, fatty acid salts, abietic acid salts, hydroxyalkane sulfonic acid salts, alkane sulfonic acid salts, dialkyl sulfosuccinic acid salts, linear alkyl benzene sulfonic acid salts, branched alkyl benzene sulfonic acid salts, Alkylnaphthalene sulfonates, alkyl diphenyl ether (di) sulfonates, alkylphenoxy polyoxyethylene alkyl sulfonates, polyoxyethylene alkyl sulfophenyl ether salts, N-alkyl-N-oleyl taurine sodium, N-alkyl sulfosuccinic acid Monoamide disodium salts, petroleum sulfonates, sulfated castor oil, sulfated beef oil, sulfate esters of fatty acid alkyl
- the cationic surfactant is not particularly limited, and conventionally known cationic surfactants can be used. Examples thereof include alkylamine salts, quaternary ammonium salts, alkyl imidazolinium salts, polyoxyethylene alkylamine salts, and polyethylene polyamine derivatives.
- the nonionic surfactant is not particularly limited, but is a polyethylene glycol type higher alcohol ethylene oxide adduct, alkylphenol ethylene oxide adduct, alkyl naphthol ethylene oxide adduct, phenol ethylene oxide adduct, naphthol ethylene oxide adduct, fatty acid.
- Ethylene oxide adduct polyhydric alcohol fatty acid ester ethylene oxide adduct, higher alkylamine ethylene oxide adduct, fatty acid amide ethylene oxide adduct, fat and oil ethylene oxide adduct, polypropylene glycol ethylene oxide adduct, dimethylsiloxane-ethylene oxide block Copolymer, dimethylsiloxane- (propylene oxide-ethylene oxide) block copolymer , Fatty acid esters of polyhydric alcohol type glycerol, fatty acid esters of pentaerythritol, fatty acid esters of sorbitol and sorbitan, fatty acid esters of sucrose, alkyl ethers of polyhydric alcohols, fatty acid amides of alkanolamines.
- those having an aromatic ring and an ethylene oxide chain are preferable, and an alkyl-substituted or unsubstituted phenol ethylene oxide adduct or an alkyl-substituted or unsubstituted naphthol ethylene oxide adduct is more preferable.
- Zwitterionic surfactants include, but are not limited to, amine oxides such as alkyldimethylamine oxide, betaines such as alkylbetaines, and amino acids such as sodium alkylamino fatty acids.
- alkyldimethylamine oxide which may have a substituent alkylcarboxybetaine which may have a substituent
- alkylsulfobetaine which may have a substituent
- the compound represented by the formula (2) in paragraph [0256] of JP-A-2008-203359, the formula (I) and the formula (II) in paragraph [0028] of JP-A-2008-276166 are disclosed.
- a compound represented by the formula (VI), and compounds represented by paragraph numbers [0022] to [0029] of JP-A-2009-47927 can be used.
- additives such as an antifoaming agent and a water softening agent can be contained as required.
- the carrier substrate 12 is peeled from the thinned device wafer 60a provided with the molding layer
- the thinned device wafer 60a provided with the molding layer is subjected to various known treatments to reduce the thickness as necessary.
- a semiconductor device having the device wafer 60a is manufactured.
- the carrier base material can be regenerated by removing the temporary adhesive layer.
- a method of removing the temporary adhesive layer as a film, a method of physically removing by brush, ultrasonic wave, ice particles, aerosol spraying, a method of dissolving and removing by dissolving in an aqueous solution or an organic solvent, A chemical removal method such as a method of decomposing or vaporizing by irradiation with actinic rays, radiation, or heat can be mentioned, and conventionally known cleaning methods can be used depending on the carrier substrate. For example, when a device substrate is used as a carrier substrate, a conventionally known silicon wafer cleaning method can be used.
- an aqueous solution or an organic solvent that can be used for chemical removal includes strong acid, strong base, Strong oxidizers or mixtures thereof are raised, specifically, acids such as sulfuric acid, hydrochloric acid, hydrofluoric acid, nitric acid, organic acids, bases such as tetramethylammonium, ammonia, organic bases, hydrogen peroxide, etc.
- the carrier substrate cleaning liquid preferably contains an acid (strong acid) having a pKa of less than 0 and hydrogen peroxide.
- the acid having a pKa of less than 0 is selected from inorganic acids such as hydrogen iodide, perchloric acid, hydrogen bromide, hydrogen chloride, nitric acid and sulfuric acid, or organic acids such as alkylsulfonic acid and arylsulfonic acid.
- an inorganic acid is preferable, and sulfuric acid is most preferable.
- 30% by mass hydrogen peroxide water can be preferably used, and the mixing ratio of the strong acid and 30% by mass hydrogen peroxide water is preferably 0.1: 1 to 100: 1 by mass ratio. : 1 to 10: 1 is more preferable, and 3: 1 to 5: 1 is most preferable.
- FIGS. 3A to 3E are schematic cross-sectional views (FIGS. 3A and 3B) for explaining temporary adhesion between a carrier substrate and a device wafer provided with a molding layer, respectively.
- FIGS. 3C and 3D A state in which the device wafer having the molding layer temporarily bonded is thinned (FIG. 3C), a state in which the device wafer having the carrier substrate and the molding layer is peeled off (FIG. 3D), and a molding layer.
- FIG. 3A It is a schematic sectional drawing which shows the state (FIG.3 (E)) after removing a temporary adhesive layer from a device wafer.
- the point that the temporary adhesive layer 11 is formed on the surface of the molding layer 15 is different from the first embodiment.
- the temporary adhesive composition is applied (preferably applied) to the surface of the molding layer 15 and then dried (baked). Can do. Drying can be performed, for example, at 60 to 150 ° C. for 10 seconds to 2 minutes.
- FIG. 3B the carrier substrate 12 and the device wafer 60 provided with the molding layer 15 are pressure-bonded, and the carrier substrate 12 and the molding layer 15 are temporarily bonded.
- the back surface 61b of the device substrate 61 is subjected to mechanical or chemical treatment, and the thickness of the device substrate 61 is reduced as shown in FIG. A thinned device wafer 60a having a molding layer is obtained.
- the carrier substrate 12 is separated from the thinned device wafer 60a provided with a molding layer.
- the temporary adhesive layer 11 is removed from the thinned device wafer 60a provided with the molding layer.
- the method for manufacturing a semiconductor device according to the present invention is not limited to the above-described embodiment, and appropriate modifications and improvements can be made.
- the device wafer (device substrate) is mechanically or chemically treated as a device wafer thinning process and a through silicon via formation process, but is not limited thereto. Any processing required in the method of manufacturing a semiconductor device is included.
- the shape, dimensions, number, arrangement location, and the like of the circuit surface in the device wafer exemplified in the above-described embodiment are arbitrary and are not limited.
- ⁇ Method of forming molding layer Z> In molding layer X, Sumicon EME-G770 (manufactured by Sumitomo Bakelite) was changed to a liquid molding material (CEL-C-5400) and baked at 100 ° C for 30 minutes and then at 150 ° C for 2 hours to form a molding layer. did.
- ⁇ Composition 1 for temporary adhesion> -Septon S2104 (manufactured by Kuraray): 45 parts by mass-Tuftec P2000 (manufactured by Asahi Kasei Chemicals: 45 parts by mass)-Irganox 1010 (manufactured by BASF): 5 parts by mass-Sumitizer TP-D (manufactured by Sumitomo Chemical): 5 parts by mass F-553 (manufactured by DIC): 0.1 parts by mass / mesitylene (manufactured by Toyo Gosei): 190 parts by mass
- ⁇ Measurement of amount of component having molecular weight of 1000 or less in molding layer For the molding layer after performing any one or more of heat treatment, solvent washing treatment, and ashing treatment, the amount (mass%) of the component having a molecular weight of 1000 or less was measured using GCMS (Shimadzu Corporation, model number: P2010), and the headspace Part oven temperature 180 ° C., needle temperature 180 ° C., transfer temperature 200 ° C., pressurization time 3 minutes, carrier gas 140 kPa, gas chromatography column vaporization chamber temperature 220 ° C., RESTX Rtx column (length 60 m), 40 ° C. to 310 ° C. The gas generated under the conditions of a temperature rising rate of 10 ° C./min, a mass spectrum in scan mode, an interface temperature of 220 ° C., and an ion source temperature of 200 ° C. was measured.
- the film surface on the temporary adhesive layer side of the obtained laminate B is perpendicular to the film surface of the temporary adhesive layer at a magnification of 50 times with an optical microscope (manufacturer: Olympus, product number: MX-80).
- the number of voids having a maximum length of 30 ⁇ m or more per 700 cm 2 of the temporary adhesive layer was measured.
- ⁇ Arithmetic surface roughness (Ra)> The arithmetic average surface roughness (Ra) of the surface of the obtained laminate B on the temporary adhesive layer side was measured using a stylus type surface roughness meter (manufacturer: KLA-Tencor, product number: P-15). . The unit is shown in ⁇ m.
- a molding layer was formed on the surface of a 12-inch silicon wafer provided with a circuit surface on the surface by the molding layer X method to obtain a laminate A, and then the surface of the molding layer was subjected to a solvent cleaning treatment.
- a temporary bonding composition 1 was applied to each of the surface of the molding layer of the laminate A and the surface of another 12-inch silicon wafer (carrier substrate) at 50 rpm with a wafer bonding apparatus (Tokyo Electron, Synapse V). While rotating, 7.5 mL was dropped during 30 seconds, heated at 110 ° C. for 3 minutes using a hot plate, and further heated at 190 ° C. for 3 minutes, so that the temporary adhesive layer was formed on the laminate A.
- a layered product B in which a temporary adhesive layer was formed on the formed layered product B and a carrier substrate was obtained.
- the laminated body B and the laminated body E are pressure-bonded at 190 ° C. and a pressure of 0.11 MPa for 3 minutes under a vacuum by a wafer bonder wafer bonding apparatus (manufactured by Tokyo Electron, Synapse V) so that the temporary adhesive layer side is in contact.
- a laminated body F was obtained.
- the previously used silicon wafer side of the laminate F was polished to a thickness of 35 ⁇ m using a back grinder DFG8540 (manufactured by Disco) to obtain a thin laminate G.
- the arithmetic surface roughness (Ra) and the number of voids were measured in the same manner as described above. As a result, each was 1.1 ⁇ m and the number of cracks in the thinned laminate G was 0. It was a piece.
- the laminate of the present invention suppresses cracks in the device wafer after being thinned.
- a crack occurs in a device wafer, there arises a problem that the yield of device chips is reduced due to breakage.
- the present invention is highly technical in that the number of cracks can be greatly reduced.
- Temporary adhesive layer 12 Carrier base material 15: Molding layer 60: Device wafer 60a: Thinning device wafer 61: Device substrate 61a: Front surface 61b :, 61b1: Back surface 62: Circuit surface
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Abstract
Description
電子機器の更なる小型化および高性能化のニーズに伴い、電子機器に搭載されるICチップについても更なる小型化および高集積化が求められているが、デバイスウェハの面方向における集積回路の高集積化は限界に近づいている。
しかしながら、厚さ200μm以下のデバイスウェハは非常に薄く、これを基材とする半導体デバイス製造用部材も非常に薄いため、このような部材に対して更なる処理を施したり、あるいは、このような部材を単に移動したりする場合等において、部材を安定的に、かつ、損傷を与えることなく支持することは困難である。
例えば、特許文献1には、接着剤層を介してウェハに貼り付けられた支持体を、ウェハから剥離する剥離方法であって、上記仮接着剤層を膨潤させて、その表面の接着性を低下させる溶剤を、上記仮接着剤層に供給する溶剤供給工程と、上記ウェハから、膨潤した上記仮接着剤層を剥離する剥離工程と、を包含することを特徴とする剥離方法が開示されている。
ここで、モールディング材料を用いる技術として、例えば、特許文献1には、基板と、基板の少なくとも一方側に設けられる半導体素子と、基板と、半導体素子と、半導体素子との間を充填する第1の樹脂組成物を硬化させて得られる第1の樹脂と、基板と、第1の樹脂とを覆い、第1の樹脂組成物を硬化した後に、第2の樹脂組成物を硬化させて得られる第2の樹脂と、を有し、第1の樹脂と第2の樹脂との接着強度が、室温で18MPa以上であることを特徴とする半導体装置が開示されている。
本発明はかかる課題を解決することを目的としたものであって、モールディング材料でデバイスウェハの回路面を覆った後、その表面に仮接着剤層を設けて、デバイスウェハとキャリア基材を貼り合せても、良好なデバイスウェハの加工性を達成できる積層体を提供することを目的とする。
<1>回路面を有するデバイスウェハ、上記回路面の表面を覆うモールディング層、上記モールディング層の表面に位置する仮接着剤層を有する積層体であって、
上記仮接着剤層の膜面に垂直な方向から光学顕微鏡で観察した、最大長さ30μm以上のボイドの数が、仮接着剤層の膜面700cm2あたり、3個以下であり、上記仮接着剤層の算術平均表面粗さであるRaがRa≦10.0μmである、積層体。
<2>モールディング層における、分子量1000以下の成分が5質量%以下である、<1>に記載の積層体。
<3>上記モールディング層が、液状のモールディング材料をベークすることで形成されてなる、<1>または<2>に記載の積層体。
<4>上記モールディング層が、固体のコンプレッションモールディング材料により形成されてなる、<1>または<2>に記載の積層体。
<5>モールディング層に処理を行った後、仮接着剤層を設けてなり、上記処理後のモールディング層の100℃から200℃まで、10℃/分で昇温した際の、熱質量減少度が、5質量%以下である、<1>~<4>のいずれかに記載の積層体。
<6>上記回路面の表面を覆っているモールディング層を100℃~250℃で加熱処理した後に、仮接着剤層を設けてなる、<5>のいずれかに記載の積層体。
<7>上記回路面の表面を覆っているモールディング層の表面を有機溶剤で洗浄した後に、仮接着剤層を設けてなる、<5>または<6>に記載の積層体。
<8>上記回路面の表面を覆っているモールディング層の表面をアッシング処理した後に、仮接着剤層を設けてなる、<5>~<7>のいずれかに記載の積層体。
<9>上記回路面の表面を覆っているモールディング層を100℃~250℃で加熱処理すること、上記回路面の表面を覆っているモールディング層の表面を有機溶剤で洗浄すること、および、上記回路面の表面を覆っているモールディング層の表面をアッシング処理することのうち、2つ以上を行った後に、仮接着剤層を設けてなる、<1>~<8>のいずれかに記載の積層体。
<10>上記アッシング処理は、酸素プラズマで行う、<8>または<9>に記載の積層体。
<11>モールディング層および仮接着剤層が、それぞれ独立に、樹脂を含む、<1>~<10>のいずれかに記載の積層体。
<12>上記仮接着剤層の、モールディング層と接している側と反対側の上に、キャリア基材を有する、<1>~<11>のいずれかに記載の積層体。
<13>上記デバイスウェハの厚さが、200μm以下である、<1>~<12>のいずれかに記載の積層体。
<14>上記仮接着剤層が、キャリア基材と接している、<1>~<13>のいずれかに記載の積層体。
<15>上記仮接着剤層が1層である、<14>に記載の積層体。
本明細書における基(原子団)の表記において、置換および無置換を記していない表記は、置換基を有さないものと共に置換基を有するものをも包含するものである。例えば、「アルキル基」とは、置換基を有さないアルキル基(無置換アルキル基)のみならず、置換基を有するアルキル基(置換アルキル基)をも包含するものである。
本明細書中における「活性光線」または「放射線」は、例えば、可視光線、紫外線、遠紫外線、電子線、X線等を含むものを意味する。
本明細書において、「光」とは、活性光線または放射線を意味している。
本明細書において、「露光」とは、特に断らない限り、水銀灯、紫外線、エキシマレーザーに代表される遠紫外線、X線、極端紫外線光(EUV光)等による露光のみならず、電子線およびイオンビーム等の粒子線による描画をも意味している。
本明細書において、全固形分とは、組成物の全組成から溶剤を除いた成分の総質量をいう。
本明細書において、「(メタ)アクリレート」は、アクリレートおよびメタアクリレートを表し、「(メタ)アクリル」は、アクリルおよびメタクリルを表し、「(メタ)アクリロイル」は、「アクリロイル」および「メタクリロイル」を表す。
本明細書において、重量平均分子量および数平均分子量は、特記しない限り、ゲルパーミエーションクロマトグラフィー(GPC)測定によるポリスチレン換算値として定義される。本明細書において、重量平均分子量(Mw)および数平均分子量(Mn)は、例えば、HLC-8220(東ソー(株)製)を用い、カラムとしてTSKgel Super AWM―H(東ソー(株)製、内径(ID)6.0mm×15.0cm)を、溶離液として10mmol/L リチウムブロミドNMP(N-メチルピロリドン)溶液を用いることによって求めることができる。
本明細書において、「親油基」とは、親水性基を含まない官能基を意味する。また、「親水性基」とは、水との間に親和性を示す官能基を意味する。
なお、以下に説明する実施の形態において、既に参照した図面において説明した部材等については、図中に同一符号あるいは相当符号を付すことにより説明を簡略化あるいは省略する。
このメカニズムは推定であるが、モールディング層の表面に仮接着剤層を設けることにより、モールディング層由来のアウトガスが発生し、このアウトガスが仮接着剤層にボイドを形成したり、仮接着剤層の表面を粗くしていると考えられる。そして、このような仮接着剤層のボイドや表面の粗さは、わずかなものではあるが、デバイスウェハの薄膜化においては、大きな影響を与えることが分かった。そして、仮接着剤層のボイドの数を所定の値以下とし、さらに、算術平均表面粗さ(Ra)を所定の値以下とすることにより、デバイスウェハの加工性を顕著に向上させたものである。仮接着剤層のわずかなボイドや表面の粗さがデバイスウェハの加工性に大きな影響を与えることは驚くべきことである。
図1は、本発明の積層体1の層構成を示す断面概略図であって、61はデバイスウェハの基板(デバイス基板)を、62デバイスウェハの表面に位置する回路面を、15は回路面を覆うモールディング層を、11はモールディング層の表面に位置する仮接着剤層を、12はキャリア基材をそれぞれ示している。本発明の積層体1は、基板61表面の回路面62をモールディング層15で覆った後、仮接着剤層11の、モールディング層15と接している側と反対側の上に、キャリア基材12を設けている。図1では、キャリア基材12は、仮接着剤層11と接しているが、キャリア基材12と仮接着剤層11の間に他の層があっても良い。
積層体1の各構成要素の詳細な説明については、後述する。
本発明では、仮接着剤層の膜面に垂直な方向から光学顕微鏡で観察した、最大長さ30μm以上のボイドの数を、仮接着剤層の膜面700cm2あたり、3個以下とし、かつ、仮接着剤層の表面の算術平均表面粗さであるRaをRa≦10.0μmとすることにより、この点を解決している。
ここで、最大長さとは、仮接着剤層の膜面に垂直な方向から光学顕微鏡で観察したボイド部分の外周上の2点の長さのうち、最も長いものの長さをいう。例えば、ボイドが円形の場合、円の直径が最大長さとなる。
また、本発明におけるボイドは、仮接着剤層の膜表面が窪んで形成されているものであってもよいし、仮接着剤層の内部に形成されているボイドであってもよい。仮接着剤層の内部に形成されるボイドは、通常球状である。
尚、「仮接着剤層の膜面700cm2あたり」とは、仮接着剤層を平面と仮定した膜面の面積を意味する。つまり、光学顕微鏡で観察される面の面積に対する、ボイドの数となる。
ボイドの数の測定方法は、具体的には実施例に記載の方法に従う。但し、実施例に記載の機器等が廃版等で入手困難な場合、他の機能を有する機器等を採用できる。
上記揮発する成分の量は、モールディング層に対し、1質量%以下がより好ましい。また、上記分子量1000以下の成分の量は、2質量%以下がより好ましく、1.5質量%以下がさらに好ましく、0.9質量%以下とすることもできる。下限値については、0質量%が望ましいが、実施形態の一例として、0.001質量%以上であることが挙げられる。
本発明における分子量1000以下の成分の量の測定方法は、それぞれ、後述する実施例に記載の方法に従う。
ベーク温度については、モールディング材料の種類等にもよるが、例えば、100~200℃とすることができ、さらには、150~300℃とすることができる。
本発明における熱質量減少度の測定方法は、後述する実施例に記載の方法に従う。
洗浄は、モールディング層を有機溶剤に浸漬しても良いし、モールディング層をスピンさせた状態で、モールディング層の表面を有機溶剤でリンスしてもよい。
アッシング処理は、オゾンによるアッシング処理、酸素プラズマおよびアルゴンプラズマによるアッシング処理、および、酸素プラズマによるアッシング処理が例示され、酸素プラズマによるアッシング処理がより好ましい。
このように、2種類以上の手段を組み合わせることにより、より効果的に仮接着剤層のボイドの数を減らし、表面粗さを抑制できる。本発明では、特に、上記手段を2~4種類組み合わせることが好ましく、2種類または3種類組み合わせることがより好ましく、2種類組み合わせることが特に好ましい。
モールディング層を形成するモールディング材料は、本発明の趣旨を逸脱しない限り、特に定めるものでは無いが、樹脂を含むことが好ましく、硬化性樹脂を含むことがより好ましい。また、モールディング材料は、無機充填材および硬化剤の少なくとも1種を含むことが好ましく、さらに他の成分を含んでいても良い。
特に、モールディング層の主成分の樹脂としてエポキシ樹脂を用い、仮接着剤層の主成分の樹脂としてスチレン系エラストマーを用いることが好ましい実施形態として例示される。このような組み合わせを採用することにより、デバイスウェハの研磨時に必要な密着性を保ちつつ、剥離時に容易に剥離でき好ましい。尚、ここでの主成分の樹脂とは、モールディング層または仮接着剤層に含まれる樹脂成分のうち、最も含有量が多い成分のことをいい、通常は、上記樹脂成分の80質量%以上である。
樹脂として、上述のエポキシ樹脂を用いる場合、硬化剤は、特に限定されないが、フェノール性水酸基を有する硬化剤を用いるのが好ましい。フェノール性水酸基を有する硬化剤は、他の硬化剤と比較して樹脂の反応を制御することが容易となるため、半導体装置を製造する際の良好な流動性を確保することができる。また、フェノール性水酸基を有する硬化剤は、その反応性制御が容易なことにより無機充填材の高充填化も可能となる。そのため、半導体装置の優れた信頼性を確保することができる。ここでフェノール性水酸基を有する硬化剤とは、1分子内にフェノール性水酸基を2個以上有するモノマー、オリゴマー、ポリマー全般であり、その分子量、分子構造を特に限定するものではない。具体的にはフェノールノボラック樹脂、クレゾールノボラック樹脂などのノボラック型フェノール樹脂、トリフェノールメタン型フェノール樹脂、テルペン変性フェノール樹脂、ジシクロペンタジエン変性フェノール樹脂などの変性フェノール樹脂、フェニレンおよび/またはビフェニレン骨格を有するフェノールアラルキル樹脂、フェニレンおよび/またはビフェニレン骨格を有するナフトールアラルキル樹脂などのアラルキル型フェノール樹脂、ビスフェノール化合物などが挙げられ、これらは単独でも混合して使用してもよい。
また、上記樹脂がエポキシ樹脂である場合、硬化剤としてフェノール性水酸基を有する硬化剤が好ましく用いられ、その場合、上記エポキシ樹脂のエポキシ基とフェノール性水酸基を有する硬化剤のフェノール性水酸基との当量比(エポキシ基/フェノール性水酸基)は、特に限定されないが、0.5~2.0が好ましく、特に0.7~1.5が好ましい。当量比が上記範囲内であると、特に硬化性および耐湿信頼性に優れる。
液状のモールディング材料を用いてベークする場合90℃~110℃、15分~30分予備ベークしたのち、120℃~150℃、2時間~4時間追加でベークすることでモールディング材料を成膜することができる。
溶融樹脂を用いる場合、モールディング材料は、例えばミキサーなどを用いて原料を充分に均一に混合した後、更に熱ロール、ニーダー、押出機などの混練機で溶融混練し、冷却後粉砕して得られる。
モールディング材料で封止する際の粘度は、特に限定されないが、例えば、3.0Pa・s以上、好ましくは、5.0Pa・s以上である。一方、かかる粘度は、好ましくは30.0Pa・s以下、より好ましくは20.0Pa・s以下である。これにより、ボイドの発生を抑制できる。
粘度は、例えば高化式フローテスターなどで求めることができる。
モールディング材料で封止した後に、モールディング材料を硬化する。モールディング材料を硬化する方法としては、加熱する方法、光照射する方法などが挙げられる。
上記のモールディング材料の加熱硬化後に、さらに、モールディング材料を加熱することにより、後硬化することも好ましい。
デバイスウェハは、デバイス基板とその表面に位置する回路面を有する。デバイス基板としては、公知のものを制限なく使用することができ、例えば、シリコン基板、化合物半導体基板などが挙げられる。化合物半導体基板の具体例としては、SiC基板、SiGe基板、ZnS基板、ZnSe基板、GaAs基板、InP基板、GaN基板などが挙げられる。
デバイスウェハの表面には、回路面を有する。回路面を有するデバイスウェハとしては、例えば、MEMS(Micro Electro Mechanical Systems)、パワーデバイス、イメージセンサー、マイクロセンサー、発光ダイオード(LED)、光学デバイス、インターポーザー、埋め込み型デバイス、マイクロデバイスなどが挙げられる。
デバイスウェハは、金属バンプ等の構造を有していることが好ましい。本発明によれば、表面に構造を有しているデバイスウェハに対しても、安定して仮接着できるとともに、デバイスウェハに対する仮接着を容易に解除できる。構造の高さは、特に限定はないが、例えば、1~150μmが好ましく、5~100μmがより好ましい。
薄型化した後のデバイスウェハの膜厚は、例えば、500μm未満が好ましく、400μm以下がより好ましく、300μm以下が更に好ましく、200μm以下が一層好ましく、100μm以下がより一層好ましく、50μm以下がさらに一層好ましい。下限は、例えば、1μm以上が好ましく、5μm以上がより好ましく、20μm以上がさらに好ましい。
キャリア基材としては、シリコンウェハ、SiCウェハ、GaNウェハ等の各種ウェハ、ガラス、有機基材等の各種材質の基板、および、基板上に有機膜や無機膜が形成されたものが例示される。キャリア基材の厚みは、特に限定されるものではないが、例えば、300μm~100mmが好ましく、300μm~10mmがより好ましい。
上述のとおり、本発明の積層体は、キャリア基材(図1の12)と仮接着剤層(図1の11)の間に他の層を有していてもよい。他の層としては、キャリア基材と仮接着剤層の分離を容易にするための層(分離層や剥離層と称されることがある)が例示される。キャリア基材と仮接着剤層の分離を容易にするための層としては、光や熱等をかけることによって変性し、デバイス基板と仮接着剤層の間を分離させる層や、特定の溶剤に溶解しやすい層であって、積層体のデバイス基板を薄型化した後に、特定の溶剤に浸漬して、デバイス基板とキャリア基材を分離する態様などが例示される。これらの層の例としては、例えば、特開2014-212292号公報の段落0025~0055の記載、および、WO2013-065417号パンフレットの段落0069~0124の記載を参酌でき、これらの内容は本明細書に組み込まれる。
仮接着剤層は、モールディング層とキャリア基材とを、貼りあわせるために用いる。貼りあわせは、通常、加熱圧着することにより製造できる。従来は、加熱圧着の際に、アウトガスが生じて、デバイスウェハにクラックを生じさせていたが、本発明では、仮接着剤層のボイドの数および表面の粗さを所定の値以下とすることにより、この問題を回避している。
加圧接着条件は、例えば、温度100~210℃、圧力0.01~1MPa、時間1~15分が好ましい。
本発明における仮接着剤層がバインダーを含む場合、バインダーは、仮接着剤層の全固形分中に50.00~99.99質量%の割合で含まれることが好ましく、70.00~99.99質量%がより好ましく、88.00~99.99質量%が特に好ましい。
また、バインダーとしてエラストマーを用いる場合、エラストマーは、仮接着剤層の全固形分中に50.00~99.99質量%の割合で含まれることが好ましく、70.00~99.99質量%がより好ましく、88.00~99.99質量%が特に好ましい。
バインダーの詳細については、後述する。
本発明における仮接着剤層は、酸化防止剤などのその他添加剤をさらに含むことができる。これらの詳細については、後述する。
本発明では、仮接着剤層は1層であっても、2層以上であってもよいが、1層(例えば、単層)が好ましい。
仮接着剤層は、上述のとおり、モールディング層の表面に位置するように形成される。仮接着剤層は、モールディング層の表面に形成してもよいし、キャリア基材の上に設けてモールディング層と貼りあわせてもよいし、モールディング層とは、別の支持体の表面に形成して、転写してもよい。また、モールディング層上に仮接着剤層A、キャリア基材上に仮接着剤層Bをそれぞれ設け、仮接着剤層Aと仮接着剤層Bとを接着させてもよい。この場合、仮接着剤層Aと仮接着剤層Bとは同じであっても異なっていてもよい。異なっている場合、後述するバインダー成分の種類を変えたり、あるいはバインダー成分以外の添加剤の種類や添加量を変えることで、剥離選択性(モールディング層界面とキャリア基材界面の剥離選択性)や剥離力を適宜調整することができる。
以下、別の支持体の表面に形成する場合を例にとって仮接着剤層の製造方法について説明するが、モールディング層の表面およびキャリア基材の上に形成する場合も、同様に行うことができる。
仮接着用組成物の適用方法として、スピンコート法、ブレードコート法、スプレー法、ローラーコート法、フローコート法、ドクターコート法、スクリーン印刷法、ディップコート法などが挙げられ、スピンコート法およびブレードコート法が好ましい。また、スリット状の開口から仮接着用組成物を圧力で押し出して、支持体上に仮接着用組成物を塗布する方法であってもよい。
仮接着用組成物の塗布量は、用途により異なるが、たとえば、乾燥後の仮接着剤層の平均膜厚が0.1~500μmとなる塗布量が好ましい。下限は、1μm以上が好ましい。上限は、200μm以下が好ましく、100μm以下がより好ましい。
なお、本発明において、仮接着剤層の平均膜厚は、仮接着剤層の一方向に沿った断面において、一方の端面から他方の端面に向かって、等間隔で5か所の場所における膜厚を、マイクロメータにより測定した値の平均値と定義する。また、本発明において、「仮接着剤層の一方向に沿った断面」とは、仮接着剤層が多角形状である場合は、長辺方向に直交する断面とする。また、仮接着剤層が正方形状である場合は、いずれか一方の辺に直交する断面とする。また、仮接着剤層が円形または楕円形である場合は、重心を通過する断面とする。
乾燥条件は、仮接着用組成物の種類や、仮接着剤層の膜厚により異なる。乾燥条件は、例えば、60~220℃で、10~600秒が好ましい。乾燥温度は、80~200℃がより好ましい。乾燥時間は、30~500秒がより好ましく、40~400秒が更に好ましい。
乾燥は、二段階に分けて段階的に温度を上げて実施してもよい。例えば、90~130℃で、30秒~250秒加熱した後、170~220℃で、30秒~250秒加熱することが挙げられる。
支持体上に仮接着剤層(フィルム)を形成した場合、フィルム状の仮接着剤層は、支持体から剥がした仮接着剤層のみからなる膜であってもよいし、一方の表面に剥離シートを有する仮接着剤層であってもよいし、両面に剥離シートを有する仮接着剤層であってもよい。
これらの処理を連続的に行うことで、ロール状の長尺フィルムを得ることができる。長尺フィルムの長さは、特に限定はないが、下限は、例えば5000mm以上が好ましく、1000mm以上がより好ましい。上限は、例えば500000mm以下が好ましく、200000mm以下がより好ましい。剥離シートは、使用する際に剥離除去する。
支持体上に仮接着剤層を形成した場合、モールディング層表面およびキャリア基材の上の一方に、フィルム状の仮接着剤層を適用し、熱および圧力をかけてラミネートすることで形成することが好ましい。
本発明で用いる仮接着用組成物は、バインダーを少なくとも1種含むことが好ましい。本発明において、バインダーは、上記仮接着剤層の各種特性を達成できる限り、その種類等は特に定めるものでは無い。
バインダーは、ブロック共重合体、ランダム共重合体、グラフト共重合体が挙げられ、ブロック共重合体が好ましい。ブロック共重合体であれば、加熱プロセス時の仮接着用組成物の流動を抑えることができるため、加熱プロセス時においても接着を維持でき、また加熱プロセス後でも剥離性が変化しないという効果が期待できる。
バインダーの種類としては、特に限定はなく、ポリスチレン系共重合体、ポリエステル系共重合体、ポリオレフィン系共重合体、ポリウレタン系共重合体、ポリアミド系共重合体、ポリアクリル系共重合体、シリコーン系共重合体、ポリイミド系共重合体などが使用できる。特に、ポリスチレン系共重合体、ポリエステル系共重合体、ポリアミド系共重合体が好ましく、耐熱性と剥離性の観点からポリスチレン系共重合体がより好ましい。なかでも、バインダーは、スチレンと他のモノマーとのブロック共重合体であることが好ましく、片末端または両末端がスチレンブロックのスチレンブロック共重合体が特に好ましい。
また、バインダーは、ブロック共重合体の水添物が好ましい。バインダーが水添物であると、熱安定性や保存安定性が向上する。さらには、剥離性および剥離後の仮接着剤層の洗浄除去性が向上する。なお、水添物とは、ブロック共重合体が水添された構造の重合体を意味する。
なお、本明細書において、エラストマーとは、弾性変形を示す高分子化合物を表す。すなわち外力を加えたときに、その外力に応じて瞬時に変形し、かつ外力を除いたときには、短時間に元の形状を回復する性質を有する高分子化合物と定義する。
本発明において、エラストマーの重量平均分子量は、2,000~200,000以下が好ましく、10,000~200,000がより好ましく、50,000~100,000がさらに好ましい。この範囲にあることで、キャリア基材をデバイスウェハから剥離後、デバイスウェハおよび/またはキャリア基材に残存するエラストマー由来の残渣を除去する際にも、溶剤への溶解性が優れるため、デバイスウェハやキャリア基材などに残渣が残らないなど利点がある。
本発明で用いるエラストマーは、元の大きさを100%としたときに、室温(20℃)において小さな外力で200%まで変形させることができ、かつ外力を除いたときに、短時間で130%以下に戻る性質を有することが好ましい。
ポリスチレン系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、スチレン-ブタジエン-スチレンブロック共重合体(SBS)、スチレン-イソプレン-スチレンブロック共重合体(SIS)、スチレン-エチレン-ブチレン-スチレンブロック共重合体(SEBS)、スチレン-ブタジエン-ブチレン-スチレン共重合体(SBBS)およびこれらの水添物、スチレン-エチレン-ブチレン-スチレンブロック共重合体(SEBS)、スチレン-エチレン-プロピレン-スチレンブロック共重合体(SEPS)、スチレン-エチレン-エチレン-プロピレン-スチレンブロック共重合体等が挙げられる。
すなわち、エラストマーAは、比較的柔らかい材料であるため、弾性を有する仮接着剤層を形成しやすい。このため、本発明で用いる仮接着用組成物を用いて基材と支持体との積層体を製造し、基材を研磨して薄膜化する際に、研磨時の圧力が局所的に加わっても、仮接着剤層が弾性変形して元の形状に戻り易くできる。その結果、優れた平坦研磨性が得られる。また、研磨後の積層体を、加熱処理し、その後冷却しても、仮接着剤層によって、冷却時に発生する内部応力を緩和でき、反りの発生を効果的に抑制できる。
また、上記エラストマーBは、比較的硬い材料であるため、エラストマーBを含むことで、剥離性に優れた仮接着剤層を製造できる。
エラストマーAの硬度は、20~82が好ましく、60~79がより好ましい。なお、硬度は、JIS(日本工業規格)K6253の方法に従い、タイプAデュロメーターで測定した値である。
エラストマーBの硬度は、83~100が好ましく、90~99がより好ましい。
また、ポリスチレン系エラストマーは水添物であると、熱に対する安定性が向上し、分解や重合等の変質が起こりにくい。さらに、溶剤への溶解性およびレジスト溶剤への耐性の観点からもより好ましい。
ポリスチレン系エラストマーの不飽和二重結合量としては、剥離性の観点から、ポリスチレン系エラストマー1gあたり、15mmol未満であることが好ましく5mmol未満であることがより好ましく、0.5mmol未満であることが最も好ましい。なお、ここでいう不飽和二重結合量は、スチレン由来のベンゼン環内の不飽和二重結合を含まない。不飽和二重結合量は、NMR(核磁気共鳴)測定により算出することができる。
ポリエステル系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、ジカルボン酸又はその誘導体と、ジオール化合物又はその誘導体とを重縮合して得られるものが挙げられる。
ジカルボン酸としては、例えば、テレフタル酸、イソフタル酸、ナフタレンジカルボン酸等の芳香族ジカルボン酸及びこれらの芳香環の水素原子がメチル基、エチル基、フェニル基等で置換された芳香族ジカルボン酸、アジピン酸、セバシン酸、ドデカンジカルボン酸等の炭素数2~20の脂肪族ジカルボン酸、及びシクロヘキサンジカルボン酸などの脂環式ジカルボン酸などが挙げられる。これらは、1種単独で使用してもよく、2種以上併用してもよい。
ジオール化合物としては、例えば、エチレングリコール、1,3-プロパンジオール、1,4-ブタンジオール、1,6-ヘキサンジオール、1,10-デカンジオール、1,4-シクロヘキサンジオールなどの脂肪族ジオール、脂環式ジオール、下記構造式で表される2価のフェノールなどが挙げられる。
また、ポリエステル系エラストマーとして、芳香族ポリエステル(例えば、ポリブチレンテレフタレート)部分をハードセグメント成分に、脂肪族ポリエステル(例えば、ポリテトラメチレングリコール)部分をソフトセグメント成分にしたマルチブロック共重合体を用いることもできる。マルチブロック共重合体としては、ハードセグメントとソフトセグメントとの種類、比率、及び分子量の違いによりさまざまなグレードのものが挙げられる。具体例としては、ハイトレル(デュポン-東レ(株)製)、ペルプレン(東洋紡(株)製)、プリマロイ(三菱化学製)、ヌーベラン(帝人化成製)、エスペル1612、1620(日立化成工業(株)製)などが挙げられる。
ポリオレフィン系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、エチレン、プロピレン、1-ブテン、1-ヘキセン、4-メチル-ペンテン等の炭素数2~20のα-オレフィンの共重合体などが挙げられる。例えば、エチレン-プロピレン共重合体(EPR)、エチレン-プロピレン-ジエン共重合体(EPDM)等が挙げられる。また、ジシクロペンタジエン、1,4-ヘキサジエン、シクロオクタジエン、メチレンノルボルネン、エチリデンノルボルネン、ブタジエン、イソプレンなどの炭素数2~20の非共役ジエンとα-オレフィン共重合体などが挙げられる。また、ブタジエン-アクリロニトリル共重合体にメタクリル酸を共重合したカルボキシ変性ニトリルゴムが挙げられる。具体的には、エチレン-α-オレフィン共重合体ゴム、エチレン-α-オレフィン・非共役ジエン共重合体ゴム、プロピレン-α-オレフィン共重合体ゴム、ブテン-・α-オレフィン共重合体ゴムなどが挙げられる。
市販品として、ミラストマー(三井化学(株)製)、サーモラン(三菱化学製)EXACT(エクソン化学製)、ENGAGE(ダウケミカル製)、エスポレックス(住友化学製)、Sarlink(東洋紡製)、ニューコン(日本ポリプロ製)、EXCELINK(JSR製)などが挙げられる。
ポリウレタン系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、低分子のグリコールおよびジイソシアネートからなるハードセグメントと、高分子(長鎖)ジオールおよびジイソシアネートからなるソフトセグメントとの構造単位を含むエラストマーなどが挙げられる。
高分子(長鎖)ジオールとしては、ポリプロピレングリコール、ポリテトラメチレンオキサイド、ポリ(1,4-ブチレンアジペート)、ポリ(エチレン・1,4-ブチレンアジペート)、ポリカプロラクトン、ポリ(1,6-ヘキシレンカーボネート)、ポリ(1,6-ヘキシレン・ネオペンチレンアジペート)などが挙げられる。高分子(長鎖)ジオールの数平均分子量は、500~10,000が好ましい。
低分子のグリコールとしては、エチレングリコール、プロピレングリコール、1,4-ブタンジオール、ビスフェノールA等の短鎖ジオールを用いることができる。短鎖ジオールの数平均分子量は、48~500が好ましい。
ポリウレタン系エラストマーの市販品としては、PANDEX T-2185、T-2983N(DIC(株)製)、ミラクトラン(日本ミラクトラン製)、エラストラン(BASF製)、レゼミン(大日精化工業製)、ペレセン(ダウ・ケミカル製)、アイアンラバー(NOK社製)、モビロン(日清紡ケミカル製)などが挙げられる。
ポリアミド系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、ポリアミド-6、11、12などのポリアミドをハードセグメントに用い、ポリオキシエチレン、ポリオキシプロピレン、ポリテトラメチレングリコールなどのポリエーテルおよび/またはポリエステルをソフトセグメントに用いたエラストマーなどが挙げられる。このエラストマーは、ポリエーテルブロックアミド型、ポリエーテルエステルブロックアミド型の2種類に大別される。
市販品として、UBEポリアミドエラストマー、UBESTA XPA(宇部興産(株)製)、ダイアミド(ダイセルエボニック(株)製)、PEBAX(ARKEMA社製)、グリロンELX(エムスケミージャパン(株)製)、ノパミッド(三菱化学(株)製)、グリラックス(東洋紡製)、ポリエーテルエステルアミドPA-200、PA-201、TPAE-12、TPAE-32、ポリエステルアミドTPAE-617、TPAE-617C((株)T&K TOKA製)などが挙げられる。
ポリアクリル系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、エチルアクリレート、ブチルアクリレート、メトキシエチルアクリレート、エトキシエチルアクリレートなどのアクリル酸エステルを主成分としたものや、
アクリル酸エステルと、グリシジルメタクリレート、アリルグリシジルエーテルなどとが共重合してなるものが挙げられる。さらに、アクリロニトリルやエチレンなどの架橋点モノマーとを共重合してなるものなどが挙げられる。具体的には、アクリロニトリル-ブチルアクリレート共重合体、アクリロニトリル-ブチルアクリレート-エチルアクリレート共重合体、アクリロニトリル-ブチルアクリレート-グリシジルメタクリレート共重合体などが挙げられる。
シリコーン系エラストマーとしては、特に制限はなく、目的に応じて適宜選択することができる。例えば、オルガノポリシロキサンを主成分としたもので、ポリジメチルシロキサン系、ポリメチルフェニルシロキサン系、ポリジフェニルシロキサンなどが挙げられる。市販品の具体例としては、KEシリーズ(信越化学工業(株)製)、SEシリーズ、CYシリーズ、SHシリーズ(以上、東レダウコーニングシリコーン(株)製)などが挙げられる。
本発明では、エラストマーとして、ゴム変性したエポキシ樹脂(エポキシ系エラストマー)を用いることができる。エポキシ系エラストマーは、例えば、ビスフェノールF型エポキシ樹脂、ビスフェノールA型エポキシ樹脂、サリチルアルデヒド型エポキシ樹脂、フェノールノボラック型エポキシ樹脂あるいはクレゾールノボラック型エポキシ樹脂の一部又は全部のエポキシ基を、両末端カルボン酸変性型ブタジエン-アクリロニトリルゴム、末端アミノ変性シリコーンゴム等で変性することによって得られる。
本発明では、バインダーとして、上述したエラストマー以外の高分子化合物(他の高分子化合物ともいう)を用いることができる。他の高分子化合物は、1種または2種以上を併用することができる。
他の高分子化合物の具体例としては、例えば、炭化水素樹脂、ノボラック樹脂、フェノール樹脂、エポキシ樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル樹脂、アルキド樹脂、ポリアミド樹脂、ポリイミド樹脂、ポリアミドイミド樹脂、ポリベンズイミダゾール樹脂、ポリベンゾオキサゾール樹脂、ポリ塩化ビニル樹脂、ポリ酢酸ビニル樹脂、ポリアセタール樹脂、ポリカーボネート樹脂、ポリフェニレンエーテル樹脂、ポリブチレンテレフタレート樹脂、ポリエチレンテレフタレート樹脂、ポリフェニレンスルフィド樹脂、ポリスルホン樹脂、ポリエーテルスルホン樹脂、ポリアリレート樹脂、ポリエーテルエーテルケトン樹脂などが挙げられる。なかでも、炭化水素樹脂、ポリイミド樹脂、ポリカーボネート樹脂が好ましく、炭化水素樹脂がより好ましい。
また、本発明では、バインダーとして後述するフッ素原子を含むものを用いることができるが、フッ素原子を含むバインダー(以下、フッ素系バインダーともいう)は、実質的に含まないことが好ましい。フッ素系バインダーを実質的に含まないとは、フッ素系バインダーの含有量が、バインダーの全質量に対し、例えば、0.1質量%以下が好ましく、0.05質量%以下がより好ましく、含有しないことが一層好ましい。
本発明において、炭化水素樹脂として任意のものを使用できる。
炭化水素樹脂は、基本的には炭素原子と水素原子のみからなる樹脂を意味するが、基本となる骨格が炭化水素樹脂であれば、側鎖としてその他の原子を含んでいても良い。すなわち、炭素原子と水素原子のみからなる炭化水素樹脂に、アクリル樹脂、ポリビニルアルコール樹脂、ポリビニルアセタール樹脂、ポリビニルピロリドン樹脂のように、主鎖に炭化水素基以外の官能基が直接結合する場合も本発明における炭化水素樹脂に包含されるものであり、この場合、主鎖に炭化水素基が直接結合されてなる繰り返し単位の含有量が、樹脂の全繰り返し単位に対して30モル%以上であることが好ましい。
上記条件に合致する炭化水素樹脂としては例えば、テルペン樹脂、テルペンフェノール樹脂、変性テルペン樹脂、水添テルペン樹脂、水添テルペンフェノール樹脂、ロジン、ロジンエステル、水添ロジン、水添ロジンエステル、重合ロジン、重合ロジンエステル、変性ロジン、ロジン変性フェノール樹脂、アルキルフェノール樹脂、脂肪族石油樹脂、芳香族石油樹脂、水添石油樹脂、変性石油樹脂、環状脂肪族石油樹脂、クマロン石油樹脂、インデン石油樹脂、ポリスチレン-ポリオレフィン共重合体、オレフィンポリマー(例えば、メチルペンテン共重合体)、および、シクロオレフィンポリマー(例えば、ノルボルネン共重合体、ジシクロペンタジエン共重合体、テトラシクロドデセン共重合体)などが挙げられる。
炭化水素樹脂は、中でも、テルペン樹脂、ロジン、石油樹脂、水素化ロジン、重合ロジン、オレフィンポリマー、または、シクロオレフィンポリマーであることが好ましく、テルペン樹脂、ロジン、オレフィンポリマー、または、シクロオレフィンポリマーであることがより好ましく、であることが更に好ましく、シクロオレフィンポリマーであることが特に好ましい。
一般式(III)中、R5およびR6は、水素原子またはメチル基であることが好ましく、X3およびY3は水素原子であることが好ましく、その他の基は適宜選択される。このノルボルネン系重合体は、JSR(株)からアートン(Arton)GあるいはアートンFという商品名で発売されており、また日本ゼオン(株)からゼオノア(Zeonor)ZF14、ZF16、ゼオネックス(Zeonex)250、同280、同480Rという商品名で市販されており、これらを使用することができる。
ポリイミド樹脂は、テトラカルボン酸二無水物とジアミンを公知の方法で縮合反応させて得られるものを用いることができる。
公知の方法としては、例えば、有機溶剤中で、テトラカルボン酸二無水物とジアミンを略等モル混合し、反応温度80℃以下で反応させて得られたポリアミック酸を脱水閉環させる方法などが挙げられる。ここで、略等モルとは、テトラカルボン酸二無水物とジアミンのモル比が1:1近傍であることを言う。なお、必要に応じて、テトラカルボン酸二無水物とジアミンの組成比が、テトラカルボン酸二無水物の合計1.0モルに対して、ジアミンの合計が0.5~2.0モルとなるように調整してもよい。テトラカルボン酸二無水物とジアミンの組成比を上記の範囲内で調整することによって、ポリイミド樹脂の重量平均分子量を調整することができる。
これらのジアミンの中でも、3-(4-アミノフェニル)-1,1,3-トリメチル-5-アミノインダン、1,3-ビス(3-アミノプロピル)テトラメチルジシロキサン、ポリオキシプロピレンジアミン、2,2-ビス(4-アミノフェノキシフェニル)プロパン、4,9-ジオキサドデカン-1,12-ジアミン、1,6-ジアミノヘキサン、及び、4,9,14-トリオキサへプタデカン-1,17-ジアミンからなる群から選択される1種以上が好ましく、3-(4-アミノフェニル)-1,1,3-トリメチル-5-アミノインダンがより好ましい。
上記テトラカルボン酸二無水物とジアミンとの反応温度は、好ましくは100℃未満、さらに好ましくは90℃未満である。また、ポリアミック酸のイミド化は、代表的には不活性雰囲気(代表的には、真空または窒素雰囲気)下で加熱処理することにより行われる。加熱処理温度は、好ましくは150℃以上、さらに好ましくは180~450℃である。
このような溶解度を有するポリイミド樹脂は、例えば、3,4,3',4'-ベンゾフェノンテトラカルボン酸二無水物と、3-(4-アミノフェニル)-1,1,3-トリメチル-5-アミノインダンとを反応させて得られるポリイミド樹脂などが挙げられる。このポリイミド樹脂は、耐熱性が特に優れる。
本発明において、ポリカーボネート樹脂は、下記一般式(1)で表される繰り返し単位を有することが好ましい。
これらの芳香族基は、置換基を有していてもよいが、有していない方が好ましい。
芳香族基が有していてもよい置換基の例としては、ハロゲン原子、アルキル基、アルコキシ基、アリール基などが挙げられる。
ハロゲン原子としては、フッ素原子、塩素原子、臭素原子、ヨウ素原子等が挙げられる。
アルキル基としては、炭素数1~30のアルキル基が挙げられる。アルキル基の炭素数は、1~20がより好ましく、1~10がさらに好ましい。アルキル基は、直鎖、分岐のいずれであってもよい。また、アルキル基の水素原子の一部または全部は、ハロゲン原子で置換されていてもよい。ハロゲン原子としては、フッ素原子、塩素原子、臭素原子、ヨウ素原子等が挙げられ、フッ素原子が好ましい。
アルコキシ基としては、炭素数1~30のアルコキシ基が好ましい。アルコキシ基の炭素数は、1~20がより好ましく、1~10がさらに好ましい。アルコキシ基は、直鎖、分岐、環状のいずれでもよい。
アリール基としては、炭素数6~30のアリール基が好ましく、炭素数6~20のアリール基がより好ましい。
バインダーとしてエラストマーを用いる場合、エラストマーは、仮接着用組成物の全固形分中に50.00~99.99質量%の割合で含むことが好ましく、70.00~99.99質量%がより好ましく、88.00~99.99質量%が特に好ましい。エラストマーの含有量が上記範囲であれば、接着性および剥離性に優れる。エラストマーを2種類以上使用した場合は、合計が上記範囲であることが好ましい。
また、バインダーとしてエラストマーを用いる場合、バインダー全質量におけるエラストマーの含有量は、50~100質量%が好ましく、70~100質量%がより好ましく、80~100質量%がさらに好ましく、90~100質量%が一層好ましい。また、バインダーは、実質的にエラストマーのみであってもよい。なお、バインダーが、実質的にエラストマーのみであるとは、バインダー全質量におけるエラストマーの含有量が、99質量%以上が好ましく、99.9質量%以上がより好ましく、エラストマーのみからなることが一層好ましい。
本発明における仮接着用組成物は、フッ素系液体状化合物を含有することが好ましい。
本発明において、液体状とは、25℃で流動性を有する化合物であって、例えば、25℃での粘度が、1~100,000mPa・sである化合物を意味する。ここで、粘度は、B型粘度計を用いて測定することができ、粘度の測定方法としては、B型粘度計(ビスコリードアドバンス、ファンギラボ社製)を用いて粘度測定した値を用いている。
フッ素系液体状化合物の25℃での粘度は、例えば、10~20,000mPa・sがより好ましく、100~15,000mPa・sが一層好ましい。フッ素系液体状化合物の粘度が上記範囲であれば、仮接着剤層の表層にフッ素系液体状化合物が偏在しやすい。
フッ素系液体状化合物は、耐熱性等の観点から、オリゴマー、ポリマーおよびこれらの混合物が好ましい。
オリゴマー、ポリマーとしては、例えば、ラジカル重合体、カチオン重合体、アニオン重合体などが挙げられ、何れも好ましく用いることができる。ビニル系重合体が特に好ましい。
フッ素系液体状化合物の重量平均分子量は、500~100000が好ましく、1000~50000がより好ましく、2000~20000が更に好ましい。
このような特性を有するフッ素系液体状化合物としては、反応性基を有さない、非熱硬化性化合物であることが好ましい。ここでいう反応性基とは、250℃の加熱で反応する基全般を指し、重合性基、加水分解性基などが挙げられる。具体的には、例えば、メタ(アクリル)基、エポキシ基、イソシアナト基などが挙げられる。
また、フッ素系液体状化合物は、25℃から、20℃/分で昇温した10%熱質量減少温度が、250℃以上であることが好ましく、280℃以上がより好ましい。また、上限値は、特に限定はないが、例えば、1000℃以下が好ましく、800℃以下がより好ましい。この態様によれば、耐熱性に優れた仮接着剤層を形成しやすい。なお、熱質量減少温度とは、TG/DTA(熱質量測定装置)により、窒素気流下において、上記昇温条件で測定した値である。
アルキル基は、置換基を有していてもよい。置換基としては、ハロゲン原子、アルコキシ基、芳香族基などが挙げられる。
ハロゲン原子としては、塩素原子、フッ素原子、臭素原子、ヨウ素原子などが挙げられ、フッ素原子が好ましい。
アルコキシ基の炭素数は、1~30が好ましく、1~20がより好ましく、1~10がさらに好ましい。アルコキシ基は、直鎖または分岐が好ましい。
芳香族基は、単環であってもよく、多環であってもよい。芳香族基の炭素数は、6~20が好ましく、6~14がより好ましく、6~10が最も好ましい。
シクロアルキル基は、上述した置換基を有していてもよい。
芳香族基は、上述した置換基を有していてもよい。
フッ素系液体状化合物は、一分子中に親油基を1個以上有し、2~100個有することが好ましく、6~80個有することが特に好ましい。
含フッ素アルキル基の炭素数は、1~30が好ましく、1~20がより好ましく、1~15がさらに好ましい。含フッ素アルキル基は、直鎖、分岐、環状のいずれであってもよい。また、エーテル結合を有していてもよい。また、含フッ素アルキル基は、水素原子の全てがフッ素原子に置換されたペルフルオロアルキル基であってもよい。
含フッ素アルキレン基の炭素数は、2~30が好ましく、2~20がより好ましく、2~15がさらに好ましい。含フッ素アルキレン基は、直鎖、分岐、環状のいずれであってもよい。また、エーテル結合を有していてもよい。また、含フッ素アルキレン基は、水素原子の全てがフッ素原子に置換されたペルフルオロアルキレン基であってもよい。
フッ素原子の含有率は、「{(1分子中のフッ素原子数×フッ素原子の質量)/1分子中の全原子の質量}×100」で定義される。
また、本発明で用いる仮接着用組成物は、フッ素系液体状化合物とバインダーとの質量比が、フッ素系液体状化合物:バインダー=0.001:99.999~10:90.00が好ましく、0.001:99.999~5:95.00がより好ましく、0.010:99.99~5:95.00がさらに好ましい。フッ素系液体状化合物とバインダーとの質量比を上記範囲とすることで、仮接着剤層の空気界面側にフッ素系液体状化合物をより多く偏在させ易い。
本発明で用いる仮接着用組成物は、必要に応じて可塑剤を含んでいてもよい。可塑剤を配合することにより、上記諸性能を満たす仮接着剤層とすることができる。
可塑剤としては、フタル酸エステル、脂肪酸エステル、芳香族多価カルボン酸エステル、ポリエステルなどが使用できる。
脂肪酸エステルとしては例えば、ブチルステアレート、ユニスターM-9676、ユニスターM-2222SL、ユニスターH-476、ユニスターH-476D、パナセート800B、パナセート875、パナセート810(以上、日油製)、DBA、DIBA、DBS、DOA、DINA、DIDA、DOS、BXA、DOZ、DESU(以上、大八化学製)などが挙げられる。
芳香族多価カルボン酸エステルとしては、TOTM(大八化学製)、モノサイザーW-705(大八化学製)、UL-80、UL-100(ADEKA製)などが挙げられる。
ポリエステルとしては、ポリサイザーTD-1720、ポリサイザーS-2002、ポリサイザーS-2010(以上、DIC製)、BAA-15(大八化学製)などが挙げられる。
上記可塑剤の中では、DIDP、DIDA、TOTM、ユニスターM-2222SL、ポリサイザーTD-1720が好ましく、DIDA、TOTMがより好ましく、TOTMが特に好ましい。
可塑剤は1種のみを用いてもよいし、2種類以上を組み合わせてもよい。
本発明で用いる仮接着用組成物は、酸化防止剤を含有してもよい。酸化防止剤としては、フェノール系酸化防止剤、硫黄系酸化防止剤、リン系酸化防止剤、キノン系酸化防止剤、アミン系酸化防止剤などが使用できる。
フェノール系酸化防止剤としては例えば、p-メトキシフェノール、2,6-ジ-tert-ブチル-4-メチルフェノール、BASF(株)製「Irganox1010」、「Irganox1330」、「Irganox3114」、「Irganox1035」、住友化学(株)製「Sumilizer MDP-S」、「Sumilizer GA-80」などが挙げられる。
硫黄系酸化防止剤としては例えば、3,3’-チオジプロピオネートジステアリル、住友化学(株)製「Sumilizer TPM」、「Sumilizer TPS」、「Sumilizer TP-D」などが挙げられる。
リン系酸化防止剤としては例えば、トリス(2,4-ジ-tert-ブチルフェニル)ホスフィト、ビス(2,4-ジ-tert-ブチルフェニル)ペンタエリスリトールジホスフィト、ポリ(ジプロピレングリコール)フェニルホスフィト、ジフェニルイソデシルホスフィト、2-エチルヘキシルジフェニルホスフィト、トリフェニルホスフィト、BASF(株)製「Irgafos168」、「Irgafos38」などが挙げられる。
キノン系酸化防止剤としては例えば、p-ベンゾキノン、2-tert-ブチル-1,4-ベンゾキノンなどが挙げられる。
アミン系酸化防止剤としては例えば、ジメチルアニリンやフェノチアジンなどが挙げられる。
酸化防止剤は、Irganox1010、Irganox1330、3,3’-チオジプロピオネートジステアリル、Sumilizer TP-Dが好ましく、Irganox1010、Irganox1330がより好ましく、Irganox1010が特に好ましい。
また、上記酸化防止剤のうち、フェノール系酸化防止剤と、硫黄系酸化防止剤またはリン系酸化防止剤とを併用することが好ましく、フェノール系酸化防止剤と硫黄系酸化防止剤とを併用することが最も好ましい。特に、エラストマーとして、ポリスチレン系エラストマーを使用した場合において、フェノール系酸化防止剤と硫黄系酸化防止剤とを併用することが好ましい。このような組み合わせにすることにより、酸化反応によるバインダーの劣化を、効率よく抑制できる効果が期待できる。フェノール系酸化防止剤と硫黄系酸化防止剤とを併用する場合、フェノール系酸化防止剤と硫黄系酸化防止剤との質量比は、フェノール系酸化防止剤:硫黄系酸化防止剤=95:5~5:95が好ましく、75:25~25:75がより好ましい。
酸化防止剤の組み合わせとしては、Irganox1010とSumilizer TP-D、Irganox1330とSumilizer TP-D、および、Sumilizer GA-80とSumilizer TP-Dが好ましく、Irganox1010とSumilizer TP-D、Irganox1330とSumilizer TP-Dがより好ましく、Irganox1010とSumilizer TP-Dが特に好ましい。
酸化防止剤は1種類のみでもよいし、2種類以上であってもよい。酸化防止剤が2種類以上の場合は、その合計が上記範囲であることが好ましい。
本発明で用いる仮接着用組成物は、溶剤を含有することが好ましい。溶剤は、公知のものを制限なく使用でき、有機溶剤が好ましい。
本発明で用いられる有機溶剤としては、酢酸エチル、酢酸-n-ブチル、酢酸イソブチル、ギ酸アミル、酢酸イソアミル、酢酸イソブチル、プロピオン酸ブチル、酪酸イソプロピル、酪酸エチル、酪酸ブチル、乳酸メチル、乳酸エチル、オキシ酢酸アルキル(例:オキシ酢酸メチル、オキシ酢酸エチル、オキシ酢酸ブチル(例えば、メトキシ酢酸メチル、メトキシ酢酸エチル、メトキシ酢酸ブチル、エトキシ酢酸メチル、エトキシ酢酸エチル等))、3-オキシプロピオン酸アルキルエステル類(例:3-オキシプロピオン酸メチル、3-オキシプロピオン酸エチル等(例えば、3-メトキシプロピオン酸メチル、3-メトキシプロピオン酸エチル、3-エトキシプロピオン酸メチル、3-エトキシプロピオン酸エチル等))、2-オキシプロピオン酸アルキルエステル類(例:2-オキシプロピオン酸メチル、2-オキシプロピオン酸エチル、2-オキシプロピオン酸プロピル等(例えば、2-メトキシプロピオン酸メチル、2-メトキシプロピオン酸エチル、2-メトキシプロピオン酸プロピル、2-エトキシプロピオン酸メチル、2-エトキシプロピオン酸エチル))、2-オキシ-2-メチルプロピオン酸メチルおよび2-オキシ-2-メチルプロピオン酸エチル(例えば、2-メトキシ-2-メチルプロピオン酸メチル、2-エトキシ-2-メチルプロピオン酸エチル等)、ピルビン酸メチル、ピルビン酸エチル、ピルビン酸プロピル、アセト酢酸メチル、アセト酢酸エチル、2-オキソブタン酸メチル、2-オキソブタン酸エチル、1-メトキシ-2-プロピルアセテート等のエステル類;
ジエチレングリコールジメチルエーテル、テトラヒドロフラン、エチレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、メチルセロソルブアセテート、エチルセロソルブアセテート、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノブチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテルアセテート、プロピレングリコールモノエチルエーテルアセテート、プロピレングリコールモノプロピルエーテルアセテート等のエーテル類;
メチルエチルケトン、シクロヘキサノン、2-ヘプタノン、3-ヘプタノン、N-メチル-2-ピロリドン、γブチロラクトン等のケトン類;
トルエン、キシレン、アニソール、メシチレン、エチルベンゼン、プロピルベンゼン、クメン、n-ブチルベンゼン、sec-ブチルベンゼン、イソブチルベンゼン、tert-ブチルベンゼン、アミルベンゼン、イソアミルベンゼン、(2,2-ジメチルプロピル)ベンゼン、1-フェニルへキサン、1-フェニルヘプタン、1-フェニルオクタン、1-フェニルノナン、1-フェニルデカン、シクロプロピルベンゼン、シクロヘキシルベンゼン、2-エチルトルエン、1,2-ジエチルベンゼン、o-シメン、インダン、1,2,3,4-テトラヒドロナフタレン、3-エチルトルエン、m-シメン、1,3-ジイソプロピルベンゼン、4-エチルトルエン、1,4-ジエチルベンゼン、p-シメン、1,4-ジイソプロピルベンゼン、4-tert-ブチルトルエン、1,4-ジ-tert-ブチルベンゼン、1,3-ジエチルベンゼン、1,2,3-トリメチルベンゼン、1,2,4-トリメチルベンゼン、4-tert-ブチル-o-キシレン、1,2,4-トリエチルベンゼン、1,3,5-トリエチルベンゼン、1,3,5-トリイソプロピルベンゼン、5-tert-ブチル-m-キシレン、3,5-ジ-tert-ブチルトルエン、1,2,3,5-テトラメチルベンゼン、1,2,4,5-テトラメチルベンゼン、ペンタメチルベンゼン、デカヒドロナフタレン、等の芳香族炭化水素類;
エチルシクロヘキサン、リモネン(特に、d-リモネン)、p-メンタン、ノナン、デカン、ドデカン、デカリン等の脂肪族炭化水素類が例示される。
溶剤は1種類のみでもよいし、2種類以上であってもよい。溶剤が2種類以上の場合は、その合計が上記範囲であることが好ましい。
界面活性剤としては、アニオン系、カチオン系、ノニオン系、または、両性のいずれでも使用することができるが、好ましい界面活性剤はノニオン系界面活性剤である。
ノニオン系界面活性剤の好ましい例としては、ポリオキシエチレン高級アルキルエーテル類、ポリオキシエチレン高級アルキルフェニルエーテル類、ポリオキシエチレングリコールの高級脂肪酸ジエステル類、シリコーン系界面活性剤を挙げることができる。
シリコーン系界面活性剤として、例えば、特開昭62-36663号、特開昭61-226746号、特開昭61-226745号、特開昭62-170950号、特開昭63-34540号、特開平7-230165号、特開平8-62834号、特開平9-54432号、特開平9-5988号、特開2001-330953号各公報記載の界面活性剤を挙げることができ、市販の界面活性剤を用いることもできる。
市販のシリコーン系界面活性剤として、例えば、KP-301、KP-306、KP-109、KP-310、KP-310B、KP-323、KP-326、KP-341、KP-104、KP-110、KP-112、KP-360A、KP-361、KP-354、KP-355、KP―356、KP-357、KP-358、KP-359、KP-362、KP-365、KP-366、KP-368、KP-369、KP-330、KP-650、KP-651、KP-390、KP-391、KP-392(信越化学工業(株)製)を用いることができる。
本発明で用いる仮接着用組成物は、本発明の効果を損なわない範囲で、必要に応じて、各種添加物、例えば、硬化剤、硬化触媒、シランカップリング剤、充填剤、密着促進剤、紫外線吸収剤、凝集防止剤等を配合することができる。これらの添加剤を配合する場合、その合計配合量は仮接着用組成物の全固形分の3質量%以下が好ましい。
仮接着用組成物から金属等の不純物を除去する方法としては、例えば、フィルタを用いた濾過を挙げることができる。フィルタ孔径としては、ポアサイズ10nm以下が好ましく、5nm以下がより好ましく、3nm以下が更に好ましい。フィルタの材質としては、ポリテトラフロロエチレン製、ポリエチレン製、ナイロン製のフィルタが好ましい。フィルタは、有機溶剤であらかじめ洗浄したものを用いてもよい。フィルタ濾過工程では、複数種類のフィルタを直列又は並列に接続して用いてもよい。複数種類のフィルタを使用する場合は、孔径及び/又は材質が異なるフィルタを組み合わせて使用しても良い。また、各種材料を複数回濾過してもよく、複数回濾過する工程が循環濾過工程であっても良い。
また、仮接着用組成物に含まれる金属等の不純物を低減する方法としては、仮接着用組成物を構成する原料として金属含有量が少ない原料を選択する、仮接着用組成物を構成する原料に対してフィルタ濾過を行う、装置内をポリテトラフロロエチレン等でライニングしてコンタミネーションを可能な限り抑制した条件下で蒸留を行う等の方法を挙げることができる。仮接着用組成物を構成する原料に対して行うフィルタ濾過における好ましい条件は、上述した条件と同様である。
フィルタ濾過の他、吸着材による不純物の除去を行っても良く、フィルタ濾過と吸着材を組み合わせて使用しても良い。吸着材としては、公知の吸着材を用いることができ、例えば、シリカゲル、ゼオライトなどの無機系吸着材、活性炭などの有機系吸着材を使用することができる。
本発明で用いる仮接着用組成物は、上述の各成分を混合して調製することができる。各成分の混合は、通常、0℃~100℃の範囲で行われる。また、各成分を混合した後、例えば、フィルタでろ過することが好ましい。ろ過は、多段階で行ってもよいし、多数回繰り返してもよい。また、ろ過した液を再ろ過することもできる。
フィルタとしては、従来からろ過用途等に用いられているものであれば特に限定されることなく用いることができる。例えば、PTFE(ポリテトラフルオロエチレン)等のフッ素樹脂、ナイロン-6、ナイロン-6,6等のポリアミド系樹脂、ポリエチレン、ポリプロピレン(PP)等のポリオレフィン樹脂(高密度、超高分子量のものを含む)等によるフィルタが挙げられる。これら素材の中でもポリプロピレン(高密度ポリプロピレンを含む)およびナイロンが好ましい。
フィルタの孔径は、例えば、0.003~5.0μm程度が適している。この範囲とすることにより、ろ過詰まりを抑えつつ、組成物に含まれる不純物や凝集物など、微細な異物を確実に除去することが可能となる。
フィルタを使用する際、異なるフィルタを組み合わせても良い。その際、第1のフィルタでのフィルタリングは、1回のみでもよいし、2回以上行ってもよい。異なるフィルタを組み合わせて2回以上フィルタリングを行う場合は1回目のフィルタリングの孔径より2回目以降の孔径が同じ、もしくは小さい方が好ましい。また、上述した範囲内で異なる孔径の第1のフィルタを組み合わせてもよい。ここでの孔径は、フィルタメーカーの公称値を参照することができる。市販のフィルタとしては、例えば、日本ポール株式会社、アドバンテック東洋株式会社、日本インテグリス株式会社(旧日本マイクロリス株式会社)又は株式会社キッツマイクロフィルタ等が提供する各種フィルタの中から選択することができる。
<<第一の実施形態>>
以下、積層体を製造する工程を経た半導体装置の製造方法の一実施形態について、図2を合わせて参照しながら説明する。なお、本発明は、以下の実施形態に限定されるものではない。
図2(A)~(E)は、それぞれ、キャリア基材とモールディング層を設けたデバイスウェハとの仮接着を説明する概略断面図(図2(A)、(B))、キャリア基材に仮接着された、モールディング層を設けたデバイスウェハが薄型化された状態(図2(C))、キャリア基材とモールディング層を設けたデバイスウェハを剥離した状態(図2(D))、モールディング層を有するデバイスウェハから仮接着剤層を除去後の状態(図2(E))を示す概略断面図である。
仮接着剤層11は、実質的に溶剤を含まない態様であることが好ましい。
デバイスウェハ60は、デバイス基板61の表面61aに複数の回路面62が設けられてなる。
デバイス基板61の厚さは、例えば、200~1200μmが好ましい。回路面62は例えば金属構造体であることが好ましく、高さは10~100μmが好ましい。
さらに、デバイスウェハの表面に回路面を覆うようにモールディング層15が設けられている。モールディング層は、デバイス基板の基板面上に、回路面を覆うように設けられた平坦な層であることが好ましい。
さらに、本発明では、回路面の高さがXμm、モールディング層の厚みをYμmの場合、「X+100≧Y>X」の関係を満たすことが好ましい。
モールディング層15が、平坦な層であることにより、薄型化デバイスウェハのTTV(Total Thickness Variation)をより低下したい場合(すなわち、薄型化デバイスウェハの平坦性をより向上させたい場合)に有効である。
また、機械的または化学的な処理として、薄膜化処理の後に、薄型化デバイスウェハ60aの裏面61b1からデバイス基板を貫通する貫通孔(図示せず)を形成し、この貫通孔内にシリコン貫通電極(図示せず)を形成する処理を行ってもよい。
また、キャリア基材12とモールディング層を設けたデバイスウェハ60とを仮接着した後、剥離するまでの間に加熱処理を行っても良い。加熱処理の一例として、機械的または化学的な処理を行う際に、加熱を伴った処理とすることが挙げられる。
上記加熱処理における最高到達温度は80~400℃が好ましく、130℃~400℃がより好ましく、180℃~350℃がさらに好ましい。加熱処理における最高到達温度は仮接着剤層の分解温度よりも低い温度とすることが好ましい。加熱処理は、最高到達温度での30秒~30分の加熱であることが好ましく、最高到達温度での1分~10分の加熱であることがより好ましい。
この実施形態では、キャリア基材12と仮接着剤層11の界面で剥離されることが好ましい。
また、仮接着剤層11に後述する剥離液に接触させ、その後、必要に応じて、キャリア基材12に対してモールディング層15を設けた薄型化デバイスウェハ60aを摺動させた後に、上記と同様に分離することもできる。
B≦4N/cm ・・・・式(2)
仮接着剤層を、剥離液を用いて除去する場合、以下の剥離液を好ましく用いることができる。
剥離液としては、水および、溶剤(有機溶剤)を使用することができる。
また、剥離液としては、仮接着剤層を溶解する有機溶剤が好ましい。有機溶剤としては、例えば、脂肪族炭化水素類(ヘキサン、ヘプタン、アイソパーE、H、G(エッソ化学(株)製)、リモネン、p-メンタン、ノナン、デカン、ドデカン、デカリン、等)、芳香族炭化水素類(トルエン、キシレン、アニソール、メシチレン、エチルベンゼン、プロピルベンゼン、クメン、n-ブチルベンゼン、sec-ブチルベンゼン、イソブチルベンゼン、tert-ブチルベンゼン、アミルベンゼン、イソアミルベンゼン、(2,2-ジメチルプロピル)ベンゼン、1-フェニルへキサン、1-フェニルヘプタン、1-フェニルオクタン、1-フェニルノナン、1-フェニルデカン、シクロプロピルベンゼン、シクロヘキシルベンゼン、2-エチルトルエン、1,2-ジエチルベンゼン、o-シメン、インダン、1,2,3,4-テトラヒドロナフタレン、3-エチルトルエン、m-シメン、1,3-ジイソプロピルベンゼン、4-エチルトルエン、1,4-ジエチルベンゼン、p-シメン、1,4-ジイソプロピルベンゼン、4-tert-ブチルトルエン、1,4-ジ-tert-ブチルベンゼン、1,3-ジエチルベンゼン、1,2,3-トリメチルベンゼン、1,2,4-トリメチルベンゼン、4-tert-ブチル-o-キシレン、1,2,4-トリエチルベンゼン、1,3,5-トリエチルベンゼン、1,3,5-トリイソプロピルベンゼン、5-tert-ブチル-m-キシレン、3,5-ジ-tert-ブチルトルエン、1,2,3,5-テトラメチルベンゼン、1,2,4,5-テトラメチルベンゼン、ペンタメチルベンゼン、等)、ハロゲン化炭化水素(メチレンジクロライド、エチレンジクロライド、トリクレン、モノクロルベンゼン等)、極性溶剤が挙げられる。極性溶剤としては、アルコール類(メタノール、エタノール、プロパノール、イソプロパノール、1-ブタノール、1-ペンタノール、1-ヘキサノール、1-ヘプタノール、1-オクタノール、2-オクタノール、2-エチル-1-ヘキサノール、1-ノナノール、1-デカノール、ベンジルアルコール、エチレングリコールモノメチルエーテル、2-エトキシエタノール、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノヘキシルエーテル、トリエチレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノメチルエーテル、ポリエチレングリコールモノメチルエーテル、ポリプロピレングリコール、テトラエチレングリコール、エチレングリコールモノブチルエーテル、エチレングリコールモノベンジルエーテル、エチレングリコールモノフェニルエーテル、プロピレングリコールモノフェニルエーテル、メチルフェニルカルビノール、n-アミルアルコール、メチルアミルアルコール等)、ケトン類(アセトン、メチルエチルケトン、エチルブチルケトン、メチルイソブチルケトン、シクロヘキサノン等)、エステル類(酢酸エチル、酢酸プロピル、酢酸ブチル、酢酸アミル、酢酸ベンジル、乳酸メチル、乳酸ブチル、エチレングリコールモノブチルアセテート、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールアセテート、ジエチルフタレート、レブリン酸ブチル等)、その他(トリエチルフォスフェート、トリクレジルフォスフェート、N-フェニルエタノールアミン、N-フェニルジエタノールアミン、N-メチルジエタノールアミン、N-エチルジエタノールアミン、4-(2-ヒドロキシエチル)モルホリン、N,N-ジメチルアセトアミド、N-メチルピロリドン等)等が挙げられる。
さらに剥離性の観点から、2種以上の有機溶剤および水、2種以上のアルカリ、酸および界面活性剤を混合する形態も好ましい。
界面活性剤の含有量を上記した範囲内とすることにより、仮接着剤層11と薄型化デバイスウェハ60aとの剥離性をより向上できる傾向となる。
例えば、キャリア基材としてデバイス基板を使用した場合、従来既知のシリコンウェハの洗浄方法を使用することができ、例えば化学的に除去する場合に使用できる水溶液または有機溶剤としては、強酸、強塩基、強酸化剤、またはそれらの混合物が上げられ、具体的には、硫酸、塩酸、フッ酸、硝酸、有機酸などの酸類、テトラメチルアンモニウム、アンモニア、有機塩基などの塩基類、過酸化水素などの酸化剤、またはアンモニアと過酸化水素の混合物、塩酸と過酸化水素水の混合物、硫酸と過酸化水素水の混合物、フッ酸と過酸化水素水の混合物、フッ酸とフッ化アンモニウムとの混合物などが挙げられる。
キャリア基材洗浄液は、pKaが0未満の酸(強酸)と過酸化水素を含んでいることが好ましい。pKaが0未満の酸としては、ヨウ化水素、過塩素酸、臭化水素、塩化水素、硝酸、硫酸などの無機酸、又はアルキルスルホン酸、アリールスルホン酸などの有機酸から選択される。キャリア基材上の仮接着剤層の洗浄性の観点から無機酸であることが好ましく、硫酸が最も好ましい。
積層体を製造する工程を経た半導体装置の製造方法の第二の実施形態について、図3を合わせて参照しながら説明する。上述した第一の実施形態と同一箇所は、同一符号を付してその説明を省略する。
図3(A)~(E)は、それぞれ、キャリア基材とモールディング層を設けたデバイスウェハとの仮接着を説明する概略断面図(図3(A)、(B))、キャリア基材に仮接着されたモールディング層を有するデバイスウェハが薄型化された状態(図3(C))、キャリア基材とモールディング層を有するデバイスウェハを剥離した状態(図3(D))、モールディング層を有するデバイスウェハから仮接着剤層を除去後の状態(図3(E))を示す概略断面図である。
この実施形態では、図3(A)に示すように、モールディング層15の表面に仮接着剤層11を形成する点が上記第一の実施形態と相違する。
モールディング層15の表面上に、仮接着剤層11を設ける場合は、モールディング層15の表面に仮接着用組成物を適用(好ましくは塗布)し、次いで、乾燥(ベーク)することにより形成することができる。乾燥は、例えば、60~150℃で、10秒~2分行うことができる。
次いで、図3(B)に示す通り、キャリア基材12とモールディング層15を設けたデバイスウェハ60とを圧着させ、キャリア基材12とモールディング層15とを仮接着させる。次いで、図3(C)に示すように、デバイス基板61の裏面61bに対して、機械的または化学的な処理を施して、図3(C)に示すように、デバイス基板61の厚さを薄くし、モールディング層を有する薄型化デバイスウェハ60aを得る。次いで、図3(D)に示すように、キャリア基材12を、モールディング層を設けた薄型化デバイスウェハ60aから分離させる。そして、図3(E)に示すように、モールディング層を設けた薄型化デバイスウェハ60aから仮接着剤層11を除去する。
また、上述した実施形態においては、デバイスウェハ(デバイス基板)に対する機械的または化学的な処理として、デバイスウェハの薄膜化処理、および、シリコン貫通電極の形成処理を挙げたが、これらに限定されるものではなく、半導体装置の製造方法において必要ないずれの処理も挙げられる。
その他、上述した実施形態において例示した、デバイスウェハにおける回路面の形状、寸法、数、配置箇所等は任意であり、限定されない。
トランスファー成形機を用い、金型温度175℃、注入圧力7.8MPa、硬化時間2分で、固体のコンプレッションモールディング材料であるスミコンEME-G770(住友ベークライト製)を封止成形し、175℃、2時間で後硬化してモールディング層を形成した。
モールディング層Xにおいて、スミコンEME-G770(住友ベークライト製)を液体のモールディング材料である(CEL-C-5020)に変更し、100℃、30分、次いで150℃、2時間ベークしモールディング層を形成した。
モールディング層Xにおいて、スミコンEME-G770(住友ベークライト製)を液体のモールディング材料である(CEL-C-5400)に変更し、100℃、30分、次いで150℃、2時間ベークしモールディング層を形成した。
・セプトンS2104(クラレ製):45質量部
・タフテックP2000(旭化成ケミカルズ製:45質量部
・Irganox 1010(BASF製):5質量部
・Sumilizer TP-D(住友化学製):5質量部
・メガファックF-553(DIC製):0.1質量部
・メシチレン(東洋合成工業製):190質量部
・セプトンS2104(クラレ製):90質量部
・Irganox 1010(BASF製):5質量部
・Sumilizer TP-D(住友化学製):5質量部
・メガファックF-553(DIC製):0.1質量部
・メシチレン(東洋合成工業製):190質量部
表面に回路面が設けられた12インチシリコンウェハ(1インチは、2.54cmである)の表面に、表1に示す通り、上記モールディング層X~Zの形成方法のいずれかの方法によって、モールディング層を形成し、積層体Aを得た。
その後、表1に示す通り、後述する加熱処理、溶剤洗浄処理、アッシング処理のいずれか1つ以上を行った。
次いで、モールディング層の表面に、仮接着用組成物1または仮接着用組成物2をウェハボンディング装置(東京エレクトロン製、Synapse V)により50rpmで回転させながら、30秒間の間に15mL滴下した。ホットプレートを用いて、110℃で3分加熱し、さらに、190℃で3分加熱することで、シリコンウェハの表面に仮接着剤層を形成し、積層体Bを得た。
ついで、上記積層体Cの、先に用いたシリコンウェハ側を、バックグラインダーDFG8540(ディスコ製)を用いて35μmの厚さまで研磨し、薄型化した積層体Dを得た。
積層体Aに、120℃で、8時間加熱処理を行った。
積層体Aのモールディング層の表面にシクロヘキサンを回転数800rpmで、スピン塗布を5分間行った後、液を振り切り2000rpmで1分間スピン乾燥し、ついで100℃、1分間、溶剤を乾燥させる為のベークを実施した。
積層体Aのモールディング層の表面を酸素プラズマによりアッシング処理で洗浄した。
加熱処理、溶剤洗浄処理、アッシング処理のいずれか1つ以上を行った後のモールディング層について、分子量1000以下の成分の量(質量%)をGCMS(島津製作所、型番:P2010)を用い、ヘッドスペース部オーブン温度180℃、ニードル温度180℃、トランスファ温度200℃、加圧時間3分、キャリアガス140kPa、ガスクロカラム気化室温度220℃、レステック社製Rtxカラム(長さ60m)、40℃から310℃まで昇温速度10℃/分、マススペクトラムをスキャンモードで、インターフェース温度220℃、イオン源温度200℃の条件で発生したガスを計測した。
得られた積層体Bの仮接着剤層側の膜面について、光学顕微鏡(製造元:オリンパス社製、品番:MX-80 )により50倍の倍率で、仮接着剤層の膜面から垂直な方向から観察し、仮接着剤層の膜面700cm2あたりの最大長さが30μm以上のボイドの数を測定した。
得られた積層体Bの仮接着剤層側の表面の算術平均表面粗さ(Ra)を、触針式表面粗さ計(製造元:KLA-Tencor、品番:P-15)を用いて測定した。単位は、μmで示した。
積層体Bについて、100℃から200℃まで、10℃/分で昇温した際の、熱質量減少度を測定した。熱質量減少度は、熱重量分析装置Q500(TA社製)により、2-3mgの試料をアルミパン上で60mL/分の窒素気流下、初期温度25℃から10℃/分の一定昇温条件で400℃まで昇温し、400℃に達した際の残存重量を測定した。
を用いて行った。
上記薄型化した積層体Dについて、クラックの有無を目視にて確認した。
11:仮接着剤層
12:キャリア基材
15:モールディング層
60:デバイスウェハ
60a:薄型化デバイスウェハ
61:デバイス基板
61a:表面
61b:、61b1:裏面
62:回路面
Claims (15)
- 回路面を有するデバイスウェハ、前記回路面の表面を覆うモールディング層、前記モールディング層の表面に位置する仮接着剤層を有する積層体であって、
前記仮接着剤層の膜面に垂直な方向から光学顕微鏡で観察した、最大長さ30μm以上のボイドの数が、仮接着剤層の膜面700cm2あたり、3個以下であり、前記仮接着剤層の算術平均表面粗さであるRaがRa≦10.0μmである、積層体。 - モールディング層における、分子量1000以下の成分が5質量%以下である、請求項1に記載の積層体。
- 前記モールディング層が、液状のモールディング材料をベークすることで形成されてなる、請求項1または2に記載の積層体。
- 前記モールディング層が、固体のコンプレッションモールディング材料により形成されてなる、請求項1または2に記載の積層体。
- モールディング層に処理を行った後、仮接着剤層を設けてなり、前記処理後のモールディング層の100℃から200℃まで、10℃/分で昇温した際の、熱質量減少度が、5質量%以下である、請求項1~4のいずれか1項に記載の積層体。
- 前記回路面の表面を覆っているモールディング層を100℃~250℃で加熱処理した後に、仮接着剤層を設けてなる、請求項5に記載の積層体。
- 前記回路面の表面を覆っているモールディング層の表面を有機溶剤で洗浄した後に、仮接着剤層を設けてなる、請求項5または6に記載の積層体。
- 前記回路面の表面を覆っているモールディング層の表面をアッシング処理した後に、仮接着剤層を設けてなる、請求項5~7のいずれか1項に記載の積層体。
- 前記回路面の表面を覆っているモールディング層を100℃~250℃で加熱処理すること、前記回路面の表面を覆っているモールディング層の表面を有機溶剤で洗浄すること、および、前記回路面の表面を覆っているモールディング層の表面をアッシング処理することのうち、2つ以上を行った後に、仮接着剤層を設けてなる、請求項1~8のいずれか1項に記載の積層体。
- 前記アッシング処理は、酸素プラズマで行う、請求項8または9に記載の積層体。
- モールディング層および仮接着剤層が、それぞれ独立に、樹脂を含む、請求項1~10のいずれか1項に記載の積層体。
- 前記仮接着剤層の、モールディング層と接している側と反対側の上に、キャリア基材を有する、請求項1~11のいずれか1項に記載の積層体。
- 前記デバイスウェハの厚さが、200μm以下である、請求項1~12のいずれか1項に記載の積層体。
- 前記仮接着剤層が、キャリア基材と接している、請求項1~13のいずれか1項に記載の積層体。
- 前記仮接着剤層が1層である、請求項14に記載の積層体。
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