CN110088160A - Resin particle, connecting material and connection structural bodies - Google Patents
Resin particle, connecting material and connection structural bodies Download PDFInfo
- Publication number
- CN110088160A CN110088160A CN201880005079.3A CN201880005079A CN110088160A CN 110088160 A CN110088160 A CN 110088160A CN 201880005079 A CN201880005079 A CN 201880005079A CN 110088160 A CN110088160 A CN 110088160A
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- CN
- China
- Prior art keywords
- mentioned
- resin particle
- particle
- resin
- unit
- Prior art date
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- Granted
Links
- 239000002245 particle Substances 0.000 title claims abstract description 277
- 229920005989 resin Polymers 0.000 title claims abstract description 192
- 239000011347 resin Substances 0.000 title claims abstract description 192
- 239000000463 material Substances 0.000 title claims description 64
- 229910020447 SiO2/2 Inorganic materials 0.000 claims abstract description 8
- 229910020388 SiO1/2 Inorganic materials 0.000 claims abstract description 7
- 229910020487 SiO3/2 Inorganic materials 0.000 claims abstract description 7
- 229910020485 SiO4/2 Inorganic materials 0.000 claims abstract description 7
- 125000006850 spacer group Chemical group 0.000 claims description 29
- 230000036961 partial effect Effects 0.000 claims description 27
- 239000000853 adhesive Substances 0.000 claims description 21
- 230000001070 adhesive effect Effects 0.000 claims description 21
- 238000007906 compression Methods 0.000 claims description 16
- 230000006835 compression Effects 0.000 claims description 15
- 238000011084 recovery Methods 0.000 claims description 10
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 4
- -1 polysiloxanes Polymers 0.000 description 104
- 239000004973 liquid crystal related substance Substances 0.000 description 58
- 229910000077 silane Inorganic materials 0.000 description 38
- 125000004429 atom Chemical group 0.000 description 30
- 238000000034 method Methods 0.000 description 28
- 238000004519 manufacturing process Methods 0.000 description 27
- 229910052799 carbon Inorganic materials 0.000 description 25
- 229910052710 silicon Inorganic materials 0.000 description 25
- 229920001296 polysiloxane Polymers 0.000 description 24
- 150000001721 carbon Chemical group 0.000 description 23
- 239000000758 substrate Substances 0.000 description 23
- 230000000116 mitigating effect Effects 0.000 description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 21
- 150000001875 compounds Chemical class 0.000 description 20
- 229910052751 metal Inorganic materials 0.000 description 16
- 125000000962 organic group Chemical group 0.000 description 16
- 239000004215 Carbon black (E152) Substances 0.000 description 15
- 239000012790 adhesive layer Substances 0.000 description 15
- 229930195733 hydrocarbon Natural products 0.000 description 15
- 230000002209 hydrophobic effect Effects 0.000 description 15
- 239000000565 sealant Substances 0.000 description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 13
- 239000011521 glass Substances 0.000 description 13
- 229910052709 silver Inorganic materials 0.000 description 13
- 239000004332 silver Substances 0.000 description 13
- 239000002184 metal Substances 0.000 description 12
- 229910044991 metal oxide Inorganic materials 0.000 description 12
- 150000004706 metal oxides Chemical class 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 125000004430 oxygen atom Chemical group O* 0.000 description 11
- 238000007789 sealing Methods 0.000 description 11
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 11
- 239000010408 film Substances 0.000 description 10
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- 239000003638 chemical reducing agent Substances 0.000 description 9
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
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- 238000009826 distribution Methods 0.000 description 6
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
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- 239000002253 acid Substances 0.000 description 5
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229920002554 vinyl polymer Polymers 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
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- 235000019441 ethanol Nutrition 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 229910000765 intermetallic Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000007870 radical polymerization initiator Substances 0.000 description 4
- 229920002050 silicone resin Polymers 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229920006387 Vinylite Polymers 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
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- 239000000806 elastomer Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000010556 emulsion polymerization method Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- KAJZYANLDWUIES-UHFFFAOYSA-N heptadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCN KAJZYANLDWUIES-UHFFFAOYSA-N 0.000 description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
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- 239000000203 mixture Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
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- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical compound CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
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- 239000000523 sample Substances 0.000 description 3
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- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 2
- VSKJLJHPAFKHBX-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical compound CC(=C)C=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 VSKJLJHPAFKHBX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
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- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
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- 125000000524 functional group Chemical group 0.000 description 2
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- GOQYKNQRPGWPLP-UHFFFAOYSA-N heptadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
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- 125000004665 trialkylsilyl group Chemical group 0.000 description 2
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- XRFILHRQJFQRHX-UHFFFAOYSA-N C[SiH](C1=CC=CC=C1)OCCC=C Chemical compound C[SiH](C1=CC=CC=C1)OCCC=C XRFILHRQJFQRHX-UHFFFAOYSA-N 0.000 description 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
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- 239000005751 Copper oxide Substances 0.000 description 1
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
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- KXFSUVJPEQYUGN-UHFFFAOYSA-N trimethyl(phenyl)silane Chemical compound C[Si](C)(C)C1=CC=CC=C1 KXFSUVJPEQYUGN-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1339—Gaskets; Spacers; Sealing of cells
- G02F1/13392—Gaskets; Spacers; Sealing of cells spacers dispersed on the cell substrate, e.g. spherical particles, microfibres
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
- C08F299/02—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
- C08F299/08—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/442—Block-or graft-polymers containing polysiloxane sequences containing vinyl polymer sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L83/10—Block- or graft-copolymers containing polysiloxane sequences
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/0806—Silver
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention, which provides one kind, can effectively mitigate internal stress, and effectively inhibit the resin particle of the generation of rebound.The present invention provides a kind of resin particle, wherein by general formula [(R)3SiO1/2] indicate M unit, by general formula [(R)2SiO2/2] indicate D unit, by general formula [(R) SiO3/2] indicate T unit and by general formula [SiO4/2] in the total number 100% of Q unit that indicates, the total number of the T unit and the Q unit is 4% or less.
Description
Technical field
The present invention relates to the resin particles comprising organic siliconresin.The invention further relates to the companies for having used above-mentioned resin particle
Connect material and connection structural bodies.
Background technique
Miniaturization, lighting, the slimming of Electrical and Electronic component are rapidly developing.At the same time, printed wiring board
Or multiple-plate dimensional stability, reduction warpage and the generation for preventing crack etc. have become technical problem.It is above-mentioned as solving
The method of technical problem can enumerate the method etc. for mitigating internal stress.As the method for mitigation internal stress, such as have been presented for
Silicone particles iso-stress mitigation material is added to method in resin combination etc..
As an example of above-mentioned Silicone particles, following patent documents 1 disclose a kind of spherical polysiloxanes bullet
Property body particle.The main component of above-mentioned spherical shape silicone elastomer particle is silicone elastomer.The above-mentioned poly- silicon oxygen of spherical shape
The average grain diameter of alkane elastomer particle is 0.1~500 μm.Above-mentioned spherical shape silicone elastomer particle, which is substantially free of, to be originated from admittedly
Change the metallic element of catalyst.
In addition, following patent documents 2 disclose a kind of Silicone particles, the polysiloxanes bullet with 100 mass parts
Property body spheroidal particle and 0.5~25 mass parts cladding its surface organic poly sesquisiloxane.Above-mentioned silicone elastomer
The volume average particle size of spheroidal particle is 0.1~100 μm.Above-mentioned organic poly sesquisiloxane is granular.It is above-mentioned to gather organic times
The size of half siloxanes is 60nm or less.
In addition, following patent documents 3 disclose a kind of spongy Silicone particles, obtained by following methods:
Make to have shown in formula (1) silane compound of three functional groups and the silane chemical combination with Liang Ge functional group shown in formula (2)
Object carries out combined polymerization.Above-mentioned spongy Silicone particles are formed by following methods: making the average grain diameter of primary particle
0.1~50 μm of spherical Silicone particles connect into cotton-shaped.The average grain diameter of above-mentioned spongy Silicone particles be 1~
100μm.70% or more of the oil of temporary absorption can be discharged in above-mentioned spongy Silicone particles again.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2006-104456 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2013-40241 bulletin
Patent document 3: Japanese Unexamined Patent Publication 2015-140356 bulletin
Summary of the invention
Invent the technical issues of solved
When the interconnecting piece being attached between shape paired electrode and the adhesive layer being bonded to two connecting object components
When, preferably heating interconnecting piece or adhesive layer are used to make the adhesive curings such as resin.When interconnecting piece or adhesive layer are heated, have
When internal stress generated due to cure shrinkage of the adhesives such as resin etc..The internal stress of generation becomes interconnecting piece or adhesive layer
The main reason for middle generation crack etc., therefore, it is necessary to mitigate internal stress.For documented existing poly- in Patent Documents 1 to 3
Silicone particles, it is difficult to sufficiently mitigate the internal stress generated in interconnecting piece or adhesive layer.
In addition, making to compress when using that documented existing Silicone particles are as spacer in Patent Documents 1 to 3
Silicone particles restore the effect of its original-shape and can cause so-called rebound phenomenon.If be blended in as spacer viscous
The Silicone particles for connecing oxidant layer are sprung back, then after a period of time, the interface between adhesive layer and clung body may
It is peeling-off.
The purpose of the present invention is to provide can effectively mitigate internal stress, and effectively inhibit the resin of the generation of rebound
Particle.It is further an object that providing the connecting material and connection structural bodies for having used above-mentioned resin particle.
Technical means to solve problem
Broad aspect according to the present invention provides a kind of resin particle, wherein by general formula [(R)3SiO1/2] indicate M it is mono-
Member, by general formula [(R)2SiO2/2] indicate D unit, by general formula [(R) SiO3/2] indicate T unit and by general formula [SiO4/2]
In the total number 100% of the Q unit of expression, the total number of the T unit and the Q unit is 4% or less.
In the specified scheme of resin particle of the invention, compression recovery when compressive deformation 40% is 10% or less.
In the specified scheme of resin particle of the invention, 10%K value is 500N/mm2Below.
In the specified scheme of resin particle of the invention, partial size is 0.5 μm or more and 500 μm or less.
In the specified scheme of resin particle of the invention, the resin particle is the particle comprising organic siliconresin.
In the specified scheme of resin particle of the invention, the resin particle is used as spacer.
Broad aspect according to the present invention provides a kind of connecting material, and it includes above-mentioned resin particles, also includes adhesive
Or the particle containing metallic atom.
In the specified scheme of resin particle of the invention, the connecting material includes adhesive.
In the specified scheme of resin particle of the invention, the connecting material includes the particle containing metallic atom.
In the specified scheme of resin particle of the invention, the thermal decomposition temperature of the resin particle is higher than described containing gold
Belong to the fusing point of atomic particle.
In the specified scheme of resin particle of the invention, the connecting material is used to form two connecting object portions of connection
The interconnecting piece of part；
And the sintered body by the particle containing metallic atom is used for form the interconnecting piece.
Broad aspect according to the present invention provides a kind of connection structural bodies, has:
First connecting object component,
Second connecting object component and
The interconnecting piece that the first connecting object component and the second connecting object component are linked together, wherein
The material of the interconnecting piece includes the resin particle.
The effect of invention
In resin particle of the invention, by general formula [(R)3SiO1/2] indicate M unit, by general formula [(R)2SiO2/2] indicate
D unit, by general formula [(R) SiO3/2] indicate T unit and by general formula [SiO4/2] indicate Q unit total number 100%
In, the total number of the T unit and the Q unit is 4% or less.Resin particle of the invention is special due to having above-mentioned technology
Sign, therefore internal stress can be effectively mitigated, and effectively inhibit the generation of rebound.
Detailed description of the invention
Fig. 1 is the sectional view for indicating to have used an example of the connection structural bodies of resin particle of the invention.
Fig. 2 is to indicate the liquid crystal display element for having used resin particle of the invention as spacer used for liquid crystal display element
An example sectional view.
Specific embodiment
In the following, the present invention is described in detail.
(resin particle)
In resin particle of the invention, by general formula [(R)3SiO1/2] indicate M unit, by general formula [(R)2SiO2/2] indicate
D unit, by general formula [(R) SiO3/2] indicate T unit and by general formula [SiO4/2] indicate Q unit total number 100%
In, the total number of the T unit and the Q unit is 4% or less.It should be noted that M unit, D unit, T unit, Q unit
It is well known by the expression of above-mentioned general formula.R in above-mentioned general formula indicates any group.As any group of R, exclude to lead to above-mentioned
The O of Si bonding outside formula unit1/2Group.
For resin particle of the invention due to having above-mentioned technical characteristic, mitigation internal stress can be imitated by having, and be had
Effect inhibits the generation of rebound.
For resin particle of the invention due to having above-mentioned technical characteristic, compression recovery is relatively low, makes to be compressed
Resin particle restore original-shape effect it is opposite be not easy to work, to be not susceptible to spring back.For example, when will be of the invention
When resin particle is used as spacer, spacer and component used for liquid crystal display element etc. can be made to come into full contact with, and can be with more
High precision controlling gap.
When the interconnecting piece that shape paired electrode is electrically connected or the adhesive layer being bonded to two connecting object components,
It is preferred that heating interconnecting piece or adhesive layer are used to make the adhesive curings such as resin.When interconnecting piece or adhesive layer are heated, sometimes
Cure shrinkage due to adhesives such as resins etc. and generate internal stress.The internal stress of generation becomes the original that crack etc. occurs
Cause, therefore preferably remove internal stress.As the method for removing internal stress, the method etc. that heat treatment can be enumerated.However, such as
Resin etc. is used for interconnecting piece or adhesive layer by fruit, then is difficult to sufficiently remove internal stress through heat treatment.The present invention
Resin particle due to having above-mentioned technical proposal, compression recovery is relatively low, restores compressed resin particle
The effect of original-shape is opposite to be not easy to work.Resin particle of the invention is used for interconnecting piece or adhesive layer, though as a result, by
Internal stress is generated in interconnecting piece or adhesive layer in heating etc., and the internal stress of interconnecting piece or adhesive layer is also due to resin particle
Son deformation and effectively mitigated.Occurs crack etc. in interconnecting piece or adhesive layer as a result, can effectively inhibit.
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point sets out, and above-mentioned resin particle preferably comprises the particle of organic siliconresin.Above-mentioned organic siliconresin preferably comprises specific organic
Siloxy units (siliceous key unit).
Above-mentioned organic siloxy units include: the organic siloxy units of simple function of referred to as M unit, are known as D
The organic siloxy units of difunctionality of unit, are known as Q unit at the organic siloxy units of trifunctional for being known as T unit
The organic siloxy units of tetrafunctional.It should be noted that Q unit without containing Direct Bonding on the silicon atoms
The unit of the organic group of carbon atom, but in the present invention, as organic siloxy units.
In above-mentioned organic siloxy units, since siloxanes key is that two silicon atoms pass through an oxygen atoms bond
Made of key, therefore the oxygen atomicity of each silicon atom is considered as 1/2 in siloxanes key, and is expressed as in usually
O1/2.Specifically, for example in a D unit, the silicon atom and two oxygen atoms bonds for including in D unit, and it is each
The silicon atom bonding of a oxygen atom and other unit.That is, the structure of D unit is [- O1/2-(R)2Si-O1/2], due to existing
Two O1/2Unit, D unit are expressed as general formula [(R)2SiO2/2]。
Above-mentioned M unit is by general formula [(R)3SiO1/2] indicate organic siloxy units.Specifically, above-mentioned M is mono-
Member has the structure indicated by following formula (1).
[chemical formula 1]
In above formula (1), R1, R2, R3 respectively indicate arbitrary group.R1, R2, R3 respectively it is preferred indicate alkyl, aryl,
The bivalent organic group that allyl, hydrogen atom or carbon atom number are 1~5.Above-mentioned organic group can containing carbon atom, hydrogen atom,
Oxygen atom.Above-mentioned organic group can be the bivalent hydrocarbon radical that carbon atom number is 1~5.The main chain of above-mentioned organic group is preferably two
Valency alkyl.In above-mentioned organic group, carboxyl or hydroxyl etc. can be bonded on bivalent hydrocarbon radical.The structure indicated by above formula (1)
It can be bonded by R1, R2, R3 with another structure.Oxygen atom in above-mentioned general formula (1) can be with the silicon atom shape of another structure
At siloxanes key, key can also be formed with the atom in addition to the silicon atom of another structure.
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point sets out, and structure shown in above-mentioned formula (1) preferably passes through bivalent hydrocarbon radical and is bonded with other structures.From further effectively mitigating
From the perspective of the viewpoint of internal stress, and the further generation for effectively inhibiting rebound, the oxygen atom in above formula (1) is preferred
Siloxanes key is formed with the silicon atom of another structure, it is also preferred that being bonded with the bivalent hydrocarbon radical of another structure.
Above-mentioned D unit is by general formula [(R)2SiO2/2] indicate polysiloxanes oxygroup unit.Specifically, above-mentioned D unit
With the structure indicated by following formula (2).
[chemical formula 2]
In above formula (2), R4, R5 respectively indicate arbitrary group.R4, R5 preferably respectively indicate alkyl, aryl, allyl
The bivalent organic group that base, hydrogen atom or carbon atom number are 1~5.Above-mentioned organic group can be former containing carbon atom, hydrogen atom, oxygen
Son.Above-mentioned organic group can be the bivalent hydrocarbon radical that carbon atom number is 1~5.The main chain of above-mentioned organic group is preferably divalent hydrocarbon
Base.In above-mentioned organic group, carboxyl or hydroxyl etc. can be bonded on bivalent hydrocarbon radical.It can be with by the structure that above formula (2) indicate
It is bonded by R4, R5 with another structure.Oxygen atom in above-mentioned general formula (2) can form siloxanes with the silicon atom of another structure
Key can also form key with the atom in addition to the silicon atom of another structure.
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point sets out, and structure shown in above-mentioned formula (2) preferably passes through bivalent hydrocarbon radical and is bonded with other structures.From further effectively mitigating
From the perspective of the viewpoint of internal stress, and the further generation for effectively inhibiting rebound, the oxygen atom in above formula (2) is preferred
Siloxanes key is formed with the silicon atom of another structure, it is also preferred that being bonded with the bivalent hydrocarbon radical of another structure.
Above-mentioned T unit is by general formula [(R) SiO3/2] indicate organic siloxy units.Specifically, above-mentioned T is mono-
Member has the structure indicated by following formula (3).
[chemical formula 3]
In above formula (3), R6 indicates arbitrary group.R6 preferably indicates that alkyl, aryl, allyl, hydrogen atom or carbon are former
The bivalent organic group that subnumber is 1~5.Above-mentioned organic group can contain carbon atom, hydrogen atom, oxygen atom.Above-mentioned organic group
It can be the bivalent hydrocarbon radical that carbon atom number is 1~5.The main chain of above-mentioned organic group is preferably bivalent hydrocarbon radical.In above-mentioned organic group
In group, carboxyl or hydroxyl etc. can be bonded on bivalent hydrocarbon radical.R6 and another structure can be passed through by the structure that above formula (3) indicate
Bonding.Oxygen atom in above-mentioned general formula (3) can form siloxanes key with the silicon atom of another structure, can also with remove another knot
Atom except the silicon atom of structure forms key.
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point sets out, and structure shown in above-mentioned formula (3) preferably passes through bivalent hydrocarbon radical and is bonded with other structures.From further effectively mitigating
From the perspective of the viewpoint of internal stress, and the further generation for effectively inhibiting rebound, the oxygen atom in above formula (3) is preferred
Siloxanes key is formed with the silicon atom of another structure, it is also preferred that being bonded with the bivalent hydrocarbon radical of another structure.
Above-mentioned Q unit is by general formula: [SiO4/2] indicate organic siloxy units (siloxane unit).It is specific and
Speech, above-mentioned Q unit have the structure indicated by following formula (4).
[chemical formula 4]
Oxygen atom in above formula (4) can form siloxanes key with the silicon atom of another structure, can also with remove another knot
Atom except the silicon atom of structure forms key.From the viewpoint for further effectively mitigating internal stress, and further effectively
From the perspective of ground inhibits the generation of rebound, the oxygen atom in above formula (4) preferably forms siloxanes with the silicon atom of another structure
Key, it is also preferred that being bonded with the bivalent hydrocarbon radical of another structure.
In resin particle of the invention, by general formula [(R)3SiO1/2] indicate M unit, by general formula [(R)2SiO2/2] indicate
D unit, by general formula [(R) SiO3/2] indicate T unit and by general formula [SiO4/2] indicate Q unit total number 100%
In, the total number (TnQn) of the T unit and the Q unit is 4% or less.
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point sets out, above-mentioned M unit, above-mentioned D unit, above-mentioned T unit, in the total number 100% of above-mentioned Q unit, above-mentioned TnQn is preferably
3% hereinafter, more preferably 2% or less.The lower limit of above-mentioned TnQn is not particularly limited.Above-mentioned TnQn can be 0%, and (number is
It 0), can also be more than 0%.
Above-mentioned TnQn can pass through29Si- solid NMR analyzes resin particle to be calculated.Specifically, can be with as follows
Mode is calculated.
The calculation method of TnQn:
Using the resin particle by sufficiently drying, and by under following determination conditions29The measurement of Si- solid NMR
(DD/MAS method), can obtain the integrated value of the semaphore of above-mentioned each unit.According to the semaphore of the above-mentioned each unit of acquisition
Integrated value can calculate TnQn.
29Si- solid NMR measures the determination condition of (DD/MAS method):
Device: " JNM-ECX400 " of Jeol Resonance company manufacture
Observing nuclear:29Si
Probe: solid NMR 8mm probe
MAS rotation speed: 7kHz
Measuring method: pulse (DD/MAS)
Pulse width: 3.45 μ s (29Si/90 degree)
Delay time: 315 seconds
Acquisition time: 21 milliseconds
Scanning times: 500 times
In addition, being originated from above-mentioned each unit29The chemical shift of Si- solid NMR is described generally below.From above-mentioned each unit
's29The chemical shift of Si- solid NMR can be considered any group being bonded with Si base and suitably be determined.
M unit: 5ppm~15ppm
D unit: -30ppm~-5ppm
T unit: -75ppm~-50ppm
Q unit: -120ppm~-100ppm
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point set out, compression recovery when by above-mentioned resin particle compressive deformation 40% be preferably 10% hereinafter, more preferably 9% with
Under, and preferably 0.1% or more, more preferably 1% or more.
Compression recovery when above-mentioned resin particle compressive deformation 40% can be measured by following manner.
Resin particle is dispersed on sample stage.For each resin particle of distribution, using Mini compressed testing machine,
On the flat surface of cylindrical body (100 μm of diameter, be made of diamond), at 25 DEG C, the center position along resin particle applies
Load, until resin particle compressive deformation 40% (reversion load value).Then, it carries out except lotus, until original load value
Until (0.40mN).Load-compression displacement during this is measured, it according to the following formula, can be in the hope of at 25 DEG C when compressive deformation 40%
Compression recovery.It should be noted that loading speed is set as 0.33mN/sec.As above-mentioned Mini compressed testing machine, such as
" the Mini compressed testing machine MCT-W200 " of Shimadzu Scisakusho Ltd's manufacture, Fischer company can be used to manufacture
" Fischer Scope H-100 " etc..
Compression recovery (%)=[L2/L1] × 100
L1: from origin load value when applying load to the compression displacement of reverse load value
L2: the lotus that removes from reverse load value when liberating load to origin load value is displaced
The 10%K value of above-mentioned resin particle is preferably 5N/mm2More than, more preferably 10N/mm2More than, and preferably
500N/mm2Hereinafter, more preferably 200N/mm2Hereinafter, further preferably 150N/mm2Hereinafter, particularly preferably 100N/mm2
Below.It, can further effectively when the 10%K value of above-mentioned resin particle is above-mentioned lower limit or more and the above-mentioned upper limit or less
Internal stress is mitigated, furthermore, it is possible to further effectively inhibit the generation of rebound.
The 10%K value of above-mentioned resin particle can be measured in the following way.
Using Mini compressed testing machine, on the flat surface of cylindrical body (100 μm of diameter, Buddha's warrior attendant is made of stones), at 25 DEG C,
A resin particle is compressed under conditions of compression speed is 0.3mN/sec, maximum test load is 20mN.Measurement at this time negative
Load value (N) and compression displacement (mm).According to obtained measured value, the 10%K value at 25 DEG C can be obtained by following formula.As
Above-mentioned Mini compressed testing machine, such as " the Mini compressed testing machine MCT- of Shimadzu Scisakusho Ltd's manufacture can be used
W200 ", " the Fischer Scope H-100 " of the manufacture of Fischer company etc..The 10%K value of above-mentioned resin particle preferably passes through
Arithmetic average is carried out to the 10%K value of 50 optional resin particles to calculate.
10%K value (N/mm2)=(3/21/2)·F·S-3/2·R-1/2
F: the load value (N) when resin particle compressive deformation 10%
S: the compression displacement (mm) when resin particle compressive deformation 10%
R: the radius (mm) of resin particle
Above-mentioned K value is universal and quantitatively indicates the hardness of resin particle.It, can be quantitatively and clear by using above-mentioned K value
The hardness of ground expression resin particle.
The partial size of above-mentioned resin particle can be appropriately configured depending on the application.The partial size of above-mentioned resin particle is preferably 0.5 μ
M or more, more preferably 1 μm or more, and preferably 500 μm hereinafter, more preferably 450 μm hereinafter, further preferably 100 μm with
Under, still more preferably for 50 μm hereinafter, particularly preferably 20 μm or less.When above-mentioned resin particle partial size be above-mentioned lower limit with
When below the upper and described upper limit, internal stress further can be effectively mitigated, and can further effectively inhibit
The generation of rebound.When the partial size of above-mentioned resin particle is 0.5 μm or more and 20 μm or less, above-mentioned resin particle is applicable to answer
The purposes of power mitigation material.When the partial size of above-mentioned resin particle is 1 μm or more and 100 μm or less, above-mentioned resin particle can be fitted
Purposes for gap control material.
When resin particle is spherical shape, the partial size of above-mentioned resin particle indicates diameter, when resin particle is not spherical shape,
Indicate maximum inner diameter.
The partial size of above-mentioned resin particle is preferably average grain diameter, more preferably number average bead diameter.The partial size of above-mentioned resin particle
Particle size distribution device etc. can be used to acquire.It is, for example, possible to use laser light scattering light, resistance variations, imaging is utilized
The particle size distribution device of the principles such as image analysis afterwards.Specifically, the measuring method of the partial size as resin particle, example
As the following methods can be given: using the particle size distribution device (" Multisizer of Beckman Coulter company manufacture
4 ") partial size of about 100000 resin particles, is measured, and calculates average value.The partial size of resin particle preferably passes through following
Method acquires: by electron microscope or optical microscopy, observing 50 arbitrary resin particles, and calculates average value.
From the viewpoint of further effectively mitigating internal stress, the coefficient of variation of the partial size of above-mentioned resin particle
(CV value) is preferably 10% hereinafter, more preferably 7% hereinafter, further preferably 5% or less.When the partial size of above-mentioned resin particle
The coefficient of variation (CV value) when being the above-mentioned upper limit or less, resin particle is applicable to stress and mitigates material or gap control material
Purposes.
The above-mentioned coefficient of variation (CV value) can be measured by following manner.
CV value (%)=(ρ/Dn) × 100
ρ: the standard deviation of the partial size of resin particle
Dn: the average value of the partial size of resin particle
The shape of above-mentioned resin particle is not particularly limited.The shape of above-mentioned resin particle can be spherical shape, be also possible to
The shape in addition to spherical shape such as pancake.
The use of above-mentioned resin particle is not particularly limited.Above-mentioned resin particle is suitable for various uses.Above-mentioned resin particle
Son is preferably used as spacer.It as the application method of above-mentioned spacer, can enumerate: spacer used for liquid crystal display element, gap control
System spacer and stress mitigation spacer etc..Above-mentioned gap control spacer, can be used in order to ensure interval height and
The gap of the laminated chips of planarization controls, and can be used for the thickness of the flatness and adhesive layer in order to ensure glass surface
Optical component gap control etc..The stress that above-mentioned stress mitigation spacer can be used for sensor chip etc. mitigates, and
The stress for the interconnecting piece that two connecting object components are linked together mitigates.Above-mentioned stress mitigation spacer can be used for power
Connecting material, bonding agent of sensor of device etc..Above-mentioned spacer is preferred for the connecting material of power device, and
It is preferred for the bonding agent of sensor.
Above-mentioned resin particle is preferably used as spacer used for liquid crystal display element, and is preferred for week used for liquid crystal display element
Side sealant.In above-mentioned perimeter seal used for liquid crystal display element, above-mentioned resin particle works preferably as spacer.By
There is good compression deflection characteristics in above-mentioned resin particle, therefore as spacer and configured in base when by above-mentioned resin particle
When between plate, spacer can be efficiently configured between substrate.In addition, liquid crystal can be inhibited for above-mentioned resin particle
Show the scratch of element component etc., therefore in the liquid crystal display element for having used above-mentioned spacer used for liquid crystal display element, no
It is bad that display easily occurs.
In addition, above-mentioned resin particle is suitable as inorganic filler, the additive of toner, shock absorbent or absorption of vibrations
Agent.For example, above-mentioned resin particle can be used as the substitute of rubber or spring etc..
(other details of resin particle)
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point sets out, and above-mentioned resin particle is preferably the particle for including organic siliconresin.
The material of above-mentioned organic siliconresin is preferably the silane compound that there is radically polymerizable group to roll into a ball and has carbon former
The silane compound for the hydrophobic grouping that subnumber is 5 or more, it is however preferred to have radically polymerizable group group and carbon atom number are 5 or more
Hydrophobic grouping silane compound, preferably two ends have radically polymerizable group group silane compound.When making this
When a little materials are reacted, siloxanes key is formed.In obtained organic siliconresin, it will usually residual free radicals polymerizable group
The hydrophobic grouping for being 5 or more with carbon atom number.By using such material, can be readily available comprising partial size be 1 μm with
Upper and 200 μm of above-mentioned organic siliconresins below particle, and it is possible to improve the resistance to of the particle containing above-mentioned organic siliconresin
Chemical agent simultaneously reduces its penetrability.
In the silane compound rolled into a ball with above-mentioned radically polymerizable group, radically polymerizable group rolls into a ball preferably direct bonding
On the silicon atoms.It can be used alone the above-mentioned silane compound with radically polymerizable group group, can also combine makes
With two or more.
The above-mentioned silane compound with radically polymerizable group group is preferably alkoxysilane compound containing trialkylsilyl group in molecular structure.As above-mentioned tool
Have radically polymerizable group roll into a ball silane compound, can enumerate: vinyltrimethoxysilane, vinyltriethoxysilane,
Dimethoxymethylvinylchlane, diethoxymethylvinylschane, divinyl methoxy-ethylene base silane, divinyl
Base oxethyl vinyl silanes, divinyl dimethoxysilane, divinyl diethoxy silane and 1,3- divinyl
Tetramethyl disiloxane etc..
In the silane compound of the above-mentioned hydrophobic grouping for being 5 or more with carbon atom number, preferably carbon atom number is 5 or more
Hydrophobic grouping be bonded directly on silicon atom.It can be used alone the hydrophobic grouping for being 5 or more with carbon atom number
Above-mentioned silane compound can also be applied in combination two or more.
The silane compound of the above-mentioned hydrophobic grouping for being 5 or more with carbon atom number is preferably alkoxysilane compound containing trialkylsilyl group in molecular structure.
As the silane compound of the above-mentioned hydrophobic grouping for being 5 or more with carbon atom number, can enumerate: phenyltrimethoxysila,e, two
Methoxymethylphenyl silane, diethoxymethyl phenyl silane, dimethyl methyl phenyl silane, dimethylethyloxy phenyl
Silane, hexaphenyldisiloxane, 1,3,3,5- tetramethyl -1,1,5,5- tetraphenyl trisiloxanes, five phenyl -1 1,1,3,5,5-,
3,5- trimethyl trisiloxanes, hexaphenyl cyclotrisiloxane, (trimethyl silicane alkoxy) silane of phenyl three and octaphenyl ring four
Siloxanes etc..
In the above-mentioned silane compound for 5 or more hydrophobic grouping with radically polymerizable group group and carbon atom number,
It is preferred that free radical polymerizable group is bonded directly on silicon atom, and preferably carbon atom number is direct for 5 or more hydrophobic grouping
It is bonded on silicon atom.It is above-mentioned with radically polymerizable group group and carbon atom number be 5 or more hydrophobic grouping silane chemical combination
Object can be used alone, and can also be applied in combination two or more.
As it is above-mentioned with radically polymerizable group group and carbon atom number be 5 or more hydrophobic grouping silane compound,
It can enumerate: phenyl vinyl dimethoxysilane, phenyl vinyl diethoxy silane, phenyl methyl ethenylmethoxy silicon
Alkane, phenyl methyl vinylethoxysilane, diphenylethlene methoxylsilane, diphenylacetylene Ethoxysilane, benzene
Base divinyl methoxy silane, diethylamino phenyl alkenyl Ethoxysilane and 1,1,3,3- tetraphenyl -1,3- divinyl two
Siloxanes etc..
In use state the silane compound with radically polymerizable group group and it is above-mentioned with carbon atom number be 5 or more
In the case that the silane compound of hydrophobic grouping is to obtain the particle comprising organic siliconresin, preferably with the use of following weight ratios.
It is preferred that the above-mentioned silane compound with radically polymerizable group group and the above-mentioned hydrophobic grouping for being 5 or more with carbon atom number
Silane compound is 1:1~1:20 use with weight ratio, more preferably with 1:5~1:15 use.
In whole silane compounds for obtaining the above-mentioned particle comprising organic siliconresin, radically polymerizable group group
Quantity and carbon atom number be 5 or more the ratio of number of hydrophobic grouping be preferably 1:0.5~1:20m, more preferably 1:1~1:
15。
The above-mentioned particle comprising organic siliconresin, which preferably has, is bonded to diformazan made of on a silicon atom there are two methyl
Radical siloxane skeleton, also, the material of above-mentioned organic siliconresin is preferably made of two methyl are bonded on a silicon atom
Silane compound.In such a case, it is possible to further effectively mitigate internal stress, and can further effectively
Inhibit the generation of rebound.
From the viewpoint for further effectively mitigating internal stress, and further effectively inhibit the sight of the generation of rebound
Point set out, in the above-mentioned particle comprising organic siliconresin, preferably make above-mentioned silane compound pass through radical polymerization initiator into
Row reaction, forms siloxanes key.In general, when the polycondensation by using acid or base catalyst is above-mentioned comprising organosilicon tree to synthesize
When the particle of rouge, it is difficult to obtain the particle containing partial size for 10 μm or more and 500 μm organic siliconresins below, be particularly difficult to obtain
Obtain the particle containing partial size for 100 μm of organic siliconresins below.In this regard, by using radical polymerization initiator and having upper
State the silane compound of technical characteristic, available is the grain of 1 μm or more and 500 μm organic siliconresin below containing partial size
Son, also it is available containing partial size be 10 μm or more organic siliconresin particle, can also obtain containing partial size for 100 μm with
Under organic siliconresin particle.
In order to obtain the above-mentioned particle comprising organic siliconresin, can without using have and the hydrogen atom of silicon atom bonding
Silane compound.In which case it is possible to use radical polymerization initiator polymerize silane compound, without the use of gold
Metal catalyst.As a result, can make include machine silicone resin particle without containing metallic catalyst, it is possible to reduce comprising above-mentioned organic
The content of metallic catalyst in the particle of silicone resin, and further can effectively mitigate internal stress, further have
Effect ground inhibits the generation of rebound.
From the viewpoint of reducing penetrability, above-mentioned resin particle is preferably resin particle as described below: comprising organic
Silicone resin and resin different from organic siliconresin, and the outer surface of the organic siliconresin is coated with and above-mentioned is different from organosilicon
The resin of resin.From the viewpoint of reducing penetrability, the above-mentioned particle comprising organic siliconresin is preferably grain as described below
Son: comprising organic siliconresin and different from the resin of organic siliconresin, and the outer surface of the organic siliconresin be coated with it is above-mentioned
Different from the resin of organic siliconresin.
When above-mentioned resin particle is comprising organic siliconresin and different from the resin of organic siliconresin, above-mentioned organic siliconresin
Entire outer surface can be coated by the above-mentioned resin different from organic siliconresin, there may also be not by it is above-mentioned be different from have
The part that the resin of machine silicone resin is coated.
As the above-mentioned resin different from organic siliconresin, the resin (vinylite) etc. with vinyl can be enumerated.
It as the above-mentioned resin different from organic siliconresin, can be used alone, can also be applied in combination two or more.
From the viewpoint of further decreasing penetrability, the above-mentioned resin different from organic siliconresin preferably has ethylene
The resin of base, more preferably divinylbenzene or styrene.
The specific preparation method of the above-mentioned particle comprising organic siliconresin include: by suspension polymerization, dispersion copolymerization method,
Fine emulsion polymerization or emulsion polymerization method etc. carry out the polymerization reaction of silane compound, to prepare the grain for including organic siliconresin
The method etc. of son.After the polymerization for carrying out silane compound obtains oligomer, by suspension polymerization, dispersion copolymerization method, thin
Emulsion polymerization or emulsion polymerization method etc. carry out the polymerization reaction of the silane compound as polymer (oligomer etc.), preparation
Particle comprising organic siliconresin.For example, the silane compound with vinyl can be made to be polymerize, acquisition has in end
With the silane compound of the vinyl of silicon atom bonding.The silane compound with phenyl can be made to be polymerize, obtained in side
Have on chain with the silane compound of the phenyl of silicon atom bonding as polymer (oligomer etc.).Make the silane with vinyl
Compound and silane compound with phenyl are polymerize, with obtain end have with the vinyl of silicon atom bonding and
Have on side chain with the silane compound of the phenyl of silicon atom bonding as polymer (oligomer etc.).
It is different from made of the resin cladding of above-mentioned organic siliconresin to obtain the outer surface of above-mentioned organic siliconresin
Resin particle can make the organic siliconresin and the above-mentioned resin different from organic siliconresin after preparing organic siliconresin
Carry out polymerization reaction.
(connecting material)
Above-mentioned connecting material is used to form the interconnecting piece of two connecting object components of connection.Above-mentioned connecting material includes above-mentioned
Resin particle also includes adhesive or the particle containing metallic atom.Above-mentioned connecting material is preferably by containing metallic atom
The sintered body of particle is used to form above-mentioned interconnecting piece.Resin particle of the invention is not included in above-mentioned adhesive.It is above-mentioned to contain gold
Belong to and does not include resin particle of the invention in atomic particle.
The thermal decomposition temperature of above-mentioned resin particle is preferably higher than the fusing point of the above-mentioned particle containing metallic atom.Above-mentioned resin
The thermal decomposition temperature of particle preferably than high 10 DEG C of fusing point or more of the above-mentioned particle containing metallic atom, more preferably high 30 DEG C with
On, most preferably high 50 DEG C or more.
It as the above-mentioned particle containing metallic atom, can enumerate: metallic and metallic compound particle etc..Above-mentioned metal
Compound particles include metallic atom and the atom in addition to the metallic atom.Specific reality as above-mentioned metallic compound particle
Example, can enumerate: metal oxide particle, metal carbonate particles, carboxylate metal salt particle and metal complex particle etc..
Above-mentioned metallic compound particle is preferably metal oxide particle.For example, for above-mentioned metal oxide particle, in reducing agent
In the presence of, after heating when by connection forms metallic, it is sintered.Above-mentioned metal oxide particle is clipped wire
The precursor of son.As above-mentioned carboxylate metal salt particle, metal acetate particle etc. can be enumerated.
It as the metal for constituting above-mentioned metallic and above-mentioned metal oxide particle, can enumerate: silver, copper and gold etc..Structure
It is preferably silver or copper, particularly preferably silver at the metal of above-mentioned metallic and above-mentioned metal oxide particle.Therefore, above-mentioned gold
Belonging to particle is preferably silver particles or copper particle, more preferably silver particles.Above-mentioned metal oxide particle preferably aoxidizes silver particles
Or copper oxide particle, more preferably aoxidize silver particles.Using silver particles and oxidation silver particles, it is possible to reduce connection
Residue afterwards, and volume reduction rate can be made very small.As the example of the silver oxide in above-mentioned oxidation silver particles, can arrange
It lifts: Ag2O and AgO.
The above-mentioned particle containing metallic atom is preferably sintered by the heating lower than 400 DEG C.It is above-mentioned to contain metal
Atomic particle is sintered temperature (sintering temperature) and is more preferably 350 DEG C hereinafter, and preferably 300 DEG C or more.Contain when above-mentioned
Have the particle of metallic atom be sintered temperature be the lower limit more than and the upper limit below when, burning can be effectively performed
Knot, energy needed for further decreasing sintering, and carrying capacity of environment can be reduced.
When the above-mentioned particle containing metallic atom is metal oxide particle, it is preferable to use reducing agent.It is gone back as above-mentioned
The example of former agent can be enumerated: alcoholic compound (compound with alcoholic extract hydroxyl group), carboxylic acid compound (with carboxyl compound),
Amine compounds (compound with amino) etc..Above-mentioned reducing agent can be used alone, can also be applied in combination two kinds with
On.
As above-mentioned alcoholic compound, alkylol etc. can be enumerated.As the specific example of above-mentioned alcoholic compound, can enumerate, example
Such as: ethyl alcohol, propyl alcohol, butanol, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, tip-nip, dodecanol, tridecanol, ten
Four alkanols, pentadecanol, hexadecanol, heptadecanol, octadecanol, nonadecanol, eicosanol etc..In addition, above-mentioned alcohol compound
Object is not limited to primary alcohol compound, and secondary alcohol compounds, tertiary alcohols compound, alkanediol can be used and have cyclic annular knot
The alcoholic compound of structure.In addition, the change that ethylene glycol and triethylene glycol etc. have multiple alcohol radicals can be used as above-mentioned alcoholic compound
Close object.In addition it is possible to use the compounds such as citric acid, ascorbic acid and glucose are as above-mentioned alcoholic compound.
As above-mentioned carboxylic acid compound, alkyl carboxylic acid etc. can be enumerated.The specific example of above-mentioned carboxylic acid compound includes: fourth
Acid, valeric acid, caproic acid, enanthic acid, octanoic acid, n-nonanoic acid, capric acid, hendecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecane
Acid, hexadecanoic acid, Heptadecanoic acide, octadecanoid acid, nonadecylic acid, arachic acid etc..In addition, above-mentioned carboxylic acid compound is not limited to primary
Secondary carboxylic ester class compound, tertiary carboxylic acid class compound, dicarboxylic acids and with cyclic structure also can be used in carboxylic acid compound
Carboxyl compound.
It as the example of above-mentioned amine compounds, can enumerate: alkylamine etc..The specific example of above-mentioned amine compounds includes: fourth
Amine, amylamine, hexylamine, heptyl amice, octylame, nonyl amine, decyl amine, heptadecyl-amine, dodecyl amine, tridecyl amine, tetradecylamine, pentadecane
Amine, cetylamine, heptadecylamine (HDA), octadecylamine, nonadecane amine, eicosane amine etc..In addition, above-mentioned amine compounds can have branch link
Structure.The example of amine compounds with branched structure can be enumerated: 2 ethyl hexylamine and 1,5- dimethylhexylamine.Above-mentioned amine compounds
Object is not limited to primary amine compound, and secondary-amine compound, tertiary amine compounds and the amination with cyclic structure can be used
Close object.
Above-mentioned reducing agent can be the organic matter with aldehyde radical, ester group, sulfonyl, ketone group etc., be also possible to carboxylic acid metal
The organic matters such as salt.Carboxylic metallic salt may be used as the precursor of metallic, further, since containing organic matter, therefore also be used as
The reducing agent of metal oxide particle.
Relative to above-mentioned 100 parts by weight of metal oxide particle, the content of above-mentioned reducing agent is preferably 1 parts by weight or more,
More than more preferably 10 parts by weight, and preferably 1000 parts by weight are hereinafter, more preferably 500 parts by weight are hereinafter, further more excellent
It is selected as 100 parts by weight or less.When the content of above-mentioned reducing agent is the lower limit or more, can make above-mentioned containing metallic atom
Particle is further fine and close to be sintered.As a result, the interconnecting piece formed by the sintered body of the above-mentioned particle containing metallic atom
Exothermicity and heat resistance increase.
Use the reducing agent with the melting point lower than the sintering temperature of the above-mentioned particle containing metallic atom (connection temperature)
When, it can be aggregated in connection, exist and be easy to produce the tendency in gap in interconnecting piece.It, should due to having used carboxylic metallic salt
Carboxylic metallic salt will not melt in connection due to heating, be able to suppress the generation of hole.In addition, in addition to carboxylic acid metal
Other than salt, the metallic compound for containing organic matter can be used as reducing agent.
From the viewpoint of further effectively improving bonding strength, above-mentioned connecting material preferably comprises adhesive.On
Adhesive is stated to be not particularly limited.Well known insulative resin can be used as above-mentioned adhesive.Above-mentioned adhesive preferably comprises thermoplastic
Property ingredient (thermoplastic compound) or curability composition, further preferably curability composition.Reality as above-mentioned curability composition
Example, can enumerate: photo-curable ingredient and thermosetting component.Above-mentioned photo-curable ingredient preferably comprises photocurable compound and light
Polymerization initiator.Above-mentioned thermosetting component preferably comprises heat-curable compounds and thermal curing agents.As the example of above-mentioned adhesive,
It can enumerate: vinylite, thermoplastic resin, curable resin, thermoplastic block copolymers and elastomer.Above-mentioned adhesive
It can be used alone, can also be applied in combination two or more.
As above-mentioned vinylite, can enumerate, such as: vinyl acetate resin, acrylic resin, styrene resin
Deng.As above-mentioned thermoplastic resin, can enumerate, such as: polyolefin resin, vinyl-vinyl acetate copolymer and polyamide resin
Rouge etc..As above-mentioned curable resin, can enumerate, such as: epoxy resin, polyurethane resin, polyimide resin and unsaturation
Polyester resin etc..It should be noted that can be normal temperature cured type resin, thermohardening type resin, light solid for above-mentioned curable resin
Change type resin or moisture-curable resin.Above-mentioned curable resin can be applied in combination with curing agent.It is embedding as above-mentioned thermoplasticity
Section copolymer, such as can enumerate: Styrene-Butadiene-Styrene Block Copolymer, styrene-isoprene-phenylethene block
Copolymer, the hydrogenated products of Styrene-Butadiene-Styrene Block Copolymer and styrene-isoprene-phenylethene are embedding
The hydrogenated products etc. of section copolymer.As above-mentioned elastomer, can enumerate, such as: styrene-butadiene copolymer rubber and third
Alkene nitrile-styrene block copolymer rubber etc..
In addition, above-mentioned adhesive can be solvent.As above-mentioned solvent, water and organic solvent can be enumerated.From further mentioning
From the perspective of the removability of high solvent, above-mentioned solvent is preferably organic solvent.As above-mentioned organic solvent, can enumerate: ethyl alcohol
Equal alcoholic compounds；The ketone compounds such as acetone, methyl ethyl ketone, cyclohexanone；The aromatic hydrocarbon chemical combination such as toluene, dimethylbenzene, durol
Object；Cellosolve, methyl cellosolve, butyl cellosolve, carbitol, methyl carbitol, butyl carbitol, propylene glycol monomethyl ether, two
The glycol ethers compound such as propylene glycol monomethyl ether, dipropylene glycol diethyl ether, Tripropylene glycol monomethyl Ether；Ethyl acetate, butyl acetate,
Butyl lactate, cellosolve acetate, acetic acid butyl cellosolve, carbitol acetate, acetic acid butyl carbitol, propylene glycol monomethyl ether acetic acid
The ester compounds such as ester, dipropylene glycol monomethyl ether acetic acid esters, propene carbonate；The aliphatic hydrocarbon compounds such as octane, decane；And stone
Petroleum solvents such as oily ether, naphtha etc..
From the viewpoint of further effectively improving bonding strength, above-mentioned connecting material preferably comprises epoxy resin.
It include former containing metal in above-mentioned connecting material due to can effectively play resin particle bring effect of the invention
In the case where the particle of son, the content of the particle in above-mentioned connecting material containing metallic atom is preferably higher than above-mentioned resin particle
Content, more preferably higher than 10 weight % or more are further preferably higher than 20 weight % or more.
In above-mentioned 100 weight % of connecting material, the content of above-mentioned resin particle is preferably 0.1 weight % or more, more excellent
It is selected as 1 weight % or more, and preferably 50 weight % are hereinafter, more preferably 30 weight % or less.When containing for above-mentioned resin particle
When amount is above-mentioned lower limit or more and the above-mentioned upper limit or less, the internal stress in interconnecting piece further can be effectively mitigated.
When above-mentioned connecting material includes the above-mentioned particle containing metallic atom, the above-mentioned particle containing metallic atom is upper
The content stated in 100 weight % of connecting material is preferably 0.3% weight or more, more preferably 3 weight % or more, and preferably 50
Weight % is hereinafter, more preferably 40 weight % or less.When the content of the above-mentioned particle containing metallic atom is above-mentioned lower limit or more
And when below the above-mentioned upper limit, connection resistance is further decreased.
When above-mentioned connecting material contains adhesive, content of the above-mentioned adhesive in above-mentioned 100 volume % of connecting material
Preferably 5 volume % or more, more preferably 10 volume % or more, and preferably 40 volume % are hereinafter, more preferably 20 volume %
Below.When the content of above-mentioned adhesive is above-mentioned lower limit or more and the above-mentioned upper limit or less, connection can be further effectively improved
Intensity.
(connection structural bodies)
It by using comprising above-mentioned resin particle, and include that the connecting material of adhesive or the particle containing metallic atom is come
Connecting object component is connected, connection structural bodies can be obtained.
Above-mentioned connection structural bodies has: the first connecting object component, the second connecting object component, by it is above-mentioned first connection pair
The interconnecting piece to link together as component and above-mentioned second connecting object component.The material of above-mentioned interconnecting piece includes above-mentioned resin particle
Son.The material of above-mentioned interconnecting piece is preferably above-mentioned connecting material.Above-mentioned interconnecting piece is preferably the company formed by above-mentioned connecting material
Connect structural body.
Fig. 1 is the sectional view for indicating to have used an example of the connection structural bodies of resin particle of the invention.
Connection structure 51 shown in FIG. 1 has: the first connecting object component 52, the second connecting object component 53, connection the
The interconnecting piece 54 of one connecting object component 52 and the second connecting object component 53.
Interconnecting piece 54 includes above-mentioned resin particle 1.Resin particle 1 is not connect with the first connecting object component 52 and second pair
As the contact of both components 53.Resin particle 1 is used as stress mitigation and uses spacer.In Fig. 1, for ease of description, schematically
Ground shows resin particle 1.
Interconnecting piece 54 includes gap control particle 61 and metallic connection parts 62.In interconnecting piece 54, a gap controls grain
Son 61 is contacted with both the first connecting object component 52 and the second connecting object component 53.Gap control particle 61, which can be, leads
Conductive particles or particle without electric conductivity.Metallic connection parts 62 are the sintered bodies of the particle containing metallic atom.Metal connects
Socket part 62 is formed and being sintered to the particle containing metallic atom.Metallic connection parts 62 are by making containing metallic atom
Then pellet melting is solidified to form it.Metallic connection parts 62 are the melting and solidification products of the particle containing metallic atom.
Above-mentioned first connecting object component can have first electrode on the surface.Above-mentioned second connecting object component can be with
There is second electrode on the surface.Above-mentioned first electrode and above-mentioned second electrode preferably pass through above-mentioned interconnecting piece and realize electrical connection.
The manufacturing method of above-mentioned connection structural bodies is not particularly limited.One reality of the manufacturing method as connection structural bodies
Example, can enumerate: configure above-mentioned connecting material between the first connecting object component and the second connecting object component to obtain lamination
Body, the method etc. that then laminated body is heated and pressurizeed.The pressure of above-mentioned pressurization is 9.8 × 104~4.9 × 106Pa is left
It is right.The temperature of above-mentioned heating is 120~220 DEG C or so.For connecting the electricity of the electrode, configuration of flexible printed board on resin film
The pressure of the above-mentioned pressurization of the electrode of pole and Trackpad is 9.8 × 104~1.0 × 106Pa or so.
The specific example of above-mentioned connecting object component includes: the electronic components such as semiconductor chip, capacitor and diode, print
The electronic component etc. of the circuit boards such as brush substrate, flexible printed board, glass epoxy board and glass substrate etc..Above-mentioned connecting object
Component is preferably electronic component.At least one of above-mentioned first connecting object component and above-mentioned second connecting object component are preferred
For semiconductor wafer or semiconductor chip.Above-mentioned connection structural bodies is preferably semiconductor device.
Above-mentioned connecting material is also applied for Trackpad.Therefore, above-mentioned connecting object component is preferably flexible substrate or resin
Configured with connecting object component made of electrode on the surface of film.Above-mentioned connecting object component is preferably flexible substrate, and excellent
It is selected as on the surface of resin film configured with connecting object component made of electrode.It is flexible printed board etc. in above-mentioned flexible substrate
In the case of, flexible substrate usually has electrode on the surface thereof.
It as electrode of the configuration on above-mentioned connecting object component, can enumerate: gold electrode, nickel electrode, tin electrode, aluminium electricity
Pole, copper electrode, silver electrode, molybdenum electrode and tungsten electrode etc..In the case where above-mentioned connecting object component is flexible substrate, above-mentioned electricity
Highly preferred is gold electrode, nickel electrode, tin electrode or copper electrode.In the case where above-mentioned connecting object component is glass substrate, on
Stating electrode is preferably aluminium electrode, copper electrode, molybdenum electrode or tungsten electrode.It should be noted that when above-mentioned electrode is aluminium electrode, it can
To be the electrode individually formed by aluminium, it is also possible to the surface superimposed layer aluminium layer of metal oxide layer and the electrode that is formed.As
The material of above-mentioned metal oxide layer can be enumerated: doped with the indium oxide of trivalent metallic element, doped with trivalent metallic element
Zinc oxide etc..It as above-mentioned trivalent metallic element, can enumerate: Sn, Al, Ga etc..
In addition, above-mentioned resin particle is applicable to make spacer used for liquid crystal display element.Above-mentioned first connecting object component can
To be the first component used for liquid crystal display element.Above-mentioned second connecting object component can be the second component used for liquid crystal display element.
Above-mentioned interconnecting piece can be, and make the above-mentioned first component used for liquid crystal display element and above-mentioned second component used for liquid crystal display element
In the state of opposed, to the periphery of the above-mentioned first component used for liquid crystal display element and above-mentioned second component used for liquid crystal display element into
The sealing of row sealing.
Above-mentioned resin particle also is used as sealing material for liquid crystal display device.Liquid crystal display element has: the first liquid crystal
Show element component, the second component, sealing and liquid crystal used for liquid crystal display element.Above-mentioned sealing is making above-mentioned first liquid
In the state that crystal display element component and above-mentioned second component used for liquid crystal display element are opposed, to above-mentioned first liquid crystal display member
The periphery of part component and above-mentioned second component used for liquid crystal display element is sealed.Above-mentioned liquid crystal is on the inside of sealing, configuration
Between the above-mentioned first component used for liquid crystal display element and above-mentioned second component used for liquid crystal display element.In the liquid crystal display element
In, it is applicable in liquid crystal dripping process, and form above-mentioned sealing by making sealant for liquid crystal dripping process heat cure.
Fig. 2 is to indicate the liquid crystal display element for having used resin particle of the invention as spacer used for liquid crystal display element
An example sectional view.
Liquid crystal display element 81 shown in Fig. 2 has a pair of of transparent glass substrate 82.Transparent glass substrate 82 is opposed
There is insulating film (not shown) on surface.As the material of insulating film, such as SiO can be enumerated2Deng.Transparent electrode 83 is formed in
On the insulating film of bright glass substrate 82.As the material of transparent electrode 83, ITO etc. can be enumerated.Transparent electrode 83 can for example pass through
The patterning of photoetching method is utilized to be formed.In the transparent electrode 83 on the surface of transparent glass substrate 82, it is formed with orientation
Film 84.As the material of alignment films 84, polyimides etc. can be enumerated.
Between a pair of of transparent glass substrate 82, be sealed with liquid crystal 85 it is close enter.Between a pair of of transparent glass substrate 82, match
It is equipped with multiple resin particles 1.Resin particle 1 is used as spacer used for liquid crystal display element.Between a pair of of transparent glass substrate 82
Interval is limited by multiple resin particles 1.Between the edge of a pair of of transparent glass substrate 82, it is configured with sealant 86.By close
Agent 86 is sealed, prevents liquid crystal 85 from flowing out to outside.Sealant 86 includes the only partial size resin particle 1A different from resin particle 1.?
In Fig. 2, for ease of description, it is schematically shown that resin particle 1 and resin particle 1A.
In above-mentioned liquid crystal display element, 1mm2Spacer used for liquid crystal display element configuration density be preferably 10/
mm2More than, and preferably 1000/mm2Below.When above-mentioned configuration density is 10/mm2When above, cell gap become more into
One step it is uniform.When above-mentioned configuration density is 1000/mm2When following, the contrast of liquid crystal display element is further increased.
Hereinafter, by reference implementation example and comparative example, to specifically describe the present invention.The present invention is not limited only to following implementation
Example.
(embodiment 1)
(1) preparation of resin particle A (Silicone particles A)
Solution A is prepared, by the way that (polymerization initiator, day are oily by the tert-butyl -2- ethyl peroxy caproic acid ester of 0.5 parts by weight
" the PERBUTYL O " of Co., Ltd.'s manufacture) it is dissolved in two terminal acrylic acid silicone oil (SHIN-ETSU HANTOTAI's chemical industry strain formula of 30 parts by weight
" X-22-2445 " of commercial firm's manufacture) and obtain.In addition, prepare aqueous solution B, by by the lauryl sulfate three of 0.8 parts by weight
40 weight % aqueous solution (emulsifier) of ethanolamine salt and 80 parts by weight polyvinyl alcohol (degree of polymerization: about 2000, saponification degree: 86.5
~89 moles of %, " the GOHSENOL GH-20 " of the Nippon Synthetic Chemical Industry Co., Ltd's manufacture) 5 weight % aqueous solutions are mixed in
It is obtained in the ion exchange water of 150 parts by weight.Above-mentioned solution A is added into the removable flask being configured in warm bath slot,
Then aqueous solution B is added.Then, cream is carried out using Shirasu Porous Glass (SPG) film (about 5 μm of hole average diameter)
Change.Then, temperature is risen to 85 DEG C, carries out polymerization 9 hours.By centrifuge separation, water is carried out to the particle after whole polymerizations
It washes, then carries out progressive operation, then be freeze-dried, obtain resin particle A (Silicone particles A).
(2) preparation of connecting material
Silver particles (average grain diameter 15nm), the divinylbenzene resin particle (average grain diameter of 1 parts by weight to 40 parts by weight
30 μm, CV value 5%), the toluene as solvent of the above-mentioned resin particle A of 10 parts by weight and 40 parts by weight carries out with merging
Mixing, to prepare connecting material.
(3) preparation of connection structural bodies
Prepare power semiconductor as the first connecting object component.Prepare aluminium nitride substrate as the second connecting object
Component.
Above-mentioned connecting material is coated on the second connecting object component, and makes it have about 30 μm of thickness, with shape
At connecting material layer.Then, above-mentioned first connecting object component is stacked on connecting material layer, obtains laminated body.It will obtain
Laminated body heated at 300 DEG C 10 minutes, thus the silver particles for including in connecting material layer are sintered, preparation connection knot
Structure body.
(4) preparation of liquid crystal display element
The preparation of sealant for liquid crystal dripping process:
Prepare following material.
The resin particle A (Silicone particles A) of 30 parts by weight
Bisphenol type epoxy methacrylate (heat-curable compounds, DAICEL-ALLNEX Co., Ltd. of 50 parts by weight
" KRM7985 " of manufacture)
Caprolactone modification bisphenol-a epoxy acrylate (DAICEL-ALLNEX plants of formulas of heat-curable compounds of 20 parts by weight
" EBECRYL3708 " of commercial firm's manufacture)
30 parts by weight part acrylic acid modified bisphenol E type epoxy resin (heat-curable compounds, DAICEL-ALLNEX plants
" KRM8276 " of formula commercial firm manufacture)
2,2- dimethoxy -2- phenyl acetophenone (optical free radical polymerization initiator, Japan plants of formulas of BASF of 2 parts by weight
" IRGACURE651 " of commercial firm's manufacture)
The acid dihydrazide (thermal curing agents, " MDH " of Otsuka Kagaku K.K.'s manufacture) of 10 parts by weight
The silica (filler, " the ADMAFINE SO-C2 " of the manufacture of ADMATECHS Co., Ltd.) of 20 parts by weight
3- glycidoxypropyltrimewasxysilane (silane coupling agent, the SHIN-ETSU HANTOTAI's chemical industry strain formula meeting of 2 parts by weight
" KBM-403 " of society's manufacture)
After mixing above-mentioned material, by planetary agitating device, (THINKY Co., Ltd. is manufactured
" AWATORIRENTARO ") it is stirred, it is then uniformly mixed by ceramic three roller mills, to obtain liquid crystal display
Element is with sealant (sealant).
The preparation of liquid crystal display element:
By the spacer particles of 1 parts by weight (5 μm of average grain diameter, Sekisui Chemical Co., Ltd's manufacture
" MICROPEARL SP-205 ") it is mixed with the obtained sealant of 100 parts by weight, and planetary agitating device is used, it will be spaced
Disperse in the encapsulant to object uniform particle.The obtained sealant containing spacer particle is filled into distribution syringe
In (" PSY-10E " of the manufacture of MUSASHI ENGINEERING Co., Ltd.), and carry out defoaming treatment.Hereafter, using distributor
(" SHOTMASTER300 " of the manufacture of MUSASHI ENGINEERING Co., Ltd.), is coated with the sealing containing spacer particle
Agent, and it is made to be depicted as rectangular frame on the transparent electrode substrate for be formed with ito thin film.Then, using being filled under liquid crystal drop
It sets, by the fine drop of TN liquid crystal (" JC-5001LA " of the manufacture of CHISSO Co., Ltd.), drips to the painting of transparent electrode substrate
It is furnished on the inside of the rectangle of the sealant containing spacer particle, and is coated.Using vacuum forming apparatus, in the vacuum of 5Pa
Under, be coated with sealant and TN liquid crystal transparent electrode substrate and uncoated sealant and TN liquid crystal transparent electrode substrate into
Row fitting.Then, using metal halide lamp, with 100mW/cm2Ultraviolet light irradiation be coated with the part 30 seconds of sealant,
Then it is heated 1 hour at 120 DEG C, makes sealant heat cure, to obtain liquid crystal display element (5 μm of cell gap).
(embodiment 2)
In addition to " X-22-1602 " that has used SHIN-ETSU HANTOTAI's Chemical Co., Ltd. to manufacture when preparing resin particle replaces SHIN-ETSU HANTOTAI
Except " X-22-2445 " that learns Co., Ltd.'s manufacture, resin particle B (polysiloxanes grain is made in the same manner as example 1
Sub- B).Other than resin particle A is changed to resin particle B, connecting material is made in the same manner as example 1, connects
Connect structural body and liquid crystal display element.
(embodiment 3)
(1) preparation of resin particle C (resin coats Silicone particles C)
16 of resin particle A (Silicone particles A), 0.6 parts by weight obtained in embodiment 1 by 6.5 parts by weight
The methanol investment configuration of alkyl trimethyl ammonium bromide, the distilled water of 240 parts by weight and 120 parts by weight is in warm bath slot
In the removable flask of 500ml, stirred 1 hour at 40 DEG C.Then, by the divinylbenzene of 3.0 parts by weight and 0.5 parts by weight
Styrene is added in removable flask, and temperature is risen to 75 DEG C, is stirred 0.5 hour.Then, by the 2 of 0.4 parts by weight,
2 '-azo two (isobutyric acid) dimethyl esters are added in removable flask, are stirred 8 hours, to carry out polymerization reaction.In polymerization reaction
Afterwards, by centrifuge separation, obtained particle is washed, to obtain resin particle C (resin coats Silicone particles C).
Other than resin particle A is changed to resin particle C, obtain in the same manner as example 1 connecting material,
Connection structural bodies and liquid crystal display element.
(comparative example 1)
In addition to having used polysiloxanes powder " KMP-605 " (SHIN-ETSU HANTOTAI in preparation connecting material and liquid crystal display element
Learn Industrial Co., Ltd's manufacture) it replaces except resin particle A, in the same manner as example 1, obtain connecting material, connection
Structure and liquid crystal display element.
(comparative example 2)
In addition to having used polysiloxanes powder " KMP-590 " (SHIN-ETSU HANTOTAI in preparation connecting material and liquid crystal display element
Learn Industrial Co., Ltd's manufacture) it replaces except resin particle A, in the same manner as example 1, obtain connecting material, connection
Structure and liquid crystal display element.
(evaluation)
(1) sum (TnQn) of T unit and Q unit
Pass through29Si- solid NMR analysis, in the above way calculate above-mentioned M unit, above-mentioned D unit, above-mentioned T unit and
The sum (TnQn) of above-mentioned T unit and above-mentioned Q unit in the sum 100% of above-mentioned Q unit.
(2) partial size
Using particle size distribution device (" Multisizer 4 " of the manufacture of Beckman Coulter company), measurement is about
The partial size of 100000 resin particles, and average value is calculated, the partial size of resin particle obtained from thus finding out.
(3) coefficient of variation (CV value)
It is measured by the coefficient of variation of the above method to obtained resin particle.
(4) 10%K value
It is measured by 10%K value of the above method to obtained resin particle.
(5) compression recovery when compressive deformation 40%
Compression recovery of the obtained resin particle in compressive deformation 40% is measured by the above method.
(6) bonding strength
Using MOUNT strength detection device, bonding strength of the obtained connection structural bodies at 260 DEG C is measured.
Bonding strength is determined based on following standard.
[criterion of bonding strength]
00: shear strength 150N/cm2More than
Zero: shear strength 100N/cm2More than and less than 150N/cm2
×: shear strength is less than 100N/cm2
(7) it springs back
By scanning electron microscope, whether sprung back at the interconnecting piece for the connection structural bodies observed.Based on
Lower standard determines to spring back.
[criterion of rebound]
Zero: there is no rebounds
×: it is sprung back
(8) internal stress relaxation properties
By scanning electron microscope, whether observation there is crack at the interconnecting piece of obtained connection structural bodies.It is based on
Following standard determines internal stress relaxation properties.
[judgment criterias of internal stress relaxation properties]
Zero: there is no cracks
×: crack has occurred
(9) cold cycling characteristic (connection reliability)
Obtained connection structural bodies is implemented to carry out that 150 DEG C will be heated to from -65 DEG C 1000 times, is cooled to -65 DEG C
The thermal cycling test that process is recycled as one.By ultrasonic flaw detecting device (SAT), observes and whether split in interconnecting piece
Seam and removing.Cold cycling characteristic (connection reliability) is determined based on following standard.
[judgment criteria of cold cycling characteristic (connection reliability)]
Zero: there is no crack or removings for interconnecting piece
×: crack or removing has occurred in interconnecting piece
(10) penetrability
Obtained liquid crystal display element is saved 72 hours in the environment of 80 DEG C of temperature, humidity 90%RH, is then carried out
The voltage of AC 3.5V drives, and observes by the naked eye around the sealing of semi-tone.Penetrability is determined based on following standard.
[criterion of penetrability]
Zero: there is no irregular colours around sealing
△: slight irregular colour has occurred around sealing
×: apparent irregular colour has occurred around sealing
As a result as shown in table 1 below.
[table 1]
Symbol description
1... resin particle
1A... resin particle
51... connection structural bodies
52... the first connecting object component
53... the second connecting object component
54... interconnecting piece
61...... gap controls particle
62... metallic connection parts
81... liquid crystal display element
82... transparent glass substrate
83... transparent electrode
84... alignment films
85... liquid crystal
86... sealant
Claims (12)
1. a kind of resin particle, wherein
By general formula [(R)3SiO1/2] indicate M unit, by general formula [(R)2SiO2/2] indicate D unit, by general formula [(R) SiO3/2]
The T unit of expression and by general formula [SiO4/2] indicate Q unit total number 100% in, the T unit and the Q unit
Total number be 4% or less.
2. resin particle according to claim 1, compression recovery when compressive deformation 40% is 10% or less.
3. resin particle according to claim 1 or 2,10%K value is 500N/mm2Below.
4. resin particle described in any one of claim 1 to 3, partial size is 0.5 μm or more and 500 μm or less.
5. resin particle according to any one of claims 1 to 4 is the particle comprising organic siliconresin.
6. resin particle according to any one of claims 1 to 5 is used as spacer.
7. a kind of connecting material, it includes resin particles according to any one of claims 1 to 6, also comprising adhesive or contain
There is the particle of metallic atom.
8. connecting material according to claim 7, it includes adhesives.
9. connecting material according to claim 7 or 8, it includes the particles containing metallic atom.
10. connecting material according to claim 9, wherein
The thermal decomposition temperature of the resin particle is higher than the fusing point of the particle containing metallic atom.
11. connecting material according to claim 9 or 10 is used to form the connection of two connecting object components of connection
Portion；
And the sintered body by the particle containing metallic atom is used for form the interconnecting piece.
12. a kind of connection structural bodies, has:
First connecting object component,
Second connecting object component and
The interconnecting piece that the first connecting object component and the second connecting object component are linked together, wherein
The material of the interconnecting piece includes resin particle according to any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310664640.1A CN116675819A (en) | 2017-05-01 | 2018-04-25 | Resin particle, connection material, and connection structure |
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| JP2017-091123 | 2017-05-01 | ||
| JP2017091123 | 2017-05-01 | ||
| PCT/JP2018/016745 WO2018203500A1 (en) | 2017-05-01 | 2018-04-25 | Resin particle, connecting material, and connection structure |
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| CN201880005079.3A Active CN110088160B (en) | 2017-05-01 | 2018-04-25 | Resin particle, connection material, and connection structure |
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|---|---|
| JP (1) | JP7092670B2 (en) |
| KR (1) | KR102584161B1 (en) |
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| WO2023090456A1 (en) * | 2021-11-22 | 2023-05-25 | 積水化学工業株式会社 | Adhesive particles and laminate |
| WO2023090457A1 (en) * | 2021-11-22 | 2023-05-25 | 積水化学工業株式会社 | Adhesive particles and laminate |
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|---|---|---|---|---|
| JP2009052005A (en) * | 2007-07-30 | 2009-03-12 | Sanyo Chem Ind Ltd | Method for producing resin particles |
| CN102666620A (en) * | 2009-10-23 | 2012-09-12 | 道康宁公司 | Hydrophilically-modified silicone compositions |
| CN102918087A (en) * | 2010-05-31 | 2013-02-06 | 三洋化成工业株式会社 | Resin particle and method for producing same |
| WO2016088812A1 (en) * | 2014-12-04 | 2016-06-09 | 積水化学工業株式会社 | Silicone particles, sealing agent for liquid crystal dropping methods, and liquid crystal display element |
| JP2016108563A (en) * | 2014-12-04 | 2016-06-20 | 積水化学工業株式会社 | Base material particle, conductive particle, conductive material and connection structure |
| CN107709414A (en) * | 2015-11-11 | 2018-02-16 | 积水化学工业株式会社 | Particle, particulate material, connecting material and connection structural bodies |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4860214B2 (en) | 2004-09-07 | 2012-01-25 | モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社 | Method for producing spherical silicone elastomer fine particles and cosmetics |
| JP5607001B2 (en) | 2011-08-11 | 2014-10-15 | 信越化学工業株式会社 | Silicone fine particles and method for producing the same |
| JP6165625B2 (en) * | 2012-01-20 | 2017-07-19 | 積水化学工業株式会社 | Conductive particles, conductive materials, and connection structures |
| JP2015140356A (en) | 2014-01-27 | 2015-08-03 | 大東化成工業株式会社 | Spongy silicone fine particle, manufacturing method therefor and cosmetic |
| JP6859077B2 (en) * | 2015-11-11 | 2021-04-14 | 積水化学工業株式会社 | Particle material, connecting material and connecting structure |
-
2018
- 2018-04-25 JP JP2018532346A patent/JP7092670B2/en active Active
- 2018-04-25 CN CN202310664640.1A patent/CN116675819A/en active Pending
- 2018-04-25 KR KR1020197010950A patent/KR102584161B1/en active IP Right Grant
- 2018-04-25 CN CN201880005079.3A patent/CN110088160B/en active Active
- 2018-04-25 WO PCT/JP2018/016745 patent/WO2018203500A1/en active Application Filing
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009052005A (en) * | 2007-07-30 | 2009-03-12 | Sanyo Chem Ind Ltd | Method for producing resin particles |
| CN102666620A (en) * | 2009-10-23 | 2012-09-12 | 道康宁公司 | Hydrophilically-modified silicone compositions |
| CN102918087A (en) * | 2010-05-31 | 2013-02-06 | 三洋化成工业株式会社 | Resin particle and method for producing same |
| WO2016088812A1 (en) * | 2014-12-04 | 2016-06-09 | 積水化学工業株式会社 | Silicone particles, sealing agent for liquid crystal dropping methods, and liquid crystal display element |
| JP2016108563A (en) * | 2014-12-04 | 2016-06-20 | 積水化学工業株式会社 | Base material particle, conductive particle, conductive material and connection structure |
| CN107709414A (en) * | 2015-11-11 | 2018-02-16 | 积水化学工业株式会社 | Particle, particulate material, connecting material and connection structural bodies |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110088160B (en) | 2023-06-13 |
| TW201843214A (en) | 2018-12-16 |
| KR20190139194A (en) | 2019-12-17 |
| JP7092670B2 (en) | 2022-06-28 |
| KR102584161B1 (en) | 2023-10-04 |
| WO2018203500A1 (en) | 2018-11-08 |
| JPWO2018203500A1 (en) | 2020-03-12 |
| CN116675819A (en) | 2023-09-01 |
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