JP2018076486A - 安定化アミノシラン基含有シリカ粒子の水性組成物 - Google Patents
安定化アミノシラン基含有シリカ粒子の水性組成物 Download PDFInfo
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- JP2018076486A JP2018076486A JP2017198635A JP2017198635A JP2018076486A JP 2018076486 A JP2018076486 A JP 2018076486A JP 2017198635 A JP2017198635 A JP 2017198635A JP 2017198635 A JP2017198635 A JP 2017198635A JP 2018076486 A JP2018076486 A JP 2018076486A
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- silica
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- polishing composition
- aminosilane
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 264
- 239000000203 mixture Substances 0.000 title claims abstract description 154
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 84
- 238000005498 polishing Methods 0.000 claims abstract description 66
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 38
- 239000007787 solid Substances 0.000 claims abstract description 36
- 150000001875 compounds Chemical class 0.000 claims abstract description 35
- 239000000126 substance Substances 0.000 claims abstract description 25
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 98
- 239000002245 particle Substances 0.000 claims description 85
- 229910052757 nitrogen Inorganic materials 0.000 claims description 52
- 230000032683 aging Effects 0.000 claims description 36
- 239000000872 buffer Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 150000003512 tertiary amines Chemical group 0.000 claims description 5
- -1 alkane ammonium dihydroxide Chemical class 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- 125000001302 tertiary amino group Chemical group 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 claims 1
- 238000003878 thermal aging Methods 0.000 abstract description 13
- 238000003860 storage Methods 0.000 abstract description 10
- 238000004062 sedimentation Methods 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 73
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 47
- 229910017604 nitric acid Inorganic materials 0.000 description 47
- 239000000243 solution Substances 0.000 description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 238000002296 dynamic light scattering Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002253 acid Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 239000000178 monomer Substances 0.000 description 8
- 150000003335 secondary amines Chemical group 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 7
- 238000007865 diluting Methods 0.000 description 7
- 238000009472 formulation Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 229960000583 acetic acid Drugs 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 5
- 239000000499 gel Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 230000001143 conditioned effect Effects 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 239000012212 insulator Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 3
- 238000010979 pH adjustment Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical group [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000008351 acetate buffer Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- NHBRUUFBSBSTHM-UHFFFAOYSA-N n'-[2-(3-trimethoxysilylpropylamino)ethyl]ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCNCCN NHBRUUFBSBSTHM-UHFFFAOYSA-N 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 2
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N sarcosine Chemical compound C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 description 2
- 125000005372 silanol group Chemical group 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 238000000733 zeta-potential measurement Methods 0.000 description 2
- PHIQHXFUZVPYII-ZCFIWIBFSA-O (R)-carnitinium Chemical compound C[N+](C)(C)C[C@H](O)CC(O)=O PHIQHXFUZVPYII-ZCFIWIBFSA-O 0.000 description 1
- 241000408939 Atalopedes campestris Species 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- PHIIOKFICBAPOS-UHFFFAOYSA-N NCCNCCC[SiH3] Chemical class NCCNCCC[SiH3] PHIIOKFICBAPOS-UHFFFAOYSA-N 0.000 description 1
- 108010077895 Sarcosine Proteins 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- KXHPPCXNWTUNSB-UHFFFAOYSA-N benzyl(trimethyl)azanium;hydrochloride Chemical compound Cl.C[N+](C)(C)CC1=CC=CC=C1 KXHPPCXNWTUNSB-UHFFFAOYSA-N 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 229960004203 carnitine Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- FIRQYUPQXNPTKO-UHFFFAOYSA-N ctk0i2755 Chemical class N[SiH2]N FIRQYUPQXNPTKO-UHFFFAOYSA-N 0.000 description 1
- KSFBTBXTZDJOHO-UHFFFAOYSA-N diaminosilicon Chemical compound N[Si]N KSFBTBXTZDJOHO-UHFFFAOYSA-N 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000004693 imidazolium salts Chemical group 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- UMXXGDJOCQSQBV-UHFFFAOYSA-N n-ethyl-n-(triethoxysilylmethyl)ethanamine Chemical compound CCO[Si](OCC)(OCC)CN(CC)CC UMXXGDJOCQSQBV-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000006384 oligomerization reaction Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003141 primary amines Chemical group 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 229940043230 sarcosine Drugs 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
Description
全カチオン性窒素原子=1×アミノシラン+2×ビス又はジアミノシラン+1×二つの第四級アンモニウム基を含有する化合物
式中、単位は、シリカ表面積1m2あたりカチオン性窒素原子のナノモル数である。
以下の実施例が本発明の様々な特徴を説明する。
AEAPS=N−(2−アミノエチル)−3−アミノプロピルトリメトキシシラン、98%(Gelest Inc., Morrisville, PA);
DEAMS=(N,N−ジエチルアミノメチル)トリエトキシシラン、98%(Gelest Inc.);
BMIC=塩化1−ブチル−3−メチルイミダゾリウム、98%(Sigma-Aldrich, Milwaukee, WI);
BTMAC=塩化ベンジルトリメチルアンモニウム、98%(Sigma-Aldrich)。
指示された組成物を13暦日間放置したのち、熱老化試験を開始した。結果を以下の表1に示す。
DEAMS(124nM/m2シリカ)スラリーを製造するために、脱イオン水16.8グラムをスラリーA392グラムと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMSモノマー3.7%w/wである加水分解DEAMS溶液11.2グラムを加えた。DEAMSとシリカとの30分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.0に調節した。次いで、28%w/wシリカであるDEAMS(124nM/m2シリカ)溶液のアリコットを使用して、以下の表2に示すように、加えられた重量ミリモル量の第四級アンモニウム及び/又はカルボン酸により、シリカ24%のDEAMSの溶液(124nM/m2シリカ)を調製した。得られたスラリーを、熱老化のために、必要ならば硝酸/KOHを使用して約4.1にpH調節した。
3A〜3FのDEAMS(156nM/m2シリカ)スラリーを製造するために、脱イオン水4.66グラムをスラリーA130.66グラムと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMSモノマー3.7%w/wである加水分解DEAMS溶液4.67グラムを加えた。DEAMSとシリカとの60分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.0に調節した。比較例3Aにおいて、熱老化を受けず(室温で6日間貯蔵)、余分な添加物を有しないDEAMS(156nM/m2シリカ)溶液の粒子径は、固形分1%及びpH3.5で計測して36.91nm(Z平均)であった。
28%w/wシリカでDEAMS(140nM/m2シリカ)スラリーを製造するために、脱イオン水12.83グラムをスラリーA326.66グラムと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMSモノマー3.7%w/wである加水分解DEAMS溶液10.50グラムを加えた。DEAMSとシリカとの30分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.3に調節した。実施例4A〜4Sにおけるアミノシラン基含有シリカ粒子(140nM/m2シリカ)の粒子径は、室温で30分後、余分な添加物なしで、36.51nm(Z平均、固形分1重量%及びpH3.5で実施)であった。次いで、DEAMS(140nM/m2シリカ)溶液のアリコットを使用して、以下の表4A及び4Bに示すように、加えられた重量ミリモル量の第四級アンモニウム及び/又は酢酸により、アミノシラン基含有シリカ粒子固形分24重量%の溶液を調製した。得られたスラリーを、熱老化のために、必要ならば硝酸/KOHを使用して4.2〜4.3にpH調節し、50℃で6日間老化させた。
実施例5AのDEAMS(181nM/m2シリカ)スラリーを製造するために、脱イオン水1166.63グラムをスラリーA5599.94グラムと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMSモノマー3.7%w/wである加水分解DEAMS溶液233.43グラムを加えた。DEAMSとシリカとの180分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.1に調節した。実施例5BのDEAMS(181nM/m2シリカ)の場合、同じ手順を使用したが、180分後、HBBAH(硝酸塩形態)を加えてHBBAH中0.7mmのスラリーを製造した。実施例5CのDEAMS(181nM/m2シリカ)の場合、同じ手順を使用したが、180分後、モノアセテート/モノニトレート形態のHBBAHを加えてHBBAH中0.7mmのスラリー及びアセテート中0.7mmのスラリーを製造した。45℃での熱老化の結果を以下の表5Aに示す。粒子径計測は、スラリー濃縮物を水で固形分1%の溶液に希釈することによって実施した。
実施例6A〜6JにおけるDEAMS(199nM/m2シリカ)スラリーの場合:脱イオン水32.66グラムをスラリーA160グラムと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMS3.7%w/wである加水分解DEAMS溶液7.34グラムを加えた。DEAMSとスラリーAのシリカとの10分間及び60分間の反応それぞれののち、KOH及び/又は硝酸を使用してpHを4.2に調節した。18時間後、硝酸を使用して粒子をpH3.5に調節し、7日間貯蔵した。
AEAPS(43.5nM/m2シリカ)スラリーの場合:脱イオン水18.81グラムをスラリーA80グラムと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したAEAPSモノマー2.22%w/wである加水分解AEAPS溶液1.19グラムを加えた。AEAPSとシリカとの10分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.2に調節し、室温で貯蔵した。翌日、粒子を使用して老化調合物を製造した。
試薬の量が表8Aに掲載されている。脱イオン水をスラリーAと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMSモノマー3.7%w/wである加水分解DEAMS溶液を加えた。DEAMSとシリカとの30分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.2に再調節した。次いで、4.25にpH調節したスラリーB又はそのままのスラリーCの10%w/w溶液を任意選択で加えた。任意選択で、DEAMS溶液の二回目の添加を実施した。さらに30分後、ビス酢酸HBBAH(pH4.4の原液から)を加え、pHを4.4に再調節した。最終溶液を対流オーブン中50℃で28日間熱老化させた。
混合した後の水性シリカスラリー調合物が以下の表9Aに掲載されている。脱イオン水をスラリーAと混合した。硝酸を使用して溶液のpHを4.25に低下させた。この混合物に、硝酸を使用してpH4.25に調節したDEAMSモノマー3.7%w/wである加水分解DEAMS溶液を加えた。DEAMSとシリカとの30分間の反応ののち、KOH及び/又は硝酸を使用してpHを4.2に再調節した。次いで、以下の表9Aに示すように、4.25にpH調節したスラリーB又はそのままのスラリーCの24%w/w溶液を加えた。任意選択で、二回目のDEAMS溶液の添加を実施した。さらに30分後、ビス酢酸HBBAH(pH4.4の原液から)を加え、pHを硝酸によって以下の表9Aに掲載されるように調節した。最終溶液を対流オーブン中45℃で28日間熱老化させた。
Claims (10)
- 二つの第四級アンモニウム基を含有する化合物と、組成物の全重量に基づいて固形分として1〜30重量%の量の、一つ以上のカチオン性窒素原子を含有するアミノシラン基含有シリカ粒子との混合物を含む、3〜5の範囲のpHを有する水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物であって、前記シリカ粒子上のアミノシラン及び前記二つの第四級アンモニウム基を含有する化合物からのカチオン性窒素原子の全量が、水性CMP研磨組成物中のシリカ粒子1m2あたり170〜500nMの範囲であり、さらに、45℃の温度で少なくとも6日間の熱老化ののち、固形分15重量%で目に見える沈殿又は沈降に対して安定である、水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 前記二つの第四級アンモニウム基を含有する化合物が、ヘキサブチルC1〜C8アルカンジアンモニウム二水酸化物又はその塩から選択される、請求項1記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 前記二つの第四級アンモニウム基を含有する化合物がN,N,N,N′,N′,N′−ヘキサブチル−1,4−ブタンジアンモニウム二水酸化物(HBBAH)である、請求項2記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 前記アミノシラン基含有シリカ粒子が、一つ以上の第三級アミン基又は一つ以上の第二級アミン基を含有するアミノシラン類を含む、請求項1記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 前記アミノシラン基含有シリカ粒子が、N,N−(ジエチルアミノメチル)トリエトキシシラン(DEAMS)である、一つ以上の第三級アミノ基を含有するアミノシラン類を含む、請求項4記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- シリカ粒子表面積1平方メートルあたりの前記シリカ粒子上のカチオン性窒素原子のナノモル数(nM/m2シリカ)単位のアミノシランの量が、水性CMP研磨組成物中、70〜500nM/m2シリカの範囲である、請求項1記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- アミノシランの量が100〜300nM/m2シリカの範囲である、請求項6記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 前記二つの第四級アンモニウム基を含有する化合物の量が、水性CMP研磨組成物中、シリカ粒子1m2あたり、二つの第四級アンモニウム基を含有する化合物18〜100nM(nM/m2シリカ)の範囲である、請求項1記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 3〜7の(ジ)カルボン酸pKaのカルボン酸塩である緩衝液を全組成物1kgあたり0〜50ミリモルの量でさらに含む、請求項1記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
- 前記組成物が、アミノシラン基含有シリカ粒子を、組成物の全重量に基づいて固形分として15〜22重量%の量で含む、請求項1記載の水性ケミカルメカニカルプラナリゼーション(CMP)研磨組成物。
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