KR100558259B1 - Slurry Composition for Silicon Wafer Mirror Polishing - Google Patents
Slurry Composition for Silicon Wafer Mirror Polishing Download PDFInfo
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- KR100558259B1 KR100558259B1 KR1020030084065A KR20030084065A KR100558259B1 KR 100558259 B1 KR100558259 B1 KR 100558259B1 KR 1020030084065 A KR1020030084065 A KR 1020030084065A KR 20030084065 A KR20030084065 A KR 20030084065A KR 100558259 B1 KR100558259 B1 KR 100558259B1
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- polypyrrolidone
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- 238000005498 polishing Methods 0.000 title claims abstract description 77
- 239000002002 slurry Substances 0.000 title claims abstract description 43
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 15
- 239000010703 silicon Substances 0.000 title claims abstract description 15
- 239000000203 mixture Substances 0.000 title description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 20
- 229920001007 Nylon 4 Polymers 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000008119 colloidal silica Substances 0.000 claims abstract description 12
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 8
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 8
- 235000012431 wafers Nutrition 0.000 claims description 27
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000011163 secondary particle Substances 0.000 claims description 6
- 239000011164 primary particle Substances 0.000 claims description 5
- KNHNLCHRGUQAAO-UHFFFAOYSA-M tetramethoxyazanium;hydroxide Chemical compound [OH-].CO[N+](OC)(OC)OC KNHNLCHRGUQAAO-UHFFFAOYSA-M 0.000 claims description 4
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Substances [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 abstract description 20
- 239000000377 silicon dioxide Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 5
- 238000007517 polishing process Methods 0.000 abstract description 2
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 abstract 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 229920003169 water-soluble polymer Polymers 0.000 description 6
- -1 NO 3 Inorganic materials 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000001856 Ethyl cellulose Substances 0.000 description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 229920001249 ethyl cellulose Polymers 0.000 description 3
- 235000019325 ethyl cellulose Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- DSTUCEHQQBNLHQ-UHFFFAOYSA-N trimethyl-(2-methylprop-2-enoylamino)azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)N[N+](C)(C)C DSTUCEHQQBNLHQ-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000001253 polyvinylpolypyrrolidone Substances 0.000 description 2
- 235000013809 polyvinylpolypyrrolidone Nutrition 0.000 description 2
- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 description 2
- 125000001453 quaternary ammonium group Chemical class 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- XXMBEHIWODXDTR-UHFFFAOYSA-N 1,2-diaminoethanol Chemical compound NCC(N)O XXMBEHIWODXDTR-UHFFFAOYSA-N 0.000 description 1
- 229910020366 ClO 4 Inorganic materials 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical group [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007518 final polishing process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
Classifications
-
- 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
-
- 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
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02024—Mirror polishing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
본 발명은 실리콘 웨이퍼 연마용 슬러리 및 이를 이용한 경면연마 방법에 관한 것으로, 보다 상세하게는 평균 입경이 10-200nm인 콜로이드 실리카, 아크릴레이트 또는 암모늄염과 공중합된 폴리피롤리돈 공중합체, TMAH, pH 조절제 및 탈이온수를 포함하는 실리콘 웨이퍼 연마용 슬러리 및 상기 연마용 슬러리를 2차 연마 단계에서 사용하는 것을 특징으로 하는 다단계 경면연마 방법에 관한 것이다. 본 발명에 따른 연마용 슬러리를 사용하여 경면연마 공정을 수행하면 미크론 단위 이하의 LPD(submicron LPD)가 크게 감소되는 효과를 제공할 수 있다.The present invention relates to a slurry for polishing a silicon wafer and a mirror polishing method using the same, and more particularly, a polypyrrolidone copolymer copolymerized with colloidal silica, acrylate or ammonium salt having an average particle diameter of 10-200 nm, TMAH, pH adjuster and The present invention relates to a slurry for polishing a silicon wafer containing ionic water and a method for polishing a mirror in multiple stages, wherein the polishing slurry is used in a secondary polishing step. Performing a mirror polishing process using the polishing slurry according to the present invention can provide an effect of greatly reducing submicron LPD (LPD) of less than a micron unit.
실리콘 웨이퍼, 경면연마, 실리카. 폴리피롤리돈 공중합체, TMAH, pH조절제 Silicon wafer, mirror polishing, silica. Polypyrrolidone copolymer, TMAH, pH adjuster
Description
본 발명은 실리콘 웨이퍼 연마용 슬러리에 관한 것으로, 보다 상세하게는 평균 입경이 10-200nm인 콜로이드 실리카, 아크릴레이트 또는 암모늄염과 공중합된 폴리피롤리돈 공중합체, TMAH, pH조절제 및 탈이온수를 포함하는 미크론 단위 이하의 LPD가 크게 감소된 실리콘 웨이퍼 연마용 슬러리 및 이를 이용한 경면연마 방법에 관한 것이다.The present invention relates to a slurry for polishing a silicon wafer, and more particularly, to a micron unit including polypyrrolidone copolymer copolymerized with colloidal silica, acrylate or ammonium salt having an average particle diameter of 10-200 nm, TMAH, pH adjusting agent and deionized water. The present invention relates to a slurry for polishing a silicon wafer, and a mirror polishing method using the same.
반도체 제조시 기판이 되는 실리콘 웨이퍼는 단결정성장(single crystal growing), 절단(slicing), 연마(lapping), 식각(etching), 경면연마(polishing), 세정 (cleaning) 등의 여러 공정을 거쳐 제조된다. 제조공정의 최종 단계인 경면연마 공정은 이전 공정에서 생성된 표면이나 표면 이하(subsurface)의 결함 즉 긁힘, 갈라짐, 결정 디스토션(grain distortion), 표면 거칠기 또는 표면의 지형 (topography)의 결함을 제거하여 무결점 거울면의 웨이퍼로 가공하게 된다. 실리콘 웨이퍼의 제조 공정에서 마지막 공정인 CMP 공정은 웨이퍼 표면의 마이크로스크래 치(Microscratch)등의 물리적 표면 결함을 제거하고 미세 거칠음(Microroughness)을 낮추어 부드러운 표면을 만드는 단계이다. 이러한 CMP 공정을 거친 웨이퍼는 비로소 저표면 결함의 경면을 구현하는 것이다. 웨이퍼 표면에 잔류하는 마이크로디펙트(microdefect)는 회로를 구현하는 포토리소그래피(photolithography) 공정의 문제를 일으키는 원인을 제공하는 결함으로서 CMP 공정에서 마이크로디펙트를 제거하는 것은 중요한 과제이다.Silicon wafers that serve as substrates in semiconductor manufacturing are manufactured through various processes such as single crystal growing, slicing, lapping, etching, polishing, and cleaning. . Mirror polishing, the final stage of the manufacturing process, eliminates surface or subsurface defects created by previous processes, such as scratches, cracks, grain distortions, surface roughness or surface topography. It is processed into a wafer of flawless mirror surface. The final CMP process in the silicon wafer manufacturing process is to remove physical surface defects such as microscratch on the wafer surface and to reduce the microroughness to make the smooth surface. Wafers that have undergone this CMP process are capable of producing mirror surfaces of low surface defects. Microdefects remaining on the wafer surface are defects that cause problems in the photolithography process that implements the circuit, and it is an important task to remove microfects in the CMP process.
웨이퍼의 CMP 공정은 다단계를 거치는데 표면의 딥 스크래치(deep scratch)를 제거하기 위하여 빠른 연마속도를 요하는 1차 연마단계와 여전히 잔류하는 마이크로스크래치를 제거하고 표면의 미세 거칠음를 낮추어(수Å 수준) 경면을 구현하는 2차 연마 단계로 구성된다. 이러한 연마 가공에는 연마기(polisher)와 탈이온수 (deionized water) 이외에 연질 혹은 경질의 우레탄 연마포와 연마액인 실리카 슬러리이다. 웨이퍼 표면의 연마는 화학적 기계적 연마(Chemical Mechanical Polishing)의 반응으로 설명하는데, 연마포는 기계적 연마의 역할을 하고, 연마액은 패드(pad)의 기계적 연마를 보조하고 또한 화학적인 연마를 일으키는 역할을 하는 것이다. 웨이퍼의 대구경화와 이에 따른 고도의 품질요구는 연마포와 슬러리의 성능 향상의 원인이 되고 있다. 특히 대구경 300mm 웨이퍼의 가공 특성상 높은 수준의 무결점 표면을 구현하기 위한 슬러리의 개발이 중요시되고 있다.The wafer CMP process is a multi-step process, which requires a first polishing step that requires a fast polishing speed to remove deep scratches on the surface, removes residual microscratches and lowers the surface microscopic roughness (several levels). It is composed of a second polishing step to implement a mirror surface. Such polishing is a soft or hard urethane polishing cloth and a silica slurry in addition to a polisher and deionized water. Polishing of the wafer surface is explained by the reaction of Chemical Mechanical Polishing. The polishing cloth serves as mechanical polishing, and the polishing liquid assists in mechanical polishing of the pad and also causes chemical polishing. It is. The large diameter of the wafer and the high quality requirements are contributing to the improvement of the performance of the polishing cloth and the slurry. In particular, the development of a slurry to realize a high level of defect-free surface due to the processing characteristics of large diameter 300mm wafer is important.
상기 슬러리는 연마제(Abrasive), pH 조절제인 염기 및 탈이온수(deionized water)를 일반적으로 포함하고 특수한 연마품질을 발휘시키기 위하여 유기 혹은 무기 첨가제를 첨가하기도 한다. CMP 공정별로 공정 특성에 부합하는 별도의 슬러리 를 사용하는 것이 보편화되어 있는데, 연마제는 주로 실리카가 사용되고, pH 조절제로는 수산화칼륨이나 수산화나트륨을 사용하거나 암모니아수를 사용하는 것이 일반적이다. 이러한 성분에 부가적으로 첨가물을 사용하는데 연마속도를 향상하거나 연마표면의 세정도를 향상시키고 연마제의 분산성을 증진하는 비이온성 계면활성제, 아민류의 연마속도 촉진제등이 그것이다.The slurry generally includes an abrasive, a pH adjuster base and deionized water, and may be added with an organic or inorganic additive to achieve a special polishing quality. It is common to use a separate slurry that meets the process characteristics for each CMP process. Silica is mainly used as an abrasive, and potassium hydroxide, sodium hydroxide, or ammonia water is generally used as a pH adjusting agent. In addition to these components, additives are used, such as nonionic surfactants and amines for improving the polishing rate, improving the cleanliness of the polishing surface, and improving the dispersibility of the abrasive.
트레닉(Trednnick) 등은 미국특허 US3715842(1973) 에서 100nm이하의 실리카 입자를 물에 분산시키고, 여기에 암모니아를 0.05퍼센트 이상으로 첨가하여 pH를 7 이상으로 한 후 여기에 수산화메틸셀룰로오스(HMC), 수산화에틸셀룰로오스(HEC), 수산화프로필셀룰로오스(HPC)를 0.05～2.5 무게 퍼센트가 되도록 첨가하여 최종연마용 슬러리를 제조하였는데 실리카의 침전을 억제하여 스크레치를 감소시키고자 하였다. Trennnick et al., In US Patent US3715842 (1973), disperses silica particles of 100 nm or less in water, adds ammonia to 0.05% or more to bring the pH to 7 or more, and adds methyl cellulose (HMC). Ethyl cellulose hydroxide (HEC) and propyl cellulose hydroxide (HPC) were added to 0.05 to 2.5 weight percent to prepare a slurry for final polishing. To reduce scratches by inhibiting silica precipitation.
페인(Payne)등은 미국특허(US4169337-1979, US4462188-1984, US4588421-1986)에서 4-100nm 크기의 입자를 사용하고 아미노에탄올아민(aminoethanolamine) 또는 에틸렌디아민(ethylenediamine)등의 아민을 2 또는 4 퍼센트로 첨가하거나 테트라메틸암모늄 클로라이드(tetramethylammonium chloride) 혹은 수산화사메틸암모늄(TMAH)등의 사급암모늄염을 2% 또는 4%로 첨가한 조성물로써 연마속도를 개선하고자 하였다.Payne et al. Use 4-100 nm size particles in US patents (US4169337-1979, US4462188-1984, US4588421-1986) and use 2 or 4 amines such as aminoethanolamine or ethylenediamine. In order to improve the polishing rate, the composition was added in percent or tetramethylammonium chloride or quaternary ammonium salt such as tetramethylammonium hydroxide (TMAH) at 2% or 4%.
사사키(Sasaki)등은 미국특허 US5352277(1994)에서 콜로이달 실리카, 수용성 고분자, 수용성 염을 사용한 슬러리를 제안하였다. 실리카는 5-500nm인 것을 20-50 퍼센트가 되도록 하였으며, 수용성 고분자의 양은 약 100ppm, 염은 양이온이 Na, K, NH4인 것 중에서, 음이온이 Cl, F, NO3, ClO4인 것 중에서 선택하였으며, 농도는 20-100ppm이 되도록 하였다. 이러한 슬러리를 사용하여 표면 거칠기를 5nm 미만으로 감소시킨 고운(soft)표면을 구현시켰다.Sasaki et al. Proposed a slurry using colloidal silica, a water-soluble polymer, and a water-soluble salt in US Pat. No. 5,535,277 (1994). Silica is 5-500nm 20-50 percent, the amount of water-soluble polymer is about 100ppm, the salt is cation of Na, K, NH 4 , the anion of Cl, F, NO 3 , ClO 4 The concentration was 20-100 ppm. This slurry was used to produce a soft surface with reduced surface roughness below 5 nm.
마사토키 등은 미국특허 US0003672A1(2001) 에서 2차 혹은 최종의 연마 조성물을 제시하였다. 조성물의 연마제는 20~300nm인 실리카를 사용하였고 염기로는 TMAH를 0.001~0.3 무게 퍼센트로 사용하였다. 분자량 130만 이상인 수산화에틸셀룰로오스(HEC)를 첨가하여 연마 후 웨이퍼 표면의 친수성을 개선한 것을 언급하였는데 일반적인 연마용 슬러리의 조성에서 벗어나지 못하였다.Masatoki et al. Proposed a secondary or final polishing composition in US Pat. No. US0003672A1 (2001). The abrasive used in the composition was 20 to 300 nm of silica and TMAH was used as the base at 0.001 to 0.3 weight percent. It was mentioned to improve the hydrophilicity of the wafer surface after polishing by adding ethyl cellulose hydroxide (HEC) having a molecular weight of 1.3 million or more, but did not deviate from the composition of the general polishing slurry.
미야시타 등은 미국특허 US6354913B1(2002)에서 수용성 셀룰로오스 특히 수산화에틸셀룰로오스(HEC)를 사용하고 암모니아로 pH를 조절하고 연마속도 촉진제로 아민 특히 트리에탄올 아민을 사용한 단결정 실리콘 혹은 다결정 실리콘 표면 연마용 슬러리 조성물을 제시하였다. 특이한 것은 조성물이 금속함량을 낮추기 위하여 주 오염원인 셀룰로오스를 이온 교환법으로 정제하여 사용하는 것을 부가하였다. 그러나 연마 조성상에서는 일반적인 수준을 벗어나지 못하였고, 특히 연마속도 이외의 핵심 품질인 LPD, HAZE, 미세 거칠음 등의 향상 성능은 제시하지 못하였다. Miyashita et al., In US Patent US6354913B1 (2002), discloses a slurry composition for monocrystalline silicon or polycrystalline silicon surface polishing using water-soluble cellulose, in particular ethyl cellulose (HEC), pH adjustment with ammonia and amine, in particular triethanol amine, as polishing rate promoter. Presented. Of particular note was that the composition used to purify cellulose, the main contaminant, by ion exchange to reduce metal content. However, the polishing composition did not deviate from the general level, and in particular, improvement performances such as LPD, HAZE, and fine roughness, which are core quality other than polishing rate, were not presented.
상기 예에서 보듯이 실리콘 웨이퍼 연마용 슬러리는 콜로이드 실리카 암모니아수 그리고 표면 친수성 개선제로 수용성 고분자류로 구성되는 것이 일반적이다. 최근에 Haze나 LPD는 물론 미세 거칠음의 표면 지형 측면을 고려한 슬러리가 요구되고 있다. 특히 반도체 회로선폭이 작아지고 웨이퍼 대국경화가 진전됨에 따라 0.1미크론 이하의 LPD의 발생량을 줄이고 나노 토포그래피(Nano Topography) 범위의 미세 거칠음 수준을 5Å수준으로 구현하는 슬러리 조성물의 개발이 이루어지고 있다. As shown in the above example, the silicon wafer polishing slurry is generally composed of water-soluble polymers as colloidal silica ammonia water and surface hydrophilicity improving agent. Recently, a slurry considering the surface topography of fine roughness as well as Haze and LPD has been required. In particular, as the semiconductor circuit line width is reduced and wafer hardening is advanced, a slurry composition for reducing the generation of LPD of 0.1 micron or less and achieving a fine roughness level in the nanotopography range to 5 kW is being developed.
본 발명의 목적은 상기와 같은 종래기술의 문제점을 해결하기 위한 것으로 평균 입경이 10-200nm인 콜로이드 실리카, 아크릴레이트 또는 암모늄염과 공중합된폴리피롤리돈 공중합체, TMAH, pH 조절제, 및 탈이온수를 혼용함으로써 연마재 실리카 크기인 0.1미크론 이하의 LPD를 효과적으로 제거하고 표면의 나노 토포그래피(Nano Topography), 즉 100× 100미크론 범위의 미세 거칠음 수준을 1.0Å 수준으로 구현하는 고성능 웨이퍼 연마용 슬러리 조성물을 제공하는 것이다. An object of the present invention is to solve the problems of the prior art by mixing a polypyrrolidone copolymer copolymerized with colloidal silica, acrylate or ammonium salt having an average particle diameter of 10-200nm, TMAH, pH adjuster, and deionized water It is to provide a high performance wafer polishing slurry composition that effectively removes the silica silica size of 0.1 microns or less LPD and realizes the nano topography of the surface, that is, the micro roughness level in the range of 100 x 100 microns to 1.0 micron. .
본 발명의 다른 목적은 상기 연마용 슬러리를 사용하는 방법을 최적화하여 미크론 단위 이하의 LPD가 크게 감소시킨 경면연마 방법을 제공하는 것이다. Another object of the present invention is to provide a mirror polishing method in which LPD of less than a micron unit is greatly reduced by optimizing the method of using the polishing slurry.
즉, 본 발명은 실리콘 웨이퍼 연마용 슬러리 및 이를 이용한 경면연마 방법에 관한 것으로, 보다 상세하게는 평균 입경이 10-200nm인 콜로이드 실리카, 폴리피롤리돈 공중합체, TMAH, pH 조절제 및 탈이온수를 포함하는 실리콘 웨이퍼 연마용 슬러리 및 상기 연마용 슬러리를 최종 연마 단계에서 사용하는 것을 특징으로 하는 경면연마 방법을 제공한다.That is, the present invention relates to a slurry for polishing a silicon wafer and a mirror polishing method using the same, and more particularly, a silicon including colloidal silica, a polypyrrolidone copolymer, TMAH, a pH adjuster, and deionized water having an average particle diameter of 10-200 nm. Provided is a mirror polishing method, wherein the polishing slurry and the polishing slurry are used in the final polishing step.
본 발명은 최종 연마 슬러리의 조성에 관한 것으로, 보다 상세하게는 평균 입경이 10-200nm인 콜로이드 실리카, 아크릴레이트 또는 암모늄염과 공중합된 폴리피롤리돈 공중합체, TMAH, pH조절제 및 탈이온수를 포함하는데, 이하 본 발명의 연마용 조성물의 각 구성성분을 더욱 상세하게 설명한다.The present invention relates to the composition of the final polishing slurry, and more particularly includes a polypyrrolidone copolymer copolymerized with colloidal silica, acrylate or ammonium salt having an average particle diameter of 10-200nm, TMAH, pH adjuster and deionized water. Each component of the polishing composition of the present invention will be described in more detail.
상기 실리카의 함량은 전체 슬러리에 대하여 0.2~ 10중량%, 바람직하게는 4~6중량%이며, 상기 범위를 벗어나면 본 발명의 목적을 달성할 수 없다. 이러한 저농도화는, 2차 입경이 커지는 효과로 연마속도가 증가하였기 때문에 최종 연마공정에 적절한 연마속도(0.5~1㎛/분)로 조절하기 위한 결과이다. 더욱이 실리카의 저농도화로 분산 안정성(저장 안정성)이 증가하는 효과를 얻을 수 있었는데 이러한 분산안정화로 슬러리내 거대 입자 불순물의 생성이 억제되어 미크론 단위 이하의 LPD, 즉 0.065~0.12미크론의 LPD가 감소하는 연마품질을 얻을 수 있다. 실리카 연마제는 기계연마의 효과를 낮추기 위하여 평균 크기가 10~200㎚인, 바람직하게는 20~120nm인, 더욱 바람직하게는 30~80nm 콜로이드 실리카를 사용한다. 입경이 10nm보다 작은 경우는 기계적 연마효과가 작고 연마 중 연마제거물(실록산치환체류)에 대하여 불안정화 될 수 있어 바람직하지 않다. 연마 제거물에 대하여 입자가 불안정화하는 경우는 웨이퍼표면상에 LPD(Light Point Defect)가 잔류하게 되어 웨이퍼품질저하의 원인이 되기도 한다. 반면에 200nm이상의 입자를 사용하는 경우는 연마속도가 크나 표면 혹은 표면이하(sub surface)에 손상을 주기 때문에 최종 연마 슬 러리에는 적당하지 않다. 특히, 1차 입경이 30~50nm이고 2차 입경이 60~80nm인 경우에는 우수한 연마품질 결과를 얻는다. 이때 응집비율(agglomerate ratio), 즉 1차 입자에 대한 2차 입자의 비율은 1.6 ~ 1.8인 경우에 앞의 결과를 얻을 수 있다. The content of the silica is 0.2 to 10% by weight, preferably 4 to 6% by weight based on the total slurry, the object of the present invention can not be achieved outside the above range. This low concentration is a result for controlling the polishing rate (0.5 to 1 탆 / min) suitable for the final polishing process because the polishing rate was increased due to the effect of the secondary particle size being increased. In addition, low concentrations of silica resulted in an increase in dispersion stability (storage stability). Such dispersion stabilization inhibits the generation of large particle impurities in the slurry, thereby reducing the LPD below the micron unit, i.e., the LPD of 0.065 to 0.12 microns. Quality can be obtained. Silica abrasives use colloidal silica having an average size of 10-200 nm, preferably 20-120 nm, more preferably 30-80 nm, in order to lower the effect of mechanical polishing. If the particle diameter is smaller than 10 nm, the mechanical polishing effect is small and may be unstable with respect to the abrasive removal product (siloxane substitution) during polishing. When the particles are destabilized with respect to the abrasive removal product, LPD (Light Point Defect) remains on the wafer surface, which may cause a decrease in wafer quality. On the other hand, when particles larger than 200 nm are used, the polishing rate is high but it is not suitable for the final polishing slurry because it damages the surface or sub-surface. In particular, when the primary particle size is 30 to 50 nm and the secondary particle size is 60 to 80 nm, excellent polishing quality results are obtained. At this time, when the agglomeration ratio (agglomerate ratio), that is, the ratio of the secondary particles to the primary particles is 1.6 to 1.8 can obtain the previous results.
상기 아크릴레이트 또는 암모늄염과 공중합된 폴리피롤리돈 공중합체는 입자의 분산안정성을 증진하고 슬러리의 점도를 조절하며 웨이퍼 표면의 친수화를 유도하기 위해 사용된다. 상기 아크릴레이트와 공중합된 폴리피롤리돈 공중합체는 폴리비닐피롤리돈/디메틸아미노 에틸메틸 메타크리레이트 (Polyvinylpolypyrrolidone/ Dimethylaminoethylmethacrylate)이고, 상기 암모늄염과 공중합된 폴리비닐피롤리돈/메타크릴아미도트리메틸암모니움 클로라이드(Polyvinylpolypyrrolidone/ Methacrylamidotrimethylammonium chloride)의 공중합체이다. 사급암모늄염이 치환된 폴리비닐피롤리돈 공중합체는 무게 평균분자량이 10만인 것을 사용하며 이 경우 점도가 30~50cP가 되도록 무게중량비가 0.2~0.5중량%가 되도록 하는 것이 바람직하며 이 때 0.065~0.12미크론의 LPD 감소화가 우수하다. 특히 사급암모늄염이 치환된 폴리비닐피롤리돈은 실리카 분산제의 기능 이외에 암모늄 치환기가 실록산 (silicic acid)류의 활성연마 제거물이 실리카나 수용성 고분자의 안정화를 저하시키지 못하도록 실록산류를 안정화시키는 작용을 하는데 이는 암모늄 치환기가 음전하를 나타내는 웨이퍼 표면에 이온결합을 하여 친수화를 효과적으로 유도하는 특성에 의한 것이다.The polypyrrolidone copolymer copolymerized with the acrylate or ammonium salt is used to enhance the dispersion stability of the particles, control the viscosity of the slurry and induce hydrophilization of the wafer surface. The polypyrrolidone copolymer copolymerized with the acrylate is polyvinylpyrrolidone / dimethylamino ethylmethyl methacrylate (Polyvinylpolypyrrolidone / Dimethylaminoethylmethacrylate) and polyvinylpyrrolidone / methacrylamidotrimethylammonium chloride copolymerized with the ammonium salt (Polyvinylpolypyrrolidone / Methacrylamidotrimethylammonium chloride). The quaternary ammonium salt-substituted polyvinylpyrrolidone copolymer has a weight average molecular weight of 100,000, and in this case, the weight ratio is preferably 0.2 to 0.5% by weight so that the viscosity is 30 to 50 cP. Micron LPD reduction is excellent. In particular, the quaternary ammonium salt-substituted polyvinylpyrrolidone acts to stabilize the siloxanes so that the ammonium substituent does not reduce the stabilization of silica or water-soluble polymers by the ammonium substituent in addition to the function of the silica dispersant. This is due to the property that the ammonium substituents ionically bond to the wafer surface that exhibits a negative charge, effectively inducing hydrophilization.
연마 속도의 개선을 위해 상기 유기염기로 테트라메톡시암모늄히드록사이드 (TMAH)를 첨가한다. 전체 슬러리 조성물 대비 0.05~0.5중량%가 바람직하며 이 범위를 벗어나는 경우 연마속도는 감소하고 분산안정성이 저하되는 효과가 나타난다.Tetramethoxyammonium hydroxide (TMAH) is added to the organic base to improve the polishing rate. 0.05 to 0.5% by weight relative to the total slurry composition is preferred, if out of this range, the polishing rate is reduced and the dispersion stability is reduced.
상기 pH 조절제는 실리카의 화학적 분산성을 배가하고 CMP에서 화학적 연마효과를 부가하기 위하여 사용하는데, 약염기인 암모니아가 바람직하며 전체 슬러리 조성물 대비 0.5 ~ 3중량%를 사용하여 pH가 10.4~10.7이 되도록 한다.The pH adjusting agent is used to double the chemical dispersibility of silica and add chemical polishing effect in CMP. Ammonia, which is a weak base, is preferably used, and the pH is adjusted to 10.4 to 10.7 by using 0.5 to 3% by weight of the total slurry composition. .
이하 실시예에서 본 발명을 구체적으로 설명하고자 한다. 그러나 다음의 예가 본 발명의 범위를 한정하는 것은 아니다.Hereinafter, the present invention will be described in detail. However, the following examples do not limit the scope of the present invention.
실시예 1-2 및 비교예 1-3Example 1-2 and Comparative Example 1-3
1차 입경이 35~45nm이고 2차 입경이 65~80nm인 콜로이달 실리카를 탈이온수로 희석하여 입자함량이 전체 슬러리 조성물의 4중량%가 되도록 하였고, pH가 10.3~10.5가 되도록 암모니아를 전체 슬러리 조성물의 1중량%가 되도록 첨가하였으며 테트라메톡시암모늄히드록사이드(TMAH)를 전체 슬러리 조성물의 0.08중량%로 사용하여 pH 가 10.5~10.6 이 되도록 하였다. 실시예 1-2에서는 하기 표 1과 같은 폴리피롤리돈 공중합체를 각각 사용하여 점도가 30~50cP가 되도록 하였고, 비교예 1-3에서는 폴리피롤리돈 공중합체 대신에 표 1과 같은 친수성 증점제인 수용성 고분자로 PVA(polyvinylalcohol), PVP(polyvinylpyrrolidone), HEC (hdroxyethylcellulose)를 사용하여 점도가 30~50cP가 되도록 하여 슬러리의 조합 을 완성하였다. The colloidal silica having a primary particle size of 35 to 45 nm and a secondary particle size of 65 to 80 nm was diluted with deionized water so that the particle content was 4% by weight of the entire slurry composition, and the ammonia was entirely slurry so that the pH was 10.3 to 10.5. 1 wt% of the composition was added and the pH was 10.5-10.6 using tetramethoxyammonium hydroxide (TMAH) as 0.08 wt% of the total slurry composition. In Example 1-2, each of the polypyrrolidone copolymers shown in Table 1 was used to have a viscosity of 30 to 50 cP. In Comparative Example 1-3, instead of the polypyrrolidone copolymer, a water-soluble polymer as a hydrophilic thickener such as Table 1 was used. PVA (polyvinylalcohol), PVP (polyvinylpyrrolidone), HEC (hdroxyethylcellulose) using a viscosity of 30 ~ 50 cP to complete the slurry combination.
이와 같이 제조한 슬러리를 탈이온수로 10배 희석하여 2차와 최종 연마에 사용하였고, 100배향의 p형(p-type) 200mm 플랫(flat) 웨이퍼를 경질의 우레탄 연마포가 부착된 Speedfam Multihead 연마기로 연마하였다. STRASBAUGH Doublehead에서 8인치 웨이퍼에 대한 연마품질을 비교하였다. 연마표면은 KLA-TENCOR 사의 SURFSCAN SP-1으로 분석하였는데, 연마 품질중 특히 0.065~0.12미크론 LPD항목을 평가하였고 미세 거칠음(Microroughness)은 5000×5000미크론의 웨이비니스 (Waveness) 범위를 스캐닝하여 100×100미크론 단위로 필터하여 지형 특성을 평가하였다.The slurry thus prepared was diluted 10 times with deionized water and used for secondary polishing and final polishing. A 100-direction p-type 200mm flat wafer was used for a Speedfam Multihead grinder with a hard urethane polishing cloth. Polished by Abrasive qualities of 8 inch wafers were compared in STRASBAUGH Doublehead. The polishing surface was analyzed by SURFSCAN SP-1 of KLA-TENCOR. Especially, 0.065 ~ 0.12 micron LPD items were evaluated among the polishing quality, and the microroughness was 100 × Terrain characteristics were evaluated by filtering at 100 micron units.
표 1의 결과에 나타난 바와 같이 실시예 1-2는 비교예 1 내지 3의 조성물과 비교하여 submicron LPD의 품질 측면에서 우수한 결과를 나타내었고, 웨이비니스 (Waveness) 범위에서 나타나는 미세 거칠음(Microroughness) 품질이 우수하였다. As shown in the results of Table 1, Examples 1-2 showed excellent results in terms of the quality of the submicron LPD compared to the compositions of Comparative Examples 1 to 3, and the microroughness quality appearing in the waveiness range. Was excellent.
상기에서 설명한 바와 같이, 본 발명의 연마용 슬러리를 사용하여 경면연마 공정을 수행하면 서브미크론 LPD(submicron LPD)가 크게 감소되고 웨이비니스 (Waveness) 범위의 표면거칠기가 5Å 수준인 슬러리 조성물을 제공할 수 있다.As described above, performing a mirror polishing process using the polishing slurry of the present invention can provide a slurry composition having a greatly reduced submicron LPD and having a surface roughness of 5 kW in the range of waveiness. Can be.
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