KR100504605B1 - Slurry Composition for Chemical Mechanical Polishing of Tungsten with Improved Removal Rate and Dispersability - Google Patents
Slurry Composition for Chemical Mechanical Polishing of Tungsten with Improved Removal Rate and Dispersability Download PDFInfo
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- KR100504605B1 KR100504605B1 KR10-2002-0085246A KR20020085246A KR100504605B1 KR 100504605 B1 KR100504605 B1 KR 100504605B1 KR 20020085246 A KR20020085246 A KR 20020085246A KR 100504605 B1 KR100504605 B1 KR 100504605B1
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- Prior art keywords
- polishing
- slurry
- slurry composition
- tungsten
- present
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- 238000005498 polishing Methods 0.000 title claims abstract description 88
- 239000002002 slurry Substances 0.000 title claims abstract description 60
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000000203 mixture Substances 0.000 title claims abstract description 13
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 11
- 239000010937 tungsten Substances 0.000 title claims abstract description 11
- 239000000126 substance Substances 0.000 title description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007800 oxidant agent Chemical class 0.000 claims abstract description 9
- 150000004697 chelate complex Chemical class 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 4
- 239000012498 ultrapure water Substances 0.000 claims abstract description 4
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 7
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- LMSDCGXQALIMLM-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;iron Chemical compound [Fe].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O LMSDCGXQALIMLM-UHFFFAOYSA-N 0.000 claims description 2
- UGCGKZYEELIHCG-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid;iron Chemical compound [Fe].OC(=O)CN(CC(O)=O)C(C)CN(CC(O)=O)CC(O)=O UGCGKZYEELIHCG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- PKORBOCCIRQQBW-UHFFFAOYSA-N C(C(C)N(CC(=O)O)CC(=O)O)N(CC(=O)O)CC(=O)O.[Mg] Chemical compound C(C(C)N(CC(=O)O)CC(=O)O)N(CC(=O)O)CC(=O)O.[Mg] PKORBOCCIRQQBW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004343 Calcium peroxide Substances 0.000 claims description 2
- ZJRXSAYFZMGQFP-UHFFFAOYSA-N barium peroxide Chemical compound [Ba+2].[O-][O-] ZJRXSAYFZMGQFP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- LHJQIRIGXXHNLA-UHFFFAOYSA-N calcium peroxide Chemical compound [Ca+2].[O-][O-] LHJQIRIGXXHNLA-UHFFFAOYSA-N 0.000 claims description 2
- 235000019402 calcium peroxide Nutrition 0.000 claims description 2
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 16
- 150000002334 glycols Chemical class 0.000 abstract description 11
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 239000013522 chelant Chemical class 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 31
- 239000002184 metal Substances 0.000 description 31
- 239000010410 layer Substances 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000009920 chelation Effects 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 2
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 2
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 229910002014 Aerosil® 130 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 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 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011369 resultant mixture Substances 0.000 description 1
- 239000013589 supplement Substances 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
- H01L21/04—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]
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
본 발명은 텅스텐 배선 연마용 슬러리 조성물에 관한 것으로, 본 발명의 슬러리 조성물은 초순수에 실리카 입자, 산화제, 킬레이트 착물, 글리콜 및 pH 조절제를 분산시켜 제조되며, 본 발명에서는 킬레이트 착물과 글리콜류를 병용함으로써 텅스텐 배선의 연마시 코로젼이나 심 등의 결함 없이 연마속도를 증가시키고 연마입자의 분산안정성 및 그에 따른 연마재현성을 개선하여, 반도체 제조 공정에서 높은 수율을 확보하는 것을 가능케 하였다.The present invention relates to a tungsten wire polishing slurry composition, wherein the slurry composition of the present invention is prepared by dispersing silica particles, oxidizing agents, chelate complexes, glycols, and pH adjusting agents in ultrapure water, and in the present invention, by using a chelate complex and glycols in combination When polishing tungsten wires, the polishing rate was increased without defects such as coronation or seam, and the dispersion stability of the abrasive particles and the polishing reproducibility thereof were improved, thereby making it possible to secure a high yield in the semiconductor manufacturing process.
Description
본 발명은 반도체 공정 중 웨이퍼의 광역 평탄화를 달성하기 위한 공정인 CMP(Chemical Mechanical Polishing/Planarization) 공정에 연마액으로 사용되는 슬러리 조성물에 관한 것으로, 보다 상세하게는 연마속도 및 분산안정성이 향상된 텅스텐 배선 연마용 슬러리 조성물에 관한 것이다.The present invention relates to a slurry composition used as a polishing liquid in a chemical mechanical polishing / planarization (CMP) process, which is a process for achieving wide-area planarization of a wafer in a semiconductor process, and more particularly, to a tungsten wiring having improved polishing speed and dispersion stability. It relates to a polishing slurry composition.
일반적으로 CMP 공정에서는 웨이퍼를 폴리우레탄 재질의 연마용 패드에 접촉시킨 상태에서 회전 운동과 직선 운동을 결합한 오비탈 운동을 수행하여 연마를 진행한다. 이때 화학적 및 기계적 연마 작용을 할 수 있는 슬러리를 패드 위에 떨어뜨려 CMP 공정에 적합한 성능을 가지도록 한다. CMP 공정에 사용되는 슬러리는 연마대상에 따라서 절연층 연마용 슬러리와 금속층 연마용 슬러리로 구분지을 수 있다. 절연층 연마용 슬러리는 반도체 공정 중 ILD(interlayer dielectric) 공정 및 IMD(intermetal dielectric), STI(shallow trench isolation) 공정에 적용된다. 그리고, 금속층 연마용 슬러리는 텅스텐 또는 알루미늄, 구리 배선의 평탄화 또는 플러그, 이중상감 공정에 사용된다.In general, in the CMP process, polishing is performed by performing an orbital motion combining a rotational motion and a linear motion while the wafer is in contact with a polishing pad made of polyurethane. At this time, the slurry capable of chemical and mechanical polishing is dropped on the pad to have a performance suitable for the CMP process. The slurry used in the CMP process may be classified into an insulating layer polishing slurry and a metal layer polishing slurry depending on the polishing target. The insulating layer polishing slurry is applied to an interlayer dielectric (ILD) process, an intermetal dielectric (IMD), and a shallow trench isolation (STI) process during semiconductor processing. The slurry for polishing the metal layer is used in the planarization or plugging of tungsten or aluminum or copper wiring, and the double damascene process.
일반적으로, 금속층 연마용 슬러리에는, 기계적 연마를 위한 연마입자, 금속층을 산화시켜 연마입자에 의한 기계적 연마를 용이하게 해주는 산화제와 산화보조제, 연마입자의 분산안정성을 향상시키기 위한 분산제, 연마대상인 금속배선의 부식이 발생하지 않고 산화가 잘 일어날 수 있는 pH를 맞추기 위한 pH 조절제 등이 필수성분으로 포함되며, 그 외 목적에 따라 슬러리의 성능을 개선하거나 보완할 수 있는 각종 첨가제들이 첨가된다.In general, a slurry for polishing a metal layer includes abrasive particles for mechanical polishing, an oxidizing agent and an oxidizing aid for oxidizing the metal layer to facilitate mechanical polishing by the abrasive particles, a dispersant for improving the dispersion stability of the abrasive particles, and a metal wiring to be polished. It is included as an essential ingredient such as a pH adjuster to adjust the pH that can occur oxidation well without corrosion, and various additives that can improve or supplement the performance of the slurry is added according to the other purposes.
금속층 연마용 슬러리의 연마 메카니즘은 다음과 같다. 우선, 금속층 표면을 산화제로 산화시켜 금속층을 연화시킨다. 그런 다음, 연화된 금속층을 기타 첨가제에 의해 화학적으로 제거시키면서, 연마입자를 통해 연마를 진행하게 된다. 이러한 과정의 연속적인 반복을 통해 금속층의 연마가 이루어진다.The polishing mechanism of the metal layer polishing slurry is as follows. First, the surface of the metal layer is oxidized with an oxidizing agent to soften the metal layer. Then, the softened metal layer is chemically removed by other additives, and the polishing is performed through the abrasive particles. The continuous repetition of this process leads to polishing of the metal layer.
상기와 같이 금속막질의 산화를 진행시키기 위해서는 슬러리의 pH가 연마대상인 금속의 산화가 진행될 수 있는 pH 영역에 들어야 한다. 텅스텐 연마용 슬러리의 경우에는 pH가 4 이하이어야 하는데, pH 3∼4에서 등전위점을 갖는 실리카 입자를 연마입자로 사용할 경우, 슬러리의 저장안정성은 매우 불안하게 된다. 한편, 알루미늄 연마용 슬러리의 경우에는, 알루미늄의 산화가 pH 4∼10의 범위에서 일어나기 때문에 중성 내지는 염기성 pH를 가져야 하는데, 실리카는 물론, 알루미나를 연마입자로 사용할 경우에도 알루미나의 등전위점이 pH 8∼9의 범위를 갖기 때문에 슬러리의 분산안정성이 크게 떨어진다. 이와 같이 슬러리의 분산안정성이 떨어지는 경우 연마재현성이 크게 감소하여 균일한 연마속도 및 연마균일도를 유지하기 어려울 뿐만 아니라, 양산공정에 적용시 사용 직전 슬러리의 분산상태를 균일하게 만들어 주기 위한 추가의 교반공정이 필요하게 되어, 사용상의 불편이 초래된다.In order to proceed with the oxidation of the metal film as described above, the pH of the slurry must be in the pH range where the oxidation of the metal to be polished can proceed. In the case of tungsten polishing slurry, the pH should be 4 or less. When silica particles having an equipotential point at pH 3 to 4 are used as the abrasive particles, the storage stability of the slurry becomes very unstable. On the other hand, in the case of aluminum polishing slurry, since the oxidation of aluminum occurs in the range of pH 4-10, it should have neutral or basic pH. When the alumina is used as abrasive particles as well as silica, the isoelectric point of alumina is pH 8- Since it has a range of 9, the dispersion stability of the slurry is greatly inferior. As such, when the dispersion stability of the slurry is inferior, the abrasive reproducibility is greatly reduced, so that it is difficult to maintain a uniform polishing rate and polishing uniformity, and an additional stirring process for making the dispersion state of the slurry immediately before use in the mass production process uniform. This becomes necessary, resulting in inconvenience in use.
또한, 금속층 연마용 슬러리에는 금속층에 대한 높은 연마속도는 물론 금속층과 절연층 간의 현저한 연마속도 차이가 요구된다. 즉, 금속배선에 대해서는 높은 연마속도가 요구되고 절연층에 대해서는 낮은 연마속도가 요구되는데, 그 이유는 금속배선과 절연층 간에 연마속도의 차이가 적으면 패턴 밀도가 높은 곳에서 에로젼 등의 결함이 발생될 수 있기 때문이다. 이러한 문제는, 금속배선과 절연층의 연마속도가 모두 높으면 패턴 밀도가 높은 부분만 부분적으로 연마속도가 높아지는데 기인한다. 따라서, 이를 방지하기 위해서는 금속층의 연마속도는 높게 유지하면서 절연층의 연마속도는 낮추어야 하며, 금속층과 절연층의 연마속도비가 적어도 30:1 내지 100:1의 범위에 들도록 해야 한다.In addition, the metal polishing slurry requires a high polishing rate for the metal layer as well as a significant difference in polishing rate between the metal layer and the insulating layer. That is, high polishing rate is required for metal wiring and low polishing rate is required for insulating layer, because the reason is that defects such as erosion at high pattern density when the difference in polishing rate between metal wiring and insulating layer is small. This can happen. This problem is due to the fact that the polishing rate of both the metal wiring and the insulating layer is high, so that only the portion having the high pattern density increases in part. Therefore, in order to prevent this, the polishing rate of the insulating layer should be kept low while the polishing rate of the metal layer is high, and the polishing rate ratio of the metal layer and the insulating layer should be in the range of at least 30: 1 to 100: 1.
미국특허 제5,958,288호 등에서는 과산화수소와 금속촉매를 사용하여 금속층에 대해 높은 연마속도를 갖는 연마용 슬러리를 제조하였으나, 이 특허에 사용된 것과 같이 다단계 산화가를 갖는 금속촉매의 경우, 연마 중 웨이퍼의 금속오염을 초래하여 반도체 칩의 신뢰성 저하 원인으로 작용하거나, 또는 지나치게 강한 산화력으로 인하여 코로젼(corrosion) 또는 심(seam) 등의 현상을 유발하는 문제점이 있다.US Pat. No. 5,958,288 et al. Prepared a polishing slurry having a high polishing rate for a metal layer using hydrogen peroxide and a metal catalyst. However, in the case of a metal catalyst having a multistage oxidation value, as used in this patent, There is a problem that causes a metal contamination to act as a cause of lowering the reliability of the semiconductor chip, or cause a phenomenon such as corrosion or seam due to excessively strong oxidation.
이에 본 발명은 상기와 같은 종래기술의 문제점들을 해결하기 위한 것으로, 연마성능과 분산안정성이 향상된 금속층 연마용 슬러리 조성물로서, 특히 텅스텐 배선의 연마에 적합한 연마용 슬러리 조성물을 제공함을 목적으로 한다.Accordingly, the present invention is to solve the problems of the prior art as described above, and an object of the present invention is to provide a slurry composition for polishing a metal layer having improved polishing performance and dispersion stability, in particular, a polishing slurry composition suitable for polishing a tungsten wire.
상기와 같은 목적을 달성하기 위한 첨가제로서 본 발명에서는 킬레이트 착물과 글리콜류를 사용한다.As the additive for achieving the above object, in the present invention, chelate complexes and glycols are used.
즉, 본 발명은 다음의 성분들을 포함하는 텅스텐 배선 연마용 슬러리 조성물을 제공한다:That is, the present invention provides a tungsten wire polishing slurry composition comprising the following components:
(a) 실리카 입자;(a) silica particles;
(b) 산화제;(b) an oxidizing agent;
(c) 킬레이트 착물;(c) chelate complexes;
(d) 글리콜;(d) glycols;
(e) pH 조절제; 및(e) pH adjusters; And
(f) 초순수. (f) ultrapure water.
이하, 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
일반적으로 CMP 슬러리의 연마입자로는 금속산화물의 미분말이 사용되며, 본 발명의 텅스텐 배선 연마용 슬러리에는 실리카(성분 a)가 사용된다.Generally, a fine powder of metal oxide is used as the abrasive grain of the CMP slurry, and silica (component a) is used as the tungsten wire polishing slurry of the present invention.
실리카는 산화된 피연마물을 탈리시키는 작용을 함으로써 슬러리의 기계적 연마 성능을 담당하는데, 실리카의 첨가량이 많아지면 높은 연마속도를 얻을 수는 있으나 연마 중 발생되는 스크래치나 연마 후 웨이퍼에 잔류하는 연마입자 등의 결함이 발생될 수 있다. 또한, 실리카의 농도가 증가할수록 슬러리의 저장안정성 또는 분산안정성이 떨어져 슬러리를 장기간 사용하는데 어려움이 있다. 반면, 실리카의 첨가량이 적을 경우, 연마속도가 낮아지거나 광역 평탄화를 실현하는데 어려움이 있다. 따라서, 본 발명의 연마용 슬러리의 실리카 함량은 1중량%에서 25중Silica is responsible for the mechanical polishing performance of the slurry by desorbing the oxidized abrasive, and if the amount of silica is added, a high polishing rate can be obtained, but scratches generated during polishing or abrasive particles remaining on the wafer after polishing A defect may occur. In addition, as the concentration of silica increases, the storage stability or dispersion stability of the slurry decreases, making it difficult to use the slurry for a long time. On the other hand, when the addition amount of silica is small, it is difficult to realize a low polishing rate or wide area planarization. Therefore, the silica content of the polishing slurry of the present invention is 1 to 25 weight percent
량%가 바람직하며, 보다 바람직하게는 3중량%에서 15중량%로 한정된다.Amount% is preferable, More preferably, it is limited to 3 weight% to 15 weight%.
금속층 연마용 슬러리에는 통상적으로 금속 배선을 산화시키기 위한 산화제가 첨가되는데, 본 발명에서는 산화제(성분 b)로서 과산화수소, 과산화벤조일, 과산화칼슘, 과산화바륨 및 과산화나트륨으로 구성된 군에서 선택되는 1종 이상의 과산화물을 사용하며, 가장 바람직하게는 높은 산화전위를 갖는 과산화수소를 연마직전에 슬러리에 첨가한다.An oxidizing agent for oxidizing metal wiring is usually added to the metal polishing slurry, and in the present invention, at least one peroxide selected from the group consisting of hydrogen peroxide, benzoyl peroxide, calcium peroxide, barium peroxide, and sodium peroxide as the oxidizing agent (component b). Most preferably, hydrogen peroxide having a high oxidation potential is added to the slurry just before polishing.
상기 과산화물의 첨가량은 1중량%에서 5중량%인 것이 바람직하며, 보다 바람직하게는 1.5중량%에서 4중량%의 범위 내에서 첨가된다. 과산화물의 첨가량이 이보다 많을 경우에는 산화력이 너무 강하여 코로젼(corrosion) 또는 심(seam) 현상이 발생될 수 있는 반면, 연마속도 증가에는 큰 도움이 되지 않는다. 그리고 이보다 적은 양을 첨가할 경우에는 산화력이 너무 약하여 CMP 공정에서 기대하는 연마속도를 얻을 수 없다.The amount of the peroxide added is preferably 1% by weight to 5% by weight, more preferably 1.5% by weight to 4% by weight. If the amount of peroxide added is higher than this, the oxidizing power may be so strong that corrosion or seam may occur, but it does not help to increase the polishing rate. In addition, when a smaller amount is added, the oxidation power is so weak that the polishing rate expected in the CMP process cannot be obtained.
과산화물 중에서도 특히 과산화수소는 상술하였듯이 산화력이 너무 높기 때문에, 금속 배선 상층에 산화막을 형성시킴으로써 금속층의 지속적인 산화를 방해하며, 따라서 적절한 연마속도를 유지하는 것을 어렵게 한다. 이러한 문제를 해결하기 위하여, 본 발명에서는 상기 산화제에 의해 생성된 후 연마입자의 기계적 연마작용에 의해 탈리된 금속산화물을 킬레이팅하여 연마대상에의 재흡착을 방지함으로써 높은 연마속도를 갖도록 하기 위해 킬레이트 착물(성분 c)을 사용한다. 킬레이트 착물의 경우 자체 산화력을 가지고 있지 않아 추가적인 부식으로 인한 코로젼 현상이 발생되지 않으며, 산화막 표면에서 킬레이트제의 역할을 하므로 심(seam) 현상을 방지할 수 있다.Among the peroxides, in particular, hydrogen peroxide has a high oxidizing power as described above, thereby forming an oxide film on the upper portion of the metal wiring to prevent continuous oxidation of the metal layer, thus making it difficult to maintain an appropriate polishing rate. In order to solve this problem, the present invention chelates to have a high polishing rate by chelating the metal oxide produced by the oxidizing agent and then desorbed by the mechanical polishing action of the abrasive particles to prevent resorption to the polishing object. Complex (component c) is used. Since the chelate complex does not have its own oxidizing power, no corrosion phenomenon occurs due to additional corrosion, and the chelating agent acts as a chelating agent on the surface of the oxide film, thereby preventing seam.
본 발명에 유용한 킬레이트 착물의 예에는 철-프로필렌다이아민테트라아세트산(PDTA-Fe), 철-에틸렌다이아민테트라아세트산(EDTA-Fe), 마그네슘-프로필렌다이아민테트라아세트산(PDTA-Mg) 등이 포함되며, 그 첨가량은 0.001중량%에서 1.0중Examples of chelate complexes useful in the present invention include iron-propylenediaminetetraacetic acid (PDTA-Fe), iron-ethylenediaminetetraacetic acid (EDTA-Fe), magnesium-propylenediaminetetraacetic acid (PDTA-Mg), and the like. The addition amount is 0.001% by weight in 1.0
량%인 것이 바람직하고, 보다 바람직하게는 0.005중량%에서 0.5중량%의 함량으로 첨가된다. 킬레이트 착물의 첨가량이 상기의 양보다 적을 경우 산화막 제거 속도가 낮아져 CMP 공정에서 기대하는 연마속도를 얻기 어려우며, 상기의 양보다 많을 경우 연마속도가 약간 증가되기는 하나 그 증가 정도가 그다지 현저하지 않아 비효율적이다. 그리고 너무 과량을 첨가시 연마후 웨이펴 위에 금속 잔류물이 남아 오히려 반도체 칩의 신뢰도를 저하시키는 원인으로 작용할 수 있다.It is preferably in the amount of% by weight, more preferably in an amount of 0.005% by weight to 0.5% by weight. If the amount of the chelate complex is less than the above amount, the removal rate of the oxide film is lowered, which makes it difficult to obtain the polishing rate expected in the CMP process. If the amount of the chelate complex is more than the above amount, the rate of polishing is slightly increased, but the increase is not so significant. . If too much is added, a metal residue may remain on the wafer after polishing, which may act as a cause of lowering the reliability of the semiconductor chip.
본 발명에서와 같이 킬레이트 착물을 사용하는 경우 촉매를 사용한 경우에 비해 약간 낮은 연마속도를 갖게 된다. 따라서, 본 발명에서는 산화물의 킬레이트화가 보다 잘 진행될 수 있도록 글리콜류(성분 d)를 첨가한다. 본 발명에 사용되는 글리콜로는 모노에틸렌글리콜(mono-ethylene glycol), 다이에틸렌글리콜(di-ethylene glycol) 및 트리에틸렌글리콜(tri-ethylene glycol)이 바람직하며, 이들 중 1종을 단독으로 사용하거나 또는 2종 이상을 병용한다. 그 외의 글리콜도 킬레이트의 윤활작용을 할 수 있으나, 슬러리의 비이상적인 점도 증가 등의 문제로 인하여 CMP 공정에서 요구되는 평탄성을 얻기에 부적절하다.As in the present invention, the use of the chelate complex has a slightly lower polishing rate than that of the catalyst. Therefore, in the present invention, glycols (component d) are added to facilitate the chelation of the oxide. As the glycol used in the present invention, mono-ethylene glycol, di-ethylene glycol and tri-ethylene glycol are preferable, and one of these may be used alone or Or use 2 or more types together. Other glycols may also lubricate the chelates, but are inadequate for obtaining the flatness required in the CMP process due to problems such as non-ideal viscosity increase of the slurry.
본 발명에 사용된 글리콜류는 상기와 같이 킬레이트화를 촉진하는 효과 이외에, 연마입자의 분산성을 개선하는 효과도 있어 본 발명의 슬러리의 분산안정성을 향상시키는데 기여한다. 앞에서 언급한 바와 같이 금속층 연마용 슬러리의 경우 금속산화막을 형성하기 위해 낮은 pH를 갖는데, 이로 인하여 슬러리의 분산안정성이 매우 불안해진다. 그런데, 본 발명에서와 같이 글리콜류를 첨가시 연마입자 주위의 음전하를 보호하는 역할을 하기 때문에, 슬러리의 분산안정성 개선과 킬레이트화의 촉진이 결과되는 것으로 추정된다.In addition to the effect of promoting chelation as described above, the glycols used in the present invention also have an effect of improving the dispersibility of the abrasive particles, contributing to improving the dispersion stability of the slurry of the present invention. As mentioned above, the slurry for polishing a metal layer has a low pH to form a metal oxide film, which makes the dispersion stability of the slurry very unstable. However, since it plays a role of protecting the negative charge around the abrasive particles when the glycols are added as in the present invention, it is estimated that the improvement of the dispersion stability of the slurry and the promotion of the chelation are resulted.
본 발명에서는 글리콜류를 슬러리에 0.001중량%에서 3중량%까지 첨가할 수 있으며, 보다 바람직하게는 0.1중량%에서 1중량%의 함량으로 첨가한다. 이보다 적은 양을 첨가시 글리콜류 첨가의 목적인 분산안정성 개선과 킬레이팅 효과 개선을 이루기 어렵다. 반면 이보다 많은 양을 첨가시 슬러리의 점도가 지나치게 상승되어 연마시 평탄성이 떨어지거나 첨가량에 비해 성능 개선효과가 미미하여 효율성이 떨어진다.In the present invention, glycols can be added to the slurry from 0.001% by weight to 3% by weight, more preferably from 0.1% by weight to 1% by weight. When a smaller amount is added, it is difficult to achieve improvement in dispersion stability and chelating effect for the purpose of adding glycols. On the other hand, when a larger amount is added, the viscosity of the slurry is excessively increased, resulting in poor flatness during polishing or inefficient efficiency compared to the added amount.
텅스텐 배선을 연마하는데 사용되는 슬러리의 경우 pH가 4 이하인 조건에서 텅스텐의 산화막이 형성되기 때문에, 본 발명에서는 질산 또는 황산과 같은 산과 수산화칼륨 또는 암모니아와 같은 염기를 첨가하여 pH를 4 이하로 조정한다. 특히 저장안정성의 개선 측면에서는 수산화칼륨보다는 암모니아가 바람직한데, 그 이유는 수산화칼륨으로 pH를 조절시 슬러리의 점도가 암모니아로 조절한 슬러리에 비해 상대적으로 높아져 슬러리의 장기 보관 사용시 어려움이 크기 때문이다. 본 발명의 연마용 슬러리의 pH는 2 내지 4의 범위에 드는 것이 바람직하며, 보다 바람직하게는 2.5 내지 3.5로 유지된다. 상기 범위를 벗어나는 pH를 갖는 경우, 텅스텐 배선에 산화막이 형성되지 않고 부식이 발생되거나, 슬러리가 화학적인 연마 효과를 발휘할 수 없어 연마속도가 급격히 떨어지는 현상이 발생할 수 있다.In the case of the slurry used to polish the tungsten wire, since an oxide film of tungsten is formed at a pH of 4 or less, in the present invention, the pH is adjusted to 4 or less by adding an acid such as nitric acid or sulfuric acid and a base such as potassium hydroxide or ammonia. . In particular, in terms of improving storage stability, ammonia is preferable to potassium hydroxide because the viscosity of the slurry is relatively high when the pH is adjusted with potassium hydroxide, compared to the slurry adjusted with ammonia, and thus the difficulty of long-term storage of the slurry is large. The pH of the polishing slurry of the present invention is preferably in the range of 2 to 4, more preferably maintained at 2.5 to 3.5. In the case of having a pH outside the above range, corrosion may occur without forming an oxide film on the tungsten wiring, or the slurry may not exhibit a chemical polishing effect, which may cause a sharp drop in polishing rate.
이하, 실시예를 통하여 본 발명을 보다 구체적으로 설명하고자 하나, 이러한 실시예들은 단지 설명의 목적을 위한 것으로 본 발명을 제한하는 것으로 해석되어서는 안된다.Hereinafter, the present invention will be described in more detail with reference to examples, but these examples are for illustrative purposes only and should not be construed as limiting the present invention.
비교예 1 및 실시예 1-1 내지 1-3: 모노에틸렌글리콜의 연마속도 개선효과Comparative Example 1 and Examples 1-1 to 1-3: effect of improving the polishing rate of monoethylene glycol
2ℓ의 폴리에틸렌 플라스크에, Aerosil 130(Degussa社) 350g, PDTA-Fe 8g, 및 50% 과산화수소수 50g을 투입하고, 모노에틸렌글리콜(MEG)을 0.0g, 10.0g, 30.0g 또는 60.0g씩 첨가한 다음, 초순수로 최종 부피를 2ℓ로 맞춘 후, 2,000rpm에서 2시간 동안 교반하였다. 교반이 완료된 후, 결과되는 혼합물을 고압분산법을 이용하여 1,200psi에서 1회 분산시켜 얻어진 예비 슬러리를 질산과 암모니아로 pH를 3.0으로 조절한 다음, 1㎛ 필터를 통해 여과하여 최종 슬러리를 수득하였다.Into a 2-liter polyethylene flask, 350 g of Aerosil 130 (Degussa), 8 g of PDTA-Fe, and 50 g of 50% hydrogen peroxide were added, and 0.0 g, 10.0 g, 30.0 g or 60.0 g of monoethylene glycol (MEG) was added. Next, the final volume was adjusted to 2 L with ultrapure water, and then stirred at 2,000 rpm for 2 hours. After stirring was completed, the resultant mixture was dispersed once at 1,200 psi using a high pressure dispersion method, and the resulting slurry was adjusted to pH 3.0 with nitric acid and ammonia, and then filtered through a 1 μm filter to obtain a final slurry. .
각각의 슬러리를 사용하여 아래와 같이 2분간 연마를 수행한 후, 제거된 텅스텐층의 두께로부터 연마속도를 측정하였으며, 그 결과는 하기 표 1에 기재된 바와 같다.After polishing for 2 minutes using each slurry as described below, the polishing rate was measured from the thickness of the removed tungsten layer, the results are shown in Table 1 below.
o 연마기 모델: 6EC(STRASBAUGH社)o Grinder model: 6EC (STRASBAUGH)
o 연마조건:o Polishing condition:
- 패드 타입: IC1400/SubaⅣ Stacked(Rodel社) Pad Type: IC1400 / SubaIV Stacked (Rodel)
- 평탄화 속도: 75rpm -Flattening Speed: 75rpm
- 퀼(quill) 속도: 35rpm Quill speed: 35 rpm
- 압력: 4psi Pressure: 4 psi
- 배압: 0psi Back pressure: 0psi
- 온도: 25℃ Temperature: 25 ℃
- 슬러리 유속: 250㎖/min Slurry flow rate: 250 ml / min
o 연마대상: 10,000Å 두께의 텅스텐(W)층이 증착된 6인치 웨이퍼o Polishing target: 6-inch wafer with 10,000 tungsten (W) layer deposited
비교예 2 및 실시예 2-1 내지 2-3: 다이에틸렌글리콜의 연마속도 개선효과Comparative Example 2 and Examples 2-1 to 2-3: the effect of improving the polishing rate of diethylene glycol
모노에틸렌글리콜 대신에 다이에틸렌글리콜(DEG)을 첨가한 것을 제외하고는, 상기 실시예 1과 동일한 방법으로 슬러리를 제조 후 연마속도를 측정하였다. 그 결과는 하기 표 2와 같다.Except that diethylene glycol (DEG) was added instead of monoethylene glycol, the slurry was prepared in the same manner as in Example 1 and then the polishing rate was measured. The results are shown in Table 2 below.
비교예 3 및 실시예 3-1 내지 3-3: 트리에틸렌글리콜의 연마속도 개선효과Comparative Example 3 and Examples 3-1 to 3-3: the effect of improving the polishing rate of triethylene glycol
모노에틸렌글리콜 대신에 트리에틸렌글리콜(TEG)을 첨가한 것을 제외하고는, 상기 실시예 1과 동일한 방법으로 슬러리를 제조 후 연마속도를 측정하였다. 그 결과는 하기 표 3과 같다.Except that triethylene glycol (TEG) was added instead of monoethylene glycol, the slurry was prepared in the same manner as in Example 1 and then the polishing rate was measured. The results are shown in Table 3 below.
실시예 4-1 내지 4-5: 다이에틸렌글리콜의 분산안정성 개선효과Examples 4-1 to 4-5: effect of improving dispersion stability of diethylene glycol
상기 실시예 2-1에서 제조된, 다이에틸렌글리콜이 10.0g 첨가된 슬러리를 상온에서 0일, 30일, 60일, 90일 및 180일을 방치한 후, 연마속도와 평균 입자크기를 측정하여 비교하였다. 이때 연마속도는 상기 실시예 1에서와 동일한 방법으로 측정되었다. 측정 결과는 하기 표 4와 같다.After the slurry prepared in Example 2-1, 10.0g of diethylene glycol is added, and left at 0, 30, 60, 90 and 180 days at room temperature, the polishing rate and average particle size were measured. Compared. At this time, the polishing rate was measured in the same manner as in Example 1. The measurement results are shown in Table 4 below.
비교예 4-1 내지 4-5: 다이에틸렌글리콜의 분산안정성 개선효과Comparative Examples 4-1 to 4-5: effect of improving dispersion stability of diethylene glycol
상기 비교예 2에서 제조된, 다이에틸렌글리콜이 첨가되지 않은 슬러리를 상온에서 0일, 30일, 60일, 90일 및 180일을 방치한 후, 연마속도와 평균 입자크기를 측정하여 비교하였다. 이때 연마속도는 상기 실시예 1에서와 동일한 방법으로 측정되었다. 측정 결과는 하기 표 5와 같다.The slurry prepared in Comparative Example 2, which was not added with diethylene glycol, was left at room temperature for 0 days, 30 days, 60 days, 90 days, and 180 days, and then the polishing rate and average particle size were measured and compared. At this time, the polishing rate was measured in the same manner as in Example 1. The measurement results are shown in Table 5 below.
이상에서 상세히 설명한 바와 같이, 본 발명에서는 킬레이트 착물과 글리콜류를 병용함으로써 텅스텐 배선의 연마시 코로젼이나 심 등의 결함 없이 연마속도를 증가시키고 연마입자의 분산안정성 및 그에 따른 연마재현성을 개선하여, 반도체 제조 공정에서 높은 수율을 확보하는 것을 가능케 하였다.As described in detail above, in the present invention, by using a chelating complex and glycols together, the polishing rate is increased without defects such as coronation or seam when polishing tungsten wires, and the dispersion stability of the abrasive particles and the abrasive reproducibility thereof are improved. It was possible to ensure high yield in the semiconductor manufacturing process.
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