WO2012009959A1 - Chemical mechanical polishing slurry - Google Patents
Chemical mechanical polishing slurry Download PDFInfo
- Publication number
- WO2012009959A1 WO2012009959A1 PCT/CN2011/001186 CN2011001186W WO2012009959A1 WO 2012009959 A1 WO2012009959 A1 WO 2012009959A1 CN 2011001186 W CN2011001186 W CN 2011001186W WO 2012009959 A1 WO2012009959 A1 WO 2012009959A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polishing liquid
- liquid according
- sulfate
- polishing
- silver
- Prior art date
Links
- 238000005498 polishing Methods 0.000 title claims abstract description 131
- 239000000126 substance Substances 0.000 title claims abstract description 48
- 239000002002 slurry Substances 0.000 title claims abstract description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 32
- 239000010937 tungsten Substances 0.000 claims abstract description 32
- 239000007800 oxidant agent Substances 0.000 claims abstract description 17
- 239000012190 activator Substances 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 125
- 239000007788 liquid Substances 0.000 claims description 44
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 26
- -1 silver ions Chemical class 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- 229910052709 silver Inorganic materials 0.000 claims description 16
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 14
- 239000004332 silver Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- 230000001590 oxidative effect Effects 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 8
- 229940120146 EDTMP Drugs 0.000 claims description 7
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000003112 inhibitor Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 6
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 5
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052755 nonmetal Inorganic materials 0.000 claims description 4
- 150000002978 peroxides Chemical group 0.000 claims description 4
- RBWNDBNSJFCLBZ-UHFFFAOYSA-N 7-methyl-5,6,7,8-tetrahydro-3h-[1]benzothiolo[2,3-d]pyrimidine-4-thione Chemical compound N1=CNC(=S)C2=C1SC1=C2CCC(C)C1 RBWNDBNSJFCLBZ-UHFFFAOYSA-N 0.000 claims description 3
- 229940096017 silver fluoride Drugs 0.000 claims description 3
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical group [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 claims description 3
- 239000012425 OXONE® Substances 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical group N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims 2
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 18
- 230000000694 effects Effects 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000000354 decomposition reaction Methods 0.000 description 11
- 101100203596 Caenorhabditis elegans sol-1 gene Proteins 0.000 description 10
- ZODDGFAZWTZOSI-UHFFFAOYSA-N nitric acid;sulfuric acid Chemical compound O[N+]([O-])=O.OS(O)(=O)=O ZODDGFAZWTZOSI-UHFFFAOYSA-N 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 9
- RQCJDSANJOCRMV-UHFFFAOYSA-N [Mn].[Ag] Chemical compound [Mn].[Ag] RQCJDSANJOCRMV-UHFFFAOYSA-N 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 150000007524 organic acids Chemical class 0.000 description 6
- 239000003381 stabilizer Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 description 5
- JMVRYCYAKSQJPJ-UHFFFAOYSA-N [K].[Ag] Chemical compound [K].[Ag] JMVRYCYAKSQJPJ-UHFFFAOYSA-N 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229960005191 ferric oxide Drugs 0.000 description 3
- 238000010979 pH adjustment Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- XFKVHUONJVDEIW-UHFFFAOYSA-N [Cl].S(O)(O)(=O)=O Chemical compound [Cl].S(O)(O)(=O)=O XFKVHUONJVDEIW-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000002925 chemical effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- VFNGKCDDZUSWLR-UHFFFAOYSA-N disulfuric acid Chemical compound OS(=O)(=O)OS(O)(=O)=O VFNGKCDDZUSWLR-UHFFFAOYSA-N 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- BSWGGJHLVUUXTL-UHFFFAOYSA-N silver zinc Chemical compound [Zn].[Ag] BSWGGJHLVUUXTL-UHFFFAOYSA-N 0.000 description 1
- CBXWGGFGZDVPNV-UHFFFAOYSA-N so4-so4 Chemical compound OS(O)(=O)=O.OS(O)(=O)=O CBXWGGFGZDVPNV-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
-
- 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]
Definitions
- the present invention relates to a chemical mechanical polishing liquid, and in particular to a chemical mechanical polishing liquid containing an activator and a strong oxidant precursor.
- the invention further relates to the use of the chemical mechanical polishing liquid of the present invention for tungsten chemical mechanical polishing.
- CMP chemical mechanical polishing
- CMP Chemical mechanical polishing
- It usually consists of a polishing table with a polishing pad and a polishing head for carrying the chip.
- the polishing head holds the chip and then presses the front side of the chip against the polishing pad.
- the polishing head moves linearly on the polishing pad or in the same direction of motion as the polishing table.
- the slurry containing the abrasive is dropped onto the polishing pad and laid flat on the polishing pad by centrifugation.
- the surface of the chip achieves global planarization under both mechanical and chemical effects.
- CMP chemical mechanical polishing
- Metal tungsten one of the chemical mechanical polishing (CMP) objects, has high electron current resistance at high current density and can form a good ohmic contact with silicon, so it can be used as a contact window and
- CMP chemical mechanical polishing
- U.S. Patent 5,340,370 discloses a formulation for tungsten chemical mechanical polishing (CMP) containing 0.1 M potassium ferricyanide, 5% silica, and acetate as a pH buffer. Since potassium ferricyanide decomposes highly toxic hydrocyanic acid under ultraviolet light or sunlight, and in an acidic medium, its widespread use is limited.
- CMP chemical mechanical polishing
- U.S. Patent No. 5,527,423, U.S. Patent No. 6,008,119, U.S. Patent No. 6,284,151, et al. discloses the use of the <RTIgt;Fe(N0< 3> ;>>3>, alumina system for tungsten mechanical polishing (CMP).
- CMP tungsten mechanical polishing
- the high concentration of ferric nitrate makes the pH of the polishing liquid strongly acidic, which seriously corrodes the equipment, and at the same time, generates rust and contaminates the polishing pad.
- high concentrations of iron ions act as mobile metal ions, which seriously reduce the reliability of semiconductor components.
- U.S. Patent No. 5,225, 034, U.S. Patent No. 5,354, 490 discloses the use of the use of hydrogen peroxide and silver nitrate as a oxidizing agent for the polishing of metal (copper).
- the amount of silver nitrate is large (greater than 2%), resulting in excessive polishing solution cost, unstable abrasive, easy precipitation, and rapid decomposition of hydrogen peroxide.
- U.S. Patent 5,958,288 discloses the use of ferric nitrate as a catalyst and hydrogen peroxide as an oxidant.
- a method of performing chemical mechanical polishing of tungsten It should be noted that in this patent, a variety of transition metal elements are mentioned, and only iron elements have been experimentally proven to be significantly effective. Therefore, the actual implementation effect and scope of the invention are limited. Although the method greatly reduces the amount of ferric nitrate, since the iron ion still exists and the Fenton reaction occurs between the hydrogen peroxide and the hydrogen peroxide, the hydrogen peroxide rapidly and violently decomposes and fails, so the polishing solution has a problem of poor stability.
- U.S. Patent No. 5,980,775 and U.S. Patent No. 6,068,787 incorporates an organic acid as a stabilizer to improve the rate of decomposition of hydrogen peroxide.
- the pH of the polishing solution is low (usually below about 2. 7), causing corrosion of the equipment.
- the polishing solution containing iron nitrate has a narrow pH adjustment range. Because when the pH is higher than 2. 7, the ferric nitrate will be hydrolyzed to form iron hydroxide precipitate, which will cause the polishing solution to fail, which limits its pH adjustment ability.
- the organic matter content (COD) in the polishing waste liquid is increased due to the addition of organic acid, which is not conducive to environmental protection.
- the stability of the oxidant hydrogen peroxide still exists.
- organic acid as a stabilizer improves the decomposition rate of hydrogen peroxide, the decomposition rate is still high, and the hydrogen peroxide concentration is usually reduced by more than 10% in two weeks, resulting in a decrease in polishing speed and a gradual decomposition failure of the polishing liquid.
- Chinese Patent No. CN 1966 594 A discloses a method of adding an etch inhibitor to the above catalytic system, but since the catalyst used is still iron, the problem of easy decomposition of hydrogen peroxide and poor stability still exists.
- the present invention provides a novel chemical mechanical polishing liquid for tungsten which is different from the above methods.
- the main differences between the present invention and the aforementioned U.S. Patents 5,225,034, 5,354,490 are:
- the combination of silver and hydrogen peroxide does not have a significant effect of increasing the polishing speed of tungsten, and only a combination of iron and hydrogen peroxide can significantly increase the polishing speed of tungsten.
- the present inventors have found that this new combination can significantly increase the polishing rate of tungsten as long as sulfate is further added to the system of hydrogen peroxide plus silver nitrate.
- the technical problem solved by the present invention is to provide a chemical mechanical polishing liquid which significantly increases the chemical mechanical polishing speed of tungsten.
- the chemical mechanical polishing liquid of the present invention contains an activator, a strong oxidant precursor, an abrasive, and water.
- the activator is a composition composed of silver ions and an oxidizing agent.
- the silver ions are derived from silver salts.
- the silver salt is silver fluoride, silver perchlorate, silver sulfate, and/or silver nitrate.
- the weight percentage of the silver salt is 0.05% ⁇ 0.3%.
- the oxidizing agent is a peroxide.
- the peroxide is one or more of hydrogen peroxide, ammonium persulfate and/or potassium monopersulfate.
- the oxidizing agent has a weight percentage of 0.1 to 5%.
- the strong oxidant precursor is a non-nitrate anion.
- the non-nitrate anion is a sulfate ion.
- the sulfate ion is derived from a sulfate.
- the sulfate is a non-metal sulfate or a metal sulfate.
- the non-metal sulfate is ammonium sulfate, and the metal sulfate is one or more of manganese sulfate, potassium sulfate and/or zinc sulfate.
- the abrasive is one or more selected from the group consisting of fumed silica, silica sol, alumina and/or cerium oxide.
- the abrasive has a weight percentage of 0.1 to 10%.
- the polishing liquid further contains a pH adjusting agent.
- the polishing solution has a pH of 0.5 to 5.
- the polishing liquid further contains a static etch rate inhibitor.
- the static corrosion rate inhibitor is an organophosphine compound.
- the organophosphine compound is ethylenediaminetetramethylene phosphonic acid (EDTMP).
- ETMP ethylenediaminetetramethylene phosphonic acid
- the static etch rate 005 ⁇ 0. 05% ⁇ The weight percentage of the preparation is 0. 005 ⁇ 0. 05%.
- the method for tungsten chemical mechanical polishing of the present invention comprises: using the chemical mechanical polishing liquid according to the present invention for dock chemical mechanical polishing.
- the positive effects of the present invention are:
- Hydrogen peroxide can still be present in the polishing solution very stably without the addition of a hydrogen peroxide stabilizer.
- the problem of rapid decomposition of hydrogen peroxide is solved, the use time of the polishing liquid is prolonged, the polishing speed is stabilized, and the cost is further saved.
- the chemical mechanical polishing method of the present invention may be free of organic substances (stabilizers such as organic acids, etc.). Therefore, the content of organic matter (COD emissions) in the polishing waste liquid is reduced, which is favorable for environmental protection.
- organic substances stabilizers such as organic acids, etc.
- the chemical mechanical polishing liquid used has a wider pH adjustment range, and can lower the corrosion of equipment by raising the pH value, and is applied to a wider CMP field.
- Fig. 1 is a schematic view showing the decomposition rate of hydrogen peroxide in the chemical mechanical polishing liquid of Example 6 and conventional Fe-HA.
- Table 1 shows the formulations of the chemical mechanical polishing liquids of Examples 1 to 24 and Comparative Examples 1 to 2 of the present invention, which are uniformly mixed in deionized water according to the components and contents thereof listed in Table 1, using PH Conditioning agent A chemical mechanical polishing solution can be prepared at the desired pH.
- Table 1 Chemical mechanical polishing liquid of the present invention Examples 1 to 24 and Comparative Examples 1 to 2
- Alumina 10. 00% 0. 2 Hydrogen peroxide 1 3 11 Silver
- Polishing machine is Logitech (UK) 1PM52 type, polytex polishing pad, 4cmx4cm square wafer (Wafer), grinding pressure 4psi, grinding table rotation speed 70rev/min, grinding head rotation speed 150rev/min, polishing droplet Acceleration of 100 ml / min.
- Comparative Example 1 shows that the polishing rate of tungsten is low only in the presence of hydrogen peroxide.
- Comparative Example 2 shows that: in combination with hydrogen peroxide and silver nitrate, the polishing rate of tungsten is very low.
- Examples 1 to 7, 23, 24 show that the combination of silver ions, sulfate groups and hydrogen peroxide in the presence of sulfate can significantly increase the polishing rate of tungsten.
- the silver ions may be derived from silver fluoride, silver perchlorate, silver sulfate, and silver nitrate. Effect Example 2
- Polishing conditions 8 inch wafer, IC1000 polishing pad, pressure 4ps i.
- Table 3 Examples 18 and 19 for tungsten polishing
- the data in Table 3 is the tungsten polishing rate of the chemical mechanical polishing liquid of Examples 18, 19 on the industrial machine of the present invention.
- the results show that the chemical mechanical polishing liquid of the present invention can achieve a very high polishing speed on an industrial machine. Effect Example 3
- Table 3 shows the formulations of Comparative Examples 3 to 16. According to the components listed in Table 3 and their contents, they are uniformly mixed in the deionized water to prepare a chemical mechanical polishing liquid.
- Polishing machine is Log i tech (UK) 1PM52 type, polytex polishing pad, 4 cm x 4cm square wafer (Wafer), grinding pressure 4ps i, grinding table speed 70 rev / min, grinding head rotation speed 150 rpm /min, polishing droplet acceleration of 100 ml / min.
- Table 5 lists some representative transition metal elements. As can be seen from the results in Table 5, the effect of the present invention (achieving a high tungsten polishing rate) can be achieved without a combination of any transition metal and hydrogen peroxide. Comparative Examples 4, 8, 9 also show that the effect of the present invention can be achieved without any metal sulfate. In contrast, the combination of silver ions and sulfate in the present invention (including silver sulfate itself) achieves a very high polishing rate, which is not obvious. Comparative Example 2
- Table 6 shows the formulations of Comparative Examples 17 to 19, which were prepared by mixing them in deionized water according to the components listed in Table 6 and their contents, to prepare a chemical mechanical polishing solution.
- Polishing machine is Logitech (UK) 1PM52 type, polytex polishing pad, 4cmx4cm square wafer (Wafer), grinding pressure 4psi, grinding table rotation speed 70rev/min, grinding head rotation speed 150rev/min, polishing droplet Acceleration of 100 ml / min.
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Abstract
Disclosed is a chemical mechanical polishing (CMP) slurry, comprising an activator, a strong oxidizer precursor, an abrasive, and water. The chemical mechanical polishing of the present invention enables a significant increase in the speed of tungsten polishing.
Description
一种化学机械抛光液 Chemical mechanical polishing liquid
技术领域 Technical field
本发明涉及一种化学机械抛光液， 具体涉及用一种含有激发剂和强氧化 剂前体的化学机械抛光液。本发明进一步涉及将本发明所述的化学机械抛光 液用于钨化学机械抛光。 The present invention relates to a chemical mechanical polishing liquid, and in particular to a chemical mechanical polishing liquid containing an activator and a strong oxidant precursor. The invention further relates to the use of the chemical mechanical polishing liquid of the present invention for tungsten chemical mechanical polishing.
技术背景 technical background
随着半导体技术的不断发展， 以及大规模集成电路互连层的不断增加， 导电层和绝缘介质层的平坦化技术变得尤为关键。 二十世纪 80年代， 由 IBM 公司首创的化学机械抛光 （CMP )技术被认为是目前全局平坦化的最有效的 方法。 With the continuous development of semiconductor technology and the increasing number of interconnect layers of large-scale integrated circuits, the planarization technology of conductive layers and dielectric layers has become particularly critical. In the 1980s, the chemical mechanical polishing (CMP) technology pioneered by IBM was considered the most effective method for global planarization.
化学机械抛光（CMP ) 由化学作用、 机械作用以及这两种作用结合而成。 它通常由一个带有抛光垫的研磨台， 及一个用于承载芯片的研磨头组成。 其 中研磨头固定住芯片， 然后将芯片的正面压在抛光垫上。 当进行化学机械抛 光时， 研磨头在抛光垫上线性移动或是沿着与研磨台一样的运动方向旋转。 与此同时， 含有研磨剂的浆液被滴到抛光垫上， 并因离心作用平铺在抛光垫 上。 芯片表面在机械和化学的双重作用下实现全局平坦化。 Chemical mechanical polishing (CMP) is a combination of chemical action, mechanical action, and both. It usually consists of a polishing table with a polishing pad and a polishing head for carrying the chip. The polishing head holds the chip and then presses the front side of the chip against the polishing pad. When chemical mechanical polishing is performed, the polishing head moves linearly on the polishing pad or in the same direction of motion as the polishing table. At the same time, the slurry containing the abrasive is dropped onto the polishing pad and laid flat on the polishing pad by centrifugation. The surface of the chip achieves global planarization under both mechanical and chemical effects.
对金属层化学机械抛光 （CMP ) 的主要机制被认为是： 氧化剂先将金属 表面氧化成膜， 以二氧化硅和氧化铝为代表的研磨剂将该层氧化膜机械去 除， 产生新的金属表面继续被氧化， 这两种作用协同进行。 The main mechanism of chemical mechanical polishing (CMP) of metal layers is considered as follows: The oxidant first oxidizes the surface of the metal into a film, and the abrasive film represented by silica and alumina mechanically removes the oxide film to produce a new metal surface. Continued to be oxidized, these two effects work together.
作为化学机械抛光 （CMP ) 对象之一的金属钨， 在高电流密度下， 抗电 子迁移能力强， 并且能够与硅形成很好的欧姆接触， 所以可作为接触窗及介 Metal tungsten, one of the chemical mechanical polishing (CMP) objects, has high electron current resistance at high current density and can form a good ohmic contact with silicon, so it can be used as a contact window and
^ 认 本
层洞的填充金属及扩散阻挡层。 ^ Recognition Filler metal and diffusion barrier of the layer.
钨的化学机械抛光 （CMP), 有多种方法： There are several methods for chemical mechanical polishing (CMP) of tungsten:
1991年， F. B. Kaufman等报道了铁***用于钨化学机械抛光的方法 ( "Chemical Mechanical Polishing for Fabricating Patterned W Metal Features as Chip Interconnects" , Journal of the Electro chemical Society, Vol.138, No.11, 1991年 11月）。 In 1991, FB Kaufman et al. reported the use of potassium ferricyanide for tungsten chemical mechanical polishing ("Chemical Mechanical Polishing for Fabricating Patterned W Metal Features as Chip Interconnects", Journal of the Electro Chemical Society, Vol. 138, No. 11 , November 1991).
美国专利 5340370公开了一种用于钨化学机械抛光（CMP) 的配方， 其 中含有 0.1M铁***， 5%氧化硅， 同时含有作为 pH缓冲剂的醋酸盐。 由于 铁***在紫外光或日光照射下， 以及在酸性介质中， 会分解出剧毒的氢氰 酸， 因而限制了其广泛使用。 U.S. Patent 5,340,370 discloses a formulation for tungsten chemical mechanical polishing (CMP) containing 0.1 M potassium ferricyanide, 5% silica, and acetate as a pH buffer. Since potassium ferricyanide decomposes highly toxic hydrocyanic acid under ultraviolet light or sunlight, and in an acidic medium, its widespread use is limited.
美国专利 5527423， 美国专利 6008119， 美国专利 6284151等公开了将 Fe (N03) 3, 氧化铝体系用于钨机械抛光（CMP) 的方法。 该抛光体系在静态 腐蚀速率 （static etch rate)方面具有优势， 但是由于釆用氧化铝作为研 磨剂， 产品缺陷 （defect)方面存在显著不足。 同时高浓度的硝酸铁使得抛 光液的 pH值呈强酸性， 严重腐蚀设备， 同时， 生成铁锈， 污染抛光垫。 除 此之外， 高浓度的铁离子作为可移动的金属离子， 严重降低了半导体元器件 的可靠性。 U.S. Patent No. 5,527,423, U.S. Patent No. 6,008,119, U.S. Patent No. 6,284,151, et al. discloses the use of the <RTIgt;Fe(N0<3>>>3>, alumina system for tungsten mechanical polishing (CMP). The polishing system has an advantage in terms of static etch rate, but due to the use of alumina as an abrasive, there are significant deficiencies in product defects. At the same time, the high concentration of ferric nitrate makes the pH of the polishing liquid strongly acidic, which seriously corrodes the equipment, and at the same time, generates rust and contaminates the polishing pad. In addition, high concentrations of iron ions act as mobile metal ions, which seriously reduce the reliability of semiconductor components.
美国专利 5225034, 美国专利 5354490公开了将过氧化氢和硝酸银共同 使用， 用做氧化剂进行金属（铜） 的抛光方法。 但是在该类型方法中， 硝酸 银用量很大 （大于 2%)， 造成抛光液成本过高， 研磨剂不稳定、 容易沉淀， 双氧水快速分解等问题。 U.S. Patent No. 5,225, 034, U.S. Patent No. 5,354, 490 discloses the use of the use of hydrogen peroxide and silver nitrate as a oxidizing agent for the polishing of metal (copper). However, in this type of method, the amount of silver nitrate is large (greater than 2%), resulting in excessive polishing solution cost, unstable abrasive, easy precipitation, and rapid decomposition of hydrogen peroxide.
美国专利 5958288公开了将硝酸铁用做催化剂， 过氧化氢用做氧化剂，
进行钨化学机械抛光的方法。 需要注意的是： 在该专利中， 提到了多种过渡 金属元素， 被实验证实显著有效的只有铁元素。 因此该发明的实际实施效果 和范围很有限。 该方法虽然大幅度降低了硝酸铁的用量， 但是由于铁离子仍 然存在， 和双氧水之间发生 Fenton反应， 双氧水会迅速、 并且剧烈地分解 失效， 因此该抛光液存在稳定性差的问题。 U.S. Patent 5,958,288 discloses the use of ferric nitrate as a catalyst and hydrogen peroxide as an oxidant. A method of performing chemical mechanical polishing of tungsten. It should be noted that in this patent, a variety of transition metal elements are mentioned, and only iron elements have been experimentally proven to be significantly effective. Therefore, the actual implementation effect and scope of the invention are limited. Although the method greatly reduces the amount of ferric nitrate, since the iron ion still exists and the Fenton reaction occurs between the hydrogen peroxide and the hydrogen peroxide, the hydrogen peroxide rapidly and violently decomposes and fails, so the polishing solution has a problem of poor stability.
美国专利 5980775和美国专利 6068787在美国专利 5958288基础上， 加 入有机酸做稳定剂， 改善了过氧化氢的分解速率。 但是由于有机酸的引入， 使得抛光液 pH值较低（通常低于 2. 7左右）， 造成设备腐蚀。 此外， 含有硝 酸铁的抛光液， PH值调节范围很窄。 因为当 pH值高于 2. 7时， 硝酸铁会水 解， 生成氢氧化铁沉淀， 造成抛光液失效， 限制了其 PH值调节能力。 在环 保上， 由于有机酸的加入， 提高了抛光废液中有机物含量（COD )， 不利于环 保。 此外， 氧化剂双氧水的稳定性问题仍然存在。 虽然加入有机酸做为稳定 剂， 改善了双氧水的分解速率， 但是其分解速率仍然较高， 通常两周内双氧 水浓度会降低 10%以上， 造成抛光速度下降， 抛光液逐渐分解失效。 U.S. Patent No. 5,980,775 and U.S. Patent No. 6,068,787, each of which is incorporated herein by reference to U.S. Patent No. 5,958, 288, incorporates an organic acid as a stabilizer to improve the rate of decomposition of hydrogen peroxide. However, due to the introduction of organic acids, the pH of the polishing solution is low (usually below about 2. 7), causing corrosion of the equipment. In addition, the polishing solution containing iron nitrate has a narrow pH adjustment range. Because when the pH is higher than 2. 7, the ferric nitrate will be hydrolyzed to form iron hydroxide precipitate, which will cause the polishing solution to fail, which limits its pH adjustment ability. In environmental protection, the organic matter content (COD) in the polishing waste liquid is increased due to the addition of organic acid, which is not conducive to environmental protection. In addition, the stability of the oxidant hydrogen peroxide still exists. Although the addition of organic acid as a stabilizer improves the decomposition rate of hydrogen peroxide, the decomposition rate is still high, and the hydrogen peroxide concentration is usually reduced by more than 10% in two weeks, resulting in a decrease in polishing speed and a gradual decomposition failure of the polishing liquid.
中国专利 CN1966594A公开了一种在上述催化体系中加入 etch抑制剂的 方法， 但是由于其所用催化剂仍然是铁元素， 双氧水易分解、 稳定性差等问 题仍然存在。 Chinese Patent No. CN 1966 594 A discloses a method of adding an etch inhibitor to the above catalytic system, but since the catalyst used is still iron, the problem of easy decomposition of hydrogen peroxide and poor stability still exists.
本发明提供了一种不同于以上各方法的、 新型的钨的化学机械抛光液。 本发明和上述美国专利 5225034， 5354490的主要区别在于： The present invention provides a novel chemical mechanical polishing liquid for tungsten which is different from the above methods. The main differences between the present invention and the aforementioned U.S. Patents 5,225,034, 5,354,490 are:
美国专利 5225034以及 5354490虽然利用过氧化氢和硝酸银共同作用进 行化学机械抛光， 但是该抛光方法针对铜， 没有提到钨。 在我们的试验中发 现： 实际上， 双氧水和硝酸银的组合不能显著提高钨的抛光速度。 在上述两
篇专利中只提到硝酸银， 没有提到硫酸银， 更没有揭示出硫酸银中的硫酸根 离子， 具有显著提高钨的抛光速度的特殊作用。 U.S. Patents 5,225,034 and 5,354,490, although chemical mechanical polishing is performed by the combination of hydrogen peroxide and silver nitrate, but the polishing method is directed to copper, and tungsten is not mentioned. In our experiments, it was found that: in fact, the combination of hydrogen peroxide and silver nitrate does not significantly increase the polishing speed of tungsten. In the above two In the patent, only silver nitrate is mentioned, silver sulfate is not mentioned, and sulfate ion in silver sulfate is not revealed, which has a special effect of significantly increasing the polishing speed of tungsten.
本发明和上述美国专利 5980775 , 6068787 以及 5958288的主要区别在 于： The main differences between the present invention and the aforementioned U.S. Patents 5,980,775, 6,068,787 and 5,958,288 are:
上述 3篇专利中， 银和双氧水的组合（例如， 双氧水加硝酸银）， 不具 有显著提高钨的抛光速度的作用， 能显著提高钨的抛光速度的只有铁和双氧 水的组合， （上述三篇专利自身的实施例证明了这两点）。 与之不同的是， 本发明发现： 只要在双氧水加硝酸银的体系中再进一步加入硫酸根， 这种新 的组合能够非常显著地提高钨的抛光速度。 In the above three patents, the combination of silver and hydrogen peroxide (for example, hydrogen peroxide plus silver nitrate) does not have a significant effect of increasing the polishing speed of tungsten, and only a combination of iron and hydrogen peroxide can significantly increase the polishing speed of tungsten. The implementation of the patent itself clarifies these two points). In contrast, the present inventors have found that this new combination can significantly increase the polishing rate of tungsten as long as sulfate is further added to the system of hydrogen peroxide plus silver nitrate.
在上述 3篇专利的 Fe- H202体系中， 铁会和过氧化氢之间产生 Fenton反 应， 产生强氧化性的羟自由基， 有利于提高钨的抛光速度。 而银和双氧水之 间， 没有 Fenton反应。 因此， 本发明在抛光机理上显著区别于上述 3篇专 利。 In the Fe-H 2 0 2 system of the above three patents, the Fenton reaction between iron and hydrogen peroxide produces a strong oxidizing hydroxyl radical, which is advantageous for increasing the polishing speed of tungsten. There is no Fenton reaction between silver and hydrogen peroxide. Therefore, the present invention is significantly different from the above-mentioned three patents in the polishing mechanism.
需要着重指出的是 ，在上述 5篇美国专利：5225034 , 5354490, 5980775 , 6068787以及 5958288中都没有发现、 也不能推断出： 双氧水、 银离子和硫 酸根的组合对提高钨的抛光作用具有非常奇特的作用， 因此， 本发明中的银 离子和硫酸根的组合是非显而易见的， 这种组合的实施效果是出乎意料的。 It should be emphasized that none of the above five US patents: 5225034, 5354490, 5980775, 6068787 and 5958288 have been inferred: the combination of hydrogen peroxide, silver ion and sulfate is very peculiar to improve the polishing effect of tungsten. The effect, therefore, the combination of silver ions and sulfate in the present invention is not obvious, and the effect of the combination is unexpected.
在美国专利 5980775 , 6068787以及 5958288的 Fe-HA抛光体系中， 由 于铁会和过氧化氢之间产生 Fenton反应， 过氧化氢会迅速分解， 因此必须 加入有机络合剂络合铁离子， 抑制这一分解过程。 而在本发明的体系中， 由 于没有 Fenton反应， 不需要加稳定剂， 过氧化氢也能长期保持非常稳定。
发明概要 In the Fe-HA polishing system of U.S. Patent Nos. 5,980,775, 6,068,787 and 5,958,288, since Fenton reaction occurs between iron and hydrogen peroxide, hydrogen peroxide decomposes rapidly, so it is necessary to add an organic complexing agent to complex iron ions, thereby suppressing this. A decomposition process. In the system of the present invention, since there is no Fenton reaction, no stabilizer is added, and hydrogen peroxide can be kept very stable for a long period of time. Summary of invention
本发明解决的技术问题是提供一种化学机械抛光液， 显著提高钨的化学 机械抛光速度。 The technical problem solved by the present invention is to provide a chemical mechanical polishing liquid which significantly increases the chemical mechanical polishing speed of tungsten.
本发明的化学机械抛光液，其含有：激发剂，强氧化剂前体（ precursor ), 研磨剂和水。 The chemical mechanical polishing liquid of the present invention contains an activator, a strong oxidant precursor, an abrasive, and water.
本发明中， 所述的激发剂为由银离子和氧化剂组成的组合物。 所述的银 离子来自于银盐。 所述银盐为氟化银、 高氯酸银、 硫酸银和 /或硝酸银。 所 述的银盐重量百分比 0.05% ~ 0.3%。 In the present invention, the activator is a composition composed of silver ions and an oxidizing agent. The silver ions are derived from silver salts. The silver salt is silver fluoride, silver perchlorate, silver sulfate, and/or silver nitrate. The weight percentage of the silver salt is 0.05% ~ 0.3%.
本发明中， 所述的氧化剂为过氧化物。 所述的过氧化物为过氧化氢、 过 硫酸铵和 /或单过硫酸钾中的一种或多种。 所述的氧化剂的重量百分比为 0.1 ~ 5%。 In the present invention, the oxidizing agent is a peroxide. The peroxide is one or more of hydrogen peroxide, ammonium persulfate and/or potassium monopersulfate. The oxidizing agent has a weight percentage of 0.1 to 5%.
本发明中， 所述的强氧化剂前体（precursor)为非硝酸根阴离子。 所 述的非硝酸根阴离子为硫酸根离子。 所述的硫酸根离子来自于硫酸盐。 所述 的硫酸盐为非金属硫酸盐或金属硫酸盐。 所述的非金属硫酸盐为硫酸铵， 所 述的金属硫酸盐为硫酸锰、 硫酸钾和 /或硫酸锌中的一种或多种。 In the present invention, the strong oxidant precursor is a non-nitrate anion. The non-nitrate anion is a sulfate ion. The sulfate ion is derived from a sulfate. The sulfate is a non-metal sulfate or a metal sulfate. The non-metal sulfate is ammonium sulfate, and the metal sulfate is one or more of manganese sulfate, potassium sulfate and/or zinc sulfate.
本发明中， 所述的研磨剂为气相二氧化硅、 硅溶胶、 氧化铝和 /或氧化 铈中的一种或多种。 所述的研磨剂的重量百分比为 0.1~10%。 In the present invention, the abrasive is one or more selected from the group consisting of fumed silica, silica sol, alumina and/or cerium oxide. The abrasive has a weight percentage of 0.1 to 10%.
本发明中， 所述的抛光液还含有 PH调节剂。 所述的抛光液的 pH值为 0.5~5。 In the present invention, the polishing liquid further contains a pH adjusting agent. The polishing solution has a pH of 0.5 to 5.
本发明中， 所述的抛光液还含有静态腐蚀速度（static etch rate)抑 制剂。 所述的静态腐蚀速度抑制剂为有机膦化合物。 所述的有机膦化合物为 乙二胺四甲叉膦酸（EDTMP)。 所述的静态腐蚀速度 （static etch rate)抑
制剂的重量百分比为 0. 005 ~ 0. 05%。 本发明的用于钨化学机械抛光方法， 包括： 将根据本发明所述的化学机 械抛光液用于坞化学机械抛光。 本发明的积极进步效果在于： In the present invention, the polishing liquid further contains a static etch rate inhibitor. The static corrosion rate inhibitor is an organophosphine compound. The organophosphine compound is ethylenediaminetetramethylene phosphonic acid (EDTMP). The static etch rate 005〜 0. 05%。 The weight percentage of the preparation is 0. 005 ~ 0. 05%. The method for tungsten chemical mechanical polishing of the present invention comprises: using the chemical mechanical polishing liquid according to the present invention for dock chemical mechanical polishing. The positive effects of the present invention are:
1、 显著提高了钨的抛光速度， 提高了生产效率， 降低制造成本。 1. Significantly increase the polishing speed of tungsten, increase production efficiency and reduce manufacturing costs.
2、 在不加入过氧化氢稳定剂的情况下， 过氧化氢仍能非常稳定地存在 于抛光液中。 解决了过氧化氢快速分解的问题， 延长了抛光液的使用时限， 保证了抛光速度的稳定， 从而进一步节约成本。 2. Hydrogen peroxide can still be present in the polishing solution very stably without the addition of a hydrogen peroxide stabilizer. The problem of rapid decomposition of hydrogen peroxide is solved, the use time of the polishing liquid is prolonged, the polishing speed is stabilized, and the cost is further saved.
3、 本发明的化学机械抛光方法， 可以不含有机物 （稳定剂， 诸如有机 酸等） 。 因此， 降低了抛光废液中有机物的含量（COD排放量） ， 有利于环 保。 3. The chemical mechanical polishing method of the present invention may be free of organic substances (stabilizers such as organic acids, etc.). Therefore, the content of organic matter (COD emissions) in the polishing waste liquid is reduced, which is favorable for environmental protection.
4、 本发明的化学机械抛光方法中， 使用的化学机械抛光液具有更宽的 pH调节范围， 可以通过升高 pH值来降低对设备的腐蚀， 应用于更广的 CMP 领域。 4. In the chemical mechanical polishing method of the present invention, the chemical mechanical polishing liquid used has a wider pH adjustment range, and can lower the corrosion of equipment by raising the pH value, and is applied to a wider CMP field.
附图说明 DRAWINGS
图 1 实施例 6和传统 Fe-HA的化学机械抛光液中过氧化氢的分解速度 示意图。 Fig. 1 is a schematic view showing the decomposition rate of hydrogen peroxide in the chemical mechanical polishing liquid of Example 6 and conventional Fe-HA.
发明内容 Summary of the invention
制备实施例 表 1给出了本发明的化学机械抛光液实施例 1 ~ 24及对比例 1 ~ 2的配 方， 按表 1 中所列组分及其含量， 在去离子水中混合均匀， 用 PH调节剂调
到所需 PH值， 即可制得化学机械抛光液。 表 1本发明的化学机械抛光液实施例 1 ~ 24及对比例 1 ~ 2 Preparation Examples Table 1 shows the formulations of the chemical mechanical polishing liquids of Examples 1 to 24 and Comparative Examples 1 to 2 of the present invention, which are uniformly mixed in deionized water according to the components and contents thereof listed in Table 1, using PH Conditioning agent A chemical mechanical polishing solution can be prepared at the desired pH. Table 1 Chemical mechanical polishing liquid of the present invention Examples 1 to 24 and Comparative Examples 1 to 2
组分 组分 抑制 Component component inhibition
研磨剂 wt% wt% wt wt% 氧化剂 wt% PH Abrasives wt% wt% wt wt% oxidizer wt% PH
1 2 剂 1 2 dose
对比例 Comparative example
硅溶胶 1. 00% 双氧水 2 2. 5 Silica sol 1. 00% hydrogen peroxide 2 2. 5
1 1
对比例 硝酸 Comparative example
硅溶胶 1. 00% 0. 2 双氧水 2 2. 5 Silica sol 1. 00% 0. 2 hydrogen peroxide 2 2. 5
2 银 2 silver
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
硅溶胶 1. 00% 0. 2 0. 01 双氧水 2 2. 5 1 银 锰 Silica sol 1. 00% 0. 2 0. 01 hydrogen peroxide 2 2. 5 1 silver manganese
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
硅溶胶 1. 00% 0. 2 0. 02 双氧水 2 2. 5 2 银 锰 Silica sol 1. 00% 0. 2 0. 02 hydrogen peroxide 2 2. 5 2 silver manganese
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
硅溶胶 1. 00% 0. 2 0. 1 双氧水 2 2. 5 3 银 锰 Silica sol 1. 00% 0. 2 0. 1 hydrogen peroxide 2 2. 5 3 silver manganese
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
硅溶胶 1. 00% 0. 2 0. 1 双氧水 2 2. 5 4 银 铵 Silica sol 1. 00% 0. 2 0. 1 hydrogen peroxide 2 2. 5 4 silver ammonium
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
硅溶胶 1. 00% 0. 2 0. 5 双氧水 2 2. 5 5 银 钾 Silica sol 1. 00% 0. 2 0. 5 hydrogen peroxide 2 2. 5 5 silver potassium
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
硅溶胶 1. 00% 0. 2 0. 5 双氧水 2 2. 5 6 银 锰 Silica sol 1. 00% 0. 2 0. 5 hydrogen peroxide 2 2. 5 6 silver manganese
实施例 硫酸 Example sulfuric acid
硅溶胶 1. 00% 0. 2 双氧水 2 2. 5 7 银 Silica sol 1. 00% 0. 2 hydrogen peroxide 2 2. 5 7 silver
实施例 气相二 硫酸 EXAMPLES Gas phase disulfuric acid
0. 10% 0. 05 双氧水 0. 1 0. 5 8 氧化硅 银 0. 10% 0. 05 Hydrogen peroxide 0. 1 0. 5 8 Silica Silver
实施例 气相二 硝酸 硫酸 Examples Gas phase dinitrous acid sulfuric acid
0. 10% 0. 1 0. 005 双氧水 3 5 9 氧化硅 银 钾 0. 10% 0. 1 0. 005 Hydrogen peroxide 3 5 9 Silica Silver Potassium
实施例 气相二 硝酸 硫酸 Examples Gas phase dinitrous acid sulfuric acid
2. 00% 0. 15 0. 1 双氧水 4 2 10 氧化硅 银 铵 2. 00% 0. 15 0. 1 hydrogen peroxide 4 2 10 silica silver ammonium
实施例 硫酸 Example sulfuric acid
氧化铝 10. 00% 0. 2 双氧水 1 3 11 银 Alumina 10. 00% 0. 2 Hydrogen peroxide 1 3 11 Silver
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
氧化铝 6. 00% 0. 3 0. 5 双氧水 2 5 Alumina 6. 00% 0. 3 0. 5 Hydrogen peroxide 2 5
12 银 锌 12 silver zinc
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
氧化铝 4. 00% 0. 2 0. 1 双氧水 2 3 13 银 铵 Alumina 4. 00% 0. 2 0. 1 hydrogen peroxide 2 3 13 silver ammonium
实施例 硫酸 Example sulfuric acid
氧化铈 2. 00% 0. 2 双氧水 2 4 14 银 Cerium oxide 2. 00% 0. 2 hydrogen peroxide 2 4 14 silver
实施例 硝酸 硫酸 Examples Nitric acid Sulfuric acid
氧化铈 2. 00% 0. 2 0. 3 双氧水 5 4 15 银 钾 Cerium oxide 2. 00% 0. 2 0. 3 hydrogen peroxide 5 4 15 silver potassium
实施例 硝酸 硫酸 过硫酸 Examples Nitric acid Sulfuric acid Persulfuric acid
氧化铈 2. 00% 0. 3 0. 5 5 4 16 银 铵 铵 Cerium oxide 2. 00% 0. 3 0. 5 5 4 16 silver ammonium ammonium
实施例 硝酸 硫酸 单过硫 Examples nitric acid sulfuric acid monopersulfuric acid
硅溶胶 1. 00% 0. 2 0. 5 2 2. 5 17 银 钾 酸氢钾 Silica sol 1. 00% 0. 2 0. 5 2 2. 5 17 silver potassium potassium hydrogen hydride
实施例 气相二 硝酸 硫酸 Examples Gas phase dinitrous acid sulfuric acid
1. 30% 0. 2 0. 5 双氧水 1 2. 5 18 氧化硅 银 锰 1. 30% 0. 2 0. 5 hydrogen peroxide 1 2. 5 18 silica silver manganese
实施例 气相二 硝酸 硫酸 Examples Gas phase dinitrous acid sulfuric acid
1. 30% 0. 2 0. 5 双氧水 2 2. 5 19 氧化硅 银 锰 1. 30% 0. 2 0. 5 hydrogen peroxide 2 2. 5 19 silica silver manganese
实施例 气相二 1. 30% 硝酸 0. 2 硫酸 0. 5 EDTMP 0. 005 双氧水 2 2. 5
20 氧化硅 银 锰 The embodiment of the gas phase II 1. 30% nitric acid 0. 2 sulfuric acid 0. 5 EDTMP 0. 005 hydrogen peroxide 2 2. 5 20 silica silver manganese
实施例 气相二 硝酸 硫酸 Examples Gas phase dinitrous acid sulfuric acid
1.30% 0.2 0.5 EDTMP 0.01 双氧水 2 2.5 21 氧化硅 银 锰 1.30% 0.2 0.5 EDTMP 0.01 hydrogen peroxide 2 2.5 21 silica silver manganese
实施例 气相二 硝酸 硫酸 Examples Gas phase dinitrous acid sulfuric acid
1.30% 0.2 0.5 EDTMP 0.05 双氧水 2 2.5 22 氧化硅 银 锰 1.30% 0.2 0.5 EDTMP 0.05 hydrogen peroxide 2 2.5 22 silica silver manganese
实施例 氟化 硫酸 Examples Fluorinated sulfuric acid
硅溶胶 1.00% 0.2 0.2 双氧水 2 1.9 23 银 铵 Silica sol 1.00% 0.2 0.2 hydrogen peroxide 2 1.9 23 silver ammonium
实施例 高氯 硫酸 Examples High Chlorine Sulfuric Acid
硅溶胶 1.00% 0.2 0.2 双氧水 2 1.9 24 酸银 铵 效果实施例 1 Silica sol 1.00% 0.2 0.2 hydrogen peroxide 2 1.9 24 acid silver ammonium effect example 1
抛光条件： 抛光机台为 Logitech (英国） 1PM52型， polytex抛光垫， 4cmx4cm正方形晶圆 （Wafer), 研磨压力 4psi， 研磨台转速 70转 /分钟, 研磨头自转转速 150转 /分钟， 抛光液滴加速度 100 ml/分钟。 Polishing conditions: Polishing machine is Logitech (UK) 1PM52 type, polytex polishing pad, 4cmx4cm square wafer (Wafer), grinding pressure 4psi, grinding table rotation speed 70rev/min, grinding head rotation speed 150rev/min, polishing droplet Acceleration of 100 ml / min.
表 2用于钨抛光的实施例 1~ 7， 23, 24及对比例 1 ~2 Table 2 Examples for tungsten polishing 1~ 7, 23, 24 and comparative examples 1 ~ 2
对比例 2表明： 双氧水和硝酸银组合， 钨的抛光速度很低。 Comparative Example 2 shows that: in combination with hydrogen peroxide and silver nitrate, the polishing rate of tungsten is very low.
实施例 1 ~ 7, 23, 24表明： 在有硫酸根的存在下， 银离子、 硫酸根和 双氧水的组合， 能显著提高钨的抛光速度。 其中银离子可以来源于氟化银、 高氯酸银、 硫酸银、 以及硝酸银。
效果实施例 2 Examples 1 to 7, 23, 24 show that the combination of silver ions, sulfate groups and hydrogen peroxide in the presence of sulfate can significantly increase the polishing rate of tungsten. The silver ions may be derived from silver fluoride, silver perchlorate, silver sulfate, and silver nitrate. Effect Example 2
抛光条件： 8 英寸晶圆， IC1000抛光垫， 压力 4ps i。 Polishing conditions: 8 inch wafer, IC1000 polishing pad, pressure 4ps i.
表 3用于钨抛光的实施例 18和 19
表 3中的数据为本发明的化学机械抛光液实施例 18， 19在工业机台上 的钨抛光速率。结果表明本发明的化学机械抛光液在工业机台上可以实现非 常高的抛光速度。 效果实施例 3 Table 3 Examples 18 and 19 for tungsten polishing The data in Table 3 is the tungsten polishing rate of the chemical mechanical polishing liquid of Examples 18, 19 on the industrial machine of the present invention. The results show that the chemical mechanical polishing liquid of the present invention can achieve a very high polishing speed on an industrial machine. Effect Example 3
静态腐蚀速率测试： 将 wafer在室温下， 浸泡于抛光液中 30分钟测得。 Static Corrosion Rate Test: The wafer was immersed in a slurry for 30 minutes at room temperature.
表 4用于钨抛光的实施例 6及 14 ~ 16 Table 4 Examples 6 and 14 ~ 16 for tungsten polishing
表 3给出了对比例 3 ~ 16的配方， 按表 3中所列组分及其含量， 在去离 子水中混合均匀， 即可制得化学机械抛光液。 Table 3 shows the formulations of Comparative Examples 3 to 16. According to the components listed in Table 3 and their contents, they are uniformly mixed in the deionized water to prepare a chemical mechanical polishing liquid.
抛光条件： 抛光机台为 Log i tech (英囯） 1PM52型， polytex抛光垫， 4cm x 4cm正方形晶圆 （Wafer ), 研磨压力 4ps i， 研磨台转速 70转 /分钟， 研磨头自转转速 150转 /分钟， 抛光液滴加速度 100 ml /分钟。 Polishing conditions: Polishing machine is Log i tech (UK) 1PM52 type, polytex polishing pad, 4 cm x 4cm square wafer (Wafer), grinding pressure 4ps i, grinding table speed 70 rev / min, grinding head rotation speed 150 rpm /min, polishing droplet acceleration of 100 ml / min.
表 5对比例 5 ~ 18的化学机械抛光液 Table 5 Comparative chemical mechanical polishing solution of 5 ~ 18
对比例 14 Si02 1.5 Cr ( N03 ) 3 0.1 H202 2 176 Comparative Example 14 Si0 2 1.5 Cr ( N0 3 ) 3 0.1 H 2 0 2 2 176
对比例 15 Si02 1.5 RuCl3 0.1 H2O2 2 187 Comparative Example 15 Si0 2 1.5 RuCl 3 0.1 H2O2 2 187
对比例 16 Si02 1.5 肌 V03 0.1 H202 2 101 Comparative Example 16 Si0 2 1.5 Muscle V0 3 0.1 H 2 0 2 2 101
表 5列出了一些代表性的过渡金属元素。 从表 5中的结果可以看出， 不 是任意的过渡金属和双氧水的组合， 就能够实现本发明的效果（实现很高的 钨抛光速率）。 对比例 4， 8, 9 同时也表明： 不是任意金属硫酸盐就能够实 现本发明的效果。 作为对比， 本发明中的银离子和硫酸根结合在一起（包括 硫酸银自身）却可实现非常高的抛光速度， 是非显而易见的。 对比实施例 2 Table 5 lists some representative transition metal elements. As can be seen from the results in Table 5, the effect of the present invention (achieving a high tungsten polishing rate) can be achieved without a combination of any transition metal and hydrogen peroxide. Comparative Examples 4, 8, 9 also show that the effect of the present invention can be achieved without any metal sulfate. In contrast, the combination of silver ions and sulfate in the present invention (including silver sulfate itself) achieves a very high polishing rate, which is not obvious. Comparative Example 2
表 6给出了对比例 17 ~ 19的配方， 按表 6中所列组分及其含量， 在去 离子水中混合均匀， 即可制得化学机械抛光液。 Table 6 shows the formulations of Comparative Examples 17 to 19, which were prepared by mixing them in deionized water according to the components listed in Table 6 and their contents, to prepare a chemical mechanical polishing solution.
抛光条件: 抛光机台为 Logitech (英国） 1PM52型， polytex抛光垫， 4cmx4cm正方形晶圆 (Wafer), 研磨压力 4psi, 研磨台转速 70转 /分钟， 研磨头自转转速 150转 /分钟， 抛光液滴加速度 100 ml/分钟。 Polishing conditions: Polishing machine is Logitech (UK) 1PM52 type, polytex polishing pad, 4cmx4cm square wafer (Wafer), grinding pressure 4psi, grinding table rotation speed 70rev/min, grinding head rotation speed 150rev/min, polishing droplet Acceleration of 100 ml / min.
表 6对比例 17~19的化学机械抛光液 Table 6 Comparative chemical mechanical polishing solution of 17~19
Claims
权利要求 、 一种化学机械抛光液， 其含有： 激发剂， 强氧化剂前体（precursor ), 研磨剂和水。 Claims: A chemical mechanical polishing liquid comprising: an activator, a strong oxidant precursor, an abrasive, and water.
、 根据权利要求 1所述的抛光液， 所述的激发剂为由银离子和氧化剂组成 的组合物。 The polishing liquid according to claim 1, wherein the activator is a composition composed of silver ions and an oxidizing agent.
、 根据权利要求 2所述的抛光液， 所述的银离子来自于银盐。 The polishing liquid according to claim 2, wherein the silver ions are derived from a silver salt.
、 根据权利要求 3所述的抛光液， 所述银盐为氟化银、 高氯酸银、 硫酸银 和 /或硝酸银。 The polishing liquid according to claim 3, wherein the silver salt is silver fluoride, silver perchlorate, silver sulfate, and/or silver nitrate.
、 根据权利要求 3所述的抛光液， 所述的银盐重量百分比 0. 05% ~ 0. 3%。 、 根据权利要求 2所述的抛光液， 所述的氧化剂为过氧化物。 The 5% by weight of the silver salt is 0. 05% ~ 0. 3%. The polishing liquid according to claim 2, wherein the oxidizing agent is a peroxide.
、 根据权利要求 6所述的抛光液， 所述的过氧化物为过氧化氢、 过硫酸铵 和 /或单过硫酸钾中的一种或多种。 The polishing liquid according to claim 6, wherein the peroxide is one or more of hydrogen peroxide, ammonium persulfate and/or potassium monopersulfate.
、 根据权利要求 2所述的抛光液， 所述的氧化剂的重量百分比为 0. 1 - 5%。 、 根据权利要求 1所述的抛光液， 所述的强氧化剂前体（precursor )为非 硝酸根阴离子。5%。 By weight of the oxidizing agent is 0. 1 - 5%. The polishing liquid according to claim 1, wherein said strong oxidant precursor is a non-nitrate anion.
0、 根据权利要求 9所述的抛光液， 所述的非硝酸根阴离子为硫酸根离子。1、 根据权利要求 10所述的抛光液， 所述的硫酸根离子来自于硫酸盐。The polishing liquid according to claim 9, wherein the non-nitrate anion is a sulfate ion. 1. The polishing liquid according to claim 10, wherein the sulfate ion is derived from a sulfate.
2、 根据权利要求 11所述的抛光液， 所述的硫酸盐为非金属硫酸盐。2. The polishing liquid according to claim 11, wherein the sulfate is a non-metal sulfate.
3、 根据权利要求 12所述的抛光液， 所述的非金属硫酸盐为硫酸铵。3. The polishing liquid according to claim 12, wherein the non-metal sulfate is ammonium sulfate.
4、 根据权利要求 11所述的抛光液， 所述的硫酸盐为金属硫酸盐。4. The polishing liquid according to claim 11, wherein the sulfate is a metal sulfate.
5、 根据权利要求 14所述的抛光液， 所述的金属硫酸盐为硫酸锰、 硫酸钾 和 /或硫酸锌中的一种或多种。 、根据权利要求 1所述的抛光液，所述的研磨剂为气相二氧化硅、硅溶胶、 氧化铝和 /或氧化铈中的一种或多种。 5. The polishing liquid according to claim 14, wherein the metal sulfate is one or more of manganese sulfate, potassium sulfate, and/or zinc sulfate. The polishing liquid according to claim 1, wherein the abrasive is one or more selected from the group consisting of fumed silica, silica sol, alumina, and/or cerium oxide.
、根据权利要求 1所述的抛光液，所述的研磨剂的重量百分比为 0. 1 ~ 10%。 、 根据权利要求 1所述的抛光液， 还含有 pH调节剂。 1 至 10%。 By weight of the polishing agent is 0. 1 ~ 10%. The polishing liquid according to claim 1, further comprising a pH adjuster.
、 根据权利要求 1所述的抛光液， 所述的抛光液的 pH值为 0. 5 ~ 5。 5至五。 The pH of the slurry is 0. 5 ~ 5.
、根据权利要求 1所述的抛光液，还含有静态腐蚀速度（ s tat ic etch rate ) 抑制剂。 The polishing liquid according to claim 1, further comprising a s tat ic etch rate inhibitor.
、 根据权利要求 20所述的抛光液， 所述的静态腐蚀速度抑制剂为有机膦 化合物。 The polishing liquid according to claim 20, wherein said static corrosion rate inhibitor is an organic phosphine compound.
、 根据权利要求 21所述的抛光液， 所述的有机膦化合物为乙二胺四甲叉 膦酸（ EDTMP )。 The polishing liquid according to claim 21, wherein the organic phosphine compound is ethylenediaminetetramethylene phosphonic acid (EDTMP).
、根据权利要求 20所述的抛光液，所述的静态腐蚀速度（s tat ic etch rate ) 抑制剂的重量百分比为 0. 005 - 0. 05%。 005 - 0. 05%。 The weight percentage of the inhibitor is 0. 005 - 0. 05%.
、 一种用于钨化学机械抛光方法， 其特征在于： 将根据权利要求 1-22 中 任一项所述的抛光液用于钨化学机械抛光。 A method for chemical polishing of tungsten, characterized in that the polishing liquid according to any one of claims 1 to 22 is used for chemical mechanical polishing of tungsten.
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| CN105729065A (en) * | 2016-03-16 | 2016-07-06 | 芜湖东光大华机械制造有限公司 | Surface treatment process for flywheel production |
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| WO2011054193A1 (en) * | 2009-11-06 | 2011-05-12 | Wang Chen | Chemical-mechanical polishing liquid |
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| CN1629238A (en) * | 2003-11-13 | 2005-06-22 | Cmp罗姆和哈斯电子材料控股公司 | Compositions and methods for polishing copper |
| CN1721493A (en) * | 2004-02-23 | 2006-01-18 | Cmp罗姆和哈斯电子材料控股公司 | Multiple process polishing solution for chemical mechanical planarization |
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