WO2011072494A1 - 一种化学机械抛光液 - Google Patents
一种化学机械抛光液 Download PDFInfo
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- WO2011072494A1 WO2011072494A1 PCT/CN2010/002065 CN2010002065W WO2011072494A1 WO 2011072494 A1 WO2011072494 A1 WO 2011072494A1 CN 2010002065 W CN2010002065 W CN 2010002065W WO 2011072494 A1 WO2011072494 A1 WO 2011072494A1
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- Prior art keywords
- acid
- polishing liquid
- liquid according
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- amino
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 13
- 239000001257 hydrogen Substances 0.000 description 13
- 229910052739 hydrogen Inorganic materials 0.000 description 13
- 229910021529 ammonia Inorganic materials 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000003852 triazoles Chemical class 0.000 description 3
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229940009098 aspartate Drugs 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 125000003831 tetrazolyl group Chemical group 0.000 description 2
- WRFPVMFCRNYQNR-UHFFFAOYSA-N 2-hydroxyphenylalanine Chemical compound OC(=O)C(N)CC1=CC=CC=C1O WRFPVMFCRNYQNR-UHFFFAOYSA-N 0.000 description 1
- GUOVBFFLXKJFEE-UHFFFAOYSA-N 2h-benzotriazole-5-carboxylic acid Chemical compound C1=C(C(=O)O)C=CC2=NNN=C21 GUOVBFFLXKJFEE-UHFFFAOYSA-N 0.000 description 1
- OPGUZRRLMQSMAQ-UHFFFAOYSA-N 5-(4-methoxyphenyl)-1-phenylbenzimidazole Chemical compound C1=CC(OC)=CC=C1C1=CC=C(N(C=N2)C=3C=CC=CC=3)C2=C1 OPGUZRRLMQSMAQ-UHFFFAOYSA-N 0.000 description 1
- GDGIVSREGUOIJZ-UHFFFAOYSA-N 5-amino-3h-1,3,4-thiadiazole-2-thione Chemical compound NC1=NN=C(S)S1 GDGIVSREGUOIJZ-UHFFFAOYSA-N 0.000 description 1
- HHDRWGJJZGJSGZ-UHFFFAOYSA-N 5-benzyl-2h-tetrazole Chemical compound C=1C=CC=CC=1CC=1N=NNN=1 HHDRWGJJZGJSGZ-UHFFFAOYSA-N 0.000 description 1
- XZGLNCKSNVGDNX-UHFFFAOYSA-N 5-methyl-2h-tetrazole Chemical compound CC=1N=NNN=1 XZGLNCKSNVGDNX-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- HAKFWHINKUNSIR-UHFFFAOYSA-N CP(O)(O)=O.[O] Chemical compound CP(O)(O)=O.[O] HAKFWHINKUNSIR-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 229940120146 EDTMP Drugs 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000005819 Potassium phosphonate Substances 0.000 description 1
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- DQPBABKTKYNPMH-UHFFFAOYSA-N amino hydrogen sulfate Chemical compound NOS(O)(=O)=O DQPBABKTKYNPMH-UHFFFAOYSA-N 0.000 description 1
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- LOGBRYZYTBQBTB-UHFFFAOYSA-N butane-1,2,4-tricarboxylic acid Chemical compound OC(=O)CCC(C(O)=O)CC(O)=O LOGBRYZYTBQBTB-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000021523 carboxylation Effects 0.000 description 1
- 238000006473 carboxylation reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- XQRLCLUYWUNEEH-UHFFFAOYSA-N diphosphonic acid Chemical compound OP(=O)OP(O)=O XQRLCLUYWUNEEH-UHFFFAOYSA-N 0.000 description 1
- YXXXKCDYKKSZHL-UHFFFAOYSA-M dipotassium;dioxido(oxo)phosphanium Chemical compound [K+].[K+].[O-][P+]([O-])=O YXXXKCDYKKSZHL-UHFFFAOYSA-M 0.000 description 1
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
- 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 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- QCHWBGRKGNYJSM-UHFFFAOYSA-N ethene Chemical group C=C.C=C.C=C QCHWBGRKGNYJSM-UHFFFAOYSA-N 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- ZWLPBLYKEWSWPD-UHFFFAOYSA-N o-toluic acid Chemical compound CC1=CC=CC=C1C(O)=O ZWLPBLYKEWSWPD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 229930015704 phenylpropanoid Natural products 0.000 description 1
- 150000002995 phenylpropanoid derivatives Chemical class 0.000 description 1
- PTMHPRAIXMAOOB-UHFFFAOYSA-L phosphoramidate Chemical compound NP([O-])([O-])=O PTMHPRAIXMAOOB-UHFFFAOYSA-L 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- KYKNRZGSIGMXFH-ZVGUSBNCSA-M potassium bitartrate Chemical compound [K+].OC(=O)[C@H](O)[C@@H](O)C([O-])=O KYKNRZGSIGMXFH-ZVGUSBNCSA-M 0.000 description 1
- 239000001472 potassium tartrate Substances 0.000 description 1
- 229940111695 potassium tartrate Drugs 0.000 description 1
- 235000011005 potassium tartrates Nutrition 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- YPPQYORGOMWNMX-UHFFFAOYSA-L sodium phosphonate pentahydrate Chemical compound [Na+].[Na+].[O-]P([O-])=O YPPQYORGOMWNMX-UHFFFAOYSA-L 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- VXKWYPOMXBVZSJ-UHFFFAOYSA-N tetramethyltin Chemical compound C[Sn](C)(C)C VXKWYPOMXBVZSJ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- ZJHHPAUQMCHPRB-UHFFFAOYSA-N urea urea Chemical compound NC(N)=O.NC(N)=O ZJHHPAUQMCHPRB-UHFFFAOYSA-N 0.000 description 1
- 238000001039 wet etching Methods 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
- 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
-
- 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.
- 5,527,423 discloses a A chemical mechanical polishing slurry of a metal layer
- US Pat. No. 6,821,897 discloses a method of copper CMP using a polymer complexing agent
- Patent No. CN 02114147.9 discloses a copper chemical-mechanical polishing process polishing liquid
- No. CN 01818940.7 discloses a slurry for chemical mechanical polishing of copper
- No. CN 98120987.4 discloses a CMP slurry manufacturing process for copper and a manufacturing method for an integrated circuit.
- an acidic polishing pad cleaning solution to remove copper residue after polishing.
- polishing slurries especially those with a higher pH, are often incompatible with the polishing pad cleaning solution, resulting in a lower copper removal rate after using the cleaning solution. Therefore, it is necessary to develop a new chemical mechanical polishing slurry for copper.
- the technical problem to be solved by the present invention is that the chemical mechanical polishing liquid for polishing copper is incompatible with the polishing pad cleaning solution, resulting in a decrease in the removal rate of copper, thereby providing a high retention after using the polishing pad cleaning solution.
- Chemical mechanical polishing solution for copper removal rate is incompatible with the polishing pad cleaning solution, resulting in a decrease in the removal rate of copper, thereby providing a high retention after using the polishing pad cleaning solution.
- the chemical mechanical polishing liquid of the present invention contains abrasive particles, a corrosion inhibitor, an oxidizing agent, water and at least two complexing agents.
- the two complexing agents are amino group-containing compounds and salts thereof, and organic acids and salts thereof.
- the salt is selected from one or more of a potassium salt, a sodium salt and/or an ammonium salt.
- the amino group-containing compound is an amino acid and/or a polyamine.
- the amino acid is selected from the group consisting of glycine, alanine, valine, leucine, valine, phenylalanine, methionine, threonine, tyrosine, tryptophan, lysine
- glycine alanine
- valine leucine
- valine leucine
- valine phenylalanine
- methionine threonine
- tyrosine tryptophan
- lysine One or more of arginine, histidine, serine, aspartic acid, glutamic acid, asparagine and/or glutamine.
- the polyamine is selected from one of r ethylenediamine, diethylenetriamine, pentamethyldiethylenetriamine, triethylenetetramine, tetraethylenepentamine, and/or polyethenepolyamine or A variety.
- the organic acid is an organic carboxylic acid and/or an organic phosphonic acid.
- the organic carboxylic acid is selected from the group consisting of acetic acid, oxalic acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid, lactic acid, maleic acid, gallic acid and/or sulfosalicylic acid. One or more.
- the organic phosphonic acid is selected from the group consisting of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid, aminotrimethylene phosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediamine tetramethylene phosphonic acid Or one or more of diethylenetriamine pentamethylphosphonic acid, 2-hydroxyphosphonic acid acetic acid, and/or polyaminopolyether methylphosphonic acid.
- the amino group-containing compound and the salt thereof are contained in an amount of 0.01 to 10% by mass.
- the organic acid and the salt thereof are contained in an amount of 0.01 to 3% by mass.
- the oxidizing agent is selected from the group consisting of hydrogen peroxide, urea peroxide, peroxyformic acid, peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, perboric acid, potassium permanganate. And / or one or more of ferric nitrate.
- the oxidizing agent has a mass percentage of 0.01 - 10%.
- the abrasive particles are selected from the group consisting of silica, alumina, aluminum-doped silica, aluminum-coated silica, ceria, titania, and/or polymer abrasive particles. kind or more.
- the abrasive particles have a mass percentage of 0.1 to 5%.
- the abrasive particles have a particle diameter of 20 to 150 nm.
- the corrosion inhibitor is one or more selected from the group consisting of azole, imidazole, thiazole, pyridine and/or pyrimidine.
- the azole compound is selected from the group consisting of benzotriazole, 5-methyl-1,2,3-benzotriazole, 5-carboxybenzotriazole, 1-hydroxy-one Benzotriazole, 1, 2, 4-triazole, 3-amino-1, 2,4-triazole, 4-amino-1, 2,4-triazole, 3, 5-diamino -1, 2, 4-triazole, 5-carboxy-3-amino-1, 2,4-triazole, 3-amino-5-mercapto-1, 2,4-triazole, 5-acetic acid -1H-tetrazole, 5-methyltetrazole, 5-phenyltetrazolium, 5-amino-1H-tetrazole and/or 1-phenyl-5-anthracene One or more of benzyl-tetrazole.
- the imidazole compound is benzimidazole and/or 2-mercaptobenzimidazole.
- the thiazole compound is selected from the group consisting of 2-mercapto-benzothiazole, 2-mercaptothiadiazole and/or 5-amino-2-mercapto-1,3,4-thiadiazole. Or a variety.
- the pyridine is one or more selected from the group consisting of 2,3-diaminopyridine, 2-aminopyridine and/or 2-pyridinecarboxylic acid.
- the pyrimidine is a 2-aminopyrimidine.
- the corrosion inhibiting mass percentage is 0.001 to 5%.
- the polishing liquid of the invention has a pH of 4 to 11, preferably 5 to 8.
- the polishing liquid of the present invention may further contain one or more other conventional additives in the art such as a pH adjuster, a viscosity modifier, an antifoaming agent and/or a bactericide.
- the polishing liquid of the present invention can be prepared by concentration as needed, diluted with deionized water and mixed with an oxidizing agent before use.
- the reagents and starting materials used in the present invention are commercially available.
- a positive development of the present invention is that a high polishing rate can be maintained after the polishing pad cleaning solution is used.
- Table 1 shows Examples 1 to 24 of the chemical mechanical polishing liquid of the present invention. According to the formulation given in the table, the components other than the oxidizing agent were uniformly mixed, and the mass percentage was made up to 100% with water. Adjust to the desired pH with KOH or 1 ⁇ 0 3 . Add oxidizing agent before use and mix well. Table 1 Chemical mechanical polishing liquid of the present invention Examples 1 to 24 Solid abrasive particle corrosion inhibitor First complexing agent First-two complexing agent Oxidation PH
- Sulfuric acid hinge 24 5 polymethyl propylene 0.5 5-methyl four gas 0.05 diethyl 0.01 oxalic acid hinge 3 over 8 acid carbazole ene oxide
- Table 2 shows the preparation examples of the comparative polishing liquids 1 to 2 and the polishing liquids 25 to 28 of the present invention. According to the formulation given in Table 2, the mass percentage is made up to 100% with water, and the oxidizing agent is The other components were mixed well and adjusted to the desired pH with KOH or HNO 3 . Add oxidizing agent before use, and mix and tick.
- the copper (Cu) wafer was polished using the polishing liquids of Comparative Examples 1 to 2 and the polishing liquids of Examples 25 to 28 of the present invention, and the removal rates are shown in Table 3.
- Polishing material Empty copper wafer; Polishing conditions: Downforce 3Psi, polishing disc and polishing head speed 70/80rpm, polishing pad PPG MX710, polishing liquid flow rate 100ml/min, polishing machine for Logitech PM5 Polisher o;
- Polishing pad cleaning After cleaning with 25 ml of polishing pad cleaning solution (1% citric acid), rinse the polishing pad with 1 liter of deionized water.
- the polishing pad is used in comparison with the comparative examples 1 to 2 in which the second complexing agent is not added. After the cleaning solution, the copper removal rate is greatly reduced. However, when the second complexing agent of different concentrations is added to the polishing liquid of Examples 25 to 28 of the present invention, the removal rate of copper is substantially unchanged, and the removal rate of copper can be maintained even after the polishing pad cleaning solution is used. .
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Description
一种化学机械抛光液 技术领域
本发明涉及一种化学机械抛光液。
技术背景
随着微电子技术的发展,甚大规模集成电路芯片集成度己达几十亿个元 器件, 特征尺寸已经进入纳米级, 这就要求微电子工艺中的几百道工序, 尤 其是多层布线、衬底、 介质必须要经过化学机械平坦化。 甚大规模集成布线 正由传统的 A1向 Cu转化。与 A1相比, Cu布线具有电阻率低, 抗电迁移能 率高, RC延迟时间短, Cu布线的优势已使其替代 A1成为半导体制作中的 互联金属。
但是目前还没有对铜材进行有效地等离子蚀刻或湿法蚀刻, 以使铜互连 在集成电路中充分形成的公知技术, 因此铜的化学 械抛光方法被认为是最 有效的工艺方法。铜的化学机械抛光方法的工作原理一般是先用快且高效的 去除速率除去衬底表面上大量的铜, 当快要接近阻挡层时即软着陆, 降低去 除速率抛光剩余的金属铜并停在阻挡层。 目前, 出现了一系列的适合于抛光 Cu的化学机械抛光浆料, 如: 专利号为 US 6,616,717公开了一种用于金属 CMP的组合物和方法; 专利号为 US 5,527,423公开了一种用于金属层的化 学机械抛光浆料;专利号为 US 6,821,897公开了一种使用聚合体络合剂的铜 CMP的方法;专利号为 CN 02114147.9公开了一种铜化学一机械抛光工艺用 抛光液; 专利号为 CN 01818940.7公开了铜的化学机械抛光所用的浆料; 专
利号为 CN 98120987.4公开了一种用于铜的 CMP浆液制造以及用于集成电 路的制造方法。但是使用铜的抛光过程中由于铜的去除较多, 常常会残留在 抛光垫上, 影响抛光性能, 因此需要在抛光后使用酸性的抛光垫清洗液来去 除铜的残留。 但抛光浆料, 特别是 pH值较高的抛光浆料往往与抛光垫清洗 液不相容, 导致使用清洗液后铜的去除速率降低。 因此有必要开发出新的用 于铜的化学机械抛光浆料。
发明概要
本发明所要解决的技术问题是用于抛光铜的化学机械抛光液与抛光垫 清洗液不相容, 导致铜的去除速率降低, 从而提供一种在使用抛光垫清洗液 后也能保持较高的铜去除速率的化学机械抛光液。
本发明的化学机械抛光液, 含有研磨颗粒, 腐蚀抑制剂, 氧化剂, 水和 至少两种络合剂。
本发明中, 所述的两种络合剂为含氨基的化合物及其盐和有机酸及其 盐。 所述的盐选自钾盐、 钠盐和 /或铵盐中的一种或多种。
本发明中, 所述的含氨基的化合物为氨基酸和 /或多胺。
本发明中, 所述的氨基酸选自甘氨酸、 丙氨酸、 缬氨酸、 亮氨酸、 脯氨 酸、 苯丙氨酸、 蛋氨酸、 苏氨酸、 酪氨酸、 色氨酸、 赖氨酸、 精氨酸、 组氨 酸、 丝氨酸、 天冬氨酸、 谷氨酸、 天冬酰胺和 /或谷氨酰胺中的一种或多种。
本发明中, 所述的多胺选自 r乙二胺、 二乙烯三胺、 五甲基二乙烯三胺、 三乙烯四胺、 四乙烯五胺和 /或多乙烯多胺中的一种或多种。
本发明中, 所述的有机酸为有机羧酸和 /或有机膦酸。
本发明中, 所述的有机羧酸选自醋酸、草酸、柠檬酸、酒石酸、丙二酸、 丁二酸、苹果酸、乳酸、马来酸、没食子酸和 /或磺基水杨酸中的一种或多种。
本发明中, 所述的有机膦酸选自 2-膦酸丁烷 -1, 2, 4-三羧酸、氨基三甲 叉膦酸、 羟基乙叉二膦酸、 乙二胺四甲叉膦酸、 二乙烯三胺五甲叉膦酸、 2- 羟基膦酸基乙酸和 /或多氨基多醚基甲叉膦酸中的一种或多种。
本发明中,所述的含氨基的化合物及其盐的质量百分含量为 0.01〜10%。 本发明中, 所述的有机酸及其盐的质量百分含量为 0.01〜3%。
本发明中, 所述的氧化剂选自过氧化氫、 过氧化脲、 过氧甲酸、 过氧乙 酸、 过硫酸盐、 过碳酸盐、 高碘酸、 高氯酸、 高硼酸、 高锰酸钾和 /或硝酸铁 中的一种或多种。 所述的氧化剂的质量百分含量为 0.01 -10 %。
本发明中, 所述的研磨颗粒选自二氧化硅、 三氧化二铝、 掺杂铝的二氧 化硅、覆盖铝的二氧化硅、二氧化铈、二氧化钛和 /或高分子研磨颗粒中的一 种或多种。 所述的研磨颗粒的质量百分含量为 0.1 ~5 %。 所述的研磨颗粒的 粒径为 20~150nm。
本发明中, 所述的腐蚀抑制剂选自氮唑、咪唑、噻唑、吡啶和 /或嘧啶类 化合物中的一种或多种。
本发明 '中, 所述的氮唑类化合物选自苯并三氮唑、 5-甲基 -1, 2, 3-苯并 三氮唑、 5-羧基苯并三氮唑、 1-羟基一苯并三氮唑、 1, 2, 4-三氮唑、 3-氨 基 -1, 2, 4-三氮唑、 4-氨基 -1, 2, 4-三氮唑、 3, 5-二氨基 -1, 2, 4-三氮唑、 5-羧基 -3-氨基 -1, 2, 4-三氮唑、 3-氨基 -5-巯基 -1, 2, 4-三氮唑、 5-乙酸 -1H- 四氮唑、 5-甲基四氮唑、 5-苯基四氮唑、 5-氨基 -1H-四氮唑和 /或 1-苯基 -5-巯
基 -四氮唑中的一种或多种。
本发明中, 所述的咪唑类化合物为苯并咪唑和 /或 2-巯基苯并咪唑。
本发明中,所述的噻唑类化合物选自 2-巯基 -苯并噻唑、 2-巯基噻二唑和 /或 5-氨基 -2-巯基 -1, 3, 4-噻二唑中的一种或多种。 本发明中, 所述的吡啶选自 2, 3-二氨基吡啶、 2-氨基吡啶和 /或 2-吡啶 甲酸中的一种或多种。
本发明中, 所述的嘧啶为 2-氨基嘧啶。 本发明中, 所述的腐蚀抑制的质量百分含量为 0.001~5%。
发明的抛光液, pH为 4〜11, 较佳地为 5~8。 本发明的抛光液中,还可以含有本领域其他常规添加剂,如 pH调节剂、 粘度调节剂、 消泡剂和 /或杀菌剂中的一种或多种。
本发明的抛光液可根据需要浓缩制备,使用前用去离子水稀释并加入氧 化剂混合均匀。 本发明所用试剂及原料均市售可得。 本发明的积极进步效果在于:可在使用抛光垫清洗液后仍保持较高的抛 光速率。
发明内容
制备实施例 1
下面用实施例来进一步说明本发明, 但本发明并不受其限制。
表 1给出了本发明的化学机械抛光液的实施例 1~24, 按表中所给配方, 将除氧化剂以外的其他组分混合均匀,用水补足质量百分比至 100%。用 KOH 或 1^03调节到所需要的 pH值。 使用前加氧化剂, 混合均匀即可。
表 1本发明的化学机械抛光液实施例 1~24 实 研磨颗粒 腐蚀抑制剂 第一络合剂 第-二络合剂 氧化 PH 施 剂
例
含量 具体物质 含量 具体物质 含量 具体 含量 具体物质 含量 具 wt% wt% wt% 物质 wt% wt% 体
物 质
1 3 Si02 5 4-氨基 10 甘氨 0.5 草酸 0.05 过 4
(20nm) -1,2,4-三氮 酸 硫
唑 酸
铵
2 2 Si02 0.0005 苯并三氮唑 0.01 甘氨 0.01 丁二酸 5 过 5
(35nm) 酸 氧
甲 酸
3 1 Si02 0.005 5-氨基 -1H- 0.8 丙氨 0.1 丙二酸 3 5
(45nm) 四氮唑 酸 锰
酸 钾
4 1.5 Si02 2 1,2,4-三氮 1 缬氨 0.2 苹果酸 0.5 硝 5
(50nm) 唑 酸 酸
铁
5 1 Si02 0.02 1-苯基 -5-巯 1 0.3 乳酸 5 过 6
(60nm) 基-四氮唑 酸 氧
化 脲 .
6 1 '■ Si02 0.01 2-巯基 -苯并 2 色氨 0.5 没食子酸 8 高 6
(70nm) 噻唑 酸 碘
酸
7 1 Si02 0.5 2,3-二氨基 3 蛋氨 0.5 磺基水杨 10 过 7
(70nm) 吡啶 酸 酸 氧
乙 酸
8 0.5 A1203 0.5 2-吡啶甲酸 3 天冬 0.5 醋酸 1 过 7
(30nm) 氨酸 氧
化 氢
9 0.1 Ce02 0.001 5-羧基苯并 2 苯丙 0.2 柠檬酸铰 5 过 8
(50nm) 三氮唑 氨酸 氧
乙 酸
10 0.5 Ti02 0.005 苯并咪唑 2 苏氨 0.2 酒石酸钾 0.5 过 9
(120nm) 酸 硫
酸 钾
11 1 Si02 5-苯基四氮 2 天冬 0.2 2-膦酸丁 3 过 6
(150 唑 酰胺 焼基 氧
-1,2,4-三 化 羧酸 氢
2 Si02 0.08 2-巯基苯并 2 丝氨 0.8 乙二胺四 4 过 6
(80nm) 咪唑 酸 亚甲基膦 氧
酸 化
氢
1.2 Si02 0.5 5-乙酸 -1H- 2 精氣 0.5 二乙烯三 2.5 过 6
(lOOnm) 四氮唑 酸 胺五甲叉 氧
- 膦酸 化
氢
0.5 Si02 1 2-巯基噻二 2 1.5 羟基亚乙 3.5 过 7
(70nm) 唑 酸 基二膦酸 碳
酸 钠
0.6 Si02 2 2-氨基嘧啶 2 组氨 0.8 氨基三亚 4.5 过 5
(80nm) 酸 甲基膦酸 氧
化 氢
0.5 Si02 1 2-氨基吡啶 0.05 五甲 1 2-羟基膦 0.8 过 9
(lOOnm) 基二 酸基乙酸 氧
乙烯 化 三胺 氢
0.5 Si02 0.02 5-甲基 1,2,3- 0.1 多乙 0.05 多氨基多 0.8 过 . 10
(lOOnm) 苯并三氮唑 烯多 醚基亚甲 氧
胺 基膦酸 化
氢
0.3 Si02 0.2 3-氨基 -5-巯 · 1 三乙 0.5 二乙烯三 3 过 11
(lOOnm) 基 -1,2,4-三 烯四 胺五甲叉 t
氮唑 胺 膦酸钾 化
氢
0.5 Si02 0.5 5-氨基 -2-巯 3 四乙 2 酒石酸铰 0.1 9
(lOOnm) 基 -1,3,:4 -噻 烯五 硼
二 (½ ' 胺 酸
0.5 掺杂铝的 0.6 3-氨基 1 谷氨 3 草酸钾 3 过 7
Si02 -1,2,4-三氮 酰胺 氧
(20nm) 唑
酸
1 覆盖铝的 0.001 5-羧基 -3-氨 10 乙二 2 马来酸 5 过 8
Si02 基 -1,2,4-三 胺 氧
(70 氮唑 化
0.01 苯并三氮唑 氢
4 聚苯^烯 0. 5 3, 5-二氨基 1 脯氨 0.5 马来酸 7 局 8
(120 - 1, 2, 4-三 酸 氣
氮唑 2 酪氨 酸
酸
2 Si02 0.5 1-羟基一苯 5 甘氨 1 二乙烯三 1 过 6
(70nm) 并三氮唑 酸 胺五甲叉 氧
膦酸钠 化
氢
0.01 过
硫 酸 铰
24 5 聚甲基丙烯 0.5 5-甲基四氣 0.05 二乙 0.01 草酸铰 3 过 8 酸甲酯 唑 烯三 氧
(150nm) 胺 化
氢 添加剂(wt%) 甲基纤维素 (0.01%) 聚硅垸消泡剂
(0.01%)
制备实施例 2 表 2给出了对比抛光液 1〜2和本发明的抛光液 25〜28的制备实施例, 按表 2中所给配方, 用水补足质量百分比至 100%, 将除氧化剂以外的其他 组分混合均匀, 用 KOH或 HN03调节到所需要的 pH值。使用前加氧化剂, 混合均勾即可。
¾ 2 本发明的化学机械抛光液实施例 25〜28以及对比例 1〜2 抛
光 研磨颗粒 第一络合剂 第:二络合剂 腐蚀抑制剂 氧化剂 pH 液
具体物质 具 具 含量 含量 体 含量 含量 具体物 含量 体 wt% 具体物质
wt% 物 wt% wt% 质 wt% 物
质 质 对 过
Si02 甘 4-氨基
比 0.5 0.7 氧
氨 0.1 -1, 2, 4- 2.3 5 (60nm)
例 1 化
酸
氢 对 乙 过
Si02
比 0.5 0.5 苯并三
0.005 氧
1 8 例 2 ( lOOnm) 氮唑 化
氢 胺
实 过
Si02 甘 4-氨基
施
0.5 0.7 氨 0.2 氧
草酸铵 0.1 -1, 2, 4- 2.3 5 例 (60nm) 化
25 酸 三氮唑
氢 实 过 施 Si02 甘 2-膦酸丁垸
0.5 0.7 氨 0.15 基 -1,2,4-三 0.1 氧
-1, 2, 4- 2.3 5 例 (60nm)
羧酸 化
26 酸 三氮唑
一
实 过
乙
施 Si02
0.5 苯并三
0.5 氧
炼 0.1 丙二酸 0.005 1 8 例 ( lOOnm) 氮唑 化
27
胺
实 过 施 Si02 乙 二乙稀三
苯并三
0.5 0.5 0.1 氧
胺五甲叉 0.005 1 8 例 ( lOOnm) 氮唑 化
膦酸钾
28 氢
胺 效果实施例
采用对比例 1〜2的抛光液和本发明实施例 25〜28 的抛光液对空片铜 (Cu) 晶片进行抛光, 去除速率见表 3。 抛光材料: 空片铜晶片; 抛光条件: 下压力 3Psi, 抛光盘及抛光头转速 70/80rpm,抛光垫 PPG MX710,抛光液流速 100ml/min,抛光机台为 Logitech PM5 Polisher o;
抛光垫清洗: 25毫升抛光垫清洗液(1%柠檬酸)清洗后, 再用 1升去 离子水清洗抛光垫。
表 3 对比例 1〜2和实施例 25〜28抛光液对金属铜的去除速率
由表 3可见, 与未添加第二络合剂的对比例 1〜2相比, 在使用抛光垫
清洗液后, 铜的去除速率大幅度降低。 而本发明的实施例 25〜28的抛光液 中添加了不同浓度的第二络合剂后, 铜的去除速率基本不变, 而且在使用抛 光垫清洗液后也能保持铜的去除速率不变。
Claims
1、根据权利要求 2所述的抛光液, 所述的有机酸及其盐的质量百分含量为 0.01〜3%。
2、根据权利要求 1所述的抛光液,所述的氧化剂选自过氧化氢、过氧化脲、 过氧甲酸、 过氧乙酸、 过硫酸盐、 过碳酸盐、 高碘酸、 高氯酸、 高硼酸、 高锰酸钾和 /或硝酸铁中的一种或多种。
3、根据权利要求 1所述的抛光液,所述的氧化剂的质量百分含量为 0.01〜10 %。
4、根据权利要求 1所述的抛光液, 所述的研磨颗粒选自二氧化硅、三氧化 二铝、 掺杂铝的二氧化硅、 覆盖铝的二氧化硅、 二氧化铈、 二氧化钛和 / 或高分子研磨颗粒中的一种或多种。
5、根据权利要求 1所述的抛光液,所述的研磨颗粒的质量百分含量为 0.1〜5 %。
6、 根据权利要求 1所述的抛光液, 所述的研磨颗粒的粒径为 20~150nm。
7、根据权利要求 1所述的抛光液, 所述的腐蚀抑制剂选自氮唑、 咪唑、 噻 唑、 吡啶和 /或嘧啶类化合物中的一种或多种。
8、根据权利要求 17所述的抛光液, 所述的氮唑类化合物选自苯并三氮唑、 5-甲塞 -1, 2, 3-苯并三氮唑、 5-羧基苯并三氮唑、 1-羟基一苯并三氮唑、 1, 2, 4-三氮唑、 3-氨基 -1, 2, 4-三氮唑、 4-氨基 -1, 2, 4-三氮唑、 3,
5-二氨基 -1, 2, 4-三氮唑、 5-羧基 -3-氨基 -1, 2, 4-三氮唑、 3-氨基 -5-巯 基 -1, 2, 4-三氮唑、 5-乙酸 -1H-四氮唑、 5-甲基四氮唑、 5-苯基四氮唑、 5-氨基 -1H-四氮唑和 /或 1-苯基 -5-巯基 -四氮唑中的一种或多种。
、 根据权利要求 17所述的抛光液, 所述的咪唑类化合物为苯并咪唑和 /或 2-巯基苯并咪唑。
、 根据权利要求 17所述的抛光液, 所述的噻唑类化合物选自 2-巯基 -苯并 噻唑、 2-巯基噻二唑和 /或 5-氨基 -2-巯基 -1 , 3 , 4-孿二唑中的一种或多种。 、 根据权利要求 17所述的抛光液, 所述的吡啶选自 2, 3-二氨基吡啶、 2- 氨基吡啶和 /或 2-吡啶甲酸中的一种或多种。
、 :根据权利要求 17所述的抛光液, 所述的嘧啶为 2-氨基嘧啶。
、 裉据权利要求 1 所述的抛光液, 所述的腐蚀抑制的质量百分含量为 0.00卜 5%。
、 根据权利要求 1所述的抛光液, pH为 4~11。
、 根据权利要求 1所述的抛光液, 含有 pH调节剂、 粘度调节剂、 消泡剂 和 /或杀菌剂中的一种或多种。
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Publication number | Priority date | Publication date | Assignee | Title |
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CN102516875A (zh) * | 2011-07-05 | 2012-06-27 | 复旦大学 | 一种基于金属Co的抛光工艺的抛光液及其应用 |
WO2014059744A1 (zh) * | 2012-10-17 | 2014-04-24 | 安集微电子(上海)有限公司 | 一种碱性化学机械抛光液 |
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