CN114591687A - Rare earth polishing powder for semiconductor wafer polishing treatment and preparation method thereof - Google Patents
Rare earth polishing powder for semiconductor wafer polishing treatment and preparation method thereof Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 233
- 239000000843 powder Substances 0.000 title claims abstract description 176
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000004065 semiconductor Substances 0.000 title claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 21
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 21
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000654 additive Substances 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 27
- 230000000996 additive effect Effects 0.000 claims abstract description 24
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 11
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 12
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 9
- 229920002125 Sokalan® Polymers 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 9
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000004584 polyacrylic acid Substances 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- 238000003682 fluorination reaction Methods 0.000 claims description 8
- 238000007517 polishing process Methods 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 75
- 235000012431 wafers Nutrition 0.000 abstract description 39
- 239000006185 dispersion Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 description 31
- 238000005054 agglomeration Methods 0.000 description 16
- 230000002776 aggregation Effects 0.000 description 16
- 239000013078 crystal Substances 0.000 description 15
- 229910000420 cerium oxide Inorganic materials 0.000 description 13
- 238000002835 absorbance Methods 0.000 description 12
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 12
- 239000002904 solvent Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000725 suspension Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- -1 dichloro zirconia Chemical compound 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002120 nanofilm Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
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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
-
- 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Abstract
The application relates to the technical field of polishing powder, and particularly discloses rare earth polishing powder for semiconductor wafer polishing and a preparation method thereof. A rare earth polishing powder for polishing a semiconductor wafer comprises the following substances in parts by weight: 10-20 parts of cerium nitrate, 0.5-2 parts of a dispersing agent and 0.5-1 part of an additive, wherein the dispersing agent comprises polyvinylpyrrolidone and sodium polyacrylate in a mass ratio of 1-1.5: 0-1. The preparation method comprises the following steps: s1, preparing a precursor; s2, preparing polishing powder: and (3) roasting the precursor at the temperature of 700-900 ℃, cooling and crushing to obtain the polishing powder. The rare earth polishing powder can be used for polishing wafers and silicon wafers, and has the advantages of uniform dispersion and stable polishing; in addition, the preparation method has the advantages of convenience in operation and convenience in adjusting the particle size of the polishing powder.
Description
Technical Field
The application relates to the field of polishing materials, in particular to rare earth polishing powder for polishing semiconductor wafers and a preparation method thereof.
Background
A semiconductor wafer is a semiconductor component commonly used in electronic circuits, and is obtained by doping polycrystalline silicon into monocrystalline silicon, then generating a silicon ingot, and accurately cutting the silicon ingot by using a diamond saw. And grinding, thinning, etching, cleaning, chamfering, polishing and the like are carried out on the wafer to obtain a semiconductor wafer finished product. When the wafer is used, the polished surface of the wafer needs to be used for producing circuits, so that the polished surface does not have any bulge, micro-texture, scratch and residual damage, and the wafer is usually cleaned and inspected after polishing to ensure that the polished surface is smooth and has no defects and then is put into use.
At present, a wafer is usually polished by a CMP method (chemical mechanical polishing method), which is a technique for removing a surface material of a workpiece by comprehensively utilizing chemical oxidation, mechanical friction and fluid action, and the polished surface of the workpiece meets the requirement of smoothness and no damage by mainly utilizing the grinding action of a nano abrasive and the chemical corrosion action of slurry. The chemical mechanical polishing method needs to use polishing solution, and the polishing solution is prepared by matching polishing powder and a solvent.
In view of the above-mentioned related art, the inventors believe that the polishing powder has a defect of poor polishing effect due to the uneven dispersion of the polishing powder in the solvent, which results in poor uniformity of the particles of the polishing solution.
Disclosure of Invention
In order to overcome the defect that the polishing effect is poor due to poor dispersibility of the polishing powder, the application provides the rare earth polishing powder for polishing the semiconductor wafer.
In a first aspect, the present application provides a rare earth polishing powder for semiconductor wafer polishing, which adopts the following technical scheme:
a rare earth polishing powder for polishing a semiconductor wafer comprises the following substances in parts by weight: 10-20 parts of cerium nitrate, 0.5-2 parts of a dispersing agent and 0.5-1 part of an additive, wherein the dispersing agent comprises polyvinylpyrrolidone and sodium polyacrylate in a mass ratio of 1-1.5: 0-1.
By adopting the technical scheme, the proportion among the cerium nitrate, the dispersing agent and the additive is optimized, so that the dispersing agent and the additive are stably loaded with charged ions on the surfaces of the polishing powder particles, the electrostatic repulsion among the polishing powder particles is increased, and the possibility of agglomeration of the polishing powder particles is reduced. Meanwhile, the proper charged ions form a stable double electric layer on the surface of the polishing powder particles, the repelling and dispersing effects among the polishing powder particles are increased, the possibility of bridging or flocculation of the polymer chain segments grafted on the polishing powder particles is reduced, and the stability of the polishing powder in a solvent is improved.
Because the polyvinylpyrrolidone is used as the dispersing agent, after the cerium nitrate is matched with the polyvinylpyrrolidone, the polyvinylpyrrolidone enables the cerium nitrate to be converted into cerium oxide with an octahedral structure, and the octahedral structure of the cerium oxide enables the surfaces of the polishing powder particles to obtain more active functional groups, enhances the oxidability of the polishing powder, and improves the polishing effect of the polishing powder on the wafer. Meanwhile, polyvinylpyrrolidone precipitates on the surface of cerium oxide to form a molecular film, so that mutual collision of polishing powder particles is prevented, the possibility of agglomeration among the polishing powder particles is reduced, and the dispersion effect of the polishing powder particles is improved.
The sodium polyacrylate and the polyvinylpyrrolidone are matched to be used as the dispersing agent, the sodium polyacrylate can be stably adsorbed and loaded on the surface of cerium oxide, and meanwhile, through weak flocculation, the volume and the inter-particle repulsion of polishing powder particles are increased, the possibility of agglomeration of the polishing powder is reduced, the dispersing effect of the polishing powder in a solvent is improved, the polishing powder is uniformly suspended in the solvent, and the polishing effect of the polishing powder is improved.
Preferably, the dispersing agent further comprises sodium tripolyphosphate and sodium citrate, and the mass ratio of the polyvinylpyrrolidone to the sodium polyacrylate to the sodium tripolyphosphate to the sodium citrate is 1-1.5:0-1:1-3: 1-4.
By adopting the technical scheme, the sodium tripolyphosphate and the sodium citrate are matched with each other to form the double-layer electrostatic layer outside the polishing powder particles, so that the Zeta potential of the polishing powder particles can be effectively increased, the polishing powder particles are mutually repelled, the dispersing force among the polishing powder particles can resist the agglomeration force, the possibility of agglomeration among the polishing powder particles is reduced, the dispersion uniformity of the polishing powder in a solvent is improved, and the polishing effect of the polishing powder is improved.
Meanwhile, sodium tripolyphosphate and sodium citrate are used as dispersing agents to be matched with cerium nitrate, so that the dissociation effect of the polishing powder on a monomer in a wafer can be effectively enhanced, namely, the polishing removal rate of the polishing powder on the wafer is increased, and the polishing effect of the polishing powder is enhanced.
Preferably, the composite material also comprises a doped filler, wherein the doped filler comprises titanium sulfate and hydrous zirconium oxychloride, and the mass ratio of the titanium sulfate to the hydrous zirconium oxychloride is 4-5: 1-2.
By adopting the technical scheme, the technical scheme of the application adopts the coordination of titanium sulfate and hydrous zirconium oxychloride as the doping filler, and in the process of forming cerium oxide, the zirconium oxide is formed simultaneously, and the octahedral cubic structure of the cerium oxide and the four sides of the zirconium oxide are matched, so that the polishing powder particles are in multi-stage coordination, the synergistic polishing effect is achieved when the wafer is polished, and the polishing efficiency of the polishing powder is improved.
Secondly, the lattice sites of part of cerium and zirconium are replaced by titanium with different particle radii, so that part of lattices are distorted, the surface activity of the polishing powder particles is increased, and the polishing effect of the polishing powder in CMP is improved. Meanwhile, the crystal lattice of the titanium is substituted, and the shape of the polishing powder particles is regulated, so that the polishing powder particles are more round, the possibility of agglomeration among the polishing powder particles is reduced, the uniform dispersion of the polishing powder in a solvent is facilitated, and the polishing effect of the polishing powder is improved.
Preferably, the doped filler also comprises silica, and the mass ratio of the silica to the titanium sulfate to the hydrous zirconium oxychloride is 2-4:4-5: 1-2.
Through adopting above-mentioned technical scheme, this application technical scheme adopts silica, titanium sulfate and hydration dichloro zirconia to mutually support, and then the polishing powder can form the shell nuclear structure of silica-cerium oxide, through titanium sulfate as the kernel for the polishing powder particle is in the growth process, when generating octahedron structure, makes the edge of octahedron comparatively mellow and smooth, when maintaining the polishing powder to the polishing strength of wafer promptly, reduces the fish tail of polishing powder to the wafer.
And secondly, the silicon dioxide is used as a core structure, so that the particle size of polishing powder particles can be effectively reduced, and the polishing fineness, namely the polishing effect, of the polishing powder is improved. In addition, the silicon dioxide has better dispersibility, so that the dispersibility of the polishing powder is stably improved, the possibility of hard agglomeration of the polishing powder in a solvent is reduced, the damage of the polishing powder to a wafer is reduced, and the polishing effect of the polishing powder is improved.
Preferably, the doped filler is a doped filler subjected to fluorination treatment, and the fluorination treatment comprises the following preparation steps: taking 1-5 parts by weight of doped filler and 2-10 parts by weight of hydrofluoric acid, stirring and mixing the hydrofluoric acid and the doped filler to obtain a mixed solution, adjusting the pH =6-7 of the mixed solution, washing, filtering, retaining solids, and drying to obtain the doped filler subjected to fluorination treatment.
By adopting the technical scheme, hydrofluoric acid is adopted to perform fluorination modification on the doped filler, has strong activity, and can be fully combined with the doped filler to react, so that fluorine ions are loaded on the doped filler, and particle lattices in the doped filler are replaced. Therefore, when the polishing powder is prepared by doping the raw material, fluorine ions on the doping raw material promote the crystallization degree of the polishing powder particles, enhance the edge angles of the polishing powder particles and improve the cutting capability of the polishing powder particles; and the particles are refined, so that the possibility of agglomeration of the polishing powder particles is reduced, and the polishing powder obtains a high-efficiency and fine polishing effect.
Preferably, the additive comprises zinc nitrate and boric acid in a mass ratio of 0.1-1: 1-2.
Through adopting above-mentioned technical scheme, this application technical scheme adopts zinc nitrate and boric acid to mutually support, increases the surface activity of polishing powder particle, promotes the polishing effect of polishing powder. Meanwhile, in the process of converting cerium nitrate into cerium oxide, loose pores are easily generated on the surfaces of the formed polishing powder particles, and the additive is diffused to the periphery to fill the loose pores of the polishing powder particles, so that the compactness of the polishing powder particles is effectively increased, the possibility of mutual attraction among the polishing powder particles is reduced, the dispersibility of the polishing powder is improved, and the polishing effect of the polishing powder is improved.
Preferably, the additive also comprises carboxymethyl cellulose and polyacrylic acid, and the mass ratio of the zinc nitrate to the boric acid to the carboxymethyl cellulose to the polyacrylic acid is 0.1-1:1-2:1-2: 1-3.
By adopting the technical scheme, the polyacrylic acid and the carboxymethyl cellulose are matched to be used as the additive, and the polyacrylic acid has larger molecular weight, so that after the polyacrylic acid is adsorbed on the surfaces of the polishing powder particles, the long-chain structure is fully extended, an adsorption layer is formed on the surfaces of the polishing powder particles, the steric hindrance of the polishing powder particles is increased, the agglomeration among the particles is prevented, and the dispersibility of the polishing powder in a solvent is improved.
Meanwhile, the carboxymethyl cellulose provides anion groups for the polishing powder, and the anion groups are extruded into the adsorption layer, so that the thickness of a double electric layer is increased, and the electrostatic repulsion among polishing powder particles is increased; but also the possibility of collision between the polishing powder particles is hindered and the possibility of agglomeration of the polishing powder particles is reduced.
In addition, the long chain structure can be dissociated to increase the charge of the polishing powder particles, so that the polishing powder particles are stably suspended in the solvent through the electrostatic steric stabilization effect, i.e., the polishing powder is uniformly distributed in the solvent.
In a second aspect, the present application provides a method for preparing a rare earth polishing powder for semiconductor wafer polishing, which adopts the following technical scheme:
a preparation method of rare earth polishing powder for polishing semiconductor wafers comprises the following steps: s1, precursor preparation: respectively weighing 10-20 parts of cerium nitrate, 0.5-2 parts of dispersing agent, 0.5-1 part of additive and 10-40 parts of water according to parts by weight, stirring and mixing the cerium nitrate, the additive, the dispersing agent and the water to prepare intermediate liquid, ultrasonically dispersing, continuously stirring, filtering, and drying to obtain a precursor; s2, preparing polishing powder: and (3) roasting the precursor at the temperature of 700-900 ℃, cooling and crushing to obtain the polishing powder.
By adopting the technical scheme, the hydrothermal method is adopted to prepare the polishing powder, the particle size and the shape of the polishing powder can be easily controlled by the hydrothermal method, so that the polishing powder can obtain a small particle size and a round and regular shape, and the wafer can be efficiently ground while scratches on the wafer are reduced. Meanwhile, the roasting temperature is optimized, the precursor is roasted at the proper roasting temperature, the crystallization of crystal grains in the polishing powder is gradually and completely, and the sharp corners of the polishing powder particles are relatively rounded, so that the possibility of scratching a wafer by the polishing powder is reduced, and the polishing effect of the polishing powder is stably improved.
Preferably, the intermediate solution pH =4-6 is adjusted in step S1.
Through adopting above-mentioned technical scheme, this application technical scheme has optimized the pH value of intermediate solution for intermediate solution is in acid environment moderately, and suitable pH makes in the polishing powder particle nucleation quantity suitable, is difficult for taking place to reunite, and the crystal nucleus size is suitable, and the crystal nucleus is difficult for growing up, and then the particle diameter of control polishing powder crystalline grain is nanometer particle, makes the polishing powder to the polishing effect preferred of wafer.
Preferably, the time of the roasting treatment in the step S2 is 2-4 h.
By adopting the technical scheme, the roasting treatment time and the suitable roasting treatment time are optimized by the technical scheme, so that the precursor is completely reacted and converted into the target crystal product, the target crystal product is uniform in particle size, difficult to agglomerate and moderate in hardness, and therefore the polishing powder can be uniformly dispersed and suspended in the solvent, the wafer is efficiently polished, and the polishing effect of the wafer is improved.
In summary, the present application has the following beneficial effects:
1. because the polyvinylpyrrolidone and the sodium polyacrylate are matched as the dispersing agent, the polyvinylpyrrolidone can convert cerium nitrate into cerium oxide with an octahedral structure, and active functional groups on polishing powder particles are increased, so that a wafer can be stably oxidized and polished in CMP (chemical mechanical polishing); meanwhile, a molecular film can be deposited on the surface of the cerium oxide octahedron structure to prevent the polishing powder particles from colliding, namely the possibility of agglomeration among the polishing powder particles is reduced; and secondly, the sodium polyacrylate can be stably loaded on the surfaces of the polishing powder particles, so that the suspension effect of the polishing powder particles is stably enhanced, and the polishing powder obtains a uniform and stable polishing effect.
2. In the application, the silicon dioxide, the titanium sulfate and the hydrous zirconium oxychloride are preferably matched with each other to be used as the doped filler, firstly, a tetragonal phase structure is added in an octahedral structure of the polishing powder, so that the polishing effect of the polishing powder on a wafer is enhanced; secondly, partial lattices of cerium and zirconium are replaced by titanium, so that the lattices of the polishing powder particles are distorted, and the shapes of the polishing powder particles are regulated; in addition, a coated shell-core structure can be formed, the possibility of agglomeration among polishing powder particles is further reduced, and the dispersibility of the polishing powder is stably improved, so that the polishing powder has high-efficiency and high-quality polishing effect.
3. According to the method, the precursor is prepared by a hydrothermal method, so that the polishing powder particles obtain smaller particle size and regular morphology, and meanwhile, the roasting temperature of the precursor is optimized, so that the grains in the polishing powder are completely crystallized, sharp corners of the grains are wrapped, the possibility of agglomeration of the polishing powder is stably reduced, and the polishing powder obtains a high-efficiency and stable polishing effect.
Detailed Description
The present application will be described in further detail with reference to examples.
In the embodiment of the present application, the selected apparatuses are as follows, but not limited thereto:
the instrument comprises the following steps: a rotary polisher of the dennaemer environmental protection technology ltd.
Medicine preparation: k60 polyvinylpyrrolidone of Shandong Guangshi electronic technology Co., Ltd, cerous nitrate hexahydrate of Shandong De Sheng New Material Co., Ltd, carboxymethyl cellulose of Gallery XingBing cellulose Co., Ltd, and electroplating grade boric acid of Jinan hong Cheng chemical Co., Ltd.
Preparation example
Preparation example of dispersant
Preparation examples 1 to 6
Weighing polyvinylpyrrolidone, sodium polyacrylate, sodium tripolyphosphate and sodium citrate respectively, wherein the specific mass is shown in Table 1, stirring and mixing to obtain dispersing agent 1-6
TABLE 1 preparation examples 1-6 dispersant compositions
Preparation of doped Filler
Preparation examples 7 to 10
Respectively weighing titanium sulfate, hydrous zirconium oxychloride and silicon dioxide, wherein the specific mass is shown in Table 2, and stirring and mixing to obtain the doped filler 1-4.
TABLE 2 PREPARATION EXAMPLES 7-10 DOPED FILLER COMPOSITIONS
Preparation examples 11 to 13
The difference from preparation example 10 is that: carrying out fluorination modification treatment on the doped filler, respectively weighing the doped filler and hydrofluoric acid with the mass fraction of 40%, wherein the specific mass is shown in table 3, stirring and mixing the hydrofluoric acid with the mass fraction of 40% and the doped raw material to obtain a mixed solution, adding ammonium bicarbonate into the mixed solution, adjusting the pH =6, washing with deionized water, filtering, retaining solids, and drying at 60 ℃ for 2h to obtain the fluorinated doped filler 1-3.
TABLE 3 PREPARATION EXAMPLES 11-13 DOPED FILLER AND HYDROFLUORIC ACID RATIO
Preparation example 14
The difference from preparation example 12 is that: pH =7 was adjusted to give fluorinated doped filler 4.
Examples of preparation of additives
Preparation examples 15 to 18
Zinc nitrate, boric acid, carboxymethyl cellulose and polyacrylic acid are respectively weighed, the specific mass is shown in table 4, and the additives 1-4 are obtained by stirring and mixing.
TABLE 4 preparation examples 15-18 additive composition
Examples
Examples 1 to 3
In one aspect, the present application provides a rare earth polishing powder for use in a semiconductor wafer polishing process, comprising: cerium nitrate, additive 1, dispersant 1 and water, and the specific mass is shown in Table 5.
In another aspect, the present application provides a method for preparing a rare earth polishing powder for a semiconductor wafer polishing process, comprising the steps of: stirring and mixing cerium nitrate, an additive, a dispersing agent and water to prepare an intermediate solution, performing ultrasonic dispersion, adjusting the pH =8, continuing stirring, performing suction filtration and drying to obtain a precursor; and (3) roasting the precursor at 700 ℃ for 2h, cooling, and crushing by a one-step dry method to obtain the polishing powder 1-3.
TABLE 5 examples 1-3 polishing powder compositions
Example 4
The difference from example 3 is that: baking at 800 deg.C to obtain polishing powder 4.
Example 5
The difference from example 3 is that: and roasting at 900 ℃ to prepare polishing powder 5.
Example 6
The difference from example 3 is that: pH =5 was adjusted to prepare polishing powder 6.
Example 7
The difference from example 3 is that: pH =6 was adjusted to prepare polishing powder 7.
Example 8
The difference from example 3 is that: the time of the roasting treatment was 3 hours, and polishing powder 8 was prepared.
Example 9
The difference from example 3 is that: the time of the baking treatment was 4 hours, and polishing powder 9 was prepared.
Examples 10 to 12
The difference from example 3 is that: polishing powders 10 to 12 were prepared using additives 2 to 4 instead of additive 1 in example 3.
Examples 13 to 17
The difference from example 3 is that: polishing powders 13 to 17 were prepared using dispersants 2 to 6 instead of dispersant 1 in example 3.
Examples 18 to 25
The difference from example 3 is that: adding 1-4 doped fillers and 1-4 fluorinated modified doped fillers into the intermediate solution respectively to prepare 18-25 polishing powder.
Comparative example
Comparative example 1
The difference from example 3 is that: polishing powder 26 was prepared without additive 1.
Comparative example 2
The difference from example 3 is that: the polishing powder 27 was prepared by baking at 1000 ℃.
Performance test
Adding the polishing powder 1-27 into deionized water, magnetically stirring for 10min, ultrasonically dispersing for 20min to obtain polishing suspension 1-27, and polishing the silicon wafer by using the polishing suspension.
1. Potential detection: the potentials of suspensions 1-27 were measured using a Zeta Sizer Analyzer and recorded.
2. And (3) detecting absorbance: the absorbance of suspensions 1-27 was measured using a spectrophotometer and recorded.
3. And (3) micro roughness detection: the silicon wafers were measured for roughness using a zygo surface profiler and the average was recorded.
4. Material removal rate: and measuring the reduction of the thickness of the silicon wafer per minute by using a thickness gauge, and recording.
Table 6 examples 1-25 performance testing
In combination with the comparison of the performance tests in table 6, it can be found that:
(1) a comparison of examples 1 to 3 with comparative example 1 shows that: the absolute values of the potential, the absorbance and the removal rate of the polishing powder prepared in examples 1 to 3 were increased, and the microroughness was decreased, which indicates that the hydrothermal method was used to convert cerium nitrate into cerium oxide having an octahedral structure, so that the diameter of the polishing powder particles was small, and the dispersibility of the polishing powder particles was improved and the polishing effect of the polishing powder was improved by adding the dispersant and the additive. As can be seen from Table 6, the polishing powder obtained in example 3 had high absolute values of potential, absorbance and removal rate, and low microroughness, indicating that the proportions of the components in the polishing powder were suitable.
(2) A comparison of examples 4-5, examples 6-7, examples 8-9 and comparative example 2 shows that: the polishing powders obtained in examples 4 to 9 have improved absolute values of potential, absorbance and removal rate and reduced microroughness, which indicates that the application adopts proper calcination temperature, calcination time and pH of intermediate solution to prepare a precursor, so that crystal grains obtain crystal nuclei with proper grain diameter, the grain diameter of the crystal grains is controlled, nanoscale crystal grains are formed, the number of the crystal nuclei is reduced, and the crystal grain agglomeration is reduced. And during roasting, the crystal grains are completely crystallized, and the sharp positions of the formed crystal grains are relatively smooth, so that the polishing efficiency of the polishing powder is improved, and the possibility that the wafer is scratched by the polishing powder is reduced. As can be seen from Table 6, the polishing powders obtained in examples 5, 6 and 8 had high absolute values of potential, absorbance and removal rate and low microroughness, indicating that the calcination temperature was suitable in example 5, the pH of the intermediate solution was suitable in example 6, and the calcination time was suitable in example 8.
(3) A comparison of examples 10 to 12 with comparative example 1 shows that: the absolute values of the potential, the absorbance and the removal rate of the polishing powders obtained in examples 10 to 12 were improved, and the microroughness was reduced, which indicates that zinc nitrate, boric acid, carboxymethyl cellulose and polyacrylic acid were used as additives in the present application, and on the one hand, the additive can fill pores of cerium oxide during the formation of cerium oxide, which is advantageous for the formation of dense polishing powder particles; on the other hand, the additive can form an adsorption layer on the surface of the polishing powder particles, so that the steric hindrance between the polishing powder particles is increased, the possibility of agglomeration of the polishing powder is reduced, and the dispersion uniformity of the polishing powder is improved. As can be seen from Table 6, the polishing powders obtained in example 11 had high absolute values of potential, absorbance and removal rate, and low microroughness, indicating that the proportions of the respective components in the additive were suitable.
(4) By combining example 13, examples 14-16, and example 17, it can be found that: the absolute values of the potentials, absorbances and removal rates of the polishing powders obtained in examples 13 to 17 were improved, and the microroughness was reduced, which indicates that the application uses polyvinylpyrrolidone, sodium polyacrylate, sodium tripolyphosphate and sodium citrate in combination to form a molecular layer on the surface of the polishing particles, thereby increasing the steric hindrance between the molecules, and at the same time, a double-layer electrostatic layer is formed on the polishing powder particles, thereby reducing the possibility of agglomeration of the polishing particles by electrostatic repulsion, and improving the dispersion uniformity of the polishing powder. As can be seen from Table 6, the polishing powders obtained in example 16 had high absolute values of potential, absorbance and removal rate, and low microroughness, indicating that the proportions of the respective components in the dispersant were suitable.
(5) A comparison of example 18, examples 19 to 21, examples 22 to 24 and example 25 shows that: the absolute values of the potentials, the absorbances and the removal rates of the polishing powders prepared in examples 18 to 25 were improved, and the microroughness was reduced, which indicates that the polishing powders of the present invention adopt silica, titanium sulfate and hydrous zirconium oxychloride as a dopant filler to substitute the crystal lattices in the polishing powder particles, so that the lattices are distorted, the morphologies of the polishing powder particles are regulated, and a shell-core coating structure is formed, thereby improving the polishing efficiency and the polishing quality of the polishing powders. As can be seen from table 6, the polishing powders obtained in examples 20 and 22 had high absolute values of potential, absorbance, and removal rate, and low microroughness, indicating that the respective compositions of the doped filler in example 20 were suitable, and the mixture ratio of the doped filler and hydrofluoric acid in example 22 was suitable.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The rare earth polishing powder for polishing the semiconductor wafer is characterized by comprising the following components in parts by weight: 10-20 parts of cerium nitrate, 0.5-2 parts of a dispersing agent and 0.5-1 part of an additive, wherein the dispersing agent comprises polyvinylpyrrolidone and sodium polyacrylate in a mass ratio of 1-1.5: 0-1.
2. A rare earth polishing powder for use in a semiconductor wafer polishing process according to claim 1, wherein: the dispersing agent also comprises sodium tripolyphosphate and sodium citrate, and the mass ratio of the polyvinylpyrrolidone to the sodium polyacrylate to the sodium tripolyphosphate to the sodium citrate is 1-1.5:0-1:1-3: 1-4.
3. A rare earth polishing powder for use in a semiconductor wafer polishing process according to claim 1, wherein: the cerium nitrate is subjected to doping treatment by using a doping filler, the doping filler comprises titanium sulfate and hydrous zirconium oxychloride, and the mass ratio of the titanium sulfate to the hydrous zirconium oxychloride is 4-5: 1-2.
4. A rare earth polishing powder for use in a semiconductor wafer polishing process according to claim 3, wherein: the doped filler also comprises silicon dioxide, and the mass ratio of the silicon dioxide, the titanium sulfate and the hydrous zirconium oxychloride is 2-4:4-5: 1-2.
5. A rare earth polishing powder for use in semiconductor wafer polishing treatment according to claim 3, wherein the doped filler is a doped filler subjected to fluorination treatment, and the fluorination treatment comprises the following preparation steps: taking 1-5 parts by weight of doped filler and 2-10 parts by weight of hydrofluoric acid, stirring and mixing the hydrofluoric acid and the doped filler to obtain a mixed solution, adjusting the pH =6-7 of the mixed solution, washing, filtering, retaining solids, and drying to obtain the doped filler subjected to fluorination treatment.
6. A rare earth polishing powder for use in a semiconductor wafer polishing process according to claim 1, wherein: the additive comprises zinc nitrate and boric acid in a mass ratio of 0.1-1: 1-2.
7. A rare earth polishing powder for use in a semiconductor wafer polishing process according to claim 6, wherein: the additive also comprises carboxymethyl cellulose and polyacrylic acid, wherein the mass ratio of the zinc nitrate to the boric acid to the carboxymethyl cellulose to the polyacrylic acid is 0.1-1:1-2:1-2: 1-3.
8. A method for preparing a rare earth polishing powder for use in a semiconductor wafer polishing process according to any one of claims 1 to 7, comprising the steps of:
s1, precursor preparation: respectively weighing 10-20 parts of cerium nitrate, 0.5-2 parts of dispersing agent, 0.5-1 part of additive and 10-40 parts of water according to parts by weight, stirring and mixing the cerium nitrate, the additive, the dispersing agent and the water to prepare intermediate liquid, ultrasonically dispersing, continuously stirring, filtering, and drying to obtain a precursor;
s2, preparing polishing powder: and (3) roasting the precursor at the temperature of 700-900 ℃, cooling and crushing to obtain the polishing powder.
9. The method of claim 8, wherein the polishing powder comprises at least one of the following components: adjusting the intermediate solution pH =4-6 in step S1.
10. The method of claim 8, wherein the polishing powder comprises at least one of the following components: the roasting time in the step S2 is 2-4 h.
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