CN115851137A - Polishing solution for semiconductor material and preparation method thereof - Google Patents
Polishing solution for semiconductor material and preparation method thereof Download PDFInfo
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- CN115851137A CN115851137A CN202211640163.7A CN202211640163A CN115851137A CN 115851137 A CN115851137 A CN 115851137A CN 202211640163 A CN202211640163 A CN 202211640163A CN 115851137 A CN115851137 A CN 115851137A
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- 238000005498 polishing Methods 0.000 title claims abstract description 106
- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000004065 semiconductor Substances 0.000 title claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 36
- 229940075614 colloidal silicon dioxide Drugs 0.000 claims abstract description 22
- 239000011941 photocatalyst Substances 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 71
- 239000002245 particle Substances 0.000 claims description 43
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 42
- 230000001276 controlling effect Effects 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000011863 silicon-based powder Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008119 colloidal silica Substances 0.000 claims description 16
- 238000012216 screening Methods 0.000 claims description 15
- 239000003381 stabilizer Substances 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007800 oxidant agent Substances 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- 239000002738 chelating agent Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229910021487 silica fume Inorganic materials 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 229910021536 Zeolite Inorganic materials 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 6
- 238000006703 hydration reaction Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 5
- 239000012964 benzotriazole Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 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 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 4
- XWNSFEAWWGGSKJ-UHFFFAOYSA-N 4-acetyl-4-methylheptanedinitrile Chemical compound N#CCCC(C)(C(=O)C)CCC#N XWNSFEAWWGGSKJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002319 Poly(methyl acrylate) Polymers 0.000 claims description 2
- 239000004153 Potassium bromate Substances 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229940094037 potassium bromate Drugs 0.000 claims description 2
- 235000019396 potassium bromate Nutrition 0.000 claims description 2
- -1 potassium ferricyanide Chemical compound 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 230000006378 damage Effects 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 9
- 230000002776 aggregation Effects 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 7
- 238000007517 polishing process Methods 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 238000005299 abrasion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- 238000009826 distribution Methods 0.000 description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 11
- 230000007547 defect Effects 0.000 description 10
- 229910010271 silicon carbide Inorganic materials 0.000 description 10
- 239000003082 abrasive agent Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 230000009471 action Effects 0.000 description 2
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- 239000006260 foam Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
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- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Images
Abstract
The invention relates to the technical field of polishing solution preparation, in particular to a polishing solution for a semiconductor material and a preparation method thereof, and the polishing solution for the semiconductor material and the preparation method thereof have the advantages that the prepared mixed abrasive of cerium dioxide and colloidal silicon dioxide has better comprehensive performance compared with a single abrasive, and the polishing rate can be improved by matching the chemical corrosion capacity of the polishing solution; meanwhile, the polishing solution can better avoid mechanical damage caused in the polishing process based on CMP technology, film-forming agent and other components, and is beneficial to reducing abrasion and improving polishing quality; in addition, the efficiency in the chemical mechanical polishing process can be further optimized by matching with other auxiliary agents such as a photocatalyst and the like with a CMP technology, and meanwhile, the polishing solution has better dispersibility and anti-settling capacity, can be uniformly distributed in the polishing process, avoids agglomeration and abrasion of the surface of a workpiece, and has stable and reliable polishing performance.
Description
Technical Field
The invention relates to the technical field of polishing solution preparation, in particular to a polishing solution for a semiconductor material and a preparation method thereof.
Background
The third-generation semiconductor material is represented by silicon carbide (SiC), wherein SiC is a typical polycrystalline compound, has the characteristics of high strength, high thermal shock resistance, high saturated electron drift rate, high thermal conductivity, chemical corrosion resistance, large forbidden bandwidth and the like, can meet the application of electronic devices in severe environments such as high frequency, high temperature and the like, and is an advanced semiconductor material at present; the surface appearance and damage degree of SiC can directly influence the service performance of a workpiece, the hardness of SiC is very high, the Mohs hardness is 9.5 grade, and is only second to the hardest diamond in the world, and SiC and other semiconductor materials mainly eliminate surface defects based on Chemical Mechanical Polishing (CMP) treatment at present.
The CMP technology is one of the key technologies for processing the surface of a semiconductor wafer, and can eliminate a damaged layer on the surface of the semiconductor wafer by a polishing principle of organically combining chemical corrosion and mechanical grinding, so as to realize the technology of removing nanoscale micro units on the surface of a workpiece and planarizing the surface of the workpiece, thereby obtaining an ultra-precise surface.
The core of the CMP technology comprises the application of polishing solution, the polishing solution is one of the key factors influencing the polishing quality in CMP, the existing polishing solution mainly comprises grinding materials, oxidizing agents and the like, the components of the existing polishing solution generally have synergistic action, and the components of the existing polishing solution can influence the quality of the surface of a polished semiconductor wafer; for example, the kind and particle size of the abrasive affect the polishing efficiency and polishing precision, and the particle size of the abrasive affects the dispersibility in the polishing liquid, which in turn affects the roughness and polishing efficiency of the polished surface. And because the SiC of the third-generation semiconductor material is hard and has excellent wear resistance, the preparation of the polishing solution with higher polishing efficiency and polishing quality is important. In view of the above, we propose a polishing solution for semiconductor materials and a preparation method thereof.
Disclosure of Invention
In order to make up for the above deficiencies, the invention provides a polishing solution for semiconductor materials and a preparation method thereof.
The technical scheme of the invention is as follows:
the polishing solution for the semiconductor material comprises 10-50% of grinding materials, 2-6% of dispersing agents, 0.75-8% of oxidizing agents, 0.1-1% of chelating agents, deionized water and pH regulators, wherein the pH value of the polishing solution ranges from 8 to 11.5.
Preferably, other additives can be added into the polishing solution, and the other additives comprise any one or more of a stabilizer accounting for 0.5-3% of the total mass of the polishing solution, a defoaming agent accounting for 0.1-5%, a photocatalyst accounting for 0.05-2% of the total mass of the polishing solution, and a film-forming agent accounting for 0.5-2% of the total mass of the polishing solution.
Specifically, the chelating agent mainly has the effects of avoiding the influence of metal ions on a semiconductor in the polishing process to degrade the electrical characteristics of the semiconductor, reducing the reliability, reducing the surface metal ions to be stained on the surface of a semiconductor workpiece material during polishing, and ensuring that the stable and reliable service performance of the semiconductor workpiece material is not influenced; the defoaming agent is used for avoiding the generation of foams in the CMP process, the foams can cause the condition that abrasive particles are unevenly distributed at the position due to the surface tension of the film and gather to cause damage to a processing surface, and the film forming agent is used for adjusting the coating and leveling of polishing liquid on the surface of a workpiece, improving the concave-convex selectivity, forming a film structure on the unpolished surface and playing a role in protection.
Preferably, the abrasive material is a mixture of alumina, colloidal silica and cerium dioxide with the particle size of 10-260nm, and the mass part ratio of the alumina, the colloidal silica and the cerium dioxide in the mixture is 0.5-3: 1: 0.05-0.3.
Specifically, the alumina has good polishing efficiency, but has high texture density, is not easy to disperse, is easy to settle to cause uneven distribution of polishing liquid abrasives, the colloidal silica has strong activity and good dispersibility, but has high hardness to easily cause workpiece damage, the ceria has low hardness, has high polishing speed, but has poor self-dispersibility and serious agglomeration, so that the defects of the mixed abrasives can be mutually reduced, and the polishing efficiency and the particle dispersibility are good.
Preferably, the dispersing agent is any one or more of PEG, polymethyl acrylate, sodium dodecyl benzene sulfonate, sodium polyacrylate and sodium hexametaphosphate.
Specifically, the main purpose of the dispersant is to avoid aggregation and sedimentation of abrasive particles, because the abrasive nanoparticles of the polishing solution have a large specific surface area and a high surface energy, the abrasive nanoparticles are easy to agglomerate, the particle size of the aggregated particles is increased, and the surface stress distribution of a processed workpiece is uneven in the CMP process, so that the roughness is increased, the defects are increased, the CMP processing quality is not controllable, and the abrasive filtering in the preparation process is also used for further avoiding large particles, so that the abrasive particles have high uniformity and are uniformly dispersed in the polishing solution.
Preferably, the oxidant is one or more of hydrogen peroxide, ferric nitrate, potassium persulfate, potassium ferricyanide, potassium bromate and potassium permanganate.
Specifically, due to the chemical inertness and the strong mohs hardness of the semiconductor silicon carbide material, the efficiency of the CMP process needs to be improved by the oxidizing agent, but in the actual use process, part of the oxidizing agent is easy to thermally decompose under the mechanical action, for example, the chemical property of hydrogen peroxide is unstable, 0.5% -3% of the stabilizing agent added into the polishing solution can mainly prevent the oxidizing agent from decomposing, so that the content or concentration of the oxidizing agent is relatively improved, the oxidizing reaction between the oxidizing agent and the surface of the semiconductor material is favorably ensured, the mohs hardness of the semiconductor material is reduced, and the CMP efficiency is improved.
Preferably, the PH regulator is any one of sodium hydroxide, potassium hydroxide, ammonia water, and organic strong base without metal ions.
Preferably, the photocatalyst is any one or more of titanium dioxide, tin dioxide, ferric oxide, zinc oxide and zirconium dioxide.
Specifically, in the CMP process, the added photocatalyst can be matched with the added ultraviolet light to irradiate the polishing solution, so that the polishing solution catalyzes and promotes the oxidation reaction rate of the oxidant and the surface of the semiconductor material under the action of the photocatalyst, and the polishing solution containing the photocatalyst can improve the process efficiency under the same condition.
A preparation method of a polishing solution for a semiconductor material is used for preparing the polishing solution for the semiconductor material, and the preparation method of the polishing solution specifically comprises the following steps:
the method comprises the following steps: preparing an abrasive, wherein the preparation of the abrasive comprises preparing a colloidal silicon dioxide abrasive and a cerium dioxide abrasive;
step two: respectively selecting the prepared grinding materials, further screening and filtering, weighing the filtered grinding materials according to a proportion, uniformly mixing, putting the uniformly mixed grinding materials into deionized water according to a proportion, adding a dispersing agent into the deionized water, and fully and uniformly stirring to obtain a mixed solution;
step three: adding an oxidant, a stabilizer and a chelating agent into the mixed solution in sequence according to a proportion and uniformly mixing;
step four: continuously dripping the film forming agent and the photocatalyst into the mixed solution according to the proportion, stirring, adding the defoaming agent during stirring, and uniformly stirring to obtain a primary mixed solution;
step five: and dissolving the pH regulator to prepare a solution with the concentration of 0.01-0.1%, dropwise adding the solution into the primary mixed solution, and regulating the pH value to 8-11.5 to obtain the polishing solution.
Preferably, the specific method for preparing the colloidal silica abrasive comprises the following steps:
the method comprises the following steps:
the method comprises the following steps: fully soaking the elemental micro silicon powder by using a hydrofluoric acid reagent with the dilution concentration of 3-15%, taking out the activated micro silicon powder, and rinsing the micro silicon powder for multiple times by using deionized water;
step two: putting the surface activated micro silicon powder into a reaction container, controlling the reaction container to be heated to 65-95 ℃, and adding zeolite to avoid bumping;
step three: adding the silicon dioxide dispersion liquid into a reaction container in batches, adding a sodium hydroxide or potassium hydroxide catalyst aqueous solution in batches, and heating to generate hydration reaction to generate hydrogen;
step four: stopping heating after the reaction is carried out until no hydrogen exists, cooling to room temperature, and filtering out residual silica fume or impurities in the reaction container through a filtering device to obtain the colloidal silica abrasive with the particle size range of 10-120 nm;
or the second method:
hydrolysis of ethyl orthosilicate: adding ethyl silicate and deionized water into ethanol or isopropanol solvent, mixing, heating at 50-70 deg.C, stirring, adding alkali catalyst, and hydrolyzing to obtain 60-160nm colloidal silicon dioxide abrasive.
Preferably, the preparation method of the ceria and alumina abrasive comprises the following specific steps:
the method comprises the following steps: ceCl with the concentration of 0.3mol/L is selected 3 And adding CeCl at a rate of 10-16ml/min 3 0.4mol/L NH with a molar ratio of 1/4 4 HCO 3 Dropwise adding ammonia water, and controlling the initial pH value to be 3-7;
step two: mixing, controlling precipitation temperature at 65-75 deg.C, and adding CeCl dropwise 3 Polyethylene glycol surfactant with mass fraction of 2-5%, controlling aging time for 1.5-2.5h, filtering, and washing with ethanol for multiple times; the polyethylene glycol nonionic surfactant can gradually reduce the agglomerated particle size of the final powder, weaken the agglomeration, increase the surfactant, and facilitate the improvement of the dispersion degree and avoid agglomeration.
Step three: controlling the drying temperature to be 95-115 ℃, and drying for 1.5-3h;
step four: controlling the heating rate to be 8-12 ℃/min, heating to the roasting temperature of 450-600 ℃, and preserving heat for 1.8-2.2h to obtain the cerium dioxide powder abrasive with the particle size of 80-260 nm;
step five: selecting an alumina raw material, and crushing and refining the alumina raw material by a ball mill or a pulverizer;
step six: and screening the refined alumina raw material, and screening out alumina raw material particles outside the required particle size range to obtain the alumina powder abrasive meeting the particle size requirement.
Compared with the prior art, the invention has the beneficial effects that:
according to the polishing solution for the semiconductor material and the preparation method thereof, the prepared mixed abrasive of cerium dioxide and colloidal silicon dioxide has better comprehensive performance than a single abrasive, and the polishing rate can be improved by matching the chemical corrosion capacity of the polishing solution; meanwhile, the polishing solution can better avoid mechanical damage caused in the polishing process based on CMP technology, film-forming agent and other components, and is beneficial to reducing abrasion and improving polishing quality; in addition, the efficiency in the chemical mechanical polishing process can be further optimized by matching with other auxiliary agents such as a photocatalyst and the like with a CMP technology, and meanwhile, the polishing solution has better dispersibility and anti-settling capacity, can be uniformly distributed in the polishing process, avoids agglomeration and abrasion of the surface of a workpiece, and has stable and reliable polishing performance.
Drawings
FIG. 1 is a schematic view of a polishing solution according to the present invention;
FIG. 2 is a schematic view of a conventional silicon dioxide polishing solution;
FIG. 3 is one of the schematic views of the polishing surface of the workpiece of the present invention;
FIG. 4 is a second schematic view of the polishing surface of the workpiece according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention details the above technical solution by the following embodiments:
example 1
A preparation method of polishing solution for semiconductor materials specifically comprises the following steps:
abrasive preparation, which comprises the following steps: the specific method for preparing the colloidal silicon dioxide abrasive comprises the following steps: fully soaking the elemental micro silicon powder for 1h by using a hydrofluoric acid reagent with the dilution concentration of 3%, taking out the activated micro silicon powder, and rinsing for 6 times by using deionized water; then putting the surface activated micro silicon powder into a reaction kettle, controlling the reaction container to heat to 75 ℃, and adding zeolite to avoid bumping; adding the silicon dioxide dispersion liquid and the sodium hydroxide catalyst aqueous solution into a reaction vessel for three times, and carrying out hydration reaction at the temperature of 75 ℃ to generate hydrogen; stopping heating after the reaction is finished until no hydrogen exists, cooling to room temperature, and filtering out residual silica fume and impurities in the reaction container through a filtering device to obtain the colloidal silica abrasive with the particle size distribution of 30-120 nm.
The preparation method of the cerium dioxide abrasive material comprises the following steps: ceCl with the concentration of 0.3mol/L is selected 3 And CeCl was added at a rate of 12ml/min 3 0.4mol/L NH with a molar ratio of 1/4 4 HCO 3 Dropwise adding ammonia water, and controlling the initial pH value to be 5; after stirring uniformly, controllingThe precipitation temperature is 70 ℃, and CeCl is dropwise added 3 Controlling the aging time for 2h, performing suction filtration and washing for 5 times by using ethanol, wherein the mass fraction of the polyethylene glycol surfactant is 5%; and finally, controlling the drying temperature to be 105 ℃, drying for 2h, taking out, roasting, controlling the heating rate to be 10 ℃/min, heating to be 450 ℃, and preserving heat for 2h to obtain the cerium dioxide powder abrasive with the particle size distribution of 120-260 nm.
The specific method for preparing the alumina abrasive comprises the following steps: selecting an alumina raw material, crushing the alumina raw material into powder by a crusher, and then performing ball milling refinement by a ball-and-ball type ball mill; and screening the refined alumina raw material, and screening out alumina raw material particles outside the required particle size range to obtain the alumina powder abrasive with the particle size distribution of 80-210 nm.
The prepared colloidal silicon dioxide, cerium dioxide and aluminum oxide are respectively selected to be further screened and filtered to obtain 80 nm-grain-size colloidal silicon dioxide, 120 nm-grain-size cerium dioxide and 100 nm-grain-size aluminum oxide, the proportion of the colloidal silicon dioxide, the 120 nm-grain-size cerium dioxide and the 100 nm-grain-size aluminum oxide is 1.5: 1: 0.3, the abrasive materials are mixed and then are put into deionized water according to the proportion of 50 percent to be uniformly mixed, 6 percent of dispersant sodium polyacrylate is added into the deionized water, and the mixture is fully stirred and uniformly mixed to obtain mixed liquid.
Adding 8% of hydrogen peroxide, 1% of chelating agent 1,3-diketone and 3% of stabilizing agent H into the mixed solution in sequence 3 PO 4 2 percent of film-forming agent benzotriazole, 2 percent of photocatalyst titanium dioxide with the wavelength of 80nm and 5 percent of defoaming agent emulsified silicone oil, and stirring uniformly to obtain a primary mixed liquid.
And dissolving triethanolamine organic strong base serving as a pH regulator to prepare a solution with the concentration of 0.1%, dropwise adding the solution into the primary mixed solution, and regulating the pH value to 10.5 to obtain the polishing solution.
Example 2
A preparation method of polishing solution for semiconductor materials specifically comprises the following steps:
abrasive preparation, which includes preparation of colloidal silica abrasive and ceria abrasive: the specific method for preparing the colloidal silicon dioxide abrasive comprises the following steps: fully soaking the elemental micro silicon powder for 1h by using a hydrofluoric acid reagent with the dilution concentration of 3%, taking out the activated micro silicon powder, and rinsing for 6 times by using deionized water; then putting the surface activated micro silicon powder into a reaction kettle, controlling the reaction container to heat to 75 ℃, and adding zeolite to avoid bumping; adding the silicon dioxide dispersion liquid and the sodium hydroxide catalyst aqueous solution into a reaction vessel for three times, and carrying out hydration reaction at the temperature of 75 ℃ to generate hydrogen; stopping heating after the reaction is finished until no hydrogen exists, cooling to room temperature, and filtering out residual silica fume and impurities in the reaction container through a filtering device to obtain the colloidal silica abrasive with the particle size distribution of 30-120 nm.
The preparation method of the cerium dioxide abrasive material comprises the following steps: ceCl with the concentration of 0.3mol/L is selected 3 And CeCl was added at a rate of 12ml/min 3 0.4mol/L NH with a molar ratio of 1/4 4 HCO 3 Dropwise adding ammonia water, and controlling the initial pH value to be 5; after stirring evenly, controlling the precipitation temperature to be 70 ℃, and dripping CeCl 3 Controlling the aging time for 2h, performing suction filtration and washing for 5 times by using ethanol, wherein the mass fraction of the polyethylene glycol surfactant is 5%; and finally, controlling the drying temperature to be 105 ℃, drying for 2h, taking out, roasting, controlling the heating rate to be 10 ℃/min, heating to be 450 ℃, and preserving heat for 2h to obtain the cerium dioxide powder abrasive with the particle size distribution of 120-260 nm.
The specific method for preparing the alumina abrasive comprises the following steps: selecting an alumina raw material, crushing the alumina raw material into powder by a crusher, and then performing ball milling refinement by a ball-and-ball type ball mill; and screening the refined alumina raw material, and screening out alumina raw material particles outside the required particle size range to obtain the alumina powder abrasive with the particle size distribution of 80-210 nm.
The prepared colloidal silicon dioxide, cerium dioxide and aluminum oxide are respectively selected to be further screened and filtered to obtain 80 nm-grain-size colloidal silicon dioxide, 120 nm-grain-size cerium dioxide and 100 nm-grain-size aluminum oxide, the proportion of the colloidal silicon dioxide, the 120 nm-grain-size cerium dioxide and the 100 nm-grain-size aluminum oxide is 1.5: 1: 0.3, the abrasive materials are mixed and then are put into deionized water according to the proportion of 50 percent to be uniformly mixed, 6 percent of dispersant sodium polyacrylate is added into the deionized water, and the mixture is fully stirred and uniformly mixed to obtain mixed liquid.
Adding 8% of hydrogen peroxide, 1% of chelating agent 1,3-diketone and 0.5% of stabilizing agent H into the mixed solution in sequence 3 PO 4 2 percent of film-forming agent benzotriazole, 2 percent of photocatalyst titanium dioxide with the wavelength of 80nm, and 5 percent of defoaming agent emulsified silicone oilAnd uniformly stirring to obtain a primary mixed solution.
And dissolving triethanolamine organic strong base serving as a pH regulator to prepare a solution with the concentration of 0.1%, dropwise adding the solution into the primary mixed solution, and regulating the pH value to 10.5 to obtain the polishing solution.
Example 3
A preparation method of polishing solution for semiconductor materials specifically comprises the following steps:
abrasive preparation, which includes preparation of colloidal silica abrasive and ceria abrasive: the specific method for preparing the colloidal silicon dioxide abrasive comprises the following steps: fully soaking the elemental micro silicon powder for 1h by using a hydrofluoric acid reagent with the dilution concentration of 3%, taking out the activated micro silicon powder, and rinsing for 6 times by using deionized water; then putting the surface activated micro silicon powder into a reaction kettle, controlling the reaction container to heat to 75 ℃, and adding zeolite to avoid bumping; adding the silicon dioxide dispersion liquid and the sodium hydroxide catalyst aqueous solution into a reaction vessel for three times, and carrying out hydration reaction at the temperature of 75 ℃ to generate hydrogen; stopping heating after the reaction is finished until no hydrogen exists, cooling to room temperature, and filtering out residual silica fume and impurities in the reaction container through a filtering device to obtain the colloidal silica abrasive with the particle size distribution of 30-120 nm.
The preparation method of the cerium dioxide abrasive comprises the following steps: ceCl with the concentration of 0.3mol/L is selected 3 And CeCl was added at a rate of 12ml/min 3 0.4mol/L NH with a molar ratio of 1/4 4 HCO 3 Dropwise adding ammonia water, and controlling the initial pH value to be 5; after stirring evenly, controlling the precipitation temperature to be 70 ℃, and dripping CeCl 3 Controlling the aging time for 2h, performing suction filtration and washing for 5 times by using ethanol, wherein the mass fraction of the polyethylene glycol surfactant is 5%; and finally, controlling the drying temperature to be 105 ℃, drying for 2h, taking out, roasting, controlling the heating rate to be 10 ℃/min, heating to be 450 ℃, and preserving heat for 2h to obtain the cerium dioxide powder abrasive with the particle size distribution of 120-260 nm.
The specific method for preparing the alumina abrasive comprises the following steps: selecting an alumina raw material, crushing the alumina raw material into powder by a crusher, and then performing ball milling refinement by a ball-and-ball type ball mill; and screening the refined alumina raw material, and screening out alumina raw material particles outside the required particle size range by screening to obtain the alumina powder abrasive with the particle size distribution of 80-210 nm.
The prepared colloidal silicon dioxide, cerium dioxide and aluminum oxide are respectively selected to be further screened and filtered to obtain 80 nm-grain-size colloidal silicon dioxide, 120 nm-grain-size cerium dioxide and 100 nm-grain-size aluminum oxide, the proportion of the colloidal silicon dioxide, the 120 nm-grain-size cerium dioxide and the 100 nm-grain-size aluminum oxide is 1.5: 1: 0.3, the abrasive materials are mixed and then are put into deionized water according to the proportion of 50 percent to be uniformly mixed, 6 percent of dispersant sodium polyacrylate is added into the deionized water, and the mixture is fully stirred and uniformly mixed to obtain mixed liquid.
Adding 8% of hydrogen peroxide, 1% of chelating agent 1,3-diketone and 3% of stabilizing agent H into the mixed solution in sequence 3 PO 4 0.5 percent of film-forming agent benzotriazole, 2 percent of photocatalyst titanium dioxide with the wavelength of 80nm and 5 percent of defoaming agent emulsified silicone oil, and stirring uniformly to obtain a primary mixed liquid.
And dissolving triethanolamine organic strong base serving as a pH regulator to prepare a solution with the concentration of 0.1%, dropwise adding the solution into the primary mixed solution, and regulating the pH value to 10.5 to obtain the polishing solution.
Example 4
A preparation method of polishing solution for semiconductor materials specifically comprises the following steps:
abrasive preparation, which includes preparation of colloidal silica abrasive and ceria abrasive: the specific method for preparing the colloidal silicon dioxide abrasive comprises the following steps: fully soaking the elemental micro silicon powder for 1h by using a hydrofluoric acid reagent with the dilution concentration of 3%, taking out the activated micro silicon powder, and rinsing for 6 times by using deionized water; then putting the surface activated micro silicon powder into a reaction kettle, controlling the reaction container to heat to 75 ℃, and adding zeolite to avoid bumping; adding the silicon dioxide dispersion liquid and the sodium hydroxide catalyst aqueous solution into a reaction vessel for three times, and carrying out hydration reaction at the temperature of 75 ℃ to generate hydrogen; and stopping heating after the reaction is finished until no hydrogen exists, cooling to room temperature, and filtering out residual silica fume and impurities in the reaction container through a filtering device to obtain the colloidal silica abrasive with the particle size distribution of 30-120 nm.
The preparation method of the cerium dioxide abrasive comprises the following steps: ceCl with the concentration of 0.3mol/L is selected 3 And CeCl was added at a rate of 12ml/min 3 Mole of0.4mol/L NH to 1/4 4 HCO 3 Dropwise adding ammonia water, and controlling the initial pH value to be 5; after stirring evenly, controlling the precipitation temperature to be 70 ℃, and dripping CeCl 3 Controlling the aging time for 2 hours, performing suction filtration, and washing for 5 times by using ethanol, wherein the mass fraction of the polyethylene glycol surfactant is 5%; and finally, controlling the drying temperature to be 105 ℃, drying for 2h, taking out, roasting, controlling the heating rate to be 10 ℃/min, heating to be 450 ℃, and preserving heat for 2h to obtain the cerium dioxide powder abrasive with the particle size distribution of 120-260 nm.
The specific method for preparing the alumina abrasive comprises the following steps: selecting an alumina raw material, crushing the alumina raw material into powder by a crusher, and then performing ball milling refinement by a ball-and-ball type ball mill; and screening the refined alumina raw material, and screening out alumina raw material particles outside the required particle size range to obtain the alumina powder abrasive with the particle size distribution of 80-210 nm.
The prepared colloidal silicon dioxide, cerium dioxide and aluminum oxide are respectively selected to be further screened and filtered to obtain 80 nm-grain-size colloidal silicon dioxide, 120 nm-grain-size cerium dioxide and 100 nm-grain-size aluminum oxide, the proportion of the colloidal silicon dioxide, the 120 nm-grain-size cerium dioxide and the 100 nm-grain-size aluminum oxide is 1.5: 1: 0.3, the abrasive materials are mixed and then are put into deionized water according to the proportion of 50 percent to be uniformly mixed, 6 percent of dispersant sodium polyacrylate is added into the deionized water, and the mixture is fully stirred and uniformly mixed to obtain mixed liquid.
Adding 8% of hydrogen peroxide, 1% of chelating agent 1,3-diketone and 3% of stabilizing agent H into the mixed solution in sequence 3 PO 4 2 percent of film-forming agent benzotriazole, 0.05 percent of photocatalyst titanium dioxide with the wavelength of 80nm and 5 percent of defoaming agent emulsified silicone oil, and stirring evenly to obtain a primary mixed liquid.
And dissolving triethanolamine organic strong base serving as a pH regulator to prepare a solution with the concentration of 0.1%, dropwise adding the solution into the primary mixed solution, and regulating the pH value to 10.5 to obtain the polishing solution.
Comparative example 1
Comparative example 1 differs from example 1 in that: this comparative example does not add a stabilizer, and the other conditions are the same.
Comparative example 2
Comparative example 2 differs from example 1 in that: the comparative example does not add a film-forming agent, and the other conditions are the same.
Comparative example 3
Comparative example 3 differs from example 1 in that: the comparative example does not add a photocatalyst, and the other conditions are the same.
Polishing solutions were prepared according to the manufacturing methods of examples 1 to 4 and comparative examples 1 to 3, respectively, and the sedimentation rate of each sample after 5 days was tested to compare the stability thereof, and the specific data are as follows:
| sedimentation Rate (%) | |
| Example 1 | 2.4 |
| Example 2 | 3.6 |
| Example 3 | 2.7 |
| Example 4 | 2.5 |
| Comparative example 1 | 16.8 |
| Comparative example 2 | 2.8 |
| Comparative example 3 | 2.6 |
As can be seen from the data in the table above, the stabilizer affects the stability of the polishing solution, and the stabilizer is beneficial to avoiding aggregation and sedimentation of the abrasive particles.
Polishing solutions are prepared according to the manufacturing methods of the examples 1-4 and the comparative examples 1-3 respectively, diluted to be 10% in content concentration for use, based on the existing CMP technology, the polishing pressure is controlled to be 40kpa, the rotation speed of a polishing surface is controlled to be 150r/min, ultraviolet light is applied, the removal rate (v) of each polishing solution on the surface polishing of the silicon carbide wafer is detected, and the surface polishing condition of the silicon carbide wafer is observed, wherein the specific data are as follows:
| v(nm/min) | characterizing conditions | |
| Example 1 | 1100 | No defect and no damage |
| Example 2 | 1020 | No defect and no damage |
| Example 3 | 1150 | No defect and no damage |
| Example 4 | 980 | No defect and no damage |
| Comparative example 1 | 780 | No defect and no damage |
| Comparative example 2 | 1190 | No defect, micro scratch |
| Comparative example 3 | 830 | No defect and no damage |
From the above table data in conjunction with FIGS. 1-4, it can be seen that: the existence of the stabilizer is beneficial to improving the removal rate of the polishing, and the stabilizer is beneficial to the stabilization of the oxidant, so that the using effect of the stabilizer is better; the high content of the film agent is beneficial to avoiding damaging the surface of the workpiece, but slows down the polishing removal rate to a certain extent; the photocatalyst can catalyze the oxidation rate, so that the polishing removal rate is increased;
it should be noted that, fig. 3 is a schematic view of a polished surface of a workpiece according to the present invention, which is an atomic terrace surface of a silicon carbide workpiece polished by the polishing solution under an atomic force microscope, and shows that the polished surface of the silicon carbide wafer has no obvious groove, no obvious scratch, and no obvious ion residue to meet the quality requirements of customers;
FIG. 4 is a second schematic view of the polished surface of the workpiece of the present invention, which is a comparison between the conventional polishing solution and the polished surface of the polishing solution under a scanning electron microscope, wherein the polishing solution has no sub-surface damage after polishing, and the second schematic view is primarily named as FA1250 polishing solution in order to distinguish the polishing solutions in the drawings.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A polishing liquid for a semiconductor material, characterized in that: the polishing solution comprises 10-50% of abrasive, 2-6% of dispersant, 0.75-8% of oxidant, 0.1-1% of chelating agent, deionized water and a pH regulator, wherein the pH value of the polishing solution is 8-11.5.
2. The polishing liquid for semiconductor materials and the preparation method thereof according to claim 1, wherein: the polishing solution can also be added with other additives, and the other additives comprise any one or more of a stabilizer accounting for 0.5-3% of the total mass of the polishing solution, 0.1-5% of a defoaming agent, 0.05-2% of a photocatalyst and 0.5-2% of a benzotriazole film-forming agent.
3. The polishing liquid for semiconductor materials and the preparation method thereof according to claim 1, wherein: the grinding material is a mixture of alumina, colloidal silica and cerium dioxide with the particle size of 10-260nm, and the mass part ratio of the alumina, the colloidal silica and the cerium dioxide in the mixture is 0.5-3: 1: 0.05-0.3.
4. The polishing liquid for semiconductor materials and the preparation method thereof according to claim 1, wherein: the dispersing agent is any one or more of PEG, polymethyl acrylate, sodium dodecyl benzene sulfonate, sodium polyacrylate and sodium hexametaphosphate.
5. The polishing liquid for semiconductor materials and the preparation method thereof according to claim 1, wherein: the oxidant is one or more of hydrogen peroxide, ferric nitrate, potassium persulfate, potassium ferricyanide, potassium bromate and potassium permanganate.
6. The polishing liquid for semiconductor materials and the preparation method thereof according to claim 1, wherein: the pH regulator adopts any one of sodium hydroxide, potassium hydroxide, ammonia water and organic strong base without metal ions.
7. The polishing liquid for semiconductor materials and the preparation method thereof according to claim 2, wherein: the photocatalyst is any one or more of titanium dioxide, tin dioxide, ferric oxide, zinc oxide and zirconium dioxide.
8. A method for preparing a polishing liquid for semiconductor materials, for preparing the polishing liquid for semiconductor materials according to any one of claims 1 to 7, characterized in that: the preparation method of the polishing solution specifically comprises the following steps:
the method comprises the following steps: abrasive preparation, including colloidal silica abrasive, ceria and alumina abrasive preparation;
step two: respectively selecting the prepared grinding materials, further screening and filtering, weighing the filtered grinding materials according to a proportion, uniformly mixing, putting the uniformly mixed grinding materials into deionized water according to a proportion, adding a dispersing agent into the deionized water, and fully and uniformly stirring to obtain a mixed solution;
step three: adding an oxidant, a stabilizer and a chelating agent into the mixed solution in sequence according to a proportion and uniformly mixing;
step four: continuously dripping the film forming agent and the photocatalyst into the mixed solution according to the proportion, stirring, adding the defoaming agent during stirring, and uniformly stirring to obtain a primary mixed solution;
step five: and dissolving a pH regulator to prepare a solution with the concentration of 0.01-0.1%, dropwise adding the solution into the initial mixed solution, and regulating the pH value to 8-11.5 to obtain the polishing solution.
9. The method for preparing a polishing liquid for semiconductor materials according to claim 8, characterized in that: the specific method for preparing the colloidal silicon dioxide abrasive comprises the following steps:
the method comprises the following steps:
the method comprises the following steps: fully soaking the elemental micro silicon powder by using a hydrofluoric acid reagent with the dilution concentration of 3-15%, taking out the activated micro silicon powder, and rinsing the micro silicon powder for multiple times by using deionized water;
step two: putting the surface-activated silica fume into a reaction vessel, controlling the reaction vessel to be heated to 65-95 ℃, and adding zeolite to avoid bumping;
step three: adding the silicon dioxide dispersion liquid into a reaction container in batches, adding a sodium hydroxide or potassium hydroxide catalyst aqueous solution in batches, and heating to generate hydration reaction to generate hydrogen;
step four: stopping heating after the reaction is finished until no hydrogen exists, cooling to room temperature, and filtering out residual silica fume or impurities in the reaction container through a filtering device to obtain the colloidal silica abrasive with the particle size range of 10-120 nm.
Or the second method:
hydrolysis of ethyl orthosilicate: adding ethyl orthosilicate and deionized water into ethanol or isopropanol solvent, mixing, heating at 50-70 deg.C, stirring, adding alkali catalyst, and hydrolyzing to obtain 60-160nm colloidal silicon dioxide abrasive.
10. The method of preparing a polishing liquid for semiconductor materials according to claim 8, wherein: the preparation method of the cerium dioxide and alumina abrasive comprises the following steps:
the method comprises the following steps: ceCl with the concentration of 0.3mol/L is selected 3 And adding CeCl at a rate of 10-16ml/min 3 0.4mol/L NH with a molar ratio of 1/4 4 HCO 3 Dropwise adding ammonia water, and controlling the initial pH value to be 3-7;
step two: mixing, controlling precipitation temperature at 65-75 deg.C, and adding CeCl dropwise 3 Polyethylene glycol surfactant with mass fraction of 2-5%, controlling aging time for 1.5-2.5h, filtering, and washing with ethanol for multiple times;
step three: controlling the drying temperature to be 95-115 ℃, and drying for 1.5-3h;
step four: controlling the heating rate to be 8-12 ℃/min, heating to the roasting temperature of 450-600 ℃, and preserving heat for 1.8-2.2h to obtain the cerium dioxide powder abrasive with the particle size of 80-260 nm;
step five: selecting an alumina raw material, and crushing and refining the alumina raw material by a ball mill or a pulverizer;
step six: and screening the refined alumina raw material, and screening out alumina raw material particles outside the required particle size range to obtain the alumina powder abrasive meeting the particle size requirement.
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