CN113980579A - Chemical mechanical polishing slurry and preparation method thereof - Google Patents
Chemical mechanical polishing slurry and preparation method thereof Download PDFInfo
- Publication number
- CN113980579A CN113980579A CN202111345380.9A CN202111345380A CN113980579A CN 113980579 A CN113980579 A CN 113980579A CN 202111345380 A CN202111345380 A CN 202111345380A CN 113980579 A CN113980579 A CN 113980579A
- Authority
- CN
- China
- Prior art keywords
- polishing
- ceo
- sio
- parts
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005498 polishing Methods 0.000 title claims abstract description 148
- 239000002002 slurry Substances 0.000 title claims abstract description 46
- 239000000126 substance Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000007613 slurry method Methods 0.000 title description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 68
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 65
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 65
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 65
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 65
- 239000000843 powder Substances 0.000 claims abstract description 64
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 239000007800 oxidant agent Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- 239000002562 thickening agent Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 238000013329 compounding Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 claims abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 29
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 13
- 229920000570 polyether Polymers 0.000 claims description 13
- MBZLJHHVUVLDSX-UHFFFAOYSA-N cerium hydrochloride Chemical compound Cl.[Ce] MBZLJHHVUVLDSX-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- VJLOFJZWUDZJBX-UHFFFAOYSA-N bis(2-hydroxyethyl)azanium;chloride Chemical compound [Cl-].OCC[NH2+]CCO VJLOFJZWUDZJBX-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- PMUNIMVZCACZBB-UHFFFAOYSA-N 2-hydroxyethylazanium;chloride Chemical compound Cl.NCCO PMUNIMVZCACZBB-UHFFFAOYSA-N 0.000 claims description 3
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 3
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 150000001413 amino acids Chemical class 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- -1 polydimethylsiloxane Polymers 0.000 claims description 3
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 3
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 3
- 229920000136 polysorbate Polymers 0.000 claims description 3
- 229940114930 potassium stearate Drugs 0.000 claims description 3
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 239000000344 soap Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 235000002639 sodium chloride Nutrition 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000004448 titration Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 4
- 230000003628 erosive effect Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000003486 chemical etching Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses chemical mechanical polishing slurry and a preparation method thereof, and relates to the technical field of polishing. The polishing solution comprises, by mass, 15-25 parts of inorganic polishing powder, 5-10 parts of an oxidizing agent, 0.1-1 part of a surfactant, 0.1-1 part of a defoaming agent, 1-2 parts of a thickening agent, 1-2 parts of a pH regulator and 100 parts of deionized water; CeO is adopted as inorganic polishing powder2‑SiO2Compounding polishing powder; the oxidant is nitric acid or sodium dichromate; the pH of the polishing slurry is 7 to 8. CeO of the invention2‑SiO2The composite polishing powder adopts CeO with different proportions2And SiO2Test results show that higher polishing erosion amount can be obtained, and CeO is abandoned2And SiO2The advantages are high grinding quantity, best polishing capacity, long service life, high polishing precision, easy cleaning, low cost and high polishing efficiency.
Description
Technical Field
The invention belongs to the technical field of polishing, and particularly relates to chemical mechanical polishing slurry and a preparation method thereof.
Background
Chemical Mechanical Polishing (CMP), which is a combined technology of mechanical grinding and chemical etching, forms a smooth and flat plane on the surface of a medium to be ground, such as a monocrystalline silicon wafer, an integrated circuit oxide film and a metal film, by means of the grinding effect of ultrafine particles and the chemical etching effect of slurry, and is now the leading technology in the semiconductor processing industry. The traditional mechanical polishing is an important step of a SiC wafer processing procedure, the quality of the processed wafer directly influences the surface quality of a product and the subsequent industrial procedures, the traditional mechanical polishing solution directly adopts silicon dioxide polishing solution, and the defects of low removal rate and long processing time are that a large amount of scratches on the surface of a processed object are easily caused in the actual production process, and the traditional mechanical polishing solution is not suitable for an industrialized sound field.
Silica hydrosol is currently the most representative polishing slurry for CMP, and it is more common to prepare polishing slurry by using polishing powders of silica, iron oxide, zirconia, alumina, chromia and ceria, but because these polishing powders have different hardness, different polishing capabilities and different use costs, the corresponding use scenarios and frequency are different. According to the comparison of the polishing capacities, the grinding amount and the polishing capacity of cerium oxide can be clearly known to be the best, and the polishing capacities of zirconium oxide and titanium oxide are poor and the titanium oxide is the second best; in practical application, cerium oxide is most widely applied in a fine grinding scene, and compared with other polishing powder, the cerium-based rare earth polishing powder has many outstanding advantages, such as good crystal form, high chemical activity, small particle size compared with other polishing powder, long service life, high polishing precision, easy cleaning and high polishing efficiency, but because the rare earth is rare, the cost is high, the price is high, the dispersibility is poor, and the agglomeration is easy to occur; therefore, in order to solve the above problems, a silicon oxide polishing powder with good dispersibility and good chemical stability is combined with cerium oxide, and the material formulation thereof is adjusted to obtain good polishing efficiency and corresponding relatively low cost, which has great potential for the market application of polishing slurry.
Disclosure of Invention
The invention provides a chemical mechanical polishing slurry and a preparation method thereof, which solve the problems.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the chemical mechanical polishing slurry comprises, by mass, 15-25 parts of inorganic polishing powder, 5-10 parts of an oxidizing agent, 0.1-1 part of a surfactant, 0.1-1 part of a defoaming agent, 1-2 parts of a thickening agent, 1-2 parts of a pH regulator and 100 parts of deionized water;
the inorganic polishing powder adopts CeO2-SiO2Compounding polishing powder;
the oxidant is nitric acid or sodium dichromate;
the surfactant is at least one of sodium stearate, potassium stearate, calcium stearate, triethanolamine soap, sodium dodecyl sulfate, dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate, tween 20, tween 40 and tween 60;
the thickener is at least one of monoethanolamine chloride, diethanolamine chloride, sodium sulfate, disodium phosphate and sodium chloride;
the pH regulator is at least one of ethylenediamine, ethanolamine, basic amino acid and ammonia water;
the defoaming agent is at least one of GP type polyether defoaming agent, GPE type polyether defoaming agent, GPES type polyether defoaming agent, polydimethylsiloxane and polyether modified organic silicon defoaming agent;
the pH value of the polishing slurry is 7-8.
A method for preparing chemical mechanical polishing slurry is characterized by comprising the following steps:
s01 preparation of crude CeO2-SiO2Compounding polishing powder: selecting CeO2Fully dissolving cerium carbonate with the concentration of more than or equal to 99.9 percent by hydrochloric acid to prepare a cerium hydrochloride solution with a certain concentration, and carrying out suction filtration, impurity removal and concentration titration on the cerium hydrochloride solution for later use; according to CeO2-SiO2Taking a certain amount of silica sol according to the required preparation proportion, and mixing the following components in percentage by volume: silica sol: anhydrous ethanol: dissolving silica sol in deionized water at a ratio of 1:2:2, and uniformly mixing to obtain a mixed solution A; according to the preparation of CeO2-SiO2Taking a certain amount of cerium hydrochloride solution B according to the mass ratio of the composite polishing powder, fixing the feeding speed, slowly adding the mixed solution A into the cerium hydrochloride solution B for mixing, then adding a proper amount of cetyl trimethyl ammonium bromide, heating in a water bath at the constant temperature of 50 ℃, stirring for 2 hours at the speed of 300r/min by using a stirrer to obtain uniform mixed solution C, then performing spray drying on the obtained mixed solution C on a spray dryer to obtain a mixed precursor, heating the prepared mixed precursor and drying to obtain the mixed precursorRoasting the CeO in the furnace at 980 ℃ for 6 hours, taking out the CeO, cooling the furnace and taking out the CeO to obtain crude CeO2-SiO2Compounding polishing powder;
s02 crude CeO2-SiO2Pretreating the composite polishing powder: the crude CeO obtained2-SiO2Grinding the composite polishing powder and carrying out 220-mesh standard screening to obtain graded fine CeO2-SiO2Compounding polishing powder for later use;
s03, preparing polishing slurry: putting 100 parts by weight of deionized water into a beaker, continuously stirring at a first temperature, and adding 1-2 parts by weight of a thickening agent to obtain a first solution; continuously stirring at a second temperature, and adding 15-25 parts of inorganic polishing powder to obtain a second solution; continuously stirring at a third temperature, and adding 5-10 oxidants to obtain a third solution; continuously stirring at a fourth temperature, and sequentially adding 0.1-1 part of surfactant and 0.1-1 part of defoaming agent to obtain a fourth solution; and finally, continuously stirring at a fifth temperature, and dripping 1-2 parts of a pH regulator to stabilize the pH value to 7-8 to obtain the polishing slurry.
Further, the CeO2-SiO2The required formulation ratios include CeO2/SiO2 in mass ratios of 5:1 or 4:1 or 3:1 or 2:1 or 1: 1.
further, the first temperature is 60-90 ℃, and the corresponding stirring speed is 600-800 r/min; the second temperature is 50-80 ℃, and the corresponding stirring speed is 500-; the third temperature is 40-60 ℃, and the corresponding stirring speed is 400-; the fourth temperature is 25-35 ℃, and the corresponding stirring speed is 300-; the fifth temperature is 22-25 ℃, and the corresponding stirring speed is 300-350 r/min.
Compared with the prior art, the invention has the following beneficial effects:
the chemical mechanical polishing slurry adopts the novel prepared CeO2-SiO2The composite polishing powder is used as a raw material, and a certain amount of oxidant, surfactant, defoaming agent, thickening agent and pH regulator are mixed by using deionized water as a solvent to prepare polishing slurry, CeO2-SiO2The composite polishing powder adopts different proportionsCeO (B) of2And SiO2Test results show that higher polishing erosion amount can be obtained, and CeO is abandoned2And SiO2The respective disadvantages are combined, and the advantages of high grinding amount, best polishing capacity, long service life, high polishing precision, easy cleaning, low cost and high polishing efficiency are achieved, compared with the pure CeO2And SiO2The polishing slurry has obvious excellent effect, greatly improves the polishing efficiency, saves the cost and is convenient for market popularization and application.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a chemical mechanical polishing slurry according to the present invention;
FIG. 2 is a schematic diagram of a method of preparing a chemical mechanical polishing slurry according to the present invention;
FIG. 3 shows crude CeO in FIG. 22-SiO2The specific preparation method of the composite polishing powder is shown in the step diagram.
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 chemical mechanical polishing slurry comprises, by mass, 15-25 parts of inorganic polishing powder, 5-10 parts of an oxidizing agent, 0.1-1 part of a surfactant, 0.1-1 part of a defoaming agent, 1-2 parts of a thickening agent, 1-2 parts of a pH regulator and 100 parts of deionized water;
CeO is adopted as inorganic polishing powder2-SiO2Compounding polishing powder;
the oxidant is nitric acid or sodium dichromate;
the surfactant is at least one of sodium stearate, potassium stearate, calcium stearate, triethanolamine soap, sodium dodecyl sulfate, dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate, tween 20, tween 40 and tween 60;
the thickener is at least one of monoethanolamine chloride, diethanolamine chloride, sodium sulfate, disodium phosphate and sodium chloride;
the pH regulator is at least one of ethylenediamine, ethanolamine, basic amino acid and ammonia water;
the defoaming agent is at least one of GP type polyether defoaming agent, GPE type polyether defoaming agent, GPES type polyether defoaming agent, polydimethylsiloxane and polyether modified organic silicon defoaming agent;
the pH of the polishing slurry is 7 to 8.
Specific example 1:
the chemical mechanical polishing slurry of the embodiment comprises, by mass, 20 parts of inorganic polishing powder, 10 parts of an oxidizing agent, 0.2 part of a surfactant, 0.2 part of a defoaming agent, 1.2 parts of a thickening agent, 1.2 parts of a pH regulator and 100 parts of deionized water;
CeO is adopted as inorganic polishing powder2-SiO2The composite polishing powder is prepared from CeO2-SiO2 in a required proportion by mass2/SiO21: 5; the average diameter of the particle size is 0.154 mu m;
the oxidant is nitric acid or sodium dichromate; the surfactant is 0.5 wt% of sodium dodecyl sulfate; the thickener is 0.8 wt% of diethanolamine chloride; the pH regulator is ammonia water;
the defoaming agent is 0.6 wt% of polyether modified organic silicon type defoaming agent;
the pH value of the polishing slurry is 7;
specific example 2:
this detailed description of the inventionThe difference with respect to example 1 is that CeO was used as the inorganic polishing powder2-SiO2Composite polishing powder, CeO2-SiO2The required prepared proportion is CeO according to the mass ratio2/SiO24: 1; the average diameter of the particle diameter is 0.159 mu m;
specific example 3:
the present embodiment differs from embodiment 1 in that CeO is used as the inorganic polishing powder2-SiO2Composite polishing powder, CeO2-SiO2The required prepared proportion is CeO according to the mass ratio2/SiO21: 3; the average diameter of the particle size is 5.563 mu m;
specific example 4:
the present embodiment differs from embodiment 1 in that CeO is used as the inorganic polishing powder2-SiO2Composite polishing powder, CeO2-SiO2The required preparation proportion is that CeO2/SiO2 is 2:1 according to the mass ratio; the average diameter of the particle diameter is 5.005 mu m;
specific example 5:
the present embodiment differs from embodiment 1 in that CeO is used as the inorganic polishing powder2-SiO2Composite polishing powder, CeO2-SiO2The required prepared proportion is CeO according to the mass ratio2/SiO21: 1; the average diameter of the particle size is 4.557 mu m;
preparing a chemical mechanical polishing slurry corresponding to the specific embodiment 1-5 according to a corresponding preparation method to obtain a corresponding chemical mechanical polishing slurry; and in pure SiO alone2And pure CeO alone2The inorganic polishing powder of (1) was used as a reference example;
reference example 1:
according to the mass percentage, the polishing powder comprises 20 parts of inorganic polishing powder, 10 parts of oxidant, 0.2 part of surfactant, 0.2 part of defoaming agent, 1.2 parts of thickening agent, 1.2 parts of PH regulator and 100 parts of deionized water;
the inorganic polishing powder adopts pure CeO2Polishing powder with average particle diameter of 0.449 μm;
the oxidant is nitric acid or sodium dichromate; the surfactant is 0.5 wt% of sodium dodecyl sulfate; the thickener is 0.8 wt% of diethanolamine chloride; the pH regulator is ammonia water;
reference example 2:
the reference example differs from reference example 1 in that the inorganic polishing powder used was pure SiO2The average diameter of the particle size is 0.191 mu m;
the polishing slurries of the above embodiments 1 to 5 were prepared as follows:
referring to FIGS. 2-3, a method for preparing a chemical mechanical polishing slurry includes the steps of:
s01 preparation of crude CeO2-SiO2Compounding polishing powder: selecting CeO2Fully dissolving cerium carbonate with the concentration of more than or equal to 99.9 percent by hydrochloric acid to prepare a cerium hydrochloride solution with a certain concentration, and carrying out suction filtration, impurity removal and concentration titration on the cerium hydrochloride solution for later use; according to CeO2-SiO2Taking a certain amount of silica sol according to the required preparation proportion, and mixing the following components in percentage by volume: silica sol: anhydrous ethanol: dissolving silica sol in deionized water at a ratio of 1:2:2, and uniformly mixing to obtain a mixed solution A; according to the preparation of CeO2-SiO2Taking a certain amount of cerium hydrochloride solution B according to the mass ratio of the composite polishing powder, fixing the feeding speed, slowly adding the mixed solution A into the cerium hydrochloride solution B for mixing, then adding a proper amount of hexadecyl trimethyl ammonium bromide, carrying out water bath heating at the constant temperature of 50 ℃, stirring for 2 hours at the speed of 300r/min by using a stirrer to obtain uniform mixed solution C, then carrying out spray drying on the obtained mixed solution C on a spray dryer to obtain a mixed precursor, roasting the prepared mixed precursor in a heating furnace at the high temperature of 980 ℃ for 6 hours, taking out the mixed precursor, cooling the heating furnace, and taking out the mixed precursor to obtain crude CeO2-SiO2Compounding polishing powder;
s02 crude CeO2-SiO2Pretreating the composite polishing powder: the crude CeO obtained2-SiO2Grinding the composite polishing powder and carrying out 220-mesh standard screening to obtain graded fine CeO2-SiO2Compounding polishing powder for later use;
s03, preparing polishing slurry: putting 100 parts by weight of deionized water into a beaker, continuously stirring at a first temperature, and adding 1.2 parts by weight of a thickening agent to obtain a first solution; continuously stirring at a second temperature, and adding 20 parts of inorganic polishing powder to obtain a second solution; continuously stirring at a third temperature, and adding 10 oxidizing agents to obtain a third solution; continuously stirring at a fourth temperature, and sequentially adding 0.2 part of surfactant and 0.2 part of defoaming agent to obtain a fourth solution; and finally, continuously stirring at a fifth temperature, and dripping 1-2 parts of a pH regulator to stabilize the pH value to 7-8 to obtain the polishing slurry.
Wherein the first temperature is 90 ℃, and the corresponding stirring speed is 800 r/min; the second temperature is 75 ℃, and the corresponding stirring speed is 600 r/min; the third temperature is 55 ℃, and the corresponding stirring speed is 500 r/min; the fourth temperature is 28 ℃, and the corresponding stirring speed is 320 r/min; the fifth temperature is 23 ℃, and the corresponding stirring speed is 300 r/min.
And, similarly, the pure CeO of the reference example2Polishing powder and pure SiO2Respectively performing the above-mentioned steps of S03;
then, CeO corresponding to examples 1 to 5 was obtained2-SiO2Composite polishing slurry and pure CeO corresponding to reference example 12Polishing slurry, pure SiO comparative to reference example 22Polishing slurry; the polishing pastes of the above examples 1-5 and reference examples 1-2 were used to polish K9 glass respectively at a polishing rate of 130nm/min, the polishing amount of the glass was measured and counted after 2h polishing, and the scratch condition of the glass surface was observed under a 1000-fold microscope.
| Type (B) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Reference example 1 | Reference example 2 |
| Amount of polishing and etching | 0.2958 | 0.2960 | 0.3599 | 0.3203 | 0.3152 | 0.2203 | 0.0799 |
Table 1: throw-out corrosion amount statistical table
As can be seen from the above table, from example 1 to example 5, the polishing amounts of the K9 glasses of the different polishing slurries were increased and then decreased, and the magnitude of the polishing amounts was larger than that of reference examples 1 and 2; thus, it can be seen that CeO2-SiO2Composite polishing slurry relative to pure CeO2Polishing slurry and pure SiO2The polishing slurry has a significantly improved glass polishing effect, and if no substrate flatness is required for the purpose of polishing the glass, CeO, which is the polishing slurry of example 3, is selected2-SiO2，CeO2：SiO2The composite polishing powder with the mass ratio of 3:1 has good effect.
Has the advantages that:
the chemical mechanical polishing slurry adopts the novel prepared CeO2-SiO2The composite polishing powder is used as raw material, and is matched with a certain amount of oxidant, surfactant, defoaming agent and thickening agentMixing the agent and pH regulator with deionized water as solvent to obtain polishing slurry, CeO2-SiO2The composite polishing powder adopts CeO with different proportions2And SiO2Test results show that higher polishing erosion amount can be obtained, and CeO is abandoned2And SiO2The respective disadvantages are combined, and the advantages of high grinding amount, best polishing capacity, long service life, high polishing precision, easy cleaning, low cost and high polishing efficiency are achieved, compared with the pure CeO2And SiO2The polishing slurry has obvious excellent effect, greatly improves the polishing efficiency, saves the cost and is convenient for market popularization and application.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (4)
1. The chemical mechanical polishing slurry is characterized by comprising, by mass, 15-25 parts of inorganic polishing powder, 5-10 parts of an oxidizing agent, 0.1-1 part of a surfactant, 0.1-1 part of a defoaming agent, 1-2 parts of a thickening agent, 1-2 parts of a pH regulator and 100 parts of deionized water;
the inorganic polishing powder adopts CeO2-SiO2Compounding polishing powder;
the oxidant is nitric acid or sodium dichromate;
the surfactant is at least one of sodium stearate, potassium stearate, calcium stearate, triethanolamine soap, sodium dodecyl sulfate, dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate, tween 20, tween 40 and tween 60;
the thickener is at least one of monoethanolamine chloride, diethanolamine chloride, sodium sulfate, disodium phosphate and sodium chloride;
the pH regulator is at least one of ethylenediamine, ethanolamine, basic amino acid and ammonia water;
the defoaming agent is at least one of GP type polyether defoaming agent, GPE type polyether defoaming agent, GPES type polyether defoaming agent, polydimethylsiloxane and polyether modified organic silicon defoaming agent;
the pH value of the polishing slurry is 7-8.
2. The method of preparing a chemical mechanical polishing slurry according to claim 1, comprising the steps of:
s01 preparation of crude CeO2-SiO2Compounding polishing powder: selecting CeO2Fully dissolving cerium carbonate with the concentration of more than or equal to 99.9 percent by hydrochloric acid to prepare a cerium hydrochloride solution with a certain concentration, and carrying out suction filtration, impurity removal and concentration titration on the cerium hydrochloride solution for later use; according to CeO2-SiO2Taking a certain amount of silica sol according to the required preparation proportion, and mixing the following components in percentage by volume: silica sol: anhydrous ethanol: dissolving silica sol in deionized water at a ratio of 1:2:2, and uniformly mixing to obtain a mixed solution A; according to the preparation of CeO2-SiO2Taking a certain amount of cerium hydrochloride solution B according to the mass ratio of the composite polishing powder, fixing the feeding speed, slowly adding the mixed solution A into the cerium hydrochloride solution B for mixing, then adding a proper amount of hexadecyl trimethyl ammonium bromide, carrying out water bath heating at the constant temperature of 50 ℃, stirring for 2 hours at the speed of 300r/min by using a stirrer to obtain uniform mixed solution C, then carrying out spray drying on the obtained mixed solution C on a spray dryer to obtain a mixed precursor, roasting the prepared mixed precursor in a heating furnace at the high temperature of 980 ℃ for 6 hours, taking out the mixed precursor, cooling the heating furnace, and taking out the mixed precursor to obtain crude CeO2-SiO2Compounding polishing powder;
s02 crude CeO2-SiO2Pretreating the composite polishing powder: the crude CeO obtained2-SiO2Grinding the composite polishing powder and carrying out 220-mesh standard screening to obtain graded fine CeO2-SiO2Compounding polishing powder for later use;
s03, preparing polishing slurry: putting 100 parts by weight of deionized water into a beaker, continuously stirring at a first temperature, and adding 1-2 parts by weight of a thickening agent to obtain a first solution; continuously stirring at a second temperature, and adding 15-25 parts of inorganic polishing powder to obtain a second solution; continuously stirring at a third temperature, and adding 5-10 oxidants to obtain a third solution; continuously stirring at a fourth temperature, and sequentially adding 0.1-1 part of surfactant and 0.1-1 part of defoaming agent to obtain a fourth solution; and finally, continuously stirring at a fifth temperature, and dripping 1-2 parts of a pH regulator to stabilize the pH value to 7-8 to obtain the polishing slurry.
3. The method of claim 2, wherein the CeO is used for the chemical mechanical polishing2-SiO2The required prepared proportion comprises CeO according to the mass ratio2/SiO2Either 5:1 or 4:1 or 3:1 or 2:1 or 1: 1.
4. the method as claimed in claim 2, wherein the first temperature is 60-90 ℃ and the stirring speed is 600-; the second temperature is 50-80 ℃, and the corresponding stirring speed is 500-; the third temperature is 40-60 ℃, and the corresponding stirring speed is 400-; the fourth temperature is 25-35 ℃, and the corresponding stirring speed is 300-; the fifth temperature is 22-25 ℃, and the corresponding stirring speed is 300-350 r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111345380.9A CN113980579A (en) | 2021-11-15 | 2021-11-15 | Chemical mechanical polishing slurry and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111345380.9A CN113980579A (en) | 2021-11-15 | 2021-11-15 | Chemical mechanical polishing slurry and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113980579A true CN113980579A (en) | 2022-01-28 |
Family
ID=79748417
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111345380.9A Pending CN113980579A (en) | 2021-11-15 | 2021-11-15 | Chemical mechanical polishing slurry and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113980579A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115975510A (en) * | 2022-12-30 | 2023-04-18 | 江苏山水半导体科技有限公司 | Preparation method of silicon polishing solution |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475791A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation and use of cerium oxide / silicon oxide compound abrasive |
| CN103992743A (en) * | 2014-05-09 | 2014-08-20 | 杰明纳微电子股份有限公司 | Polishing solution containing ceric oxide powder/colloid silicon dioxide mixed abrasive and preparing process thereof |
| CN104017501A (en) * | 2014-06-12 | 2014-09-03 | 江南大学 | Ultrasonic atomization-type polishing solution suitable for TFT-LCD (Thin Film Transistor-Liquid Crystal Display) glass substrate |
| CN106281045A (en) * | 2016-08-11 | 2017-01-04 | 广州市新稀冶金化工有限公司 | A kind of nano material formula for precision stainless steel polishing and preparation technology thereof |
| CN107129762A (en) * | 2017-05-12 | 2017-09-05 | 江南大学 | A kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof |
| CN107177315A (en) * | 2017-06-18 | 2017-09-19 | 常州朋悦纺织品有限公司 | A kind of Precision Machining chemical mechanical polishing liquid |
| CN112574675A (en) * | 2019-09-27 | 2021-03-30 | 比亚迪股份有限公司 | Glass polishing solution, preparation method thereof and polishing method using glass polishing solution |
-
2021
- 2021-11-15 CN CN202111345380.9A patent/CN113980579A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475791A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation and use of cerium oxide / silicon oxide compound abrasive |
| CN103992743A (en) * | 2014-05-09 | 2014-08-20 | 杰明纳微电子股份有限公司 | Polishing solution containing ceric oxide powder/colloid silicon dioxide mixed abrasive and preparing process thereof |
| CN104017501A (en) * | 2014-06-12 | 2014-09-03 | 江南大学 | Ultrasonic atomization-type polishing solution suitable for TFT-LCD (Thin Film Transistor-Liquid Crystal Display) glass substrate |
| CN106281045A (en) * | 2016-08-11 | 2017-01-04 | 广州市新稀冶金化工有限公司 | A kind of nano material formula for precision stainless steel polishing and preparation technology thereof |
| CN107129762A (en) * | 2017-05-12 | 2017-09-05 | 江南大学 | A kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof |
| CN107177315A (en) * | 2017-06-18 | 2017-09-19 | 常州朋悦纺织品有限公司 | A kind of Precision Machining chemical mechanical polishing liquid |
| CN112574675A (en) * | 2019-09-27 | 2021-03-30 | 比亚迪股份有限公司 | Glass polishing solution, preparation method thereof and polishing method using glass polishing solution |
Non-Patent Citations (4)
| Title |
|---|
| AILIAN CHEN ET AL.: "Dependency of structural change and polishing efficiency of meso-silica/ceria core/shell composite abrasives on calcination temperatures", 《JOURNAL OF MATERIALS SCIENCE: MATERIALS IN ELECTRONICS》 * |
| 孙秋霞: "氧化铈研磨材料的制备及研究", 《郑州大学硕士学位论文》 * |
| 柴明霞等: "SiO_2-CeO_2复合氧化物的制备及抛光性能", 《无机化学学报》 * |
| 韩磊等: "喷雾干燥法制备CeO2-SiO2复合抛光粉", 《中国粉体技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115975510A (en) * | 2022-12-30 | 2023-04-18 | 江苏山水半导体科技有限公司 | Preparation method of silicon polishing solution |
| CN115975510B (en) * | 2022-12-30 | 2023-10-31 | 江苏山水半导体科技有限公司 | Preparation method of silicon polishing solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7601273B2 (en) | Polishing slurry composition and method of using the same | |
| WO2012102187A1 (en) | Cmp polishing fluid, method for manufacturing same, method for manufacturing composite particle, and method for polishing base material | |
| CN113930165B (en) | Grinding aid, preparation method and application thereof, grinding fluid and grinding method | |
| CN107189693B (en) | Polishing solution for chemical mechanical polishing of A-direction sapphire and preparation method thereof | |
| CN111040640A (en) | Composite abrasive chemical mechanical polishing slurry for silicon wafer substrate and preparation method thereof | |
| CN113549399B (en) | Chemical mechanical polishing composition suitable for rough polishing of silicon wafer and application thereof | |
| CN105950021A (en) | Aluminum oxide base polishing solution for sapphire substrate polishing and preparation method thereof | |
| JP3782771B2 (en) | Abrasive grain and method for producing abrasive | |
| US20080135520A1 (en) | Chemical composition for chemical mechanical planarization | |
| CN113980579A (en) | Chemical mechanical polishing slurry and preparation method thereof | |
| CN112521864A (en) | Chemical mechanical polishing solution for semiconductor silicon carbide chip | |
| CN111073520A (en) | Polishing powder for polishing silicon carbide wafer, preparation method thereof and polishing solution | |
| CN112975736A (en) | Grinding method of indium phosphide wafer | |
| CN115160934A (en) | Super-hydrophilic large-size silicon fine polishing solution and preparation and application methods thereof | |
| CN114591684B (en) | Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof | |
| CN101781524A (en) | Wafer precise polishing solution | |
| US20020170237A1 (en) | Polishing slurry for the chemical-mechanical polishing of silica films | |
| CN113150696B (en) | Polishing solution for reducing micro scratches on surface of silicon wafer | |
| CN101665661A (en) | Application of amine compounds and chemical mechanical polishing solution | |
| WO2019207926A1 (en) | Polishing agent for synthetic quartz glass substrates, method for producing same, and method for polishing synthetic quartz glass substrate | |
| JPH10106988A (en) | Cerium oxide abrasive agent and polishing method of substrate | |
| CN107353833B (en) | Preparation process of high-selectivity shallow-trench-isolation chemical mechanical polishing slurry | |
| JP2001007059A (en) | Cmp-polishing agent and method for polishing substrate | |
| CN114477190A (en) | Preparation method and application of silica sol for chemical polishing | |
| CN114684846A (en) | Synthesis method and use method of cerium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220128 |
|
| RJ01 | Rejection of invention patent application after publication |