CN115785818A - Polishing solution and preparation method and application thereof - Google Patents
Polishing solution and preparation method and application thereof Download PDFInfo
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- CN115785818A CN115785818A CN202211404856.6A CN202211404856A CN115785818A CN 115785818 A CN115785818 A CN 115785818A CN 202211404856 A CN202211404856 A CN 202211404856A CN 115785818 A CN115785818 A CN 115785818A
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- 238000005498 polishing Methods 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 66
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000004094 surface-active agent Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002270 dispersing agent Substances 0.000 claims abstract description 35
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000006243 chemical reaction Methods 0.000 claims description 33
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000001354 calcination Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 23
- 238000000227 grinding Methods 0.000 claims description 18
- 229910017855 NH 4 F Inorganic materials 0.000 claims description 17
- 239000002244 precipitate Substances 0.000 claims description 16
- 239000000376 reactant Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [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 10
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 10
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 10
- 238000010000 carbonizing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 19
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 19
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 229910052731 fluorine Inorganic materials 0.000 abstract description 5
- 239000011737 fluorine Substances 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 14
- 239000011521 glass Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002131 composite material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000003082 abrasive agent Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a polishing solution and a preparation method and application thereof, and belongs to the technical field of polishing solution preparation. The polishing solution is prepared from the following raw materials in parts by weight: 50-90 parts of modified alumina; 10-20 parts of zirconium oxide; 1-3 parts of modified cerium oxide; 3-8 parts of a dispersing agent; 0.1 to 1 portion of surfactant; 0.5-0.5 part of pH regulator; 20 to 40 portions of water. The preparation of the polishing solution comprises the following steps: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; then adding a pH regulator, and uniformly stirring again. The invention carries out fluorine doping modification on the aluminum oxide and the cerium oxide, reduces the agglomeration tendency of particles and improves the stability of the system; meanwhile, the aluminum oxide modified by doping fluorine, cerium oxide and zirconium oxide are used in a matching way, and the types of dispersing agents and surfactants are optimized, so that the ultrahigh polishing removal rate and polishing quality are ensured.
Description
Technical Field
The invention belongs to the technical field of polishing solution preparation, and particularly relates to a polishing solution as well as a preparation method and application thereof.
Background
An optical filter is an optical element used to select the desired radiation band, and is made of plastic or glass sheets with special dyes added. An infrared cut-off filter, whose english name is IRCF, is a filter applied to filter infrared bands, and is often installed on a camera of a solid-state electronic device to achieve high transmittance in a visible light region (400 to 630 nm) and cut-off in near infrared (700 to 1100 nm), thereby achieving the purpose of preventing infrared rays from passing through a lens of the camera to avoid picture distortion.
In the preparation of the infrared cut-off filter, a polishing process is included to remove lines, scratches and other flaws on the surface of glass, so that the refractive index and the transparency of the glass are improved; the polishing process uses a polishing liquid. Generally, the polishing solution includes an abrasive, an oxidizing agent, a surfactant, a dispersant, a complexing agent, and the like. Among them, the abrasives, as a main consumable in polishing, play a role of mechanical grinding, and common abrasives are cerium oxide, aluminum oxide, silicon dioxide, diamond, and the like. The selection of other substances such as a surfactant, a dispersing agent and the like is mainly used for improving the dispersibility, the wettability and the like, and the polishing effect is good when the polishing agent is matched with an abrasive. When the abrasive is used, the abrasive can be used singly or compositely; the composite use includes doped composite abrasive, inorganic/inorganic composite abrasive, inorganic/organic composite abrasive, and the like. The abrasive is simple and convenient when being used singly, but has the defects of poor dispersibility and poor polishing effect, for example, the problems of high viscosity and difficult cleaning after polishing exist when the single cerium oxide is used; the single alumina has the problems of poor dispersibility and easy scratch when in use. The composite abrasive material can significantly improve the polishing quality and is more and more concerned by research and development personnel. In the prior art, patent document CN109135580B provides a polishing solution in which alumina and ceria are directly mixed, the amount of ceria used is large, and the polishing effect needs to be further improved.
Therefore, the polishing solution with good polishing effect and good dispersion effect still has important significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a polishing solution and a preparation method and application thereof. The invention carries out fluorine doping modification on aluminum oxide and cerium oxide, reduces the agglomeration tendency of particles and improves the stability of the system; meanwhile, the aluminum oxide modified by doping fluorine, cerium oxide and zirconium oxide are used in a matching way, and the types of dispersing agents and surfactants are optimized, so that the ultrahigh polishing removal rate and polishing quality are ensured.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a polishing solution, which is prepared from the following raw materials in parts by weight: 50-90 parts of modified alumina; 10-20 parts of zirconia; 1-3 parts of modified cerium oxide; 3-8 parts of a dispersing agent; 0.1-1 part of surfactant; 0.5-0.5 part of pH regulator; 20-40 parts of water;
wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by addition of ethanolamine and NH 4 F, heating, stirring and reacting, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant to obtain powder; and then grinding the powder, calcining, and finally washing and drying to obtain the modified alumina.
As a further preferred embodiment of the present invention, the preparation of the modified cerium oxide comprises the following steps: adding Ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, and adding NH 4 HCO 3 Stirring the mixture evenly again and then adding NH 4 F, stirring and heating for reaction after uniform mixing; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate, and grinding after the calcination is finished to obtain the modified cerium oxide.
As further optimization of the technical scheme of the invention, in the preparation process of the modified alumina, al (NO) is added 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
As a further optimization of the technical scheme of the invention, in the preparation process of the modified alumina, the heating and stirring reaction temperature is 65-75 ℃, and the heating and stirring reaction time is 4-8 h; the carbonization temperature is 260 ℃; the calcination temperature is 1050 ℃ and the calcination time is 1.5-3 h.
As further optimization of the technical scheme of the invention, in the preparation process of the modified cerium oxide, ce (NO) is added 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:5 to 15:5 to 10:0.4 to 0.6.
As a further optimization of the technical scheme of the invention, in the preparation process of the modified cerium oxide, the reaction temperature is 80-95 ℃ by stirring and heating, and the reaction time is 4-12 h; the calcining temperature is 900 ℃, and the calcining time is 3-8 h.
As a further preferred embodiment of the present invention, the pH adjuster is one or more selected from sodium hydroxide, potassium hydroxide, and ammonia water.
As a further preferred aspect of the technical solution of the present invention, the dispersant is sodium hexametaphosphate; the surfactant is prepared by mixing 1.2 mass ratio of polyvinylpyrrolidone and sodium dodecyl sulfate.
In a second aspect, the invention provides a method for preparing the polishing solution, which comprises the following steps: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and stirring uniformly again to obtain the polishing solution.
In a third aspect, the invention provides an application of the polishing solution in polishing of an infrared cut filter.
Compared with the prior art, the invention has the following beneficial effects:
(1) The polishing solution provided by the invention is used for polishing blue glass, and has the advantages of high polishing speed, low surface roughness and good polishing quality.
(2) In the polishing solution provided by the invention, three abrasive materials of aluminum oxide, cerium oxide and zirconium oxide are used in a matching way, and the advantages of relatively less scratches of cerium oxide, relatively low surface roughness, high aluminum oxide removal rate and high hardness are combined; meanwhile, the advantage of relatively low hardness of the zirconia is utilized; the three components are used together, so that the hardness of the abrasive is moderate, the polishing speed is high, and the polishing quality is high. Oxidation of three abrasives in the inventionThe usage amount of aluminum is the largest, the rapid polishing removal rate can be guaranteed, the usage amount of cerium oxide is small, the cost is controllable, the usage amount of zirconium oxide is moderate, and the hardness of the grinding material is appropriate. In order to overcome the defects of poor dispersibility and easy agglomeration of alumina and cerium oxide and the defects of large viscosity of zirconia and cerium oxide in use, the invention adopts the following improvement measures, in particular: the invention carries out fluorine doping modification on aluminum oxide and cerium oxide, wherein NH is used 4 F modifies the aluminum oxide and the cerium oxide, can introduce an F element into the aluminum oxide and the cerium oxide, can perform complexation on metal ions in the glass for the optical filter, further improves the polishing rate, and reduces the roughness of the surface of the glass; meanwhile, the agglomeration tendency of the modified aluminum oxide and the modified cerium oxide is reduced, and the stability is good; in addition, the invention also aims at the problem of high viscosity of the composite abrasive, uses the surfactant consisting of polyvinylpyrrolidone and sodium dodecyl sulfate to reduce the surface tension of the system, and uses sodium hexametaphosphate which is an inorganic dispersant in a matching way to improve the dispersibility and suspension stability of the abrasive and ensure the stable dispersion and efficient polishing of the system. Among them, the polyvinyl pyrrolidone is a nonionic surfactant, the sodium dodecyl sulfate is an anionic surfactant, and the combination of the two surfactants has the best effect, which is discovered by the applicant through repeated experiments.
In a word, the fluorine-doped modification is carried out on the aluminum oxide and the cerium oxide, so that the agglomeration tendency of particles is reduced, and the stability of a system is improved; meanwhile, the fluorine-doped modified aluminum oxide, cerium oxide and zirconium oxide are used in a matched manner, and the types of dispersing agents and surfactants are preferably selected, so that the ultrahigh polishing removal rate and polishing quality are ensured.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with 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 obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It is understood that the chemicals or drugs used in the embodiments of the present invention may be purchased from commercial sources, unless otherwise specified.
Wherein the mass purity of the cerium oxide is not lower than 99.9%; the mass purity of the alumina is not lower than 99.99 percent; the specific surface area of the zirconia powder was 6m 2 /g。
Example 1
The polishing solution is prepared from the following raw materials in parts by mass: 70g of modified alumina; 15g parts of zirconia; 2g parts of modified cerium oxide; 5g of a dispersant; 0.6g of a surfactant; 0.5g of sodium hydroxide; 25g of water.
Wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by the addition of ethanolamine and NH 4 F, heating and stirring at 68 ℃ for reaction for 5 hours, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant at 260 ℃ for 8h to obtain powder; and then grinding the powder, calcining the powder for 1.5h at 1050 ℃, and finally washing and drying the powder to obtain the modified alumina.
Wherein Al (NO) 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
Wherein, the preparation of the modified cerium oxide comprises the following steps: adding Ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, and adding NH 4 HCO 3 Stirring the mixture evenly again and then adding NH 4 F, stirring and heating for reaction for 6 hours at 85 ℃ after uniformly mixing; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate at 900 ℃ for 4 hours, and grinding to obtain the modified cerium oxide.
Wherein, in the preparation process of the modified cerium oxide, ce (NO) 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:8:6：0.45。
wherein the surfactant is obtained by mixing polyvinylpyrrolidone and sodium dodecyl sulfate in a mass ratio of 1.2; the dispersant is sodium hexametaphosphate.
In this embodiment, a method for preparing the polishing solution is also provided, which includes the following steps: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and uniformly stirring again to obtain the polishing solution.
Example 2
The polishing solution is prepared from the following raw materials in parts by mass: 75g of modified alumina; 13g parts of zirconium oxide; 2.5g parts of modified cerium oxide; 4g of a dispersant; 0.5g of a surfactant; 0.5g of sodium hydroxide; 28g of water.
Wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by the addition of ethanolamine and NH 4 F, heating and stirring at 70 ℃ for reaction for 4 hours, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant at 260 ℃ for 8h to obtain powder; and then grinding the powder, calcining for 2h at 1050 ℃, and finally washing and drying to obtain the modified alumina.
Wherein Al (NO) 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1.1, NH 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
Wherein, the preparation of the modified cerium oxide comprises the following steps: ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, and adding NH 4 HCO 3 Stirring again and then adding NH 4 F, uniformly mixing, stirring and heating at 90 ℃ for reaction for 4 hours; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate at 900 ℃ for 5 hours, and grinding after the calcination is finished to obtain the modified cerium oxide.
Wherein, in the preparation process of the modified cerium oxide, ce (B)NO 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:10:7:0.5.
wherein the surfactant is obtained by mixing polyvinylpyrrolidone and sodium dodecyl sulfate in a mass ratio of 1.2; the dispersant is sodium hexametaphosphate.
In this embodiment, a method for preparing the polishing solution is also provided, which includes the following steps: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and uniformly stirring again to obtain the polishing solution.
Example 3
The polishing solution is prepared from the following raw materials in parts by mass: 80g of modified alumina; 14g parts of zirconium oxide; 3.5g parts of modified cerium oxide; 4.5g of dispersant; 0.7g of a surfactant; 0.6g of sodium hydroxide; 30g of water.
Wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by the addition of ethanolamine and NH 4 F, heating and stirring at 70 ℃ for reacting for 8 hours, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant at 260 ℃ for 8h to obtain powder; and then grinding the powder, calcining the powder for 3 hours at 1050 ℃, and finally washing and drying the powder to obtain the modified alumina.
Wherein Al (NO) 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
Wherein, the preparation of the modified cerium oxide comprises the following steps: ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, and adding NH 4 HCO 3 Stirring again and then adding NH 4 F, stirring and heating for reaction for 8 hours at 85 ℃ after uniformly mixing; after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate at 900 ℃ for 6h, and calciningAnd grinding after the firing is finished to obtain the modified cerium oxide.
Wherein, in the preparation process of the modified cerium oxide, ce (NO) 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:12:8:0.55.
wherein the surfactant is obtained by mixing polyvinylpyrrolidone and sodium dodecyl sulfate in a mass ratio of 1.2; the dispersant is sodium hexametaphosphate.
In this embodiment, a method for preparing the polishing solution is further provided, including the following steps: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and uniformly stirring again to obtain the polishing solution.
Comparative example 1
The polishing solution is prepared from the following raw materials in parts by mass: 70g of alumina; 15g parts of zirconia; 2g parts of modified cerium oxide; 5g of a dispersant; 0.6g of a surfactant; 0.5g of sodium hydroxide; 25g of water.
Wherein, the preparation of the modified cerium oxide comprises the following steps: adding Ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, adding NH 4 HCO 3 Stirring the mixture evenly again and then adding NH 4 F, uniformly mixing, stirring and heating at 85 ℃ for reaction for 6 hours; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate at 900 ℃ for 4 hours, and grinding after the calcination is finished to obtain the modified cerium oxide.
Wherein, in the preparation process of the modified cerium oxide, ce (NO) 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:8:6:0.45.
wherein the surfactant is obtained by mixing polyvinylpyrrolidone and sodium dodecyl sulfate in a mass ratio of 1.2; the dispersant is sodium hexametaphosphate.
In this comparative example, there is also provided a method for preparing the polishing solution, comprising the steps of: adding aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and uniformly stirring again to obtain the polishing solution.
Comparative example 2
The polishing solution is prepared from the following raw materials in parts by mass: 70g of modified alumina; 15g parts of zirconium oxide; 2g parts of cerium oxide; 5g of a dispersant; 0.6g of a surfactant; 0.5g of sodium hydroxide; 25g of water.
Wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by the addition of ethanolamine and NH 4 F, heating and stirring at 68 ℃ for reaction for 5 hours, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant at 260 ℃ for 8h to obtain powder; and then grinding the powder, calcining the powder for 1.5h at 1050 ℃, and finally washing and drying the powder to obtain the modified alumina.
Wherein Al (NO) 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
Wherein the surfactant is obtained by mixing 1.2 mass ratio of polyvinylpyrrolidone to sodium dodecyl sulfate; the dispersant is sodium hexametaphosphate.
In this comparative example, there is also provided a method for preparing the polishing solution, comprising the steps of: adding modified aluminum oxide, cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and uniformly stirring again to obtain the polishing solution.
Comparative example 3
The polishing solution is prepared from the following raw materials in parts by mass: 70g of modified alumina; 15g parts of zirconium oxide; 2g parts of modified cerium oxide; 5g of a dispersant; 0.6g of a surfactant; 0.5g of sodium hydroxide; 25g of water.
Wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by the addition of ethanolamine and NH 4 F, heating and stirring at 68 ℃ for reaction for 5 hours, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant at 260 ℃ for 8h to obtain powder; and then grinding the powder, calcining the powder for 1.5h at 1050 ℃, and finally washing and drying the powder to obtain the modified alumina.
Wherein Al (NO) 3 ) 3 ·9H 2 The molar use ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
Wherein, the preparation of the modified cerium oxide comprises the following steps: ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, and adding NH 4 HCO 3 Stirring again and then adding NH 4 F, stirring and heating for reaction for 6 hours at 85 ℃ after uniformly mixing; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate at 900 ℃ for 4 hours, and grinding to obtain the modified cerium oxide.
Wherein, in the preparation process of the modified cerium oxide, ce (NO) 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:8:6:0.45.
wherein the surfactant is polyvinylpyrrolidone; the dispersant is sodium hexametaphosphate.
In this comparative example, there is also provided a method for preparing the above polishing liquid, comprising the steps of: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and stirring uniformly again to obtain the polishing solution.
Comparative example 4
The polishing solution is prepared from the following raw materials in parts by mass: 70g of modified alumina; 15g parts of zirconia; 2g parts of modified cerium oxide; 5g of a dispersant; 0.6g of a surfactant; 0.5g of sodium hydroxide; 25g of water.
Wherein, the preparation of the modified aluminaThe method comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by addition of ethanolamine and NH 4 F, heating and stirring at 68 ℃ for reaction for 5 hours, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant at 260 ℃ for 8h to obtain powder; and then grinding the powder, calcining the powder for 1.5 hours at 1050 ℃, and finally washing and drying the powder to obtain the modified alumina.
Wherein Al (NO) 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
Wherein, the preparation of the modified cerium oxide comprises the following steps: adding Ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, adding NH 4 HCO 3 Stirring the mixture evenly again and then adding NH 4 F, stirring and heating for reaction for 6 hours at 85 ℃ after uniformly mixing; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate at 900 ℃ for 4 hours, and grinding to obtain the modified cerium oxide.
Wherein, in the preparation process of the modified cerium oxide, ce (NO) 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:8:6:0.45.
wherein the surfactant is sodium dodecyl sulfate; the dispersant is sodium hexametaphosphate.
In this comparative example, there is also provided a method for preparing the above polishing liquid, comprising the steps of: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and uniformly stirring again to obtain the polishing solution.
The polishing solutions prepared in example 1 and comparative examples 1 to 4 were subjected to polishing performance tests, and the specific test methods and test results were as follows.
And (3) testing the polishing performance: the polishing solutions prepared in example 1 and comparative examples 1 to 4 were used to polish commercially available blue glass substrates of the same lot and the same specification. Firstly, the appearance of the polished and cleaned blue glass is visually observed; then, measuring the surface roughness of the polished glass by using a surface roughness meter; measuring the thickness of the blue glass before polishing by using a thickness gauge; and (3) measuring polishing time, cleaning the glass after polishing, measuring the thickness again, and calculating the removal rate based on the following formula:
removal rate =Δh/t;
wherein, delta h is the thickness change of the blue glass, nm; t is the polishing time, min.
The measurements were performed in parallel and averaged, and the results are shown in Table 1.
TABLE 1 polishing Performance test results
Next, the polishing solutions prepared in example 1 and comparative examples 1 to 4 were subjected to a suspension dispersibility test by the following method: and (3) placing the polishing solution in a 25mL test tube, standing, observing at intervals, and recording the layering data of the powder and the liquid. The test results are shown in Table 2.
Table 2 results of the dispersion suspension test
As can be seen from Table 2, the polishing solution prepared by the embodiment of the invention has good suspension dispersibility and is not easy to agglomerate.
The technical idea of the present invention is illustrated by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must depend on the above embodiments to be implemented. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of individual materials of the product of the present invention, and the addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The polishing solution is characterized by being prepared from the following raw materials in parts by weight: 50-90 parts of modified alumina; 10-20 parts of zirconium oxide; 1-3 parts of modified cerium oxide; 3-8 parts of a dispersing agent; 0.1-1 part of surfactant; 0.5-0.5 part of pH regulator; 20-40 parts of water;
wherein, the preparation of the modified alumina comprises the following steps: mixing Al (NO) 3 ) 3 ·9H 2 Adding O into ethanol, and stirring uniformly; followed by the addition of ethanolamine and NH 4 F, heating, stirring and reacting, and heating to remove ethanol after the reaction is finished to obtain a reactant; then carbonizing the reactant to obtain powder; and then grinding the powder, calcining, and finally washing and drying to obtain the modified alumina.
2. The polishing solution according to claim 1, wherein the preparation of the modified cerium oxide comprises the following steps: adding Ce (NO) 3 ) 3 ·6H 2 Adding O into water, stirring uniformly, and adding NH 4 HCO 3 Stirring the mixture evenly again and then adding NH 4 F, stirring and heating for reaction after uniform mixing; and after the reaction is finished, filtering to obtain a precipitate, calcining the dried precipitate, and grinding to obtain the modified cerium oxide.
3. The polishing solution as set forth in claim 1, wherein Al (NO) is added during the preparation of the modified alumina 3 ) 3 ·9H 2 The molar ratio of O, ethanol and ethanolamine is 1 4 F is added in an amount of Al (NO) 3 ) 3 ·9H 2 3.5 percent of the mass of O.
4. The polishing solution according to claim 1, wherein in the preparation process of the modified alumina, the reaction temperature of heating and stirring is 65-75 ℃, and the reaction time of heating and stirring is 4-8 h; the carbonization temperature is 260 ℃; the calcining temperature is 1050 ℃, and the calcining time is 1.5-3 h.
5. The polishing solution as set forth in claim 2, wherein, in the preparation of the modified cerium oxide, ce (NO) is added 3 ) 3 ·6H 2 O, water, NH 4 HCO 3 And NH 4 The molar use ratio of F is 1:5 to 15:5 to 10:0.4 to 0.6.
6. The polishing solution according to claim 2, wherein in the preparation process of the modified cerium oxide, the reaction temperature is 80-95 ℃ under stirring and heating, and the reaction time is 4-12 h; the calcining temperature is 900 ℃, and the calcining time is 3-8 h.
7. The polishing solution according to claim 1, wherein the pH regulator is one or more selected from the group consisting of sodium hydroxide, potassium hydroxide, and ammonia.
8. The polishing solution according to claim 1, wherein the dispersant is sodium hexametaphosphate; the surfactant is prepared by mixing 1.2 mass ratio of polyvinylpyrrolidone and sodium dodecyl sulfate.
9. The method for preparing a polishing solution according to any one of claims 1 to 8, comprising the steps of: adding modified aluminum oxide, modified cerium oxide and zirconium oxide into water, then adding a dispersing agent and a surfactant, and uniformly stirring; and then adding a pH regulator, and stirring uniformly again to obtain the polishing solution.
10. Use of the polishing liquid according to any one of claims 1 to 8 for polishing an infrared cut filter.
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