CN102250552B - A kind of preparation method of cerium-doped zirconia composite polishing powder - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 56
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000005498 polishing Methods 0.000 title claims abstract description 40
- 239000000843 powder Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- RCFVMJKOEJFGTM-UHFFFAOYSA-N cerium zirconium Chemical compound [Zr].[Ce] RCFVMJKOEJFGTM-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002244 precipitate Substances 0.000 claims abstract description 33
- 150000003754 zirconium Chemical class 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 15
- 150000000703 Cerium Chemical class 0.000 claims abstract description 11
- 239000007800 oxidant agent Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 150000007530 organic bases Chemical class 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 8
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012670 alkaline solution Substances 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 241000143437 Aciculosporium take Species 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 claims description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 4
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 claims description 3
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000005304 optical glass Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- SMKFCFKIYPLYNY-UHFFFAOYSA-K cerium(3+);trichloride;hydrate Chemical compound O.Cl[Ce](Cl)Cl SMKFCFKIYPLYNY-UHFFFAOYSA-K 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
本发明公开的一种铈掺杂的氧化锆复合抛光粉的制备方法，涉及稀土抛光粉材料制备技术领域，其工艺过程为：配制锆盐溶液；将铈盐加入到锆盐溶液中，成为锆盐铈盐混合溶液；配制成有机碱溶液，并加入有机溶剂，成为碱溶液；将碱溶液加入锆盐铈盐混合溶液中进行中和反应，并加入氧化剂，陈化，过滤，得沉淀物；将沉淀物洗涤，得锆铈复合沉淀物；将锆铈复合沉淀物进行恒温干燥，得锆铈复合物；将锆铈复合物煅烧，即得铈掺杂的氧化锆复合抛光粉；具有以非稀土原料为基质、能够替代稀土抛光粉、且在制备过程中环保性较好等特点，应用本发明制备的铈掺杂的氧化锆复合抛光粉，可用于光学玻璃、透镜、液晶显示屏、半导体等抛光。The invention discloses a method for preparing a cerium-doped zirconia composite polishing powder, which relates to the technical field of preparation of rare earth polishing powder materials. The process is as follows: preparing a zirconium salt solution; A mixed solution of salt and cerium salt; prepared into an organic alkali solution, and adding an organic solvent to form an alkali solution; adding the alkali solution into the mixed solution of zirconium salt and cerium salt for neutralization reaction, adding an oxidizing agent, aging, and filtering to obtain a precipitate; The precipitate is washed to obtain a zirconium-cerium composite precipitate; the zirconium-cerium composite precipitate is dried at a constant temperature to obtain a zirconium-cerium composite; the zirconium-cerium composite is calcined to obtain a cerium-doped zirconia composite polishing powder; The rare earth raw material is the matrix, can replace the rare earth polishing powder, and has good environmental protection in the preparation process. The cerium-doped zirconia composite polishing powder prepared by the present invention can be used in optical glass, lens, liquid crystal display, semiconductor, etc. Wait for polishing.
Description
技术领域 technical field
本发明涉及稀土抛光粉材料制备技术领域，特别是一种铈掺杂的氧化锆复合抛光粉的制备方法。The invention relates to the technical field of preparation of rare earth polishing powder materials, in particular to a preparation method of cerium-doped zirconia composite polishing powder.
背景技术 Background technique
氧化铈作为效果最好的稀土抛光材料广泛应用于光学玻璃、透镜、液晶显示屏、半导体等抛光，仅次于其抛光效果的是氧化锆，但是氧化锆的使用寿命较氧化铈差。As the rare earth polishing material with the best effect, cerium oxide is widely used in the polishing of optical glass, lenses, liquid crystal displays, semiconductors, etc. The polishing effect is second only to zirconia, but the service life of zirconia is worse than that of cerium oxide.
由于稀土是一种战略性物资，目前，国家出台了稀土保护性政策，不仅对稀土开采进行了严格控制，并且大幅上调了稀土出口配额，来保护我国珍贵的稀土资源不被浪费，因此，以稀土原料为基质的抛光材料的制备和应用，受到原料来源的限制和价格高的制约。同时，现有以稀土原料为基质的抛光材料的制备过程中，需要使用氢氟酸、氟硅酸、氟化酸铵等物质，这些物质对环境及人体有较大的危害。Since rare earth is a kind of strategic material, at present, the state has issued a rare earth protection policy, which not only strictly controls the mining of rare earth, but also greatly increases the export quota of rare earth to protect my country's precious rare earth resources from being wasted. The preparation and application of polishing materials based on rare earth raw materials are restricted by the limitation of raw material sources and high price. At the same time, in the preparation process of existing polishing materials based on rare earth raw materials, hydrofluoric acid, fluorosilicic acid, ammonium fluoride and other substances need to be used, and these substances are relatively harmful to the environment and human body.
发明内容 Contents of the invention
针对现有技术所存在的不足，本发明所要解决的技术问题是提供一种以非稀土原料为基质、能够替代稀土抛光粉、且在制备过程中环保性较好的抛光材料制备方法。Aiming at the deficiencies in the prior art, the technical problem to be solved by the present invention is to provide a polishing material preparation method that uses non-rare earth raw materials as the matrix, can replace rare earth polishing powder, and has better environmental protection during the preparation process.
本发明所采取的技术方案是发明一种铈掺杂的氧化锆复合抛光粉的制备方法，其工艺流程如下：The technical scheme adopted in the present invention is to invent a kind of preparation method of cerium-doped zirconia composite polishing powder, and its technological process is as follows:
A、取一定量的锆盐，配制成锆盐含量为150g/L-200g/L的水溶液，成为锆盐溶液，备用；A. Take a certain amount of zirconium salt and prepare an aqueous solution with a zirconium salt content of 150g/L-200g/L to become a zirconium salt solution for subsequent use;
B、按锆盐物质量的5％-7％取一定量的铈盐，加入到备用的锆盐溶液中，成为锆盐铈盐混合溶液，备用；B, get a certain amount of cerium salt by 5%-7% of the zirconium salt substance quality, join in the standby zirconium salt solution, become zirconium salt cerium salt mixed solution, standby;
C、取一定量的有机碱，配制成有机碱含量为200g/L-300g/L的有机碱溶液，并加入占有机碱溶液总重量0.05％-0.5％的有机溶剂，混合均匀，成为碱溶液，备用；C. Take a certain amount of organic base, prepare an organic base solution with an organic base content of 200g/L-300g/L, add an organic solvent that occupies 0.05%-0.5% of the total weight of the organic base solution, and mix well to form an alkaline solution ,spare;
D、将上述备用的锆盐铈盐混合溶液在加热的条件下，一边搅拌一边慢慢加入上述备用的碱溶液，进行中和反应，其中锆盐铈盐混合溶液与碱溶液的有效物质的摩尔比为1∶2-1∶6，反应温度控制在40-100℃；待中和反应完全后，按照铈锆质量比的2-5倍加入氧化剂，并停止搅拌，陈化2-6小时；然后，过滤，得沉淀物，备用；D, the above-mentioned standby zirconium salt cerium salt mixed solution is under the condition of heating, slowly add the above-mentioned standby alkali solution while stirring, and carry out neutralization reaction, wherein the mole of the effective substance of the zirconium salt cerium salt mixed solution and the alkali solution The ratio is 1:2-1:6, and the reaction temperature is controlled at 40-100°C; after the neutralization reaction is complete, add an oxidant according to 2-5 times the mass ratio of cerium to zirconium, stop stirring, and age for 2-6 hours; Then, filter to get the precipitate and set aside;
E、将备用的沉淀物洗涤2-4次，得锆铈复合沉淀物，备用；E, wash the standby precipitate 2-4 times to obtain the zirconium-cerium composite precipitate, and set aside;
F、将备用的锆铈复合沉淀物在85-150℃温度下进行恒温干燥24小时，得锆铈复合物，备用；F. Dry the spare zirconium-cerium composite precipitate at a temperature of 85-150°C for 24 hours at a constant temperature to obtain a zirconium-cerium composite, which is ready for use;
G、将备用的锆铈复合物经850-1300℃温度煅烧2-4小时，即得铈掺杂的氧化锆复合抛光粉；G. Calcining the spare zirconium-cerium composite at a temperature of 850-1300° C. for 2-4 hours to obtain cerium-doped zirconia composite polishing powder;
H、所述的锆盐，是水合氧氯化锆、水合碳酸锆、水合硝酸氧锆中的一种；所述的铈盐，是水合硝酸铈、水合氯化铈中的一种；所述的有机碱，是氨水、尿素、六亚甲基四胺中的一种或二种或三种；所述的氧化剂，是过氧化氢、高锰酸钾、高氯酸钾中的一种或二种或三种作为氧化剂；所述的有机溶剂，是聚乙二醇、聚丙烯酸、有机硅的一种或二种或三种。H, the zirconium salt is one of hydrated zirconium oxychloride, hydrated zirconium carbonate, and hydrated zirconyl nitrate; the described cerium salt is one of hydrated cerium nitrate and hydrated cerium chloride; The organic base is one or two or three of ammonia, urea, and hexamethylenetetramine; the oxidizing agent is one or two of hydrogen peroxide, potassium permanganate, and potassium perchlorate or three as oxidant; the organic solvent is one or two or three of polyethylene glycol, polyacrylic acid and organic silicon.
其优化的技术方案的工艺流程如下：The technological process of its optimized technical scheme is as follows:
A、取一定量的锆盐，配制成锆盐含量为180g/L-190g/L的水溶液，成为锆盐溶液，备用；A. Take a certain amount of zirconium salt and prepare it into an aqueous solution with a zirconium salt content of 180g/L-190g/L to become a zirconium salt solution for subsequent use;
B、按锆盐物质量的5％-7％取一定量的铈盐，加入到备用的锆盐溶液中，成为锆盐铈盐混合溶液，备用；B, get a certain amount of cerium salt by 5%-7% of the zirconium salt substance quality, join in the standby zirconium salt solution, become zirconium salt cerium salt mixed solution, standby;
C、取一定量的有机碱，配制成有机碱含量为250g/L-260g/L的有机碱溶液，并加入占有机碱溶液总重量0.1％-0.2％的有机溶剂，混合均匀，成为碱溶液，备用；C. Take a certain amount of organic base, prepare an organic base solution with an organic base content of 250g/L-260g/L, add an organic solvent that occupies 0.1%-0.2% of the total weight of the organic base solution, and mix well to form an alkaline solution ,spare;
D、将上述备用的锆盐铈盐混合溶液在加热的条件下，一边搅拌一边慢慢加入上述备用的碱溶液，进行中和反应，其中锆盐铈盐混合溶液与碱溶液的有效物质的摩尔比为1∶3-1∶5；反应温度控制在50-80℃；待中和反应完全后，按照铈物质量比的2-5倍加入氧化剂，并停止搅拌，陈化3-5小时；然后，过滤，得沉淀物，备用；D, the above-mentioned standby zirconium salt cerium salt mixed solution is under the condition of heating, slowly add the above-mentioned standby alkali solution while stirring, and carry out neutralization reaction, wherein the mole of the effective substance of the zirconium salt cerium salt mixed solution and the alkali solution The ratio is 1:3-1:5; the reaction temperature is controlled at 50-80°C; after the neutralization reaction is complete, add an oxidant according to 2-5 times the mass ratio of cerium, stop stirring, and age for 3-5 hours; Then, filter to get the precipitate and set aside;
E、将备用的沉淀物洗涤2-4次，得锆铈复合沉淀物，备用；E, wash the standby precipitate 2-4 times to obtain the zirconium-cerium composite precipitate, and set aside;
F、将备用的锆铈复合沉淀物在85-150℃温度下进行恒温干燥24小时，得锆铈复合物，备用；F. Dry the spare zirconium-cerium composite precipitate at a temperature of 85-150°C for 24 hours at a constant temperature to obtain a zirconium-cerium composite, which is ready for use;
G、将备用的锆铈复合物经900-1100℃温度煅烧2-4小时，即得铈掺杂的氧化锆复合抛光粉。G. Calcining the spare zirconium-cerium composite at 900-1100° C. for 2-4 hours to obtain cerium-doped zirconia composite polishing powder.
上述各技术方案中，当采用氨水、尿素、六亚甲基四胺中的二种或三种配制碱溶液时，其各组份的用量一般采用所需碱溶液的摩尔比等量来配制；In each of the above technical solutions, when two or three of ammonia, urea, and hexamethylenetetramine are used to prepare the alkali solution, the amount of each component is generally prepared in equivalent molar ratios of the required alkali solution;
当采用过氧化氢、高锰酸钾、高氯酸钾中的二种或三种作为氧化剂，其各组份的用量一般采用所需碱溶液的摩尔比等量来配制；When two or three of hydrogen peroxide, potassium permanganate, and potassium perchlorate are used as the oxidizing agent, the amount of each component is generally prepared in equivalent molar ratios of the required alkali solution;
当采用聚乙二醇400、聚丙烯酸、有机硅的二种或三种配制有机溶剂时，其各组份的用量一般采用所需碱溶液的摩尔比等量来配制；When two or three kinds of polyethylene glycol 400, polyacrylic acid, and organic silicon are used to prepare organic solvents, the dosage of each component is generally prepared by using the molar ratio equivalent of the required alkali solution;
本发明的铈掺杂的氧化锆复合抛光粉的制备方法，采用氧化锆为基质，掺杂少量的氧化铈，通过有机碱的中和，所得沉淀物经过高温煅烧所成，因而，节约了大量的稀土材料；同时，在制备过程中，不需要使用对环境及人体有较大危害的氢氟酸、氟硅酸、氟化酸铵等物质，故其环保性较好。其产品“铈掺杂的氧化锆复合抛光粉”经过试验，具有较好的抛光效果，以下即为铈掺杂的氧化锆复合抛光粉与稀土抛光粉抛光效果对比表：The preparation method of the cerium-doped zirconia composite polishing powder of the present invention adopts zirconia as a matrix, doped with a small amount of cerium oxide, neutralizes with an organic base, and calcines the obtained precipitate at a high temperature, thus saving a large amount of At the same time, in the preparation process, there is no need to use hydrofluoric acid, fluosilicic acid, ammonium fluoride and other substances that are harmful to the environment and human body, so its environmental protection is better. Its product "cerium-doped zirconia composite polishing powder" has been tested and has a good polishing effect. The following is the comparison table of the polishing effects of cerium-doped zirconia composite polishing powder and rare earth polishing powder:
具体实施方式 Detailed ways
以下结合实施例，对本发明作进一步的说明。下面的说明是采用例举的方式，但本发明的保护范围不应局限于此。Below in conjunction with embodiment, the present invention will be further described. The following description is by way of example, but the protection scope of the present invention should not be limited thereto.
实施例一：Embodiment one:
本实施例的铈掺杂的氧化锆复合抛光粉的制备方法，其工艺流程如下：A、取1308g水合氧氯化锆，加入到7L水中，配制成为锆盐溶液，备用；The preparation method of the cerium-doped zirconia composite polishing powder of the present embodiment is as follows: A. Take 1308g hydrated zirconium oxychloride, add it to 7L water, prepare it as a zirconium salt solution, and set aside;
B、取55g水合氯化铈，加入到备用的锆盐溶液中，配制成为锆盐铈盐混合溶液，备用；B, get 55g cerium chloride hydrate, join in the standby zirconium salt solution, be mixed with zirconium salt cerium salt mixed solution, standby;
C、取589g氨水，溶于2.3L水中，并加入4.6g聚乙二醇400，混合均匀，成为碱溶液，备用；C. Take 589g of ammonia water, dissolve it in 2.3L of water, add 4.6g of polyethylene glycol 400, mix evenly, become an alkaline solution, and set aside;
D、将上述备用的锆盐铈盐混合溶液在加热的条件下，一边搅拌一边慢慢加入上述备用的碱溶液，进行中和反应，反应温度控制在50℃；待中和反应完全后，加入10g过氧化氢，并停止搅拌，陈化4小时；然后，过滤，得沉淀物，备用；D. Under the condition of heating the above-mentioned spare zirconium salt and cerium salt mixed solution, slowly add the above-mentioned standby alkali solution while stirring, and carry out neutralization reaction, and the reaction temperature is controlled at 50°C; after the neutralization reaction is complete, add 10g hydrogen peroxide, stop stirring, and age for 4 hours; then, filter to obtain a precipitate and set aside;
E、将备用的沉淀物洗涤3次，得锆铈复合沉淀物，备用；E, wash the spare precipitate 3 times to obtain the zirconium-cerium composite precipitate, which is standby;
F、将备用的锆铈复合沉淀物在95℃温度下进行恒温干燥24小时，得锆铈复合物，备用；F. Dry the spare zirconium-cerium composite precipitate at a temperature of 95°C for 24 hours at a constant temperature to obtain a zirconium-cerium composite, which is ready for use;
G、将备用的锆铈复合物经950℃温度煅烧3小时，即得525克铈掺杂的氧化锆复合抛光粉。G. Calcining the spare zirconium-cerium composite at 950° C. for 3 hours to obtain 525 grams of cerium-doped zirconia composite polishing powder.
实施例二：Embodiment two:
本实施例的铈掺杂的氧化锆复合抛光粉的制备方法，其工艺流程如下：The preparation method of the cerium-doped zirconia composite polishing powder of the present embodiment, its technological process is as follows:
A、取1190g水合碳酸锆，加入到6.6L水中，配制成为锆盐溶液，备用；A, get 1190g hydrated zirconium carbonate, join in 6.6L water, be mixed with zirconium salt solution, standby;
B、取45g水合硝酸铈，加入到备用的锆盐溶液中，配制成为锆盐铈盐混合溶液，备用；B, get 45g hydrated cerium nitrate, join in the standby zirconium salt solution, be mixed with zirconium salt cerium salt mixed solution, standby;
C、取568g氨水和11g尿素，溶于2.3L水中，并加入4.6g聚乙二醇400，混合均匀，成为碱溶液，备用；C. Take 568g of ammonia water and 11g of urea, dissolve them in 2.3L of water, add 4.6g of polyethylene glycol 400, mix evenly, become an alkaline solution, and set aside;
D、将上述备用的锆盐铈盐混合溶液在加热的条件下，一边搅拌一边慢慢加入上述备用的碱溶液，进行中和反应，反应温度控制在50℃；待中和反应完全后，加入5g过氧化氢、45g高锰酸钾，并停止搅拌，陈化4小时；然后，过滤，得沉淀物，备用；D. Under the condition of heating the above-mentioned spare zirconium salt and cerium salt mixed solution, slowly add the above-mentioned standby alkali solution while stirring, and carry out neutralization reaction, and the reaction temperature is controlled at 50°C; after the neutralization reaction is complete, add 5g hydrogen peroxide, 45g potassium permanganate, stop stirring, and age for 4 hours; then, filter to obtain a precipitate and set aside;
E、将备用的沉淀物洗涤3次，得锆铈复合沉淀物，备用；E, wash the spare precipitate 3 times to obtain the zirconium-cerium composite precipitate, which is standby;
F、将备用的锆铈复合沉淀物在95℃温度下进行恒温干燥24小时，得锆铈复合物，备用；F. Dry the spare zirconium-cerium composite precipitate at a temperature of 95°C for 24 hours at a constant temperature to obtain a zirconium-cerium composite, which is ready for use;
G、将备用的锆铈复合物经950℃温度煅烧3小时，即得525克铈掺杂的氧化锆复合抛光粉。G. Calcining the spare zirconium-cerium composite at 950° C. for 3 hours to obtain 525 grams of cerium-doped zirconia composite polishing powder.
实施例三：Embodiment three:
本实施例的铈掺杂的氧化锆复合抛光粉的制备方法，其工艺流程如下：The preparation method of the cerium-doped zirconia composite polishing powder of the present embodiment, its technological process is as follows:
A、取1742g水合硝酸氧锆，加入到9.6L水中，配制成为锆盐溶液，备用；A, get 1742g zirconium oxynitrate hydrate, join in 9.6L water, be mixed with zirconium salt solution, standby;
B、取45g水合硝酸铈，加入到备用的锆盐溶液中，配制成为锆盐铈盐混合溶液，备用；B, get 45g hydrated cerium nitrate, join in the standby zirconium salt solution, be mixed with zirconium salt cerium salt mixed solution, standby;
C、取497g氨水、37g尿素、81g六亚甲基四胺，溶于2.5L水中，并加入5.0g聚丙烯酸，混合均匀，成为碱溶液，备用；C. Take 497g of ammonia water, 37g of urea, and 81g of hexamethylenetetramine, dissolve them in 2.5L of water, add 5.0g of polyacrylic acid, mix well, and make an alkaline solution for later use;
D、将上述备用的锆盐铈盐混合溶液在加热的条件下，一边搅拌一边慢慢加入上述备用的碱溶液，进行中和反应，反应温度控制在50℃；待中和反应完全后，加入3.8g过氧化氢、30.6g高锰酸钾、26.8g高氯酸钾，并停止搅拌，陈化4小时；然后，过滤，得沉淀物，备用；D. Under the condition of heating the above-mentioned spare zirconium salt and cerium salt mixed solution, slowly add the above-mentioned standby alkali solution while stirring, and carry out neutralization reaction, and the reaction temperature is controlled at 50°C; after the neutralization reaction is complete, add 3.8g hydrogen peroxide, 30.6g potassium permanganate, 26.8g potassium perchlorate, stop stirring, and age for 4 hours; then, filter to obtain a precipitate and set aside;
E、将备用的沉淀物洗涤3次，得锆铈复合沉淀物，备用；E, wash the spare precipitate 3 times to obtain the zirconium-cerium composite precipitate, which is standby;
F、将备用的锆铈复合沉淀物在95℃温度下进行恒温干燥24小时，得锆铈复合物，备用；F. Dry the spare zirconium-cerium composite precipitate at a temperature of 95°C for 24 hours at a constant temperature to obtain a zirconium-cerium composite, which is ready for use;
G、将备用的锆铈复合物经950℃温度煅烧3小时，即得525克铈掺杂的氧化锆复合抛光粉。G. Calcining the spare zirconium-cerium composite at 950° C. for 3 hours to obtain 525 grams of cerium-doped zirconia composite polishing powder.
应用本发明的铈掺杂的氧化锆复合抛光粉的制备方法，制备的铈掺杂的氧化锆复合抛光粉，可用于光学玻璃、透镜、液晶显示屏、半导体等抛光。By applying the preparation method of the cerium-doped zirconia composite polishing powder of the present invention, the prepared cerium-doped zirconia composite polishing powder can be used for polishing optical glass, lens, liquid crystal display screen, semiconductor and the like.
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