CN102250552B - Preparation method for cerium doped zirconium composite polishing powder - Google Patents
Preparation method for cerium doped zirconium composite polishing powder Download PDFInfo
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Abstract
The invention discloses a preparation method for cerium doped zirconium composite polishing powder, and relates to the technical field of preparation of rare earth polishing powder materials. The method comprises the following steps: preparing a zirconium salt solution; adding cerium salt into the zirconium salt solution to obtain a mixed solution of zirconium salt and cerium salt; preparing organic aqueous alkali and adding an organic solvent to obtain aqueous alkali; adding the aqueous alkali into the mixed solution of zirconium salt and cerium salt for a neutralization reaction, adding oxidizing agents, and carrying out aging and filtering to obtain a precipitate; rinsing the precipitate to obtain a zirconium-cerium composite precipitate; drying the zirconium-cerium composite precipitate at a constant temperature to obtain a zirconium-cerium compound; calcining the zirconium-cerium compound to obtain the cerium doped zirconium composite polishing powder. The invention has the following characteristics: a non-rare earth raw material is used as the matrix; the polishing powder prepared in the invention can be used to substitute rare earth polishing powder; a good property of environmental protection is obtained in the process of preparation; etc. The cerium doped zirconium composite polishing powder prepared in the invention can be used for polishing of optical glass, lenses, liquid crystal display screens, semiconductors and the like.
Description
Technical field
The present invention relates to the rare earth polishing powder materials preparing technical field, particularly a kind of preparation method of zirconium oxide compound polishing powder of cerium doping.
Background technology
The cerium oxide rare-earth polishing material best as effect is widely used in the polishings such as opticglass, lens, liquid crystal display, semi-conductor, and what be only second to its polishing effect is zirconium white, but zirconic work-ing life is poor than cerium oxide.
Because rare earth is a kind of strategic goods and materials; at present; country has put into effect rare earth protectiveness policy; not only rare earth mining has been carried out to strict control; and significantly raised the rare earth export quotas, protected the rare earth resources of China's preciousness not to be wasted, therefore; preparation and the application of the polishing material that the rare earths material of take is matrix, be subject to restriction and the high restriction of price of raw material sources.Simultaneously, in existing preparation process of take the polishing material that rare earths material is matrix, need to use the materials such as hydrofluoric acid, silicofluoric acid, fluorinated, acid ammonium, these materials have larger harm to environment and human body.
Summary of the invention
For the existing deficiency of prior art, technical problem to be solved by this invention be to provide a kind of take non-rare earths material as matrix, can substitute polishing powder from rare earth and feature of environmental protection polishing material preparation method preferably in preparation process.
The technical solution used in the present invention is the preparation method of the zirconium oxide compound polishing powder of a kind of cerium doping of invention, and its technical process is as follows:
A, get a certain amount of zirconates, be mixed with the aqueous solution that zirconates content is 150g/L-200g/L, become zirconium salt solution, standby;
B, by the 5%-7% of zirconates amount, get a certain amount of cerium salt, join in standby zirconium salt solution, become zirconates cerium mixed salt solution, standby;
C, get a certain amount of organic bases, the organic bases solution that to be mixed with organic bases content be 200g/L-300g/L, and add the organic solvent that occupies machine alkaline solution gross weight 0.05%-0.5%, and mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, carry out neutralization reaction, wherein the mol ratio of the active substance of zirconates cerium mixed salt solution and alkaline solution is 1: 2-1: 6, and temperature of reaction is controlled at 40-100 ℃; Until neutralization reaction fully after, doubly add oxygenant according to the 2-5 of cerium zirconium mass ratio, and stop stirring ageing 2-6 hour; Then, filter, obtain throw out, standby;
E, by standby throw out washing 2-4 time, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 85-150 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 850-1300 ℃ of temperature calcining 2-4 hour, obtain the zirconium oxide compound polishing powder of cerium doping;
H, described zirconates are a kind of in hydration zirconium oxychloride, hydration zirconium carbonate, nitric hydrate oxygen zirconium; Described cerium salt is a kind of in nitric hydrate cerium, hydration Cerium II Chloride; Described organic bases is a kind of in ammoniacal liquor, urea, vulkacit H or two kinds or three kinds; Described oxygenant is that a kind of in hydrogen peroxide, potassium permanganate, potassium perchlorate or two kinds or three kinds are as oxygenant; Described organic solvent is polyoxyethylene glycol, polyacrylic acid, organosilyl a kind of or two kinds or three kinds.
The technical process of the technical scheme of its optimization is as follows:
A, get a certain amount of zirconates, be mixed with the aqueous solution that zirconates content is 180g/L-190g/L, become zirconium salt solution, standby;
B, by the 5%-7% of zirconates amount, get a certain amount of cerium salt, join in standby zirconium salt solution, become zirconates cerium mixed salt solution, standby;
C, get a certain amount of organic bases, the organic bases solution that to be mixed with organic bases content be 250g/L-260g/L, and add the organic solvent that occupies machine alkaline solution gross weight 0.1%-0.2%, and mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, wherein the mol ratio of the active substance of zirconates cerium mixed salt solution and alkaline solution is 1: 3-1: 5; Temperature of reaction is controlled at 50-80 ℃; Until neutralization reaction fully after, doubly add oxygenant according to the 2-5 of cerium amount ratio, and stop stirring ageing 3-5 hour; Then, filter, obtain throw out, standby;
E, by standby throw out washing 2-4 time, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 85-150 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 900-1100 ℃ of temperature calcining 2-4 hour, obtain the zirconium oxide compound polishing powder of cerium doping.
In above-mentioned each technical scheme, when in adopting ammoniacal liquor, urea, vulkacit H two kinds or three kinds of preparation alkaline solutions, the general mol ratio equivalent of required alkaline solution that adopts of the consumption of its each component is prepared;
In adopting hydrogen peroxide, potassium permanganate, potassium perchlorate two kinds or three kinds are as oxygenant, and the general mol ratio equivalent of required alkaline solution that adopts of the consumption of its each component is prepared;
When adopting poly(oxyethylene glycol) 400, polyacrylic acid, organosilyl two kinds or three kinds of preparation organic solvents, the general mol ratio equivalent of required alkaline solution that adopts of the consumption of its each component is prepared;
The preparation method of the zirconium oxide compound polishing powder of cerium doping of the present invention, the employing zirconium white is matrix, a small amount of cerium oxide that adulterates, by the neutralization of organic bases, the gained throw out becomes through high-temperature calcination, thereby, saved a large amount of rare earth materials; Simultaneously, in preparation process, do not need to use the materials such as hydrofluoric acid, silicofluoric acid, fluorinated, acid ammonium that environment and human body had to larger harm, therefore its feature of environmental protection is better.Its product " zirconium oxide compound polishing powder of cerium doping ", through overtesting, has polishing effect preferably, below is zirconium oxide compound polishing powder and the polishing powder from rare earth polishing effect contrast table of cerium doping:
| The sample title | The smooth finish grade | Scratch number | Surface adhesive |
| Cerium doped zirconia compound polishing powder | High | Few | A little less than |
| Polishing powder from rare earth | Low | Many | By force |
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.Following explanation is to adopt the mode exemplified, but protection scope of the present invention should not be limited to this.
Embodiment mono-:
The preparation method of the zirconium oxide compound polishing powder of the cerium of the present embodiment doping, its technical process is as follows: A, get 1308g hydration zirconium oxychloride, join in 7L water, preparation becomes zirconium salt solution, standby;
B, get 55g hydration Cerium II Chloride, join in standby zirconium salt solution, preparation becomes zirconates cerium mixed salt solution, standby;
C, get 589g ammoniacal liquor, be dissolved in 2.3L water, and add the 4.6g poly(oxyethylene glycol) 400, mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, temperature of reaction is controlled at 50 ℃; After neutralization reaction is complete, adds the 10g hydrogen peroxide, and stop stirring ageing 4 hours; Then, filter, obtain throw out, standby;
E, by standby throw out washing 3 times, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 95 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 950 ℃ of temperature calcining 3 hours, obtain the zirconium oxide compound polishing powder of 525 gram ceriums doping.
Embodiment bis-:
The preparation method of the zirconium oxide compound polishing powder of the cerium doping of the present embodiment, its technical process is as follows:
A, get 1190g hydration zirconium carbonate, join in 6.6L water, preparation becomes zirconium salt solution, standby;
B, get 45g nitric hydrate cerium, join in standby zirconium salt solution, preparation becomes zirconates cerium mixed salt solution, standby;
C, get 568g ammoniacal liquor and 11g urea, be dissolved in 2.3L water, and add the 4.6g poly(oxyethylene glycol) 400, mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, temperature of reaction is controlled at 50 ℃; After neutralization reaction is complete, adds 5g hydrogen peroxide, 45g potassium permanganate, and stop stirring ageing 4 hours; Then, filter, obtain throw out, standby;
E, by standby throw out washing 3 times, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 95 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 950 ℃ of temperature calcining 3 hours, obtain the zirconium oxide compound polishing powder of 525 gram ceriums doping.
Embodiment tri-:
The preparation method of the zirconium oxide compound polishing powder of the cerium doping of the present embodiment, its technical process is as follows:
A, get 1742g nitric hydrate oxygen zirconium, join in 9.6L water, preparation becomes zirconium salt solution, standby;
B, get 45g nitric hydrate cerium, join in standby zirconium salt solution, preparation becomes zirconates cerium mixed salt solution, standby;
C, get 497g ammoniacal liquor, 37g urea, 81g vulkacit H, be dissolved in 2.5L water, and add the 5.0g polyacrylic acid, mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, temperature of reaction is controlled at 50 ℃; After neutralization reaction is complete, adds 3.8g hydrogen peroxide, 30.6g potassium permanganate, 26.8g potassium perchlorate, and stop stirring ageing 4 hours; Then, filter, obtain throw out, standby;
E, by standby throw out washing 3 times, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 95 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 950 ℃ of temperature calcining 3 hours, obtain the zirconium oxide compound polishing powder of 525 gram ceriums doping.
Apply the preparation method of the zirconium oxide compound polishing powder of cerium doping of the present invention, the zirconium oxide compound polishing powder of the cerium doping of preparation, can be used for the polishings such as opticglass, lens, liquid crystal display, semi-conductor.
Claims (2)
1. the preparation method of the zirconium oxide compound polishing powder of cerium doping is characterized in that technical process is as follows:
A, get a certain amount of zirconates, be mixed with the aqueous solution that zirconates content is 150g/L-200g/L, become zirconium salt solution, standby;
B, by the 5%-7% of zirconates amount, get a certain amount of cerium salt, join in standby zirconium salt solution, become zirconates cerium mixed salt solution, standby;
C, get a certain amount of organic bases, the organic bases solution that to be mixed with organic bases content be 200g/L-300g/L, and add the organic solvent that occupies machine alkaline solution gross weight 0.05%-0.5%, and mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, carry out neutralization reaction, wherein the mol ratio of the active substance of zirconates cerium mixed salt solution and alkaline solution is 1: 2-1: 6, and temperature of reaction is controlled at 40-100 ℃; Until neutralization reaction fully after, doubly add oxygenant according to the 2-5 of cerium zirconium mass ratio, and stop stirring ageing 2-6 hour; Then, filter, obtain throw out, standby;
E, by standby throw out washing 2-4 time, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 85-150 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 850-1300 ℃ of temperature calcining 2-4 hour, obtain the zirconium oxide compound polishing powder of cerium doping;
H, described zirconates are a kind of in hydration zirconium oxychloride, hydration zirconium carbonate, nitric hydrate oxygen zirconium; Described cerium salt is a kind of in nitric hydrate cerium, hydration Cerium II Chloride; Described organic bases is a kind of in ammoniacal liquor, urea, vulkacit H or two kinds or three kinds; Described oxygenant is that a kind of in hydrogen peroxide, potassium permanganate, potassium perchlorate or two kinds or three kinds are as oxygenant; Described organic solvent is polyoxyethylene glycol, polyacrylic acid, organosilyl a kind of or two kinds or three kinds.
2. the preparation method of the zirconium oxide compound polishing powder that cerium according to claim 1 adulterates is characterized in that technical process is as follows:
A, get a certain amount of zirconates, be mixed with the aqueous solution that zirconates content is 180g/L-190g/L, become zirconium salt solution, standby;
B, by the 5%-7% of zirconates amount, get a certain amount of cerium salt, join in standby zirconium salt solution, become zirconates cerium mixed salt solution, standby;
C, get a certain amount of organic bases, the organic bases solution that to be mixed with organic bases content be 250g/L-260g/L, and add the organic solvent that occupies machine alkaline solution gross weight 0.1%-0.2%, and mix, become alkaline solution, standby;
D, by above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, wherein the mol ratio of the active substance of zirconates cerium mixed salt solution and alkaline solution is 1: 3-1: 5; Temperature of reaction is controlled at 50-80 ℃; Until neutralization reaction fully after, doubly add oxygenant according to the 2-5 of cerium amount ratio, and stop stirring ageing 3-5 hour; Then, filter, obtain throw out, standby;
E, by standby throw out washing 2-4 time, obtain zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing is carried out to freeze-day with constant temperature 24 hours at 85-150 ℃ of temperature, obtain zirconium cerium mixture, standby;
G, by standby zirconium cerium mixture through 900-1100 ℃ of temperature calcining 2-4 hour, obtain the zirconium oxide compound polishing powder of cerium doping.
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| CN103708851B (en) * | 2013-12-21 | 2015-05-27 | 湖南立发釉彩科技有限公司 | Microcrystalline zirconium glaze and preparation technology of efficient microcrystalline zirconium glaze glass polishing powder thereof |
| CN104130818A (en) * | 2013-12-25 | 2014-11-05 | 吉林市东燃新能源科技有限责任公司 | Oil shale semi-coke activator, and preparation method and application thereof |
| CN104673100A (en) * | 2015-02-12 | 2015-06-03 | 柳州豪祥特科技有限公司 | Preparation technology of cerium oxide-based polishing powder |
| TW202134364A (en) | 2020-01-31 | 2021-09-16 | 美商恩特葛瑞斯股份有限公司 | Cmp composition for polishing hard materials |
| CN111925732B (en) * | 2020-08-17 | 2021-09-21 | 湖南皓志科技股份有限公司 | Preparation method of nano neodymium oxide coated zirconia powder |
| CN114591687A (en) * | 2022-03-18 | 2022-06-07 | 深圳市瑞来稀土材料有限公司 | Rare earth polishing powder for semiconductor wafer polishing treatment and preparation method thereof |
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| CN101268016A (en) * | 2005-07-20 | 2008-09-17 | 特莱巴赫工业有限公司 | Ceria based glass polishing composition and a process for the manufacture thereof |
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| CN101268016A (en) * | 2005-07-20 | 2008-09-17 | 特莱巴赫工业有限公司 | Ceria based glass polishing composition and a process for the manufacture thereof |
Non-Patent Citations (2)
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| "Ce-Zr-O超细粉末制备工艺的优化机器抛光性能";郝仕油等;《稀土》;20040229;第25卷(第1期);第13-16页 * |
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