CN102358826B - Method for preparing aluminum-doped zirconium oxide compound polishing powder - Google Patents
Method for preparing aluminum-doped zirconium oxide compound polishing powder Download PDFInfo
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Abstract
The invention discloses a method for preparing aluminum-doped zirconium oxide compound polishing powder, which relates to the technical field of preparation of polishing materials. The process comprises the following steps of: preparing a zirconium salt solution; adding an aluminum salt into a zirconium salt solution to obtain a zirconium salt-aluminum salt mixed solution; preparing an organic alkali solution and adding an organic solvent to obtain an alkaline solution; adding the alkaline solution into the zirconium salt-aluminum salt mixed solution for undergoing a neutralization reaction, ageing, and filtering to obtain a precipitate; washing the precipitate to obtain a zirconium-aluminum compound precipitate; drying the zirconium-aluminum compound precipitate at constant temperature to obtain a zirconium-aluminum compound; and calcining the zirconium-aluminum compound to obtain the aluminum-doped zirconium oxide compound polishing powder. The prepared aluminum-doped zirconium oxide compound polishing powder has the characteristics of high cutting performance, capability of replacing rare earth polishing powder and the like, and can be applied to polishing of optical glass, lenses, liquid crystal display screens, semiconductors and the like.
Description
Technical field
The present invention relates to the polishing material preparing technical field, particularly a kind of preparation method of zirconium white composite polishing powder of aluminium doping.
Background technology
The hardness of zirconium white and cerium oxide is suitable, and all the hardness with silicate glass is close, but effect is poor slightly than polishing powder from rare earth; And the relative zirconium white hardness of aluminum oxide is very big, and it is had good cutting force as polishing material, scratches but easily glass surface is produced.
Chinese patent (200580020894.X) " the alumina-zirconia grains mixture of fusion "; this disclosure of the Invention a kind of mixture of particle of the aluminium oxide-zirconium oxide that contains fusion, described mixture contains the following chemical composition of representing with weight percentage: 40-45.5%ZrO+HfO in 100% content
246-58%Al
2O
3The additive of 0-10%;＜0.8%SiO
2With＜1.2% impurity.The feature of described mixture be its granule number that contains impurity less than 2% with under at least 50% situation, the joint knot concentration of measuring in the transverse section of any particle of mixture is greater than 500 joint knot/mm
2Chinese patent (200610026974.2) " preparation method of alumina/silica Compostie abrasive particles " and for example relates to a kind of preparation method of alumina/silica Compostie abrasive particles, belongs to high precision polishing with the fabricating technology field of abrasive material.Preparation method of the present invention prepares α-Al earlier
2O
3Dispersion liquid: in deionized water, add a certain amount of α-Al
2O
3And sodium hexametaphosphate dispersant, stirring evenly, the back adds diluted alkaline and dilute acid soln, and regulating pH value is 9, adopts ultra-sonic dispersion and Ball milling; Be heated to 80～100 ℃ of temperature of reaction then, again at α-Al
2O
3Add a certain amount of Na in the dispersion liquid
2SiO
3With rare H
2SO
4, ageing was 2 hours after reaction finished, and centrifugation then, purification, oven dry finally make and are coated with SiO
2The alumina/silica Compostie abrasive particles.Polishing fluid by this Compostie abrasive particles is mixed with polishes computer hard disc substrate and CD glass substrate, can obviously reduce roughness and the percent ripple on surface.Also have Chinese patent (201010010121.6) " polishing fluid that a kind of chemically mechanical polishing single-crystal magnesium oxide substrate is used ", belong to the polishing fluid that chemically machinery polished is used, particularly chemically mechanical polishing single-crystal magnesium oxide is used the polishing fluid field.The pH value of polishing fluid is 1.5～7.0.The moiety of polishing fluid is as follows by weight percentage: abrasive material 0.5～30%; Inhibitor 0.0001～1%; Complexing agent 0.001～10%; Surplus is deionized water.The abrasive size of polishing fluid is 10～500nm, is selected from SiO
2, ZrO
2, Al
2O
3, TiO
2, MgO or CeO
2The water-sol.The complexing agent of polishing fluid be selected from the organic acid that contains the two keys of phosphorus oxygen,
Organic acid salt, mineral acid, inorganic acid salt.The inhibitor of polishing fluid is selected from and contains pentacyclic compound.Polishing fluid material removing rate height of the present invention, polishing sample surfaces roughness is low, defectives such as surperficial no marking and pit; The preparation of polishing fluid is easy, and cost is low.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who has better cutting ability and can substitute the polishing material of polishing powder from rare earth.
The technical solution used in the present invention is the preparation method of the zirconium white composite polishing powder of a kind of aluminium doping of invention, it is characterized in that technical process is as follows:
A, get certain amount of zirconium salt, be mixed with the aqueous solution that zirconates content is 150g/L-250g/L, become zirconium salt solution, standby;
B, get a certain amount of aluminium salt, join in the standby zirconium salt solution, be mixed with the aqueous solution that the aluminium salts contg is 100g/L-200g/L, become zirconates aluminium mixed salt solution, standby;
C, get a certain amount of organic bases, being mixed with organic bases content is the organic bases solution of 200g/L-300g/L, and adds the organic solvent that occupies machine alkaline solution gross weight 0.01%-1%, mixes, and becomes alkaline solution, standby;
D, with above-mentioned standby zirconates aluminium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, wherein alkaline solution doubly adds according to the 1-5 of zirconates aluminium salt integral molar quantity, carries out neutralization reaction, and temperature of reaction is controlled at 40-100 ℃; After treating that neutralization reaction fully, stop to stir ageing 2-6 hour; Then, filter, get throw out, standby;
E, with standby throw out washing 2-4 time, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 85-150 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 850-1300 ℃ of temperature calcining 2-4 hour, namely get the zirconium white composite polishing powder that aluminium mixes;
H, described zirconates are a kind of in zirconium oxychloride, zirconium carbonate, the Zircosol ZN; Described aluminium salt is a kind of in nitric hydrate aluminium, the crystal aluminum chloride; Described organic bases is a kind of in ammoniacal liquor, urea, the diethylamine or two kinds or three kinds; Described organic solvent is a kind of in sodium polyacrylate, polyacrylamide, the toxilic acid or two kinds or three kinds.
The technical process of the technical scheme of its optimization is as follows:
A, get certain amount of zirconium salt, be mixed with the aqueous solution that zirconates content is 220g/L-230g/L, become zirconium salt solution, standby;
B, get a certain amount of aluminium salt, join in the standby zirconium salt solution, be mixed with the aqueous solution that the aluminium salts contg is 160g/L-180g/L, become zirconates aluminium mixed salt solution, standby;
C, get a certain amount of organic bases, being mixed with organic bases content is the organic bases solution of 270g/L-290g/L, and adds the organic solvent that occupies machine alkaline solution gross weight 0.05%-0.1%, mixes, and becomes alkaline solution, standby;
D, with above-mentioned standby zirconates aluminium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, wherein alkaline solution doubly adds according to the 2-4 of zirconates aluminium salt integral molar quantity and carries out neutralization reaction, and temperature of reaction is controlled at 50-80 ℃; After treating that neutralization reaction fully, stop to stir ageing 3-5 hour; Then, filter, get throw out, standby;
E, with standby throw out washing 2-4 time, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 85-150 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 900-1100 ℃ of temperature calcining 2-4 hour, namely get the zirconium white composite polishing powder that aluminium mixes.
In above-mentioned each technical scheme, when preparing alkaline solutions for two kinds in employing ammoniacal liquor, urea, the diethylamine or three kinds, the general amount of substance equal portions of required alkali that adopt of the consumption of its each component are prepared;
When preparing organic solvents for two kinds in employing sodium polyacrylate, polyacrylamide, the toxilic acid or three kinds, the consumption of its each component generally adopts equal portions to prepare.
The preparation method of the zirconium white composite polishing powder that aluminium of the present invention mixes, the employing zirconates is matrix, a spot of aluminium salt mixes, by the neutralization of organic bases, the gained throw out forms through high-temperature calcination, need not any rare earth element, thereby, can save precious rare earth material.In its product " the zirconium white composite polishing powder that aluminium mixes ", contain more zirconium white and a spot of aluminum oxide, have cutting ability preferably, through overtesting, polishing effect is preferably arranged, following table is the polishing contrast table of above-mentioned two kinds of polishing powders:
| The sample title | The smooth finish grade | Scratch the bar number | Surface adhesive |
| The zirconium white composite polishing powder that aluminium mixes | High | 5-15 | A little less than |
| Polishing powder from rare earth | Low | 15-30 | By force |
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.Following explanation is to adopt the mode that exemplifies, but protection scope of the present invention should not be limited to this.
Embodiment one:
The preparation method of the zirconium white composite polishing powder that the aluminium of present embodiment mixes, its technical process is as follows:
A, get 1111g hydration zirconium oxychloride, join in the 5L water, preparation becomes zirconium salt solution, and is standby;
B, get 92g nitric hydrate aluminium, dissolve in 0.6L water and be mixed with aluminum solutions; Join then in the standby zirconium salt solution, preparation becomes zirconates aluminium mixed salt solution, and is standby;
C, get 576g ammoniacal liquor, be dissolved in the 2L water, and add the 2g sodium polyacrylate and mix, become alkaline solution, standby;
D, with above-mentioned standby zirconates aluminium 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 treating that neutralization reaction fully, stop to stir ageing 4 hours; Then, filter, get throw out, standby;
E, with standby throw out washing 3 times, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 95 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 950 ℃ of temperature calcining 3 hours, namely get the zirconium white composite polishing powder that 525 gram aluminium mix.
Embodiment two:
The preparation method of the zirconium white composite polishing powder that the aluminium of present embodiment mixes, its technical process is as follows:
A, get 1190g hydration zirconium carbonate, join in the 5.4L water, preparation becomes zirconium salt solution, and is standby;
B, get the 32.7g crystal aluminum chloride, dissolve in 0.2L water and be made into aluminum solutions; Join then in the standby zirconium salt solution, preparation becomes zirconates aluminium mixed salt solution, and is standby;
C, get 240g ammoniacal liquor, 154.8g urea, be dissolved in the 1.4L water, and add the 1.4g polyacrylamide and mix, become alkaline solution, standby;
D, with above-mentioned standby zirconates aluminium 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 treating that neutralization reaction fully, stop to stir ageing 4 hours; Then, filter, get throw out, standby;
E, with standby throw out washing 3 times, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 95 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 950 ℃ of temperature calcining 3 hours, namely get the zirconium white composite polishing powder that 525 gram aluminium mix.
Embodiment three:
The preparation method of the zirconium white composite polishing powder that the aluminium of present embodiment mixes, its technical process is as follows:
A, get 1742g nitric hydrate oxygen zirconium, join in the 7.9L water, preparation becomes zirconium salt solution, and is standby;
B, get 91.9g nitric hydrate aluminium, dissolve in the 0.6L water and be made into aluminum solutions; Join then in the standby zirconium salt solution, preparation becomes zirconates aluminium mixed salt solution, and is standby;
C, get 162.4g ammoniacal liquor, 104.4g urea, 621.7g diethylamine, be dissolved in the 3.2L water, and add the 3.2g toxilic acid and mix, become alkaline solution, standby;
D, with above-mentioned standby zirconates aluminium 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 treating that neutralization reaction fully, stop to stir ageing 4 hours; Then, filter, get throw out, standby;
E, with standby throw out washing 3 times, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 95 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 950 ℃ of temperature calcining 3 hours, namely get the zirconium white composite polishing powder that 525 gram aluminium mix.
Use the preparation method of the zirconium white composite polishing powder of aluminium doping of the present invention, the zirconium white composite polishing powder that the aluminium of preparation mixes can be used for polishings such as opticglass, lens, liquid crystal display, semi-conductor.
Claims (2)
1. the preparation method of the zirconium white composite polishing powder that mixes of an aluminium is characterized in that technical process is as follows:
A, get certain amount of zirconium salt, be mixed with the aqueous solution that zirconates content is 150g/L-250g/L, become zirconium salt solution, standby;
B, get a certain amount of aluminium salt, join in the standby zirconium salt solution, be mixed with the aqueous solution that the aluminium salts contg is 100g/L-200g/L, become zirconates aluminium mixed salt solution, standby;
C, get a certain amount of alkali, be mixed with the alkaline solution that alkali content is 200g/L-300g/L, and add the organic additive that accounts for alkaline solution gross weight 0.01%-1%, mix, become standby alkaline solution;
D, with above-mentioned standby zirconates aluminium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, wherein standby alkaline solution doubly adds according to the 1-5 of zirconates aluminium salt integral molar quantity, carries out neutralization reaction, and temperature of reaction is controlled at 40-100 ℃; After treating that neutralization reaction fully, stop to stir ageing 2-6 hour; Then, filter, get throw out, standby;
E, with standby throw out washing 2-4 time, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 85-150 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 850-1300 ℃ of temperature calcining 2-4 hour, namely get the zirconium white composite polishing powder that aluminium mixes;
H, described zirconates are a kind of in zirconium oxychloride, zirconium carbonate, the Zircosol ZN; Described aluminium salt is a kind of in nitric hydrate aluminium, the crystal aluminum chloride; Described alkali is a kind of in ammoniacal liquor, urea, the diethylamine or two kinds or three kinds; Described organic additive is a kind of in sodium polyacrylate, polyacrylamide, the toxilic acid or two kinds or three kinds.
2. the preparation method of the zirconium white composite polishing powder that mixes of aluminium according to claim 1 is characterized in that technical process is as follows:
A, get certain amount of zirconium salt, be mixed with the aqueous solution that zirconates content is 220g/L-230g/L, become zirconium salt solution, standby;
B, get a certain amount of aluminium salt, join in the standby zirconium salt solution, be mixed with the aqueous solution that the aluminium salts contg is 160g/L-180g/L, become zirconates aluminium mixed salt solution, standby;
C, get a certain amount of alkali, be mixed with the alkaline solution that alkali content is 270g/L-290g/L, and add the organic additive that accounts for alkaline solution gross weight 0.05%-0.1%, mix, become standby alkaline solution;
D, with above-mentioned standby zirconates aluminium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, wherein standby alkaline solution doubly adds according to the 2-4 of zirconates aluminium salt integral molar quantity and carries out neutralization reaction, and temperature of reaction is controlled at 50-80 ℃; After treating that neutralization reaction fully, stop to stir ageing 3-5 hour; Then, filter, get throw out, standby;
E, with standby throw out washing 2-4 time, get zirconium aluminium composite precipitation thing, standby;
F, standby zirconium aluminium composite precipitation thing is carried out freeze-day with constant temperature 24 hours under 85-150 ℃ of temperature, get zirconium aluminium mixture, standby;
G, with standby zirconium aluminium mixture through 900-1100 ℃ of temperature calcining 2-4 hour, namely get the zirconium white composite polishing powder that aluminium mixes.
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| CN103450813B (en) * | 2013-01-10 | 2014-09-17 | 湖南皓志新材料股份有限公司 | Preparation method of iron-doped zirconium oxide polishing solution |
| CN103450811B (en) * | 2013-01-10 | 2014-11-26 | 湖南皓志新材料股份有限公司 | Preparation method of aluminium-doped cerium-zirconium solid-solution polishing powder |
| CN103965790B (en) * | 2014-04-25 | 2015-06-03 | 泰安麦丰新材料科技有限公司 | Zr-Al-Ce polishing solution and preparation method thereof |
| JP7071495B2 (en) | 2017-11-15 | 2022-05-19 | サン－ゴバン セラミックス アンド プラスティクス，インコーポレイティド | Compositions for performing material removal operations and methods for forming them |
| CN110256969B (en) * | 2019-05-29 | 2020-11-10 | 湖南皓志科技股份有限公司 | Blue glass fine polishing solution and preparation method thereof |
| CN112321458B (en) * | 2020-10-26 | 2023-04-07 | 宿迁科思化学有限公司 | Preparation method of sunscreen intermediate etoricine |
| CN114538508B (en) * | 2022-02-28 | 2023-12-26 | 深圳陶陶科技有限公司 | Zirconium dioxide powder and preparation method thereof |
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Address after: Whitewater Jianye road 426141 Yongzhou city of Hunan province Qiyang County No. 7 Applicant after: Hunan Haozhi New Materials Co., Ltd. Address before: Baishui town 426141 Hunan County of Qiyang province (Qiyang science and Technology Industrial Park) Applicant before: Yongzhou Haozhi RareEarth Co.,Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: YONGZHOU HAOZHI RARE EARTH CO., LTD. TO: HU NAN HAOZHI NEW MATERIALS CO.,LTD. |
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Owner name: HUNAN HAOZHI TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: HU NAN HAOZHI NEW MATERIALS CO., LTD. Effective date: 20141117 |
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Effective date of registration: 20141117 Address after: Whitewater Jianye road 426141 Yongzhou city of Hunan province Qiyang County No. 7 Patentee after: HUNAN HAOZHI TECHNOLOGY CO., LTD. Address before: Whitewater Jianye road 426141 Yongzhou city of Hunan province Qiyang County No. 7 Patentee before: Hunan Haozhi New Materials Co., Ltd. |