CN102559064A - Cerium-zirconium praseodymium sosoloid and preparation method thereof - Google Patents
Cerium-zirconium praseodymium sosoloid and preparation method thereof Download PDFInfo
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- CN102559064A CN102559064A CN2011104220717A CN201110422071A CN102559064A CN 102559064 A CN102559064 A CN 102559064A CN 2011104220717 A CN2011104220717 A CN 2011104220717A CN 201110422071 A CN201110422071 A CN 201110422071A CN 102559064 A CN102559064 A CN 102559064A
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Abstract
The invention provides a cerium-zirconium praseodymium sosoloid and a preparation method thereof. The cerium-zirconium praseodymium sosoloid comprises the following components in percentage by mass: 44 to 95% of cerium oxide, 4 to 50% of zirconia, and 0.1 to 10% of praseodymium oxide. In the cerium-zirconium praseodymium sosoloid provided by the invention, polishing powder is the cubic-phase cerium-zirconium praseodymium sosoloid. The cerium-zirconium praseodymium sosoloid has advantages of low cost, low suspension property of the polishing powder, high abrasive resistance, high effective utilization rate of the polishing powder, stable product quality, and the like. The cerium-zirconium praseodymium sosoloid can be applied to the precocious polishing processing in the fields of liquid crystal displays, optical components, integrated circuits and the like.
Description
Technical field
The present invention relates to a kind of polishing powder from rare earth and preparation method thereof, or rather, is about a kind of cerium zirconium praseodymium sosoloid polishing powder from rare earth and preparation method thereof.
Background technology
Cerium base polishing powder from rare earth is one of rare-earth products of outbalance; Because cerium base polishing powder from rare earth has more excellent chemistry and physicals; Have advantages such as cutting power is strong, polishing time short, polishing precision height, clean operation environment; So better, and be called " king of polishing powder " by people than the result of use of other polishing powders.This product is very fast in China's development at present; Ever-growing use; Obtained widespread use in the polishing field of various opticglass devices, television picture tube, optical lens, oscillatron, sheet glass, semiconductor wafer and metal precision goods etc., development prospect is good.
The main in the market polishing powder that uses is mainly the mishmetal polishing powder, comprises cerium oxide, fluorine cerium lanthanum oxide, fluorine cerium lanthanum oxide praseodymium etc.Like CN1156749, it is raw material that the CN1205354 patent adopts hamartite, and CN101010402A has announced mixed rare-earth oxide, mixed rare earth fluoride, used the abrasive material based on cerium of this material; CN101284983A has announced a kind of ultra-fine, and spheroidizing rare-earth polish, this polishing powder from rare earth also are rare earth oxyfluoride.
But because of rare earth price amount of increase is bigger recently, simple use rare earth makes cost too high as the raw material of polishing powder, has been unfavorable for the development of downstream electronic information industry.Simultaneously, China's polishing powder is in use inhomogeneous because of particle size distribution, and proportion is bigger, causes the effective rate of utilization of polishing powder from rare earth lower, has caused the waste of a large amount of Nonrenewable resources.A large amount of mishmetal polishing powders that use have also increased the weight of the workload of ore dressing in the upper reaches, have caused a large amount of environmental pollutions.
Cerium zirconium sosoloid is widely used in purifying vehicle exhaust at present; Announced a kind of solid solution composition of cerium zirconium compound oxide with high specific surface and preparation method thereof like CN200510115874.2; CN200610117192.X has announced a kind of spherical Ce-Zr based composite oxide and preparation method thereof, and CN02110040.3 has announced a kind of preparation technology based on cerium oxide and zirconic composite oxides.But requiring of in this field, using in requirement of the cerium zirconium based solid solution of cerium zirconium and the polishing process is inconsistent, generally in the preparation process, adds a lot of additives, complicated process of preparation, and condition is harsh, and cost is high, and the while can not directly apply to the polishing field.
Summary of the invention
The object of the present invention is to provide a kind of cerium zirconium praseodymium sosoloid polishing powder from rare earth and preparation method thereof,, satisfy the requirement of commerce the polishing precision of production cost and increasingly stringent to overcome the above-mentioned defective that prior art exists.
Cerium zirconium based solid solution polishing powder from rare earth of the present invention, contain following components in weight percentage:
Cerium oxide 44～95wt%
Zirconium white 4～50wt%
Praseodymium trioxide 0.1～10wt%
Preferably, contain following components in weight percentage:
Zirconium white 4.9～49.9wt%
Praseodymium trioxide accounts for 0.1～10wt%
The preparation method of described cerium zirconium praseodymium sosoloid may further comprise the steps:
The mixed salt solution of cerium, zirconium and praseodymium is mixed with ammonium bicarbonate soln, co-precipitation, presoma, then with presoma through drying, roasting, pulverizing, obtain said accurate cerium zirconium based solid solution polishing powder from rare earth;
Concrete, may further comprise the steps:
(1) mixed solution A of cerium salt, zirconates and praseodymium salt is mixed with ammonium bicarbonate soln B, control pH value is 6.0-6.5, gets suspension liquid C, at 50～90 ℃, and insulation 0.5～2h deposition, collecting precipitation thing then;
The concentration of the aqueous solution of described bicarbonate of ammonia is 100-200g/L;
In the mixing salt solution of said cerium salt, zirconates and praseodymium salt, in corresponding oxide compound:
Cerium oxide accounts for 44～95wt% of mixing salt gross weight
Zirconium white accounts for 4～50wt% of mixing salt gross weight
Praseodymium trioxide accounts for 0.1～10wt% of metal-salt gross weight
Preferably, in the mixing salt solution of said cerium salt, zirconates and praseodymium salt, in corresponding oxide compound:
Cerium oxide accounts for 50～95%wt% of mixing salt gross weight
Zirconium white accounts for 4.9～49.9wt% of mixing salt gross weight
Praseodymium trioxide accounts for 0.1～10wt% of metal-salt gross weight;
Among the mixing salt solution A of said cerium salt, zirconates and praseodymium salt, the total weight content of cerium salt, zirconates and praseodymium salt is 3～7%;
Said hybrid mode is: the A drips of solution is added in the B solution, or the B drips of solution is added in the A solution, or A, B solution and drip are added in the reaction kettle;
The compound method of the mixed salt solution A of cerium, zirconium and praseodymium comprises the steps:
Cerium salt, zirconates and praseodymium salt is water-soluble, get solution A;
Or with the carbonate of cerium, the carbonate of zirconium and the soluble salt that acid-respons gets cerium, zirconium, the oxide compound of praseodymium and acid-respons get the soluble salt of praseodymium, and thorough mixing gets solution A;
The soluble salt of described cerium salt, zirconates and praseodymium salt is respectively nitrate salt or muriate;
Preferably, the soluble salt of cerium is a cerous nitrate;
Preferably, the soluble salt of zirconium is a zirconium nitrate;
Preferably, the soluble salt of praseodymium is a praseodymium nitrate;
Described acid is hydrochloric acid or nitric acid;
(2) with roasting after the drying precipitate of collecting;
Drying temperature is 80～160 ℃, and be 12-24h time of drying;
Maturing temperature is 950～1100 ℃, and roasting time is 4～6h;
(3) product of roasting is got title product cerium zirconium praseodymium sosoloid polishing powder from rare earth through comminution by gas stream, particle diameter is that D50 is 0.7～4 μ m;
Utilize preparation method of the present invention, polishing powder is a cube phase cerium zirconium praseodymium sosoloid.Adopt the polishing powder of the present invention's preparation, it is low to have a cost, and the suspension of polishing powder is little, and wear resistance is high, and the effective rate of utilization of polishing powder is high, and advantages such as constant product quality can be applicable to the precise polished processing in fields such as liquid-crystal display, optical element, unicircuit.
Description of drawings
Fig. 1 is the XRD figure of accurate cerium zirconium praseodymium sosoloid polishing powder from rare earth among the embodiment 1.
Embodiment
Embodiment 1
Get cerous carbonate 111g, zirconium carbonate 125g adds deionized water 7550g, with hydrochloric acid it is dissolved respectively fully, and the pH value of terminal point is 2, and praseodymium nitrate 0.5g is dissolved in the 10g deionized water, joins in the above-mentioned solution to mix, and is heated to 50 ℃, gets mixing salt solution A; The ammonium bicarbonate aqueous solution of preparation 200g/L is added drop-wise among the mixing salt solution A, and the pH value of control terminal point is 6.0, continues to stir 2h down at 50 ℃.With the suspension liquid that obtains through centrifuge dehydration, 120 ℃ of dry 12h, 950 ℃ of roasting 6h.With product of roasting through comminution by gas stream to D50 be 4 μ m, title product, wherein cerium oxide content 50%, zirconia content 49.9%, Praseodymium trioxide content 0.1%.
Embodiment 2
Get cerous carbonate 111g, zirconium carbonate 100g, Praseodymium trioxide 10g adds deionized water 2772g, and with nitric acid with its dissolving fully, the pH value of terminal point is 3, mixes, and is heated to 90 ℃, gets mixing salt solution A.The ammonium bicarbonate soln of preparation 100g/L slowly is added drop-wise to mixing salt solution A in the ammonium bicarbonate aqueous solution then, and the pH value of control terminal point is 6.5, continues to stir 0.5h down at 90 ℃.With the suspension liquid that obtains through centrifuge dehydration, 80 ℃ of dry 24h, 950 ℃ of roasting 6h.With product of roasting through comminution by gas stream to D50 be 2.6 μ m, title product, wherein cerium oxide content 50%, zirconia content 40%, Praseodymium trioxide content 10%.
Embodiment 3
Get cerous nitrate 211g, zirconium oxychloride 13g, praseodymium nitrate 2.5g adds deionized water 5000g, and dissolving is heated to 60 ℃ fully; The ammonium bicarbonate aqueous solution of preparation 150g/L; Then mixing salt solution A and ammonium bicarbonate aqueous solution and drip are added in the reaction kettle, the pH value of control terminal point is 6.2, continue at 60 ℃ of stirring 1h down, with the suspension liquid that obtains through centrifuge dehydration, 160 ℃ of dry 18h, 1100 ℃ of roasting 4h.With product of roasting through comminution by gas stream to D50 be 0.7 μ m, title product, wherein cerium oxide content 95%, zirconia content 4.9%, Praseodymium trioxide content 0.1%.
Claims (9)
1. cerium zirconium praseodymium sosoloid is characterized in that, contains following components in weight percentage:
Cerium oxide 44～95wt%
Zirconium white 4～50wt%
Praseodymium trioxide 0.1～10wt%.
2. cerium zirconium praseodymium sosoloid according to claim 1 is characterized in that, contains following components in weight percentage:
Cerium oxide 50～95%wt%
Zirconium white 4.9～49.9wt%
Praseodymium trioxide accounts for 0.1～10wt%.
3. prepare the method for claim 1 or 2 described cerium zirconium praseodymium sosoloid, it is characterized in that, may further comprise the steps:
(1) mixed solution A of cerium salt, zirconates and praseodymium salt is mixed with ammonium bicarbonate soln B, control pH value is 6.0-6.5, gets suspension liquid C, at 50～90 ℃, and insulation 0.5～2h deposition, collecting precipitation thing then;
(2) with roasting after the drying precipitate of collecting, maturing temperature is 950～1100 ℃, and roasting time is 4～6h;
(3) product of roasting is got cerium zirconium praseodymium sosoloid polishing powder from rare earth through comminution by gas stream.
4. method according to claim 3 is characterized in that, the concentration of the aqueous solution of described bicarbonate of ammonia is 100-200g/L;
Among the mixing salt solution A of said cerium salt, zirconates and praseodymium salt, in corresponding oxide compound:
Cerium oxide accounts for 44～95wt% of mixing salt gross weight,
Zirconium white accounts for 4～50wt% of mixing salt gross weight,
Praseodymium trioxide accounts for 0.1～10wt% of metal-salt gross weight
Among the mixing salt solution A of said cerium salt, zirconates and praseodymium salt, the total weight content of cerium salt, zirconates and praseodymium salt is 3～7%.
5. method according to claim 4 is characterized in that, in the mixing salt solution of said cerium salt, zirconates and praseodymium salt, in corresponding oxide compound:
Cerium oxide accounts for 50～95%wt% of mixing salt gross weight
Zirconium white accounts for 4.9～49.9wt% of mixing salt gross weight
Praseodymium trioxide accounts for 0.1～10wt% of metal-salt gross weight.
6. according to each described method of claim 3～5, it is characterized in that described cerium salt, zirconates and praseodymium salt are respectively nitrate salt or muriate.
7. method according to claim 6 is characterized in that, cerium salt is cerous nitrate, and zirconates is a zirconium nitrate, and praseodymium salt is praseodymium nitrate.
8. method according to claim 7 is characterized in that, described acid is hydrochloric acid or nitric acid.
9. method according to claim 3 is characterized in that, drying temperature is 80～160 ℃, and be 12-24h time of drying.
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Cited By (7)
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| CN103571335A (en) * | 2013-11-05 | 2014-02-12 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN104130716A (en) * | 2014-07-01 | 2014-11-05 | 安徽拓普森电池有限责任公司 | Polishing fluid for optical lenses and preparation method thereof |
| CN105505312A (en) * | 2015-07-16 | 2016-04-20 | 湖州华通研磨制造有限公司 | Preparation method for grinding material |
| CN105524592A (en) * | 2015-07-16 | 2016-04-27 | 湖州华通研磨制造有限公司 | Grinding material |
| CN104130716B (en) * | 2014-07-01 | 2016-11-30 | 张连江 | A kind of polishing fluid for optical glass and preparation method thereof |
| CN107201178A (en) * | 2017-05-27 | 2017-09-26 | 于长江 | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder |
| US11161751B2 (en) | 2017-11-15 | 2021-11-02 | Saint-Gobain Ceramics & Plastics, Inc. | Composition for conducting material removal operations and method for forming same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571335A (en) * | 2013-11-05 | 2014-02-12 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN104130716A (en) * | 2014-07-01 | 2014-11-05 | 安徽拓普森电池有限责任公司 | Polishing fluid for optical lenses and preparation method thereof |
| CN104130716B (en) * | 2014-07-01 | 2016-11-30 | 张连江 | A kind of polishing fluid for optical glass and preparation method thereof |
| CN105505312A (en) * | 2015-07-16 | 2016-04-20 | 湖州华通研磨制造有限公司 | Preparation method for grinding material |
| CN105524592A (en) * | 2015-07-16 | 2016-04-27 | 湖州华通研磨制造有限公司 | Grinding material |
| CN107201178A (en) * | 2017-05-27 | 2017-09-26 | 于长江 | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder |
| CN107201178B (en) * | 2017-05-27 | 2018-03-06 | 泰安麦丰新材料科技有限公司 | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder |
| US11161751B2 (en) | 2017-11-15 | 2021-11-02 | Saint-Gobain Ceramics & Plastics, Inc. | Composition for conducting material removal operations and method for forming same |
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