CN102352188A - Precision cerium-zirconium-based solid solution rare earth polishing powder and preparation method thereof - Google Patents

Precision cerium-zirconium-based solid solution rare earth polishing powder and preparation method thereof Download PDF

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CN102352188A
CN102352188A CN201110261047XA CN201110261047A CN102352188A CN 102352188 A CN102352188 A CN 102352188A CN 201110261047X A CN201110261047X A CN 201110261047XA CN 201110261047 A CN201110261047 A CN 201110261047A CN 102352188 A CN102352188 A CN 102352188A
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cerium
zirconium
solution
iron
salt
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CN102352188B (en
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贾嘉
赵月昌
李冉
曹红霞
蒙素玲
赵秀娟
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SHANGHAI HUAMING GONA RARE EARTH NEW MATERIALS CO Ltd
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Abstract

The invention discloses precision cerium-zirconium-based solid solution rare earth polishing powder and a preparation method thereof. The precision cerium-zirconium-based solid solution rare earth polishing powder comprises the following components in percentage by weight: 50 to 95 percent of cerium oxide, 5 to 40 percent of zirconium oxide and 0.1 to 10 percent of iron oxide. The polishing powder prepared by the method has the advantages of low cost and suspension property, high wear resistance and effective utilization rate, stable product quality and the like, and can be applied to precision polishing in the fields of liquid crystal displays, optical elements, integrated circuits and the like.

Description

Accurate cerium zirconium based solid solution polishing powder from rare earth and preparation method thereof
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 based solid solution 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 accurate cerium zirconium based solid solution 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.
Accurate cerium zirconium based solid solution polishing powder from rare earth of the present invention is characterised in that, contains the component of following weight part:
Cerium oxide 50-95%
Zirconium white 5-40%
Red stone 0.1-10%
The preparation method of described accurate cerium zirconium based solid solution may further comprise the steps:
The mixed salt solution of cerium, zirconium and iron 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) the mixed salt solution A with cerium, zirconium and iron mixes with ammonium bicarbonate soln B, and the pH value of control terminal point is 7-8, 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 mixed salt solution of said cerium, zirconium and iron, in corresponding oxide compound, cerium oxide accounts for the 44-93wt% of metal-salt gross weight, and zirconium white accounts for the 7-51wt% of metal-salt gross weight, and red stone accounts for the 0.1-10wt% of metal-salt gross weight;
In the mixed salt solution of said cerium, zirconium and iron, the total weight content of metal-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 iron comprises the steps:
The soluble salt of cerium, zirconium and iron is water-soluble, or soluble salt, the oxide compound of iron and the soluble salt that acid-respons gets iron that the carbonate and the acid-respons of cerium, zirconium got cerium, zirconium, thorough mixing, solution A;
The soluble salt of described cerium, zirconium, iron is 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 iron is an iron nitrate;
Described acid is hydrochloric acid or nitric acid;
(2) with roasting after the drying precipitate of collecting;
Described drying temperature is 80~160 ℃, and be 12-24h time of drying;
Described maturing temperature is 950~1100 ℃, and roasting time is 4~6h;
(3) product of roasting is got title product through comminution by gas stream, accurate cerium zirconium base polishing powder from rare earth, particle diameter are that D50 is 0.7~4 μ m;
Utilize preparation method of the present invention, polishing powder is a cube phase cerium zirconium based solid solution.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 based solid solution 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, the pH value of terminal point is 2, and iron nitrate 0.5g is dissolved in the 10g deionized water; Join in the above-mentioned solution and mix, be heated to 50 ℃, mixed salt solution; The ammonium bicarbonate aqueous solution of preparation 200g/L is added drop-wise in the mixed salt solution, and the pH value of control terminal point is 8, 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, the accurate polishing powder from rare earth of title product, wherein cerium oxide content 50%, zirconia content 49.9%, iron oxide content 0.1%
Embodiment 2
Get cerous carbonate 111g, zirconium carbonate 100g, red stone 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 mixed salt solution.The ammonium bicarbonate soln of preparation 100g/L slowly is added drop-wise to mixed salt solution in the ammonium bicarbonate aqueous solution then, and the pH value of control terminal point is 8, 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, the accurate polishing powder from rare earth of title product, wherein cerium oxide content 50%, zirconia content 40%, iron oxide content 10%.
Embodiment 3
Get cerous nitrate 211g, zirconium oxychloride 13g, iron nitrate 2.5g adds deionized water 5000g, and dissolving is heated to 60 ℃ fully; The ammonium bicarbonate aqueous solution of preparation 150g/L; Then mixed salt solution and ammonium bicarbonate aqueous solution and drip are added in the reaction kettle, the pH value of control terminal point is 8, 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, the accurate polishing powder from rare earth of title product, wherein cerium oxide content 95%, zirconia content 4.9%, iron oxide content 0.1%.

Claims (8)

1. accurate cerium zirconium based solid solution polishing powder from rare earth is characterized in that, contains the component of following weight part:
Cerium oxide 50-95%
Zirconium white 5-40%
Red stone 0.1-10%.
2. accurate cerium zirconium based solid solution polishing powder from rare earth according to claim 1 is characterized in that, particle diameter is that D50 is 0.7~4 μ m.
3. the preparation method of accurate cerium zirconium based solid solution according to claim 1 and 2; It is characterized in that; May further comprise the steps: the mixed salt solution of cerium, zirconium and iron is mixed with ammonium bicarbonate soln, and co-precipitation gets presoma; Then with presoma through drying, roasting, pulverizing, obtain said accurate cerium zirconium based solid solution polishing powder from rare earth.
4. method according to claim 3 is characterized in that, may further comprise the steps:
(1) the mixed salt solution A with cerium, zirconium and iron mixes with ammonium bicarbonate soln B, and the pH value of control terminal point is 7-8, 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 mixed salt solution of said cerium, zirconium and iron, in corresponding oxide compound, cerium oxide accounts for the 44-93wt% of metal-salt gross weight, and zirconium white accounts for the 7-51wt% of metal-salt gross weight, and red stone accounts for the 0.1-10wt% of metal-salt gross weight;
In the mixed salt solution of said cerium, zirconium and iron, the total weight content of metal-salt is 3~7%.
5. method according to claim 4 is characterized in that, 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.
6. method according to claim 3 is characterized in that, the compound method of the mixed salt solution A of cerium, zirconium and iron comprises the steps:
The soluble salt of cerium, zirconium and iron is water-soluble, or, mix with soluble salt, the oxide compound of iron and the soluble salt that acid-respons gets iron that the carbonate and the acid-respons of cerium, zirconium gets cerium, zirconium, solution A;
(2) with roasting after the drying precipitate of collecting;
Described drying temperature is 80~160 ℃, and be 12-24h time of drying;
Described maturing temperature is 950~1100 ℃, and roasting time is 4~6h;
(3) with product of roasting through comminution by gas stream, accurate cerium zirconium base polishing powder from rare earth.
7. method according to claim 6 is characterized in that, the soluble salt of described cerium, zirconium, iron is nitrate salt or muriate.
8. method according to claim 7 is characterized in that, the soluble salt of cerium is a cerous nitrate; The soluble salt of zirconium is a zirconium nitrate; The soluble salt of iron is an iron nitrate; Described acid is hydrochloric acid or nitric acid.
CN 201110261047 2011-09-05 2011-09-05 Precision cerium-zirconium-based solid solution rare earth polishing powder and preparation method thereof Active CN102352188B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103450811A (en) * 2013-01-10 2013-12-18 湖南皓志新材料股份有限公司 Preparation method of aluminium-doped cerium-zirconium solid-solution polishing powder
CN103694956A (en) * 2013-12-27 2014-04-02 福达合金材料股份有限公司 Mixed powder capable of rapidly removing punched burrs from sheet-type electrical contact and use method of mixed powder
CN103773312A (en) * 2013-12-27 2014-05-07 福达合金材料股份有限公司 Mixed powder for rapidly removing forged burrs of rivet electrical contact and application 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
CN106010298A (en) * 2016-06-29 2016-10-12 上海华明高纳稀土新材料有限公司 Zirconium oxide polishing solution 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
CN107201178A (en) * 2017-05-27 2017-09-26 于长江 A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder
CN111019529A (en) * 2019-12-30 2020-04-17 中国科学院长春光学精密机械与物理研究所 Magnetic jet polishing solution and preparation method thereof
US11161751B2 (en) 2017-11-15 2021-11-02 Saint-Gobain Ceramics & Plastics, Inc. Composition for conducting material removal operations and method for forming same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1583260A (en) * 2004-05-28 2005-02-23 清华大学 Nano cerium and zirconium based oxide with transition elements added and its preparation
CN101010402A (en) * 2004-09-03 2007-08-01 昭和电工株式会社 Mixed rare earth oxide, mixed rare earth fluoride, cerium-based abrasive using the materials and production processes thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1583260A (en) * 2004-05-28 2005-02-23 清华大学 Nano cerium and zirconium based oxide with transition elements added and its preparation
CN101010402A (en) * 2004-09-03 2007-08-01 昭和电工株式会社 Mixed rare earth oxide, mixed rare earth fluoride, cerium-based abrasive using the materials and production processes thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103450811A (en) * 2013-01-10 2013-12-18 湖南皓志新材料股份有限公司 Preparation method of aluminium-doped cerium-zirconium solid-solution polishing powder
CN103694956A (en) * 2013-12-27 2014-04-02 福达合金材料股份有限公司 Mixed powder capable of rapidly removing punched burrs from sheet-type electrical contact and use method of mixed powder
CN103773312A (en) * 2013-12-27 2014-05-07 福达合金材料股份有限公司 Mixed powder for rapidly removing forged burrs of rivet electrical contact and application method thereof
CN103694956B (en) * 2013-12-27 2015-06-24 福达合金材料股份有限公司 Mixed powder capable of rapidly removing punched burrs from sheet-type electrical contact and use method of mixed powder
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
CN106010298A (en) * 2016-06-29 2016-10-12 上海华明高纳稀土新材料有限公司 Zirconium oxide polishing solution 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
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
CN111019529A (en) * 2019-12-30 2020-04-17 中国科学院长春光学精密机械与物理研究所 Magnetic jet polishing solution and preparation method thereof
CN111019529B (en) * 2019-12-30 2021-07-06 中国科学院长春光学精密机械与物理研究所 Magnetic jet polishing solution and preparation method thereof

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