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CN102559064B - Cerium-zirconium praseodymium sosoloid and preparation method thereof - Google Patents

Cerium-zirconium praseodymium sosoloid and preparation method thereof Download PDF

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CN102559064B
CN102559064B CN201110422071.7A CN201110422071A CN102559064B CN 102559064 B CN102559064 B CN 102559064B CN 201110422071 A CN201110422071 A CN 201110422071A CN 102559064 B CN102559064 B CN 102559064B
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praseodymium
cerium
salt
zirconium
sosoloid
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CN102559064A (en
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赵月昌
杨筱琼
赵秀娟
蒙素玲
李冉
曹红霞
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SHANGHAI HUAMING GONA RARE EARTH NEW MATERIALS CO Ltd
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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

Cerium zirconium praseodymium sosoloid 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 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 preferably chemistry and physicals, there is the advantages such as cutting power is strong, polishing time is short, polishing precision is high, clean operation environment, therefore the result of use than other polishing powders is good, and by people, be called " king of polishing powder ".This product is very fast in China's development at present, ever-growing use, in the polishing field of various opticglass devices, television picture tube, optical lens, oscillatron, sheet glass, semiconductor wafer and metal precise product etc., be widely applied, development prospect is good.
The main polishing powder using is mainly mishmetal polishing powder in the market, comprises cerium oxide, fluorine cerium lanthanum oxide, fluorine cerium lanthanum oxide praseodymium etc.As CN1156749, it is raw material that 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, spheroidizing rare-earth polish, and this polishing powder from rare earth is also rare earth oxyfluoride.
But because rare earth price amount of increase is larger recently, simple use rare earth makes high cost as the raw material of polishing powder, has been unfavorable for the development of downstream electronic information industry.Meanwhile, China's polishing powder is in use inhomogeneous because of particle size distribution, and proportion is larger, 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 upstream, have caused a large amount of environmental pollutions.
Cerium zirconium sosoloid is widely used in purifying vehicle exhaust at present, as CN200510115874.2 has announced a kind of solid solution composition of cerium zirconium compound oxide with high specific surface and preparation method thereof, 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 using in the requirement of the cerium zirconium based solid solution of cerium zirconium and polishing process in this field is inconsistent, generally adds a lot of additives in preparation process, complicated process of preparation, condition is harsh, and cost is high, can not directly apply to polishing field simultaneously.
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, the above-mentioned defect existing to overcome prior art, meets the requirement of business to the polishing precision of production cost and increasingly stringent.
Cerium zirconium based solid solution polishing powder from rare earth of the present invention, the component that contains following weight percent:
Cerium oxide 44~95wt%
Zirconium white 4~50wt%
Praseodymium trioxide 0.1~10wt%
Preferably, the component that contains following weight percent:
Cerium oxide 50~95%wt%
Zirconium white 4.9~49.9wt%
Praseodymium trioxide accounts for 0.1~10wt%
The preparation method of described cerium zirconium praseodymium sosoloid, comprises the following steps:
The mixed salt solution of cerium, zirconium and praseodymium is mixed with ammonium bicarbonate soln, and co-precipitation, obtains presoma, then by presoma drying, roasting, pulverizing, obtains described precision cerium-zirconium-based solid solution rare earth polishing powder;
Concrete, comprise the following steps:
(1) mixed solution A of cerium salt, zirconates and praseodymium salt is mixed with ammonium bicarbonate soln B, controlling pH value is 6.0-6.5, obtains suspension liquid C, at 50~90 ℃, is incubated 0.5~2h precipitation, then collecting precipitation thing;
The concentration of the aqueous solution of described bicarbonate of ammonia is 100-200g/L;
In the mixing salt solution of described 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 described 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;
In the mixing salt solution A of described cerium salt, zirconates and praseodymium salt, the total weight content of cerium salt, zirconates and praseodymium salt is 3~7%;
Described hybrid mode is: A solution is added drop-wise in B solution, or B solution is added drop-wise in A solution, or A, B solution drip are added in reactor;
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, obtain solution A;
Or the carbonate of the carbonate of cerium, zirconium and acid-respons being obtained to the soluble salt of cerium, zirconium, the oxide compound of praseodymium and acid-respons obtain the soluble salt of praseodymium, fully mix, and obtain solution A;
The soluble salt of described cerium salt, zirconates and praseodymium salt is respectively nitrate or muriate;
Preferably, the soluble salt of cerium is cerous nitrate;
Preferably, the soluble salt of zirconium is zirconium nitrate;
Preferably, the soluble salt of praseodymium is praseodymium nitrate;
Described acid is hydrochloric acid or nitric acid;
(2) by 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 obtained to target 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 Emission in Cubic cerium zirconium praseodymium sosoloid.The polishing powder that adopts the present invention to prepare, has cost low, 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 the advantages such as constant product quality can be applicable to the precise polished processing in the fields such as liquid-crystal display, optical element, unicircuit.
Accompanying drawing explanation
Fig. 1 is the XRD figure of precision cerium zirconium praseodymium sosoloid polishing powder from rare earth in embodiment 1.
Embodiment
Embodiment 1
Get cerous carbonate 111g, zirconium carbonate 125g, adds deionized water 7550g, with hydrochloric acid, is distinguished dissolve complete, and the pH value of terminal is 2, and praseodymium nitrate 0.5g is dissolved in 10g deionized water, joins in above-mentioned solution and mixes, and is heated to 50 ℃, obtains mixing salt solution A; The ammonium bicarbonate aqueous solution of preparation 200g/L, is added drop-wise in mixing salt solution A, and the pH value of controlling terminal is 6.0, continues to stir 2h at 50 ℃.By the suspension liquid obtaining through centrifuge dehydration, 120 ℃ of dry 12h, 950 ℃ of roasting 6h.By product of roasting through comminution by gas stream to D50 be 4 μ m, obtain target 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, by its dissolve complete, the pH value of terminal is 3, mixes, and is heated to 90 ℃, obtains mixing salt solution A.The ammonium bicarbonate soln of preparation 100g/L, is then slowly added drop-wise to mixing salt solution A in ammonium bicarbonate aqueous solution, and the pH value of controlling terminal is 6.5, continues to stir 0.5h at 90 ℃.By the suspension liquid obtaining through centrifuge dehydration, 80 ℃ of dry 24h, 950 ℃ of roasting 6h.By product of roasting through comminution by gas stream to D50 be 2.6 μ m, obtain target 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 dissolve complete is heated to 60 ℃; The ammonium bicarbonate aqueous solution of preparation 150g/L; Then mixing salt solution A and ammonium bicarbonate aqueous solution drip are added in reactor, the pH value of controlling terminal is 6.2, and continuation is stirred 1h at 60 ℃, by the suspension liquid obtaining through centrifuge dehydration, 160 ℃ of dry 18h, 1100 ℃ of roasting 4h.By product of roasting through comminution by gas stream to D50 be 0.7 μ m, obtain target product, wherein cerium oxide content 95%, zirconia content 4.9%, Praseodymium trioxide content 0.1%.

Claims (7)

1. cerium zirconium praseodymium sosoloid, is characterized in that, the component that contains following weight percent:
Cerium oxide 44~95wt%
Zirconium white 4~50wt%
Praseodymium trioxide 0.1~10wt%;
The method of the cerium zirconium praseodymium sosoloid that preparation is described, comprises the following steps:
(1) mixed solution A of cerium salt, zirconates and praseodymium salt is mixed with ammonium bicarbonate soln B, controlling pH value is 6.0-6.5, obtains suspension liquid C, at 50~90 ℃, is incubated 0.5~2h precipitation, then collecting precipitation thing;
(2) by roasting after the drying precipitate of collecting, maturing temperature is 950~1100 ℃, and roasting time is 4~6h;
(3) product of roasting is obtained to cerium zirconium praseodymium sosoloid polishing powder from rare earth through comminution by gas stream.
2. cerium zirconium praseodymium sosoloid according to claim 1, is characterized in that the component that contains following weight percent:
Cerium oxide 50~95wt%
Zirconium white 4.9~49.9wt%
Praseodymium trioxide accounts for 0.1~10wt%.
3. cerium zirconium praseodymium sosoloid according to claim 1, is characterized in that, the concentration of the aqueous solution of described bicarbonate of ammonia is 100-200g/L;
In the mixing salt solution A of described 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 mixing salt gross weight
In the mixing salt solution A of described cerium salt, zirconates and praseodymium salt, the total weight content of cerium salt, zirconates and praseodymium salt is 3~7%.
4. cerium zirconium praseodymium sosoloid according to claim 1, is characterized in that, in the mixing salt solution of described cerium salt, zirconates and praseodymium salt, in corresponding oxide compound:
Cerium oxide accounts for 50~95wt% 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 mixing salt gross weight.
5. cerium zirconium praseodymium sosoloid according to claim 1, is characterized in that, described cerium salt, zirconates and praseodymium salt are respectively nitrate or muriate.
6. cerium zirconium praseodymium sosoloid according to claim 1, is characterized in that, cerium salt is cerous nitrate, and zirconates is zirconium nitrate, and praseodymium salt is praseodymium nitrate.
7. cerium zirconium praseodymium sosoloid according to claim 1, is characterized in that, drying temperature is 80~160 ℃, and be 12-24h time of drying.
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CN105524592A (en) * 2015-07-16 2016-04-27 湖州华通研磨制造有限公司 Grinding material
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
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
WO2019099655A1 (en) 2017-11-15 2019-05-23 Saint-Gobain Ceramics & Plastics, Inc. Composition for conducting material removal operations and method for forming same

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