CN102965026A - Rare-earth polishing powder and preparation method thereof - Google Patents
Rare-earth polishing powder and preparation method thereof Download PDFInfo
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- CN102965026A CN102965026A CN2012104511416A CN201210451141A CN102965026A CN 102965026 A CN102965026 A CN 102965026A CN 2012104511416 A CN2012104511416 A CN 2012104511416A CN 201210451141 A CN201210451141 A CN 201210451141A CN 102965026 A CN102965026 A CN 102965026A
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Abstract
The invention provides a rare-earth polishing powder and a preparation method thereof. The rare-earth polishing powder is a uniform solid solution composed by using crystal forms of one or more of cerium oxide, lanthanum oxide and praseodymium oxide as cubic phase rare-earth oxides. The preparation method comprises the following steps: carrying out ball milling on rare-earth carbonate in an alkaline solution, drying and roasting. Compared with the prior art, the invention has the advantages of low cost, simple production technique, no pollution and the like since fluorine is not introduced; and the polishing powder has the advantages of high polishing accuracy, high polishing speed, no corrosion and the like.
Description
Technical field
The present invention relates to a kind of polishing powder from rare earth and preparation method thereof, particularly polishing powder from rare earth of a kind of surface finish that is applied to the electronics such as unicircuit, plane demonstration, opticglass and microelectronics information industry accurate device and preparation method thereof.
Background technology
In recent years, the polishing powder from rare earth take cerium oxide as main component is widely used in the surface finish of the glass baseplates such as lens, sheet glass, liquid-crystal display (LCD), glasses, optical element and stupalith.Fast development along with electronic information technology, widening of polishing powder Application Areas, also had higher requirement to its precision, polishing speed in continuous increase for the demand of polishing powder, this just impels manufacturer to improve constantly product specification, to adapt to the requirement of New Products.Polishing powder from rare earth becomes now applied widely, consumption rare earth application product large, with high content of technology.
It is raw material that early stage polishing powder from rare earth adopts hamartite, be that the patent of invention of CN101215446A discloses the method that a kind of rare earth ore concentrate prepares high cerium nanometer scale polishing powder from rare earth such as patent publication No., from rare earth ore concentrate concentrated sulfuric acid roasting, infusion, directly make mixed rare earth carbonate with hydrogen-carbonate by the precipitator method; Mixed rare earth carbonate mixes with alkali, is heated to melting, and is incubated 1-4 hour in molten state, cools off, pulverizes, then adds industrial hydrofluoric acid, obtains fluorine rare earth oxide enriched substance; The rare enriched substance of fluorine oxidation, pulverize washing, drainage, even in stirrer for mixing, then pack in the band sieve high energy ball mill, be filled with nitrogen, carry out the wet-milling high-energy ball milling, the below of sieving behind the high-energy ball milling chamber is with the high pressure draft rotating channel, the lower powder of sieve dries processing to the moisture of powder under the high velocity air promotion, carry out drying and processing again and get polishing powder from rare earth.
At present, the polishing powder from rare earth production technique that is widely used on the market mainly contains two kinds, a kind of is to fluoridize first the heavy technique of rear carbon, namely in earth solution, add again bicarbonate of ammonia behind the adding silicofluoric acid formation fluorochemical first and precipitate fully, obtain the polishing powder from rare earth product after drying, roasting, pulverizing, the classification.
Be that the patent of invention of CN101899281A discloses a kind of polishing powder from rare earth and manufacture method thereof such as patent publication No., this polishing powder contains cerium oxide CeO as abrasive substance
2, lanthanum trioxide La
2O
3, Praseodymium trioxide Pr
6O
11, its total amount of rare earth TREO more than 90wt%, simultaneously among the 877-3 type polishing powder from rare earth total amount of rare earth TREO, CeO
2The ratio of content accounts for 70-80%, La
2O
3The ratio of content accounts for 19-29%, Pr
6O
11Content ratio accounts for 0.05-2%, Nd
2O
3Content ratio is less than 0.2%; Its production method is used ammonium bicarbonate precipitation for to have added silicofluoric acid at the wet method synthesis procedure, then through boil, dehydration, roasting, wet classification, dry classification, prepare corresponding polishing powder from rare earth.
Another kind is the heavy rear flaorination process of first carbon, namely adds first bicarbonate of ammonia and precipitates, and adds hydrofluoric acid after the washing again and fluoridizes.
Be the production method that the patent of invention of CN100497508C discloses a kind of high-cerium rare-earth polishing powder such as patent publication No., prepare first and add hydrofluoric acid behind the Phosbloc cerium and fluoridize that roasting gets high-cerium rare-earth polishing powder.
The polishing powder original grain degree that adopts existing above-mentioned production technique to produce is inhomogeneous, therefore just inconsistent with the uniformity coefficient of fluorine reaction, can affect on the one hand the degree of crystallinity of product after the roasting, the free state fluorion of polishing precision and the speed of can exerting an influence on the other hand, the agglomerating particles size and the intensity that form after the roasting also have very large difference, and mainly being size and agglomeration strength by the coacervate particle that forms behind the high temperature sintering, the polishing precision of polishing powder and polishing speed determined, can cause series of problems like this, for example the glass surface in polishing produces cut or polishing speed fast reducing within the very short time, particularly when throwing the hard glass surface, it is fatal that polishing speed reduces rapidly.
The introducing of fluorine causes environmental pollution in process of production easily simultaneously, in use causes easily corrosion simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of polishing powder from rare earth and preparation method thereof, to overcome the problem that exists on the prior art.
The invention provides a kind of polishing powder from rare earth, it is characterized in that, described polishing powder from rare earth is the homogeneous sosoloid that the Emission in Cubic rare earth oxide forms by one or more crystal formations that form in cerium oxide, lanthanum trioxide, the Praseodymium trioxide;
Polishing powder from rare earth preparation method's of the present invention, comprise the steps:
Carbonated rare earth is sized mixing, add alkaline solution, high-energy ball milling is 1～5 μ m to D50, drying, and roasting gets described polishing powder from rare earth.
Concrete, comprise following concrete steps:
(1) pre-treatment of carbonated rare earth: with the making beating of carbonated rare earth and water, add alkali, then ball milling to D50 be 1～3 μ m, get the carbonated rare earth slurries;
Described carbonated rare earth is one or more in cerous carbonate, Phosbloc cerium, the carbonic acid La-Ce-Pr, and wherein the TREO of cerous carbonate, Phosbloc cerium, carbonic acid La-Ce-Pr is 45%～50%, cerous carbonate CeO
2/ TREO＞99%, Phosbloc cerium or carbonic acid La-Ce-Pr CeO
2/ TREO is 62%～65%;
Described carbonated rare earth and water making beating, carbonated rare earth accounts for 40～60% of total mass;
Described alkali is one or more in sodium hydroxide, potassium hydroxide, sodium bicarbonate or the yellow soda ash, and the add-on of alkali in massfraction, accounts for 0.5～3% of carbonated rare earth;
(2) drying: with the carbonated rare earth slurry dried that obtains, drying conditions is 80 ~ 120 ℃ of lower dry 10-20h.
(3) roasting: dried carbonated rare earth is carried out roasting, get described polishing powder from rare earth, maturing temperature is 950-1100 ℃, and roasting time is 3-6h.
Term " REO " refers to rare earth oxide (abbreviation of Rare Earth Oxide);
Term " TREO " refers to total amount of the rare earth oxide (abbreviation of Total Rare Earth Oxides)
Term " CeO
2/ TREO " refer to the ratio that cerium oxide accounts for total amount of the rare earth oxide;
Corresponding particle diameter when the cumulative particle sizes percentile that term " D50 " refers to a sample reaches 50%.To be particle diameter account for 50% greater than its particle to its physical significance, also accounts for 50% less than its particle.
Compared with prior art, owing to do not introduce fluorine, therefore, precision rare-earth polishing powder provided by the invention and preparation method thereof has the advantages such as cost is low, production technique is simple, pollution-free; Polishing powder has the advantages such as the polishing precision is high, polishing velocity is fast, nothing corrosion.
Description of drawings
Fig. 1 is the synoptic diagram that embodiments of the invention 1 get the XRD of polishing powder from rare earth.
Fig. 2 is the synoptic diagram that embodiments of the invention 3 get the XRD of polishing powder from rare earth.
Embodiment
Under agitation condition, (TREO is 45.7%, CeO with the 1000kg cerous carbonate
2/ TREO is 99.5%)) join in the 1000kg pure water, add 5kg sodium hydroxide, ball milling to D50 be 3 μ m.The slurries that obtain at 120 ℃ of dry 10h, then at 950 ℃ of roasting 3h, are got polishing powder from rare earth.
Under agitation condition, (TREO is 48.5%, CeO with 1500kg Phosbloc cerium
2/ TERO is 62.3%) join in the 2750kg pure water, add 10kg potassium hydroxide, ball milling to D50 be 1.8 μ m.The slurries that obtain at 100 ℃ of dry 15h, then at 1000 ℃ of roasting 4.5h, are got polishing powder from rare earth.
Under agitation condition, (TREO is 49.7%, CeO with 1500kg carbonic acid La-Ce-Pr
2/ TERO is 64.8%) join in the 1000kg pure water, add the 45kg sodium bicarbonate, ball milling to D50 be 1 μ m.The slurries that obtain at 80 ℃ of dry 20h, then at 1000 ℃ of roasting 4.5h, are got polishing powder from rare earth.
Under agitation condition, (TREO is 48.5%, CeO with 1500kg Phosbloc cerium
2/ TERO is 62.3%) join in the 2750kg pure water, add 10kg yellow soda ash, ball milling to D50 be 5 μ m.The slurries that obtain at 100 ℃ of dry 15h, then at 1000 ℃ of roasting 4.5h, are got polishing powder from rare earth.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and the specification sheets is principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the present invention.The protection domain that the present invention requires is defined by appending claims and equivalent thereof.
Claims (7)
1. polishing powder from rare earth is characterized in that, is the homogeneous sosoloid that the Emission in Cubic rare earth oxide forms by one or more crystal formations that form in cerium oxide, lanthanum trioxide, the Praseodymium trioxide.
2. the preparation method of polishing powder from rare earth is characterized in that, comprises the steps: carbonated rare earth is sized mixing, and adds alkaline solution, and ball milling is 1～5 μ m to D50, drying, and roasting gets described polishing powder from rare earth.
3. method according to claim 2 is characterized in that, may further comprise the steps:
(1) with the making beating of carbonated rare earth and water, add alkali, then ball milling to D50 be 1～3 μ m, get the carbonated rare earth slurries;
(2) with the carbonated rare earth slurry dried that obtains.
(3) dried carbonated rare earth is carried out roasting, get described polishing powder from rare earth.
4. method according to claim 3 is characterized in that, drying conditions is 80 ~ 120 ℃ of lower dry 10-20h.
5. method according to claim 3 is characterized in that, maturing temperature is 950-1100 ℃, and roasting time is 3-6h.
6. each described method according to claim 3～5, it is characterized in that, described carbonated rare earth is one or more in cerous carbonate, Phosbloc cerium, the carbonic acid La-Ce-Pr, and wherein the TREO of cerous carbonate, Phosbloc cerium, carbonic acid La-Ce-Pr is 45%～50%, cerous carbonate CeO
2/ TREO＞99%, Phosbloc cerium or carbonic acid La-Ce-Pr CeO
2/ TREO is 62%～65%.
7. method according to claim 6 is characterized in that, described carbonated rare earth and water making beating, and carbonated rare earth accounts for 40～60% of total mass;
Described alkali is one or more in sodium hydroxide, potassium hydroxide, sodium bicarbonate or the yellow soda ash, and the add-on of alkali in massfraction, accounts for 0.5～3% of carbonated rare earth.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288119A (en) * | 2013-06-17 | 2013-09-11 | 上海华明高纳稀土新材料有限公司 | Preparation method of rear-earth polishing powder |
| CN103333663A (en) * | 2013-06-18 | 2013-10-02 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN103361030A (en) * | 2013-07-23 | 2013-10-23 | 内蒙古科技大学 | Praseodymium-containing ultrafine high-precision rare earth polishing powder and its preparation method |
| CN103571334A (en) * | 2013-11-05 | 2014-02-12 | 上海华明高纳稀土新材料有限公司 | Cerium oxide polishing powder and preparation method 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 |
| CN104877573A (en) * | 2015-06-08 | 2015-09-02 | 四川大学 | Preparation method of spherical nano fluorine-doped CeO2 polishing powder |
| CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
| CN107603491A (en) * | 2017-10-16 | 2018-01-19 | 淄博包钢灵芝稀土高科技股份有限公司 | Polishing powder from rare earth and preparation method thereof |
| CN109825198A (en) * | 2019-04-11 | 2019-05-31 | 苏州孚纳特电子新材料有限公司 | A kind of high-precision polishing powder and preparation method thereof |
| CN110128950A (en) * | 2019-06-18 | 2019-08-16 | 拓米(成都)应用技术研究院有限公司 | A kind of glass polishing agent and preparation method thereof, polishing hairbrush |
| CN112724839A (en) * | 2021-01-21 | 2021-04-30 | 包头华明高纳稀土新材料有限公司 | System and method for preparing rare earth polishing powder |
| CN113845847A (en) * | 2021-08-02 | 2021-12-28 | 北京工业大学 | Method for preparing lanthanum-cerium solid solution polishing powder with controllable particle size by roasting method |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288119A (en) * | 2013-06-17 | 2013-09-11 | 上海华明高纳稀土新材料有限公司 | Preparation method of rear-earth polishing powder |
| CN103333663A (en) * | 2013-06-18 | 2013-10-02 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN103333663B (en) * | 2013-06-18 | 2014-12-17 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN103361030A (en) * | 2013-07-23 | 2013-10-23 | 内蒙古科技大学 | Praseodymium-containing ultrafine high-precision rare earth polishing powder and its preparation method |
| CN103571334A (en) * | 2013-11-05 | 2014-02-12 | 上海华明高纳稀土新材料有限公司 | Cerium oxide polishing powder and preparation method 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 |
| CN104877573B (en) * | 2015-06-08 | 2017-07-14 | 四川大学 | A kind of ball shaped nano fluorine doped CeO2The preparation method of polishing powder |
| CN104877573A (en) * | 2015-06-08 | 2015-09-02 | 四川大学 | Preparation method of spherical nano fluorine-doped CeO2 polishing powder |
| CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
| CN106044829B (en) * | 2016-05-25 | 2018-03-23 | 南昌大学 | A kind of preparation method of white pure zirconia cerium |
| CN106044829B8 (en) * | 2016-05-25 | 2018-11-27 | 赣州湛海工贸有限公司 | A kind of preparation method of white pure zirconia cerium |
| CN107603491A (en) * | 2017-10-16 | 2018-01-19 | 淄博包钢灵芝稀土高科技股份有限公司 | Polishing powder from rare earth and preparation method thereof |
| CN107603491B (en) * | 2017-10-16 | 2019-08-30 | 淄博包钢灵芝稀土高科技股份有限公司 | Polishing powder from rare earth and preparation method thereof |
| CN109825198A (en) * | 2019-04-11 | 2019-05-31 | 苏州孚纳特电子新材料有限公司 | A kind of high-precision polishing powder and preparation method thereof |
| CN110128950A (en) * | 2019-06-18 | 2019-08-16 | 拓米(成都)应用技术研究院有限公司 | A kind of glass polishing agent and preparation method thereof, polishing hairbrush |
| CN112724839A (en) * | 2021-01-21 | 2021-04-30 | 包头华明高纳稀土新材料有限公司 | System and method for preparing rare earth polishing powder |
| CN113845847A (en) * | 2021-08-02 | 2021-12-28 | 北京工业大学 | Method for preparing lanthanum-cerium solid solution polishing powder with controllable particle size by roasting method |
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Application publication date: 20130313 |