CN103013444A - Precision-type mischmetal polishing powder and preparation method thereof - Google Patents
Precision-type mischmetal polishing powder and preparation method thereof Download PDFInfo
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- CN103013444A CN103013444A CN2011102854826A CN201110285482A CN103013444A CN 103013444 A CN103013444 A CN 103013444A CN 2011102854826 A CN2011102854826 A CN 2011102854826A CN 201110285482 A CN201110285482 A CN 201110285482A CN 103013444 A CN103013444 A CN 103013444A
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Abstract
The invention provides precision-type mischmetal polishing powder and a preparation method thereof. The precision-type mischmetal polishing powder is a uniform solid solution composed of an oxyfluoride-crystal form rare earth and a cubic-phase rare-earth oxide. Compared with the existing products, the precision-type mischmetal polishing powder has the advantages that 1, through ball-milling crushing and utilization of a homogenization assistant, a rare-earth carbonate precursor comprises uniform crystal grains; a fluorination reaction is uniform and complete; dissociative fluorinions and fluorides influencing a polishing precision and a polishing rate are not produced; and a high crystallization degree is obtained; 2, wear resistance is good; a polishing rate is fast; and a polishing precision can be controlled easily; 3, product uniformity is good; production efficiency is high; pollution is not produced; and a cost is low; and 4, the precision-type mischmetal polishing powder is suitable for surface polishing processing of precision components such as integrated circuits, flat panel displays and optical glass in the electronic information industry and realizes the purpose of the invention.
Description
Technical field
The present invention relates to a kind of polishing powder from rare earth and preparation method thereof, particularly accurate mishmetal polishing powder of a kind of surface finish that is applied to the electronics and information industry accurate devices such as unicircuit, plane demonstration, opticglass 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 polishing powder product that just need to pick out certain agglomeration strength, certain particle size in order to satisfy condition, and these characteristics are very rambunctious, and complex manufacturing, cost increases and introduces foreign ion, causes quality fluctuation.
Although be that the patent of invention of CN1903962A discloses and adopts ammonium oxalate to prepare the method for polishing powder from rare earth as precipitation agent such as patent publication No., the method adopts tensio-active agent control precursor size, but the defective that this method exists is that undersized particle is too many, so that there is major defect in polishing speed.
Therefore, need especially a kind of accurate mishmetal polishing powder and preparation method thereof, to solve the above-mentioned existing problem that exists.
Summary of the invention
The object of the present invention is to provide a kind of accurate mishmetal polishing powder and preparation method thereof, to overcome the problem that exists on the prior art, median size is little, narrow particle size distribution, polishing speed are fast.
To achieve these goals, technical scheme of the present invention is as follows:
On the one hand, the invention provides a kind of accurate mishmetal polishing powder, it is characterized in that, described mishmetal polishing powder is the homogeneous sosoloid that oxyfluoride rare earth and Emission in Cubic rare earth oxide form by crystal formation.
In one embodiment of the invention, the particle diameter D of described mishmetal polishing powder
50Be 0.6-4.0 μ m, specific surface area is 2.0-6.0m
2/ g, relatively polishing efficiency＞80%.
On the other hand, the invention provides a kind of preparation method of accurate mishmetal polishing powder, it is characterized in that it comprises the steps:
(1) ball milling: carbonated rare earth is mixed with water, and then ball milling gets the carbonated rare earth slurry;
(2) fluoridize: with the heating of carbonated rare earth slurry, under agitation condition, drip 40% hydrofluoric acid solution, add the homogenizing auxiliary agent and be incubated 1-3h after dropping finishes, get the fluorine carbonated rare earth;
(3) roasting: the fluorine carbonated rare earth is carried out roasting, get the fluorine rare earth oxide;
(4) pulverize: the fluorine rare earth oxide is pulverized to get the mishmetal polishing powder.
In one embodiment of the invention, described carbonated rare earth is selected from one or more in cerous carbonate, Phosbloc cerium or the carbonic acid La-Ce-Pr.
In one embodiment of the invention, contain weight percent carbonated rare earth 50%-70% in the described carbonated rare earth slurry, all the other are water.
In one embodiment of the invention, the Heating temperature of described carbonated rare earth slurry heating is 30-60 ℃.
In one embodiment of the invention, the consumption of described dropping 40% hydrofluoric acid solution is 40-80kg acid/ton carbonated rare earth.
In one embodiment of the invention, described homogenizing auxiliary agent is selected from one or more in ammonium sulfate, ammonium nitrate, ammonium chloride or the ammonium phosphate; The add-on of described auxiliary agent is 20-60kg/ ton carbonated rare earth.
In one embodiment of the invention, the maturing temperature of described fluorine carbonated rare earth roasting is 950-1100 ℃, and roasting time is 4-8h.
In one embodiment of the invention, the grinding mode of described fluorine rare earth oxide pulverizing is selected from fluid bed airflow milling or mechanical disintegration.
Accurate mishmetal polishing powder of the present invention and preparation method thereof, compare with present product, interpolation by ball mill pulverizing and homogenizing auxiliary agent, so that the even grain size of carbonated rare earth precursor, fluoridation is evenly complete, free state fluorion and the fluorochemical of polishing precision and the speed of not exerting an influence, degree of crystallinity is high; The wear resistance of product polishing powder is good, and polishing speed is fast, and the polishing precision is controlled easily; The homogeneity of product is good, and production efficiency is high, and cost is low, pollution-free, is applicable to the surface finish processing of the accurate close device of the electronics and information industries such as unicircuit, plane demonstration, opticglass, realizes purpose of the present invention.
Characteristics of the present invention can be consulted the detailed description of the graphic and following better embodiment of this case and be obtained to be well understood to.
Description of drawings
Fig. 1 is the synoptic diagram of the XRD contrast of embodiments of the invention 1 and Comparative Examples 1 gained mishmetal polishing powder.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, further set forth the present invention below in conjunction with specific embodiment.
Accurate mishmetal polishing powder of the present invention, described mishmetal polishing powder is the oxyfluoride rare earth.
In the present invention, the particle diameter D of described mishmetal polishing powder
50Be 0.6-4.0 μ m, specific surface area is 2.0-6.0m
2/ g, relatively polishing efficiency＞80%.
The preparation method of accurate mishmetal polishing powder of the present invention, it comprises the steps:
(1) ball milling: carbonated rare earth is mixed with water, and then ball milling gets the carbonated rare earth slurry;
(2) fluoridize: with the heating of carbonated rare earth slurry, under agitation condition, drip 40% hydrofluoric acid solution, add the homogenizing auxiliary agent and be incubated 1-3h after dropping finishes, get the fluorine carbonated rare earth;
(3) roasting: the fluorine carbonated rare earth is carried out roasting, get the fluorine rare earth oxide;
(4) pulverize: the fluorine rare earth oxide is pulverized to get the mishmetal polishing powder.
In the present invention, described carbonated rare earth is selected from one or more in cerous carbonate, Phosbloc cerium or the carbonic acid La-Ce-Pr.
In the present invention, contain weight percent carbonated rare earth 50%-70% in the described carbonated rare earth slurry, all the other are water.
In the present invention, the Heating temperature of described carbonated rare earth slurry heating is 30-60 ℃.
In the present invention, the consumption of described dropping 40% hydrofluoric acid solution is 40-80kg acid/ton carbonated rare earth.
In the present invention, described homogenizing auxiliary agent is selected from one or more in ammonium sulfate, ammonium nitrate, ammonium chloride or the ammonium phosphate; The add-on of described auxiliary agent is 20-60kg/ ton carbonated rare earth.
In the present invention, the maturing temperature of described fluorine carbonated rare earth roasting is 950-1100 ℃, and roasting time is 4-8h.
In the present invention, the grinding mode of described fluorine rare earth oxide pulverizing is selected from fluid bed airflow milling or mechanical disintegration.
The relative polishing efficiency of the polishing powder from rare earth that relates among the present invention carries out according to GB/T20165-2006.
Embodiment 1
(1) ball milling: with 400kg Phosbloc cerium, the 100kg cerous carbonate mixes with 330kg water, and the preparation solid content is the Phosbloc cerium slurries of 60wt%, through ball milling 2h, after the filtering grinding bead, gets Phosbloc cerium slurries;
(2) fluoridize: Phosbloc cerium slurries are heated to 50 ℃, according to 60kg acid/ton carbonated rare earth, drip hydrofluoric acid 30kg, add ammonium sulfate 10kg after dropping finishes, insulation reaction 1h gets fluorine Phosbloc cerium slurries;
(3) roasting: Phosbloc cerium slurries at 980 ℃ of lower roasting 4h, are obtained the fluorine cerium lanthanum oxide;
(4) pulverize: (3) gained fluorine cerium lanthanum oxide promoting the circulation of qi stream is pulverized, namely obtained polishing powder from rare earth of the present invention, the laser particle analyzer test result is: D
50=1.82 μ m, specific surface area is 4.24m
2/ g.
Embodiment 2
(1) ball milling: 500kg Phosbloc cerium is mixed with 500kg water, and the preparation solid content is the Phosbloc cerium slurries of 50wt%, through ball milling 2h, after the filtering grinding bead, gets Phosbloc cerium slurries;
(2) fluoridize: Phosbloc cerium slurry agitation is even, be heated to 30 ℃, according to 40kg acid/ton carbonated rare earth, drip hydrofluoric acid 20kg, after dropping finishes, add ammonium phosphate 30kg, insulation reaction 2h gets fluorine Phosbloc cerium slurries;
(3) roasting: fluorine carbonated rare earth slurries at 950 ℃ of lower roasting 8h, are obtained the fluorine cerium lanthanum oxide;
(4) pulverize: (3) gained fluorine cerium lanthanum oxide is carried out comminution by gas stream, namely obtain polishing powder from rare earth of the present invention, the laser particle analyzer test result is: D
50=0.61 μ m, specific surface area is 2.91m
2/ g.
Embodiment 3
(1) ball milling: 500kg carbonic acid La-Ce-Pr is mixed with 214kg water, and the preparation solid content is the carbonic acid La-Ce-Pr slurries of 70wt%, through ball milling 3h, after the filtering grinding bead, gets carbonic acid La-Ce-Pr slurries.
(2) fluoridize: carbonic acid La-Ce-Pr slurry agitation is even, be heated to 60 ℃, according to 80kg acid/ton carbonated rare earth, drip hydrofluoric acid 40kg, after dropping finishes, add ammonium sulfate 5kg, ammonium nitrate 5kg, insulation reaction 3h gets fluorine carbonated rare earth slurries.
(3) roasting: fluorine carbonated rare earth slurries at 1100 ℃ of lower roasting 4h, are obtained fluorine cerium lanthanum oxide praseodymium.
(4) pulverize: (3) gained fluorine cerium lanthanum oxide praseodymium is carried out comminution by gas stream, namely obtain polishing powder from rare earth of the present invention, the laser particle analyzer test result is: D
50=3.97 μ m, specific surface area is 3.48m
2/ g.
Embodiment 4
(1) ball milling: 500kg carbonic acid La-Ce-Pr is mixed with 500kg water, and the preparation solid content is the carbonic acid La-Ce-Pr slurries of 50wt%, through ball milling 3h, after the filtering grinding bead, gets carbonic acid La-Ce-Pr slurries;
(2) fluoridize: carbonic acid La-Ce-Pr slurry agitation is even, be heated to 50 ℃, according to 80kg acid/ton carbonated rare earth, drip hydrofluoric acid 40kg, insulation reaction 3h after dropping finishes gets fluorine carbonated rare earth slurries;
(3) roasting: fluorine carbonated rare earth slurries at 950 ℃ of lower roasting 4h, are obtained fluorine cerium lanthanum oxide praseodymium;
(4) pulverize: (3) gained fluorine cerium lanthanum oxide praseodymium is carried out comminution by gas stream, namely obtain polishing powder from rare earth of the present invention, the laser particle analyzer test result is: D
50=2.61 μ m, specific surface area is 5.97m
2/ g.
Comparative Examples 1
With 400kg Phosbloc cerium, the 100kg cerous carbonate mixes with 330kg water, and the preparation solid content is the Phosbloc cerium slurries of 60wt%, gets Phosbloc cerium slurries.Phosbloc cerium slurries are heated to 50 ℃, according to 60kg acid/ton carbonated rare earth, drip hydrofluoric acid aqueous solution 30kg, insulation reaction 1h after dropping finishes gets fluorine Phosbloc cerium slurries.Phosbloc cerium slurries at 980 ℃ of lower roasting 4h, are obtained the fluorine cerium lanthanum oxide.The fluorine cerium lanthanum oxide is carried out comminution by gas stream, namely obtain corresponding polishing powder from rare earth, the laser particle analyzer test result is: D
50=1.79 μ m, specific surface area is 4.38m
2/ g.
The particle diameter D of embodiment 1, embodiment 2, embodiment 3 and embodiment 4 and Comparative Examples 1
50(μ m), specific surface area (m
2/ g) and the Data Comparison of polishing speed (%) as shown in table 1.
Table 1
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 (9)
1. an accurate mishmetal polishing powder is characterized in that, described mishmetal polishing powder is the homogeneous sosoloid that oxyfluoride rare earth and Emission in Cubic rare earth oxide form by crystal formation.
2. accurate mishmetal polishing powder according to claim 1 is characterized in that, the particle diameter D of described mishmetal polishing powder
50Be 0.6-4.0 μ m, specific surface area is 2.0-6.0m
2/ g, relatively polishing efficiency＞80%.
3. the preparation method of an accurate mishmetal polishing powder is characterized in that, it comprises the steps:
(1) ball milling: carbonated rare earth is mixed with water, and then ball milling gets the carbonated rare earth slurry;
(2) fluoridize: with the heating of carbonated rare earth slurry, under agitation condition, drip 40% hydrofluoric acid solution, add the homogenizing auxiliary agent and be incubated 1-3h after dropping finishes, get the fluorine carbonated rare earth;
(3) roasting: the fluorine carbonated rare earth is carried out roasting, get the fluorine rare earth oxide;
(4) pulverize: the fluorine rare earth oxide is pulverized to get the mishmetal polishing powder.
In one embodiment of the invention, described carbonated rare earth is selected from one or more in cerous carbonate, Phosbloc cerium or the carbonic acid La-Ce-Pr.
4. preparation method according to claim 3 is characterized in that, contains weight percent carbonated rare earth 50%-70% in the described carbonated rare earth slurry, and all the other are water.
5. preparation method according to claim 3 is characterized in that, the Heating temperature of described carbonated rare earth slurry heating is 30-60 ℃.
6. preparation method according to claim 3 is characterized in that, the consumption of described dropping 40% hydrofluoric acid solution is 40-80kg acid/ton carbonated rare earth.
7. preparation method according to claim 3 is characterized in that, described homogenizing auxiliary agent is selected from one or more in ammonium sulfate, ammonium nitrate, ammonium chloride or the ammonium phosphate; The add-on of described auxiliary agent is 20-60kg/ ton carbonated rare earth.
8. preparation method according to claim 3 is characterized in that, the maturing temperature of described fluorine carbonated rare earth roasting is 950-1100 ℃, and roasting time is 4-8h.
9. preparation method according to claim 3 is characterized in that, the grinding mode that described fluorine rare earth oxide is pulverized is selected from fluid bed airflow milling or mechanical disintegration.
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Cited By (6)
| 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 |
| CN104673098A (en) * | 2013-11-28 | 2015-06-03 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
| 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 |
| CN106675417A (en) * | 2016-12-21 | 2017-05-17 | 安徽中创电子信息材料有限公司 | Spherical lanthanum cerium oxyfluoride rare earth polishing liquid and preparation method thereof |
| 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 |
| CN115678436A (en) * | 2022-11-04 | 2023-02-03 | 包头市科蒙新材料开发有限责任公司 | Preparation method of novel cerium-rich rare earth polishing powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475777A (en) * | 2008-11-07 | 2009-07-08 | 上海华明高纳稀土新材料有限公司 | High precision rare earth polishing powder and preparation thereof |
-
2011
- 2011-09-23 CN CN201110285482.6A patent/CN103013444B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475777A (en) * | 2008-11-07 | 2009-07-08 | 上海华明高纳稀土新材料有限公司 | High precision rare earth polishing powder and preparation thereof |
Cited By (7)
| 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 |
| CN104673098A (en) * | 2013-11-28 | 2015-06-03 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
| CN104673098B (en) * | 2013-11-28 | 2017-01-18 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
| 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 |
| CN106675417A (en) * | 2016-12-21 | 2017-05-17 | 安徽中创电子信息材料有限公司 | Spherical lanthanum cerium oxyfluoride rare earth polishing liquid and preparation method thereof |
| 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 |
| CN115678436A (en) * | 2022-11-04 | 2023-02-03 | 包头市科蒙新材料开发有限责任公司 | Preparation method of novel cerium-rich rare earth polishing powder |
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Effective date of registration: 20181018 Address after: 014030 Shanghai Jiaotong University Industrial Park, south of the East marsh road between Labor Road and Shuguang Road, Baotou Rare Earth Development Zone, Inner Mongolia Autonomous Region Patentee after: Baotou Huaming high new rare earth new material Co., Ltd. Address before: 201613 No. 81, Fan Hua Road, Songjiang District, Shanghai Patentee before: Shanghai Huaming Gona Rare Earth New Materials Co., Ltd. |
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