Cerium-based mixed rare earth polishing powder and preparation method thereof

A technology of mixing rare earth and polishing powder, which is applied in chemical instruments and methods, polishing compositions containing abrasives, and other chemical processes, can solve problems such as difficult dehydration, polishing scratches, uneven fluorination reactions, etc., to ensure Uniformity of fluorination reaction, ensuring uniformity of fluorination, and easy polishing accuracy

Active Publication Date: 2013-06-05
上海华明高纳稀土新材料有限公司
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AI Technical Summary

Problems solved by technology

[0007] The polishing powder produced by the above-mentioned existing production process will be due to the one-time fluorination, so the fluorination reaction will be uneven or partially fluorinated. On the one hand, it will affect the crystal phase structure of the product after roasting. On the other hand It will produce free fluorine ions that affect the polishing accuracy and rate, and the size and strength of the agglomerated particles formed after roasting are also very different. The polishing accuracy and polishing rate of the polishing powder are mainly determined by the size and Determined by the agglomeration strength, this will lead to a series of problems, such as scratches on the polished glass surface or a rapid decrease in the polishing rate in a very short period of time, especially when polishing a hard glass surface, the rapid decrease in the polishing rate is fatal; At the same time, the rare earth fluorocarbonate obtained in the fluorination process has a small particle size and is difficult to dehydrate, resulting in a low yield.
[0008] In order to meet the conditions, it is necessary to select a polishing powder product with a certain agglomeration strength and a certain particle size, and these characteristics are difficult to control, and the production process is complicated, the cost increases and the introduction of impurity ions causes quality fluctuations
[0009] In addition, for example, the invention patent with the patent publication number CN101010402A discloses a method of mixing rare earth oxide and rare earth fluoride, grinding, drying, roasting, and grading to prepare rare earth polishing powder. Although this method avoids the situation of uneven fluorination, However, the defect of this method is that the secondary sintering of the particles will occur, and some particles will grow abnormally after secondary roasting, forming local coarse particles, which will cause scratches during the polishing process.

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  • Cerium-based mixed rare earth polishing powder and preparation method thereof

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[0035] The preparation method of cerium-based mixed rare earth polishing powder of the present invention, it comprises the steps:

[0036] (1) Preparation of partial fluorination of rare earth carbonate: mix rare earth carbonate with water for beating, after ball milling, heat to 30-50°C, add inorganic acid to pH 3-4, then add diluted fluorinating agent, After fully stirring, adjust the pH value to 6.5-7 with ammonium bicarbonate solution, dehydrate and dry after holding for a certain period of time, and obtain a partially fluorinated rare earth carbonate mixture;

[0037] (2) mixing: mixing the rare earth fluorocarbonate mixture obtained above with the corresponding rare earth carbonate;

[0038] (3) roasting: the above-mentioned mixed product is roasted at high temperature to obtain a rare earth polishing powder precursor;

[0039] (4) Pulverization and classification: the rare earth polishing powder precursor is pulverized and classified to obtain cerium-based mixed rare e...

Embodiment 1

[0044]Mix 1000kg of lanthanum cerium carbonate with 650kg of water, ball mill for 2 hours, heat to 30°C, and add nitric acid to pH 3 while stirring. Mix 120kg of 40% hydrofluoric acid and 120kg of water, slowly add to the above feed solution, stir for 1h, add 10% ammonium bicarbonate solution until the pH value is 6.5, and dry at 160°C for 10h after centrifugal dehydration to obtain partial fluorination The rare earth carbonate mixture; mix the partially fluorinated rare earth carbonate mixture with 1000kg of lanthanum cerium carbonate, and roast at 1000°C for 5 hours to obtain the rare earth polishing powder precursor. After jet crushing and classification, the rare earth polishing powder described in the invention is obtained.

[0045] Laser particle size analyzer test results: D 50 =0.82μm, the grinding rate is 88%, and the surface roughness of the product is

Embodiment 2

[0047] Mix 1000kg lanthanum cerium praseodymium carbonate with 1500kg water, ball mill for 2 hours, heat to 50°C, and add phosphoric acid to pH 3 while stirring. Mix 80kg of 40% fluosilicic acid with 80kg of water, slowly add to the above feed solution, stir for 1h, add 15% ammonium bicarbonate solution until the pH value is 7, and dry at 160°C for 20h after centrifugal dehydration to obtain partial fluorination The mixture of rare earth carbonates; the partially fluorinated rare earth carbonate mixture is mixed with 800kg of lanthanum cerium carbonate and 200kg of cerium carbonate, and roasted at 1100°C for 4h to obtain the precursor of rare earth polishing powder. After jet crushing and classification, the invention described Rare earth polishing powder.

[0048] Laser particle size analyzer test results: D 50 =3.89μm, the grinding rate is 90%, and the surface roughness of the product is

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Abstract

The invention discloses cerium-based mixed rare earth polishing powder and a preparation method thereof. The cerium-based mixed rare earth polishing powder is a uniform solid solution composed of a rare earth oxyfluoride and a cubic-phase rare earth oxide. Compared with the prior art, the preparation method has the advantages that partly fluorinated rare earth carbonate is mixed with rare earth carbonate so that fluoridation reaction uniformity is guaranteed and the problems of poor dehydration effects and a low yield of rare earth carbonate one-step fluorination are solved; through control of fluorine content, fluorination uniformity is guaranteed, the problem of free fluorions and fluorides which are produced because of non-uniformity of fluorination and influence a polishing precision and a polishing rate is solved, and a particle having an abnormally large part is not produced in calcination; product wear resistance is good, a polishing rate is fast, and a polishing precision can be controlled easily; product uniformity is good, production efficiency is high, a cost is low, and pollution is avoided; and the cerium-based mixed rare earth polishing powder is suitable for surface polishing processes on precision devices such as an integrated circuit, a flat-panel displayer and optical glass in an electronic information industry.

Description

technical field [0001] The invention relates to a rare earth polishing powder and a preparation method thereof, in particular to a cerium-based mixed rare earth polishing powder used for surface polishing of precision devices in the electronic information industry such as integrated circuits, flat displays, and optical glasses, and a preparation method thereof. Background technique [0002] At present, various glass materials are widely used, and these materials need to undergo necessary surface polishing before being applied. In the early days, materials such as zirconia, iron oxide or silicon dioxide were mainly used to polish various glass surfaces. In recent years, considering the polishing efficiency and precision, polishing materials with rare earth oxides (especially cerium oxide) as the main component have been used. It is considered more suitable for surface polishing of glass materials. [0003] With the rapid development of electronic information technology, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K3/14C09G1/02
Inventor 杨筱琼赵月昌郝祥赵秀娟李冉李雪云
Owner 上海华明高纳稀土新材料有限公司
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