CN101486879A - Rare earth fine polished material and process for manufacturing the same - Google Patents
Rare earth fine polished material and process for manufacturing the same Download PDFInfo
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- CN101486879A CN101486879A CNA200910004984XA CN200910004984A CN101486879A CN 101486879 A CN101486879 A CN 101486879A CN A200910004984X A CNA200910004984X A CN A200910004984XA CN 200910004984 A CN200910004984 A CN 200910004984A CN 101486879 A CN101486879 A CN 101486879A
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- rare earth
- fine polishing
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- earth fine
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Abstract
The invention relates to a rare-earth fine polishing material and a manufacturing technology thereof. The rare-earth fine polishing material consists of La2O3, CeO2 and Pr6O11 with proportion by weight as follows: La2O3:CeO2:Pr6O11 is equal to 0.4-0.55:1:0.07-0.082. The manufacturing technology comprises the following steps: slurry mixed by rare earth carbonate and water is subjected to wet grinding and then precise elutriation method; particle size distribution range is controlled to be between 20 Mum and 0.2 Mum and the particle size distribution is even; fluorating, filtering and drying are carried out, wherein, the weight proportion between the rare earth carbonate and the water is equal to 1:2-3; selected materials adopt the calcination system of gradient-slope temperature rise so as to control the specific surface area to be within the range of 1.8 to 12m<2>/g; the gradient-slope temperature rise starts from 600 DEG C; the maximum temperature is not higher than 1150 DEG C; and the total calcination time is 6-8 hours. The advantages are as follows: the rare-earth fine polishing material overcomes the shortcomings of the prior art; the polishing effect can reach the demand of fine polishing; the polished product has high finish degree; the rare-earth fine polishing material does not cause scratch or sinking to glass baseplate and can be used repeatedly for a plurality of times; and the technology is scientific and reasonable, and can ensure that the rare-earth fine polishing material is stably produced.
Description
Technical field:
The present invention relates to a kind of rare earth fine polishing material and manufacturing process thereof, particularly a kind of devitrified glass precise polished rare earth fine polishing material and manufacturing process thereof of being used for, more precisely be to be main component, be used for the devitrified glass being that liquid-crystal display, the mobile phone face of base material pulled, the mirror polish material and the production technique thereof of hard disk, high gear wrist-watch illiteracy, mp4, mp5, GPS (global positioning system (GPS)) panel with the mixed light rare earth oxyfluoride.
Background technology:
Devitrified glass is the also base mateiral of industry of modern photovoltaic manufacturing, and this material must carry out polished finish before use, to reach the minute surface requirement.Base material for TFT-LCD (thin-layer transistor liquid-crystal display), TN-LCD (distortion array liquid-crystal display), hard disc of computer, LSI (large-scale integrated circuit is pulled) must carry out precise polished to reach planeness, smooth finish requirement especially.
For the 6th generation LCD display, must reach lightweight and be thickness less than 0.3mm, high chemical stability, temperature stability, high tenacity and physical strength are in order to following process.In order to reach above-mentioned requirements, lithium silico-aluminate, magnesium silico-aluminate microcrystalline glass in series have been developed both at home and abroad.
Common polishing material is low for the polishing efficiency of this kind hard glass, recycle the life-span low, easily cause cut, planeness low, polishing process carries out under High Temperature High Pressure, conventional polishing material is the easily fragmentation requirement that do not reach production technique with this understanding.
Summary of the invention:
The objective of the invention is provides a kind of rare earth fine polishing material and manufacturing process thereof for the shortcoming that solves on the above-mentioned prior art, and this technology can be stable produces the precise polished polishing material of workpiece to the devitrified glass being substrate.
Rare earth fine polishing material of the present invention is by La
2O
3, CeO
2And Pr
6O
11, to form, each component by weight proportion is: La
2O
3: CeO
2: Pr
6O
11=0.4～0.55:1:0.07～0.082;
The specific surface area of above-mentioned polishing material (BET) 2.8-6.2m
2/ g, size-grade distribution D
100.1 μ m, D
50=0.9-1.1 μ m, Dmax＜5 μ m, camber [(D90-D10)]/D50＜2.6;
The cerium content of above-mentioned polishing material is by weight CeO
2/ TREO (total amount of rare earth)=65-90%, TREO=86-95%;
X-ray diffraction (x-ray) the figure main peak LaOF:CeO of above-mentioned polishing material
240%.
The screen overflow that its per kilogram of above-mentioned polishing material is crossed 500 mesh sieves is no more than 0.003 gram, and the aqeous suspension pH value of its 10wt% of polishing material is 6-7.
The raw material for preparing above-mentioned polishing material is the Rare Earth Separation product: single rare earth carbonate or mishmetal carbonate.
Manufacturing process of the present invention is: to anticipating of material carbon hydrochlorate, promptly, with carbonated rare earth and water blended slurry through wet-milling, again through accurate moisture level, the control size distribution range is between 20 μ m～0.2 μ m, make even particle size distribution, fluoridize, filter, dry, wherein: carbonated rare earth: water=1:2～3 (w/w);
Adopt the calcinating system of gradient increased temperature to make specific surface area be controlled at (BET) 1.8-12m the material that sub-elects
2Between/the g, 2.8-4.2m preferably
2/ g.Gradient increased temperature is by 600 ℃ of beginnings, and top temperature is no more than 1150 ℃, total calcination time 6-8 hour.
The polishing of rare earth fine polishing material of the present invention is the process that chemistry, mechanical effect (CMP) combine to the polishing mechanism of glass baseplate.Mechanical effect is to rely on the cutting of the hardness of polishing material powder granule to glass, and thus, the hardness that requires granular powder is a little more than glass baseplate.Too high scuffing, the depression of easily causing crossed the low polishing action that then do not rise.The light rare earths oxyfluoride is the polishing material of main component, and the Mohs' hardness of fluorine cerium oxide wherein can play effective mechanical polishing effect a little more than the devitrified glass base material.The fluorine that of at high temperature dissociating plays the effect of chemical milling, and action principle is as follows:
F
-+↑SiO2＝SiF
4
Thus, be that the polishing material of main component can satisfy fully to devitrified glass with the light rare earths oxyfluoride be the polishing of the workpiece of base material, and the harder composition of unnecessary interpolation, as aluminum oxide.
Want to reach that high-flatness, smooth finish require with the rare earth oxyfluoride is that the polishing material of main component must have that definite component proportions, uniform grain sizes distribute, certain specific surface area scope.For composition, lanthanum wherein, cerium, praseodymium must strictly be controlled.Since the lanthanum trioxide lubricate, and lanthanum fluoride is easy to cause cut.The fluorine cerium oxide plays main polishing action, and the fluorine Praseodymium trioxide plays collaborative polishing action.Ratio will cause a large amount of generations of lanthanum fluoride improperly, influences result of use.Size-grade distribution: D
100.1 μ m D
50=0.9-1.1 Dmax＜5 μ m, meticulous as fruit granule, no polishing action, and fine grain specific surface area is big, and adsorptive power is strong, is bonded on the substrate to clean, and causes the waste product of subsequent handling to increase.Largest particle (Dmax) causes cut, depression greater than 5 μ m.The specific surface area of polishing powder has determined the hardness of crystal grain.Specific surface area is crossed low easily low cause cut, depression, and the too high polishing efficiency of specific surface area reduces.
Advantage of the present invention is: rare earth fine polishing material of the present invention has overcome the shortcoming on the prior art, polishing effect can reach meticulous polishing requirements, the product glossiness height of polishing, polishing can not cause scuffing, depression to glass baseplate, and polishing material can recycle repeatedly; Craft science of the present invention is reasonable, can guarantee the stable rare earth fine polishing material of producing.
Embodiment:
Embodiment 1: add 2000 liters of deionized waters at 10m for 1000 kilograms with few neodymium carbonated rare earth
3Stirred 30 minutes in the reactor, squeeze into wet wheeling machine with the flow of 10L/min, the slurry behind the mill removes fine particle through the current fine grading.By the fluorine that is metered into 7wt%, fluoridized 4 hours.Filter, 350 ℃ of oven dry, 600 ℃ in rotary kiln 0.5 hour, 680 ℃ 0.5 hour, 7600 ℃ 0.5 hour, 850 ℃ 0.5 hour, 980 ℃ 3 hours, 1080 ℃ 1 hour.
Embodiment 2: with embodiment 1 preparation polishing material, different is adjusted 980 ℃ of wet-milling input speed 8L/min. calcination times 2 hours.
Measure ree distribution pattern with ICP, atomic absorption detecting CaO, Fe
2O
3, distillation method is measured F, and laser particle size analyzer is measured granularity (Beckman Coulter), and the specific surface determinator is measured specific surface (BeckmanCoulter), and the x-ray diffractometer is measured x diffraction index (Philips).
Granularity with than clothing area estimation result as the table-1
Table-1: polishing material size-grade distribution and specific surface area
The polishing powder 1kg that produces is added 10 liters of pure water, with this slurry to the TFT-LCD glass polishing.
Polishing machine: Twp-sided polishing machine
Sheet glass:
20 every batch
Base plate rotating speed 120rpm
Flow rate of slurry: 100mL/min
Working pressure: 210g/cm
2
Table-2: polishing effect
Higher specific surface area helps improving smooth finish as can be seen from Table 2.This kind polishing powder can recycle repeatedly under this condition(s) of calcination.
Claims (6)
1, a kind of rare earth fine polishing material, it is characterized in that: polishing material is by La
2O
3, CeO
2And Pr
6O
11, to form, each component by weight proportion is: La
2O
3: CeO
2: Pr
6O
11=0.4～0.55:1:0.07～0.082.
2, rare earth fine polishing material according to claim 1 is characterized in that: the specific surface area of polishing material is 2.8-6.2m
2/ g, size-grade distribution D
100.1 μ m, D
50=0.9-1.1 μ m, Dmax＜5 μ m, camber [(D90-D10)]/D50＜2.6.
3, rare earth fine polishing material according to claim 1 is characterized in that: the cerium content of polishing material is by weight CeO
2/ TREO=65-90%, TRE0=86-95%.
4, rare earth fine polishing material according to claim 1 is characterized in that: the X-ray diffractogram main peak LaOF:CeO of polishing material
240%.
5, rare earth fine polishing material according to claim 1 is characterized in that: the screen overflow that the polishing material per kilogram is crossed 500 mesh sieves is no more than 0.003 gram, and the aqeous suspension pH value of polishing material 10wt% is 6-7.
6, a kind of manufacturing process of rare earth fine polishing material as claimed in claim 1, it is characterized in that: use carbonated rare earth and water blended slurry through wet-milling, again through accurate moisture level, the control size distribution range is between 20 μ m～0.2 μ m, make even particle size distribution, fluoridize, filter, dry, wherein: by weight carbonated rare earth: water=1:2～3; Adopt the calcinating system of gradient increased temperature to make specific surface area be controlled at 1.8-12m the material that sub-elects
2Between/the g, gradient increased temperature is by 600 ℃ of beginnings, and top temperature is no more than 1150 ℃, total calcination time 6-8 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910004984XA CN101486879A (en) | 2009-02-20 | 2009-02-20 | Rare earth fine polished material and process for manufacturing the same |
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|---|---|---|---|
| CNA200910004984XA CN101486879A (en) | 2009-02-20 | 2009-02-20 | Rare earth fine polished material and process for manufacturing the same |
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|---|---|
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Family
ID=40889946
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643614A (en) * | 2012-04-17 | 2012-08-22 | 江苏中晶科技有限公司 | Efficient glass polishing powder and preparation method thereof |
| CN102965026A (en) * | 2012-11-12 | 2013-03-13 | 上海华明高纳稀土新材料有限公司 | Rare-earth polishing powder and preparation method thereof |
| CN102976340A (en) * | 2012-11-16 | 2013-03-20 | 西安交通大学 | Method using gradient way to prepare highly dense monox microballoon |
| CN104673098A (en) * | 2013-11-28 | 2015-06-03 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
| CN110256970A (en) * | 2019-07-06 | 2019-09-20 | 深圳市瑞来稀土材料有限公司 | A kind of polishing powder and preparation method thereof |
| CN111094502A (en) * | 2017-10-31 | 2020-05-01 | Hoya株式会社 | Polishing liquid, method for producing glass substrate, and method for producing magnetic disk |
| CN112500801A (en) * | 2020-12-24 | 2021-03-16 | 德米特（苏州）电子环保材料有限公司 | Cerium-based rare earth polishing powder and preparation method and application 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 |
-
2009
- 2009-02-20 CN CNA200910004984XA patent/CN101486879A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643614B (en) * | 2012-04-17 | 2014-02-12 | 江苏中晶科技有限公司 | Efficient glass polishing powder and preparation method thereof |
| CN102643614A (en) * | 2012-04-17 | 2012-08-22 | 江苏中晶科技有限公司 | Efficient glass polishing powder and preparation method thereof |
| CN102965026A (en) * | 2012-11-12 | 2013-03-13 | 上海华明高纳稀土新材料有限公司 | Rare-earth polishing powder and preparation method thereof |
| CN102976340A (en) * | 2012-11-16 | 2013-03-20 | 西安交通大学 | Method using gradient way to prepare highly dense monox microballoon |
| 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 |
| CN111094502B (en) * | 2017-10-31 | 2021-11-16 | Hoya株式会社 | Polishing liquid, method for producing glass substrate, and method for producing magnetic disk |
| CN111094502A (en) * | 2017-10-31 | 2020-05-01 | Hoya株式会社 | Polishing liquid, method for producing glass substrate, and method for producing magnetic disk |
| US11680187B2 (en) | 2017-10-31 | 2023-06-20 | Hoya Corporation | Polishing liquid, method for manufacturing glass substrate, and method for manufacturing magnetic disk |
| US11214713B2 (en) | 2017-10-31 | 2022-01-04 | Hoya Corporation | Polishing liquid, method for manufacturing glass substrate, and method for manufacturing magnetic disk |
| CN110256970A (en) * | 2019-07-06 | 2019-09-20 | 深圳市瑞来稀土材料有限公司 | A kind of polishing powder and preparation method thereof |
| CN112500801A (en) * | 2020-12-24 | 2021-03-16 | 德米特（苏州）电子环保材料有限公司 | Cerium-based rare earth polishing powder and preparation method and application 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 |
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Open date: 20090722 |