CN104031561A - Preparation method for polishing powder used for high performance devices such as liquid crystal display - Google Patents
Preparation method for polishing powder used for high performance devices such as liquid crystal display Download PDFInfo
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- CN104031561A CN104031561A CN201310688124.9A CN201310688124A CN104031561A CN 104031561 A CN104031561 A CN 104031561A CN 201310688124 A CN201310688124 A CN 201310688124A CN 104031561 A CN104031561 A CN 104031561A
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Abstract
The invention discloses a preparation method for polishing powder used for high performance devices such as liquid crystal display, which is characterized in that polishing powder microscopic morphology is polyhedral spherical shape, the corner angle of the particle with the above morphology is standard and uniform, scratch is not generated during a polishing process, the polyhedral structural powder has controllable morphology; the particle size distribution is uniform, average volume particle size D50 by a laser diffraction method is 0.7-2.0mum, specific surface area is 1.0-3.5m<2>/g; the dispersibility and suspensibility are good, potential of Zeta is -47mV, the polished surface is shine and neat, no scratch is generated on the surface; the cleaning performance and grinding speed of the product are better than that of certain product on market; the method comprises the following steps: adding cerous carbonate, lanthanum cerium carbonate or lanthanum cerium carbonate praseodymium in a hydrochloric acid solution for dissolving, adjusting pH value to 4-4.5, generating a cerium chloride, lanthanum chloride cerium or lanthanum chloride cerium praseodymium solution, taking the solution as a stock solution, adding a saturated ammonium bicarbonate precipitant with pH value at 8-9 to prepare the rare earth oxide polishing powder, and adding a chemical auxiliary agent in a chlorination rare earth solution or a precipitating agent solution for improving the powder performance before a precipitation reaction process.
Description
Technical field
The present invention relates to a kind of polishing powder preparation technology who is applicable to the contour performance device of liquid-crystal display, polishing powder narrow diameter distribution prepared by employing the method is and even, and morphology microstructure is controlled, good dispersity.
Background technology
At present, cerium based relief polishing powder is the most widely used polishing powder.It has good crystalline form; granularity is little and even; chemically reactive is high; polishing efficiency is high; consumption is few and the life-span is long, and polishing workpiece qualification rate is high, easy cleaning; the plurality of advantages such as pollution-free, is widely used in the polishing of the goods such as eyeglass, opticglass, aeronautical glasses, ic substrate, liquid-crystal display, photomask base plate and various jewels.
In recent years, due to the rapid growth of LCD TV and computer requirements, the high device such as LCD, optical lens grows with each passing day to the demand of high-performance rare-earth polishing powder, LCD factory of China polishing powder from rare earth majority used will be from external import at present, there is following problem in the polishing powder of domestic production: the polishing powder size-grade distribution of 1, producing in enormous quantities is inhomogeneous, when the excessive polishing of granularity, easily produce cut, the throwing erosion effect that undersized does not reach; 2, polishing powder microscopic appearance disunity, the overgenerous particle polishing process of corner angle easily produces scuffing, and smooth surfacing cut power is on the low side.
The present invention is directed to above domestic existing issue, a kind of polishing powder preparation method who is applicable to the contour performance device of liquid-crystal display is provided, the polishing powder microscopic appearance that adopts the method to prepare is that polyhedron is spherical, when polishing, the cutting effect of existing abundance is also difficult for producing cut, and diameter of particle narrow size distribution, laser diffractometry volume average particle size D
50be 0.7~2.0 μ m, good dispersity, can replace imported product.
Summary of the invention
The object of the present invention is to provide a kind of polishing powder preparation method who is applicable to the contour performance device of liquid-crystal display, demand high-performance rare-earth polishing powder being grown with each passing day to solve the high device such as LCD, optical lens.The powder that adopts the inventive method to prepare has following characteristics:
Polishing powder microscopic appearance is that polyhedron is spherical, and the grain corner specification of this kind of pattern is even, be difficult for producing scratching, and polyhedral structure pattern is controlled when polishing;
Even particle size distribution, laser diffractometry volume average particle size D
50be 0.7~2.0 μ m, specific surface area is 1.0~3.5m
2/ g; Dispersiveness and suspension are good, and Zeta potential is-47mV that polished surface light is clean and tidy, surface nothing scuffing; On this product cleaning performance and grinding rate, be better than some product on market.
This polishing powder can be used for the polishing of liquid-crystal display, the contour performance device of opticglass.
Polishing powder preparation method of the present invention comprises the steps:
Cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr are joined in hydrochloric acid soln and dissolved, regulate pH=4~4.5, generate Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution, then set it as stoste, add precipitation agent to prepare the as above Rare earth oxide polishing powder of feature, before precipitin reaction process, in re chloride or in precipitant solution, add chemical assistant to improve powder characteristic.
Particular content is as follows:
(1) raw material preparation: preparation hydrochloric acid soln, cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr are joined in hydrochloric acid soln, stirring at normal temperature is dissolved and is obtained corresponding Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution, with hydrochloric acid and carbonated rare earth regulator solution pH=4~4.5; Preparation unsaturated carbonate hydrogen ammonium solution is as precipitation agent, and regulating pH with ammoniacal liquor is 8~9, gets chemical assistant and joins in re chloride or in precipitant solution.
The said Cerium II Chloride of the present invention, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution are the mixture of itself and water, and concentration is 0.4~0.8mol/L;
Said inorganic additives is one or more in magnesium chloride, Repone K, sodium-chlor, calcium chloride, iron(ic) chloride, and the RE oxide powder mass percent of its content and preparation is 15%~35%.
Said organic additive is one or more in tributyl phosphate, PEG 20000, silane coupling agent KH570, Sodium dodecylbenzene sulfonate, sodium polyacrylate, oleic acid, diethanolamine, dispersion agent LBD-1, and the RE oxide powder mass percent of its content and preparation is 1%~15%.
(2) fluoridize: in Cerium II Chloride, lanthanum-cerium chloride or the lanthanum-cerium chloride praseodymium solution of step (1) gained, add silicofluoric acid to fluoridize, under normal temperature, at the uniform velocity stir 5min~30min, the add-on of silicofluoric acid accounts for 5~8% of cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr quality percentage composition;
(3) precipitation: add unsaturated carbonate hydrogen ammonium solution in Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution after the fluoridizing of step (2) gained, temperature of reaction is 70~90 DEG C, to pH=7, obtain white precipitate fluorine cerous carbonate, fluorine Phosbloc cerium or fluorine carbonic acid La-Ce-Pr, insulation ageing 0.5~4h;
(4) washing: at 60~70 DEG C of distilled water washs three times for the fluorine cerous carbonate of step (3) gained, fluorine Phosbloc cerium or fluorine carbonic acid La-Ce-Pr precipitation, once, then suction filtration oven dry obtains presoma to absolute ethanol washing.
Said bake out temperature is 80~150 DEG C.
(5) calcining: the presoma at step (4) gained is calcined 2~4h at 600~1000 DEG C, obtains rare earth oxide polishing powder of the present invention.
The present invention is the preparation method of main a kind of high-performance polishing powder taking cerium dioxide as main body, the contamination of the chemical assistant adding by adjusting, thereby change the performance such as microscopic appearance, granularity, surface electrical behavior of preparing powder, and do not change product crystal formation.Use brilliant 802 flat polishers of Shenyang section to detect.Feed concentration 25%, master rotating speed 200r/min, 9 times/min of swing arm speed, milling time 40min, counterweight amount 1360g, properties of samples diameter 80mmK9 glass cake, stock removal 61mg, polished surface is without scuffing.
Brief description of the drawings
10000 times of SEM photos of polishing powder powder that accompanying drawing 1 is prepared for embodiment 2
5000 times of SEM photos of polishing powder powder that accompanying drawing 2 is prepared for embodiment 2
The polishing powder SEM photo of accompanying drawing 3 for not adding chemical assistant to prepare
Accompanying drawing 4 is polishing powder for liquid crystal display device preparation technology schema
The polishing powder testing graininess result that accompanying drawing 5 is prepared for embodiment 2
The polishing powder XRD test result that accompanying drawing 6 is prepared for embodiment 2
Embodiment
Embodiment 1
(1) raw material preparation: take 1kg Phosbloc cerium and add hydrochloric acid preparation 0.5mol/L solution of cerium chloride by oxidation, with hydrochloric acid and carbonated rare earth regulator solution pH=4~4.5.Take 0.305kg bicarbonate of ammonia and be mixed with unsaturated carbonate hydrogen ammonium solution as precipitation agent, regulating pH with ammoniacal liquor is 8~9.Preparation 2mol/L Klorvess Liquid, take content and account for 30% of RE oxide powder mass percent, the PEG 20000 solution of preparation 30%, takes content and accounts for 2% of RE oxide powder mass percent, join in lanthanum-cerium chloride solution simultaneously, stir;
(2) fluoridize: take weight concentration and be 30% silicofluoric acid, at the uniform velocity join in lanthanum-cerium chloride solution under stirring at normal temperature condition, silicofluoric acid and cerium lanthanum oxide mass ratio are 5%, continue to stir 20min;
(3) precipitation: the lanthanum-cerium chloride solution of fluoridizing is warming up to 70 DEG C, at the uniform velocity adds while stirring precipitation agent, to pH=7, obtain white precipitate, insulation ageing 4h;
(4) washing: by 60~70 DEG C of distilled water washs three times for white precipitate, absolute ethanol washing once, is dried after suction filtration in 100 DEG C of baking ovens.
(5) calcining: the presoma of gained, at 700 DEG C of calcining 4h, obtains rare earth oxide polishing powder of the present invention.
Embodiment 2
(1) raw material preparation: take 0.6kg cerous carbonate and add hydrochloric acid preparation 0.4mol/L solution of cerium chloride by oxidation, with hydrochloric acid and carbonated rare earth regulator solution pH=4~4.5.Take 0.184g bicarbonate of ammonia and be mixed with unsaturated carbonate hydrogen ammonium solution as precipitation agent, regulating pH with ammoniacal liquor is 8~9.Preparation 2mol/L sodium chloride solution, take content and account for 18% of RE oxide powder mass percent, the sodium polyacrylate solution of preparation 30%, takes content and accounts for 1% of RE oxide powder mass percent, join in solution of cerium chloride by oxidation simultaneously, stir;
(2) fluoridize: take weight concentration and be 30% silicofluoric acid, at the uniform velocity join in solution of cerium chloride by oxidation under stirring at normal temperature condition, silicofluoric acid and cerium oxide mass ratio are 7%, continue to stir 10min;
(3) precipitation: the solution of cerium chloride by oxidation of fluoridizing is warming up to 80 DEG C, at the uniform velocity adds while stirring precipitation agent, to pH=7, obtain white precipitate, insulation ageing 2h;
(4) washing: by 60~70 DEG C of distilled water washs three times for white precipitate, absolute ethanol washing once, is dried after suction filtration in 90 DEG C of baking ovens.
(5) calcining: the presoma of gained, at 850 DEG C of calcining 2.5h, obtains rare earth oxide polishing powder of the present invention.
Embodiment 3
(1) raw material preparation: take 0.8kg cerous carbonate and add hydrochloric acid preparation 0.8mol/L solution of cerium chloride by oxidation, with hydrochloric acid and carbonated rare earth regulator solution pH=4~4.5.Take 0.245g bicarbonate of ammonia and be mixed with unsaturated carbonate hydrogen ammonium solution as precipitation agent, regulating pH with ammoniacal liquor is 8~9.Preparation 2mol/L magnesium chloride solution, take content and account for 25% of RE oxide powder mass percent, the dispersion agent LBD-1 solution of preparation 30%, takes content and accounts for 5% of RE oxide powder mass percent, join in solution of cerium chloride by oxidation simultaneously, stir;
(2) fluoridize: take weight concentration and be 30% silicofluoric acid, at the uniform velocity join in solution of cerium chloride by oxidation under stirring at normal temperature condition, silicofluoric acid and cerium oxide mass ratio are 8%, continue to stir 15min;
(3) precipitation: the solution of cerium chloride by oxidation of fluoridizing is warming up to 90 DEG C, at the uniform velocity adds while stirring precipitation agent, to pH=7, obtain white precipitate, insulation ageing 3h;
(4) washing: by 60~70 DEG C of distilled water washs three times for white precipitate, absolute ethanol washing once, is dried after suction filtration in 120 DEG C of baking ovens.
(5) calcining: the presoma of gained, at 950 DEG C of calcining 2h, obtains rare earth oxide polishing powder of the present invention.
Embodiment 4
(1) raw material preparation: take 0.4kg carbonic acid La-Ce-Pr and add hydrochloric acid preparation 0.6mol/L lanthanum-cerium chloride praseodymium solution, with hydrochloric acid and carbonated rare earth regulator solution pH=4~4.5.Take 0.123g bicarbonate of ammonia and be mixed with unsaturated carbonate hydrogen ammonium solution as precipitation agent, regulating pH with ammoniacal liquor is 8~9.Preparation 2mol/L calcium chloride and magnesium chloride mixture solution, ammonium nitrate accounts for 40%, magnesium chloride accounts for 60%, take content and account for 12% of RE oxide powder mass percent, oleic acid and diethanolamine mixing solutions that preparation mol ratio is 1:1, take content and account for 15% of RE oxide powder mass percent, join in lanthanum-cerium chloride praseodymium solution simultaneously, stir;
(2) fluoridize: take weight concentration and be 30% silicofluoric acid, at the uniform velocity join in lanthanum-cerium chloride praseodymium solution under stirring at normal temperature condition, silicofluoric acid and rare earth oxide mass ratio are 6%, continue to stir 10min;
(3) precipitation: the lanthanum-cerium chloride praseodymium solution of fluoridizing is warming up to 75 DEG C, at the uniform velocity adds while stirring precipitation agent, to pH=7, obtain white precipitate, insulation ageing 1.5h;
(4) washing: by 60~70 DEG C of distilled water washs three times for white precipitate, absolute ethanol washing once, is dried after suction filtration in 90 DEG C of baking ovens.
(5) calcining: the presoma of gained, at 800 DEG C of calcining 2h, obtains rare earth oxide polishing powder of the present invention.
Claims (7)
1. polishing powder for liquid crystal display device, is characterized in that:
Polishing powder microscopic appearance is that polyhedron is spherical, and the grain corner specification of this kind of pattern is even, be difficult for producing scratching, and polyhedral structure pattern is controlled when polishing; Even particle size distribution, laser diffractometry volume average particle size D
50be 0.7~2.0 μ m, specific surface area is 1.0~3.5m
2/ g; Dispersiveness and suspension are good, and Zeta potential is-47mV that polished surface light is clean and tidy, surface nothing scuffing; On this product cleaning performance and grinding rate, be better than some product on market.
2. the requirement of polishing powder for liquid crystal display device according to claim 1, it is characterized in that, comprise the steps: cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr to join in hydrochloric acid soln and dissolve, regulate pH=4~4.5, generate Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution, then set it as stoste, adding pH is 8~9 precipitation agent, generate monodispersed white precipitate, calcining preparation volume average particle size D
50be the spherical polishing powder for liquid crystal display device of polyhedron of 0.7~2.0 μ m, in precipitin reaction process, add chemical assistant to improve powder characteristic.
3. method according to claim 2, is characterized in that, comprises the following steps:
(1) raw material preparation: preparation hydrochloric acid soln, cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr are joined in hydrochloric acid soln, stirring at normal temperature is dissolved and is obtained corresponding Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution, with hydrochloric acid and the rare upper adjusting of carbonic acid pH value of solution=4~4.5; Preparation unsaturated carbonate hydrogen ammonium solution, as precipitation agent, is got inorganic additives and is joined in re chloride or in precipitant solution.
(2) fluoridize: in Cerium II Chloride, lanthanum-cerium chloride or the lanthanum-cerium chloride praseodymium solution of step (1) gained, at the uniform velocity under agitation condition, add silicofluoric acid to fluoridize at normal temperature;
(3) precipitation: add unsaturated carbonate hydrogen ammonium solution in Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution after the fluoridizing of step (2) gained, to pH=7, obtain white precipitate fluorine cerous carbonate, fluorine Phosbloc cerium or fluorine carbonic acid La-Ce-Pr, insulation ageing 0.5~4h;
(4) washing: at 60~70 DEG C of distilled water washs three times for the fluorine cerous carbonate of step (3) gained, fluorine Phosbloc cerium or fluorine carbonic acid La-Ce-Pr precipitation, once, then suction filtration oven dry obtains presoma to absolute ethanol washing.
(5) calcining: the presoma at step (4) gained is calcined 2~4h at 600~1000 DEG C, obtains rare earth oxide polishing powder of the present invention.
4. method according to claim 3, it is characterized in that, in step (1), Cerium II Chloride concentration is 0.4~0.8mol/L, said chemical assistant is one or more in magnesium chloride, Repone K, sodium-chlor, calcium chloride, iron(ic) chloride, and the RE oxide powder mass percent of its content and preparation is 15%~35%.
5. method according to claim 3, it is characterized in that, in step (2), in Cerium II Chloride, lanthanum-cerium chloride or the lanthanum-cerium chloride praseodymium solution of gained, add silicofluoric acid to fluoridize, under normal temperature, at the uniform velocity stir 5min~30min, the add-on of silicofluoric acid accounts for 5~8% of cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr quality percentage composition.
6. method according to claim 3, it is characterized in that, in step (3), in Cerium II Chloride, lanthanum-cerium chloride or lanthanum-cerium chloride praseodymium solution after the fluoridizing of gained, add unsaturated carbonate hydrogen ammonium solution, temperature of reaction is 70~90 DEG C, the time that adds precipitation agent is 0.5~1.5h, insulation digestion time 0.5~4h.
7. method according to claim 3, is characterized in that, in step (3), said bake out temperature is 80~150 DEG C.
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Cited By (7)
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CN105754488A (en) * | 2016-02-22 | 2016-07-13 | 郑州宏基研磨科技有限公司 | Grinding and polishing powder and preparation method thereof |
CN107254259A (en) * | 2017-06-08 | 2017-10-17 | 包头海亮科技有限责任公司 | Novel rare-earth polishing powder and preparation method thereof |
CN111302382A (en) * | 2018-11-23 | 2020-06-19 | 甘肃稀土新材料股份有限公司 | Preparation method of lanthanum-cerium oxide powder containing lanthanum oxychloride structure |
CN114262569A (en) * | 2021-12-02 | 2022-04-01 | 甘肃金阳高科技材料有限公司 | Preparation method of large-caliber optical glass polishing solution |
CN115321578A (en) * | 2022-09-08 | 2022-11-11 | 内蒙古科技大学 | Nano quasi-spherical rare earth fluoride polishing powder and preparation method thereof |
CN115557527A (en) * | 2022-09-29 | 2023-01-03 | 包头市安德窑炉科技有限公司 | Radiation material prepared from waste recovered lanthanum cerium chloride solution |
CN115724454A (en) * | 2022-09-30 | 2023-03-03 | 深圳市聚芯半导体材料有限公司 | Lanthanum-cerium oxide solid solution particle and preparation method and application thereof |
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CN103131385A (en) * | 2011-11-23 | 2013-06-05 | 上海华明高纳稀土新材料有限公司 | Cerium-based mixed rare earth polishing powder and preparation method thereof |
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Patent Citations (1)
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CN103131385A (en) * | 2011-11-23 | 2013-06-05 | 上海华明高纳稀土新材料有限公司 | Cerium-based mixed rare earth polishing powder and preparation method thereof |
Cited By (11)
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CN105754488A (en) * | 2016-02-22 | 2016-07-13 | 郑州宏基研磨科技有限公司 | Grinding and polishing powder and preparation method thereof |
CN105754488B (en) * | 2016-02-22 | 2017-12-26 | 郑州宏基研磨科技有限公司 | Grinding and polishing powder and preparation method thereof |
CN107254259A (en) * | 2017-06-08 | 2017-10-17 | 包头海亮科技有限责任公司 | Novel rare-earth polishing powder and preparation method thereof |
CN111302382A (en) * | 2018-11-23 | 2020-06-19 | 甘肃稀土新材料股份有限公司 | Preparation method of lanthanum-cerium oxide powder containing lanthanum oxychloride structure |
CN111302382B (en) * | 2018-11-23 | 2022-06-07 | 甘肃稀土新材料股份有限公司 | Preparation method of lanthanum-cerium oxide powder containing lanthanum oxychloride structure |
CN114262569A (en) * | 2021-12-02 | 2022-04-01 | 甘肃金阳高科技材料有限公司 | Preparation method of large-caliber optical glass polishing solution |
CN115321578A (en) * | 2022-09-08 | 2022-11-11 | 内蒙古科技大学 | Nano quasi-spherical rare earth fluoride polishing powder and preparation method thereof |
CN115321578B (en) * | 2022-09-08 | 2023-09-19 | 内蒙古科技大学 | Nano sphere-like rare earth fluoride polishing powder and preparation method thereof |
CN115557527A (en) * | 2022-09-29 | 2023-01-03 | 包头市安德窑炉科技有限公司 | Radiation material prepared from waste recovered lanthanum cerium chloride solution |
CN115557527B (en) * | 2022-09-29 | 2023-08-18 | 包头市安德窑炉科技有限公司 | Radiation material prepared from lanthanum cerium chloride solution recovered by waste material |
CN115724454A (en) * | 2022-09-30 | 2023-03-03 | 深圳市聚芯半导体材料有限公司 | Lanthanum-cerium oxide solid solution particle and preparation method and application thereof |
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Application publication date: 20140910 |