CN101899264B - Rare earth polishing powder and preparation method thereof - Google Patents
Rare earth polishing powder and preparation method thereof Download PDFInfo
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- CN101899264B CN101899264B CN200910022672.1A CN200910022672A CN101899264B CN 101899264 B CN101899264 B CN 101899264B CN 200910022672 A CN200910022672 A CN 200910022672A CN 101899264 B CN101899264 B CN 101899264B
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Abstract
The invention discloses rare earth polishing powder and a preparation method thereof. The polishing powder comprises cerium oxide CeO2 and lanthanum oxide La2O3, wherein the total rare earth amount TREO is over 90 weight percent; and meanwhile, the cerium oxide CeO2 accounts for 75 to 80 percent and the lanthanum oxide La2O3 accounts for 20 to 25 percent of the total rare earth amount TREO of 739-2 type rare earth polishing powder. In order to ensure necessary grinding velocity, a fluorine F element having chemical action is added in a wet synthesis process and the initial forming of product granularity is controlled to make the grinding velocity higher and reduce the damage to a grinding surface.
Description
Technical field
The invention belongs to rare-earth products preparation field, particularly a kind of polishing powder from rare earth and manufacture method thereof.
Background technology
Polishing powder from rare earth, as a kind of new grinding material, is widely used as the grinding of glass material etc., glass substrate of using as crystal works, water brill, CD, disk, LCD, HD etc.Using the every field of grinding-material, more and more higher to the requirement of grinding-material, comprise its performance, price.Especially in the polishing of crystal works, wrist-watch, electronic component etc., they are main mainly with manual throwing greatly.Require grinding rate more and more faster, and reduce the damage of abradant surface.At present, polishing powder is made probably dry method and two kinds of techniques of wet method.Dry method be directly Rare Earth Mine pulverized, calcine, fluoridized, ball milling; Wet method is that re chloride that Rare Earth Mine is made through sulfuric acid baking, water logging, organic solvent extraction is through synthetic, calcining, wet classification.Raw material forms mainly with cerium oxide CeO2, lanthana La
2o
3, praseodymium oxide Pr
6o
11, neodymia Nd
2o
3be main.In short supply due to rare earth mineral resources in recent years, the price of praseodymium oxide, neodymia is fault wall liter not.Be that raw material making polishing powder is more and more difficult with lanthanum, cerium, praseodymium, neodymium.In view of the situation, invented the polishing powder from rare earth take sufficient lanthanum on market, cerium as raw material.And the grinding rate that has guaranteed it is fast and the polishing powder from rare earth of higher abradant surface precision, has reduced grinding-material cost, has effectively utilized rare earth resources.
Summary of the invention
The object of this invention is to provide one take lanthanum, cerium as raw material manufacture grinding rate is higher, damage the polishing powder from rare earth and the manufacture method thereof that occur still less.
For achieving the above object, a kind of polishing powder from rare earth of the present invention, in the total amount of rare earth TREO of polishing powder from rare earth, cerium oxide CeO
2the ratio of content accounts for 73-80%, lanthana La
2o
3the ratio of content accounts for 20-25%, praseodymium oxide Pr
6o
11content ratio 1%; Neodymia Nd
2o
3content ratio 0.2%.
The manufacture method of above-mentioned a kind of polishing powder from rare earth, realizes by following steps:
One, by cerium oxide CeO
2the ratio of content accounts for 73-80%, lanthana La
2o
3the ratio of content accounts for 20-25%, praseodymium oxide Pr
6o
11content ratio 1%; Neodymia Nd
2o
3content ratio 0.2% is mixed with into few neodymium rare earth chloride solution raw material for standby with water;
Two, with nertralizer ammoniacal liquor NH
3h
2the pH value to 4.0 of few neodymium rare earth chloride material liquid prepared by O regulating step one, then carries out plate and frame filter press filtration, removes the non-rare earth impurities such as thorium, iron, slag, puts into storage tank for subsequent use;
Three, being first 45% with content by the few neodymium rare earth chloride material liquid making in step 2, silicofluoric acid and content are that 93% sulfate additive is together put into enamel tank diameter, be warming up to 85 ℃～95 ℃ after stirring time, precipitate, precipitation reagent is selected carbonic hydroammonium NH
4hCO
3, because the speed that adds of precipitation reagent directly affects the nucleation rate of precipitation, precipitation reaction is fast, and nucleation rate is fast, and particle is difficult for growing up, so the sedimentation time is controlled at 2 hours;
Four, etc. after the precipitation of step 3 completes, will lack neodymium rare earth chloride solution and boil 1h through 85 ℃～95 ℃, and impel sediment to be changed into the subcarbonate that is conducive to rubbing down by carbonate, in rinsing bowl, wash away micro-superfine powder and excessive ammonium chloride NH
4cl;
Five, few neodymium rare earth chloride solution step 4 being made is crossed moisture content through vacuum filtering system, carry out roasting with tunnel cave,, temperature is controlled at 900 ℃-980 ℃, roasting time is 5-7h, after roasting, material and 4 parts of pure water are sized mixing, and then carry out classification through 500 order wet method vibration screening, the spray-dried machine atomizer of slip is injected into vaporific, at 500 ℃, moment is removed moisture, and gained material carries out dry method grading with dry classification machine again, obtains the polishing powder from rare earth that meets granularity requirements.
Repeatedly study by the grinding rate to polishing powder from rare earth, damage, determined lanthanum, cerium amount control regulation ratio, granule size, technological process.Grinding rate is higher, damages littlely, and completes thus the present invention.Its feature is that laser diffractometry volume average particle size D50 is 1.5um～2.5um, and the granular size of polishing powder has directly determined the grinding effect that polishing velocity and polishing can reach; Though the too large grinding rate of granularity is fast but damage occurrence degree is high; The too little grinding rate of granularity is slow but damage occurrence degree is low, and it is bad to be prone to cleaning; The glass hard (HRC65Yi Shang)s such as crystal works, wrist-watch, electronic component are larger, must guarantee that it has good hardness and chemism.In raw material, cerium oxide CeO2 content accounts for 75wt%-80wt% in the ratio of total amount of the rare earth oxide TREO, can make and have the above polishing powder from rare earth that requires level of performance.Therefore, be set as 1.5um-2.5um take laser diffractometry volume average particle sizes D50 as benchmark carries out particle diameter, the particle state of polishing powder from rare earth be controlled, thereby produce the polishing powder from rare earth of adaptation.
As mentioned above, the better scope of laser diffractometry volume average particle size D50 is 1.5un-2.5um, and D50 is lower than lower limit for this volume average particle sizes, and rubbing down speed does not reach application requirements; If exceed higher limit, in application, can scratch the lapped face of polished object, even refine in later process, be to be also difficult for eliminating.Therefore, the factor of comprehensive two aspects, the long-pending mean particle size D 50 of laser diffractometry Ma Er style is preferably controlled at 1.5um-2.5um.
Polishing powder from rare earth, its rare earth oxide TREO total amount is better more than 90wt%, in each component ratio one timing of rare earth, the ratio of cerium oxide CeO2 content and rare earth oxide TREO total amount is larger, the ratio of cerium oxide CeO2 in polishing powder composition is just larger, the content of other impurity is just lower, thereby can effectively reduce the generation that scratches phenomenon.Result of study shows, the ratio of cerium oxide CeO2 content in rare earth oxide TREO total amount is preferably controlled at 75wt%-80wt%, and the ratio of cerium oxide is higher, more easily produces cut, if exceed the upper limit, scratches polished object lapped face; The ratio of cerium oxide is lower, and rubbing down speed can be affected.Praseodymium oxide Pr
6o
11, neodymia Nd
2o
3content in the proportional control of total amount of the rare earth oxide TREO at trace.
Fluorine F content is at the ratio general control of total amount of the rare earth oxide TREO at 4wt%-6wt%, and the ratio of fluorine F content is higher, stronger in the chemical action on rubbing down surface, causes lapped face roughness large, causes grinding effect on the low side.If exceed the upper limit, in use rubbing down surface there will be rough interface, is mainly the result due to chemical action; Because rubbing down speed is along with the reduction of fluorine F content reduces, so fluorine F content ratio, lower than lower limit, reduces grinding rate greatly, be mainly that chemical action effect is faint; Therefore, the factor of comprehensive two aspects, fluorine F content is preferably controlled at 4.5wt%-5.5wt% in the ratio of total amount of the rare earth oxide TREO.Fluorine F element plays very important effect in polishing powder from rare earth polishing process, it directly affects the formation of crystal structure, and participate in chemisorbed, in polishing powder from rare earth, the introducing of fluorine F element is to be additive by silicofluoric acid and sulfuric acid, take ammonium bicarbonate soln as precipitation reagent, form fluorine carbonated rare earth intermediate with rare earth, in roasting process, form a kind of fluorine F atmosphere, facilitate the formation of product; Only has micro-fluorine F ion with cerous fluoride CeF
3form in finished product, generate; This polishing powder experiences twice crystal grain and makes brilliant process, forms for the first time the rare earth fluoro carbonate precursor particle that there is no grainding capacity completely, and for the second time through high-temperature roasting, circular configuration part is originally destroyed, and forms the product that meets application requirements.Be the research situation to repeatedly roasting below, consequently: the sintering temperature of polishing powder from rare earth is better controlled at 900 ℃-980 ℃, sintering temperature is lower than lower limit, and in sintering procedure, the particle diameter of polishing powder can not become greatly, causes rubbing down speed to decline; If sintering temperature is higher, the particle diameter of output powder is large, easily scratches the lapped face that is polished body in application; Therefore, the factor of comprehensive two aspects, sintering temperature is preferably controlled at 900 ℃-980 ℃.Roasting time is controlled at 5-7 hour, and roasting time is lower than lower limit, and particle transforms not exclusively, lower hardness, and cutting force declines; Roasting time is higher than higher limit, and particle aggregation is serious, and wear extent increases.
Embodiment
First prepare few neodymium rare earth chloride solution raw material, its rare earth component is cerium oxide CeO
2the ratio of content accounts for 75-80%, lanthana La
2o
3the ratio of content accounts for 20-25%, praseodymium oxide Pr
6o
11content ratio is less than 1%; Neodymia Nd
2o
3content ratio is less than 0.2%.
First use nertralizer ammoniacal liquor NH
3h
2o regulates the pH value to 4.0 of material liquid, then carries out plate and frame filter press filtration, removes the non-rare earth impurities such as thorium, iron, slag, puts into storage tank for subsequent use; Manufacture polishing powder from rare earth presoma with ready few neodymium rare earth chloride solution raw material: the silicofluoric acid 10L that the few neodymium rare earth chloride solution 850L that is first 198g/L by the content preparing and content are 45% and content are that 93% sulfate additive 6L together puts into enamel tank diameter, be warming up to 85 ℃～95 ℃ after stirring time, precipitate, precipitation reagent is selected carbonic hydroammonium NH
4hCO
3.Because the speed that adds of precipitation reagent directly affects the nucleation rate of precipitation, precipitation reaction is fast, and nucleation rate is fast, and particle is difficult for growing up, so the sedimentation time is controlled at 2 hours; After precipitation reaction completes, boil 1h through 85 ℃～95 ℃, impel sediment to be changed into the subcarbonate that is conducive to rubbing down by carbonate, in rinsing bowl, wash away micro-superfine powder and excessive ammonium chloride NH
4cl, ammonium chloride NH
4cl content is less than 15g/L; Cross moisture content through vacuum filtering system, carry out roasting with tunnel cave,, temperature is controlled at 900 ℃-980 ℃, roasting time is 5-7h, after roasting, material and 4 parts of pure water are sized mixing, and 500 order wet method vibration screening are carried out classification, the spray-dried machine atomizer of slip is injected into vaporific, at 500 ℃, moment is removed moisture, and gained material carries out dry method grading with dry classification machine again, obtains the polishing powder from rare earth that meets granularity requirements.
Claims (1)
1. a manufacture method for polishing powder from rare earth, is characterized in that: in the total amount of rare earth TREO of described polishing powder from rare earth, and cerium oxide CeO
2the ratio of content accounts for 73-80%, lanthana La
2o
3the ratio of content accounts for 20-25%, praseodymium oxide Pr
6o
11content ratio l%, neodymia Nd
2o
3content ratio 0.2%; This polishing powder from rare earth is prepared by following steps:
One, by cerium oxide CeO
2the ratio of content accounts for 73-80%, lanthana La
2o
3the ratio of content accounts for 20-25%, praseodymium oxide Pr
6o
11content ratio l%, neodymia Nd
2o
3content ratio 0.2% mixes and is prepared into few neodymium rare earth chloride solution raw material for standby with water;
Two, with nertralizer ammoniacal liquor NH
3h
2the pH value to 4.0 of few neodymium rare earth chloride material liquid prepared by O regulating step one, then carries out plate and frame filter press filtration, removes the non-rare earth impurities such as thorium, iron, slag, puts into storage tank for subsequent use;
Three, being first 45% with content by the few neodymium rare earth chloride material liquid making in step 2, silicofluoric acid and content are that 93% sulfate additive is together put into enamel tank diameter, be warming up to 85 ℃～95 ℃ after stirring time, precipitate, precipitation reagent is selected carbonic hydroammonium NH
4hCO
3, because the speed that adds of precipitation reagent directly affects the nucleation rate of precipitation, certainly, nucleation rate is fast in precipitation reaction, and particle is difficult for growing up, so the sedimentation time is controlled at 2 hours;
Four, etc. after the precipitation of step 3 completes, will lack neodymium rare earth chloride solution and boil 1 h through 85 ℃～95 ℃, and impel sediment to be changed into the subcarbonate that is conducive to rubbing down by carbonate, in rinsing bowl, wash away micro-superfine powder and excessive ammonium chloride NH
4cl, ammonium chloride NH
4cl content is less than 15g/L;
Five, few neodymium rare earth chloride solution step 4 being made is crossed moisture content through vacuum filtering system, carry out roasting with tunnel cave, temperature is controlled at 900 ℃～980 ℃, and roasting time is 5-7h, after roasting, material and 4 parts of pure water are sized mixing, then carry out classification through 500 order wet method vibration screening, the spray-dried machine atomizer of slip is injected into vaporific, and at 500 ℃, moment is removed moisture, gained material carries out dry method grading with dry classification machine again, obtains the polishing powder from rare earth that meets granularity requirements.
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102114615B (en) * | 2010-12-21 | 2012-08-08 | 珠海市吉昌稀土有限公司 | Rare earth polishing disc |
| CN102585707B (en) * | 2012-02-28 | 2014-01-29 | 上海华明高纳稀土新材料有限公司 | Preparation method of cerium-based mixed rare earth polishing powder |
| 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 |
| CN102992385B (en) * | 2012-12-24 | 2015-10-14 | 安阳金石研磨材料有限公司 | The production technique of nano level octahedral bodily form cerium lanthanum oxide polishing powder from rare earth |
| CN103011237A (en) * | 2012-12-24 | 2013-04-03 | 安阳金石研磨材料有限公司 | Production process of nano mono-spherical lanthanum oxide cerium rare earth polishing powder |
| CN102992386A (en) * | 2012-12-24 | 2013-03-27 | 安阳金石研磨材料有限公司 | Production process of nanoscale tetragonal lanthanum-cerium-rare earth oxide polishing powder |
| 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 |
| CN103468149A (en) * | 2013-09-18 | 2013-12-25 | 苏州市博飞光学有限公司 | Chlorinated rare earth polishing powder and production method thereof |
| CN103923569B (en) * | 2014-05-06 | 2015-07-08 | 济南大学 | Preparation method of jade polishing powder |
| CN104828853B (en) * | 2015-04-29 | 2016-09-14 | 甘肃稀土新材料股份有限公司 | A kind of preparation method of the few neodymium rare earth oxide of spherical middle specific surface area |
| CN106978090A (en) * | 2017-04-20 | 2017-07-25 | 德米特（苏州）电子环保材料有限公司 | A kind of preparation method of rare earth fluoride polishing powder |
| CN107556922B (en) * | 2017-09-27 | 2020-05-19 | 甘肃稀土新材料股份有限公司 | Samarium-containing rare earth polishing powder and preparation process thereof |
| CN108864948A (en) * | 2018-08-17 | 2018-11-23 | 蓝思科技（长沙）有限公司 | Glass polishing powder, polishing fluid and preparation method thereof, glass and electronic product |
| CN109111855A (en) * | 2018-08-24 | 2019-01-01 | 甘肃稀土新材料股份有限公司 | A kind of LaCePrNd yttrium element polishing powder and its preparation process |
| CN110564304B (en) * | 2019-09-24 | 2021-07-13 | 四川虹科创新科技有限公司 | High-aluminum alkali-containing glass polishing solution and preparation method thereof |
| CN111471865A (en) * | 2020-05-26 | 2020-07-31 | 湖南稀土金属材料研究院 | Method for recovering rare earth polishing powder waste |
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| TWI313707B (en) * | 2003-04-17 | 2009-08-21 | Mitsui Mining & Smelting Co | Cerium-based abrasive |
| CN1194060C (en) * | 2003-07-24 | 2005-03-23 | 南开大学 | Preparation method of rare-earth polishing powder |
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