CN103058254B - Preparation method of large-particle lutetium oxide - Google Patents
Preparation method of large-particle lutetium oxide Download PDFInfo
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- CN103058254B CN103058254B CN201210386972.XA CN201210386972A CN103058254B CN 103058254 B CN103058254 B CN 103058254B CN 201210386972 A CN201210386972 A CN 201210386972A CN 103058254 B CN103058254 B CN 103058254B
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Abstract
The invention relates to a preparation method of large-particle lutetium oxide, belonging to a preparation technology of material. The method comprises the following steps of: preparing an ammonium bicarbonate solution with ammonium bicarbonate, ammonia water and deionized water, adding lutetium nitrate hydrate solution to the ammonium bicarbonate solution to obtain a mixed solution of ammonium bicarbonate, ammonia water and lutetium nitrate hydrate, adding hydrogen peroxide to the mixed solution, reacting for 6 hours to generate a lutetium carbonate hydrate precipitation, aging for 24-48 hours, filtering and washing the precipitation, keeping the firing temperature at 900-1200 DEG C for thermal insulation for 4 hours to obtain the large-particle gadolinium oxide product, which has the characteristics of uniform particle, favorable liquidity, and the morphology of which appears to be a petal piled by sheet and the central grain size D50 of which is 50-165 micrometers.
Description
Technical field
The present invention relates to a kind of method of preparing macrobead lutecium oxide, belong to a kind of material preparation process.
Background technology
Lutecium oxide is for the manufacture of tinting material, laserable material, luminescent material, the electronic material of magneticsubstance, opticglass, pottery.Lutecia based transparent ceramics material, by playing an important role in following digital radial imaging technological system, is particularly suitable for the application of static number imaging and fluoroscopy aspect, is also a kind of novel polycrystalline laser working medium.Along with scientific and technical development, macrobead lutecium oxide demand is more and more, the amount that forms the fine granular of superfusion due to macrobead lutecium oxide as hot spray powder when the thermospray can reduce, the fine granular that small-particle forms in the time of thermospray adheres to and be deposited on the nozzle inner walls of hot spray apparatus and the settling that forms comes off from inwall, and be blended in hot spray coating, the anti-characteristic of concentration of hot spray coating is declined, directly preparation meets the lutecium oxide powder particle of thermospray requirement, can improve coating density, anti-characteristic of concentration and wear resistance.And the lutecium oxide granularity of utilizing rare-earth industry traditional method oxalic acid lutetium precipitation or carbonic acid lutetium precipitation is generally within the scope of 1-15 μ m, this lutecium oxide is as hot spray powder after granulation, and its coating is not as the performance of macrobead lutecium oxide direct spraying coating.
Summary of the invention
The object of the present invention is to provide a kind of uniform particles, good fluidity, medium particle diameter D
50for 50-165 μ m, pattern are made up of the preparation method of flower-shaped macrobead lutecium oxide thin slice.
Technical solution: the present invention adds respectively ammoniacal liquor and the deionized water that bicarbonate of ammonia, concentration are 28% in reactor, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the lutecium nitrate solution of 1.47mol/L, bicarbonate of ammonia and lutecium nitrate mol ratio are 1: 0.096, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and lutecium nitrate; Be 30% hydrogen peroxide to adding concentration in mixing solutions, lutecium nitrate and hydrogen peroxide mol ratio are 1: 5.2, react and within 6 hours, start to produce precipitation, ageing 24-48 hour, obtains carbonic acid lutetium precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50for 50-165 μ m, even particle distribution, good fluidity, pattern form flower-shaped macrobead lutecium oxide by thin slice.
Invention effect
In the present invention, carbonic acid lutetium precipitation digestion time and calcination temperature are crucial, and digestion time is the key factor that determines carbonic acid lutetium granularity, and digestion time is less than 4 hours, and carbonic acid lutetium deposit seeds is very thin, sad filter, and static ageing more than 24 hours, obtains macrobead carbonic acid lutetium; Carbonic acid lutetium calcination temperature selects suitability for industrialized production oxalic acid lutetium to be decomposed into the temperature range of lutecium oxide, is convenient to suitability for industrialized production Device-General, and calcination temperature is 900-1200 DEG C, according to the market requirement, and can suitability for industrialized production uniform particles, good fluidity, medium particle diameter D
50for 50-165 μ m, pattern form flower-shaped macrobead lutecium oxide by thin slice.
Brief description of the drawings
Fig. 1 is the XRD figure of macrobead lutecium oxide of the present invention;
Fig. 2 is the particle size distribution figure of macrobead lutecium oxide of the present invention;
Fig. 3 is the SEM figure of macrobead lutecium oxide of the present invention.
Embodiment
Embodiment 1
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 290ml concentration be the lutecium nitrate solution of 1.47mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and lutecium nitrate; Be 30% hydrogen peroxide to adding 230ml concentration in mixing solutions, react and within 6 hours, start to produce precipitation, ageing 32 hours, obtains carbonic acid lutetium precipitation, and by sedimentation and filtration, washing, calcination temperature is 900 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead lutecium oxide of 51.01 μ m.
Embodiment 2
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 290ml concentration be the lutecium nitrate solution of 1.47mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and lutecium nitrate; Be 30% hydrogen peroxide to adding 230ml concentration in mixing solutions, react and within 6 hours, start to produce precipitation, ageing 40 hours, obtains carbonic acid lutetium precipitation, and by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead lutecium oxide of 129.1 μ m.
Embodiment 3
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 290ml concentration be the lutecium nitrate solution of 1.47mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and lutecium nitrate; Be 30% hydrogen peroxide to adding 230ml concentration in mixing solutions, react and within 6 hours, start to produce precipitation, ageing 48 hours, obtains carbonic acid lutetium precipitation, and by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead lutecium oxide of 165.8 μ m.
Claims (1)
1. prepare the method for macrobead lutecium oxide, it is characterized in that, in reactor, add respectively ammoniacal liquor and the deionized water that bicarbonate of ammonia, concentration are 28%, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the lutecium nitrate solution of 1.47mol/L, bicarbonate of ammonia and lutecium nitrate mol ratio are 1: 0.096, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and lutecium nitrate; Be 30% hydrogen peroxide to adding concentration in mixing solutions, lutecium nitrate and hydrogen peroxide mol ratio are 1: 5.2, react and within 6 hours, start to produce precipitation, ageing 24-48 hour, obtains carbonic acid lutetium precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50for 50-165 μ m, even particle distribution, good fluidity, pattern form flower-shaped macrobead lutecium oxide by thin slice.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210386972.XA CN103058254B (en) | 2012-09-22 | 2012-09-22 | Preparation method of large-particle lutetium oxide |
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| CN201210386972.XA CN103058254B (en) | 2012-09-22 | 2012-09-22 | Preparation method of large-particle lutetium oxide |
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| CN103058254A CN103058254A (en) | 2013-04-24 |
| CN103058254B true CN103058254B (en) | 2014-12-03 |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2868176B2 (en) * | 1993-04-27 | 1999-03-10 | 信越化学工業株式会社 | Method for producing rare earth element oxide powder |
| JPH08119631A (en) * | 1994-10-21 | 1996-05-14 | Shin Etsu Chem Co Ltd | Production of spherical oxide of rare earth element and its precursor |
| CN1255560C (en) * | 2004-06-28 | 2006-05-10 | 辽宁美宝稀土材料有限公司 | Process for recovering rare earth from neodymium-ion-boron waste materials |
| CN100336777C (en) * | 2005-06-28 | 2007-09-12 | 中国科学院上海硅酸盐研究所 | Method for preparing lutecia based transparent ceramics |
| CN101020580A (en) * | 2006-02-13 | 2007-08-22 | 宜兴新威集团有限公司 | Process of preparing nanometer level RE oxide |
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