CN102992381B - Method for preparing macrogranular ytterbium oxide - Google Patents
Method for preparing macrogranular ytterbium oxide Download PDFInfo
- Publication number
- CN102992381B CN102992381B CN201210386963.0A CN201210386963A CN102992381B CN 102992381 B CN102992381 B CN 102992381B CN 201210386963 A CN201210386963 A CN 201210386963A CN 102992381 B CN102992381 B CN 102992381B
- Authority
- CN
- China
- Prior art keywords
- ytterbium
- hours
- macrogranular
- concentration
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a method for preparing macrogranular ytterbium oxide, belonging to material preparation processes. The method comprises the steps of preparing an ammonium bicarbonate solution by using ammonium bicarbonate, ammonia water and deionized water, adding an ytterbium nitrate solution into the ammonium bicarbonate solution to obtain a mixed solution consisting of the ammonium bicarbonate, the ammonia water and the ytterbium nitrate, adding hydrogen peroxide into the mixed solution, reacting for 4 hours till ytterbium carbonate precipitates begin to generate, ageing for 24-48 hours, filtering and washing the precipitates, scorching the precipitates at 900-1200 DEG C, and preserving heat for 4 hours to obtain macrogranular ytterbium oxide products, which have the medium particle diameter D50 being 55-60 microns, are uniform in particle and good in flowability and take the shape of a petal formed by lamella stacking.
Description
Technical field
The present invention relates to a kind of method preparing macrogranular ytterbium oxide, belong to a kind of material preparation process.
Background technology
Ytterbium oxide for the manufacture of permanent magnet material, glass, pottery tinting material, laserable material, for barrier coating material, electronic material, battery material, bio-pharmaceuticals, electronic industry and chemical research application demonstrate superior performance.Along with the development of science and technology, macrogranular ytterbium oxide is applied to coating, sputtering, the fields such as vacuum plating, as ytterbium oxide plated film on diamond surface, infrared transmittivity is made to make raising 12%, and there is higher anti-rain corrosive nature, macrogranular ytterbium oxide demand gets more and more, the amount forming the fine granular of superfusion due to macrogranular ytterbium oxide as hot spray powder when thermospray can reduce, the fines adhesion that small-particle is formed when thermospray is also deposited on the nozzle inner walls of hot spray apparatus and the settling formed comes off from inwall, and be mixed in hot spray coating, the anti-characteristic of concentration of hot spray coating is declined, direct preparation meets the ytterbium oxide powder particle of thermospray requirement, coating density can be improved, anti-characteristic of concentration and wear resistance.And utilizing the ytterbium oxide granularity of rare-earth industry traditional method ytterbium oxalate precipitation or ytterbium carbonate precipitation generally within the scope of 1-15 μm, this ytterbium oxide is as hot spray powder after granulation, and its coating is not as the performance of macrogranular ytterbium oxide direct spraying coating.
Summary of the invention
A kind of uniform particles, good fluidity, pattern is the object of the present invention is to provide to build up petal-shaped, medium particle diameter D by thin slice
50for the macrogranular ytterbium oxide preparation method of 55-60 μm.
Technical solution: the present invention adds bicarbonate of ammonia respectively in reactor, concentration is 28% ammoniacal liquor and deionized water, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, add the ytterbium nitrate solution that concentration is 1.75mol/L, bicarbonate of ammonia and ytterbium nitrate mol ratio are 1: 0.078, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add the hydrogen peroxide of 30%, ytterbium nitrate and hydrogen peroxide mol ratio are 1: 4.6, react and within 4 hours, start to produce precipitation, ageing 24-48 hour, obtains ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50for 55-60 μm, even particle distribution, good fluidity, pattern build up petal-like macrogranular ytterbium oxide by thin slice.
Invention effect
In the present invention, ytterbium carbonate precipitation digestion time and calcination temperature are crucial, and digestion time is the key factor determining ytterbium carbonate granularity, and digestion time is less than 4 hours, and ytterbium carbonate deposit seeds is very thin, sad filter, and static ageing more than 24 hours, obtains ytterbium carbonate; Ytterbium carbonate calcination temperature selects suitability for industrialized production ytterbium oxalate to be decomposed into the temperature range of ytterbium oxide, be convenient to suitability for industrialized production Device-General, calcination temperature is 900-1200 DEG C, according to the market requirement, suitability for industrialized production uniform particles, good fluidity, pattern can build up petal-shaped, medium particle diameter D by thin slice
50for the macrogranular ytterbium oxide of 55-60 μm.
Accompanying drawing explanation
Fig. 1 is the XRD figure of macrogranular ytterbium oxide of the present invention;
Fig. 2 is the particle size distribution figure of macrogranular ytterbium oxide of the present invention;
Fig. 3 is the SEM figure of macrogranular ytterbium oxide of the present invention.
Embodiment
Embodiment 1
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the ytterbium nitrate solution that 215ml concentration is 1.53mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add the hydrogen peroxide that 120ml concentration is 30%, react and within 4 hours, start to produce precipitation, ageing 28 hours, obtain ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 900 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrogranular ytterbium oxide of 55.03 μm.
Embodiment 2
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the ytterbium nitrate solution that 215ml concentration is 1.53mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add the hydrogen peroxide that 120ml concentration is 30%, react and within 4 hours, start to produce precipitation, ageing 40 hours, obtain ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrogranular ytterbium oxide of 59.51 μm.
Embodiment 3
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the ytterbium nitrate solution that 215ml concentration is 1.53mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add the hydrogen peroxide that 120ml concentration is 30%, react and within 4 hours, start to produce precipitation, ageing 48 hours, obtain ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrogranular ytterbium oxide of 60.89 μm.
Claims (2)
1. prepare the method for macrogranular ytterbium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the ytterbium nitrate solution that 215 ml concentration are 1.53 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add 120 ml concentration is the hydrogen peroxide of 30%, reacts and within 4 hours, starts to produce precipitation, ageing 28 hours, and obtain ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 900 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrogranular ytterbium oxide of 55.03 μm.
2. prepare the method for macrogranular ytterbium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the ytterbium nitrate solution that 215 ml concentration are 1.53 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add 120 ml concentration is the hydrogen peroxide of 30%, reacts and within 4 hours, starts to produce precipitation, ageing 40 hours, and obtain ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrogranular ytterbium oxide of 59.51 μm.
3. prepare the method for macrogranular ytterbium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the ytterbium nitrate solution that 215 ml concentration are 1.53 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and ytterbium nitrate; In mixing solutions, add 120 ml concentration is the hydrogen peroxide of 30%, reacts and within 4 hours, starts to produce precipitation, ageing 48 hours, and obtain ytterbium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrogranular ytterbium oxide of 60.89 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210386963.0A CN102992381B (en) | 2012-09-22 | 2012-09-22 | Method for preparing macrogranular ytterbium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210386963.0A CN102992381B (en) | 2012-09-22 | 2012-09-22 | Method for preparing macrogranular ytterbium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102992381A CN102992381A (en) | 2013-03-27 |
| CN102992381B true CN102992381B (en) | 2015-06-03 |
Family
ID=47921587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210386963.0A Active CN102992381B (en) | 2012-09-22 | 2012-09-22 | Method for preparing macrogranular ytterbium oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102992381B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110902710B (en) * | 2019-05-13 | 2021-12-07 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity ytterbium fluoride optical glass additive |
| CN112010338B (en) * | 2020-07-27 | 2023-10-31 | 常州市卓群纳米新材料有限公司 | Method for preparing monodisperse low-sodium nanometer ytterbium oxide by sodium salt precipitation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093059A (en) * | 1993-03-29 | 1994-10-05 | 中国科学院长春应用化学研究所 | Preparation of rare earth oxide ultramicro powder by carbonate precipitation method |
| CN101049952A (en) * | 2007-03-23 | 2007-10-10 | 内蒙古科技大学 | Powder of rare-earth oxides with high apparent density and low specific surface area, and preparation method |
| CN101759221A (en) * | 2008-12-25 | 2010-06-30 | 国家纳米技术与工程研究院 | Method for preparing nano cerium dioxide powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4248937B2 (en) * | 2002-06-07 | 2009-04-02 | 昭和電工株式会社 | Method for recovering rare earth oxide from waste liquid containing rare earth element |
-
2012
- 2012-09-22 CN CN201210386963.0A patent/CN102992381B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093059A (en) * | 1993-03-29 | 1994-10-05 | 中国科学院长春应用化学研究所 | Preparation of rare earth oxide ultramicro powder by carbonate precipitation method |
| CN101049952A (en) * | 2007-03-23 | 2007-10-10 | 内蒙古科技大学 | Powder of rare-earth oxides with high apparent density and low specific surface area, and preparation method |
| CN101759221A (en) * | 2008-12-25 | 2010-06-30 | 国家纳米技术与工程研究院 | Method for preparing nano cerium dioxide powder |
Non-Patent Citations (3)
| Title |
|---|
| 唐定骥等主编.草酸盐重量法测定硅铁稀土合金中稀土含量.《稀土金属材料》.2011,第816-817页. * |
| 沈旭.沉淀条件.《化学选矿技术》.2011,第113页. * |
| 洪广言等.纳米级氧化镜的制备与表征.《江西师范大学(自然科学版)》.2002,第696-699页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102992381A (en) | 2013-03-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110997198B (en) | Silver particles and method for producing same | |
| CN102580721B (en) | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method | |
| KR102033542B1 (en) | Silver particle containing inner void and method of manufacture thereof | |
| CN102115214B (en) | Method for preparing small-particle-size cobalt carbonate | |
| CN103253717A (en) | Method for preparing small-size nickel-cobalt lithium manganate precursor | |
| CN102386391A (en) | Method for preparing ternary complex anode material (LiNixCoyMn1-x-yO2) | |
| CN102745662B (en) | Preparation method of amorphous iron phosphate | |
| CN102441675B (en) | Preparation method for high-crystallinity silver powder | |
| CN104478699A (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN102992381B (en) | Method for preparing macrogranular ytterbium oxide | |
| CN104528803A (en) | Preparation method of ZnO flaky porous nanometer material | |
| CN102357658A (en) | Hydrosol for preparing solar photo-thermal conversion absorption film | |
| CN105152231A (en) | Method for preparing lithium battery anode material cobaltous hydroxide | |
| CN102557098A (en) | Method for preparing superfine high-purity barium carbonate powder | |
| CN103058256B (en) | Method for preparing large-granule dysprosium oxide | |
| CN102992379B (en) | Method for preparing spherical macro-granular neodymium oxide | |
| CN102502779A (en) | Quick preparation method for silver-loaded zinc oxide nanometer composite powder | |
| CN103011231B (en) | Method for preparing multihole sheet large-grain praseodymium oxide | |
| CN107098378A (en) | A kind of polymolecularity ITO raw powder's production technologies | |
| CN109317165B (en) | ZnS-SnS2Method for preparing composite | |
| CN102134104A (en) | Method for preparing superfine octahedral cobaltosic oxide through cobalt salt precipitated microwave-induced pyrolysis method | |
| CN103614139B (en) | Reverse co-precipitation is adopted to prepare Gd 2ti 2o 7: the method for Ce nano-luminescent powder body | |
| CN102886526B (en) | Reduction method for preparing superfine cobalt powder by hydrazine hydrate | |
| CN104986799A (en) | Gd2Hf2O7 nano-powder synthesis method through coprecipitation | |
| CN105314667A (en) | Method for preparing ultrathin and uniform dysprosium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |