CN102079950A - Preparation method of monodisperse rare earth polishing powder - Google Patents
Preparation method of monodisperse rare earth polishing powder Download PDFInfo
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- CN102079950A CN102079950A CN2009101942023A CN200910194202A CN102079950A CN 102079950 A CN102079950 A CN 102079950A CN 2009101942023 A CN2009101942023 A CN 2009101942023A CN 200910194202 A CN200910194202 A CN 200910194202A CN 102079950 A CN102079950 A CN 102079950A
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Abstract
The invention provides monodisperse rare earth polishing powder and a preparation method thereof. In the preparation technology, one or the mixture of more than one of ammonium oxlate and urea is taken as a precipitating agent; when rare earth solution containing cerium is reacted with the precipitant solution, precursor precipitated particles with almost uniform geometry are formed by utilizing the molecule template effect of high-molecular surfactants and the synergism of high-molecular surfactants and the precipitating agent; acidity and ionic strength of the mother liquor are adjusted by adding ammonium bicarbonate and hydrofluoric acid into the slurry after precipitation, and thus surface electric property of solid particles in the slurry is enhanced; superfine rare earth polishing powder with good dispersibility and high spheroidizing rate is obtained after heating and aging, filtering, drying of the filter cake, burning, ball milling and screening, jet mill crushing and separating, and centrifugal classification. The obtained polishing powder is spherical with good dispersibility. The particle size D50 is in the range of 0.50-0.30 micrometers, and all the following conditions are met: D10 is larger than or equal to 0.8*D50; D90 is smaller than or equal to 3*D50; and D100 is smaller than or equal to 5*D50. The polishing powder possesses good suspension performance, strong dispersibility, and leaves little scratching on polished surfaces of optical glass and crystal when used in glass polishing. In addition, the polishing cutting force is large and polished surfaces have high planarity.
Description
Technical field
The present invention relates to monodisperse rare-earth polishing powder preparation method
Background technology
Rare earth oxide can be used as the high-efficiency high-quality polishing material of glass, superiority such as its polishing efficiency height, applied widely, long service life, the general chemically machinery polished that is applied to field precision glass polishing such as optical element, glasses, LCD, industrial instrument and super large-scale integration silica dioxide medium layer.Polishing powder from rare earth is a kind of mixed light rare earth oxide compound, and main component is CeO
2, La
2O
3, Pr
6O
11, Nd
2O
3Deng.The polishing powder from rare earth that China produces is more with low-grade polishing powder, and industrial scale is little, and the product homogeneity is poor.In the device polishing of having relatively high expectations, still need the high-grade polishing powder of dependence on import, the polishing performance of polishing powder and pattern and particle diameter are closely related, in high precision polishing, the granularity of powder, pattern and distributing homogeneity thereof have played significant feature, particle is thin more, subsphaeroidal more, it is even more to distribute, and then polishing effect is good more.The present invention utilizes polymeric surface active agent to control polishing powder from rare earth powder geometrical shape as molecular template.
Summary of the invention
The invention provides a kind of preparation method of the monodisperse rare-earth polishing powder based on cerium dioxide, adopt this method can obtain the polishing powder of consistent appearance, thereby help satisfying the precise polished requirement of differing materials.The total technical conceive of the present invention is, in the reaction that contains cerium, lanthanum, praseodymium, neodymium earth solution and urea, volatile salt, oxalic acid precipitation agent solution, utilize the synergy of the molecular template effect of polymeric surface active agent (AESA, lauryl alcohol ammonium sulfate and Triton X-100) and itself and precipitation agent, the precursor deposit seeds that the formation geometrical shape reaches unanimity; Then through through wet ball grinding, the airflow milling cracking and sorting, centrifugal classification, it is moderate to obtain hardness after the drying, the polishing powder from rare earth that pattern is controlled.
Technical scheme of the present invention is as follows:
1, with cerous nitrate, lanthanum nitrate, praseodymium nitrate, neodymium nitrate and tensio-active agent (AESA, lauryl alcohol ammonium sulfate and Triton X-100) be dissolved in the deionized water, the concentration range of cerium is 0.1～0.3mol/l, the concentration range of lanthanum is 0.05～0.10mol/l, the concentration range of praseodymium is 0.05～0.10mol/l, the concentration range of neodymium is 0.05～0.10mol/l, tensio-active agent is an AESA, the mixture of lauryl alcohol ammonium sulfate and Triton X-100, the content of tensio-active agent is 0.005～0.02% in the solution;
2, precipitation agent is dissolved in the deionized water, precipitation agent is urea, volatile salt, oxalic acid, the mixture of urea, and wherein urea concentration is 0.1mol/l～2.0mol/l, volatile salt concentration is 0.1mol/l～1.0mol/l, and concentration of oxalic acid is 0.1mol/l～1.0mol/l;
3, (1) and (2) mixing solutions is heated to 85 ℃, in earth solution, adds precipitant solution with spray pattern by stirring, add finish after, continue to stir 30～60min, system temperature is controlled under 85 ℃～95 ℃ the temperature and is incubated 8h;
4, add acidity and the ionic strength that a certain amount of volatile salt (0.1～0.5%) and hydrofluoric acid (0.05～0.5%) are regulated mother liquor of precipitation of ammonium at mixing solutions, ageing 12h at room temperature then,
5, solid precipitation after the washing, carries out drying under the condition at 120～200 ℃ after filtration, obtains the presoma of polishing powder, and calcining 2h obtains polishing powder from rare earth under 1000～1200 ℃ of conditions again,
6 polishing powder from rare earth process wet ball grinding, the airflow milling cracking and sorting, centrifugal classification obtains single distribution polishing powder from rare earth after the drying.
Concrete enforcement
Embodiment 1:
1, cerous nitrate, lanthanum nitrate, praseodymium nitrate, neodymium nitrate and tensio-active agent (AESA, lauryl alcohol ammonium sulfate and Triton X-100) are dissolved in the deionized water, the concentration range of cerium is 0.15mol/l, the concentration range of lanthanum is 0.05mol/l, the concentration range of praseodymium is 0.08mol/l, the concentration range of neodymium is 0.05mol/l, tensio-active agent is the mixture of AESA, lauryl alcohol ammonium sulfate and Triton X-100, and the content of tensio-active agent is 0.02% in the solution;
2, precipitation agent is dissolved in the deionized water, precipitation agent is urea, volatile salt, oxalic acid, and the mixture of urea, urea concentration are 0.2mol/l, and volatile salt concentration is 0.1mol/l, and concentration of oxalic acid is 0.1mol/l;
3, (1) and (2) mixing solutions is heated to 85 ℃, in earth solution, adds precipitant solution with spray pattern by stirring, add finish after, continue to stir 30min, system temperature is controlled under 85 ℃～90 ℃ the temperature and is incubated 8h;
4, add acidity and the ionic strength that a certain amount of volatile salt (0.1%) and hydrofluoric acid (0.05%) are regulated mother liquor of precipitation of ammonium at mixing solutions, ageing 12h at room temperature then,
5, filter, solid precipitation carries out drying under the condition at 120 ℃ after washing, obtain the presoma of polishing powder, and calcining 2h obtains cerium rouge under 1200 ℃ of conditions again,
6, cerium rouge process wet ball grinding, the airflow milling cracking and sorting, centrifugal classification obtains the monodisperse rare-earth polishing powder after the drying, and the D50 particle diameter of polishing powder is 1.8 μ m; And satisfy: D10 〉=1.0D50, D90≤3D50, D100≤4.8D50.。
Embodiment 2:
1, cerous nitrate, lanthanum nitrate, praseodymium nitrate, neodymium nitrate and tensio-active agent (AESA, lauryl alcohol ammonium sulfate and Triton X-100) are dissolved in the deionized water, the concentration range of cerium is 0.3mol/l, the concentration range of lanthanum is 0.08mol/l, the concentration range of praseodymium is 0.05mol/l, the concentration range of neodymium is 0.05mol/l, tensio-active agent is the mixture of AESA, lauryl alcohol ammonium sulfate and Triton X-100, and the content of tensio-active agent is 0.01% in the solution;
2, precipitation agent is dissolved in the deionized water, precipitation agent is urea, volatile salt, oxalic acid, and the mixture of urea, urea concentration are 1.0mol/l, and volatile salt concentration is 0.2mol/l, and concentration of oxalic acid is 0.1mol/l;
3, (1) and (2) mixing solutions is heated to 85 ℃, in earth solution, adds precipitant solution with spray pattern by stirring, add finish after, continue to stir 30min, system temperature is controlled under 90 ℃ the temperature and is incubated 8h;
4, add acidity and the ionic strength that a certain amount of volatile salt (0.1%) and hydrofluoric acid (0.1%) are regulated mother liquor of precipitation of ammonium at mixing solutions, ageing 12h at room temperature then,
5, solid precipitation filters, and after washing, carries out drying under the condition at 160 ℃, obtains the presoma of polishing powder, and calcining 2h obtains cerium rouge under 1000 ℃ of conditions again,
6, polishing powder from rare earth process wet ball grinding, the airflow milling cracking and sorting, centrifugal classification obtains the monodisperse rare-earth polishing powder after the drying, and the D50 particle diameter of polishing powder is 2.6 μ m; And satisfy: D10 〉=1.2D50, D90≤2.8D50, D100≤4.1D50.
Claims (5)
1. the preparation technology of described monodisperse rare-earth polishing powder, it is characterized in that: rare-earth salts and tensio-active agent is soluble in water, the concentration range of cerium is 0.1～0.3mol/l, the concentration range of lanthanum is 0.05～0.10mol/l, the concentration range of praseodymium is 0.05～0.10mol/l, the concentration range of neodymium is 0.05～0.10mol/l, tensio-active agent is the mixture of AESA, lauryl alcohol ammonium sulfate and Triton X-100, and the content of tensio-active agent is 0.005～0.02%.
2. the preparation technology of described monodisperse rare-earth polishing powder is characterized in that: precipitation agent is urea, volatile salt, oxalic acid.Wherein urea concentration is 0.1mol/l～2.0mol/l, and volatile salt concentration is 0.1mol/l～1.0mol/l, and concentration of oxalic acid is 0.1mol/l～1.0mol/l.
3. the preparation technology of described monodisperse rare-earth polishing powder, it is characterized in that: mixing solutions is incubated 8h under 85 ℃～95 ℃ temperature, add acidity and the ionic strength that a certain amount of ammonium salt (0.1～0.5%) and hydrofluoric acid (0.05～0.5%) are regulated mother liquor of precipitation of ammonium at mixing solutions, then ageing 12h at room temperature.
4. the preparation technology of described monodisperse rare-earth polishing powder is characterized in that: solid precipitation after the washing, carries out drying under the condition at 120 ℃ after filtration, obtains the presoma of polishing powder, and calcining 2h obtains cerium rouge under 1200 ℃ of conditions again.
5. the preparation technology of described monodisperse rare-earth polishing powder is characterized in that: polishing powder from rare earth process wet ball grinding, and the airflow milling cracking and sorting, centrifugal classification obtains polishing powder from rare earth after the drying.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102424728A (en) * | 2011-10-17 | 2012-04-25 | 南京航空航天大学 | Preparation method for highly-dispersed fine lanthanum oxide slurry |
| CN102850938A (en) * | 2011-12-19 | 2013-01-02 | 南昌大学 | Preparation method of spherical composite rare earth polishing powder |
| CN103805067A (en) * | 2012-11-07 | 2014-05-21 | 有研稀土新材料股份有限公司 | Preparation method of cerium-based polishing powder |
| 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 |
| 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 |
-
2009
- 2009-11-27 CN CN2009101942023A patent/CN102079950A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102424728A (en) * | 2011-10-17 | 2012-04-25 | 南京航空航天大学 | Preparation method for highly-dispersed fine lanthanum oxide slurry |
| CN102850938A (en) * | 2011-12-19 | 2013-01-02 | 南昌大学 | Preparation method of spherical composite rare earth polishing powder |
| CN103805067A (en) * | 2012-11-07 | 2014-05-21 | 有研稀土新材料股份有限公司 | Preparation method of cerium-based polishing powder |
| CN103805067B (en) * | 2012-11-07 | 2015-11-25 | 有研稀土新材料股份有限公司 | A kind of preparation technology of cerium based relief polishing powder |
| 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 |
| 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 |
| 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 |
| US11214713B2 (en) | 2017-10-31 | 2022-01-04 | Hoya Corporation | Polishing liquid, method for manufacturing glass substrate, and method for manufacturing 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 |
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Application publication date: 20110601 |