CN105331332A - Preparing method for nano-composite abrasive for polishing optical quartz glass - Google Patents
Preparing method for nano-composite abrasive for polishing optical quartz glass Download PDFInfo
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- CN105331332A CN105331332A CN201510878342.8A CN201510878342A CN105331332A CN 105331332 A CN105331332 A CN 105331332A CN 201510878342 A CN201510878342 A CN 201510878342A CN 105331332 A CN105331332 A CN 105331332A
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Abstract
The invention discloses a preparing method for a nano-composite abrasive for polishing optical quartz glass. A silicon dioxide nano-composite abrasive is coated with cerium oxide to form the nano-composite abrasive. The preparing method includes the following steps that 1, nano silicon dioxide is prepared; 2, the silicon dioxide nano-composite abrasive coated with cerium oxide is prepared. The preparing method for the nano-composite abrasive for polishing the optical quartz glass is simple and easy to realize, nano silicon dioxide is used as a core, the surface of the nano silicon dioxide is uniformly coated with cerium oxide, the size of the abrasive is effectively reduced, and the dispersion uniformity and surface roughness of the abrasive are improved at the same time; the polished surface performance of the quartz glass can be remarkably improved by using the composite abrasive, and the use performance of the quartz glass is improved.
Description
Technical field
The present invention relates to silica glass processing technique field, particularly relate to the preparation method of the nano combined abrasive material of a kind of optical quartz glass polishing.
Background technology
Silica glass has the high-performance such as spectral transmission wide ranges, high temperature resistant, heat shock resistance, stable chemical performance and resistance to x ray irradiation x, is widely used in manufacturing ultraviolet optics gate, prism and photomask substrate etc. in the fields such as light source, optical communication, laser, space flight and nuclear technique.But silica glass is also typical crisp and hard material, and its processability is poor, at present, chemically machinery polished (Chemicalmechanicalpolishing, CMP) is mainly adopted to carry out the important processing of super-smooth surface.Compounded abrasive is one of key factor affecting Quartz glass surfaces processing characteristics quality.Quartz glass surfaces cut after existing compounded abrasive polishing is serious, and polished surface is smooth not, has a strong impact on outward appearance and the use properties of the silica glass after processing.
Summary of the invention
The technical problem that the present invention mainly solves is to provide the preparation method of the nano combined abrasive material of a kind of optical quartz glass polishing, effectively can improve a difficult problem for silica glass polished surface poor performance.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing the nano combined abrasive material of a kind of optical quartz glass polishing, described nano combined abrasive material is the nano combined abrasive material of cerium oxide coated silica, and described preparation method comprises the steps:
(1) nano silicon is prepared: the reaction vessel of band electromagnetism agitating function is placed in 28 ~ 30 DEG C of thermostat water baths, then ammoniacal liquor, deionized water, surface-modifying agent and propyl alcohol is added wherein, after stirring and evenly mixing, slowly add tetraethoxy again, then after constant temperature stirs 5 ~ 6h, still aging 18 ~ 20h; After centrifugation, solid materials wet lapping, calcining, grinding, obtain nanometer silicon dioxide particle;
(2) the nano combined abrasive material of cerium oxide coated silica is prepared: get the nanometer silicon dioxide particle obtained in a certain amount of step (1), add deionized water and polyvinylpyrrolidone, six water cerous nitrate and alkaline matters are added after heated and stirred, stirring reaction 3 ~ 4h, then obtains described nano combined abrasive material through centrifugation, washing, drying, grinding, calcining.
In a preferred embodiment of the present invention, in described step (1), the mass ratio that adds of described ammoniacal liquor, deionized water, surface-modifying agent, propyl alcohol and tetraethoxy is 2 ~ 3:1 ~ 1.5:0.1 ~ 0.5:500 ~ 600:2 ~ 3; Described surface-modifying agent is non-ionic surface properties-correcting agent.
In a preferred embodiment of the present invention, in described step (1), the drop rate of described tetraethoxy is 2 ~ 5/s.
In a preferred embodiment of the present invention, in described step (1), described calcining temperature is 500 DEG C, and calcination time is 1.2 ~ 1.5h, and the particle diameter of described nanometer silicon dioxide particle is 30 ~ 50nm.
In a preferred embodiment of the present invention, in described step (2), described nano silicon, polyvinylpyrrolidone, the mass ratio of six water cerous nitrates and alkaline matter is 100:0.1:100:1.
In a preferred embodiment of the present invention, described alkaline matter is ammoniacal liquor, vulkacit H or urea.
The invention has the beneficial effects as follows: the polishing of a kind of optical quartz glass of the present invention is easy by the preparation method of nano combined abrasive material, easy realization, it take nano silicon as core, at its coated with uniform cerium oxide, effectively reduce the size of abrasive material, improve dispersed homogeneous degree and the surfaceness of abrasive material simultaneously, use compounded abrasive of the present invention significantly can improve the polished surface performance of silica glass, improve the use properties of silica glass.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
The nano combined abrasive material of a kind of optical quartz glass polishing, being in particular nano combined abrasive material is the nano combined abrasive material of cerium oxide coated silica, and its preparation method comprises the steps:
(1) nano silicon is prepared: the reaction vessel of band electromagnetism agitating function is placed in 28 ~ 30 DEG C of thermostat water baths, then 20g ammoniacal liquor, 10g deionized water, 0.1g non-ionic surface properties-correcting agent and 500g propyl alcohol is added wherein, after stirring and evenly mixing, 20g tetraethoxy is slowly added again with the drop rate of 2 ~ 5/s, after dropwising, constant temperature stirs 5 ~ 6h and makes it reaction and then still aging 18 ~ 20h; After centrifugation, by solid materials wet lapping 1 ~ 2h, at 500 DEG C, calcine 1.2h, carrying out dry grinding 1 ~ 2h, obtain the silica dioxide granule that median size is 30 ~ 50nm;
(2) the nano combined abrasive material of cerium oxide coated silica is prepared: get the nanometer silicon dioxide particle obtained in 100g step (1), add 30ml deionized water and 0.1g polyvinylpyrrolidone, be heated to 80 DEG C and stir, add 100g six water cerous nitrate and 1g ammoniacal liquor again, stirring reaction 3 ~ 4h, then obtains through centrifugation, priority 2 deionized waters and 1 washing with acetone, 80 DEG C of dryings, grinding 2h, 500 DEG C of calcining 2h the nano combined abrasive material that median size is 130 ~ 160nm.
Embodiment 2
The nano combined abrasive material of a kind of optical quartz glass polishing, being in particular nano combined abrasive material is the nano combined abrasive material of cerium oxide coated silica, and its preparation method comprises the steps:
(1) nano silicon is prepared: the reaction vessel of band electromagnetism agitating function is placed in 28 ~ 30 DEG C of thermostat water baths, then 30g ammoniacal liquor, 15g deionized water, 0.5g non-ionic surface properties-correcting agent and 600g propyl alcohol is added wherein, after stirring and evenly mixing, 30g tetraethoxy is slowly added again with the drop rate of 2 ~ 5/s, after dropwising, constant temperature stirs 5 ~ 6h and makes it reaction and then still aging 18 ~ 20h; After centrifugation, by solid materials wet lapping 1 ~ 2h, at 500 DEG C, calcine 1.5h, carrying out dry grinding 1 ~ 2h, obtain the silica dioxide granule that median size is 30 ~ 50nm;
(2) the nano combined abrasive material of cerium oxide coated silica is prepared: get the nanometer silicon dioxide particle obtained in 200g step (1), add 50ml deionized water and 0.2g polyvinylpyrrolidone, be heated to 100 DEG C and stir, add 200g six water cerous nitrate and 2g vulkacit H again, stirring reaction 3 ~ 4h, then obtains through centrifugation, priority 2 deionized waters and 1 washing with acetone, 80 DEG C of dryings, grinding 2h, 500 DEG C of calcining 3h the nano combined abrasive material that median size is 130 ~ 160nm.
After utilizing the obtained nano combined abrasive material of cerium oxide coated silica of aforesaid method to carry out chemically machinery polished silica glass, the polished surface of the silica glass obtained is more smooth than the polished surface under the same terms, its surfaceness reduces 0.52nm, improves the use properties using glass.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. an optical quartz glass polishing preparation method for nano combined abrasive material, is characterized in that, described nano combined abrasive material is the nano combined abrasive material of cerium oxide coated silica, and described preparation method comprises the steps:
(1) nano silicon is prepared: the reaction vessel of band electromagnetism agitating function is placed in 28 ~ 30 DEG C of thermostat water baths, then ammoniacal liquor, deionized water, surface-modifying agent and propyl alcohol is added wherein, after stirring and evenly mixing, slowly add tetraethoxy again, then after constant temperature stirs 5 ~ 6h, still aging 18 ~ 20h; After centrifugation, solid materials wet lapping, calcining, grinding, obtain nanometer silicon dioxide particle;
(2) the nano combined abrasive material of cerium oxide coated silica is prepared: get the nanometer silicon dioxide particle obtained in a certain amount of step (1), add deionized water and polyvinylpyrrolidone, six water cerous nitrate and alkaline matters are added after heated and stirred, stirring reaction 3 ~ 4h, then obtains described nano combined abrasive material through centrifugation, washing, drying, grinding, calcining.
2. the optical quartz glass polishing according to claim 1 preparation method of nano combined abrasive material, it is characterized in that, in described step (1), the mass ratio that adds of described ammoniacal liquor, deionized water, surface-modifying agent, propyl alcohol and tetraethoxy is 2 ~ 3:1 ~ 1.5:0.1 ~ 0.5:500 ~ 600:2 ~ 3; Described surface-modifying agent is non-ionic surface properties-correcting agent.
3. the optical quartz glass polishing preparation method of nano combined abrasive material according to claim 1, is characterized in that, in described step (1), the drop rate of described tetraethoxy is 2 ~ 5/s.
4. the optical quartz glass polishing according to claim 1 preparation method of nano combined abrasive material, it is characterized in that, in described step (1), described calcining temperature is 500 DEG C, calcination time is 1.2 ~ 1.5h, and the particle diameter of described nanometer silicon dioxide particle is 30 ~ 50nm.
5. the optical quartz glass polishing according to claim 1 preparation method of nano combined abrasive material, it is characterized in that, in described step (2), described nano silicon, polyvinylpyrrolidone, the mass ratio of six water cerous nitrates and alkaline matter is 100:0.1:100:1.
6. the optical quartz glass polishing preparation method of nano combined abrasive material according to claim 5, is characterized in that, described alkaline matter is ammoniacal liquor, vulkacit H or urea.
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Cited By (4)
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|---|---|---|---|---|
| CN105733507A (en) * | 2016-03-11 | 2016-07-06 | 江南大学 | Preparation method of shell-core coated cerium oxide-silicon oxide composite abrasive grains |
| CN107488439A (en) * | 2017-09-30 | 2017-12-19 | 南京航空航天大学 | A kind of grinding and polishing glass abrasive compound and preparation method thereof |
| CN115873559A (en) * | 2022-12-28 | 2023-03-31 | 河南创研新材料科技有限公司 | Silicon dioxide-silicon carbide gel composite microsphere and preparation method thereof |
| US11661539B2 (en) * | 2018-10-31 | 2023-05-30 | Shin-Etsu Chemical Co., Ltd. | Method for manufacturing polishing particles and method for polishing synthetic quartz glass substrate |
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| CN101302404A (en) * | 2008-07-01 | 2008-11-12 | 上海大学 | Preparation of nano-cerium oxide composite abrasive grain polishing solution |
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| CN103146197A (en) * | 2013-03-11 | 2013-06-12 | 深圳大学 | Method for preparing lyophobic heat conduction material with micro-nano core-shell structure |
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- 2015-12-04 CN CN201510878342.8A patent/CN105331332A/en active Pending
Patent Citations (6)
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| CN101302404A (en) * | 2008-07-01 | 2008-11-12 | 上海大学 | Preparation of nano-cerium oxide composite abrasive grain polishing solution |
| CN101475792A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation of coating type cerium oxide / silicon oxide compound abrasive |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733507A (en) * | 2016-03-11 | 2016-07-06 | 江南大学 | Preparation method of shell-core coated cerium oxide-silicon oxide composite abrasive grains |
| CN105733507B (en) * | 2016-03-11 | 2018-08-10 | 江南大学 | A kind of preparation method of shell core cladded type cerium oxide-silicon oxide Compostie abrasive particles |
| CN107488439A (en) * | 2017-09-30 | 2017-12-19 | 南京航空航天大学 | A kind of grinding and polishing glass abrasive compound and preparation method thereof |
| US11661539B2 (en) * | 2018-10-31 | 2023-05-30 | Shin-Etsu Chemical Co., Ltd. | Method for manufacturing polishing particles and method for polishing synthetic quartz glass substrate |
| CN115873559A (en) * | 2022-12-28 | 2023-03-31 | 河南创研新材料科技有限公司 | Silicon dioxide-silicon carbide gel composite microsphere and preparation method thereof |
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Application publication date: 20160217 |