CN111233308A - Opaque quartz glass ingot and preparation method thereof - Google Patents
Opaque quartz glass ingot and preparation method thereof Download PDFInfo
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- CN111233308A CN111233308A CN202010187803.8A CN202010187803A CN111233308A CN 111233308 A CN111233308 A CN 111233308A CN 202010187803 A CN202010187803 A CN 202010187803A CN 111233308 A CN111233308 A CN 111233308A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/02—Pure silica glass, e.g. pure fused quartz
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Abstract
The invention discloses a preparation method of an opaque quartz glass ingot, which comprises the following steps: s1, mixing silicon dioxide micro powder with high-purity water, stirring to prepare pasty slurry, and carrying out wet magnetic separation in the stirring process to remove magnetic impurities in the micro powder; s2, drying the obtained slurry, and crushing the dried slurry into granular materials; s3, adding the obtained granular material into a crucible for sintering, wherein the sintering temperature is 1200-1600 ℃, and the sintering time is 1-4 hours; s4, sequentially crushing, screening, magnetic separation, acid washing, cleaning and drying the obtained sintered blocks to prepare high-purity quartz sand with the specification of 100 plus 180 meshes; s5, continuously melting and depositing the prepared high-purity quartz sand by oxyhydrogen flame to prepare an opaque quartz glass ingot. The invention also discloses an opaque quartz glass ingot prepared by the method. The preparation method of the opaque quartz glass ingot overcomes the defect that the pores are manufactured by adding additives in the prior art.
Description
Technical Field
The invention relates to the technical field of quartz glass, in particular to an opaque quartz glass ingot and a preparation method thereof.
Background
The opaque quartz glass is prepared by taking high-purity natural quartz sand or fused quartz sand as a raw material and fusing at high temperature. During melting, a large number of micro bubbles are formed in quartz, so that a glass and gas two-phase system exists in the quartz, wherein the refractive index of a bubble phase is 1, the refractive index of a quartz glass phase is 1.55, visible light and infrared light are refracted, reflected and scattered for many times in the two-phase system to form a scattering effect, the transmittance of the visible light and the infrared light is reduced to be below 2% from 95% of the original transmittance when the visible light and the infrared light are transparent, most of 2 kinds of energy are absorbed, and therefore, the opaque quartz glass has excellent thermal fracture resistance, and is widely used as a heat insulation material of semiconductors and photovoltaics.
The existing opaque quartz glass preparation methods mainly comprise two methods: one is to add organic or inorganic additives to the sand, which can generate micro-bubbles during the melting process. However, the additives are not easy to be fully mixed with the quartz sand, on one hand, the organic additives cause the surface of the quartz sand to be sticky and agglomerated, and the self-flowing blanking is not easy to be utilized in the process of preparing the opaque quartz glass, so that the problems of uneven size of bubbles and the like are generated; on the other hand, the addition of additives affects the purity of the quartz glass, resulting in quality problems of the quartz glass during use. The other method is that no additive is added into the quartz sand, but a sintering process is adopted, and sintering is carried out below the melting temperature of the quartz. However, when the pores are closed by sintering, the content density of the pores becomes low, which causes a problem of lowering the infrared light shielding property, and the sintering causes a problem of generating unevenness of bubbles.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of an opaque quartz glass ingot, which overcomes the defects that in the prior art, an additive is required to be added to manufacture pores, and micro powder cannot be directly fused into the opaque quartz glass ingot due to small density and large volume and poor flowability.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a preparation method of an opaque quartz glass ingot, which comprises the following steps:
s1, mixing silicon dioxide micro powder with high-purity water, stirring to prepare pasty slurry, and carrying out wet magnetic separation in the stirring process to remove magnetic impurities in the micro powder; the resistivity of the high-purity water is more than 18M omega cm;
s2, drying the slurry obtained in the step S1, and crushing the dried slurry into granular materials;
s3, adding the granular material obtained in the step S2 into a crucible for sintering, wherein the sintering temperature is 1200-1600 ℃, and the sintering time is 1-4 hours;
s4, sequentially crushing, screening, magnetic separation, acid washing, cleaning and drying the sintered blocks obtained in the step S3 to prepare high-purity quartz sand with the specification of 100-180 meshes;
s5, continuously melting and depositing the high-purity quartz sand prepared in the step S4 through oxyhydrogen flame to prepare an opaque quartz glass ingot.
Further, in step S1, the specific surface area of the fine silica powder is 50 to 200m2In the range of/g, SiO2The content is more than or equal to 99.999 percent.
Further, in step S1, the fine silica powder is made of SiCl4Produced by pyrolysis.
Further, in step S1, the mass ratio of the fine silica powder to the high purity water is 1:2 to 2: 1.
Further, in step S2, the drying temperature is 100-120 ℃, and the drying time is 8-10 hours.
Further, in step S4, the acid solution used for acid cleaning is selected from one or more of hydrofluoric acid, hydrochloric acid, sulfuric acid, oxalic acid, and nitric acid; the concentration of the acid liquor is 5-30%, the pickling temperature is 25-90 ℃, and the pickling time is 1-100 hours.
Further, in step S4, the drying temperature is 100-120 ℃, and the drying time is 8-10 hours.
Further, in step S4,SiO in the high-purity quartz sand2The content is more than or equal to 99.9999 percent.
Further, in step S5, the feeding speed in the quartz sand melting process is 1-5 kg/h.
In a second aspect of the invention, there is provided an opaque quartz glass ingot produced by the method of the first aspect.
Compared with the prior art, the invention has the beneficial effects that:
1. in the prior art, additives are required to be added when preparing the opaque quartz glass ingot, which brings impurities and leads to the purity reduction of the opaque quartz glass. The raw material of the silicon dioxide micropowder selected by the invention has the characteristics of large specific surface area, small apparent density and the like, and the interior of the silicon dioxide micropowder contains a large number of pores. Thereby overcoming the defect that the prior art needs to add additives to manufacture pores.
2. The invention prepares the micro powder into slurry, dries the slurry and sinters the slurry, increases the apparent density of the micro powder, and solves the defect that the micro powder can not be directly fused into opaque quartz glass ingots due to small density and large volume and poor fluidity.
3. The method provided by the invention has the advantages that the sintered blocks are crushed and then purified, the purity of the opaque quartz glass ingot is improved, and the defect that the quality of a finished product is affected by the purity is reduced. Because of the purified SiO2The content is more than or equal to 99.9999 percent, so the opaque quartz glass ingot can be applied to the semiconductor industry with high purity requirement.
4. The invention solves the problem of SiCl4The utilization rate of the silicon dioxide micro powder generated by pyrolysis is low, which is beneficial to environmental protection and has strong operability.
Drawings
FIG. 1 is a photograph of an opaque quartz glass ingot produced by the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used therein are commercially available without otherwise specified.
Example 1
First, SiCl is provided420kg of pyrogenically produced fine silicon dioxide powder having a specific surface area of 50m2/g，SiO2The content is 99.9992%. The silicon dioxide micro powder and high-purity water are prepared according to the proportion of 1:1, are continuously stirred to prepare pasty slurry, and are subjected to wet magnetic separation in the stirring process. And then, heating the slurry subjected to magnetic separation to 105 ℃ for drying for 8 hours, crushing the slurry into granular materials after drying, adding the granular materials into a graphite crucible, and sintering the granular materials in an electric heating furnace at 1300 ℃ for 4 hours. And then, crushing, screening, magnetically separating, pickling, cleaning and drying the sintered blocks, wherein the pickling adopts hydrofluoric acid with the concentration of 25%, the pickling temperature is 25 ℃, the pickling time is 96h, and the sintered blocks are dried for 8h after pickling to prepare the high-purity quartz sand with the specification of 100-180 meshes. And finally, continuously melting and depositing the prepared high-purity quartz sand by oxyhydrogen flame at a blanking speed of 1kg/h to prepare an opaque quartz glass ingot.
Example 2
First, SiCl is provided420kg of silica micropowder produced by pyrolysis and with a specific surface area of 80m2/g，SiO2The content is 99.9995%. Firstly, preparing silicon dioxide micro powder and high-purity water according to the ratio of 1:2, continuously stirring to prepare pasty slurry, and carrying out wet magnetic separation in the stirring process. And then, heating the slurry subjected to magnetic separation to 105 ℃ for drying for 10 hours, crushing the slurry into granular materials after drying, adding the granular materials into a graphite crucible, and putting the graphite crucible into an electric heating furnace for sintering. Sintering at 1600 deg.CThe knot time was 3 hours. And then, crushing, screening, magnetically separating, pickling, cleaning and drying the sintered blocks, wherein the pickling adopts hydrochloric acid with the concentration of 5%, the pickling temperature is 65 ℃, and the pickling time is 24 hours. Drying for 8h after acid washing to prepare the high-purity quartz sand with the specification of 100-180 meshes. And finally, continuously melting and depositing the prepared high-purity quartz sand by oxyhydrogen flame at a blanking speed of 3kg/h to prepare the opaque quartz glass ingot.
Example 3
First, SiCl is provided420kg of silica micropowder produced by pyrolysis and having a specific surface area of 150m2/g，SiO2The content is 99.9998%, the silicon dioxide micro powder and high-purity water are prepared according to the proportion of 1:2, the mixture is continuously stirred to prepare pasty slurry, and wet magnetic separation is carried out in the stirring process. And then, heating the slurry subjected to magnetic separation to 110 ℃ for drying for 10 hours, crushing the slurry into granular materials after drying, adding the granular materials into a graphite crucible, and putting the graphite crucible into an electric heating furnace for sintering. The sintering temperature is 1500 ℃, and the sintering time is 2 hours. And then, crushing, screening, magnetically separating, pickling, cleaning and drying the sintered blocks, wherein the pickling adopts mixed acid of hydrofluoric acid and oxalic acid, the concentration is 10%, the pickling temperature is 80 ℃, and the pickling time is 8 hours. Drying for 8h after acid washing to prepare the high-purity quartz sand with the specification of 100-180 meshes. And finally, continuously melting and depositing the prepared high-purity quartz sand by oxyhydrogen flame at a blanking speed of 5kg/h to prepare an opaque quartz glass ingot.
Referring to fig. 1, the opaque quartz glass ingot prepared by the present invention is milky opaque and has high purity.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A method for preparing an opaque quartz glass ingot, comprising the steps of:
s1, mixing silicon dioxide micro powder with high-purity water, stirring to prepare pasty slurry, and carrying out wet magnetic separation in the stirring process to remove magnetic impurities in the micro powder; the resistivity of the high-purity water is more than 18M omega cm;
s2, drying the slurry obtained in the step S1, and crushing the dried slurry into granular materials;
s3, adding the granular material obtained in the step S2 into a crucible for sintering, wherein the sintering temperature is 1200-1600 ℃, and the sintering time is 1-4 hours;
s4, sequentially crushing, screening, magnetic separation, acid washing, cleaning and drying the sintered blocks obtained in the step S3 to prepare high-purity quartz sand with the specification of 100-180 meshes;
s5, continuously melting and depositing the high-purity quartz sand prepared in the step S4 through oxyhydrogen flame to prepare an opaque quartz glass ingot.
2. The method of claim 1, wherein in step S1, the silica micropowder has a specific surface area of 50 to 200m2In the range of/g, SiO2The content is more than or equal to 99.999 percent.
3. The method of claim 2, wherein in step S1, the fine silica powder is SiCl4Produced by pyrolysis.
4. The method of claim 1, wherein in step S1, the mass ratio of the fine silica powder to the high purity water is 1:2 to 2: 1.
5. The method as claimed in claim 1, wherein in step S2, the baking temperature is 100-120 ℃ and the baking time is 8-10 hours.
6. The method of claim 1, wherein in step S4, the acid solution used for pickling is selected from one or more of hydrofluoric acid, hydrochloric acid, sulfuric acid, oxalic acid, and nitric acid; the concentration of the acid liquor is 5-30%, the pickling temperature is 25-90 ℃, and the pickling time is 1-100 hours.
7. The method according to claim 1, wherein in step S4, the baking temperature is 100-120 ℃ and the baking time is 8-10 hours.
8. The method of claim 1, wherein in step S4, SiO in the high purity silica sand is2The content is more than or equal to 99.9999 percent.
9. The method of claim 1, wherein in step S5, the feeding speed of the fused silica sand is 1-5 kg/h.
10. An opaque quartz glass ingot produced according to the method of any one of claims 1 to 9.
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| CN202010187803.8A CN111233308A (en) | 2020-03-17 | 2020-03-17 | Opaque quartz glass ingot and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956102A (en) * | 2022-05-09 | 2022-08-30 | 重庆乾吉机电设备有限公司 | Process for preparing high-purity 99.9% quartz sand |
| TWI795053B (en) * | 2021-01-30 | 2023-03-01 | 日商東曹石英有限公司 | Opaque quartz glass and manufacturing method thereof |
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| JP2004131380A (en) * | 2002-09-20 | 2004-04-30 | Heraeus Quarzglas Gmbh & Co Kg | Process for manufacturing opaque quartz glass composite, composite obtained thereby, and its use |
| CN101348324A (en) * | 2008-08-27 | 2009-01-21 | 常熟华融太阳能新型材料有限公司 | Non-transparent quartz crucible for polysilicon crystallization and manufacturing method thereof |
| CN102167500A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
| JP2014088286A (en) * | 2012-10-30 | 2014-05-15 | Tosoh Corp | Opaque quartz glass and production method thereof |
| CN107417071A (en) * | 2016-05-24 | 2017-12-01 | 贺利氏石英玻璃股份有限两合公司 | The method for manufacturing the opaque silica glass containing hole |
| CN107628625A (en) * | 2017-11-09 | 2018-01-26 | 新沂市宏润石英硅微粉有限公司 | A kind of preparation method of glass sand |
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2020
- 2020-03-17 CN CN202010187803.8A patent/CN111233308A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004131380A (en) * | 2002-09-20 | 2004-04-30 | Heraeus Quarzglas Gmbh & Co Kg | Process for manufacturing opaque quartz glass composite, composite obtained thereby, and its use |
| CN101348324A (en) * | 2008-08-27 | 2009-01-21 | 常熟华融太阳能新型材料有限公司 | Non-transparent quartz crucible for polysilicon crystallization and manufacturing method thereof |
| CN102167500A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
| JP2014088286A (en) * | 2012-10-30 | 2014-05-15 | Tosoh Corp | Opaque quartz glass and production method thereof |
| CN107417071A (en) * | 2016-05-24 | 2017-12-01 | 贺利氏石英玻璃股份有限两合公司 | The method for manufacturing the opaque silica glass containing hole |
| CN107628625A (en) * | 2017-11-09 | 2018-01-26 | 新沂市宏润石英硅微粉有限公司 | A kind of preparation method of glass sand |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI795053B (en) * | 2021-01-30 | 2023-03-01 | 日商東曹石英有限公司 | Opaque quartz glass and manufacturing method thereof |
| CN114956102A (en) * | 2022-05-09 | 2022-08-30 | 重庆乾吉机电设备有限公司 | Process for preparing high-purity 99.9% quartz sand |
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Application publication date: 20200605 |