CN111320177B - Method for removing hydroxyl groups in quartz sand powder - Google Patents
Method for removing hydroxyl groups in quartz sand powder Download PDFInfo
- Publication number
- CN111320177B CN111320177B CN202010283523.7A CN202010283523A CN111320177B CN 111320177 B CN111320177 B CN 111320177B CN 202010283523 A CN202010283523 A CN 202010283523A CN 111320177 B CN111320177 B CN 111320177B
- Authority
- CN
- China
- Prior art keywords
- quartz
- purity
- quartz sand
- sand powder
- temperature
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to a method for removing hydroxyl in quartz sand powder, which comprises the steps of firstly, feeding high-purity quartz materials into a high-temperature vacuum furnace, heating to 1000-1050 ℃, and introducing H 2 Or H 2 The mixed gas of nitrogen and/or helium is used as reducing gas to carry out high-temperature reduction treatment for at least 2 hours, then a vacuum system is started to raise the temperature to 1470-1500 ℃ and the vacuum degree is 6.0x10 ‑6 ～7.0×10 ‑ 6 pa, carrying out vacuum degassing treatment for 3-4 hours to obtain the high-purity low-hydroxyl quartz sand powder material. The hydroxyl content in the quartz sand powder prepared by the method is lower than 3ppm.
Description
Technical Field
The invention relates to a method for removing hydroxyl groups in quartz sand powder, belonging to the non-metal ore deep processing industry.
Background
The transparent quartz glass and its product are prepared with high purity quartz sand powder as material and through smelting in high temperature electric smelting furnace with hydrogen or inert gas or hydrogen+nitrogen or hydrogen+nitrogen+inert gas as protecting gas to obtain glass liquid, and through eliminating the coloring of quartz glass, raising protecting effect and product quality, mechanical forming, cutting, cooling, cleaning, drying and dehydroxylation.
The transparent quartz glass tube for semiconductors JC/T597-2011 specifies: the hydroxyl group content should be 220×10 or less -6 The method comprises the steps of carrying out a first treatment on the surface of the The transparent quartz glass rod for semiconductors JC/T2064-2011 specifies: the hydroxyl group content should be 220×10 or less -6 The method comprises the steps of carrying out a first treatment on the surface of the Transparent quartz glass tube for electric light source JC/T598-2007 specifies: a) High-pressure mercury lamp tube: the hydroxyl group content is 10 x 10 or less -6 The method comprises the steps of carrying out a first treatment on the surface of the b) The hydroxyl content of the metal halide lamp tube is less than or equal to 3 multiplied by 10 -6 The method comprises the steps of carrying out a first treatment on the surface of the c) Quartz glass tube for halogen tungsten lamp tube and other lamps: agreed by both the supply and demand parties. The hydroxyl group source of quartz glass articles consists essentially of two parts: one is hydroxyl group contained in quartz sand, and the other is gas H protected in high temperature melting process 2 With quartz glass SiO 2 Hydroxyl groups generated by chemical reactions take place, with the former being higher in proportion. The hydroxyl groups of the quartz sand are mainly from structural water in the quartz crystal structure, namely (OH) - 、H + 、(H 3 O) + The ionic form of "water" being present in the crystal lattice of the quartz crystal as (OH) - Most often, the removal is quite difficult due to the strong bond strength associated with other particles in the crystal.
In the process of melting quartz glass, residual gas and liquid inclusion and structural water in the raw material quartz sand powder slowly form tiny bubbles in high-temperature glass liquid and gradually increase, and finally the tiny bubbles escape from the glass liquid. Due to the accompanying SiO in the melting process 2 The melting time and the melting temperature need to be controlled to a certain extent to reduce the loss of raw materials. In addition, the glass liquid still has a certain viscosity at high temperature, and some tiny single bubbles are difficult to overcome the viscosity resistance of the glass liquid and become large bubbles to escape, so that the bubbles remain or are dissolved in the transparent glass liquid in the later period of homogenization, and finally exist in the quartz glass product in the form of micro bubbles or hydroxyl groups. These hydroxyl groups are usually removed by high temperature and high vacuum, but the high temperature vacuum treatment has limited dehydroxylation effect, which severely limits the quality of high quality quartz glass and products. In order to solve the problem of hydroxyl groups in quartz glass raw material quartz sand and improve the qualification rate of quartz glass and products thereof, the hydroxyl groups in the raw material sand should be removed to the greatest extent while the purity of the raw material is ensured. For this reason, we have developed a method for removing hydroxyl groups from silica sand powder, which produces silica sand powder having hydroxyl groups of 1 to 3ppm.
Disclosure of Invention
The invention aims to provide a method for removing hydroxyl groups in quartz sand serving as a quartz glass raw material, wherein the quartz sand with the hydroxyl groups removed is used as a high-quality raw material of quartz glass.
The invention solves the technical problems by adopting the following scheme:
a method for removing hydroxyl groups in quartz sand powder, comprising the following steps:
(1) Feeding the high-purity quartz material into a high-temperature vacuum furnace, heating to 1000-1050 ℃, and introducing H 2 Or H 2 The mixed gas of the nitrogen and one or two of the helium is used as a reducing gas to carry out high-temperature reduction treatment, and the high-temperature reduction treatment time is not less than 2 hours;
(2) Starting the vacuum system, raising the temperature to 1470-1500 deg.c and vacuum degree of 6.0 x 10 -6 ～7.0×10 -6 pa, carrying out vacuum degassing treatment for 3-4 hours to obtain the high-purity low-hydroxyl quartz sand powder material.
Preferably, the hydroxyl content of the high-purity low-hydroxyl quartz sand powder material obtained in the step (2) is not more than 3ppm.
Preferably, the high-purity quartz material in the step (1) is prepared from igneous quartz of igneous rock, and the preparation process comprises the following steps: selecting SiO 2 The percentage (m/m) is larger than or equal to 99.90 percent of the pyrogenic vein quartz, and the high-purity quartz sand is obtained through mineral separation, crushing, acid washing, calcining, water quenching, sand making, magnetic separation, classification, flotation, acid washing, pure water washing and drying; and then chloridizing the obtained high-purity quartz sand at the high temperature of 1000-1100 ℃ for 1-1.5 h to obtain the high-purity quartz sand.
Preferably, the metal and nonmetal impurities in the high-purity quartz material in the step (1) are less than or equal to 20ppm.
Preferably, the reducing gas in the step (1) is introduced under the condition of micro negative pressure, and the micro negative pressure environment is vacuum degree of 0.001-0.01 Mpa.
The invention also aims to provide a method for melting the low-hydroxyl quartz glass device, which comprises the steps of preparing a high-purity low-hydroxyl quartz sand powder material by adopting the method, and melting the required quartz glass device at 1800-2100 ℃ by taking nitrogen as a protective gas.
Alpha-quartz (low temperature quartz) is converted to beta-quartz (high temperature quartz) at 573 ℃, and beta-quartz is stable at 573-870 ℃ under normal pressure. Beta-quartz is converted to tridymite, which is SiO, at temperatures above 870 DEG C 2 A stable phase at 870-1470 ℃; tridymite is converted to high temperature cristobalite at 1470 ℃, which is a stable equiaxed crystal modification at 1470-1728 ℃ under normal pressure. The transformation of beta-quartz into tridymite is a reconstruction phase transition, and when the quartz material is subjected to high-temperature reconstruction phase transition: the Si-O bond is broken and then rebuilt, namely the crystal lattice of the quartz crystal is opened when the Si-O bond is broken, so that the hydroxyl in the original crystal lattice can be fully exposed, and the Si-O bond in the crystal is in a transition state before rebuilt. By selecting a proper temperature range for hydrogen reduction, the hydrogen can permeate into OH exposed from the reduction lattice in the quartz material - And the generated water vapor volatilizes, thereby achieving the purpose of removing hydroxyl. For the hydroxyl groups which are not removed and the residual reducing hydrogen, the residual reducing hydrogen can be removed under the high vacuum environment of 1470-1500 ℃. The final product is a low hydroxyl or hydroxyl free quartz material.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrative of the present invention, but the contents of the present invention are not limited to the following examples only.
The hydroxyl content in the invention is checked by adopting the method in GB/T12442-2019; siO (SiO) 2 Purity was checked according to GB/T3284-2015 method; the impurity element was examined according to the method of GB/T32650-2016.
Example 1
SiO in Henan Xinyang place 2 Pulse quartz with purity of 99.98% is used as the raw materialThe high-purity quartz sand is obtained by the steps of material dressing, crushing, acid washing, calcining, water quenching, sand making, magnetic separation, grading, flotation, acid washing, pure water washing and drying; and then chloridizing the obtained high-purity quartz sand at the high temperature of 1000 ℃ for 1h to obtain the high-purity quartz sand powder of the initial raw material of 70-120 meshes. Measuring the hydroxyl group content of the initial raw material to 400ppm, siO 2 The purity is 99.98%.
The initial raw materials are treated according to the following steps:
1. placing the above initial raw materials into a 1050 deg.C vertical high temperature vacuum furnace, calcining for 2 hr under slightly negative pressure (vacuum gauge is 0.001 Mpa), and introducing 5%H from bottom of the furnace 2 Carrying out high-temperature reduction treatment for 2 hours by using a mixed gas (V/V) of +95% He, stopping ventilation, and preparing for vacuum degassing;
2. starting vacuum system, heating to 1470deg.C, and vacuum degree of 6.0-7.0X10 -6 Removing mixed gas under pa condition for 4 hours, and then delivering the obtained material into a storage bin of a melting quartz continuous melting furnace for standby;
and 3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing furnace, melting quartz glass liquid at 1800-2000 ℃, and drawing a transparent quartz glass tube for an electric light source by using high-purity nitrogen of 4N or more as a protective gas according to a conventional process method. Hydroxyl group content of the finished transparent quartz glass tube product 1ppm, siO 2 The purity is 99.999%.
Example 2
SiO in certain place of yellow oka of Hubei province 2 The pulse quartz with the purity of 99.96 percent is used as a raw material, and the high-purity quartz sand is obtained through mineral separation, crushing, pickling, calcining, water quenching, sand making, magnetic separation, classification, flotation, pickling, pure water washing and drying; and then chloridizing the obtained high-purity quartz sand at 1050 ℃ for 1.5 hours to obtain the high-purity quartz sand powder of 40-70 meshes as an initial raw material. Measuring 600ppm of hydroxyl group and SiO in the initial raw material 2 The purity was 99.96%.
The initial raw materials are treated according to the following steps:
1. initial after the high temperature chlorinationThe raw materials are put into a vertical high-temperature vacuum furnace made of tungsten metal at 1050 ℃ and calcined for 2 hours under a micro negative pressure bar (vacuum gauge is shown as 0.003 Mpa), and then 10% H is introduced from the bottom of the furnace at the temperature 2 +90％N 2 The mixed gas (V/V) high-temperature reduction treatment time is 3 hours, the feeding of the hydrogen-containing mixed gas is stopped, and the preparation for vacuum degassing is started;
2. starting vacuum system, heating to 1500deg.C, and vacuum degree of 6.0-7.0X10 -6 Removing hydrogen-containing mixed gas under pa condition for 3 hours, and then feeding the material into a storage bin of a melting quartz continuous melting furnace for standby;
and 3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing rod, melting quartz glass liquid at 1800-2100 ℃, and drawing the transparent quartz glass rod for the semiconductor by using high-purity nitrogen of 4N or more as a protective gas according to a conventional process method. The hydroxyl group content of the finished transparent quartz glass tube product is 3ppm, siO 2 ％：99.998％。
Example 3
In Shanxi Han province of SiO 2 Purity: 99.97% of vein quartz is used as a raw material, and the high-purity quartz sand is obtained through mineral separation, crushing, pickling, calcining, water quenching, sand making, magnetic separation, classification, flotation, pickling, pure water washing and drying; and then chloridizing the obtained high-purity quartz sand at 1100 ℃ for 1h to obtain the high-purity quartz sand powder of the initial raw material of 70-120 meshes. Measuring the hydroxyl group content of 500ppm, siO in the initial raw material 2 The purity was 99.97%.
The initial raw materials are treated according to the following steps:
1. placing the above high-temperature chlorinated initial raw material into a 1000 deg.C vertical high-temperature vacuum furnace made of tungsten metal, calcining for 2 hr under micro-negative pressure (vacuum gauge is shown as 0.006 Mpa), and introducing H from bottom of furnace at this temperature 2 High-temperature reduction treatment is carried out for 2 hours, gas is stopped from being introduced, and vacuum degassing is started to be prepared;
2. starting vacuum system, heating to 1480deg.C, and vacuum degree of 6.0-7.0X10 -6 Removing hydrogen-containing gas under pa condition for 3.5 hr, and feeding the material into smelting processThe storage bin of the quartz continuous melting furnace is reserved for standby;
and 3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing furnace, melting quartz glass liquid at 1800-2100 ℃, and drawing a transparent quartz glass tube for a semiconductor by using high-purity nitrogen of 4N or more as a protective gas according to a conventional process method. The hydroxyl group content of the finished transparent quartz glass tube product is 2ppm and SiO 2 ％：99.998％。
Example 4
Certain place of Hunan Yueyang SiO 2 Purity: 99.97% of vein quartz is used as a raw material, and the high-purity quartz sand is obtained through mineral separation, crushing, pickling, calcining, water quenching, sand making, magnetic separation, classification, flotation, pickling, pure water washing and drying; and then chloridizing the obtained high-purity quartz sand at 1100 ℃ for 1h to obtain the high-purity quartz sand powder of the initial raw material of 70-120 meshes. Measuring 550ppm of hydroxyl groups and SiO in the initial raw material 2 The purity was 99.97%.
The initial raw materials are treated according to the following steps:
1. placing the above high-temperature chlorinated initial raw material into a 1000 deg.C vertical high-temperature vacuum furnace made of tungsten metal, calcining for 2 hr under micro-negative pressure (vacuum gauge is shown as 0.006 Mpa), and introducing 10% H from bottom of the furnace at this temperature 2 +40％He+40％N 2 (V/V/V) high-temperature reduction treatment is carried out for 2 hours, gas introduction is stopped, and vacuum degassing is started to be prepared;
2. starting vacuum system, heating to 1480deg.C, and vacuum degree of 6.0-7.0X10 -6 Removing residual gas under pa condition for 3.5 hours, and then feeding the materials into a storage bin of the melting quartz continuous melting furnace for standby;
and 3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing furnace, melting quartz glass liquid at 1800-2100 ℃, and drawing a transparent quartz glass tube for a semiconductor by using high-purity nitrogen of 4N or more as a protective gas according to a conventional process method. The hydroxyl group content of the finished transparent quartz glass tube product is 2ppm and SiO 2 ％：99.998％。
Example 5
The same initial raw material as in example 1 was used, and the same initial raw material treatment mode and the same melting mode were adopted, except that the reducing gas was 50% H 2 +50％N 2 And (3) a mixed gas.
The final drawn transparent quartz glass tube product had a hydroxyl group content of 2ppm and SiO 2 Purity 99.998%.
Example 6
The same initial raw material, the same initial raw material treatment method and the same melting method as in example 1 were used, except that the composition of the reduced mixed gas was as follows: 30% H 2 +35％He+35％N 2 (V/V/V)。
The final drawn transparent quartz glass tube product had a hydroxyl group content of 2ppm and SiO 2 Purity 99.998%.
Comparative example 1
The same initial raw material, the same initial raw material treatment method, and the same melting method as in example 1 were employed, except that the temperature of the high-temperature reduction treatment was 900 ℃.
The final drawn transparent quartz glass tube product for electric light source has hydroxyl group content of 8ppm and SiO 2 Purity 99.996%.
Comparative example 2
The same initial raw material, the same initial raw material treatment method, and the same melting method as in example 1 were employed, except that the high-temperature reduction treatment temperature was 1100 ℃.
The final drawn transparent quartz glass tube product had a hydroxyl group content of 8ppm and SiO 2 Purity 99.995% with small amounts of SiO detected.
While the invention has been described with respect to the preferred embodiments, it will be understood that the invention is not limited thereto, but is capable of modification and variation without departing from the spirit of the invention, as will be apparent to those skilled in the art.
Claims (6)
1. A method for removing hydroxyl groups in quartz sand powder, which is characterized by comprising the following steps:
(1) Feeding the high-purity quartz material into a high-temperature vacuum furnace, preparing the high-purity quartz material by using gangue quartz of igneous rock, heating to 1000-1050 ℃, and introducing H 2 Or H 2 The mixed gas of nitrogen and/or helium is used as reducing gas to carry out high-temperature reduction treatment for at least 2 hours;
(2) Starting the vacuum system, raising the temperature to 1470-1500 deg.c and vacuum degree of 6.0 x 10 -6 ～7.0×10 -6 pa, carrying out vacuum degassing treatment for 3-4 hours to obtain the high-purity low-hydroxyl quartz sand powder material.
2. The method for removing hydroxyl groups from silica sand powder according to claim 1, wherein the hydroxyl group content of the high-purity low-hydroxyl silica sand powder material obtained in the step (2) is not more than 3ppm.
3. The method for removing hydroxyl groups from quartz sand powder according to claim 1, wherein the preparation process of the high-purity quartz material in the step (1) comprises the following steps: selecting SiO 2 The percentage (m/m) is larger than or equal to 99.90 percent of the pyrogenic vein quartz, and the high-purity quartz sand is obtained through mineral separation, crushing, acid washing, calcining, water quenching, sand making, magnetic separation, classification, flotation, acid washing, pure water washing and drying; and then chloridizing the obtained high-purity quartz sand at the high temperature of 1000-1100 ℃ for 1-1.5 h to obtain the high-purity quartz sand.
4. The method for removing hydroxyl groups from silica sand according to claim 1, wherein the metal and non-metal impurities in the high purity silica sand material in step (1) are less than or equal to 20ppm.
5. The method for removing hydroxyl groups from quartz sand powder according to claim 1, wherein the reducing gas in the step (1) is introduced under a micro negative pressure, and the micro negative pressure environment is a vacuum degree of 0.001-0.01 Mpa.
6. A method for melting a low-hydroxyl quartz glass device, which is characterized in that a high-purity low-hydroxyl quartz sand powder material is prepared by adopting the method of any one of claims 1 to 5, and then a required quartz glass device is melted at 1800-2100 ℃ by taking nitrogen as a protective gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010283523.7A CN111320177B (en) | 2020-04-13 | 2020-04-13 | Method for removing hydroxyl groups in quartz sand powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010283523.7A CN111320177B (en) | 2020-04-13 | 2020-04-13 | Method for removing hydroxyl groups in quartz sand powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111320177A CN111320177A (en) | 2020-06-23 |
| CN111320177B true CN111320177B (en) | 2023-09-15 |
Family
ID=71169902
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010283523.7A Active CN111320177B (en) | 2020-04-13 | 2020-04-13 | Method for removing hydroxyl groups in quartz sand powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111320177B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010317B (en) * | 2020-09-14 | 2022-06-07 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN112624580B (en) * | 2020-12-03 | 2021-12-14 | 东海县奥兰石英科技有限公司 | Method for removing impurities of optical fiber quartz target rod by continuous melting and intermediate frequency furnace integration method |
| CN112479560B (en) * | 2020-12-24 | 2021-12-10 | 连云港福东正佑照明电器有限公司 | Preparation method of radiation-resistant anti-crystallization high-transmittance quartz tube for ultra-high-power light source |
| CN114368757A (en) * | 2022-01-21 | 2022-04-19 | 成都光华科技发展有限公司 | Purification method of high-purity quartz sand |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE30883E (en) * | 1975-08-16 | 1982-03-16 | Heraeus Quarzscmelze GmbH | Method of producing synthetic quartz glass |
| US4650511A (en) * | 1984-06-04 | 1987-03-17 | Shin-Etsu Chemical Co., Ltd. | Method for the preparation of a dehydrated quartz glass material for light transmission |
| JPH0881226A (en) * | 1994-09-16 | 1996-03-26 | Tosoh Corp | Production of high-purity, high heat-resistant quartz glass |
| CN101050054A (en) * | 2007-03-28 | 2007-10-10 | 徐胜利 | Vacuum deshydroxy method for quartz glass cell |
| CN101337767A (en) * | 2008-08-15 | 2009-01-07 | 杜建中 | Purification method in process of production of high-pure quartz sand as raw material of quartz glass |
| CN103613102A (en) * | 2013-12-04 | 2014-03-05 | 南京工业大学东海先进硅基材料研究院 | Process for preparing ultrahigh pure quartz sand through silica raw material |
| CN107140812A (en) * | 2017-06-12 | 2017-09-08 | 江苏太平洋石英股份有限公司 | A kind of production method of low hydroxyl dark red doping quartz ampoule |
| CN109336116A (en) * | 2018-10-31 | 2019-02-15 | 黄冈师范学院 | A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite |
| CN110040942A (en) * | 2018-01-16 | 2019-07-23 | 中天科技集团有限公司 | The preparation method of body of powder deshydroxy processing method and quartz glass |
| CN110182814A (en) * | 2019-04-20 | 2019-08-30 | 黄冈师范学院 | A kind of SiO2The production method of glass sand of the purity greater than 5N |
| CN110862091A (en) * | 2019-12-25 | 2020-03-06 | 苏州纳迪微电子有限公司 | High-purity quartz sand and preparation method and application thereof |
-
2020
- 2020-04-13 CN CN202010283523.7A patent/CN111320177B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE30883E (en) * | 1975-08-16 | 1982-03-16 | Heraeus Quarzscmelze GmbH | Method of producing synthetic quartz glass |
| US4650511A (en) * | 1984-06-04 | 1987-03-17 | Shin-Etsu Chemical Co., Ltd. | Method for the preparation of a dehydrated quartz glass material for light transmission |
| JPH0881226A (en) * | 1994-09-16 | 1996-03-26 | Tosoh Corp | Production of high-purity, high heat-resistant quartz glass |
| CN101050054A (en) * | 2007-03-28 | 2007-10-10 | 徐胜利 | Vacuum deshydroxy method for quartz glass cell |
| CN101337767A (en) * | 2008-08-15 | 2009-01-07 | 杜建中 | Purification method in process of production of high-pure quartz sand as raw material of quartz glass |
| CN103613102A (en) * | 2013-12-04 | 2014-03-05 | 南京工业大学东海先进硅基材料研究院 | Process for preparing ultrahigh pure quartz sand through silica raw material |
| CN107140812A (en) * | 2017-06-12 | 2017-09-08 | 江苏太平洋石英股份有限公司 | A kind of production method of low hydroxyl dark red doping quartz ampoule |
| CN110040942A (en) * | 2018-01-16 | 2019-07-23 | 中天科技集团有限公司 | The preparation method of body of powder deshydroxy processing method and quartz glass |
| CN109336116A (en) * | 2018-10-31 | 2019-02-15 | 黄冈师范学院 | A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite |
| CN110182814A (en) * | 2019-04-20 | 2019-08-30 | 黄冈师范学院 | A kind of SiO2The production method of glass sand of the purity greater than 5N |
| CN110862091A (en) * | 2019-12-25 | 2020-03-06 | 苏州纳迪微电子有限公司 | High-purity quartz sand and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| 侯清麟等."去除石英砂中羟基的技术研究".《技术应用与研究》.2017,第32-33页. * |
| 周永恒等."石英玻璃脱羟机理的研究".《硅酸盐学报》.2001,第29卷(第1期),第59-62页. * |
| 西北轻工业学院."石英玻璃 熔制".《玻璃工艺学》.中国轻工业出版社,2007,第520-525页. * |
| 魏忠诚等."富氢还原 脱羟基".《光纤材料制备技术》.北京邮电大学出版社,2016,第147-150页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111320177A (en) | 2020-06-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111320177B (en) | Method for removing hydroxyl groups in quartz sand powder | |
| JP3751326B2 (en) | Manufacturing method of high purity transparent quartz glass | |
| CN112144115B (en) | Quartz crucible with long service life and low deformation rate and preparation method thereof | |
| JPWO2010125739A1 (en) | Silica container and method for producing the same | |
| CN107445173B (en) | Preparation method of low-hydroxyl ultrahigh-purity quartz sand | |
| RU2451635C2 (en) | Method of producing highly pure elementary silicon | |
| CN111393022B (en) | Preparation method of high-purity low-hydroxyl quartz glass raw material | |
| JP4181226B2 (en) | Manufacturing method of high purity, high heat resistant quartz glass | |
| WO2013171955A1 (en) | Silica vessel for drawing up monocrystalline silicon and method for producing same | |
| CN111056556A (en) | Method for preparing polycrystalline silicon by taking silicon dioxide and hydrogen as raw materials | |
| CN103112862A (en) | Method for producing fused obtuse quartz sand from quartz crucibles | |
| CN116444135A (en) | Preparation method of high-purity quartz sand with purity reaching raw material grade of quartz glass crucible | |
| CN111020257B (en) | Method for improving purity of nickel cupronickel material | |
| JPH0450734B2 (en) | ||
| CN111252769A (en) | Preparation method of solar polycrystalline silicon | |
| JP4526311B2 (en) | Method for producing quartz glass crucible | |
| CN112010310A (en) | Preparation method of silicon carbide powder for precision grinding | |
| JP3123696B2 (en) | Method for manufacturing quartz glass crucible | |
| JP4000399B2 (en) | Method for producing ultra-high purity silica powder, ultra-high purity silica powder obtained by the production method, and quartz glass crucible using the same | |
| CN110820041B (en) | Low-deformation-rate quartz crucible and preparation method thereof | |
| WO2024093654A1 (en) | Method for preparing high-purity quartz sand from waste quartz crucible, high-temperature furnace and method for preparing high-purity quartz sand and high-purity quartz sand | |
| CN117446808A (en) | Method for dehydroxylating quartz sand by repeating phase-change structure fracture hydroxyl principle | |
| JPH09295826A (en) | Production of high-purity transparent silica glass | |
| CN114540941A (en) | Method for preparing solar-grade silicon by utilizing crystalline silicon diamond wire cutting waste | |
| CN108164137B (en) | Method for preparing high-density fused quartz material by using Grignard reagent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |