CN111393022A - Preparation method of high-purity low-hydroxyl quartz glass raw material - Google Patents
Preparation method of high-purity low-hydroxyl quartz glass raw material Download PDFInfo
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- CN111393022A CN111393022A CN202010205947.1A CN202010205947A CN111393022A CN 111393022 A CN111393022 A CN 111393022A CN 202010205947 A CN202010205947 A CN 202010205947A CN 111393022 A CN111393022 A CN 111393022A
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/022—Purification of silica sand or other minerals
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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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/024—Chemical treatment of cullet or glass fibres
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Abstract
The invention relates to a preparation method of a high-purity low-hydroxyl quartz glass raw material, which is characterized in that high-purity quartz sand is adopted to melt quartz glass or a recycled quartz glass product as an initial raw material, and the initial raw material is subjected to dehydroxylation treatment in a high-temperature high-vacuum environment after being subjected to sand making, so that the high-purity low-hydroxyl quartz glass raw material is finally obtained. The prepared quartz glass raw material sand powder has the characteristics of high purity, high transparency, low hydroxyl and no bubble, and can greatly improve the qualification rate of quartz glass products, reduce the production cost of enterprises and improve the economic benefit of the enterprises.
Description
Technical Field
The invention relates to a preparation method of a high-purity low-hydroxyl quartz glass raw material, belonging to the deep processing industry of non-metallic ores.
Background
JC/T597-2011 provides that the content of hydroxyl groups is less than or equal to 220 × 10-6The content of hydroxyl group in transparent quartz glass rod for semiconductor JC/T2064-2011 is less than or equal to 220 × 10-6In the specification JC/T598-2007 in transparent quartz glass tube for electric light source, a) the hydroxyl group content of the high-pressure mercury lamp tube is less than or equal to 10 × 10-6B) the hydroxyl content of the metal halide lamp tube is less than or equal to 3 × 10-6(ii) a c) Halogen tungsten lamp tube, quartz glass tube for other lamp: agreed by both the supplier and the demand.
The transparent quartz glass and its product are made up by using high-purity quartz sand powder as raw material, using hydrogen or inert gas or hydrogen + nitrogen + inert gas as protective gas, melting and making them into glass liquor, then making the glass liquor undergo the processes of mechanical forming, cutting, cooling, cleaning and dehydroxylation, etc.. The hydroxyl group source of the quartz glass article is derived from two parts: one is hydroxyl contained in the quartz sand, and the other part is protective gas H in the high-temperature melting process2SiO with quartz glass2The hydroxyl group produced by the chemical reaction is higher in proportion than the former one. The hydroxyl contained in the quartz sand is mainly from structural water in the quartz crystal structure and is (OH)-、H+、(H3O)+"Water" participating in the mineral lattice in ionic form, in Order (OH)-The most common form is difficult to remove because of the strong bonding forces associated with other particles in the crystal.
In the process of melting the quartz glass, along with the rise of melting temperature and the increase of melting time, the viscosity of the glass liquid is gradually reduced, and gas, liquid inclusion, structural water and hydroxyl groups remained in the high-purity quartz sand powder slowly form tiny bubbles and gradually increase in the melting process, and finally escape from the glass liquid. Due to the SiO accompanying the melting process2Because of volatilization, the melting time and melting temperature need to be controlled to a certain extent to reduce the loss of raw materials. In addition, the molten glass still has certain viscosity at high temperature, and some fine bubbles are difficult to overcome the viscosity resistance of the molten glass and can remain or dissolve at the later stage of homogenizationDissolved in transparent glass liquid and finally exists in the quartz glass product in the form of hydroxyl. Hydroxyl groups are usually removed by adopting a high-temperature high-vacuum method, but the hydroxyl group removing effect of high-temperature vacuum treatment is limited, and if quartz glass products are subjected to hydroxyl group removing treatment and are still unmarked, the quartz glass products are difficult to rework and generally directly scrapped, so that the production of high-quality quartz glass and products is greatly limited. In order to solve the problem of hydroxyl in the raw material of the quartz glass and improve the qualification rate of the quartz glass and products thereof, people must start with controlling the hydroxyl in the raw material sand of the quartz glass, ensure the purity of the raw material, control the hydroxyl in the raw material sand within the standard required by the quartz glass products, and even realize no hydroxyl.
Therefore, we have specially developed a method for preparing high-purity low-hydroxyl quartz glass raw material, which is prepared by the method, wherein the hydroxyl of the quartz glass raw material is less than 1ppm, and SiO is2The purity is more than 99.998%.
Disclosure of Invention
The invention aims to provide a preparation method of a high-purity low-hydroxyl quartz glass raw material, and the prepared quartz glass raw material sand powder has the characteristics of high purity, high transparency and low hydroxyl, and can greatly improve the qualification rate of quartz glass products, reduce the production cost of enterprises and improve the economic benefit of the enterprises.
The scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a high-purity low-hydroxyl quartz glass raw material comprises the steps of adopting high-purity quartz sand to smelt quartz glass, taking the obtained quartz glass as an initial raw material or directly adopting a recycled quartz glass product as the initial raw material, carrying out dehydroxylation treatment on the sand-making initial raw material in a high-temperature high-vacuum environment, and finally obtaining the high-purity low-hydroxyl quartz glass raw material.
Preferably, the preparation method specifically comprises the following steps:
(1) washing the initial raw material quartz glass with clean water for later use;
(2) carrying out dry or wet sand making on the cleaned quartz glass, and grading the prepared sand powder for later use after carrying out strong magnetic separation or high-voltage electric separation;
(3) and (3) carrying out high-temperature high-vacuum hydroxyl removal treatment on the obtained material to obtain the quartz glass raw material sand powder with high purity and low hydroxyl content.
Preferably, after the raw materials are made into sand, the obtained quartz sand is subjected to acid washing for impurity removal and then subjected to dehydroxylation treatment.
Preferably, the acid solution used for acid washing impurity removal is HF, HCl and HNO3、H2C2O4One or more of (a) and (b).
Preferably, the purity of the fused silica glass or the recovered silica glass product as the starting material is 99.99% to 99.995% and the hydroxyl group content is 10ppm to 300 ppm; the purity of the quartz glass raw material with high purity and low hydroxyl content is 99.996-99.9992% and the hydroxyl content is less than 1 ppm.
Preferably, the high purity silica sand used for melting the silica glass has a purity of 4N or more.
Preferably, the step of melting the quartz glass by using the high-purity quartz sand comprises the following steps:
(1) taking quartz vein as a raw material, and performing mineral separation, crushing, acid washing, calcining, water quenching, sand making, magnetic separation, grading, acid washing, pure water washing, drying, calcining, secondary water quenching, secondary acid washing, pure water washing and drying to obtain high-purity quartz sand;
(2) the obtained high-purity quartz sand is subjected to high-temperature chlorination for 0.5 to 1 hour at the temperature of 1150-;
(3) and (3) feeding the chloridized quartz sand into a continuous melting device, and melting the quartz sand into transparent quartz glass.
Preferably, inert gas is used as protective gas in the melting process in the step (3).
According to the method, through a melting process, the crystal structure of quartz sand particles is damaged, the quartz particles are changed into amorphous quartz glass from a crystalline state, most of hydroxyl groups are removed in the structure conversion, the hydroxyl groups remained in the quartz glass are subjected to a sand making mode, the positions of the hydroxyl groups and impurities in the quartz glass can be preferentially broken due to stress concentration and exposed on the surface of the sand particles, and the high-purity and low-hydroxyl quartz glass raw material can be obtained through re-purification and high-temperature high-vacuum dehydroxylation treatment.
The method combining melting and high-temperature dehydroxylation is adopted, the melting time of the quartz glass does not need to be prolonged or the melting temperature does not need to be increased, and SiO in the production process of the high-transparency low-hydroxyl quartz glass can be reduced to a great extent2And (4) loss.
The method also opens up a new way and thought for the utilization of the high added value of the waste reclaimed materials of the transparent quartz glass and the products thereof, and saves a large amount of precious high-purity quartz resources.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
The hydroxyl content is tested by the method in GB/T12442-2019, and the purity of the quartz glass raw material is tested by the method in GB/T3284-2015; the final fused quartz glass product purity was as follows: the SJ/T3328.1/10-2016 method is used for detection, and the latter method is suitable for detection of raw materials with purity of more than 99.998%.
Example 1
Taking vein quartz with the purity of 99.98% in a certain place in Henan as a raw material, and carrying out the following steps according to the patent number 201310440921.5 and the patent name: a low-cost, continuous process for producing a high purity fused silica mass and the fused silica mass produced by the process in the apparatus are used as the starting material in this example. Detecting SiO in the obtained fused quartz material2The purity was 99.99% and the hydroxyl group content was 50 ppm.
The initial raw materials are processed according to the following steps:
1, crushing initial raw materials, then using an iron sand making machine to make sand by a wet method, carrying out magnetic separation on the prepared mortar by a 1.8T electromagnetic separator, then using a water sieve to carry out classification, collecting 40-70 meshes, 70-120 meshes and 120-200 meshes of mortar, and dehydrating for later use.
2, respectively sending the sand powder with different mesh intervals to corresponding high-purity quartz sand pickling purification devices (Z L201110247061.4), dynamically pickling and purifying for 3 hours by using mixed acid liquor consisting of 2% HF and 20% HCl at the temperature of 85 ℃, removing the acid liquor, washing the sand powder to be neutral by using tap water, washing the sand powder by using electronic grade high-purity water for at least three times, and dehydrating for later use.
3, conveying the dehydrated sand powder obtained in the step 2 into a high-temperature drying device made of high-purity quartz for drying, then conveying into a high-temperature high-vacuum dehydroxylation furnace, and performing dehydration at 1080 ℃ and 6.5 × 10-6And pa, removing hydroxyl for 5 hours to obtain the high-purity quartz glass raw material sand powder.
4, feeding the quartz glass raw material sand powder (70-120 meshes) in the step 3 into a continuous quartz tube drawing furnace to melt quartz glass liquid at 1800-2200 ℃, and drawing the transparent quartz glass tube for the electric light source by adopting high-purity helium as protective gas according to a conventional process method. The hydroxyl content of the finished product of the pulled transparent quartz glass tube is less than 1 ppm; SiO 22The purity is 99.999%.
Example 2
Taking a waste quartz glass crucible after drawing monocrystalline silicon as an initial raw material, wherein SiO in the quartz glass crucible2Purity: 99.998%, and a hydroxyl group content of 10 ppm.
The initial raw materials are processed according to the following steps:
1, breaking a quartz glass crucible, washing the quartz glass crucible clean by tap water, performing wet sand making by an iron sand making machine, performing magnetic separation on the prepared mortar by a 2.2T electromagnetic separator, classifying and collecting 40-70 meshes, 70-120 meshes, 120-sand-containing 200 meshes and 200-sand-containing 300 meshes of mortar by a water sieve, and dehydrating for later use.
2, respectively sending the sand powder with different mesh intervals to corresponding quartz sand pickling and purifying devices (Z L201310279400.6) and using 3 percent of HF and 5 percent of HNO3The mixed acid liquid is dynamically acid-washed and purified for 3 hours at the temperature of 90 ℃, then acid liquid is removed, and then the mixed acid liquid is washed to be neutral by tap water, washed by electronic grade high-purity water for at least three times and dehydrated for standby.
3, conveying the sand powder dehydrated in the step 2 into a high-temperature drying device made of high-purity quartz materials for drying to obtain high-purity quartz glass raw material sand powder, and then conveying the high-temperature quartz glass raw material sand powder into a high-temperature drying deviceIn an air-drying oxyhydrogen furnace, the temperature is 1080 ℃, and the vacuum degree is 6.5 × 10-6Carrying out dehydroxylation for 5.5 hours under pa condition to obtain high-purity low-hydroxyl quartz glass raw material sand powder;
4, feeding the quartz glass raw material sand powder (40-70 meshes) obtained in the step 3 into a continuous quartz rod pulling furnace to melt quartz glass liquid at 1800-2200 ℃, and pulling a transparent quartz glass rod for a semiconductor by adopting high-purity helium as a protective gas according to a conventional process method. The hydroxyl content of the finished product of the pulled transparent quartz glass rod is less than 1 ppm; SiO 22The purity is 99.9992%.
Example 3
Waste quartz glass ingots are used as initial raw materials, and SiO in the quartz glass ingots2The purity was 99.996%, and the hydroxyl group content was 300 ppm.
The initial raw materials are processed according to the following steps:
1, crushing quartz glass ingots by manpower, cleaning and airing, then carrying out wet-method sand making by an iron sand making machine, carrying out magnetic separation on the prepared mortar by an electromagnetic separator with the magnetic field intensity of 3.0T, then carrying out classification by a water sieve, carrying out classification on the slurry after the magnetic separation by the water sieve, collecting 40-70 meshes, 70-120 meshes and 120-mesh and 200-mesh mortar, and dehydrating for later use.
2, respectively sending the sand powder with different mesh intervals to corresponding quartz sand pickling and purifying devices (Z L201310279400.6) and using 5% HF + 10% H2C2O4The mixed acid liquid is dynamically acid-washed and purified for 3 hours at the temperature of 98 ℃, the acid liquid is removed, then the mixed acid liquid is washed to be neutral by tap water, and is washed by electronic grade high-purity water for at least three times, and then the mixed acid liquid is dehydrated for standby.
3, conveying the sand powder dehydrated in the step 2 into a high-temperature drying device made of high-purity quartz for drying, and then conveying the sand powder into a high-temperature vacuum dehydroxylation furnace at the temperature of 1080 ℃ and the vacuum degree of 6.5 × 10-6Carrying out dehydroxylation for 7 hours under pa condition to obtain high-purity quartz glass raw material sand powder;
4, feeding the quartz glass raw material sand powder (40-70 meshes) obtained in the step 3 into a continuous quartz pulling tube furnace for melting quartz glass liquid at 1800 plus 2200 ℃, and adopting high-purity helium as protective gasThe drawing of a transparent quartz glass tube for semiconductors is carried out according to conventional process methods. The hydroxyl content of the finished product of the pulled transparent quartz glass tube is less than 1 ppm; SiO 22The purity was 99.9991%.
Example 4
Using waste material of drawn quartz glass tube as initial raw material, in which SiO is contained2Purity 99.995% and hydroxyl group content 240 ppm.
The initial raw materials are processed according to the following steps:
1, crushing a quartz glass tube, cleaning and airing, performing dry-method sand making by using an iron sand making machine, performing electric separation on the prepared sand powder by using a high-voltage electric separator, classifying by using a dry sieve, and collecting 40-70 meshes, 70-120 meshes and 120-200 meshes of sand powder for later use.
2, respectively sending the sand powder with different mesh intervals to corresponding high-purity quartz sand pickling purification devices (Z L201110121881.9), dynamically pickling and purifying the sand powder for 3 hours at the temperature of 85 ℃ by using mixed acid liquor consisting of 2% HF and 10% HCl, removing the acid liquor, washing the sand powder to be neutral by using tap water, washing the sand powder for at least three times by using electronic grade high-purity water, and dehydrating the sand powder for later use.
3, conveying the sand powder dehydrated in the step 2 into a high-temperature drying device made of high-purity quartz for drying, and then conveying the sand powder into a high-temperature vacuum dehydroxylation furnace at the temperature of 1080 ℃ and the vacuum degree of 6.5 × 10-6Carrying out dehydroxylation for more than 6.5 hours under pa condition to obtain high-purity quartz glass raw material sand powder;
4, feeding the quartz glass raw material sand powder (40-70 meshes) obtained in the step 3 into a continuous quartz rod pulling furnace to melt quartz glass liquid at 1800-2200 ℃, and pulling a transparent quartz glass rod for a semiconductor by adopting high-purity helium as a protective gas according to a conventional process method. The hydroxyl content of the finished product of the pulled transparent quartz glass rod is 1 ppm; SiO 22The purity is 99.998%.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (8)
1. A preparation method of a high-purity low-hydroxyl quartz glass raw material is characterized in that high-purity quartz sand is adopted to melt quartz glass, the obtained quartz glass is used as an initial raw material or a recycled quartz glass product is directly used as the initial raw material, and after the initial raw material is subjected to sand making, dehydroxylation treatment is carried out in a high-temperature high-vacuum environment, so that the high-purity low-hydroxyl quartz glass raw material is finally obtained.
2. The method of claim 1, comprising the steps of:
(1) washing the initial raw material quartz glass with clean water for later use;
(2) carrying out dry or wet sand making on the cleaned quartz glass, and grading the prepared sand powder for later use after carrying out strong magnetic separation or high-voltage electric separation;
(3) and (3) carrying out high-temperature high-vacuum hydroxyl removal treatment on the obtained material to obtain the quartz glass raw material sand powder with high purity and low hydroxyl content.
3. The production method according to claim 1 or 2, wherein after the raw material is granulated, the obtained quartz sand is subjected to acid washing for removing impurities and then subjected to dehydroxylation.
4. The preparation method according to claim 1, wherein the acid solution used for acid washing and impurity removal is HF, HCl or HNO3、H2C2O4One or more of (a) and (b).
5. The production method according to claim 1, wherein the purity of the fused silica glass or the recovered silica glass product as a starting material is not less than 99.99% and the hydroxyl group content is 10ppm to 300 ppm; the purity of the quartz glass raw material with high purity and low hydroxyl content is 99.996-99.9992% and the hydroxyl content is less than 1 ppm.
6. The method according to claim 1, wherein the step of melting the silica glass using the high-purity silica sand comprises:
(1) subjecting a vein quartz raw material to mineral separation, crushing, acid washing, calcining, water quenching, sand making, magnetic separation, grading, acid washing, pure water washing, drying, calcining, secondary water quenching, secondary acid washing, pure water washing and drying to obtain high-purity quartz sand;
(2) the obtained high-purity quartz sand is subjected to high-temperature chlorination for 0.5 to 1 hour at the temperature of 1150-;
(3) and (3) feeding the chloridized quartz sand into a continuous melting device, and melting the quartz sand into transparent quartz glass.
7. The method according to claim 6, wherein an inert gas is used as a shielding gas during the melting in the step (3).
8. A method for preparing high-purity, high-transparency and low-hydroxyl quartz glass is characterized in that the quartz glass raw material obtained by the preparation method of any one of claims 1 to 7 is subjected to high-temperature melting under the protection of inert gas to obtain the high-purity, high-transparency and low-hydroxyl quartz glass.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114249524A (en) * | 2020-09-22 | 2022-03-29 | 中天科技精密材料有限公司 | Low-hydroxyl high-purity quartz glass and preparation method thereof |
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