Quartz glass preparation method using quartz powder as raw material and quartz products

By screening and dehydroxylation of quartz powder, and then static pressure treatment in a static pressure device made of high-purity quartz material, the impurity pollution and bubble residue problems in the preparation of quartz glass are solved, and quartz products with high purity, low stress, and high optical uniformity are prepared, suitable for semiconductors and high-energy lasers and other fields.

CN120289069BActive Publication Date: 2025-09-02NANTONG CRYSTAL CO LTD
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Patent Information

Application Number
CN202510776020.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-11
Publication Date
2025-09-02
Estimated Expiration
2045-06-11

AI Technical Summary

Technical Problem

In the preparation of quartz glass, the prior art has problems such as impurity contamination, bubble residue, difficulty in achieving high optical uniformity and low residual stress, especially in cutting-edge fields such as semiconductors and high-energy lasers.

Method used

Quartz powder is used as raw material, and after screening and dehydroxylation treatment, static pressure is performed in a static pressure device made of high-purity quartz material to avoid contact with other materials. Quartz glass is prepared in a non-melting environment through a two-step process.

Benefits of technology

Quartz products with high optical uniformity, low stress, low hydroxyl and high purity have been achieved, meeting the high-end performance requirements in semiconductors and high-energy lasers.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application provides a method for preparing quartz glass using quartz powder as a raw material and a quartz product. The method for preparing quartz glass using quartz powder as a raw material comprises the following steps: providing quartz powder as an initial raw material; pre-treating the initial raw material to obtain a statically pressed raw material containing quartz powder, wherein the pre-treatment includes at least screening and dehydroxylation of the initial raw material; placing the statically pressed raw material in a static pressing device for static pressing to obtain a quartz powder block, wherein the portion of the static pressing device that contacts the quartz powder is made of high-purity quartz; placing the quartz powder block in a container having a contact surface made of high-purity quartz, and vitrifying the quartz powder block to obtain quartz glass.
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Description

Technical Field

[0001] The present application relates to the field of materials chemistry, and in particular to a method for preparing quartz glass using quartz powder as raw material and a quartz product. Background Art

[0002] Currently, there are two main methods for preparing quartz glass: physical and chemical. The chemical method involves hydrolyzing silicon-containing raw materials to produce silica particles, which are then further converted into quartz glass. Depending on the synthesis process, the chemical method can be divided into a two-step process and a one-step process. The one-step process involves high-temperature hydrolysis of silicon sources such as silicon tetrachloride and organosilane to directly produce quartz glass ingots. Key processes include CVD and PCVD. The two-step process involves high-temperature hydrolysis of the silicon source, which is then deposited onto a substrate as a loose body in the form of silica powder. This loose body is then heated to produce quartz glass. Key processes include VAD and OVD. The physical method involves melting and solidifying high-purity quartz powder through methods such as gas or electric melting to form quartz glass. Physical melting involves pouring high-purity quartz powder into a high-temperature resistant crucible, heating it to melt, and then cooling the molten quartz to solidify it into a large block of quartz glass. Because quartz melts at extremely high temperatures (typically exceeding 1700°C), crucibles typically used for smelting are made from high-melting-point oxide ceramics (such as alumina and zirconia) and high-melting-point elements (such as molybdenum, tungsten, and carbon). Quartz obtained through direct high-temperature smelting of quartz powder retains a high viscosity even when molten, making it difficult to remove gas trapped in the powder voids, which can easily form bubbles within the quartz glass. Furthermore, high-temperature smelting inevitably involves contact with the crucible, and elements contained in the crucible's material can gradually penetrate and cause contamination. Due to the purity limitations of the crucible's material, other impurities present in the crucible can also penetrate the quartz glass, ultimately affecting its purity.

[0003] Conventional technology uses high-purity quartz powder as the raw material. The powder is poured into a dispersion consisting of water, organic matter, or a mixture of the two. The quartz powder and dispersion are then uniformly mixed through ball milling and stirring to form a slurry. The uniform slurry is then poured into a specific mold and formed by freezing or air-drying. After forming, the block is separated from the mold. A large amount of dispersion liquid still remains in the block. This residual dispersion is evaporated by drying to form a dry quartz powder block. This block is then sintered at high temperature to form transparent quartz glass. While the slurry forming method can somewhat reduce the problem of bubbles and cracking within the glass, it is affected by the purity of the dispersion itself and the material of the ball milling equipment (typically alumina, zirconia, etc.), which exacerbates the contamination of the quartz glass with impurities. Furthermore, quartz glass produced using physical smelting of quartz powder lacks the characteristics of low residual stress and high optical uniformity, making it difficult to apply to cutting-edge fields such as semiconductors and high-energy lasers. Those skilled in the art need to consider how to address these issues. Summary of the Invention

[0004] In order to solve the above problems, the embodiments of the present application provide a method for preparing high-purity quartz using quartz powder as raw material and a quartz product prepared using the method, which can obtain a quartz product with high optical uniformity, low stress, low hydroxyl content and high purity.

[0005] The present invention provides a method for preparing quartz glass using quartz powder as a raw material, which comprises the following steps:

[0006] Providing quartz powder as a starting material;

[0007] Pre-treating the initial raw material to obtain a statically pressed raw material containing quartz powder, wherein the pre-treatment at least includes a process of screening the initial raw material and a process of dehydroxylating the initial raw material;

[0008] The statically pressed raw material is placed in a static pressing device for static pressing to obtain a quartz powder block, wherein the parts of the static pressing device that are in contact with the quartz powder are all made of high-purity quartz;

[0009] The quartz powder block is placed in a container whose contact surface is high-purity quartz, and the quartz powder block is vitrified to obtain quartz glass.

[0010] In one embodiment, the step of screening the initial raw material includes:

[0011] The quartz powder is vibrated and sieved using a sieve to obtain silicon dioxide particles with a particle size of 50 nanometers to 300 micrometers.

[0012] In one embodiment, the silica particles have a particle size of 100 nanometers to 200 micrometers.

[0013] In one embodiment, the step of dehydroxylating the initial raw material comprises:

[0014] placing quartz powder in a dehydroxylation furnace, evacuating the interior of the dehydroxylation furnace to a vacuum state, and controlling the vacuum degree in the dehydroxylation furnace to be less than 10 Pa;

[0015] The quartz powder in the dehydroxylation furnace is heated to remove the hydroxyl groups inside the quartz powder. The dehydroxylation temperature of the dehydroxylation furnace is controlled to be 500° C. to 1300° C., and the dehydroxylation holding time of the dehydroxylation furnace is controlled to be 10 hours to 100 hours.

[0016] In one embodiment, the vacuum degree in the dehydroxylation furnace is controlled to be less than 1 Pa;

[0017] The dehydroxylation temperature of the dehydroxylation furnace is controlled to be 700° C. to 1100° C., and the dehydroxylation holding time of the dehydroxylation furnace is controlled to be 40 hours to 80 hours.

[0018] In one embodiment, the static pressure of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 2 MPa to 15 MPa, and the holding time of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 5 minutes to 120 minutes; the density of the quartz powder block obtained by static pressure treatment in the static pressure device is controlled to be 0.2 g / cm 3 to 1.8g / cm 3 .

[0019] In one embodiment, the static pressure of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 5 MPa to 10 MPa, and the holding time of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 30 minutes to 60 minutes; the density of the quartz powder block obtained by static pressure treatment in the static pressure device is controlled to be 0.5 g / cm 3 to 0.6g / cm 3 .

[0020] In one embodiment, the static pressure device includes a base and a plurality of static pressure components disposed around the base;

[0021] The base cooperates with the plurality of static pressure components to form a static pressure cavity, the static pressure cavity is used to accommodate quartz powder, and the positions of the plurality of static pressure components relative to the base are adjustable to squeeze the quartz powder in the static pressure cavity;

[0022] The surfaces of the base and the plurality of static pressure components that are in contact with quartz powder are all made of high-purity quartz.

[0023] In one embodiment, the vitrification temperature of the quartz powder block is controlled to be in a range of 1350° C. to 1500° C., and the vitrification time of the quartz powder block is controlled to be in a range of 10 hours to 90 hours.

[0024] In one embodiment, the vitrification temperature range of the vitrification of the quartz powder block is controlled to be 1400° C. to 1480° C., and the vitrification time range of the vitrification of the quartz powder block is controlled to be 40 hours to 60 hours.

[0025] The embodiment of the present application further provides a quartz product, which is prepared by the quartz glass preparation method using quartz powder as raw material as described in any one of the aforementioned embodiments.

[0026] Furthermore, the quartz glass preparation method using quartz powder as raw material provided in the embodiments of the present application can obtain quartz products with high optical uniformity, low stress, low hydroxyl content, and high purity. On the one hand, by dispersing, screening, and dehydroxylating the quartz powder, the hydroxyl content of the powder is controlled, thereby controlling the hydroxyl content of the quartz glass, and the preparation of quartz glass with a hydroxyl content of less than 1ppm can be achieved. On the other hand, the quartz powder is statically pressed using a static pressure device whose parts in contact with the quartz powder are all made of quartz material to avoid the introduction of impurities due to contact, and a quartz powder block with specific specifications and specific density is pressed out. On the other hand, the present application adopts a process imitating a two-step method, causing the quartz powder to slowly shrink in a non-melting environment to prepare high-purity synthetic quartz glass. The product has the characteristics of high purity, low hydroxyl content, no bubbles, no streaks, high optical uniformity, and low stress. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 A schematic flow chart of a method for preparing quartz glass using quartz powder as raw material provided in an embodiment of the present application.

[0028] Figure 2 A schematic structural diagram of a static pressure device used in a method for preparing quartz glass using quartz powder as a raw material provided in an embodiment of the present application.

[0029] Figure 3 A schematic structural diagram of a static pressure device used in a method for preparing quartz glass using quartz powder as a raw material provided in an embodiment of the present application.

[0030] Description of main component symbols

[0031] Static pressure device 10

[0032] Static pressure chamber 100

[0033] Base 11

[0034] Support portion 111

[0035] Quartz bottom 112

[0036] Static pressure components 12

[0037] Pressure rod 121

[0038] Connect push block 122

[0039] Quartz extrusion gasket 123

[0040] Quartz powder block 20

[0041] The following specific implementation methods will further illustrate the present application in conjunction with the above-mentioned drawings. DETAILED DESCRIPTION

[0042] The following description will refer to the accompanying drawings to more fully describe the contents of this application. Illustrated in the accompanying drawings are exemplary embodiments of the present application. However, the present application can be implemented in many different forms and should not be construed as limited to the exemplary embodiments set forth herein. These exemplary embodiments are provided to make this application thorough and complete and to fully convey the scope of this application to those skilled in the art. Like reference numerals represent identical or similar components.

[0043] The terms used herein are for the purpose of describing specific exemplary embodiments only and are not intended to limit the present application. As used herein, unless the context clearly indicates otherwise, the singular forms "a", "an" and "the" are intended to include the plural forms as well. In addition, when used herein, "includes" and / or "comprising" and / or "having" integers, steps, operations, components and / or components do not preclude the presence or addition of one or more other features, regions, integers, steps, operations, components and / or groups thereof.

[0044] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In addition, unless explicitly defined herein, terms such as those defined in common dictionaries should be interpreted as having a meaning consistent with their meaning in the relevant art and the context of this application, and will not be interpreted as idealized or overly formal meanings.

[0045] Typically, high-purity quartz powder is used as the raw material. The powder is poured into a dispersion consisting of water, organic matter, or a mixture of both. The quartz powder and dispersion are then uniformly mixed through ball milling and stirring to form a slurry. The homogenized slurry is then poured into a mold and formed by freezing or air-drying. After forming, the block is separated from the mold. A large amount of dispersion liquid still remains in the block. This is evaporated through drying to form a dry quartz powder block. This block is then sintered at high temperature to form transparent quartz glass. While this slurry forming method can reduce internal bubbles and cracking in the glass to a certain extent, it can exacerbate contamination of the quartz glass due to the influence of the dispersion purity and the material of the ball mill (typically alumina, zirconia, etc.).

[0046] For example, foreign patent application EP2050724A1 proposes a method for preparing quartz glass blocks from high-temperature fused quartz particles, wherein quartz powder is penetrated into the powder using a vibrating rod coated with quartz glass, and then vibrated to a density of 1.4 g / cm 3 Up to 1.6g / cm 3It is then melted at high temperature in a ceramic furnace and cooled to produce quartz glass. This method avoids the introduction of impurities by adding quartz plates or molybdenum plates inside the alumina or zirconia furnace. However, because the temperature during high-temperature melting is as high as 1790°C, the quartz plates used for blocking will also be melted, and will not be able to prevent the infiltration of impurities. Although the melting point of the molybdenum plate is relatively high, molybdenum itself will also diffuse into the quartz glass at high temperatures, affecting the purity of the melted quartz glass. At the same time, this method uses a vibrating rod to vibrate and compact the gas between the particles, which is inefficient and will intensify the friction between the quartz powder and the crucible wall during the vibration process, which also increases the risk of impurity introduction. This patent uses high-pressure helium to remove water vapor and gas molecules adsorbed by the quartz powder, and cannot effectively remove hydroxyl groups in the quartz powder. Foreign patent application EP3390306A2 proposes a method for producing quartz glass by high-temperature melting of quartz particles in a hanging sintered crucible. The quartz powder raw material is prepared by gas atomization and then continuously melted at high temperature in a molybdenum / tungsten furnace. The quartz glass product is continuously produced from the opening at the lower end of the furnace. The quartz glass produced by this method has a high concentration of common metal impurities, approaching 1 ppm. Furthermore, due to the use of molybdenum and tungsten furnace materials, metal infiltration into the furnace material is significant, also reaching 1 ppm. Furthermore, the continuous production process makes it impossible to remove moisture and hydroxyl groups from the powder, resulting in a hydroxyl content of 200-400 ppm. Foreign patent application DE102011120932A1 proposes a process for producing transparent quartz glass from a silica slurry. The slurry is a uniform mixture of silica and water, or water and organic matter, ground with alumina grinding balls. The slurry is poured into a specific mold, freeze-formed, then heated at low temperature to remove moisture, and then sintered at high temperature to produce the transparent quartz glass. The method described in this patent can solve the problem of internal bubbles in the material, but the process is complex. The complex solution system mixing process involved in this method introduces impurities from the grinding balls, solution, and other substances in contact. Furthermore, because the preparation process is a liquid phase system, the hydroxyl content of the resulting quartz glass is difficult to control. Furthermore, quartz glass produced using physical smelting of quartz powder cannot achieve high-end optical performance indicators such as low residual stress and high optical uniformity.

[0047] Correspondingly, the present application provides a method for preparing high-purity quartz with low stress, high optical uniformity, and low hydroxyl content using quartz powder as a raw material, and a quartz product prepared using the method. The method for preparing quartz glass using quartz powder as a raw material comprises the following steps: providing quartz powder as a starting raw material; pre-treating the starting raw material to obtain a statically pressed raw material containing quartz powder, wherein the pre-treatment comprises at least the steps of screening the starting raw material and dehydroxylating the starting raw material; placing the statically pressed raw material in a static pressing device for static pressing to obtain a quartz powder block, wherein the portion of the static pressing device that contacts the quartz powder is made of high-purity quartz; placing the quartz powder block in a container having a contact surface made of high-purity quartz, and vitrifying the quartz powder block to obtain quartz glass.

[0048] Furthermore, the quartz glass preparation method using quartz powder as raw material provided in the embodiments of the present application can obtain high-purity quartz products. On the one hand, by dispersing, screening and dehydroxylating the quartz powder, the hydroxyl content of the powder is controlled, thereby controlling the hydroxyl content of the quartz glass, and the preparation of quartz glass with a hydroxyl content of less than 1 ppm can be achieved. On the other hand, the quartz powder is statically pressed using a static pressure device whose parts in contact with the quartz powder are all made of high-purity quartz material, avoiding the introduction of impurities due to contact, and pressing out quartz powder blocks with specific specifications and specific density. On the other hand, the present application adopts a simulated two-step process to prepare high-purity synthetic quartz glass in a non-melting environment. The product has the characteristics of high purity, low hydroxyl, low stress, high optical uniformity, no bubbles, and no streaks.

[0049] The specific implementation methods of the present application will be described in further detail below with reference to the accompanying drawings.

[0050] A method for preparing quartz glass using quartz powder as raw material comprises the following steps:

[0051] Providing quartz powder as a starting material;

[0052] Pre-treating the initial raw material to obtain a statically pressed raw material containing quartz powder, wherein the pre-treatment at least includes the steps of screening the initial raw material and dehydroxylating the initial raw material;

[0053] The statically pressed raw material is placed in a static pressing device for static pressing to obtain a quartz powder block, wherein the parts of the static pressing device that are in contact with the quartz powder are all made of high-purity quartz;

[0054] The quartz powder block is placed in a container whose contact surface is high-purity quartz, and the quartz powder block is vitrified to obtain quartz glass.

[0055] As can be understood, during the entire process of converting quartz powder into a quartz product (quartz glass), it does not come into contact with other materials, ensuring the high purity of the quartz product. Furthermore, through the dehydroxylation process, the non-metallic impurities (e.g., hydroxyl groups) in the quartz powder are controlled to an extremely low level of less than 1 ppm. Therefore, the methods provided in the embodiments of the present application for preparing high-purity quartz using quartz powder as a raw material can produce quartz products with high optical uniformity, low stress, low hydroxyl content, and high purity.

[0056] It is understood that "high purity" means that the purity of the high-purity quartz is greater than or equal to 99.99% (4N). Furthermore, the purity of the high-purity quartz can also be greater than or equal to 99.99999% (7N). Furthermore, the "high purity" refers to ultra-high purity with a metal impurity ion ppb level (parts per billion) purity greater than 99.999999% (8N).

[0057] like Figure 1 As shown, the embodiment of the present application provides a method for preparing quartz glass using quartz powder as raw material, which includes the following steps:

[0058] Step S1: providing quartz powder as an initial raw material.

[0059] It is understandable that the quartz powder can be natural quartz powder, high-purity synthetic quartz powder, and high-purity quartz waste powder generated during the deposition process.

[0060] Step S2: Pre-treating the initial raw material to obtain a statically pressed raw material containing quartz powder, wherein the pre-treatment at least includes the steps of screening the initial raw material and dehydroxylating the initial raw material.

[0061] It can be understood that the process of screening the initial raw material and the process of dehydroxylating the initial raw material can be two independent processes, corresponding to step S21 and step S22 respectively.

[0062] Step S21, the process of screening the initial raw materials includes:

[0063] The quartz powder is vibrated and sieved using a sieve to obtain silicon dioxide particles with a particle size of 50 nanometers to 300 micrometers.

[0064] In one embodiment, the silica particles have a particle size of 100 nanometers to 200 micrometers.

[0065] In one embodiment, the silica particles have a particle size of 1 micron to 100 microns.

[0066] In this embodiment, the particle size of the silicon dioxide particles can be 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, 100 nm, 150 nm, 200 nm, 250 nm, 300 nm, 350 nm, 400 nm, 450 nm, 500 nm, 550 nm, 600 nm, 650 nm, 700 nm, 750 nm, 800 nm, 850 nm, 900 nm, 950 nm, 1000 nm; 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 1000 nm; Micron, 10 micron, 11 micron, 12 micron, 13 micron, 14 micron, 15 micron, 16 micron, 17 micron, 18 micron, 19 micron, 20 micron, 21 micron, 22 micron, 23 micron, 24 micron, 25 micron, 26 micron, 27 micron, 28 micron, 29 micron, 30 micron, 31 micron, 32 micron, 33 micron, 34 micron, 35 micron, 36 micron, 37 micron, 38 micron, 39 micron, 40 micron, 41 micron, 42 micron, 43 micron, 44 micron, 45 micron, 46 micron, 47 micron, 48 microns, 49 microns, 50 microns, 51 microns, 52 microns, 53 microns, 54 microns, 55 microns, 56 microns, 57 microns, 58 microns, 59 microns, 60 microns, 61 microns, 62 microns, 63 microns, 64 microns, 65 microns, 66 microns, 67 microns, 68 microns, 69 microns, 70 microns, 71 microns, 72 microns, 73 microns, 74 microns, 75 microns, 76 microns, 77 microns, 78 microns, 79 microns, 80 microns, 81 microns, 82 microns, 83 microns, 84 microns, 85 microns, 86 microns 100 microns, 110 microns, 120 microns, 130 microns, 140 microns, 150 microns, 160 microns, 170 microns, 180 microns, 190 microns, 200 microns, 210 microns, 220 microns, 230 microns, 240 microns, 250 microns, 260 microns, 270 microns, 280 microns, 290 microns, 300 microns.

[0067] It is understandable that the purity of the high-purity quartz powder selected in this application is greater than or equal to 4N, and the preferred purity is greater than or equal to 7N. The high-purity quartz powder is vibrated and sieved to select quartz powder with a particle size that meets the requirements. The mesh of the vibrating screen is made of high-purity nylon, and the tray, cover and mesh of the sieve are all made of high-purity plastic. Preferably, an ultrasonic vibrating screen can be used to improve the dispersibility of the powder. During the screening process, by adjusting the aperture of the mesh, high-purity silicon dioxide particles with a particle size of 50nm to 300μm and high dispersibility are obtained. The preferred quartz powder particle size is 100nm to 200 microns, and the more preferred quartz powder particle size range is 1μm to 100μm. The highly dispersible high-purity silicon dioxide micropowder obtained after screening is poured into a high-purity quartz container for standby use.

[0068] Step S22: The step of dehydroxylating the initial raw material comprises:

[0069] placing quartz powder in a dehydroxylation furnace, evacuating the interior of the dehydroxylation furnace to a vacuum state, and controlling the vacuum degree in the dehydroxylation furnace to be less than 10 Pa;

[0070] The quartz powder in the dehydroxylation furnace is heated to remove the hydroxyl groups inside the quartz powder; and / or, the dehydroxylation temperature of the dehydroxylation furnace is controlled to be 500° C. to 1300° C.; and / or, the dehydroxylation holding time of the dehydroxylation furnace is controlled to be 10 hours to 100 hours.

[0071] In one embodiment, the vacuum degree in the dehydroxylation furnace is controlled to be less than 1 Pa; and / or the dehydroxylation temperature of the dehydroxylation furnace is controlled to be 700° C. to 1100° C.; and / or the dehydroxylation holding time of the dehydroxylation furnace is controlled to be 40 hours to 80 hours.

[0072] In this embodiment, the vacuum degree in the dehydroxylation furnace may be further controlled to be less than 0.1 Pa.

[0073] As you can understand, the quartz powder obtained by high-temperature hydrolysis of the silicon source contains a large amount of hydroxyl groups, which affect the properties of quartz glass. Therefore, controlling the hydroxyl content in quartz glass is particularly important. Quartz powder itself has a large specific surface area, and the diffusion rate of hydroxyl groups is faster than in quartz glass. Removing hydroxyl groups at this stage is an opportune time to control the hydroxyl content of the quartz glass block. Placing the quartz container containing the silica powder in a dehydroxylation furnace and evacuating the furnace interior for dehydroxylation effectively removes hydroxyl groups. The vacuum level in the dehydroxylation furnace is controlled to less than 10 Pa, preferably less than 1 Pa, and more preferably less than 0.1 Pa. High-temperature heating is used to promote the release of hydroxyl groups from the quartz particles, allowing the hydroxyl content in the quartz powder to be adjusted as needed. By adjusting parameters such as the vacuum furnace's holding temperature and holding time, the hydroxyl content in the quartz powder can be controlled to below 1 ppm. The dehydroxylation temperature in the dehydroxylation furnace is controlled to be 500° C. to 1300° C., preferably 700° C. to 1100° C.; and / or the dehydroxylation holding time in the dehydroxylation furnace is controlled to be 10 hours to 100 hours, preferably 40 hours to 80 hours.

[0074] In this embodiment, the calibration value for controlling the vacuum degree in the dehydroxylation furnace can further be 0.1Pa, 0.2Pa, 0.3Pa, 0.4Pa, 0.5Pa, 0.6Pa, 0.7Pa, 0.8Pa, 0.9Pa, 1Pa, 2Pa, 3Pa, 4Pa, 5Pa, 6Pa, 7Pa, 8Pa, 9Pa, and 10Pa.

[0075] In this embodiment, the dehydroxylation temperature of the dehydroxylation furnace for dehydroxylation can be specifically 500°C, 510°C, 520°C, 530°C, 540°C, 550°C, 560°C, 570°C, 580°C, 590°C, 600°C, 610°C, 620°C, 630°C, 640°C, 650°C, 660°C, 670°C, 680°C, 690°C, 700°C, 710°C, 720°C, 730°C, 740°C, 750°C, 760°C, 770°C, 780°C, 790°C, 800°C, 810°C, 820°C, 830°C, 840°C, 850°C, 860°C, 870°C, 880°C, 890°C, 900°C, ℃, 910℃, 920℃, 930℃, 940℃, 950℃, 960℃, 970℃, 980℃, 990℃, 1000℃, 1010℃, 1020℃, 1030℃, 1040℃, 1050℃, 1060℃, 1070℃, 1080℃, 1090℃, 1100℃, 1110℃, 1120℃, 1130℃, 1140℃, 1150℃, 1160℃, 1170℃, 1180℃, 1190℃, 1200℃, 1210℃, 1220℃, 1230℃, 1240℃, 1250℃, 1260℃, 1270℃, 1280℃, 1290℃, 1300℃.

[0076] In this embodiment, the dehydroxylation holding time for controlling the dehydroxylation furnace to perform dehydroxylation can be specifically 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, 18 hours, 19 hours, 20 hours, 21 hours, 22 hours, 23 hours, 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours, 30 hours, 31 hours, 32 hours, 33 hours, 34 hours, 35 hours, 36 hours, 37 hours, 38 hours, 39 hours, 40 hours, 41 hours, 42 hours, 43 hours, 44 hours, 45 hours, 46 hours, 47 hours, 48 ​​hours, 49 hours, 50 hours, 51 hours, 52 hours Hours, 53 hours, 54 hours, 55 hours, 56 hours, 57 hours, 58 hours, 59 hours, 60 hours, 61 hours, 62 hours, 63 hours, 64 hours, 65 hours, 66 hours, 67 hours, 68 hours, 69 hours, 70 hours, 71 hours, 72 hours, 73 hours, 74 hours, 75 hours, 76 hours, 77 hours, 78 hours, 79 hours, 80 hours, 81 hours, 82 hours, 83 hours, 84 hours, 85 hours, 86 hours, 87 hours, 88 hours, 89 hours, 90 hours, 91 hours, 92 hours, 93 hours, 94 hours, 95 hours, 96 hours, 97 hours, 98 hours, 99 hours, 100 hours.

[0077] In other embodiments, dehydroxylation can also be achieved by passing chlorine and air into the dehydroxylation furnace for a long time and sintering at high temperature. Those skilled in the art will understand that this is certainly feasible and will not be elaborated here.

[0078] Step S3: placing the statically pressed raw material in a static pressing device for static pressing to obtain a quartz powder block, wherein the parts of the static pressing device that are in contact with the quartz powder are all made of high-purity quartz material.

[0079] In one embodiment, the static pressure device includes a base and a plurality of static pressure components arranged around the base; the base and the plurality of static pressure components cooperate to form a static pressure cavity, which is used to accommodate quartz powder. The positions of the plurality of static pressure components relative to the base are adjustable so as to squeeze the quartz powder in the static pressure cavity; the surfaces of the base and the plurality of static pressure components that are in contact with the quartz powder are both made of high-purity quartz material.

[0080] In one embodiment, the static pressure of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 2 MPa to 15 MPa, and the holding time of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 5 minutes to 120 minutes; the density of the quartz powder block obtained by static pressure treatment in the static pressure device is controlled to be 0.2 g / cm 3 to 1.8g / cm 3 .

[0081] Furthermore, the static pressure of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 5MPa to 10MPa, and the holding time of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 30 minutes to 60 minutes; the density of the quartz powder block obtained by static pressure treatment in the static pressure device is controlled to be 0.5g / cm 3 to 0.6g / cm 3 .

[0082] Furthermore, the static pressure of the static pressure device for performing static pressure treatment on the static pressure raw material is controlled to be 6 MPa to 8 MPa.

[0083] It is understood that the static pressure device presses the quartz powder into a quartz powder body with a specific density. The static pressure is 2MPa to 15MPa, preferably 5MPa to 10MPa, and more preferably 6MPa to 8MPa. The static pressure holding time is 5 minutes to 120 minutes, preferably 30-60 minutes. The density of the obtained quartz powder block is 0.2g / cm 3 to 1.8g / cm 3 The preferred density range of the quartz powder block is 0.5 g / cm 3 to 0.6g / cm3 。

[0084] In this embodiment, the static pressure of controlling the static pressure device to perform static pressure treatment on the static pressure raw material can be specifically 2.0MPa, 2.1MPa, 2.2MPa, 2.3MPa, 2.4MPa, 2.5MPa, 2.6MPa, 2.7MPa, 2.8MPa, 2.9MPa, 3.0MPa, 3.1MPa, 3.2MPa, 3.3MPa, 3.4MPa, 3.5MPa, 3.6MPa, 3.7MPa, 3.8MPa, 3.9MPa, 4.0MPa, 4.1MPa, 4.2MPa, 4.3MPa, 4.4MPa, 4.5MPa, 4.6MPa, 4.7MPa, 4.8MPa, 4.9MPa, 5. 0MPa, 5.1MPa, 5.2MPa, 5.3MPa, 5.4MPa, 5.5MPa, 5.6MPa, 5.7MPa, 5.8MPa, 5.9MPa, 6.0MPa, 6.1MPa, 6.2MPa, 6.3MPa, 6.4MPa, 6.5MPa, 6.6MPa, 6.7MPa, 6 .8MPa, 6.9MPa, 7.0MPa, 7.1MPa, 7.2MPa, 7.3MPa, 7.4MPa, 7.5MPa, 7.6MPa, 7.7MPa, 7.8MPa, 7.9MPa, 8.0MPa, 8.1MPa, 8.2MPa, 8.3MPa, 8.4MPa, 8.5MPa, 8.6MPa, 8.7MPa, 8.8MPa, 8.9MPa, 9.0MPa, 9.1MPa, 9.2MPa, 9.3MPa, 9.4MPa, 9.5MPa, 9.6MPa, 9.7MPa, 9.8MPa, 9.9MPa, 10.0MPa, 10.1MPa, 10.2MPa, 10. 3MPa, 10.4MPa, 10.5MPa, 10.6MPa, 10.7MPa, 10.8MPa, 10.9MPa, 11.0MPa, 11.1MPa, 11.2MPa, 11.3MPa, 11.4MPa, 11.5MPa, 11.6MPa, 11.7MPa, 11.8MPa, 11.9MPa, 12.0MPa, 12.1MPa, 12.2MPa, 12.3MPa, 12.4MPa, 12.5MPa, 12.6MPa, 12.7MPa, 12.8MPa, 12.9MPa, 13.0MPa, 13.1MPa, 13.2MPa, 13.3MPa, 13.4M Pa, 13.5MPa, 13.6MPa, 13.7MPa, 13.8MPa, 13.9MPa, 14.0MPa, 14.1MPa, 14.2MPa, 14.3MPa, 14.4MPa, 14.5MPa, 14.6MPa, 14.7MPa, 14.8MPa, 14.9MPa, 15.0MPa.

[0085] In this embodiment, the holding time of controlling the static pressure device to perform static pressure treatment on the static pressure raw material can be specifically 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, 20 minutes, 21 minutes, 22 minutes, 23 minutes, 24 minutes, 25 minutes, 26 minutes, 27 minutes, 28 minutes, 29 minutes, 30 minutes, 31 minutes, 32 minutes, 33 minutes, 34 minutes, 35 minutes, 36 minutes, 37 minutes, 38 minutes, 39 minutes, 40 minutes, 41 minutes, 42 minutes, 43 minutes, 44 minutes, 45 minutes, 46 minutes, 47 minutes, 48 ​​minutes, 49 minutes, 50 minutes, 51 minutes, 52 minutes, 53 minutes, 54 minutes, 55 minutes, 56 minutes, 57 minutes, 58 minutes, 59 minutes, 60 minutes, and 61 minutes , 62 minutes, 63 minutes, 64 minutes, 65 minutes, 66 minutes, 67 minutes, 68 minutes, 69 minutes, 70 minutes, 71 minutes, 72 minutes, 73 minutes, 74 minutes, 75 minutes, 76 minutes, 77 minutes, 78 minutes, 79 minutes, 80 minutes, 81 minutes, 82 minutes, 83 minutes, 84 minutes, 85 minutes, 86 minutes, 87 minutes, 88 minutes, 89 minutes, 90 minutes, 91 minutes, 92 minutes, 93 minutes minutes, 94 minutes, 95 minutes, 96 minutes, 97 minutes, 98 minutes, 99 minutes, 100 minutes, 101 minutes, 102 minutes, 103 minutes, 104 minutes, 105 minutes, 106 minutes, 107 minutes, 108 minutes, 109 minutes, 110 minutes, 111 minutes, 112 minutes, 113 minutes, 114 minutes, 115 minutes, 116 minutes, 117 minutes, 118 minutes, 119 minutes, 120 minutes.

[0086] In this embodiment, the density of the obtained quartz powder block can be specifically 0.2 g / cm 3 , 0.3g / cm 3 , 0.4g / cm 3 , 0.5g / cm 3 , 0.6g / cm 3 , 0.7g / cm 3 , 0.8g / cm 3 , 0.9g / cm 3 , 1.0g / cm 3 , 1.1g / cm 3 , 1.2g / cm 3 , 1.3g / cm 3 , 1.4g / cm 3 , 1.5g / cm3 , 1.6g / cm 3 , 1.7g / cm 3 , 1.8g / cm 3 .

[0087] Further integration Figure 2 and Figure 3 FIG. 1 shows an example of a static pressure device 10 provided in an embodiment of the present application. In one embodiment, the static pressure device 10 includes a base 11 and a plurality of static pressure components 12 cooperating with the base 11. The base 11 and the plurality of static pressure components 12 cooperate to form a static pressure chamber 100, which is used to accommodate quartz powder. The plurality of static pressure components 12 are adjustable relative to the base 11 to compress the quartz powder within the static pressure chamber 100. The surfaces of the base 11 and the plurality of static pressure components 12 that come into contact with the quartz powder are all made of high-purity quartz.

[0088] In this embodiment, there are five static pressure components 12, forming a semi-enclosed structure and disposed on the same side of the base 11. Four of the static pressure components 12 are in contact with and surround the base 11, while the remaining static pressure component 12 is spaced apart from the base 11 and in contact with the four static pressure components 12. Each static pressure component 12 includes a pressure rod 121, a connecting push block 122, and a quartz compression gasket 123. The connecting push block 122 is connected to the end of the pressure rod 121 and is used to abut against the quartz compression gasket 123, thereby pushing the quartz compression gasket 123 inward to compress the spatial volume of the static pressure chamber 100 to achieve static pressure. The base 11 includes a support portion 111 and a quartz pad 112. Five quartz extrusion gaskets 123 and a quartz bottom 112 enclose a static pressure chamber 100 . Quartz powder is placed in the static pressure chamber 100 and contacts the quartz extrusion gaskets 123 and the quartz bottom 112 . Multiple pressing rods 121 push and extrude the quartz powder inward to form a quartz powder block 20 .

[0089] As will be understood, the static pressure device 10 consists of five static pressure components 12 (front, rear, left, right, and top) and a base 11 embedded with a quartz plate. During operation, after the surrounding static pressure components 12 are fixed in place, quartz powder is evenly poured into the static pressure chamber 100 and extruded. The surrounding pressure rods 121 may be equipped with or connected to pressure sensors (not shown) to simultaneously provide pressure to maintain the static pressure components 12 in their working positions. After the extrusion state is maintained for a certain period of time to allow the quartz powder to bind tightly, the surrounding and top static pressure components 12 are sequentially removed to form a formed quartz powder block 20. The density of the extruded material can be controlled by adjusting the height of the extruded material.

[0090] For ease of understanding, Figure 2The base 11 and static pressure component 12 are shown as regular shapes to illustrate their essential structures; those skilled in the art will appreciate that the base 11 and static pressure component 12 may also have other shapes. Furthermore, the specific connection relationship between the pressure rod 121, the connecting push block 122, and the quartz compression gasket 123 is not limited, nor is the specific connection relationship between the support portion 111 and the quartz base 112.

[0091] Furthermore, the embodiment of the present application provides a method for preparing quartz glass using quartz powder as a raw material, in which a static pressure device 10 is used to statically press the quartz powder. The five quartz extrusion gaskets 123 and a quartz bottom 112 of the static pressure device 10 that are in contact with the quartz powder are all made of quartz material. The quartz powder will not contact containers of other materials during the vitrification process, thereby avoiding the introduction of impurity ions, so that the formed quartz product has high uniformity, low stress, low hydroxyl and other characteristics.

[0092] Furthermore, if containers are introduced during the molding process to hold quartz powder, these containers can be metal capsules or glass capsules. However, metal and ordinary glass capsules can introduce other elements that affect the properties of the quartz glass. While quartz glass capsules generally do not introduce other elements, the quartz glass capsule material itself is relatively brittle, posing production risks. Furthermore, the volume of quartz glass capsules is typically fixed, making it difficult to adapt to actual production needs. However, the five quartz extrusion gaskets 123 and one quartz pad 112 in the static pressure device 10 provided in the embodiment of the present application are movable, allowing the volume of the static pressure chamber 100 to be adjusted as the static pressure is applied. This, on the one hand, prevents the introduction of other impurity ions and ensures the excellent properties of the quartz glass. On the other hand, it makes the production process more flexible, improves production efficiency, and further ensures the excellent characteristics of the quartz glass. As a result, the quartz glass obtained in the embodiment of the present application has superior properties compared to conventional quartz glass products of ordinary purity.

[0093] Step S4: placing the quartz powder block in a container whose contact surface is high-purity quartz, and vitrifying the quartz powder block to obtain quartz glass.

[0094] In one embodiment, the vitrification temperature of the quartz powder block is controlled to be in a range of 1350° C. to 1500° C., and the vitrification time of the quartz powder block is controlled to be in a range of 10 hours to 90 hours.

[0095] In one embodiment, the vitrification temperature range of the vitrification of the quartz powder block is controlled to be 1400° C. to 1480° C., and the vitrification time range of the vitrification of the quartz powder block is controlled to be 40 hours to 60 hours.

[0096] As can be appreciated, placing the quartz powder block in a quartz container lined with high-purity quartz sand can prevent the introduction of impurities during the vitrification process, and the presence of quartz sand can effectively prevent adhesion between the quartz glass and the container. The vitrification temperature range is 1350°C to 1500°C, preferably 1400°C to 1480°C; the vitrification time is 10 to 90 hours, preferably 40 to 60 hours.

[0097] In this embodiment, the glass transition temperature for controlling the vitrification of the quartz powder block can be specifically 1350°C, 1360°C, 1370°C, 1380°C, 1390°C, 1400°C, 1410°C, 1420°C, 1430°C, 1440°C, 1450°C, 1460°C, 1470°C, 1480°C, 1490°C, or 1500°C.

[0098] In this embodiment, the vitrification time for controlling the vitrification of the quartz powder block can be specifically 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, 18 hours, 19 hours, 20 hours, 21 hours, 22 hours, 23 hours, 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours, 30 hours, 31 hours, 32 hours, 33 hours, 34 hours, 35 hours, 36 hours, 37 hours, 38 hours, 39 hours, 40 hours, 41 hours, 42 hours, 43 hours, 44 hours, 45 hours, 46 hours, 47 hours, 48 ​​hours, 49 hours, 50 hours, 51 hours, 52 hours, 53 hours, 54 hours, 55 hours, 56 hours, 57 hours, 58 hours, 59 hours, 60 hours, 61 hours, 62 hours, 63 hours, 64 hours, 65 hours, 66 hours, 67 hours, 68 hours, 69 hours, 70 hours, 71 hours, 72 hours, 73 hours, 74 hours, 75 hours, 76 hours, 77 hours, 78 hours, 79 hours, 80 hours, 81 hours, 82 hours, 83 hours, 84 hours, 85 hours, 86 hours, 87 hours, 88 hours, 89 hours, hours, 48 ​​hours, 49 hours, 50 hours, 51 hours, 52 hours, 53 hours, 54 hours, 55 hours, 56 hours, 57 hours, 58 hours, 59 hours, 60 hours, 61 hours, 62 hours, 63 hours, 64 hours, 65 hours, 66 hours, 67 hours, 68 hours, 69 hours, 70 hours, 71 hours, 72 hours, 73 hours, 74 hours, 75 hours, 76 hours, 77 hours, 78 hours, 79 hours, 80 hours, 81 hours, 82 hours, 83 hours, 84 hours, 85 hours, 86 hours, 87 hours, 88 hours, 89 hours, 90 hours.

[0099] The present invention provides a method for producing high-purity quartz using quartz powder as raw material. During the entire process of converting the quartz powder into a quartz product (quartz glass), the quartz powder does not come into contact with other materials, ensuring the high purity of the quartz product. Furthermore, through a dehydroxylation process, the non-metallic impurities (e.g., hydroxyl groups) in the quartz powder are controlled to an extremely low level of less than 1 ppm. Furthermore, the high-purity quartz is produced using a vitrification route using the two-step VAD method (a common route for producing high-performance quartz glass). This results in a quartz glass product with high uniformity and low stress.

[0100] Therefore, the embodiment of the present application provides a method for preparing high-purity quartz using quartz powder as raw material, which can obtain a quartz product with high optical uniformity, low stress, low hydroxyl content, and high purity.

[0101] The embodiment of the present application also provides a quartz product, which is prepared by the quartz glass preparation method using quartz powder as raw material as described in any one of the above embodiments.

[0102] Furthermore, the quartz glass preparation method using quartz powder as raw material provided in the embodiments of the present application can obtain high-purity quartz products. On the one hand, by dispersing, screening and dehydroxylating the quartz powder, the hydroxyl content of the powder is controlled, thereby controlling the hydroxyl content of the quartz glass, and the preparation of quartz glass with a hydroxyl content of less than 1 ppm can be achieved. On the other hand, the quartz powder is statically pressed using a static pressure device whose parts in contact with the quartz powder are all made of quartz material, avoiding the introduction of impurities due to contact, and pressing out quartz powder blocks with specific specifications and specific densities. On the other hand, the present application adopts a process imitating a two-step method to prepare high-purity synthetic quartz glass in a non-melting environment. The product has the characteristics of high purity, low hydroxyl group, low stress, high optical uniformity, no bubbles, and no streaks.

[0103] As can be appreciated, the quartz products provided herein exhibit superior performance compared to conventional quartz glass products of standard purity. The quartz products provided herein are characterized by high purity. The high-purity quartz powder selected herein has a purity of greater than or equal to 99.99% (4N), preferably greater than or equal to 99.99999% (7N). This "high purity" specifically refers to an ultra-high purity level of greater than 99.999999% (8N) for metal impurity ions at the ppb (parts per billion) level. Furthermore, the quartz products provided herein exhibit excellent properties such as high optical uniformity, low stress, and low hydroxyl content.

[0104] Example 1:

[0105] Using natural silica powder with a purity of 99.995%, quartz powder particles with a particle size of 50 nanometers to 300 microns were selected after vibration screening. The vacuum degree was evacuated to 8Pa in a vacuum furnace, and the temperature was raised to 800℃ over 2 hours and sintered for 70 hours to remove the hydroxylation. The powder was pressed at a pressure of 5MPa for 30 minutes to a density of 0.7g / cm 3 A quartz powder block with a three-dimensional size of 40cm x 40cm x 20cm was heated to 1400 degrees Celsius for 10 hours and sintered for 30 hours to obtain a quartz glass block. After processing, a quartz glass block with a three-dimensional size of 25cm x 25cm x 12cm was obtained. The metal impurity content was 53ppm; the hydroxyl content was less than 1ppm; there were no streaks or bubbles inside the product; and the optical uniformity was 6.3×10-6 ; Stress birefringence 2.1nm / cm.

[0106] Example 2:

[0107] Using natural silica powder with a purity of 99.995%, after vibration screening, quartz powder particles with a particle size of 100 nanometers to 200 microns were selected; the vacuum degree was evacuated to 5Pa in a vacuum furnace, and the temperature was raised to 1000℃ in a vacuum furnace for 2 hours and sintered for 70 hours to remove hydroxylation; the powder was pressed at a pressure of 5MPa for 25 minutes to a density of 0.6g / cm 3 A quartz powder block with a three-dimensional size of 40cm x 40cm x 20cm was heated to 1450 degrees Celsius for 10 hours and sintered for 40 hours to obtain a quartz glass block. After processing, a quartz glass block with a three-dimensional size of 25cm x 25cm x 12cm was obtained. The metal impurity content was 51ppm; the hydroxyl content was less than 1ppm; there were no streaks or bubbles inside the product; and the optical uniformity was 4.8×10 -6 ; Stress birefringence 1.9nm / cm.

[0108] Example 3:

[0109] High-purity silicon dioxide waste powder with a purity higher than 99.99999% produced by the deposition process is used. After vibration screening, quartz powder particles with a particle size of 100 nanometers to 200 microns are selected. The vacuum degree is evacuated to 5Pa in a vacuum furnace, and the temperature is raised to 1000℃ in a vacuum furnace for 2 hours and sintered for 80 hours to remove hydroxylation. The powder is pressed at a pressure of 5MPa for 25 minutes to a density of 0.53g / cm 3 A quartz powder block with a three-dimensional size of 40cm x 40cm x 20cm was heated to 1450 degrees Celsius for 10 hours and sintered for 40 hours to obtain a quartz glass block. After processing, a quartz glass block with a three-dimensional size of 25cm x 25cm x 12cm was obtained. The metal impurity content was 9.8ppb; the hydroxyl content was less than 1ppm; there were no streaks or bubbles inside the product; and the optical uniformity was 3.9×10 -6 ; Stress birefringence 1.5nm / cm.

[0110] Example 4:

[0111] Using high-purity synthetic silica powder with a purity higher than 99.999995%, after vibration screening, quartz powder particles with a particle size of 100 nanometers to 100 microns were selected; the vacuum degree was evacuated to 1Pa in a vacuum furnace, and the temperature was raised to 1000℃ in a vacuum furnace for 2 hours and sintered for 60 hours to remove hydroxylation; the powder was pressed at a pressure of 8MPa for 60 minutes to a density of 1.2g / cm 3A quartz powder block with a three-dimensional size of 40cm x 40cm x 20cm was heated to 1500 degrees Celsius for 10 hours and sintered for 40 hours to obtain a quartz glass block. After processing, a quartz glass block with a three-dimensional size of 30cm x 30cm x 15cm was obtained. The metal impurity content was 8.2ppb; the hydroxyl content was less than 1ppm; there were no streaks or bubbles inside the product; and the optical uniformity was 3.6×10 -6 ; Stress birefringence 1.9nm / cm.

[0112] Example 5:

[0113] Using high-purity synthetic silica powder with a purity higher than 99.999995%, quartz powder particles with a particle size of 1 micron to 100 microns were selected after vibration screening; the vacuum degree was evacuated to 0.1Pa in a vacuum furnace, and the temperature was raised to 1100℃ in a vacuum furnace for 4 hours and sintered for 40 hours to remove hydroxylation; the powder was pressed at a pressure of 8MPa for 20 minutes to a density of 0.58g / cm 3 A quartz powder block with a three-dimensional size of 40cm x 40cm x 40cm was heated to 1480 degrees Celsius for 20 hours and sintered for 60 hours to obtain a quartz glass block. After processing, a quartz glass block with a three-dimensional size of 20cm x 20cm x 20cm was obtained. The metal impurity content was 5.9ppb; the hydroxyl content was less than 1ppm; there were no streaks or bubbles inside the product; and the optical uniformity was 3.4×10 -6 ; Stress birefringence 1.1nm / cm.

[0114] The specific embodiments of the present application have been described above with reference to the accompanying drawings. However, those skilled in the art will appreciate that various modifications and substitutions may be made to the specific embodiments of the present application without departing from the scope of the present application. Such modifications and substitutions are within the scope of the present application.

Claims

1. A method for preparing quartz glass using quartz powder as raw material, characterized in that: The steps include: Providing quartz powder as a starting material; Pre-treating the initial raw material to obtain a static pressing raw material containing quartz powder, the pre-treatment comprising at least a step of screening the initial raw material and a step of dehydroxylating the initial raw material, wherein the step of screening the initial raw material obtains silicon dioxide particles having a particle size of 50 nanometers to 300 micrometers, and dehydroxylating the quartz powder in a vacuum state of less than 10 Pa and at a dehydroxylating temperature of 500° C. to 1300° C.; Transferring the statically pressed raw material to a static pressing device for static pressing treatment to obtain a quartz powder block, wherein the parts of the static pressing device that are in contact with the quartz powder are all made of quartz material, and controlling the static pressure of the static pressing device to perform static pressing treatment on the static pressed raw material to be 2 MPa to 15 MPa; The quartz powder block is placed in a container whose contact surface is high-purity quartz, and the quartz powder block is vitrified to obtain quartz glass, wherein the purity of the high-purity quartz is greater than or equal to 99.99%.

2. The method for preparing quartz glass using quartz powder as raw material according to claim 1, wherein: The process of screening the initial raw materials comprises: The quartz powder is vibrated and sieved using a sieve to obtain the silicon dioxide particles.

3. The method for preparing quartz glass using quartz powder as raw material according to claim 2, wherein: The particle size of the silicon dioxide particles is 100 nanometers to 200 micrometers.

4. The method for preparing quartz glass using quartz powder as raw material according to claim 1, wherein: The process of dehydroxylating the initial raw material comprises: placing the quartz powder in a dehydroxylation furnace, and evacuating the interior of the dehydroxylation furnace to the vacuum state; The quartz powder in the dehydroxylation furnace is heated to remove the hydroxyl groups in the quartz powder, and the dehydroxylation holding time of the dehydroxylation furnace is controlled to be 10 hours to 100 hours.

5. The method for preparing quartz glass using quartz powder as raw material according to claim 4, wherein: Controlling the vacuum degree in the dehydroxylation furnace to be less than 1 Pa; The dehydroxylation temperature of the dehydroxylation furnace is controlled to be 700° C. to 1100° C., and the dehydroxylation holding time of the dehydroxylation furnace is controlled to be 40 hours to 80 hours.

6. The method for preparing quartz glass using quartz powder as raw material according to claim 1, wherein: The static pressure device is controlled to perform static pressure treatment on the static pressure raw material for a holding time of 5 minutes to 120 minutes; the density of the quartz powder block obtained by static pressure treatment in the static pressure device is controlled to be 0.2 g / cm 3 to 1.8g / cm 3 .

7. The method for preparing quartz glass using quartz powder as raw material according to claim 6, wherein: The static pressure of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 5MPa to 10MPa, and the holding time of the static pressure device for static pressure treatment of the static pressure raw material is controlled to be 30 minutes to 60 minutes; the density of the quartz powder block obtained by static pressure treatment in the static pressure device is controlled to be 0.5g / cm 3 to 0.6g / cm 3 .

8. The method for preparing quartz glass using quartz powder as raw material according to claim 1, wherein: The static pressure device includes a base and a plurality of static pressure components cooperating with the base; The base cooperates with the plurality of static pressure components to form a static pressure cavity, the static pressure cavity is used to accommodate the quartz powder, and the positions of the plurality of static pressure components relative to the base are adjustable to squeeze the quartz powder in the static pressure cavity; The surfaces of the base and the plurality of static pressure components that are in contact with the quartz powder are all made of the high-purity quartz.

9. The method for preparing quartz glass using quartz powder as raw material according to claim 1, wherein: The vitrification temperature range of the vitrification of the quartz powder block is controlled to be 1350° C. to 1500° C., and the vitrification time of the vitrification of the quartz powder block is controlled to be 10 hours to 90 hours.

10. The method for preparing quartz glass using quartz powder as raw material according to claim 9, wherein: The vitrification temperature range of the vitrification of the quartz powder block is controlled to be 1400° C. to 1480° C., and the vitrification time of the vitrification of the quartz powder block is controlled to be 40 hours to 60 hours.

Citation Information

Patent Citations

  • Manufacture of transparent surface layer-containing silica glass component involves casting slurry of silica particles and liquid, cooling, drying obtained frozen material by heating, sintering, and sealing

    DE102011120932A1

  • Method of manufacturing a silica glass block

    EP2050724A1

  • Production of a silica glass article in a suspended sintered crucible

    EP3390306A2

  • Vacuum furnace and quartz glass preparation method

    CN112830666A