A preparation method of colored quartz glass and colored quartz glass

Through the sol-gel method combined with multiple colorant soaking and low-temperature calcination, the problems of complex preparation process and high energy consumption of traditional colored quartz glass are solved, and the low-cost mass production of colored quartz glass with uniform coloring is achieved, which is suitable for optical systems.

CN114380495BActive Publication Date: 2025-08-08YLX INC
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Patent Information

Application Number
CN202011112346.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-10-16
Publication Date
2025-08-08
Estimated Expiration
2040-10-16

AI Technical Summary

Technical Problem

Traditionally, the process of preparing colored quartz glass is complicated, the energy consumption is high, the cost is high, and it is difficult to achieve uniform coloring.

Method used

The nano-silica dispersion and silica sol are prepared by the sol-gel method. After the gel is cured and molded, the colorant is soaked and calcined at low temperatures. The solution injection molding is integrated to avoid high-temperature smelting and drawing processes.

Benefits of technology

The process flow is simplified, energy consumption is reduced, and it is uniform in coloring, suitable for optical systems in lighting and projection.

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Abstract

The present application discloses a method for preparing colored quartz glass and colored quartz glass, the method comprising: preparing a nano-silica dispersion and a silica sol; adding the silica sol to the nano-silica dispersion and mixing them evenly; pouring the mixed solution into a pre-formed mold for gel curing, and demolding to obtain a wet gel block; soaking the wet gel block in a colorant, and drying to obtain a dry gel; calcining the dry gel to obtain a dry silica block; soaking the dry silica block in a colorant, and drying, calcining, and cooling to obtain colored quartz glass. Through the above-mentioned method, the present application can simplify the production process, reduce energy consumption, and obtain a uniformly colored colored quartz glass.
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Description

Technical Field

[0001] The present application relates to the field of optical technology, and in particular to a method for preparing quartz glass and colored quartz glass. Background Art

[0002] Quartz glass, with its low thermal expansion coefficient, high temperature resistance, and ultraviolet and infrared transmittance, has been widely used in fiber optic communications, electronic light sources, chemical instrumentation, and aerospace. Colored quartz glass is also used as filter glass in some lasers due to its excellent uniformity, high transmittance, strong pressure and high temperature resistance, and wide filtering range. Colored quartz glass is also widely used in infrared heating components. Traditional transparent or milky white quartz glass, while fast heating and excellent insulation properties, lacks a high-end visual appeal due to its monotonous color.

[0003] Currently, the mainstream process for preparing colored quartz glass is to dope quartz sand with trace metal elements and metal oxides for mixing, and then melt and draw the mixed material at 1800-2200°C to produce colored quartz glass. However, the quartz sand doping process is relatively complex, requiring the rare earth elements and metal oxides to be dissolved and soaked in strong acids, followed by baking and high-temperature expansion treatment, followed by screening and magnetic separation, and finally high-temperature melting and drawing. This process has disadvantages such as complex procedures, high energy consumption, and high cost. Summary of the Invention

[0004] In response to the above technical problems, the present application provides a method for preparing colored quartz glass. The method has simple procedures, low energy consumption, can be integrally formed, and can mass-produce colored quartz glass with complex structures. The prepared colored quartz glass has uniform coloring and excellent performance, and is suitable for optical systems in lighting and projection.

[0005] To solve the above technical problems, the technical solution adopted in the present application is to provide a method for preparing colored quartz glass, which comprises: preparing a nano-silica dispersion and a silica sol; adding the silica sol to the nano-silica dispersion and mixing them evenly; pouring the mixed solution into a pre-formed mold to gel and solidify, and demolding to obtain a wet gel block; soaking the wet gel block in a colorant, and then drying it to obtain a dry gel; calcining the dry gel to obtain a loose and porous silica dry block; soaking the silica dry block in a colorant, and then drying, calcining, and cooling it to obtain colored quartz glass.

[0006] In one embodiment, the dry silicon dioxide block is immersed in the colorant once or multiple times. It is understood that the number of immersions and the ratio of the colorant used in each immersion can be adjusted according to the demand for different colors or color depths.

[0007] In one implementation, the step of preparing the nano-silicon dioxide dispersion includes: preparing the nano-silicon dioxide dispersion using nano-silicon dioxide powder, deionized water, and a dispersant.

[0008] Furthermore, the mass fraction of the nano-silicon dioxide powder is 15 to 30 parts, the impurity content of the nano-silicon dioxide powder is less than 30 ppm, and the specific surface area is 50 to 300 m 2 / g; the mass fraction of deionized water is 70 to 85 parts, the dispersant accounts for 0.1% to 5% of the total mass of the nano-silica powder and deionized water, and the dispersant includes at least one of ethylene glycol and glycerol.

[0009] In one implementation, the step of preparing the silica sol includes: mixing ethyl orthosilicate, deionized water, and hydrochloric acid solution, stirring for a preset time, and then adding an ammonia solution to adjust the pH value to generate the silica sol.

[0010] Furthermore, the mass fraction of ethyl orthosilicate is 15 to 30 parts, the mass fraction of deionized water is 20 to 45 parts, the concentration of the hydrochloric acid solution is 0.1 mol / L, the mass fraction thereof is 5 to 15 parts, the preset time is 30 to 90 minutes, the concentration of the ammonia solution is 1 mol / L; and the pH value of the silica sol is 3 to 5.

[0011] In one implementation, the step of calcining the dry gel to obtain a dry silica block includes placing the dry gel in an atmosphere furnace, introducing high-purity oxygen, and calcining at a temperature of 400-800° C. for 4-10 hours to obtain a dry silica block.

[0012] In one implementation, the steps of soaking a dried silica block in a colorant, drying, calcining, and cooling to obtain colored quartz glass include: immersing the dried silica block in the colorant, evacuating the colorant until there are no bubbles, and soaking for 1 to 24 hours; drying the soaked dried silica block, placing it in an atmosphere furnace, introducing high-purity oxygen, heating it to 400 to 800° C., and calcining it at this temperature for 2 to 10 hours; then switching the gas atmosphere to a helium atmosphere, heating it to 1100 to 1300° C., calcining it at this temperature for 4 to 20 hours, and cooling it to obtain the colored quartz glass.

[0013] In one implementation, the colorant is prepared in the following proportions by mass: 100 parts of deionized water, 0.01 to 0.8 parts of cerium nitrate, 0.01 to 0.6 parts of copper chloride, 0.01 to 0.5 parts of ferric chloride, 0.01 to 0.4 parts of aluminum nitrate, 0.2 to 0.4 parts of manganese chloride, and 0.3 to 0.8 parts of potassium dichromate.

[0014] The colorant with this mass ratio can dye the wet gel block and the dry silicon dioxide block black to produce black light-absorbing quartz glass.

[0015] In one implementation, the colorant is prepared in the following proportions by mass: 100 parts of deionized water, 15 to 30 parts of ethanol, 0.01 to 0.1 parts of aluminum nitrate, 0.01 to 0.5 parts of potassium nitrate, 0.01 to 0.5 parts of ferric chloride, 0.01 to 0.05 parts of copper chloride, 0.2 to 0.4 parts of manganese chloride, 0.02 to 0.5 parts of samarium chloride, 0.01 to 1 parts of butyl titanate, and 0.3 to 0.8 parts of potassium dichromate.

[0016] The colorant with this mass ratio can be used to dye the wet gel block and the dry silicon dioxide block green to produce green quartz glass.

[0017] In one implementation, the colorant includes a first colorant and a second colorant.

[0018] The step of soaking the wet gel block in a colorant includes: soaking the wet gel block in a first colorant, wherein the mass ratio of the first colorant is 100 parts of deionized water, 0.01 to 3 parts of cadmium sulfate octahydrate, 0.01 to 0.8 parts of tin chloride dihydrate, 0.01 to 0.5 parts of manganese chloride and 0.01 to 0.4 parts of ferric chloride.

[0019] The step of soaking the dry silicon dioxide block in a colorant includes soaking the dry silicon dioxide block in a second colorant, wherein the mass ratio of the second colorant is 100 parts of deionized water, 10 parts of hydrochloric acid, 1 to 3 parts of cuprous oxide, 1 to 4 parts of antimony oxide, 2 to 4 parts of samarium chloride and 0.1 to 3 parts of aluminum chloride.

[0020] By controlling the mass ratio of the first colorant to the second colorant, the wet gel block and the dry silicon dioxide block can be dyed into corresponding colors, and finally red quartz glass can be produced.

[0021] In one implementation, the colorant includes a first colorant, a second colorant, and a third colorant.

[0022] The step of soaking the wet gel block in a colorant includes: first soaking the wet gel block in a first colorant, and then soaking the wet gel block in a second colorant, wherein the mass ratio of the first colorant is 100 parts of deionized water, 5 to 8 parts of europium nitrate, 0.5 to 4 parts of sodium nitrate, 3 to 5 parts of yttrium nitrate and 0.01 to 0.4 parts of aluminum nitrate, and the mass ratio of the second colorant is 100 parts of deionized water, 2 to 4 parts of lanthanum chloride and 0.3 to 0.8 parts of sodium metavanadate.

[0023] The step of soaking the dry silicon dioxide block in a colorant includes soaking the dry silicon dioxide block in a third colorant, wherein the mass ratio of the third colorant is 100 parts of deionized water, 10-20 parts of concentrated hydrochloric acid solution and 3-8 parts of vanadium pentoxide.

[0024] By controlling the mass ratio of the first colorant, the second colorant and the third colorant, the wet gel block and the dry silicon dioxide block can be dyed into corresponding colors, and finally yellow ultraviolet-filtering quartz glass can be produced.

[0025] In order to solve the above technical problems, another technical solution adopted in the present application is to provide a colored quartz glass, which is a colored quartz glass produced by the above-mentioned preparation method of colored quartz glass.

[0026] Through the above scheme, the beneficial effects of the present application are as follows: the technical solution of the present application first forms a wet gel block by the sol-gel method, the wet gel block is first colored and then dried and calcined to obtain a loose and porous silica dry block with a certain color, and then the dry block is soaked with a colorant. The soaked silica dry block is dried, calcined, and cooled to obtain colored quartz glass. The present application combines the coloring process with the sol-gel molding technology. The wet gel block can be obtained by solution injection molding and then a two-step soaking and coloring operation is performed. This can effectively avoid the problem of the colorant salt solution hindering the gel and the cracking during the gel drying process. It can mass-produce colored quartz glass of various sizes at a lower temperature without the need for melting or high-temperature drawing processes. It has the advantages of simple process, low cost, low energy consumption and uniform coloring. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present application. For those skilled in the art, other drawings can be obtained based on these drawings without inventive efforts. Among them:

[0028] Figure 1 This is a schematic flow chart of an embodiment of a method for preparing quartz glass provided in this application;

[0029] Figure 2 Schematic diagram of the structure of an embodiment of quartz glass provided by this application. DETAILED DESCRIPTION

[0030] The following will be combined with the accompanying drawings in the embodiments of this application to clearly and completely describe the technical solutions in the embodiments of this application. Obviously, the embodiments described are only part of the embodiments of this application, not all of them. Based on the embodiments of this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0031] The present application provides a method for preparing colored quartz glass, which can combine the coloring process with the sol-gel forming technology, greatly simplifying the complicated process of quartz sand coloring in the traditional process. It does not require processes such as melting and high-temperature drawing, can reduce energy consumption, and can mass-produce various colored quartz glasses with uniform overall coloring.

[0032] See also Figure 1 , Figure 1 1 is a flow chart of an embodiment of a method for preparing quartz glass provided in the present application, the method comprising:

[0033] Step 11: Prepare nano-silica dispersion and silica sol.

[0034] High-purity fumed nano-silica powder with an impurity content of less than 30 ppm can be used to prepare a nano-silica dispersion; after mixing and stirring ethyl orthosilicate, deionized water and hydrochloric acid solution for a certain period of time, a certain amount of ammonia solution is added to prepare a silica sol; specifically, 15 to 30 parts of high-purity fumed nano-silica powder, 70 to 85 parts of deionized water and a dispersant can be used to prepare a nano-silica dispersion, wherein the specific surface area of the high-purity fumed nano-silica powder is 50 to 300 m 2 / g, the dispersant comprising at least one of ethylene glycol and glycerol; 15-30 parts of ethyl orthosilicate, 20-45 parts of deionized water, and 5-15 parts of a 0.1 mol / L hydrochloric acid solution are mixed and stirred for 30-90 minutes, followed by the addition of a 1 mol / L aqueous ammonia solution in an amount such that the pH of the resulting silica sol is 3-5. The parts described herein are by mass.

[0035] Step 12: Add silica sol to nano-silica dispersion and mix evenly. Pour the mixed solution into a preformed mold for gel solidification, and demould to obtain a wet gel block.

[0036] The silica sol is added to the nano-silica dispersion, and after being evenly mixed, the mixed solution is injected into a pre-formed mold. After the gel is solidified, it can be separated from the pre-formed mold to obtain a wet gel block.

[0037] Step 13: Soak the wet gel block in a colorant and then dry it to obtain a dry gel.

[0038] The wet gel block is immersed in a colorant of a certain concentration. The colorant is a hydrochloric acid solution containing one rare earth element, or a mixed hydrochloric acid solution containing at least two rare earth elements. The rare earth element can be titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, neodymium or samarium. After the wet gel block is immersed in the colorant for a certain period of time, the wet gel block can be taken out and placed in a constant temperature and humidity chamber for drying.

[0039] Step 14: calcining the dry gel to obtain a dry silicon dioxide block.

[0040] The dried dry gel is placed in an atmosphere furnace, introduced with high-purity oxygen, and calcined at a temperature of 400-800°C for 4-10 hours to obtain a loose and porous silica dry embryo block with a certain color, namely, a silica dry embryo.

[0041] Step 15: Soak the dry silicon dioxide block in a colorant, and then dry, calcine, and cool to obtain colored quartz glass.

[0042] The dried silica block is immersed in the colorant, vacuumed until the colorant is free of bubbles, and soaked for 1 to 24 hours. It can be understood that this step can be repeated multiple times, and the ratio or concentration of the colorant, soaking time and number of soaking times can be adjusted according to the demand for different colors or color depths.

[0043] The soaked dry silica block is then placed in an oven for drying. After drying, it is placed in an atmosphere furnace, introduced with high-purity oxygen, heated to 400-800°C, and kept warm for calcination for 2-10 hours. The gas is then switched to a helium atmosphere, heated to 1100-1300°C, kept warm for calcination for 4-20 hours, and cooled to obtain uniformly colored quartz glass.

[0044] The above scheme can be used to prepare quartz glass of various colors, such as black light-absorbing quartz glass, yellow ultraviolet-filtering quartz glass, red quartz glass, or green quartz glass. The production process of quartz glass of various colors is similar, and the specific production process will be described below.

[0045] In a specific embodiment, the colored quartz glass is black light-absorbing quartz glass, and the following steps can be used to prepare the black light-absorbing quartz glass:

[0046] a) preparing a nano-silica dispersion using 15 to 30 parts of high-purity fumed nano-silica powder having an impurity content of less than 30 ppm, 70 to 85 parts of deionized water, and a dispersant, wherein the dispersant accounts for 0.1% to 5% of the total mass of the high-purity fumed nano-silica powder and the deionized water, and is at least one of ethylene glycol and glycerol.

[0047] b) mixing 15 to 30 parts of ethyl orthosilicate, 20 to 45 parts of deionized water, and 5 to 15 parts of a 0.1 mol / L hydrochloric acid solution and stirring for 30 to 90 minutes, and then adding a certain amount of a 1 mol / L ammonia solution to adjust the pH value of the mixed silica sol to 3 to 5.

[0048] c) adding the silica sol of step (b) to the nano-silica dispersion of step (a), mixing them evenly, and then introducing them into the cavity of a preforming mold and allowing them to stand.

[0049] d) After the gel is solidified, the gel is separated from the preformed mold to obtain a wet gel block.

[0050] e) soaking the wet gel block in a colorant of a certain concentration, wherein the colorant is composed of the following proportions by weight: 100 parts of deionized water, 0.01-0.8 parts of cerium nitrate, 0.01-0.6 parts of copper chloride, 0.01-0.5 parts of ferric chloride, 0.01-0.4 parts of aluminum nitrate, 0.2-0.4 parts of manganese chloride, and 0.3-0.8 parts of potassium dichromate.

[0051] f) soaking the wet gel block in a colorant for a certain period of time, and then drying it in a constant temperature and humidity chamber to obtain a dry gel.

[0052] g) placing the dry gel in an atmosphere furnace, introducing high-purity oxygen, and calcining at a temperature of 400-800° C. for 4-10 hours to form a loose and porous silica dry block with a certain color.

[0053] h) Immerse the dry silicon dioxide block in the colorant, evacuate the colorant until there are no bubbles, and soak for 1 to 24 hours.

[0054] This step can be repeated multiple times, and the concentration of the colorant, soaking time and number of soaking times can be adjusted according to the requirements of color depth.

[0055] i) The soaked dried silica block is first placed in an oven for drying, then placed in an atmosphere furnace, introduced with high-purity oxygen, heated to 400-800° C., and calcined at this temperature for 2-10 hours; then the gas atmosphere is switched to helium, the temperature is raised to 1100-1300° C., and calcined at this temperature for 4-20 hours. After cooling, uniformly colored black light-absorbing quartz glass is obtained.

[0056] In another specific embodiment, the quartz glass is green quartz glass, and the preparation of the green quartz glass comprises the following steps:

[0057] a) preparing a nano-silica dispersion using 15 to 30 parts of high-purity fumed nano-silica powder having an impurity content of less than 30 ppm, 70 to 85 parts of deionized water, and a dispersant, wherein the dispersant accounts for 0.1% to 5% of the total mass of the high-purity fumed nano-silica powder and the deionized water, and is at least one of ethylene glycol and glycerol.

[0058] b) mixing 15 to 30 parts of ethyl orthosilicate, 20 to 45 parts of deionized water, and 5 to 15 parts of a 0.1 mol / L hydrochloric acid solution and stirring for 30 to 90 minutes, and then adding a certain amount of a 1 mol / L ammonia solution to adjust the pH value of the mixed silica sol to 3 to 5.

[0059] c) adding the silica sol of step (b) to the nano-silica dispersion of step (a), mixing them evenly, and then introducing them into the cavity of a preforming mold and allowing them to stand.

[0060] d) After the gel is solidified, the gel is separated from the preformed mold to obtain a wet gel block.

[0061] e) soaking the wet gel block in a colorant of a certain concentration, wherein the colorant is composed of the following proportions by weight: 100 parts of deionized water, 15-30 parts of ethanol, 0.01-0.1 parts of aluminum nitrate, 0.01-0.5 parts of potassium nitrate, 0.01-0.5 parts of ferric chloride, 0.01-0.05 parts of copper chloride, 0.2-0.4 parts of manganese chloride, 0.02-0.5 parts of samarium chloride, 0.01-1 parts of butyl titanate, and 0.3-0.8 parts of potassium dichromate.

[0062] f) soaking the wet gel block in a colorant for a certain period of time, and then drying it in a constant temperature and humidity chamber to obtain a dry gel.

[0063] g) placing the dry gel in an atmosphere furnace, introducing high-purity oxygen, and calcining at a temperature of 400-800° C. for 4-10 hours to form a loose and porous silica dry block with a certain color.

[0064] h) Immerse the dry silicon dioxide block in the colorant, evacuate the colorant until there are no bubbles, and soak for 1 to 24 hours.

[0065] This step can be repeated multiple times, and the concentration of the colorant, soaking time and number of soaking times can be adjusted according to the requirements of color depth.

[0066] i) The soaked dried silica block is first placed in an oven for drying, then placed in an atmosphere furnace, introduced with high-purity oxygen, heated to 400-800° C., and calcined at this temperature for 2-10 hours; then the gas atmosphere is switched to helium, the temperature is raised to 1100-1300° C., and calcined at this temperature for 4-20 hours. After cooling, uniformly colored green quartz glass is obtained.

[0067] In another specific embodiment, the quartz glass is red quartz glass, the colorant includes a first colorant and a second colorant, and the preparation of the red quartz glass includes the following steps:

[0068] a) preparing a nano-silica dispersion using 15 to 30 parts of high-purity fumed nano-silica powder having an impurity content of less than 30 ppm, 70 to 85 parts of deionized water, and a dispersant, wherein the dispersant accounts for 0.1% to 5% of the total mass of the high-purity fumed nano-silica powder and the deionized water, and is at least one of ethylene glycol and glycerol.

[0069] b) mixing 15 to 30 parts of ethyl orthosilicate, 20 to 45 parts of deionized water, and 5 to 15 parts of a 0.1 mol / L hydrochloric acid solution and stirring for 30 to 90 minutes, and then adding a certain amount of a 1 mol / L ammonia solution to adjust the pH value of the mixed silica sol to 3 to 5.

[0070] c) adding the silica sol of step (b) to the nano-silica dispersion of step (a), mixing them evenly, and then introducing them into the cavity of a preforming mold and allowing them to stand.

[0071] d) After the gel is solidified, the gel is separated from the preformed mold to obtain a wet gel block.

[0072] e) soaking the wet gel block in a first colorant of a certain concentration, wherein the mass ratio of the first colorant is 100 parts of deionized water, 0.01 to 3 parts of cadmium sulfate octahydrate, 0.01 to 0.8 parts of tin chloride dihydrate, 0.01 to 0.5 parts of manganese chloride and 0.01 to 0.4 parts of ferric chloride.

[0073] f) soaking the wet gel block in a colorant for a certain period of time, and then drying it in a constant temperature and humidity chamber to obtain a dry gel.

[0074] g) placing the dry gel in an atmosphere furnace, introducing high-purity oxygen, and calcining at a temperature of 400-800° C. for 4-10 hours to form a loose and porous silica dry block with a certain color.

[0075] h) Soaking the dried silica block in a second colorant, evacuating the solution until the second colorant is bubble-free, and soaking for 1 to 24 hours. The second colorant comprises the following components by weight: 100 parts deionized water, 10 to 20 parts concentrated hydrochloric acid solution, 1 to 3 parts cuprous oxide, 1 to 4 parts antimony oxide, 2 to 4 parts samarium chloride, and 0.1 to 3 parts aluminum chloride. The concentrated hydrochloric acid solution mentioned in the present embodiment is a commercially available concentrated hydrochloric acid solution having a mass fraction of hydrogen chloride (HCl) of approximately 37%.

[0076] This step can be repeated multiple times, and the concentration of the second colorant, the soaking time and the number of soaking times can be adjusted according to the requirements for the color depth.

[0077] i) The soaked dried silica block is first placed in an oven for drying, then placed in an atmosphere furnace, introduced with high-purity oxygen, heated to 400-800° C., and calcined at this temperature for 2-10 hours; then the gas atmosphere is switched to helium, the temperature is raised to 1100-1300° C., and calcined at this temperature for 4-20 hours. After cooling, uniformly colored red quartz glass is obtained.

[0078] In other specific embodiments, the quartz glass is yellow ultraviolet-filtering quartz glass, the colorant includes a first colorant, a second colorant, and a third colorant, and the method for preparing the yellow ultraviolet-filtering quartz glass comprises the following steps:

[0079] a) preparing a nano-silica dispersion using 15 to 30 parts of high-purity fumed nano-silica powder having an impurity content of less than 30 ppm, 70 to 85 parts of deionized water, and a dispersant, wherein the dispersant accounts for 0.1% to 5% of the total mass of the high-purity fumed nano-silica powder and the deionized water, and is at least one of ethylene glycol and glycerol.

[0080] b) mixing 15 to 30 parts of ethyl orthosilicate, 20 to 45 parts of deionized water, and 5 to 15 parts of a 0.1 mol / L hydrochloric acid solution and stirring for 30 to 90 minutes, and then adding a certain amount of a 1 mol / L ammonia solution to adjust the pH value of the mixed silica sol to 3 to 5.

[0081] c) adding the silica sol of step (b) to the nano-silica dispersion of step (a), mixing them evenly, and then introducing them into the cavity of a preforming mold and allowing them to stand.

[0082] d) After the gel is solidified, the gel is separated from the preformed mold to obtain a wet gel block.

[0083] e) using a step-by-step immersion method, first immersing the wet gel block in a first colorant of a certain concentration, wherein the mass ratio of the first colorant is 100 parts of deionized water, 5 to 8 parts of europium nitrate, 0.5 to 4 parts of sodium nitrate, 3 to 5 parts of yttrium nitrate, and 0.01 to 0.4 parts of aluminum nitrate; and then immersing the wet gel block in a second colorant of a certain concentration, wherein the mass ratio of the second colorant is 100 parts of deionized water, 2 to 4 parts of lanthanum chloride, and 0.3 to 0.8 parts of sodium metavanadate.

[0084] f) soaking the wet gel block in the first colorant and the second colorant for a certain period of time, and then placing the wet gel block in a constant temperature and humidity chamber to dry it, thereby obtaining a dry gel.

[0085] g) placing the dry gel in an atmosphere furnace, introducing high-purity oxygen, and calcining at a temperature of 400-800° C. for 4-10 hours to form a loose and porous silica dry block with a certain color.

[0086] h) soaking the dried silicon dioxide block in a third colorant, wherein the mass ratio of the third colorant is 100 parts of deionized water, 10-20 parts of concentrated hydrochloric acid solution, and 3-8 parts of vanadium pentoxide, evacuating the solution until the third colorant is free of bubbles, and soaking for 1-24 hours.

[0087] This step can be repeated multiple times, and the concentration of the third colorant, the soaking time and the number of soaking times can be adjusted according to the requirements of the color depth.

[0088] i) The soaked dried silica block is first placed in an oven for drying, then placed in an atmosphere furnace, introduced with high-purity oxygen, heated to 400-800° C., and calcined at this temperature for 2-10 hours; then the gas atmosphere is switched to helium, the temperature is raised to 1100-1300° C., and calcined at this temperature for 4-20 hours. After cooling, uniformly colored yellow UV-filtering quartz glass is obtained.

[0089] The method for preparing colored quartz glass provided in this embodiment can be used to manufacture optical devices in laser light sources or laser projectors, such as quartz filters, and can be used in conjunction with devices in laser projection systems or laser illumination systems. The two-step colorant immersion process effectively avoids the problem of the colorant hydrochloric acid solution hindering the gel and causing cracking during the gel drying process. It can also mass-produce colored quartz glass of various sizes at relatively low temperatures without the need for high-temperature melting or high-temperature drawing processes. The method has the advantages of simple process, low cost, low energy consumption, and uniform coloring.

[0090] See also Figure 2 , Figure 2 1 is a schematic structural diagram of an embodiment of colored quartz glass provided in the present application. The colored quartz glass 20 is a colored quartz glass produced by the method for producing colored quartz glass in the above embodiment.

[0091] It is understandable that the shape of the colored quartz glass 20 can be any shape and is not limited to Figure 2 The shape shown can be adjusted according to specific needs to obtain a device of corresponding shape.

[0092] The colored quartz glass 20 provided in this embodiment can be used as an optical element in an illumination system or projection. For example, the colored quartz glass 20 can be used to make a compound eye having both light shaping, homogenizing and filtering functions.

[0093] The above description is merely an embodiment of the present application and does not limit the patent scope of the present application. Any equivalent structure or equivalent process transformation made using the contents of the present application specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present application.

Claims

1. A method for preparing colored quartz glass, characterized in that: include: Preparation of nano-silica dispersion and silica sol; Adding the silica sol to the nano-silica dispersion and mixing evenly, pouring the mixed solution into a pre-molded mold for gel curing, and demoulding to obtain a wet gel block; soaking the wet gel block in a colorant and then drying it to obtain a xerogel; calcining the dry gel to obtain a dry silicon dioxide block; placing the dried silica block into the colorant, evacuating the colorant until there are no bubbles, soaking the block for 1 to 24 hours, and drying, calcining, and cooling the block to obtain the colored quartz glass; The steps of preparing the nano-silicon dioxide dispersion include: The nano-silicon dioxide dispersion is prepared by using nano-silicon dioxide powder, deionized water and a dispersant; The step of calcining the dry gel to obtain a dry silicon dioxide block comprises: The dried gel is placed in an atmosphere furnace, introduced with high-purity oxygen, and calcined at a temperature of 400-800° C. for 4-10 hours to obtain the dried silica block; The step of soaking the dry silicon dioxide block in the colorant, drying, calcining and cooling to obtain the colored quartz glass comprises: The soaked silica dry block is dried, placed in an atmosphere furnace, introduced with high-purity oxygen, heated to 400-800° C., and calcined at this temperature for 2-10 hours; the gas atmosphere is then switched to helium, heated to 1100-1300° C., calcined at this temperature for 4-20 hours, and cooled to obtain the colored quartz glass.

2. The method for preparing colored quartz glass according to claim 1, wherein: The dry silicon dioxide block is immersed in the colorant once or multiple times.

3. The method for preparing colored quartz glass according to claim 1, wherein: The mass fraction of the nano-silicon dioxide powder is 15 to 30 parts, the mass fraction of the deionized water is 70 to 85 parts, and the fraction of the dispersant in the total mass of the nano-silicon dioxide powder and the deionized water is 0.1% to 5%.

4. The method for preparing colored quartz glass according to claim 1 or 2, characterized in that: The steps of preparing silica sol include: Ethyl orthosilicate, deionized water and hydrochloric acid solution are mixed, stirred and then an ammonia solution is added to adjust the pH value to generate the silica sol.

5. The method for preparing colored quartz glass according to claim 4, wherein: The mass fraction of the ethyl orthosilicate is 15 to 30 parts, the mass fraction of the deionized water is 20 to 45 parts, and the concentration of the hydrochloric acid solution is 0.1 mol / L, and the mass fraction thereof is 5 to 15 parts.

6. The method for preparing colored quartz glass according to claim 5, characterized in that: The pH value of the silica sol is 3-5.

7. The method for preparing colored quartz glass according to claim 1 or 2, characterized in that: The colorant is prepared in the following proportions by mass: 100 parts of deionized water, 0.01 to 0.8 parts of cerium nitrate, 0.01 to 0.6 parts of copper chloride, 0.01 to 0.5 parts of ferric chloride, 0.01 to 0.4 parts of aluminum nitrate, 0.2 to 0.4 parts of manganese chloride, and 0.3 to 0.8 parts of potassium dichromate.

8. The method for preparing colored quartz glass according to claim 1 or 2, characterized in that: The colorant is prepared in the following proportions by mass: 100 parts of deionized water, 15 to 30 parts of ethanol, 0.01 to 0.1 parts of aluminum nitrate, 0.01 to 0.5 parts of potassium nitrate, 0.01 to 0.5 parts of ferric chloride, 0.01 to 0.05 parts of copper chloride, 0.2 to 0.4 parts of manganese chloride, 0.02 to 0.5 parts of samarium chloride, 0.01 to 1 parts of butyl titanate, and 0.3 to 0.8 parts of potassium dichromate.

9. The method for preparing colored quartz glass according to claim 1 or 2, characterized in that: The colorant includes a first colorant and a second colorant; The step of soaking the wet gel block in a colorant comprises: Soaking the wet gel block in the first colorant, wherein the mass ratio of the first colorant is 100 parts of deionized water, 0.01-3 parts of cadmium sulfate octahydrate, 0.01-0.8 parts of tin chloride dihydrate, 0.01-0.5 parts of manganese chloride and 0.01-0.4 parts of ferric chloride; The step of soaking the dry silicon dioxide block in the colorant comprises: The dried silica block is immersed in the second colorant, wherein the mass ratio of the second colorant is 100 parts of deionized water, 10-20 parts of concentrated hydrochloric acid solution, 1-3 parts of cuprous oxide, 1-4 parts of antimony oxide, 2-4 parts of samarium chloride and 0.1-3 parts of aluminum chloride.

10. The method for preparing colored quartz glass according to claim 1, wherein: The colorant includes a first colorant, a second colorant and a third colorant; The step of soaking the wet gel block in a colorant comprises: First, immerse the wet gel block in the first colorant, and then immerse the wet gel block in the second colorant, wherein the mass ratio of the first colorant is 100 parts of deionized water, 5-8 parts of europium nitrate, 0.5-4 parts of sodium nitrate, 3-5 parts of yttrium nitrate, and 0.01-0.4 parts of aluminum nitrate, and the mass ratio of the second colorant is 100 parts of deionized water, 2-4 parts of lanthanum chloride, and 0.3-0.8 parts of sodium metavanadate; The step of soaking the dry silicon dioxide block in the colorant comprises: The silicon dioxide dry block is immersed in the third colorant, wherein the mass ratio of the third colorant is 100 parts of deionized water, 10-20 parts of concentrated hydrochloric acid solution and 3-8 parts of vanadium pentoxide.

11. A colored quartz glass, characterized in that: The colored quartz glass is prepared by the method for preparing colored quartz glass according to any one of claims 1 to 10.

Citation Information

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