Preparation method of quartz ring for optical coating with low energy consumption

Abstract

The present invention provides a method for preparing a quartz ring for optical coating with low energy consumption, which belongs to the technical field of quartz ring preparation. The method comprises the following steps: (1) sand-grinding and mixing quartz powder, water and a dispersant to obtain a slurry; (2) mixing the slurry and a binder and granulating them to obtain granules; (3) cold isostatically pressing the granules to obtain a tubular structure blank; (4) sintering the tubular structure blank, and cutting to obtain a quartz ring for optical coating. The present invention first sand-grinds and granulates the quartz powder to obtain quartz powder granules, then forms them by cold isostatic pressing, and finally sintering and cutting to obtain a quartz ring for optical coating. The present application uses the cold isostatic pressing process to prepare quartz rings for optical coating, and does not require heating the quartz raw material to 1800°C for melting and preparation, which greatly reduces the energy consumption of the quartz ring preparation.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of quartz ring preparation, and particularly relates to a preparation method of a quartz ring for optical coating with low energy consumption. BACKGROUND

[0002] The main component of the quartz ring is silicon dioxide, has unique optical performance, is a material capable of transmitting ultraviolet light, can transmit far ultraviolet light, visible light and near infrared light, and has a wide application in the preparation of optical materials.

[0003] The processing technology of the traditional quartz ring mainly includes gas melting and electric melting, wherein the gas melting mainly utilizes the high-temperature flame generated by the combustion of hydrogen and oxygen to melt high-purity quartz powder into small droplets, the quartz droplets are deposited in a continuously rotating carrier to form a quartz lump, the quartz lump is processed into a cylindrical material by using a radial drill, and then the quartz ring is formed by using a multi-wire cutting device or a diamond grinding wheel; the electric melting mainly utilizes resistance graphite heating or induction heating to melt the quartz powder and then rotate and draw the quartz powder; the processing technologies of the above two kinds of quartz rings both need to heat the quartz powder to a temperature above the melting temperature of the product for compression molding, and have the problems of high energy consumption and high cost.

[0004] Therefore, it is urgent to provide a preparation method of a quartz ring for optical coating with low energy consumption. SUMMARY

[0005] The present application provides a preparation method of a quartz ring for optical coating with low energy consumption. The preparation method provided by the present application does not need to melt the raw material, but compresses and molds the raw material by cold isostatic pressing, thereby greatly reducing the energy consumption of preparation.

[0006] In order to achieve the above-mentioned application purposes, the present application provides the following technical solutions:

[0007] The present application provides a preparation method of a quartz ring for optical coating with low energy consumption, which comprises the following steps:

[0008] (1) mixing quartz powder, water and a dispersing agent by sand milling to obtain a slurry;

[0009] (2) mixing the slurry obtained in the step (1) and a binder to obtain granules by granulation;

[0010] (3) cold isostatic pressing the granules obtained in the step (2) to obtain a tubular structure blank;

[0011] (4) sintering the tubular structure blank obtained in the step (3) to obtain a quartz ring for optical coating after cutting.

[0012] Preferably, the quartz powder in step (1) has a purity of 99.99%, a D50 of 3-15 μm, and a tap density of 0.7-1.0 g / cm 3 .

[0013] Preferably, the dispersant in step (1) comprises polyacrylate and / or polyacrylamide.

[0014] Preferably, the mass ratio of the quartz powder to water in step (1) is 1:(0.8-1.5), and the mass ratio of the sum of the mass of the quartz powder and water to the mass of the dispersant is 100:(1-2).

[0015] Preferably, the D50 of the slurry in step (1) is 1-2 mm.

[0016] Preferably, the binder in step (2) comprises polyvinyl alcohol and / or carboxymethyl cellulose.

[0017] Preferably, the mass ratio of the slurry to the binder in step (2) is 100:(1.5-3).

[0018] Preferably, the particle size of the granules in step (2) is 0.1-0.5 mm, and the water content of the granules is 0.6-1.2 wt%.

[0019] Preferably, the loading pressure for the cold isostatic pressing in step (3) is 250-280 MPa, the pressure loading rate for the cold isostatic pressing is 8-12 MPa / min, and the pressure holding time for the cold isostatic pressing is 1-3 h.

[0020] Preferably, the sintering temperature in step (4) is 1200-1300℃, and the sintering time is 8-12 h.

[0021] The present application provides a preparation method of a quartz ring for optical coating with low energy consumption, comprising the following steps: (1) mixing quartz powder, water and a dispersant by sand milling to obtain a slurry; (2) mixing the slurry and a binder to obtain granules by granulation; (3) performing cold isostatic pressing on the granules to obtain a tubular structure blank; and (4) sintering the tubular structure blank to obtain a quartz ring for optical coating after cutting. The quartz powder is first sand milled and granulated, then formed by cold isostatic pressing, and finally sintered and cut to obtain a quartz ring for optical coating. The cold isostatic pressing process is used to prepare a quartz ring for optical coating in the present application, which does not need to melt the quartz raw material at 1800℃ for preparation, thereby greatly reducing the energy consumption for preparing the quartz ring. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1A schematic diagram of a sleeve in a mold sleeve of a cold isostatic pressing forming device used in the present application;

[0023] Figure 2 A schematic diagram of a plug in a mold sleeve of a cold isostatic pressing forming device used in the present application;

[0024] Figure 3 A schematic diagram of a steel core in a mold sleeve of a cold isostatic pressing forming device used in the present application;

[0025] Figure 4 A schematic diagram of assembly of a mold sleeve of a cold isostatic pressing forming device used in the present application. DETAILED DESCRIPTION

[0026] The present application provides a preparation method of a quartz ring for optical coating with low energy consumption, comprising the following steps:

[0027] (1) mixing quartz powder, water and a dispersing agent by sand milling to obtain a slurry;

[0028] (2) mixing the slurry obtained in the step (1) and a binder to obtain granules by granulation;

[0029] (3) cold isostatic pressing the granules obtained in the step (2) to obtain a tubular structure blank;

[0030] (4) sintering the tubular structure blank obtained in the step (3) to obtain a quartz ring for optical coating after cutting.

[0031] The present application mixes quartz powder, water and a dispersing agent by sand milling to obtain a slurry.

[0032] In the present application, the quartz powder has a purity of 99.99%, a D50 of 3-15 μm and a tap density of 0.7-1.0 g / cm 3 The present application uses quartz powder with a purity of 99.99% as raw material, which is conducive to avoiding the influence of impurities on the optical performance of the obtained quartz ring; and the D50 and tap density of the quartz powder are limited in the above range, which is conducive to the smooth progress of the subsequent cold isostatic pressing process.

[0033] In the present application, the water is preferably purified water. In the present application, the mass ratio of the quartz powder to water is preferably 1:(0.8-1.5), and more preferably 1:(1.0-1.5). The present application limits the amount of the quartz powder and water in the above range, so that a slurry meeting the specifications can be obtained, which is conducive to the subsequent granulation.

[0034] In the present application, the mass ratio of the sum of the mass of the quartz powder and water to the mass of the dispersing agent is preferably 100:

[0035] (1-2), more preferably 100:1. The present application adds dispersant when preparing the slurry, which is beneficial to the uniform dispersion of the quartz powder in water.

[0036] In the present application, the dispersant preferably comprises polyacrylate and / or polyacrylamide, more preferably polyacrylate. The present application selects the above-mentioned substances as the dispersant, which can be decomposed and removed during subsequent calcination, ensuring that no impurities are left, thereby ensuring the purity of the quartz ring.

[0037] In the present application, the sand milling is preferably performed on a sand mill. The present application does not have special provisions for the specifications of the sand mill, and a sand mill well known to those skilled in the art can be selected.

[0038] In the present application, the medium for sand milling is preferably zirconium oxide balls. In the present application, the diameter of the zirconium oxide balls is preferably 0.3-0.8 mm, more preferably 0.5 mm. In the present application, the ball-to-material mass ratio for sand milling is preferably (1-2):1, more preferably 1:1. The present application uses zirconium oxide balls for sand milling, and limits the ball-to-material ratio to the above-mentioned range, which is beneficial to the refinement of the quartz powder to the desired particle size range.

[0039] The present application does not have special provisions for the number of times and the time of sand milling, and the quartz powder is refined to the desired particle size range.

[0040] In the present application, the D50 of the slurry is preferably 1-2 mm. The present application limits the D50 value of the slurry to the above-mentioned range, which is beneficial to the smooth progress of the subsequent cold isostatic pressing forming process.

[0041] After obtaining the slurry, the present application mixes the slurry and the binder to obtain granules.

[0042] In the present application, the binder preferably comprises polyvinyl alcohol and / or carboxymethyl cellulose, more preferably polyvinyl alcohol. In the present application, the mass ratio of the slurry to the binder is preferably 100:(1.5-3), more preferably 100:2. The present application adds a binder to the slurry, which is beneficial to granulation. The present application selects the above-mentioned substances as the binder, which can be decomposed and removed during subsequent calcination, ensuring that no impurities are left, thereby ensuring the purity of the quartz ring.

[0043] The present application does not have special provisions for the mixing method of the slurry and the binder, and a mixing method well known to those skilled in the art can be used to mix the slurry and the binder uniformly.

[0044] In the present application, the inlet temperature of the granulator used for granulation is preferably 220-230°C, more preferably 225°C; and the outlet temperature of the granulator used for granulation is preferably 100-105°C, more preferably 100°C.

[0045] In the present application, the granulating method is preferably spray granulation. In the present application, the spray granulation method is preferably centrifugal rotation. In the present application, the rotation speed of the spray granulation is preferably 8000-12000 rpm, more preferably 10000 rpm. The present application limits the parameters of the granulation in the above range, which is advantageous for obtaining the required granules.

[0046] In the present application, the particle size of the granules is preferably 0.1-0.5 mm; the water content of the granules is preferably 0.6-1.2 wt%. The present application limits the specifications of the granules in the above range, which is advantageous for the smooth progress of the subsequent cold isostatic pressing forming process.

[0047] After obtaining the granules, the present application performs cold isostatic pressing forming on the granules to obtain a tubular structure blank.

[0048] In the present application, the cold isostatic pressing forming is preferably performed in a cold isostatic pressing forming device.

[0049] The present application preferably assembles the granules in a mold cover of a cold isostatic pressing forming device, then tightens and fixes the head and tail positions of the assembled mold cover with a stainless steel throat clamp, and finally places it in a cold isostatic pressing device for cold isostatic pressing forming to obtain a tubular structure blank.

[0050] In the present application, the mold cover preferably includes a cover, a plug and a steel core.

[0051] In the present application, the schematic diagram of the cover is preferably as shown in Figure 1 In the present application, the size of the cover is preferably designed according to the diameter and thickness of the prepared quartz ring. In addition, it should be noted that the product has a certain shrinkage rate of about 10% during sintering, so the shrinkage rate of the product should be calculated when designing the mold.

[0052] In the present application, the material of the cover is preferably polyurethane. In the present application, the hardness of the cover is preferably 55-65A, more preferably 60-65A. In the present application, the cover is used for powder isostatic pressing forming.

[0053] The present application does not have special provisions for the size of the plug, which can be designed according to the corresponding size of the cover. In the present application, the schematic diagram of the plug is preferably as shown in Figure 2 In the present application, the material of the plug is preferably polyurethane; the hardness of the plug is preferably 30-40A, more preferably 35A. In the present application, the plug is used for packaging granules.

[0054] The size of the steel core is not specially limited in the application, and can be designed according to actual needs. In the application, the material of the steel core is preferably 45# steel or die steel. In the application, the schematic diagram of the steel core is preferably as shown in Figure 3 In the application, the surface of the steel core is preferably plated with a chromium layer of 3-5 μm. In the application, the service life of the steel core can be improved by plating a chromium layer of 3-5 μm on the surface of the steel core.

[0055] In the application, the assembly schematic diagram of the mold cover is preferably as shown in Figure 4 The granules are between the cover and the steel core, and the granules are packaged with plugs.

[0056] In the application, the loading pressure of the cold isostatic pressing forming is preferably 250-280 MPa, and more preferably 260-280 MPa; the pressure loading rate of the cold isostatic pressing forming is preferably 8-12 MPa / min, and more preferably 10-12 MPa / min; and the pressure holding time of the cold isostatic pressing forming is preferably 1-3 h, and more preferably 2 h. In the application, the parameters of the cold isostatic pressing forming are limited in the above range, and the forming effect of the quartz ring for optical coating is better.

[0057] After obtaining the tubular structure blank, the tubular structure blank is sintered in the application, and the quartz ring for optical coating is obtained after cutting.

[0058] In the application, the sintering temperature is preferably 1200-1300℃, and more preferably 1250℃; the sintering time is preferably 8-12 h, and more preferably 10 h. In the application, the heating rate of the sintering is preferably 0.4-0.8℃ / min, and more preferably 0.6℃ / min. In the application, the cooling rate of the sintering is preferably 0.2-0.4℃ / min, and more preferably 0.3℃ / min. In the application, the temperature after cooling is preferably room temperature. In the application, the parameters of the sintering are limited in the above range, which is beneficial to obtain the quartz ring for optical coating with better comprehensive performance.

[0059] After sintering, the sintered tubular structure blank is preferably polished and cut in sequence in the application to obtain the quartz ring for optical coating.

[0060] The polishing method is not specially limited in the application, and the inner and outer diameters of the sintered tubular structure blank can be polished to the required specifications by using the polishing method known to those skilled in the art. In the embodiment of the application, the polishing method is preferably grinding machine processing and diamond grinding wheel polishing in sequence.

[0061] The application does not have special provisions for the cutting mode, and the sintered tubular structure blank is cut into a quartz ring with a required specification by using a cutting mode well known to those skilled in the art.

[0062] The application provides a preparation method of a quartz ring for optical coating with low energy consumption.

[0063] The technical solutions in the application will be clearly and completely described below with reference to the embodiments in the application. Obviously, the described embodiments are only some of the embodiments of the application, but not all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative efforts belong to the protection scope of the application.

[0064] Embodiment 1

[0065] A preparation method of a quartz ring for optical coating with low energy consumption comprises the following steps:

[0066] The raw materials used are quartz powder, water, a dispersing agent and a binder

[0067] The quartz powder has a purity of 99.99%, a D50 of 3-15 μm and a tap density of 0.7-1.0 g / cm 3 The water is pure water, the dispersing agent is polyacrylate and the binder is polyvinyl alcohol

[0068] (1) The quartz powder, water and dispersing agent are put into a sand mill, zirconia balls with a diameter of 0.5 mm are added into the sand mill, the mass ratio of the balls to the powder is 1:1, sand milling is performed to finely grind the powder to a D50 of 1-2 mm, and a slurry is obtained;

[0069] The mass ratio of the quartz powder to the water is 1:1.2, and the mass ratio of the sum of the mass of the quartz powder and the mass of the water to the mass of the dispersing agent is 100:1.

[0070] (2) The slurry obtained in the step (1) and the binder are mixed, the inlet temperature of a spray granulator is set to 225 DEG C, the outlet temperature is set to 100 DEG C, spray granulation is performed by centrifugal rotation, the spray centrifugal rotation speed is set to 10,000 r / min, and a granular material is obtained; the mass ratio of the slurry to the binder is 100:2; the particle size of the granular material is 0.1-0.5 mm; and the water content of the granular material is 0.6-1.2 wt.%;

[0071] (3) the granules are placed in a die sleeve of a cold isostatic pressing forming device according to Figure 4 assembly, the granules are located between the sleeve and the steel core, then the head and tail positions of the assembled die sleeve are fixed by tightening with a stainless steel throat clamp, and finally placed in a cold isostatic pressing device for cold isostatic pressing forming to obtain a tubular structure blank;

[0072] The die sleeve is composed of a sleeve, a steel core and a plug. The steel core is made of 45# steel, and the surface is plated with a chromium layer of 4 μm. The plug is made of polyurethane with a hardness of 35A. The sleeve is made of polyurethane with a hardness of 60A.

[0073] The loading pressure of the cold isostatic pressing forming is 260 MPa. The pressure loading rate of the cold isostatic pressing forming is 10 MPa / min. The pressure holding time of the cold isostatic pressing forming is 2 h.

[0074] (4) the tubular structure blank obtained in step (3) is vertically placed in a high-temperature sintering furnace, heated to 1250℃ at a heating rate of 0.6℃ / min, and held for 10 h, then cooled to room temperature at a cooling rate of 0.3℃ / min, to obtain a cylindrical semi-finished product; then the cylindrical semi-finished product is ground in turn by an internal and external circular grinding machine and a diamond grinding wheel piece to grind the inner and outer diameters, then sliced by a numerical control lathe and a diamond grinding wheel piece, and protective chamfers are made, to finally obtain a quartz ring for optical coating.

[0075] Therefore, the cold isostatic pressing forming process is used to prepare the quartz ring for optical coating, without the need to heat the quartz raw material to 1800℃ for melting, greatly reducing the energy consumption of the preparation of the quartz ring.

[0076] The above only describes the preferred embodiments of the present application, and it should be noted that for those skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, which should also be considered within the scope of protection of the present application.

Claims

1. A method for preparing a quartz ring for optical coating with low energy consumption, comprising the following steps: (1) sand-grinding and mixing quartz powder, water, and a dispersant to obtain a slurry; (2) mixing the slurry obtained in step (1) with a binder and granulating to obtain pellets; (3) cold isostatic pressing the pellets obtained in step (2) to obtain a tubular structure blank; (4) sintering the tubular structure blank obtained in step (3), and cutting it to obtain a quartz ring for optical coating; The specifications of the quartz powder in step (1) are: purity of 99.99%, D50 of 3-15 μm, and tap density of 0.7-1.0 g / cm 3 ; In step (1), the dispersant comprises polyacrylate and / or polyacrylamide; In step (2), the binder comprises polyvinyl alcohol and / or carboxymethyl cellulose; In step (3), the pressure of the cold isostatic pressing is 250-280 MPa, the pressure loading rate of the cold isostatic pressing is 8-12 MPa / min, and the holding time of the cold isostatic pressing is 1-3 hours; The sintering temperature in step (4) is 1200-1300° C., and the sintering time is 8-12 hours.

2. The preparation method according to claim 1, characterized in that In the step (1), the mass ratio of quartz powder to water is 1:(0.8-1.5); the mass ratio of the sum of the mass of the quartz powder and water to the dispersant is 100:(1-2).

3. The preparation method according to claim 1, characterized in that The D50 of the slurry in step (1) is 1 to 2 mm.

4. The preparation method according to claim 1, characterized in that The mass ratio of the slurry to the binder in the step (2) is 100:(1.5-3).

5. The preparation method according to claim 1, characterized in that The particle size of the pellets in step (2) is 0.1-0.5 mm; the water content of the pellets is 0.6-1.2 wt%.

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