CN109704555B - Fire polishing blackening preparation method of anti-halation step glass - Google Patents
Fire polishing blackening preparation method of anti-halation step glass Download PDFInfo
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Abstract
The invention discloses a fire polishing blackening preparation method of anti-halation step glass. The fire polishing blackening preparation method of the halo-proof step glass comprises the following steps: 1) placing the anti-halation step glass blank in a closed furnace, and introducing reducing gas in a flow mode of feeding in and discharging out simultaneously; 2) and heating the closed furnace from room temperature to a preheating temperature, removing impurities from the anti-halation step glass blank, heating to a blackening temperature for blackening, and heating to a fire polishing temperature for fire polishing. The preparation process for the corona-proof step glass fire polishing blackening has short treatment time and high efficiency, and the obtained black glass layer can achieve the polishing effect without any treatment on the smoothness.
Description
Technical Field
The invention relates to the field of optical materials, in particular to a fire polishing blackening preparation method of anti-halation step glass.
Background
The antihalation step glass is a transparent glass with a black glass layer on the surface, and the schematic diagram of the finished product is shown in figure 1. The antihalation step glass is mainly applied to an image intensifier of a low-light level night vision device, is used as an input window of a single-stage image intensifier, and is used for eliminating stray light and depositing a multi-alkali photocathode. The black glass layer can absorb the incident and reflected light to the surface, so that compared with the input window of the optical fiber panel, the antihalation step glass can eliminate the scattered light generated by stripes, bubbles and other defects and the reflected light of a light path system, and greatly improve the image resolution and the sensitivity of the low-light night vision device.
The preparation process of the antihalation step glass mainly comprises three steps of blank processing, blackening and forming treatment. The blank processing is to make the glass have a certain shape by a mechanical method to obtain the antihalation step glass blank shown in the attached figure 2. The blackening is to form a layer of black glass layer on the surface of a glass blank by a physical or chemical method to obtain the anti-halation step glass semi-finished product shown in the attached figure 3. The forming treatment is to polish the black glass layers on the upper and lower surfaces of the glass semi-finished product to leak the transparent glass inside, and simultaneously polish the black glass layers on the inclined surface, the step surface and the cylindrical surface, and to round the part of the top angle to obtain the antihalation step glass shown in fig. 1.
High elegance of optical institute of Xian applied in 1993In the third generation of glass for photocathode table screen and its blackening, 4 schemes for glass blackening are described: the ion exchange hydrogen reduction method has certain amount of univalent cation (Li) in the components+、Na+、K+) Under certain conditions, the silver in the silver nitrate is melted+Exchanged and then passed through H2Reducing the glass into Ag simple substance at high temperature to blacken the surface of the glass; ② a method for doping coloring ions in glass, wherein the glass formula is doped with coloring ions or valence-variable ions (Pb, Bi, Co, Fe, Mn, Cr, V, etc.), and the high-temperature H treatment is carried out2Reducing to blacken the surface; selecting low-melting-point glass powder matched with the expansion coefficient of the anti-halation step glass blank, doping coloring ion oxide according to a certain proportion, uniformly blending with water, coating the mixture on the surface of the step glass blank, drying in the shade, and sintering to obtain a step glass semi-finished product with a black surface; soaking the anti-halation step glass blank into sol containing coloring ions (Fe, Mn, Cr, V, etc.), taking out, and sintering at high temperature to obtain the step glass semi-finished product with the black glass layer on the surface.
In 2018, the national institute of building materials science research, ltd, filed a patent of "a borosilicate glass, an anti-halation input window glass and a preparation method thereof" (application publication No. CN108423986A), and the glass blackening process disclosed by the patent is as follows: firstly, a borosilicate glass blank doped with coloring elements is placed in a closed container and is reacted with H2Contacting and heating; ② wherein H2Is pure H2Or H2And N2Preferably borosilicate glass with pure H2Contacting; (iii) regularly replacing H in the closed container2Flow H may also be used2Preferably, the H in the closed container is replaced at regular time2By replacing H every 12 hours2(ii) a Fourthly, general H2The pressure is 0.02MPa to 0.25MPa, preferably H2The pressure is 0.05MPa to 0.17 MPa; fifthly, the heating temperature is generally 400-900 ℃, and the preferred heating temperature is 500-700 ℃; sixth, general formula H2The treatment time is 2 to 500 hours, preferably H2The treatment time is 72 to 300 hours.
The capability of the black glass layer of the anti-halation step glass for absorbing stray light is important for the quality of the anti-halation effect, the light absorption capability depends on the thickness of the black glass layer under the condition that the glass components are not changed, and the thickness of the black glass layer cannot be too thin if the stray light is completely absorbed to meet the use requirement. Generally, when the thickness of the black glass layer is more than 0.5mm, the transmittance is less than 3 percent, and the anti-halation effect is good; when the thickness of the black glass layer is about 0.4mm, the transmittance is about 7 percent, and the anti-halation effect is in a critical state; when the thickness of the black glass layer is less than 0.4mm, the transmittance of the black glass layer can be sharply reduced, even light leakage occurs, and the antihalation effect is poor. Therefore, in the process of forming the anti-halation step glass, the polishing of the black glass layer should be reduced to the maximum extent so as to ensure a good anti-halation effect.
The black glass layer of anti-halation step glass obtained by the current blackening process has the problem of insufficient surface smoothness, the forming treatment process also needs to perform manual polishing treatment on the black glass layers of the inclined plane, the step surface and the cylindrical surface to achieve the required smoothness, the thickness of the polished black glass layer is greatly reduced, the thickness of the polished black glass layer is greatly different, and the absorption effect of the black glass layer on stray light is seriously influenced. In addition, the artificial and manual polishing of the anti-halation step glass not only can thin the black glass layer, but also can cause the problem of poor parallelism due to inconsistent thinning amount.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a fire polishing blackening preparation method of anti-halation step glass, and the prepared anti-halation step glass black glass layer can achieve a polishing effect without any treatment on the smoothness.
The technical scheme adopted by the invention is as follows:
a fire polishing blackening preparation method of anti-halation step glass comprises the following steps:
1) placing the anti-halation step glass blank in a closed furnace, and introducing reducing gas in a flow mode of feeding in and discharging out simultaneously;
2) and heating the closed furnace from room temperature to a preheating temperature, removing impurities from the anti-halation step glass blank, heating to a blackening temperature for blackening, and heating to a fire polishing temperature for fire polishing.
In the fire polishing blackening preparation method of the halo-proof step glass, in the step 1), the flow modes of inlet and outlet comprise an upper inlet and lower outlet mode, an upper inlet and upper outlet mode, a lower inlet and lower outlet mode or a lower inlet and upper outlet mode, and the flow modes are mainly realized by changing the positions of an inlet and outlet air valve in a hearth; the preferred flow pattern of the present invention is a down-in-up-out pattern. Due to reducing gases (e.g. H)2) Relatively lighter, can be spontaneous toward furnace top diffusion, can also be in the gas flow in-process with the heat of furnace lower part take to furnace upper portion region, alleviate the difference in temperature that furnace self structure brought.
Preferably, in the fire polishing blackening preparation method of the halo-proof step glass, in the step 1), the pressure of reducing gas in a closed furnace is 0.01MPa to 0.05 MPa; more preferably, the pressure of the reducing gas in the closed furnace is 0.01 to 0.02 MPa. With a slight positive pressure in this range, it is advantageous to reduce the gas (e.g., H)2) Flow and diffusion in the hearth can also reduce the use H2Potential safety hazards are brought.
Preferably, in the fire polishing blackening preparation method of the halo-proof step glass, in the step 1), the flow of the reducing gas is 0.1L/min-2L/min; more preferably, the flow rate of the reducing gas is 0.2L/min to 1L/min.
Preferably, in the fire polishing blackening preparation method of the halo-proof step glass, in the step 1), the reducing gas is one of hydrogen and a mixed gas of hydrogen and nitrogen; the hydrogen and the nitrogen can be mixed in any proportion; it is further preferred that the reducing gas is hydrogen, the hydrogen having a purity of at least 99.99%.
Preferably, in the step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the preheating temperature is 450-500 ℃, and the time of impurity removal treatment is 1-5 h; further preferably, the preheating temperature is 500 ℃, and the time of impurity removal treatment is 2-4 h.
Preferably, in step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the temperature is raised to the preheating temperature in a step manner, and the step temperature raising specifically comprises the following steps: firstly heating the mixture from room temperature to 180-220 ℃, preserving the heat for 1-5 h, and then heating the mixture to a preheating temperature for impurity removal treatment. The impurity removal treatment is to remove water and other easily-desorbed impurities on the surface of the glass blank.
In some preferred embodiments of the invention, the preparation method step 2) adopts a step heating mode, the temperature is firstly increased from room temperature to 180-220 ℃ and is kept for a period of time, water molecules and other easily-desorbed impurities on the surface of the glass blank can be volatilized, and the volatilized water molecules and other easily-desorbed impurities are accompanied by H2The flow of (b) is discharged out of the furnace; then the temperature is raised to the preheating temperature and is kept for a period of time, so that the carbonized stains and grease impurities on the surface of the blank are completely decomposed and volatilized, and the surface of the anti-halation step glass blank before blackening reaches atomic level cleanness.
Further preferably, in step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the step temperature rise mode is specifically as follows: firstly heating from room temperature to 200 ℃, preserving heat for 2-4 h, then heating to preheating temperature for impurity removal treatment.
In the step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the blackening treatment means that the halo-proof step glass blank is at the temperature of more than 500 ℃ and the glass softening point TfHigh temperature and H2Reducing to form a black glass layer on the surface of the glass blank, but the glass blank does not generate plastic deformation basically.
Preferably, in the step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the blackening temperature is 550-650 ℃.
Preferably, in the step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the blackening time is 50-200 h; more preferably, the blackening treatment is carried out for 100 to 150 hours.
In the step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the fire polishing treatment is carried out at the softening point T of the glassfThe glass is subjected to heat preservation treatment at the temperature, so that the glass presents tiny plastic deformation, the integral size of the glass is ensured, and the flaws such as micro cracks, small bulges, folds, ripples and the like on the surface of the glass can be changed into smooth and flat surfaces to obtain the glassThe glass surface with excellent finish is obtained.
Preferably, in the step 2) of the fire polishing blackening preparation method of the halo-proof step glass, the fire polishing temperature is 70-200 ℃ higher than the blackening temperature, namely the fire polishing temperature is 620-850 ℃; further preferably, the fire polishing temperature is 70-150 ℃ higher than the blackening temperature, namely the fire polishing temperature is 620-800 ℃.
Preferably, in the step 2) of the preparation method for the anti-halation step glass by fire polishing and blackening, the time of the fire polishing treatment is 0.3 to 3 hours; further preferably, the time of the fire polishing treatment is 0.5h to 2 h.
Preferably, in the fire polishing blackening preparation method of the halo-proof step glass, the closed furnace is a closed high-temperature furnace with a reducing atmosphere.
An anti-halation step glass is prepared by the preparation method.
The invention has the beneficial effects that:
the preparation process for the corona-proof step glass fire polishing blackening has short treatment time and high efficiency, and the obtained black glass layer can achieve the polishing effect without any treatment on the smoothness.
The method comprises the following specific steps:
(1) the thickness of the black glass layer is determined by the time of the high temperature blackening under the condition that the glass composition is unchanged, and the longer the time of the high temperature blackening in a certain range is, the thicker the thickness of the black glass layer is. The fire polishing blackening process is adopted to reduce the high-temperature time of blackening, and an anti-halation step glass finished product with the same thickness of the black glass layer can be obtained, so that the time required by blackening is shortened, and the blackening period of the anti-halation step glass is further accelerated.
(2) The surface of the glass blank presents tiny plastic deformation in the fire polishing blackening process, the vertex angles of the inclined plane and the step surface and the vertex angles of the step surface and the cylindrical surface all have edge slipping to form arc angles, and the vertex angles do not need to be chamfered during molding treatment, so that the requirements of finished products are met.
(3) The polishing effect can be achieved without any treatment on the smooth finish of the black glass layer, the problem of uneven thickness of the black glass layer caused by polishing in the forming treatment is avoided, the working strength of the forming treatment is reduced, the anti-halation capability of the anti-halation step glass is improved, and the qualification rate of the anti-halation step glass in production and processing is also improved.
Drawings
FIG. 1 is a schematic view of a finished anti-halation step glass;
FIG. 2 is a schematic view of an anti-halation step glass blank before blackening;
FIG. 3 is a schematic view of a blackened antihalation step glass semi-finished product.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials used in the examples are, unless otherwise specified, commercially available from conventional sources.
Example 1
After the anti-halation step glass blank is formed, the glass blank is placed into a closed reducing atmosphere high-temperature furnace, and 99.99% of H is introduced into the furnace in a mode of downward feeding and upward discharging2(ii) a By controlling H2A pressure reducing valve at the gas source maintains the gas pressure in the reducing atmosphere furnace in a micro-positive pressure state of 0.01-0.02 MPa, and the gas flow is controlled within the range of 0.2L/min-1L/min; the furnace temperature is firstly increased from room temperature to 500 ℃, and is kept at 500 ℃ for 2-4 h, so that impurities on the surface of the blank are completely decomposed and volatilized, because the impurities on the surface of the glass occupy the position of the surface and form a high surface potential barrier, the impurities on the surface must be removed, and the surface of the anti-halation step glass blank is ensured to be atomically clean; secondly, heating to the temperature required by blackening from 500 ℃, and preserving the heat for a period of time, wherein the blackening temperature is 550-650 ℃, and the blackening time is 100-150 h; and raising the temperature from the blackening temperature to the fire polishing temperature again, and carrying out short-time heat preservation, wherein the polishing temperature is 70-100 ℃ higher than the blackening temperature, and the fire polishing time is 1-2 h.
Example 2
After the anti-halation step glass blank is formed, the glass blank is placed into a closed reducing atmosphere high-temperature furnace, and 99.99% of H is introduced into the furnace in a mode of downward feeding and upward discharging2(ii) a By controlling H2The pressure reducing valve at the gas source ensures that the gas pressure in the reducing atmosphere furnace is maintained at a micro-positive pressure state of 0.01-0.02 MPa and the gas flowControlling the concentration within the range of 0.2L/min to 1L/min; the temperature of the reducing atmosphere furnace is firstly increased from room temperature to 200 ℃, and is kept at 200 ℃ for 2-4H, so that water molecules and other easily desorbed impurities on the surface of the glass blank are volatilized and accompany with H2The flow of (b) is discharged out of the furnace; secondly, heating the blank to 500 ℃ from 200 ℃, and keeping the temperature at 500 ℃ for 2-4 h to completely decompose and volatilize impurities on the surface of the blank and ensure that the surface of the anti-halation step glass blank is atom-level clean; raising the temperature from 500 ℃ to the temperature required by blackening, and preserving the heat for a period of time, wherein the blackening temperature is 550-650 ℃, and the blackening time is 100-150 h; and finally, heating from the blackening temperature to the fire polishing temperature, and carrying out short-time heat preservation, wherein the polishing temperature is 70-100 ℃ higher than the blackening temperature, and the fire polishing time is 1-2 h.
Example 3
After the anti-halation step glass blank is formed, the glass blank is placed into a closed reducing atmosphere high-temperature furnace, and 99.99% of H is introduced into the furnace in a mode of downward feeding and upward discharging2(ii) a By controlling H2A pressure reducing valve at the gas source maintains the gas pressure in the reducing atmosphere furnace in a micro-positive pressure state of 0.01-0.02 MPa, and the gas flow is controlled within the range of 0.2L/min-1L/min; the temperature of the reducing atmosphere furnace is firstly increased from room temperature to 200 ℃, and the temperature is kept at 200 ℃ for 2-4 h; secondly, heating the blank to 500 ℃ from 200 ℃, and preserving the heat for 2-4 hours at 500 ℃ to completely decompose and volatilize impurities on the surface of the anti-halation step glass blank; raising the temperature from 500 ℃ to the temperature required by blackening, and preserving the heat for a period of time, wherein the blackening temperature is 550-650 ℃, and the blackening time is 100-150 h; and finally, heating from the blackening temperature to the fire polishing temperature, and carrying out short-time heat preservation, wherein the polishing temperature is 100-150 ℃ higher than the blackening temperature, and the fire polishing time is 0.5-1 h.
The method comprises measuring the smoothness (surface roughness) by microscope comparison, putting the measured surface and the roughness sample block together, observing the amplified surfaces under microscope, and judging whether the measured surface reaches the surface roughness of the corresponding sample block by using the sample block surface as standard. Through detection, the surface of the anti-halation step glass prepared by the method is a mirror-like gloss surface, the surface smoothness is 13, and Ra is less than or equal to 0.02. In the antihalation step glass obtained by CN108423986A, the surface of the black glass layer is a dark gloss surface, the surface smoothness is 11, and Ra is less than or equal to 0.08.
The black glass layer of the antihalation step glass prepared by the embodiment has uniform thickness and good surface smoothness, and the polishing effect can be achieved without manual polishing; the vertex angles of the inclined plane and the step surface and the vertex angles of the step surface and the cylindrical surface are subjected to edge slipping to form arc angles; the light transmittance of the transparent glass area after the large and small surfaces are ground in the wavelength range of 380 nm-900 nm is more than 90%, and the light transmittance of the black glass layer in the wavelength range of 380 nm-900 nm is less than 5%.
Claims (7)
1. A fire polishing blackening preparation method of anti-halation step glass is characterized by comprising the following steps of: the method comprises the following steps:
1) placing the anti-halation step glass blank in a closed furnace, and introducing reducing gas in a flow mode of feeding in and discharging out simultaneously;
2) heating the sealed furnace from room temperature to a preheating temperature, removing impurities from the anti-halation step glass blank, heating to a blackening temperature for blackening, and heating to a fire polishing temperature for fire polishing;
in the step 2), the preheating temperature is 450-500 ℃, and the time of impurity removal treatment is 1-5 h; in the step 2), the blackening temperature is 550-650 ℃, and the blackening time is 50-200 h; in the step 2), the fire polishing temperature is 70-200 ℃ higher than the blackening temperature, and the time of the fire polishing treatment is 0.3-3 h.
2. The fire polishing blackening preparation method of anti-halation step glass as claimed in claim 1, characterized in that: in the step 1), the flow mode of entering and exiting simultaneously is a downward entering and upward exiting mode.
3. The fire polishing blackening preparation method of anti-halation step glass as claimed in claim 1, characterized in that: in the step 1), the pressure of the reducing gas in the closed furnace is 0.01MPa to 0.05 MPa.
4. The fire polishing blackening preparation method of the anti-halation step glass as claimed in claim 3, characterized in that: in the step 1), the flow rate of the reducing gas is 0.1L/min-2L/min.
5. The fire-polishing blackening preparation method of an anti-halation step glass as claimed in claim 1 or 4, wherein: in the step 1), the reducing gas is one of hydrogen and a mixed gas of hydrogen and nitrogen.
6. The fire polishing blackening preparation method of anti-halation step glass as claimed in claim 1, characterized in that: in the step 2), the mode of raising the temperature to the preheating temperature is step temperature raising, and specifically comprises the following steps: firstly heating the mixture from room temperature to 180-220 ℃, preserving the heat for 1-5 h, and then heating the mixture to a preheating temperature for impurity removal treatment.
7. The utility model provides an anti-halation step glass which characterized in that: is prepared by the preparation method of any one of claims 1 to 6.
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| CN111533465B (en) * | 2020-05-18 | 2021-10-26 | 中国建筑材料科学研究总院有限公司 | Anti-halation step glass and preparation method and application thereof |
| CN111574067B (en) * | 2020-05-18 | 2021-07-27 | 中国建筑材料科学研究总院有限公司 | Optical glass with light absorption layer and preparation method thereof |
| CN111574048B (en) * | 2020-05-18 | 2021-07-20 | 中国建筑材料科学研究总院有限公司 | Anti-halation glass with high cathode sensitivity and preparation method and application thereof |
| CN118184137A (en) * | 2024-04-07 | 2024-06-14 | 中建材光子科技有限公司 | Long-service-life halation-preventing glass and preparation method and application thereof |
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| US4961025A (en) * | 1988-08-18 | 1990-10-02 | Itt Corporation | Cathode for image intensifier tube having reduced veiling glare |
| US5045510A (en) * | 1989-11-03 | 1991-09-03 | Alfred University | Process for preparing a surface darkened glass |
| CN105523706B (en) * | 2016-01-26 | 2018-05-08 | 中国建筑材料科学研究总院 | Antihalation step glass and its blank and preparation method |
| CN105710740B (en) * | 2016-04-21 | 2018-04-24 | 中国建筑材料科学研究总院 | The polishing method and fixture of glass input window element |
| CN108423986B (en) * | 2018-03-28 | 2020-11-06 | 中国建筑材料科学研究总院有限公司 | Borosilicate glass, anti-halation input window glass and preparation method thereof |
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