CN109574497B - Medium-wave infrared glass and preparation process thereof - Google Patents
Medium-wave infrared glass and preparation process thereof Download PDFInfo
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- CN109574497B CN109574497B CN201811590178.0A CN201811590178A CN109574497B CN 109574497 B CN109574497 B CN 109574497B CN 201811590178 A CN201811590178 A CN 201811590178A CN 109574497 B CN109574497 B CN 109574497B
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- wave infrared
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- 239000011521 glass Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 37
- 230000005540 biological transmission Effects 0.000 claims abstract description 15
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 15
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000004297 night vision Effects 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 238000000137 annealing Methods 0.000 claims description 12
- 238000005352 clarification Methods 0.000 claims description 7
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 230000005284 excitation Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052594 sapphire Inorganic materials 0.000 abstract description 6
- 239000010980 sapphire Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 206010066054 Dysmorphism Diseases 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 3
- 238000002834 transmittance Methods 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract 1
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008395 clarifying agent Substances 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/10—Compositions for glass with special properties for infrared transmitting glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
- C03B25/02—Annealing glass products in a discontinuous way
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/253—Silica-free oxide glass compositions containing germanium
Abstract
The application provides a medium wave infrared glass, and belongs to the field of inorganic materials. The paint is characterized by comprising the following components in percentage by mass: b is2O36~10%;GeO70~81%,Bi2O32~6%,La2O32~4%,BaO2~5%,Sb2O30.5 to 4 percent. The application provides a medium wave infrared glass, the high weatherability of stable transmittance ratio of the medium infrared transmission wavelength from 0.4-6 mu m that enables the transmission wavelength range of glass is wider, material later stage processing is convenient and reliable, have the infrared transmission performance of similar sapphire, but material processing technology and the processing and cost etc. of the optical product in later stage are less than the sapphire far away, be fine multispectral transmission infrared material, it is good to have the cost of manufacture low chemical stability, characteristics such as operating temperature high rigidity height are, be the ideal material of preparation jumbo size dysmorphism infrared window, radome fairing and infrared night vision lens.
Description
Technical Field
The application belongs to the field of inorganic materials, and particularly relates to medium-wave infrared glass.
Background
The infrared glass is optical glass capable of transmitting electromagnetic radiation in an infrared band, and can be widely applied to infrared detection and infrared imaging technologies as a window, a lens and the like.
The traditional infrared glass has the transmission wavelength range of 780-2500nm, small range, complex material processing and poor stability.
Disclosure of Invention
Technical problem to be solved
In view of above-mentioned technical problem, the application provides an infrared glass of medium wave, and the penetrating wavelength range that enables glass is wider, and the infrared glass of medium wave that the application provided is stable high, and the transmissivity is high, and the weatherability is strong, and material later stage processing is convenient reliable.
(II) technical scheme
The medium wave infrared glass is characterized by comprising the following components in percentage by mass:
B2O36~10%;GeO 70~81%,Bi2O3 2~6%,La2O3 2~4%,BaO 2~5%,Sb2O3 0.5~4%。
in some embodiments, the composition comprises the following components in percentage by mass:
B2O3 8%;GeO 81%,Bi2O3 4%,La2O3 3%,BaO 3%,Sb2O3 3%。
a preparation process of medium wave infrared glass comprises the following steps:
(1) and (3) melting the ingredients: uniformly stirring the materials of the components according to the proportioning parts, pouring the materials into a crucible, continuously heating at 1380 +/-10 ℃ for 6-10 hours, pouring the materials into the crucible, feeding the materials at the frequency of once per hour, and finishing feeding for 8 times in total;
(2) a clarification stage: controlling the temperature in the crucible to 1410 +/-10 ℃ and keeping the temperature for 6-8 hours, stirring and defoaming in the process, and stirring for four times in total, wherein the specific stirring speed is 60 revolutions per minute, 30 revolutions per minute, 20 revolutions per minute and 10 revolutions per minute in sequence; stirring for 0.5 hour, 3 hours and 0.5 hour in sequence, and precipitating for 4-5 hours after stirring;
(3) and (3) cooling: cooling the temperature in the crucible in the step (2) to 980 +/-10 ℃;
(4) and (3) annealing stage: and (3) putting the raw materials cooled in the step (3) into an annealing furnace, continuously cooling for two times, reducing the temperature to 540 +/-10 ℃ for the first time, preserving the heat for 8-12 hours, reducing the temperature from 540 +/-10 ℃ to 350 +/-10 ℃ for the second time, reducing the temperature by 10 ℃ per hour to 350 ℃ for the second time, powering off, naturally cooling to normal temperature, opening the furnace, and discharging to obtain the glass.
In some embodiments, the glass has a thickness of 0.3 to 60 mm.
In some embodiments, the glass has a transmission wavelength in the range of 0.4 to 6 μm.
In some embodiments, the glass has a refractive index nd in the range of 1.8356-1.8359 and an Abbe number vd in the range of 26.87 ± -0.02.
In some embodiments, the electric power of the annealing furnace in the step (4) is 6-30(kW/380V), the gas power is 15-60 kilocalories, and the network speed is controlled by one of AC excitation speed regulation or variable frequency speed regulation.
In some embodiments, the material purity in step (1) is 99.999%.
In some embodiments, the clarification stage in step (2) refers to a process of precipitation after stirring the material.
The medium wave infrared glass may be used in making specially shaped infrared window, fairing and infrared night vision lens.
(III) advantageous effects
According to the technical scheme, the method has at least one of the following beneficial effects:
(1) the application provides a medium wave infrared glass, the high weatherability of the stable transmittance of infrared transmission wavelength from 0.4-6 mu m that enables glass's transmission wavelength range is wider is strong, material later stage processing is convenient reliable, have the infrared transmission performance of similar sapphire, but material processing technology and the processing and the cost etc. of the optical product in later stage are less than the sapphire far away, be good multispectral infrared material that permeates, it is good to have the cost of manufacture low chemical stability, characteristics such as the high rigidity of service temperature height are made, be the ideal material of preparation dysmorphism infrared window, radome fairing and infrared night vision lens.
(2) The application provides a medium wave infrared glass, wherein a formula of the medium wave infrared glass is provided with B2O3The chemical stability and the heat resistance stability can be effectively increased.
(3) According to the medium-wave infrared glass, BaO is arranged in the formula, so that the crystallization performance of the glass can be effectively improved.
(4) The application provides a medium wave infrared glass, the formula of which is provided with Bi2O3The melting temperature can be reduced.
(5) According to the medium-wave infrared glass, the GeO is arranged in the formula, and mainly is a glass forming body which can effectively penetrate through medium-wave infrared rays.
(6) The application provides a medium wave infrared glass, and La is arranged in the formula2O3,Supplement effect, and can effectively reduce the Abbe number of the glass.
(7) The application provides a medium wave infrared glass, and Sb is arranged in the formula2O3,It can be used as clarifying agent for solute, and can be used as chemical decolouring agent for maintaining or raising transparency of transparent glass.
Detailed Description
The application provides a medium wave infrared glass, the high weatherability of stable transmittance ratio of infrared transmission wavelength from 0.4-6 mu m that enables glass's transmission wavelength range wider is strong, material later stage processing is convenient reliable, have the infrared transmission performance of similar sapphire, but material processing technology and the processing and the cost etc. of the optical product in later stage are less than the sapphire far away, be good multispectral infrared material that permeates, it is good to have the cost of manufacture low chemical stability, characteristics such as the high rigidity of service temperature height are, be the ideal material of preparation dysmorphism infrared window, radome fairing and infrared night vision lens.
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail below with reference to specific embodiments.
In one exemplary embodiment of the present disclosure, a medium wave infrared glass is provided, and each component of the present embodiment is described in detail below:
example 1:
the medium wave infrared glass is characterized by comprising the following components in percentage by mass:
B2O3 6~10%;GeO 70~81%,Bi2O3 2~6%,La2O3 2~4%,BaO 2~5%,Sb2O3 0.5~4%。
in some embodiments, the composition comprises the following components in percentage by mass:
B2O3 8%;GeO 81%,Bi2O3 4%,La2O3 3%,BaO 3%,Sb2O3 3%。
a preparation process of medium wave infrared glass comprises the following steps:
(1) and (3) melting the ingredients: uniformly stirring the materials of the components according to the proportioning parts, pouring the materials into a crucible, continuously heating at 1380 +/-10 ℃ for 6-10 hours, pouring the materials into the crucible, feeding the materials at the frequency of once per hour, and finishing feeding for 8 times in total;
(2) a clarification stage: controlling the temperature in the crucible to 1410 +/-10 ℃ and keeping the temperature for 6-8 hours, stirring and defoaming in the process, and stirring for four times in total, wherein the specific stirring speed is 60 revolutions per minute, 30 revolutions per minute, 20 revolutions per minute and 10 revolutions per minute in sequence; stirring for 0.5 hour, 3 hours and 0.5 hour in sequence, and precipitating for 4-5 hours after stirring;
(3) and (3) cooling: cooling the temperature in the crucible in the step (2) to 980 +/-10 ℃;
(4) and (3) annealing stage: and (3) putting the raw materials cooled in the step (3) into an annealing furnace, continuously cooling for two times, reducing the temperature to 540 +/-10 ℃ for the first time, preserving the heat for 8-12 hours, reducing the temperature from 540 +/-10 ℃ to 350 +/-10 ℃ for the second time, reducing the temperature by 10 ℃ per hour to 350 ℃ for the second time, powering off, naturally cooling to normal temperature, opening the furnace, and discharging to obtain the glass.
Further, the thickness of the glass is 0.3-60 mm.
Further, the glass has a transmission wavelength range of 0.4 to 6 μm.
Furthermore, the refractive index nd of the glass is within the range of 1.70-1.75, and the Abbe number upsilond is within the range of 32-38.
Further, the electric power of the annealing furnace in the step (4) is 6-30(kW/380V), the gas power is 15-60 kilocalories, and the network speed is controlled to be one of AC excitation speed regulation or variable frequency speed regulation.
Further, the purity of the material adopted in the step (1) is 99.999%.
Further, the clarification stage in the step (2) refers to a process of precipitating the materials after stirring.
The medium wave infrared glass may be used in making specially shaped infrared window, fairing and infrared night vision lens.
Example 2:
the medium wave infrared glass is characterized by comprising the following components in percentage by mass:
B2O3 6~10%;GeO 70~81%,Bi2O3 2~6%,La2O3 2~4%,BaO 2~5%,Sb2O3 0.5~4%。
in some embodiments, the composition comprises the following components in percentage by mass:
B2O3 8%;GeO 81%,Bi2O3 4%,La2O3 3%,BaO 3%,Sb2O3 3%。
a preparation process of medium wave infrared glass comprises the following steps:
(1) and (3) melting the ingredients: uniformly stirring the materials of the components according to the proportioning parts, pouring the materials into a crucible, continuously heating at 1380 +/-10 ℃ for 6-10 hours, pouring the materials into the crucible, feeding the materials at the frequency of once per hour, and finishing feeding for 8 times in total;
(2) a clarification stage: controlling the temperature in the crucible to 1410 +/-10 ℃ and keeping the temperature for 6-8 hours, stirring and defoaming in the process, and stirring for four times in total, wherein the specific stirring speed is 60 revolutions per minute, 30 revolutions per minute, 20 revolutions per minute and 10 revolutions per minute in sequence; stirring for 0.5 hour, 3 hours and 0.5 hour in sequence, and precipitating for 4-5 hours after stirring;
(3) and (3) cooling: cooling the temperature in the crucible in the step (2) to 980 +/-10 ℃;
(4) and (3) annealing stage: and (3) putting the raw materials cooled in the step (3) into an annealing furnace, continuously cooling for two times, reducing the temperature to 540 +/-10 ℃ for the first time, preserving the heat for 8-12 hours, reducing the temperature from 540 +/-10 ℃ to 350 +/-10 ℃ for the second time, reducing the temperature by 10 ℃ per hour to 350 ℃ for the second time, powering off, naturally cooling to normal temperature, opening the furnace, and discharging to obtain the glass.
Further, the thickness of the glass is 0.3-60 mm.
Further, the glass has a transmission wavelength range of 0.4 to 6 μm.
Furthermore, the refractive index nd of the glass is within the range of 1.70-1.75, and the Abbe number upsilond is within the range of 32-38.
Further, the electric power of the annealing furnace in the step (4) is 6-30(kW/380V), the gas power is 15-60 kilocalories, and the network speed is controlled to be one of AC excitation speed regulation or variable frequency speed regulation.
Further, the material purity in the step (1) is 99.999%.
Further, the clarification stage in the step (2) refers to a process of precipitating the materials after stirring.
The medium wave infrared glass may be used in making specially shaped infrared window, fairing and infrared night vision lens.
The glass produced by the present application is compared with conventional glass as follows:
from the table, the medium wave infrared glass prepared by the method has strong chemical stability and strong bending strength, and compared with the glass prepared by the traditional method, the glass prepared by the method has better silhouette in Vickers hardness and large refractive index.
So far, the present embodiment has been described in detail. From the above description, one skilled in the art should clearly recognize the present application.
It is to be understood that implementations not shown or described in the specification are all forms known to those of ordinary skill in the art and are not described in detail. Furthermore, the above definitions of the various elements and methods are not limited to the specific structures, shapes, or configurations shown in the examples.
It is also noted that the illustrations herein may provide examples of parameters that include particular values, but that these parameters need not be exactly equal to the corresponding values, but may be approximated to the corresponding values within acceptable error tolerances or design constraints. Directional terms such as "upper", "lower", "front", "rear", "left", "right", and the like, referred to in the embodiments, are not intended to limit the scope of the present application. In addition, unless steps are specifically described or must occur in sequence, the order of the steps is not limited to that listed above and may be changed or rearranged as desired by the desired design. The embodiments described above may be mixed and matched with each other or with other embodiments based on design and reliability considerations, i.e., technical features in different embodiments may be freely combined to form further embodiments.
The above-mentioned embodiments are further described in detail for the purpose of illustrating the invention, and it should be understood that the above-mentioned embodiments are only illustrative of the present invention and are not to be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The medium wave infrared glass is characterized by comprising the following components in percentage by mass:
B2O36~10%;GeO 70~81%,Bi2O32~6%,La2O3 2~4%,BaO 2~5%,Sb2O30.5~4%。
2. the process for preparing a medium wave infrared glass according to claim 1, comprising the steps of:
(1) and (3) melting the ingredients: uniformly stirring the materials of the components according to the proportioning parts, pouring the materials into a crucible, continuously heating at 1380 +/-10 ℃ for 6-10 hours, pouring the materials into the crucible, feeding the materials at the frequency of once per hour, and finishing feeding for 8 times in total;
(2) a clarification stage: controlling the temperature in the crucible to 1410 +/-10 ℃ and keeping the temperature for 6-8 hours, stirring and defoaming in the process, and stirring for four times in total, wherein the specific stirring speed is 60 revolutions per minute, 30 revolutions per minute, 20 revolutions per minute and 10 revolutions per minute in sequence; stirring for 0.5 hour, 3 hours and 0.5 hour in sequence, and precipitating for 4-5 hours after stirring;
(3) and (3) cooling: cooling the temperature in the crucible in the step (2) to 980 +/-10 ℃;
(4) and (3) annealing stage: and (3) putting the raw materials cooled in the step (3) into an annealing furnace, continuously cooling for two times, reducing the temperature to 540 +/-10 ℃ for the first time, preserving the heat for 8-12 hours, reducing the temperature from 540 +/-10 ℃ to 350 +/-10 ℃ for the second time, reducing the temperature by 10 ℃ per hour to 350 ℃ for the second time, powering off, naturally cooling to normal temperature, opening the furnace, and discharging to obtain the glass.
3. The process of claim 2, wherein the glass has a thickness of 0.3 mm to 60 mm.
4. The process according to claim 3, wherein the glass has a transmission wavelength in the range of 0.4 to 6 μm.
5. The process of claim 3 wherein the glass has a refractive index nd in the range of 1.8356-1.8359 and an Abbe number vd in the range of 26.87 ± 0.02.
6. The process for preparing medium wave infrared glass according to claim 2, wherein the electric power of the annealing furnace in the step (4) is 6-30(kW/380V), the gas power is 15-60 kilocalories, and the network speed is controlled by one of AC excitation speed regulation or variable frequency speed regulation.
7. The process of claim 2, wherein the material has a purity of 99.999%.
8. The process according to claim 7, wherein the fining stage in step (2) is a process of stirring and precipitating the material.
9. Use of a medium wave infrared glass according to claim 1 for the production of shaped infrared windows, fairings and infrared night vision lenses.
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CN101508526A (en) * | 2009-03-11 | 2009-08-19 | 昆明理工大学 | Bismuth doped germanium-zinc-boron glass and method of producing the same |
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2018
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JP2002274882A (en) * | 2001-03-16 | 2002-09-25 | National Institute Of Advanced Industrial & Technology | Transition metal-containing chalcogenide glass illuminant |
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