CN212181064U - Germanium-based 8-12um infrared window sheet - Google Patents

Germanium-based 8-12um infrared window sheet Download PDF

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CN212181064U
CN212181064U CN202020703766.7U CN202020703766U CN212181064U CN 212181064 U CN212181064 U CN 212181064U CN 202020703766 U CN202020703766 U CN 202020703766U CN 212181064 U CN212181064 U CN 212181064U
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film
germanium
thickness
window sheet
substrate
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姜海
侯强
刘瑞斌
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Liaoning Beiyu Vacuum Science & Technology Co ltd
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沈阳北理高科技有限公司
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Abstract

The utility model belongs to the optical film field, concretely relates to germanium basement 8-12um infrared window piece. The window sheet takes single crystal germanium as a substrate, two sides of the substrate are plated with single-layer antireflection film structures, and the incident angles of the two film structures are defined as 0 +/-10 degrees. The window piece can be applied to an 8-12um infrared detection system and can also be applied to a night vision device, and the manufacturing period and the manufacturing cost of the window piece are greatly reduced due to the advantages of simple coating design, common coating material, high film firmness and the like.

Description

Germanium-based 8-12um infrared window sheet
Technical Field
The utility model belongs to the optical film field, concretely relates to germanium basement 8-12um infrared window piece.
Background
An 8-12um infrared window sheet is a common infrared passive device and is used for isolating an internal system of a detector from an external environment. At present, the period and cost for manufacturing a window sheet are restricted by the selection of a substrate material and the selection of an antireflection film material in practical application, a conventional infrared antireflection film generally selects germanium and ytterbium fluoride as high-refractive index and low-refractive index materials, the designed layer number is 6-8, the thickness is 3-4um, such as CN108627889 published in 2018, 10, 9 and the transmittance of the conventional infrared antireflection film is about 94%, 8 irregular film layers need to be deposited on two surfaces of the substrate respectively, the film layers are more, the thickness is thicker, the preparation cost is high, the production time is long, and the conventional infrared antireflection film is not beneficial to large-scale popularization.
SUMMERY OF THE UTILITY MODEL
Utility model purpose:
the utility model aims to reduce the production cost of manufacturing 8-12um infrared window sheets and provide a germanium substrate 8-12um infrared window sheet with low cost performance and high transmissivity.
The technical scheme is as follows:
the utility model discloses a realize through following technical scheme:
an infrared window sheet with a germanium substrate of 8-12um is characterized in that single-crystal germanium is used as the substrate of the window sheet, and both sides of the substrate are plated with single-layer antireflection film structures.
Furthermore, the thickness of the film layer is 1.083-1.162um when the antireflection film is made of zinc sulfide material, and the thickness of the film layer is 1.090-1.145um when the antireflection film is made of KRS-6 material.
Furthermore, the average transmittance of the infrared window sheet is greater than 95%, and the extreme value transmittance is greater than 98%.
Furthermore, the thickness of the single crystal germanium ranges from 10 mm to 30 mm in diameter and 1 mm to 2 mm in thickness.
Further, the incident angles of the antireflection film structures on both sides of the window sheet are defined to be between 0 ° ± 10 °.
The advantages and effects are as follows:
the utility model has the advantages of as follows and beneficial effect:
the window piece can be applied to an 8-12um infrared detection system and can also be applied to a night vision device, and the window piece greatly reduces the period and cost for manufacturing the window piece due to the advantages of simple coating design, common coating material and high film firmness.
Compare and set up the multilayer in prior art, the utility model discloses select zinc sulfide or KRS-6 material, the design number of piles is 1 layer, and rete thickness is 1.083-1.162um when the antireflection coating is the zinc sulfide material, and rete thickness is 1.090-1.145um when the antireflection coating is KRS-6 material, and average transmissivity is greater than 95%, and extreme value transmissivity is greater than 98%. Saving cost, reducing the steps of the preparation process and the production time, and being beneficial to expanding production.
Drawings
Fig. 1 is a schematic structural view of a window sheet of the present invention;
FIG. 2 is a spectrum of a germanium wafer without an anti-reflection coating;
FIG. 3 is a spectrum of a single-layer zinc sulfide double-coated film of example 1;
FIG. 4 is a spectrum of a single-layer zinc sulfide double-coated film of example 2;
FIG. 5 is a spectrum of a single-layer zinc sulfide double-coated film obtained in example 3;
FIG. 6 is a spectrum of a single-layer zinc sulfide double-coated film of example 4;
FIG. 7 is a spectrum of KRS-6 coated on both sides with a single layer in example 5;
FIG. 8 is a spectrum of KRS-6 coated on both sides with a single layer in example 6;
FIG. 9 is a spectrum of KRS-6 coated on both sides with a single layer in example 7;
FIG. 10 is a spectrum of KRS-6 coated on both sides with a single layer in example 8;
FIG. 11 is a spectrum of a film with a thickness of 0.96 μm obtained when zinc sulfide is used as the coating material in example 9;
FIG. 12 is a spectrum of a film thickness of 1.25 μm when zinc sulfide is used as the coating material in example 9;
FIG. 13 is a spectrum of KRS-6 as the coating material in example 9, with a film thickness of 0.96 um;
FIG. 14 is a spectrum of a film with a thickness of 1.25um obtained by using KRS-6 as the coating material in example 9.
Description of reference numerals:
1. monocrystalline germanium, 2, antireflection coating structure.
Detailed Description
As shown in figure 1, the infrared window sheet with a germanium substrate of 8-12um takes single-crystal germanium as the substrate, and both sides of the substrate are plated with a single-layer antireflection film structure.
The utility model discloses a single crystal germanium 1 is the basement, and zinc sulfide or KRS-6 are as coating material, and the both sides of basement have all plated individual layer antireflection coating structure 2, greatly reduced the cycle and the cost of window piece preparation.
The thickness of the film layer is 1.083-1.162um when the anti-reflection film is made of zinc sulfide material, and the thickness of the film layer is 1.090-1.145um when the anti-reflection film is KRS-6 material.
The utility model discloses it is the important factor of simple and easy antireflection coating design to use zinc sulfide, KRS-6 as film material, and its two-sided coating back 8-12um average transmittance is greater than 95%.
The infrared window sheet of the utility model is mainly designed to be more superior in single-layer coating on two sides of the substrate and the material of the adopted antireflection film, and the transmissivity is better when the film layer is simplified.
The average transmissivity of the infrared window sheet is greater than 95%, and the extremum transmissivity is greater than 98%.
The transmissivity of zinc sulfide material and KRS-6 material (44.4% TlBr and 55.6% TlCl) as antireflection films can be greatly improved.
The thickness of the single crystal germanium 1 as a substrate is in the range of 10 to 30 mm in diameter and 1 to 2 mm in thickness.
The incident angles of the antireflection film structures 2 on both sides of the window sheet are both defined to be between 0 ° ± 10 °.
A preparation method of an infrared window sheet with a germanium substrate of 8-12um comprises the following steps:
the method comprises the following steps: preparing a substrate: wiping the surface of the monocrystalline germanium, placing the wiped lens into a wafer support, and placing the wafer support on a workpiece disc of an existing film plating machine.
Ethanol and diethyl ether (6-8) are adopted for wiping in the first step: (4-2) wiping the surface of the monocrystalline germanium by using the solution with the volume ratio; the antireflection film material is zinc sulfide or KRS-6;
the purity of the zinc sulfide material is 99.99 percent; KRS-6 is a mixture of 44.4% thallium bromide and 55.6% thallium chloride by mass fraction.
Step two: preparation before plating: placing the anti-reflection film material in a thermal evaporation crucible, vacuumizing the background of the vacuum chamber, and pre-melting the anti-reflection film material in a molten state.
And the vacuumizing condition in the second step is that the background of the vacuum chamber is vacuumized to (0.8-1.0) E-3Pa, the temperature of a deposition area is 130-150 ℃, and the constant temperature is kept for 30-40 min.
Step three: film coating: coating by adopting a vacuum thermal evaporation method;
two sides of the single crystal germanium substrate are respectively plated with 1 layer of antireflection film structure 2, and the two sides are plated with films;
setting the thickness of a coating film, wherein the thickness of the coating film is 1.083-1.162um when the antireflection film is made of a zinc sulfide material, and the thickness of the coating film is 1.090-1.145um when the antireflection film is made of a KRS-6 material.
The third concrete step is:
step a: presetting coating conditions before coating; the coating conditions of the step a are that the central wavelength of the antireflection film is 10 +/-0.01 um, the incident angle range is 0 +/-10 degrees, and the medium air is incident.
Step b: controlling the evaporation rate of the anti-reflection film material by using a quartz crystal film thickness controller; and b, controlling the evaporation rate to be 1-1.2 nm/s, controlling the thermal evaporation voltage to be 5-6V, controlling the current to be 800-plus-one 1000A, controlling the argon partial pressure to be (2.0-2.5) E-2Pa, maintaining the indoor vacuum to be (2.1-2.6) E-2Pa, and controlling the argon filling amount to be 20-40 SCCM by the quartz crystal film thickness controller.
Step c: heating the thermal evaporation crucible to a glowing state, opening a baffle plate, and starting coating; bombarding the film layer by using a Hall ion source to increase the compactness of the film layer. And c, ion energy adopted by the Hall ion source in the step c is 200-250 eV, ion beam current is 30-40 mA, and ion distribution deviation is 15-20%.
As shown in fig. 2, the transmittance of the germanium sheet without the antireflection film is only 46.9%.
Example 1
As shown in fig. 1 and fig. 3, an infrared window sheet with a germanium substrate of 8-12um has a single-crystal germanium substrate, and both sides of the substrate are plated with a single-layer antireflection film structure of zinc sulfide material with a wavelength of 8-12 um.
The thickness of the single crystal germanium is 20 mm in diameter and 1 mm in thickness.
A method for manufacturing an infrared window sheet with a germanium substrate of 8-12um comprises the following steps:
the method comprises the following steps: preparing a substrate: wiping the surface of the monocrystalline germanium, putting the wiped lens into a plate support, and putting the plate support on a workpiece disc of a film coating machine; wiping in step one was performed with ethanol and diethyl ether 6: 4, wiping the surface of the monocrystalline germanium by the solution matched with the volume ratio.
Step two: preparation before plating: placing the massive zinc sulfide material in a thermal evaporation crucible, vacuumizing the bottom of a vacuum chamber, and pre-melting the massive zinc sulfide material in a molten state; the purity of the blocky zinc sulfide in the second step is 99.99%. The vacuum-pumping condition is that the background of the vacuum chamber is vacuumized to 1.0 × E-3Pa, the temperature of the deposition area is 140 ℃, and the constant temperature is kept for 35 min.
Step three: film coating: and coating by adopting a vacuum thermal evaporation method.
The third concrete step is:
step a: presetting coating conditions before coating; the film plating conditions of the step a are that the central wavelength of the antireflection film is 10 mu m, the incident angle is 0 degree, the medium air is incident, and the thickness of the zinc sulfide is 1.13 mu m.
Step b: controlling the evaporation rate of zinc sulfide by using a quartz crystal film thickness controller; and c, controlling the evaporation rate to be 1.2 nm/s, controlling the thermal evaporation voltage to be 5V, controlling the current to be 800A, controlling the argon partial pressure to be 2.0E-2 Pa, maintaining the indoor vacuum to be 2.1E-2 Pa, and controlling the argon filling amount to be 20SCCM by the quartz crystal film thickness controller.
Step c: heating the thermal evaporation crucible to a glowing state, opening a baffle plate, and starting coating; bombarding the film layer by using a Hall ion source to increase the compactness of the film layer. And c, coating 1 zinc sulfide film layer on two sides.
And c, the Hall ion source adopts ion energy of 200 eV, ion beam current of 30 mA and ion distribution deviation of 15%.
As shown in fig. 3, measurement: the sample spectra were measured using an FTIR-850 Fourier Infrared spectrometer and found to be 1.13um thick with a maximum transmission of 98.68% and an average transmission of 95.24% between 8 and 12um at 0 incident.
Example 2
As shown in fig. 4, an infrared window sheet with a germanium substrate of 8-12um has a single-crystal germanium substrate, and both sides of the substrate are plated with a single-layer zinc sulfide antireflection film structure with a wavelength of 8-12 um.
The antireflection film had a single layer thickness of 1.09um, and the same preparation method as in example 1 was used, except that the maximum transmittance was 98.67%, and the average transmittance was 95.09% at 8 to 12 um.
Example 3
As shown in fig. 5, the antireflection film was 1.083um in monolayer thickness, and the same preparation method as in example 1 was used, except that the maximum transmittance was 98.67%, and the average transmittance was 95.01% between 8 and 12 um.
Example 4
As shown in FIG. 6, the antireflection film had a single layer thickness of 1.162um, and the same preparation method as in example 1 was used, with a maximum transmittance of 98.69% and an average transmittance of 95.01% between 8 and 12 um.
Example 5
As shown in fig. 1 and 7, an infrared window sheet with a germanium substrate of 8-12um has a single-crystal germanium substrate, and both sides of the substrate are plated with a single-layer KRS-6 antireflection film structure with a wavelength of 8-12 um.
The thickness of the single crystal germanium is in the range of 20 mm in diameter and 1 mm thick.
A method for manufacturing an infrared window sheet with a germanium substrate of 8-12um comprises the following steps:
the method comprises the following steps: preparing a substrate: wiping the surface of the monocrystalline germanium, putting the wiped lens into a plate support, and putting the plate support on a workpiece disc of a film coating machine; wiping in step one was performed with ethanol and diethyl ether 6: 4, wiping the surface of the monocrystalline germanium by the solution matched with the volume ratio.
Step two: preparation before plating: putting the block KRS-6 material in a thermal evaporation crucible, vacuumizing the background of a vacuum chamber, and pre-melting the block KRS-6 material to be in a molten state; KRS-6 is a mixture of 44.4% thallium bromide and 55.6% thallium chloride by mass fraction. The vacuum-pumping condition is that the background of the vacuum chamber is vacuumized to 1.0 × E-3Pa, the temperature of the deposition area is 140 ℃, and the constant temperature is kept for 35 min.
Step three: film coating: and coating by adopting a vacuum thermal evaporation method.
The third concrete step is:
step a: presetting coating conditions before coating; and a coating condition in the step a is that the central wavelength of the antireflection film is 10um, the incident angle is 0 degree, the medium air is incident, and the thickness of KRS-6 is 1.10 um.
Step b: controlling the KRS-6 evaporation rate by using a quartz crystal film thickness controller; and c, controlling the evaporation rate to be 1.2 nm/s, controlling the thermal evaporation voltage to be 5V, controlling the current to be 800A, controlling the argon partial pressure to be 2.0E-2 Pa, maintaining the indoor vacuum to be 2.1E-2 Pa, and controlling the argon filling amount to be 20SCCM by the quartz crystal film thickness controller.
Step c: heating the thermal evaporation crucible to a glowing state, opening a baffle plate, and starting coating; bombarding the film layer by using a Hall ion source to increase the compactness of the film layer. And c, coating 1 layer of KRS-6 film on two sides.
And c, the Hall ion source adopts ion energy of 200 eV, ion beam current of 30 mA and ion distribution deviation of 15%.
Finally, measurement: the sample spectrum was measured using an FTIR-850 Fourier Infrared spectrometer and found to be 1.10um thick with a maximum transmission of 98.53% and an average transmission of 95.07% between 8 and 12um at 0 incident.
Example 6
As shown in FIG. 8, a single layer of KRS-6 was plated on both sides with a thickness of 1.13 μm, and the other conditions were the same as those in example 5. The sample spectra were tested using FTIR-850 Fourier Infrared Spectroscopy with a maximum transmittance of 98.54% and an average 8-12um transmittance of 95.10%.
Example 7
As shown in FIG. 9, a single layer of KRS-6 was plated on both sides with a thickness of 1.09. mu.m, and other conditions were the same as in example 5. The sample spectrum was measured using FTIR-850 Fourier Infrared Spectroscopy with a maximum transmittance of 98.52% and an average transmittance of 8-12um of 95.00%
Example 8
As shown in FIG. 10, a single layer of KRS-6 was plated on both sides with a thickness of 1.145. mu.m, and the other conditions were the same as in example 5. The sample spectra were tested using FTIR-850 Fourier Infrared Spectroscopy with a maximum transmittance of 98.54% and an average 8-12um transmittance of 95.00%.
As can be seen from FIGS. 2 to 10, the transmittance of the infrared window of the present invention is better between the wavelengths of 9 to 10.5 μm.
Example 9
Zinc sulfide control:
as shown in fig. 11, when the antireflection film is a zinc sulfide material and the film thickness is 0.96um, the other conditions are the same as in example 1, and the preparation method is also the same, the maximum transmittance is 98.61%, and the average transmittance between 8 and 12um is 91.12%.
As shown in fig. 12, when the antireflection film is made of zinc sulfide, and the film thickness is 1.25um, the other conditions are the same as those in example 1, and the preparation method is also the same, the maximum transmittance is 98.72%, and the average transmittance between 8 and 12um is 92.84%.
As shown in fig. 11-12, the average transmittance is significantly reduced by a large margin, except that the thickness of the film layer exceeds the limit of the present invention.
KRS-6 Material control group:
as shown in fig. 13, when the antireflection film is KRS-6 material and the film thickness is 0.96um, the other conditions are the same as those in example 5, the preparation method is also the same, the maximum transmittance is 98.48%, and the average transmittance between 8 and 12um is 91.19%.
As shown in fig. 14, when the antireflection film is KRS-6 material and the film thickness is 1.25um, the other conditions are the same as those in example 5, and the preparation method is also the same, the maximum transmittance is 98.61%, and the average transmittance between 8-12um is 92.53%.
As shown in fig. 13-14, the average transmittance is significantly reduced by a large margin, except that the thickness of the film layer exceeds the limit of the present invention.
The above detailed description further illustrates the objects, technical solutions and advantages of the present invention, and it should be understood that the above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (4)

1. The utility model provides an infrared window piece of germanium basement 8-12um which characterized in that: the window sheet takes single crystal germanium as a substrate, and both sides of the substrate are plated with single-layer antireflection film structures;
the thickness of the film layer is 1.083-1.162um when the antireflection film is made of zinc sulfide material, and the thickness of the film layer is 1.090-1.145um when the antireflection film is KRS-6 material.
2. A germanium-based 8-12um infrared window sheet according to claim 1, wherein: the average transmittance of the infrared window sheet is greater than 95%, and the extreme value transmittance is greater than 98%.
3. A germanium-based 8-12um infrared window sheet according to claim 1, wherein: the thickness of the monocrystalline germanium is in the range of 10-30 mm in diameter and 1-2 mm in thickness.
4. A germanium-based 8-12um infrared window sheet according to claim 1, wherein: the incident angles of the antireflection film structures on both sides of the window sheet are defined to be 0 +/-10 degrees.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111443404A (en) * 2020-04-30 2020-07-24 沈阳北理高科技有限公司 Germanium-based 8-12um infrared window sheet and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111443404A (en) * 2020-04-30 2020-07-24 沈阳北理高科技有限公司 Germanium-based 8-12um infrared window sheet and preparation method thereof

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