CN109143440B - 3.50-3.90 mu m medium wave infrared micro filter and preparation method thereof - Google Patents

3.50-3.90 mu m medium wave infrared micro filter and preparation method thereof Download PDF

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CN109143440B
CN109143440B CN201811308604.7A CN201811308604A CN109143440B CN 109143440 B CN109143440 B CN 109143440B CN 201811308604 A CN201811308604 A CN 201811308604A CN 109143440 B CN109143440 B CN 109143440B
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germanium
zinc sulfide
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王济洲
王小军
李凯朋
王云飞
许斌
杨登强
汪洋
杨子文
王际充
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Wuxi Hongrui Aerospace Technology Co ltd
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Abstract

The invention belongs to the technical field of surfaces, and particularly relates to a 3.50-3.90-micrometer medium-wave infrared micro filter and a preparation method thereof. The optical filter comprises a silicon substrate and long and short wave pass film systems; the structure of the long-wave pass film system is (0.35H0.7L0.35H) ^9(0.5HL0.5H) ^13, and the central wavelength is 2800 nm; the short wave pass film system structure is (0.5LH0.5L) ^13, and the central wavelength is 4650 nm; h and L are a germanium film layer and a zinc sulfide film layer respectively; heating a silicon substrate in vacuum, depositing long and short wave through film systems on two sides of the substrate by an ion beam assisted electron gun evaporation method, and cooling to obtain the silicon substrate. The optical filter has high transmittance in a spectral band of 3.50-3.90 mu m, can cut off in spectral bands of 0.80-3.30 mu m and 4.10-5.50 mu m, can be used at a low temperature (80K), and meets the splicing requirement in a space micro combined optical filter.

Description

3.50-3.90 mu m medium wave infrared micro filter and preparation method thereof
Technical Field
The invention belongs to the technical field of optical films, and particularly relates to a 3.50-3.90 mu m medium wave infrared micro filter and a preparation method thereof.
Background
In the space micro combined filter of the current remote sensing detection system, a key filter meeting the following requirements is urgently needed: (1) has high transmittance in the spectrum range of 3.50 to 3.90 μm; (2) the spectral bands of 0.80-3.30 μm and 4.10-5.50 μm have the function of inhibiting optical signals, so that the spectral bands of 0.80-3.30 μm and 4.10-5.50 μm are cut off in width to reduce the influence of signal noise; (3) can be used at low temperature (80K); (4) the size of the substrate is small, the included angle between all surfaces of the substrate is a right angle, no chamfer exists, and the quality problems of films such as film forming or film falling are not generated when the films are spliced, so that the splicing requirement in the space micro combined optical filter is met.
The retrieved closer comparison document (CN103245994B) discloses a long-wave infrared filter with the transmission of 8-8.4 microns and a preparation method thereof, wherein the filter comprises a germanium substrate, a long-wave pass film system on one side of the substrate and a short-wave pass film system on the other side of the substrate; the structure of the long-wave pass membrane system is as follows: (0.5LH0.5L) ^10(0.57L1.14H0.57L) ^6, center wavelength is 5680nm, short wave pass film system structure is: (LH) ^10 with a central wavelength of 10900nm, wherein L and H are respectively a zinc sulfide film layer and a lead telluride film layer in sequence; heating a substrate in vacuum, depositing long and short wave through film systems on two sides of the substrate by resistance evaporation under the condition of introducing argon into an ion source, and cooling to obtain the film. However, the above-mentioned disclosed mid-wave infrared filter has a relatively narrow cut-off width, and cannot satisfy the requirements of a mid-wave infrared filter having a high transmittance in the 3.50 to 3.90 μm band and a wide cut-off in the 0.80 to 3.30 μm and 4.10 to 5.50 μm bands; meanwhile, the existing medium-wave infrared filter is mainly formed by two oxides with low difference between high refractive index and low refractive index, and has the characteristics of more film layers, large film stress and the like, so that the problems of film layer breakage, film rising and the like can be caused when the medium-wave infrared filter is plated on a micro substrate, and the requirements of splicing and low-temperature use in a space micro combined filter of a remote sensing detection system can not be met.
Disclosure of Invention
The invention aims to solve the problems and provides a 3.50-3.90 μm medium-wave infrared micro filter which has high transmittance in a spectrum band of 3.50-3.90 μm, has wide cut-off in a spectrum band of 0.80-3.30 μm and 4.10-5.50 μm and can be used at a low temperature (80K) and a preparation method thereof.
The specific technical scheme is as follows:
a3.50-3.90 μm medium-wave infrared micro-filter comprises a silicon substrate, a long-wave pass film system on one side of the silicon substrate, and a short-wave pass film system on the other side of the silicon substrate;
the specification of the silicon substrate is 29.5mm 1.6mm 1.2mm, the parallelism is less than 30', the long-wave pass film system is formed by alternately superposing germanium (Ge) film layers and zinc sulfide (ZnS) film layers, and the structure of the long-wave pass film system is as follows: (0.35H0.7L0.35H) ^9(0.5HL0.5H) ^13 with center wavelength 2800 nm; h represents a germanium film layer thickness of 1 base thickness, 0.5H represents a germanium film layer thickness of 0.5 base thickness, 0.35H represents a germanium film layer thickness of 0.35 base thickness, L represents a zinc sulfide film layer thickness of 1 base thickness, 0.7L represents a zinc sulfide film layer thickness of 0.7 base thickness, 9 is the number of cycles of the base film stack (0.35H0.7L0.35H), and 13 is the number of cycles of the base film stack (0.5 HL0.5H);
the short wave-passing film system is formed by alternately superposing germanium and zinc sulfide film layers, and the structure of the short wave-passing film system is as follows: (0.5LH0.5L) ^13 with center wavelength of 4650 nm; wherein H represents that the thickness of the germanium film layer is 1 basic thickness, L represents that the thickness of the zinc sulfide film layer is 1 basic thickness, 0.5L represents that the thickness of the zinc sulfide film layer is 0.5 basic thickness, and 13 represents the cycle number of the basic film stack (0.5 LH0.5L);
the basic thickness is one fourth of the optical thickness center wavelength of the long wave passing film system or the short wave passing film system. In certain embodiments, the silicon substrate has a gauge of 29.5mm 1.6mm 1.2mm and a parallelism of less than 30 ".
In some embodiments, the long wave pass film is as shown in table 1, and the film layer with the number of layers 1 is the outermost layer, and the film layer with the number of layers 45 is deposited on the silicon substrate as the innermost layer.
TABLE 1 Long wavelength pass film series
Figure GDA0002953703670000031
Figure GDA0002953703670000041
In some embodiments, the shortwave pass film is as shown in table 2, with the film layer number 1 being the outermost layer and the film layer number 27 being the innermost layer deposited on the silicon substrate.
TABLE 2 short wave pass membrane system
Number of layers Film material Film thickness/nm
1 Zinc sulfide 659.9517
2 Germanium (Ge) 303.1252
3 Zinc sulfide 527.663
4 Germanium (Ge) 303.4779
5 Zinc sulfide 506.0659
6 Germanium (Ge) 286.562
7 Zinc sulfide 512.5365
8 Germanium (Ge) 287.3251
9 Zinc sulfide 508.7516
10 Germanium (Ge) 281.9393
11 Zinc sulfide 517.6755
12 Germanium (Ge) 279.3932
13 Zinc sulfide 503.467
14 Germanium (Ge) 290.1305
15 Zinc sulfide 512.0884
16 Germanium (Ge) 273.1541
17 Zinc sulfide 515.9556
18 Germanium (Ge) 286.7169
19 Zinc sulfide 513.9143
20 Germanium (Ge) 282.5536
21 Zinc sulfide 504.1142
22 Germanium (Ge) 288.6436
23 Zinc sulfide 530.8378
24 Germanium (Ge) 291.8134
25 Zinc sulfide 511.3925
26 Germanium (Ge) 275.2112
27 Zinc sulfide 285.4052
The preparation method of the 3.50-3.90 mu m medium wave infrared micro filter comprises the following steps:
(1) putting the clean silicon substrate into a clean vacuum chamber, and vacuumizing to less than or equal to 3 multiplied by 10-5Torr;
(2) Heating the silicon substrate to 200 ℃ and keeping the temperature for 30 min;
(3) opening a Hall source type ion source, and bombarding and cleaning the silicon substrate for 10min by using an ion beam, wherein the working gas of the ion source is argon, and the gas flow is 17 sccm;
(4) opening a Hall source type ion source, and respectively and alternately depositing the germanium film layer and the zinc sulfide film layer in the long-wave-pass film system layer by layer on one side of the silicon substrate by adopting an ion beam assisted electron gun evaporation method, and alternately depositing the germanium film layer and the zinc sulfide film layer in the short-wave-pass film system layer by layer on the other side of the silicon substrate until the deposition of the film system is completed; the deposition rate of the germanium film layer is 1.0nm/s, the deposition rate of the zinc sulfide film layer is 0.8nm/s, the ion source working gas is argon, the gas flow is 17sccm, and the film thickness is monitored by a quartz crystal film thickness controller;
(5) and naturally cooling the silicon substrate to room temperature to obtain the 3.50-3.90 mu m medium wave infrared micro filter.
The invention has the following beneficial effects: compared with the prior art and 1, the invention provides a 3.50-3.90 μm medium-wave infrared micro-filter which is formed by alternately superposing a germanium film layer with a high refractive index and zinc sulfide with a low refractive index, and the optical filter prepared under proper preparation conditions has excellent technical indexes: the spectral band of 3.50-3.90 μm has high transmittance of more than or equal to 90%, and the spectral band of 0.8-3.3 μm and 4.10-5.50 μm is cut off, and the average transmittance in the cut-off region is less than 1%, so that the characteristics of the pass band and the cut-off band of the spectral band filter can be greatly improved, and the use requirement of a remote sensing detection system can be met; 2. the invention provides a preparation method of a 3.50-3.90 mu m medium wave infrared micro optical filter, which adopts germanium and zinc sulfide as film layer materials, the number of the film layers of the prepared optical filter is small, the thickness of the film layer can meet the plating requirements on two surfaces of a micro substrate (with the length of 29.5mm, the width of 1.6mm and the thickness of 1.2mm), and the use requirements of space micro combined optical filter splicing, working at low temperature (80K) and the like are met; 3. the invention provides a 3.50-3.90 mu m medium wave infrared micro filter, which is particularly suitable for a micro combined filter of a full spectrum camera and the like in a space remote sensing system.
Drawings
FIG. 1 is a theoretical transmission spectrum of a long-wave pass film system of a 3.50-3.90 μm medium-wave infrared micro filter in an embodiment of the present invention;
FIG. 2 is a theoretical transmission spectrum of a short-wave pass film system of a 3.50-3.90 μm mid-wave infrared micro filter in the embodiment of the present invention;
FIG. 3 is a theoretical transmission spectrum of a 3.50-3.90 μm medium-wave infrared micro-filter in the embodiment of the present invention;
FIG. 4 is a transmission spectrum of a 3.50-3.90 μm medium-wave infrared micro-filter prepared by the preparation method in the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.
The specific technical scheme is as follows:
a3.50-3.90 μm medium wave infrared micro filter comprises a silicon substrate, a long wave pass film system on one side of the silicon substrate and a short wave pass film system on the other side of the silicon substrate;
in this example the substrate is 29.5mm long, 1.6mm wide and 1.2mm thick, preferably the substrate has a parallelism of <30 "; the long-wave pass film system is formed by alternately superposing a germanium (Ge) film layer and a zinc sulfide (ZnS) film layer; the structure of the long-wave passing membrane system is as follows: (0.35H0.7L0.35H) ^9(0.5HL0.5H) ^13 with center wavelength 2800 nm; wherein, H is a germanium film layer, 0.5 is a coefficient of the thickness of the germanium film layer corresponding to the basic thickness, 0.5H represents that the thickness of the germanium film layer is 0.5 basic thicknesses, L is a zinc sulfide film layer, 1 is a coefficient of the thickness of the zinc sulfide film layer corresponding to the basic thickness, L represents that the thickness of the zinc sulfide film layer is 1 basic thickness, the basic thickness is one fourth of the central wavelength of the optical thickness of the long-wave passing film system, 9 is the period number of the basic film stack (0.35H0.7L0.35H), and 13 is the period number of the basic film stack (0.5 HL0.5H).
And optimizing the structure of the long-wave pass film system by using Macleod software to obtain the optimal long-wave pass film system, wherein the film layer with the number of layers 1 is the outermost layer of the long-wave pass film system, and the film layer with the number of layers 45 is deposited on the silicon substrate and is the innermost layer of the long-wave pass film system as shown in Table 1.
TABLE 1 Long wavelength pass film series
Figure GDA0002953703670000071
Figure GDA0002953703670000081
A theoretical transmission spectrum diagram of the long-wave pass film system can be obtained by analyzing the data in the table 1 by Macleod software, and as shown in the diagram 1, the long-wave pass film system has a wide cut-off in a spectrum band of 0.80-3.30 μm and high transmittance in a spectrum band of 4.10-5.50 μm.
The short wave pass film system is formed by alternately overlapping germanium and zinc sulfide film layers, and the structure of the short wave pass film system is as follows: (0.5LH0.5L) ^13 with center wavelength of 4650 nm; wherein H is a germanium film layer, 1 is a coefficient of the thickness of the germanium film layer corresponding to the basic thickness, H represents that the thickness of the germanium film layer is 1 basic thickness, L is a zinc sulfide film layer, 0.5 is a coefficient of the thickness of the zinc sulfide film layer corresponding to the basic thickness, and 0.5L represents that the thickness of the zinc sulfide film layer is 0.5 basic thickness; the basic thickness is one fourth of the center wavelength of the optical thickness of the short wave-pass film system, and 13 is the period number of the basic film stack (0.5 LH0.5L).
And optimizing the structure of the short wave pass film system by adopting Macleod software to obtain an optimal short wave pass film system, wherein the film layer with the number of layers of 1 is the outermost layer of the short wave pass film system, and the film layer with the number of layers of 27 is deposited on the silicon substrate and is the innermost layer of the short wave pass film system as shown in Table 2.
TABLE 2 short wave pass membrane system
Figure GDA0002953703670000082
Figure GDA0002953703670000091
A theoretical transmission spectrum diagram of the short-wave-pass film system can be obtained by analyzing data in the table 2 by using Macleod software, and as shown in the diagram 2, the short-wave-pass film system has a wide cut-off in a spectrum band of 4.10-5.5 μm and has high transmittance in a spectrum band of 3.50-3.90 μm.
The 3.50-3.90 mu m medium wave infrared micro filter in the embodiment is prepared by adopting an Intergrity-39 full-automatic optical coating machine system of DENTON company in America, and the specific steps are as follows:
(1) removing impurities in the vacuum chamber by using a dust collector, and then wiping the inner wall of the vacuum chamber by using absorbent gauze dipped with absolute ethyl alcohol; performing microwave ultrasonic treatment on the substrate with anhydrous acetone for 15min, performing microwave ultrasonic treatment on the substrate with anhydrous ethanol for 15min, wiping the substrate with absorbent cotton, mounting the cleaned substrate on a fixture, rapidly loading the fixture into a clean vacuum chamber, and vacuumizing to 3 × 10-5 Torr;
(2) heating the substrate to 200 ℃ and keeping for 30 min;
(3) bombarding and cleaning the substrate for 10min by using an ion beam, wherein the working gas of an ion source is argon, the gas flow is 17sccm, and the model of the ion source is CC-105 of a Hall source type;
(4) alternately depositing a zinc sulfide film layer and a yttrium fluoride film layer in a long-wave pass film system layer by layer on one side of a substrate by an ion beam assisted electron gun evaporation method according to data in table 1; alternately depositing a zinc sulfide film layer and a yttrium fluoride film layer in the short wave-passing film system layer by layer on the other side of the substrate according to the data in the table 2 to finish the deposition of the film system;
the deposition rate of the zinc sulfide film layer is 2.0nm/s, the deposition rate of the yttrium fluoride film layer is 0.8nm/s, the working gas of the ion source is argon, the gas flow is 17sccm, the model of the ion source is Hall source type CC-105, and the film thickness is monitored by an Inficon IC/5 quartz crystal film thickness controller;
(5) and naturally cooling the substrate to room temperature to obtain the 3.50-3.90 mu m medium-wave infrared micro-filter.
The following performance tests were performed on the filters:
(1) the transmission spectrum of the optical filter is measured by adopting a Lambda900 type spectrophotometer of the American PE company under the low-temperature environment with the test temperature of 80K and is shown in figure 3, and UVWINLAB software is used for calculating the spectral line in the figure 3, so that the average transmittance of the optical filter in a spectral band of 0.80-3.30 mu m is 0.09%, the average transmittance in a spectral band of 4.10-5.50 mu m is 0.05%, and the average transmittance in a spectral band of 3.50-3.90 mu m is 93.50%.
(2) The method is characterized in that a test is carried out according to test requirements on film surface quality, adhesive force and environment in the ministry of astronautics standard 'QJ 1697-89', the test result meets the standard specification, and the optical filter meets the spectrum and splicing requirements of the space micro combined optical filter on a high-transmittance optical filter with a spectrum band of 3.50-3.90 mu m.
In summary, the 3.50-3.90 μm medium wave infrared micro-filter and the preparation method thereof provided by the invention can effectively meet the requirements of high transmittance in a spectrum section of 3.50-3.90 μm, wide cut-off in a spectrum section of 0.80-3.30 μm and 4.10-5.50 μm, low temperature (80K) use and splicing in the spatial micro-combined filter.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the invention, and the present invention is not limited to the above examples, and those skilled in the art should also be able to make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.

Claims (4)

1. A3.50 ~ 3.90 mu m medium wave infrared microfilter is characterized in that: the optical filter consists of a silicon substrate, a long-wave pass film system on one side of the silicon substrate and a short-wave pass film system on the other side of the silicon substrate;
the specification of the silicon substrate is 29.5mm 1.6mm 1.2mm, the parallelism is less than 30', the long-wave pass film system is formed by alternately superposing germanium (Ge) film layers and zinc sulfide (ZnS) film layers, and the structure of the long-wave pass film system is as follows: (0.35H0.7L0.35H) ^9(0.5HL0.5H) ^13 with center wavelength 2800 nm; h represents a germanium film layer thickness of 1 base thickness, 0.5H represents a germanium film layer thickness of 0.5 base thickness, 0.35H represents a germanium film layer thickness of 0.35 base thickness, L represents a zinc sulfide film layer thickness of 1 base thickness, 0.7L represents a zinc sulfide film layer thickness of 0.7 base thickness, 9 is the number of cycles of the base film stack (0.35H0.7L0.35H), and 13 is the number of cycles of the base film stack (0.5 HL0.5H);
the short wave-passing film system is formed by alternately superposing germanium and zinc sulfide film layers, and the structure of the short wave-passing film system is as follows: (0.5LH0.5L) ^13 with center wavelength of 4650 nm; wherein H represents that the thickness of the germanium film layer is 1 basic thickness, L represents that the thickness of the zinc sulfide film layer is 1 basic thickness, 0.5L represents that the thickness of the zinc sulfide film layer is 0.5 basic thickness, and 13 represents the cycle number of the basic film stack (0.5 LH0.5L);
the basic thickness is one fourth of the optical thickness center wavelength of the long wave passing film system or the short wave passing film system.
2. The 3.50-3.90 μm medium wave infrared microfilter of claim 1, wherein: the long wave pass membrane system is finally obtained by optimization design calculation on the basis of the structure of the long wave pass membrane system, the long wave pass membrane system is shown in table 1, the membrane layer with the number of layers of 1 is the outermost layer, the membrane layer with the number of layers of 45 is deposited on the silicon substrate and is the innermost layer,
TABLE 1 Long wavelength pass film series
Figure FDA0002977812500000011
Figure FDA0002977812500000021
3. The method for preparing a 3.50-3.90 μm medium wave infrared micro filter according to claim 1, wherein the method comprises the following steps: the short wave through film system is finally obtained through optimization design calculation on the basis of the structure of the short wave through film system, the short wave through film system is shown in Table 2, the film layer with the number of layers of 1 is the outermost layer, the film layer with the number of layers of 27 is deposited on the silicon substrate and is the innermost layer,
TABLE 2 short wave pass membrane system
Number of layers Film material Film thickness/nm 1 Zinc sulfide 659.9517 2 Germanium (Ge) 303.1252 3 Zinc sulfide 527.663 4 Germanium (Ge) 303.4779 5 Zinc sulfide 506.0659 6 Germanium (Ge) 286.562 7 Zinc sulfide 512.5365 8 Germanium (Ge) 287.3251 9 Zinc sulfide 508.7516 10 Germanium (Ge) 281.9393 11 Zinc sulfide 517.6755 12 Germanium (Ge) 279.3932 13 Zinc sulfide 503.467 14 Germanium (Ge) 290.1305 15 Zinc sulfide 512.0884 16 Germanium (Ge) 273.1541 17 Zinc sulfide 515.9556 18 Germanium (Ge) 286.7169 19 Zinc sulfide 513.9143 20 Germanium (Ge) 282.5536 21 Zinc sulfide 504.1142 22 Germanium (Ge) 288.6436 23 Zinc sulfide 530.8378 24 Germanium (Ge) 291.8134 25 Zinc sulfide 511.3925 26 Germanium (Ge) 275.2112 27 Zinc sulfide 285.4052
4. A method for preparing a 3.50-3.90 μm medium wave infrared micro filter according to any one of claims 1-3, wherein: the method comprises the following steps:
(1) loading the clean silicon substrate into a clean vacuum chamber, and vacuumizing to less than or equal to 3 × 10-5Torr;
(2) Heating the silicon substrate to 200 ℃ and keeping the temperature for 30 min;
(3) opening a Hall source type ion source, and bombarding and cleaning the silicon substrate for 10min by using an ion beam, wherein the working gas of the ion source is argon, and the gas flow is 17 sccm;
(4) opening a Hall source type ion source, and respectively and alternately depositing the germanium film layer and the zinc sulfide film layer in the long-wave-pass film system layer by layer on one side of the silicon substrate by adopting an ion beam assisted electron gun evaporation method, and alternately depositing the germanium film layer and the zinc sulfide film layer in the short-wave-pass film system layer by layer on the other side of the silicon substrate until the deposition of the film system is completed; the deposition rate of the germanium film layer is 1.0nm/s, the deposition rate of the zinc sulfide film layer is 0.8nm/s, the ion source working gas is argon, the gas flow is 17sccm, and the film thickness is monitored by a quartz crystal film thickness controller;
(5) and naturally cooling the silicon substrate to room temperature to obtain the 3.50-3.90 mu m medium wave infrared micro filter.
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