CN106435493A - Preparation method for high-performance ZnS-substrate composite hard protection thin film - Google Patents
Preparation method for high-performance ZnS-substrate composite hard protection thin film Download PDFInfo
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- CN106435493A CN106435493A CN201610959079.XA CN201610959079A CN106435493A CN 106435493 A CN106435493 A CN 106435493A CN 201610959079 A CN201610959079 A CN 201610959079A CN 106435493 A CN106435493 A CN 106435493A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/3442—Applying energy to the substrate during sputtering using an ion beam
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
Abstract
The invention provides a preparation method for a high-performance ZnS-substrate composite hard protection thin film, and belongs to a high-performance infrared hard protection thin film preparation technology. The preparation method is mainly characterized in that the composite hard protection thin film composed of a high-refraction-rate germanium carbide (Ge1xCx) thin film and a low-refraction-rate and high-hardness diamond-like carbon (DLC) thin film is continuously prepared through an ion beam reactive sputtering method. The composite thin film is simple in film system and high in process controllability and stability. By depositing the composite hard protection thin film on a ZnS substrate, the optical property and mechanical property of the ZnS substrate can be greatly improved.
Description
Technical field
The invention belongs to function optical thin film design and the field of development, it is related to a kind of high-performance ZnS substrate composite ganoine and protects
The preparation method of shield thin film.
Background technology
The development of modern photoelectric imaging technology it is desirable to the window element of IRDS not only to have higher infrared
Transmitance and to have good mechanical performance and adaptive capacity to environment.ZnS is as most widely used LONG WAVE INFRARED at present
Window material has the defect that transmitance is relatively low, mechanical strength is relatively low.
Deposit Ge on ZnS surface1-xCx/ DLC composite ganoine protecting film, not only by between film material and substrate
Good refractive index match is improving the transmitance of ZnS substrate;And outermost layer can be used as by selecting the thin film of high rigidity
Material, provides the protective capability under good complex environment for ZnS substrate.
At present, various countries' research worker is passed through to prepare in ZnS substrate using chemical vapour deposition technique and radio-frequency magnetron sputter method
Ge1-xCx/ DLC composite ganoine protecting film.Use merely the Ge of chemical vapour deposition technique preparation1-xCx/ DLC composite ganoine is protected
Film amount containing H is higher, and infrared transmittivity is relatively low.Use merely the Ge of magnetron sputtering method preparation1-xCx/ DLC composite ganoine protecting film
Hardness is relatively low.And prepare Ge using two methods respectively1-xCx/ DLC composite ganoine protecting film can cause larger absorption, simultaneously
The outward appearance of film layer, stability are produced by certain impact, and increased process complexity.Therefore, invention one kind simply can connect
Continuous being coated with has good optical characteristics and mechanical characteristic Ge1-xCxThe process of/DLC composite ganoine protective film is very
Necessary.
Content of the invention
(1) goal of the invention
The purpose of the present invention is:A kind of preparation method of high-performance ZnS substrate composite ganoine protective film is provided, select from
The continuous preparation of beamlet reactive sputtering is combined preferable Ge by weak absorbing, high intensity with base1-xCxThin film and high rigidity, low folding
Penetrate the composite ganoine protective film of the DLC film composition of rate, overcome transmitance present in the application of ZnS substrate relatively low strong with machinery
Spend poor defect.
(2) technical scheme
In order to solve above-mentioned technical problem, the present invention provides a kind of system of high-performance ZnS substrate composite ganoine protective film
Preparation Method, it comprises the following steps:
S1:Ion beam reactive sputtering method prepares Ge1-xCxTransition zone
From ZnS substrate as substrate, Ge is prepared in ZnS substrate by ion beam reactive sputtering method1-xCxThin film;
S2:Ion beam reactive sputtering method prepares DLC film
In Ge1-xCxAbove thin film, DLC film is prepared by ion beam reactive sputtering method.
Wherein, in described step S1, ion beam reactive sputtering method prepares Ge1-xCxTransition zone comprises the following steps:
S11:Cleaning substrate
S12:Pre-sputtering
ZnS substrate after cleaning is put in ion beam reactive sputtering coater, as substrate, using Ge as target, Ar
As ion source working gas, CH4As reacting gas, start pre-sputtering;
S13:Pre- bombardment
Substrate is carried out with pre- bombardment, removes adsorption gas molecule and the other impurities of substrate surface;
S14:Sputter coating
It is filled with Ar into main ion source, be passed through reacting gas CH to vacuum chamber4, reactive sputter-deposition Ge1-xCxTransition zone.
Wherein, in described step S2, ion beam reactive sputtering method preparation DLC film comprises the following steps:
S21:Pre-sputtering
Substrate is turned to non-plated film area, rotates target, graphite target is turned to sputtering position.Start pre-sputtering target;
S22:Sputter coating
It is passed through reacting gas CH to vacuum chamber4, substrate is turned to plated film area, deposits DLC film.
Wherein, in described step S11, the process of cleaning substrate is:It is 1 with being moistened with volume ratio:1 dehydrated alcohol and ether
The absorbent carbasuss of mixed liquor tentatively wipe net substrate, subsequently dip in cerium oxide polishing slurry with absorbent carbasuss and substrate be polished,
Then the absorbent carbasuss of mixed liquor and defat cotton with being moistened with dehydrated alcohol and ether wipe substrate surface successively.
Wherein, in described step S12, during pre-sputtering, in main ion source and neutralizer, Ar total flow is in 30sccm-55sccm
Between;Main ion source beam pressure is controlled to 500V-1000V;Line controls within 300mA;Time is 2min-5min.
Wherein, in described step S13, when bombarding in advance, the Ar being filled with into assisting ion source and neutralizer, flow-control exists
Between 24sccm-55sccm;Assisting ion source beam pressure is controlled to 150V-600V;Line controls within 300mA;Substrate is turned
Move plated film position, the time is 2min-15min.
Wherein, in described step S14, during sputter coating, being filled with Ar flow in main ion source is 30sccm-55sccm, very
Empty room is passed through reacting gas CH4Between 25sccm-40sccm, regulation ion source beam pressure is 800V-1200V to flow, and line is
300mA-400mA, plated film time control is in 40min-80min.
Wherein, in described step S21, during pre-sputtering, in main ion source and neutralizer, Ar total flow is in 25sccm-55sccm
Between;Main ion source beam pressure is controlled to 500V-1000V;Line controls within 300mA;Time is 2min-5min.
Wherein, in described step S22, during sputter coating, adjusting main ion source beam pressure is 600V-1200V, and line is
300mA-400mA, is passed through reacting gas CH to vacuum chamber4Flow is between 16sccm-64sccm.
Wherein, in described step S22, the sputter coating time is 8 hours -18 hours.
(3) beneficial effect
The preparation method of the high-performance ZnS substrate composite ganoine protective film that technique scheme is provided, by adopting
Simply, reliable ion beam reactive sputtering method prepares high-performance Ge1-xCx/ DLC composite ganoine protective film, overcomes traditional plated film
Method prepares the deficiency of composite ganoine protective film performance, improves the performance of whole ZnS basement membrane layer on the whole.
Brief description
Fig. 1 is ZnS basement membrane layer structural representation;
Fig. 2 is ion beam reactive sputtering coater structural representation;
Fig. 3 be embodiment of the present invention plated film before and after ZnS substrate transmitance contrast curve chart.
Specific embodiment
For making the purpose of the present invention, content and advantage clearer, with reference to the accompanying drawings and examples, the tool to the present invention
Body embodiment is described in further detail.
For the Ge overcoming traditional method to prepare in ZnS substrate1-xCxThe shortcoming and defect of/DLC composite ganoine protecting film,
As depicted in figs. 1 and 2, the invention provides the preparation method of high-performance ZnS substrate composite ganoine protective film, walk including following
Suddenly:
1) ion beam reactive sputtering method preparation Ge1-xCxTransition zone
Cleaning substrate
ZnS substrate selected by substrate, and with the mixed liquor that is moistened with dehydrated alcohol and ether, (volume ratio is 1:1) at the beginning of absorbent carbasuss
Step wipes net substrate, subsequently dips in cerium oxide polishing slurry with absorbent carbasuss and substrate is polished, then successively with being moistened with anhydrous second
The absorbent carbasuss of the mixed liquor of alcohol and ether and defat cotton wipe substrate surface, till wiped clean.
Pre-sputtering
ZnS substrate after cleaning is put in ion beam reactive sputtering coater, as substrate, opens vacuum pumping true
Empty.Using Ge as target, Ar is as ion source working gas, CH4As reacting gas.It is down to by force 10- when vacuum chamber is intrinsic pressure3Pa
When following, start pre-sputtering.Condition is:In main ion source and neutralizer, Ar total flow is between 30sccm-55sccm;Main ion
Source beam pressure is controlled to 500V-1000V;Line controls within 300mA;Time is 2min-5min.Be then turned off main ion source with
And neutralizer.
This step can effectively remove the pollutant of target material surface attachment, reduces impurity content in thin film.
Pre- bombardment
The Ar being filled with into assisting ion source and neutralizer, flow-control is between 24sccm-55sccm;Assisting ion source
Beam pressure is controlled to 150V-600V;Line controls within 300mA;By substrate rotation to plated film position, the time is 2min-
15min.
This step, by substrate is carried out with pre- bombardment, is removed adsorption gas molecule and the other impurities of substrate surface, is made base
Basal surface reaches higher cleanliness levels, drastically increases the adhesive force between film layer and substrate.
Sputter coating
Close assisting ion source and its effusion meter, start reactive sputter-deposition Ge1-xCxTransition zone.Fill into main ion source
Entering Ar flow is 30sccm-55sccm, is passed through reacting gas CH to vacuum chamber4, flow between 25sccm-40sccm, adjust
Ion source beam pressure is 800V-1200V, and line is 300mA-400mA.Plated film time control is in 40min-80min.
The thin film of this step deposition can form good adhesive force and substrate between, also can be formed with outer layer DLC film
Good refractive index match, has the advantages that to absorb little, hardness higher simultaneously, can largely improve composite ganoine protection thin
The overall performance of film.
2) ion beam reactive sputtering method preparation DLC film
Pre-sputtering
Substrate is turned to non-plated film area.Rotate target, graphite target is turned to sputtering position.Start pre-sputtering target.
Condition is:In main ion source and neutralizer, Ar total flow is between 25sccm-55sccm;Main ion source beam pressure is controlled to 500V-
1000V;Line controls within 300mA;Time is 2min-5min.
Sputter coating
Adjusting main ion source beam pressure is 600V-1200V, and line is 300mA-400mA, is passed through reacting gas to vacuum chamber
CH4, between 16sccm-64sccm, pressure in vacuum tank is in 8 × 10- for flow2Below Pa.After ion source stable working state,
Substrate is turned to plated film area, deposits DLC film, the plated film time is 8 hours -18 hours.
This step is in Ge1-xCxTransition zone preparation complete on the basis of continuous coating, process is simple, reliability, keep away well simultaneously
Exempt from the impact that gradation plated film causes to film performance.
With specific example, the inventive method is described in further detail below.
Embodiment 1
1) ion beam reactive sputtering method preparation Ge1-xCxTransition zone
With the mixed liquor that is moistened with dehydrated alcohol and ether, (volume ratio is 1:1) absorbent carbasuss tentatively wipe net substrate, with
Dip in cerium oxide polishing slurry with absorbent carbasuss afterwards substrate is polished, then successively with being moistened with the mixed liquor of dehydrated alcohol and ether
Absorbent carbasuss and defat cotton wipe substrate surface, till wiped clean.ZnS substrate after cleaning is put into ion beam
In reactive sputtering coater, open vacuum pump evacuation.Using Ge as target, Ar is as ion source working gas, CH4As anti-
Answer gas.It is down to by force 10 when vacuum chamber is intrinsic pressure-3During below Pa, start pre-sputtering.Condition is:In main ion source and neutralizer, Ar is total
Flow is in 32sccm;Main ion source beam pressure is 1000V;Line is 300mA;Sputtering time is 5min.Subsequently substrate rotation is arrived
Plated film position, carries out pre- bombardment to substrate.Condition is:It is filled with Ar into assisting ion source and neutralizer, flow-control is
30sccm;Assisting ion source beam pressure is 200V;Line is 100mA;Time is 10min.Pre- bombard after, close assisting ion source and
Its effusion meter, starts reactive sputter-deposition Ge1-xCxTransition zone.Being filled with Ar flow into main ion source and neutralizer is 32sccm,
It is passed through reacting gas CH to vacuum chamber4, flow is 32sccm, and regulation ion source beam pressure is 1000V, and line is 300mA.During plated film
Between be 60min.
2) ion beam reactive sputtering method preparation DLC film
Substrate is turned to non-plated film area.Rotate target, graphite target is turned to sputtering position.Start pre-sputtering.Condition
For:In main ion source and neutralizer, Ar total flow is 32sccm;Main ion source beam pressure is 1000V;Line is 300mA;Time is
5min.Adjusting main ion source beam pressure is 600V, and line is 400mA, is passed through reacting gas CH to vacuum chamber4, flow is 32sccm.
After ion source stable working state, substrate is turned to plated film area, deposit DLC film, the plated film time is 12.5 hours.
From figure 3, it can be seen that the mean transmissivity of ZnS substrate brings up to 89.8% from 73% after plated film.Additionally, film hardness
Reach 15GPa.Optical characteristics and the mechanical property of ZnS substrate are greatly improved by being coated with hard coating layer.
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art
For member, on the premise of without departing from the technology of the present invention principle, some improvement can also be made and deform, these improve and deform
Also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high-performance ZnS substrate composite ganoine protective film is it is characterised in that comprise the following steps:
S1:Ion beam reactive sputtering method prepares Ge1-xCxTransition zone
From ZnS substrate as substrate, Ge is prepared in ZnS substrate by ion beam reactive sputtering method1-xCxThin film;
S2:Ion beam reactive sputtering method prepares DLC film
In Ge1-xCxAbove thin film, DLC film is prepared by ion beam reactive sputtering method.
2. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 1 is it is characterised in that institute
State in step S1, ion beam reactive sputtering method prepares Ge1-xCxTransition zone comprises the following steps:
S11:Cleaning substrate
S12:Pre-sputtering
ZnS substrate after cleaning is put in ion beam reactive sputtering coater, as substrate, using Ge as target, Ar conduct
Ion source working gas, CH4As reacting gas, start pre-sputtering;
S13:Pre- bombardment
Substrate is carried out with pre- bombardment, removes adsorption gas molecule and the other impurities of substrate surface;
S14:Sputter coating
It is filled with Ar into main ion source, be passed through reacting gas CH to vacuum chamber4, reactive sputter-deposition Ge1-xCxTransition zone.
3. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 2 is it is characterised in that institute
State in step S2, ion beam reactive sputtering method preparation DLC film comprises the following steps:
S21:Pre-sputtering
Substrate is turned to non-plated film area, rotates target, graphite target is turned to sputtering position.Start pre-sputtering target;
S22:Sputter coating
It is passed through reacting gas CH to vacuum chamber4, substrate is turned to plated film area, deposits DLC film.
4. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 3 is it is characterised in that institute
State in step S11, the process of cleaning substrate is:It is 1 with being moistened with volume ratio:1 dehydrated alcohol and the defat of the mixed liquor of ether
Gauze tentatively wipes net substrate, subsequently dips in cerium oxide polishing slurry with absorbent carbasuss and substrate is polished, then successively with being moistened with
The absorbent carbasuss of the mixed liquor of dehydrated alcohol and ether and defat cotton wipe substrate surface.
5. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 3 is it is characterised in that institute
State in step S12, during pre-sputtering, in main ion source and neutralizer, Ar total flow is between 30sccm-55sccm;Main ion source is restrainted
Voltage-controlled it is made as 500V-1000V;Line controls within 300mA;Time is 2min-5min.
6. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 3 is it is characterised in that institute
State in step S13, in advance bombard when, the Ar being filled with into assisting ion source and neutralizer, flow-control 24sccm-55sccm it
Between;Assisting ion source beam pressure is controlled to 150V-600V;Line controls within 300mA;By substrate rotation to plated film position, when
Between be 2min-15min.
7. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 3 is it is characterised in that institute
State in step S14, during sputter coating, being filled with Ar flow in main ion source is 30sccm-55sccm, and vacuum chamber is passed through reacting gas
CH4Between 25sccm-40sccm, regulation ion source beam pressure is 800V-1200V to flow, and line is 300mA-400mA, plated film
Time control is in 40min-80min.
8. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 3 is it is characterised in that institute
State in step S21, during pre-sputtering, in main ion source and neutralizer, Ar total flow is between 25sccm-55sccm;Main ion source is restrainted
Voltage-controlled it is made as 500V-1000V;Line controls within 300mA;Time is 2min-5min.
9. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 3 is it is characterised in that institute
State in step S22, during sputter coating, adjusting main ion source beam pressure is 600V-1200V, and line is 300mA-400mA, to vacuum
Room is passed through reacting gas CH4Flow is between 16sccm-64sccm.
10. the preparation method of high-performance ZnS substrate composite ganoine protective film as claimed in claim 9 is it is characterised in that institute
State in step S22, the sputter coating time is 8 hours -18 hours.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107367776A (en) * | 2017-09-06 | 2017-11-21 | 天津津航技术物理研究所 | A kind of controllable infrared optical window film design method of heat radiation |
CN111304588A (en) * | 2020-03-26 | 2020-06-19 | 中国建筑材料科学研究总院有限公司 | Infrared germanium carbide film, infrared material with germanium carbide film, and preparation method and application of infrared material |
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CN101414017A (en) * | 2008-12-01 | 2009-04-22 | 中国船舶重工集团公司第七一七研究所 | Infrared dual-band window protection film and manufacturing method thereof |
CN101464529A (en) * | 2008-01-23 | 2009-06-24 | 四川大学 | GexC1-x/DLC anti-reflection protective film and method for producing the same |
CN105543792A (en) * | 2015-12-11 | 2016-05-04 | 中国电子科技集团公司第四十八研究所 | Magnetron sputtering device and magnetron sputtering method |
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US5365345A (en) * | 1991-04-10 | 1994-11-15 | Santa Barbara Research Center | Infrared transmitting window and method of making same |
CN101464529A (en) * | 2008-01-23 | 2009-06-24 | 四川大学 | GexC1-x/DLC anti-reflection protective film and method for producing the same |
CN101414017A (en) * | 2008-12-01 | 2009-04-22 | 中国船舶重工集团公司第七一七研究所 | Infrared dual-band window protection film and manufacturing method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN107367776A (en) * | 2017-09-06 | 2017-11-21 | 天津津航技术物理研究所 | A kind of controllable infrared optical window film design method of heat radiation |
CN111304588A (en) * | 2020-03-26 | 2020-06-19 | 中国建筑材料科学研究总院有限公司 | Infrared germanium carbide film, infrared material with germanium carbide film, and preparation method and application of infrared material |
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