CN109932064A - A kind of infrared focal plane array seeker and preparation method thereof with DLC protective film - Google Patents
A kind of infrared focal plane array seeker and preparation method thereof with DLC protective film Download PDFInfo
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- CN109932064A CN109932064A CN201910232823.XA CN201910232823A CN109932064A CN 109932064 A CN109932064 A CN 109932064A CN 201910232823 A CN201910232823 A CN 201910232823A CN 109932064 A CN109932064 A CN 109932064A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000007789 gas Substances 0.000 claims abstract description 44
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 29
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- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 9
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The present invention provides a kind of preparation methods of infrared focal plane array seeker with DLC protective film, comprising the following steps: A) successively use acetone and working solution to clean the window of infrared focal plane array seeker；B) under vacuum conditions by the window of the infrared focal plane array seeker after cleaning, it is passed through argon gas, carries out radio frequency plasma cleaning；C it) is passed through carbon-source gas again, DLC protective film is deposited on the surface of the window of infrared focal plane array seeker using radio-frequency plasma enhanced chemical vapor deposition method, obtains the infrared focal plane array seeker with DLC protective film；The step C) radio-frequency power be 100~2500W, the step C) vacuum degree be 3 × 10‑3~3 × 10‑5Pa.The present invention also provides a kind of infrared focal plane array seekers with DLC protective film.
Description
Technical field
The invention belongs to Infrared Focal plane Array Technologies field more particularly to a kind of infrared coke with DLC protective film are flat
Area array detector and preparation method thereof.
Background technique
Since striding into 21st century, the development of infrared hot photography technology has gone through a year more than 30, development
Current total solids miniaturization all-electronin scanning has been developed to from mechanical scanning mechanism originally and has stared camera shooting, is especially non-system
The development of refrigeration technique makes infrared hot photography technology from long-term main military purposes expands to such as industrial detection temperature control, law enforcement is seized
Poison, health care, remote sensing, the earlier property troubles diagnosis and fixing of equipment, rescue at sea, astrosurveillance, vehicle, flies at safety precaution
The driver on play chess and naval vessel is also the wide civil fields such as enhancing scope.
The development speed of infrared hot photography technology depends primarily on the progress of infrared detector technology acquirement, currently, infrared
Focal plane array detector is to select high-index material (such as germanium) to make on the chip using vanadium oxide film as thermo-sensitive material
For substrate, the transmissivity of anti-reflection film (such as ZnSe and ZnS) Lai Zengjia infra-red radiation is plated on germanium surface.But common infrared anti-reflection
For film (such as ZnSe, ZnS) although there is excellent anti-reflection performance, mechanical strength itself is lower, easily in detector vacuum window
(infrared focal plane array seeker is multi-purpose for the production (especially component, machine core assembly and debugging stage) of window and use process
In extreme environment) in formed scratch, abrasion or corrosion, gently then cause window anti-reflection film impaired and make under infrared radiation transmission
Drop further results in detector performance decline or picture quality degradation, heavy then detector assembly is caused to fail, increase production cost
With reduction product service life.
Summary of the invention
The purpose of the present invention is to provide a kind of infrared focal plane array seeker with DLC protective film and its preparation sides
Method, the infrared focal plane array seeker in the present invention have preferable wear-resistant, corrosion resistance, while incident IR radiation
It loses small.
The present invention provides a kind of preparation method of infrared focal plane array seeker with DLC protective film, including following
Step:
A) acetone and working solution is successively used to clean the window of infrared focal plane array seeker；
B) under vacuum conditions by the window of the infrared focal plane array seeker after cleaning, it is passed through argon gas, carries out radio frequency
Plasma cleaning；
C it) is passed through carbon-source gas again, is visited using radio-frequency plasma enhanced chemical vapor deposition method in infrared focal plane array
The surface for surveying the window of device deposits DLC protective film, obtains the infrared focal plane array seeker with DLC protective film；
The step C) radio-frequency power be 100~2500W, the step C) vacuum degree be 3 × 10-3~3 × 10- 5Pa。
Preferably, the window of the infrared focal plane array seeker include the ZnSe layer successively contacted, ZnS layers, Ge layers,
ZnS layers and ZnSe layer；
The ZnSe layer is in contact with the DLC protective film.
Preferably, the step B) in vacuum degree be 0.0013~0.13Pa；
The step B) in argon gas flow be 30~90sccm；
The step B) in radio-frequency power be 300~700W.
Preferably, the carbon-source gas is methane；
The flow of the carbon-source gas is 5~100sccm.
Preferably, the step C) in deposit temperature be 20~200 DEG C；
The step C) in sedimentation time be 0.1~10min.
Preferably, the step C) deposition process in use argon gas as carrier gas；
The flow of the argon gas is 100~200sccm.
Preferably, the working solution is one or more of acetone, isopropanol and N-Methyl pyrrolidone.
The present invention provides a kind of infrared focal plane array seeker with DLC protective film, including infrared focal plane array
Detector and the DLC protective film for being deposited on the detector window discharge surface；
The infrared focal plane array seeker with DLC protective film is according to described in claim 1~7 any one
Preparation method is prepared.
Preferably, the service band of the infrared focal plane array seeker with DLC protective film be 3~5 μm or 8~
14μm。
Preferably, the refractive index of the DLC protective film is 1.8~3.1.
The present invention provides a kind of preparation methods of infrared focal plane array seeker with DLC protective film, including with
Lower step: A) successively use acetone and working solution to clean the window of infrared focal plane array seeker；B after) cleaning
Infrared focal plane array seeker window under vacuum conditions, be passed through argon gas, carry out radio frequency plasma cleaning；C it) is passed through again
Carbon-source gas, using radio-frequency plasma enhanced chemical vapor deposition method on the surface of the window of infrared focal plane array seeker
DLC protective film is deposited, the infrared focal plane array seeker with DLC protective film is obtained；The step C) radio-frequency power be
100~2500W, the step C) vacuum degree be 3 × 10-3~3 × 10-5Pa.The present invention is using radio frequency plasma enhancing chemistry
(PECVD) method of vapor deposition deposits DLC film in the window surface of detector, while controlling sedimentary condition, so that DLC film
More uniform, good film-forming property is deposited, it is also with higher resistance to while capable of guaranteeing high transmissivity and low ir-absorbance
Scuffing, rub resistance and corrosion resistance.In addition, DLC film deposition velocity in the present invention is fast, single furnace output is high, to matrix
It damages small.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the window structure schematic diagram of the infrared focal plane array seeker in the present invention with DLC protective film.
Specific embodiment
The present invention provides a kind of preparation methods of infrared focal plane array seeker with DLC protective film, including with
Lower step:
A) acetone and working solution is successively used to clean the window of infrared focal plane array seeker；
B) under vacuum conditions by the window of the infrared focal plane array seeker after cleaning, it is passed through argon gas, carries out radio frequency
Plasma cleaning；
C it) is passed through carbon-source gas again, is visited using radio-frequency plasma enhanced chemical vapor deposition method in infrared focal plane array
The surface for surveying the window of device deposits DLC protective film, obtains the infrared focal plane array seeker with DLC protective film；
The step C) radio-frequency power be 100~2500W, the step C) vacuum degree be 3 × 10-3~3 × 10- 5Pa。
The infrared focal plane array seeker absorbs infrared waves to be imaged, detector in terminal usage scenario,
Individual infrared optical lens can be added, are to be not directly contacted with the environment such as ambient atmosphere, machine core is assembled by detector, then by
Machine core addition infrared lens etc. are assembled into complete machine, and in the process of this length, no infrared optical lens or other component are protected
The window of detector is protected, therefore, we select to protect detector in window surface DLC films deposited, and window DLC film can protect
Our detector is from being made to machine core, then into complete machine whole process and subsequent product is in use, will not be scratched,
Abrasion, while will not also reduce ir transmissivity.
Detector window in the present invention for substrate, has plated anti-reflection film, specific structure such as Fig. 1 institute on germanium surface with germanium (Ge)
Show, including ZnSe layer, ZnS layers, Ge layers, ZnS layers and the ZnSe layer successively contacted；The ZnSe layer and the DLC protective film phase
Contact.
ZnSe increasing is coated with using Ge as substrate above-mentioned present invention preferably employs radio frequency plasma enhancing chemical vapour deposition technique
The infrared detector window surface of permeable membrane deposits DLC protective film.The present invention preferably first cleans vacuum chamber, removes dust, prevents from taking out
Ash pollutes substrate from when vacuum.
Then, the present invention cleans window substrates, and film-substrate cohesion reduces caused by avoiding because of foreign matter, to be film
It penetrates light rate and refractive index is affected.The present invention preferably first cleans 5~30min to window substrates under ultrasound using acetone, goes
It except surface and oil contaminant, then reuses working solution and cleans 5~20min under ultrasound, then with deionized water 5~20min of repeated flushing,
Surface impurity is removed, is dried in last dryer.
Infrared focal plane array seeker window after cleaning is put into vacuum chamber, is vacuumized, radio frequency etc. is ready for
Plasma enhanced chemical vapor deposits DLC film.
The present invention preferably first sets a vacuum degree, after vacuum degree reaches setting value, is passed through argon gas, adjusts radio-frequency power,
Argon ion cleaning is carried out to window surface.
In the present invention, the vacuum degree of the step is preferably 0.13~0.0013Pa, more preferably 0.1~0.005Pa, most
Preferably 0.01~0.005Pa；The flow of the argon gas is preferably 30~90sccm, more preferably 40~80sccm, most preferably
For 50~70sccm；The radio-frequency power is preferably 300~700W, more preferably 300~600W, most preferably 300W.
After completing above-mentioned sub- Ion Cleaning, the present invention is passed through carbon-source gas, enhances chemical gaseous phase using radio frequency plasma
Deposition method deposits DLC protective film on the surface of the window of infrared focal plane array seeker, obtains having the red of DLC protective film
Outer focal plane array detector.
Diamond thin, also known as DLC film are the abbreviations of english vocabulary Diamond Like Carbon, it is a kind of
Physicochemical properties be similar to diamond and it is unique can metastable state noncrystalline membrane, high rigidity that DLC film has,
Rub resistance, it is anticorrosive and in characteristics such as the excellent optical transmittances of infrared band, become outstanding infrared antireflective film
Material.The present invention protects window surface using DLC film, and the present invention utilizes PECVD method, in ZnSe anti-reflection film
Surface Direct precipitation DLC film, while improving technique, enable DLC film not by any bonding medium or other
Under the premise of middle layer, good binding force is kept between base, meanwhile, band due to film layer is excessive is also reduced as far as possible
The ir transmissivity loss come.
The present invention passes through gas discharge under low pressure and carbon-source gas is resolved into various neutral particle (CH3CH C H) and
Charged particle (CH5+\CH3+\CH+\H+), charged particle is nucleated by series of chemical in substrate surface, and migration is grown into
DLC film, plasma promote the chemical reaction between gas, reduce temperature (20~200 DEG C) required for deposition, low pressure
Under plasma reactant can also be promoted in the diffusion of substrate surface, improve deposition rate, etch away matrix and film layer table
Face combines illusive particle, so that film-substrate cohesion be made to enhance.Plate condenser type manifold type radio frequency glow discharge prepares film
Deposition rate is high, and film layer dense uniform, stability are good.
In the present invention, the carbon-source gas is preferably methane (CH4), the flow of the carbon-source gas is preferably 5~
100sccm, more preferably 20~70sccm, most preferably 50~70sccm；The radio-frequency power is preferably 100~2500W, more
Preferably 200~500W, specifically, in an embodiment of the present invention, can be 200W or 300W；The deposition of the DLC film
Vacuum degree is preferably 3 × 10-3~3 × 10-5Pa, more preferably 2 × 10-3~1 × 10-4Pa, most preferably 1 × 10-3~5 × 10-4Pa；The depositing temperature is preferably 20~200 DEG C, more preferably 30~150 DEG C, most preferably 50~100 DEG C, specifically,
In the embodiment of the present invention, it can be 180 DEG C；The sedimentation time is preferably 0.1~10min, more preferably 1~8min, most
Preferably 3~6min.
During depositing DLC film, present invention preferably uses argon gas as carrier gas, and the flow of the argon gas is preferably
100~200sccm.
The present invention also provides a kind of according to the infrared focal plane array made from above-mentioned preparation method with DLC protective film
Detector, including infrared focal plane array seeker and the DLC protective film for being deposited on the detector window discharge surface；
The window of the infrared focal plane array seeker is coated with anti-reflection film, specific structure such as Fig. 1 institute using Ge as substrate
Show, details are not described herein.
In the present invention, the thickness of the DLC protective film is preferably 150~1200nm；The refractive index of the DLC protective film
Preferably 1.8~3.1；The service band of the infrared focal plane array seeker with DLC protective film is 3~5 μm or 8~
14μm。
The present invention provides a kind of preparation methods of infrared focal plane array seeker with DLC protective film, including with
Lower step: A) successively use acetone and working solution to clean the window of infrared focal plane array seeker；B after) cleaning
Infrared focal plane array seeker window under vacuum conditions, be passed through argon gas, carry out radio frequency plasma cleaning；C it) is passed through again
Carbon-source gas, using radio-frequency plasma enhanced chemical vapor deposition method on the surface of the window of infrared focal plane array seeker
DLC protective film is deposited, the infrared focal plane array seeker with DLC protective film is obtained；The step C) radio-frequency power be
200~2500W, the step C) vacuum degree be 3 × 10-3~3 × 10-5Pa.The present invention is using radio frequency plasma enhancing chemistry
(PECVD) method of vapor deposition deposits DLC film in the window surface of detector, while controlling sedimentary condition, so that DLC film
More uniform, good film-forming property is deposited, it is also with higher resistance to while capable of guaranteeing high transmissivity and low ir-absorbance
Scuffing, rub resistance and corrosion resistance.In addition, DLC film deposition velocity in the present invention is fast, single furnace output is high, to matrix
It damages small.
The experimental results showed that the present invention in the detector with DLC protective film salt spray test (4.5%NaCl, 37
DEG C, 96h), thermocycling (- 60~70 DEG C) passes through；Between ir transmissivity 90%~97%.
In order to further illustrate the present invention, with reference to embodiments to provided by the invention a kind of with DLC protective film
Infrared focal plane array seeker and preparation method thereof is described in detail, but cannot be understood as to the scope of the present invention
Restriction.
Embodiment 1
Cleaning substrate: 5min is cleaned under ultrasound using acetone, removes surface and oil contaminant, then with acetone working solution under ultrasound
Clean 5min, then use deionized water repeated flushing 10min, removing surface impurity.It is dried in dryer, and immediately will be washed
Window is placed on vacuum chamber pole plate, is vacuumized.
Deposition DLC film: being passed through argon gas when vacuum degree reaches setting value 0.0013Pa, and argon flow 30Sccm is adjusted
Radio-frequency power to 300W carry out argon ion cleaning,
It is passed through carbon-source gas CH again4, set radio-frequency power as 300W, 200 DEG C of cavity temperature, substrate bias 250v, vacuum
Degree 3 × 10-3Pa, carbon-source gas flow 60sccm start to deposit DLC film.
Radio-frequency power supply is closed after the completion of deposition, stops being passed through for carbon-source gas, increases argon flow, discharges vacuum, is taken out
Product.
Embodiment 2
Cleaning substrate: 10min is cleaned under ultrasound using acetone, removes surface and oil contaminant, then with acetone working solution in ultrasound
Lower cleaning 20min, then with deionized water repeated flushing 10min, remove surface impurity.It dries in dryer, and will wash immediately
Good window is placed on vacuum chamber pole plate, is vacuumized.
Deposition DLC film: argon gas, argon flow 90Sccm are passed through when vacuum degree reaches setting value 0.13Pa, adjusting is penetrated
Frequency power to 300W carry out argon ion cleaning,
It is passed through carbon-source gas CH again4, set radio-frequency power as 300W, 175 DEG C of cavity temperature, substrate bias, vacuum degree 5 ×
10-4Pa, carbon-source gas flow 40sccm start to deposit DLC film.
Radio-frequency power supply is closed after the completion of deposition, stops being passed through for carbon-source gas, adjusts argon flow, discharges vacuum, is taken out
Product.
Embodiment 3
Cleaning substrate: 10min is cleaned under ultrasound using acetone, removes surface and oil contaminant, then with acetone working solution in ultrasound
Lower cleaning 10min, then with deionized water repeated flushing 10min, remove surface impurity.It dries in dryer, and will wash immediately
Good window is placed on vacuum chamber pole plate, is vacuumized.
Deposition DLC film: argon gas, argon flow 30Sccm are passed through when vacuum degree reaches setting value 0.01Pa, adjusting is penetrated
Frequency power to 300W carry out argon ion cleaning,
It is passed through carbon-source gas CH again4, set radio-frequency power as 200W, 175 DEG C of cavity temperature, substrate bias, vacuum degree 3 ×
10-5Pa, carbon-source gas flow 30sccm start to deposit DLC film.
Radio-frequency power supply is closed after the completion of deposition, stops being passed through for carbon-source gas, adjusts argon flow, discharges vacuum, is taken out
Product.
Comparative example 1
The infrared focal plane array seeker with DLC protective film is prepared according to the method in embodiment 1, it is different
It is that the vacuum degree in the present embodiment during deposition DLC film is 1Pa.Power 200W, carbon source flow 20Sccm.
According to the test method of MIL-48616, to the spy for being deposited with DLC protective film in Examples 1 to 3 and comparative example 1
Device is surveyed to be detected, the results are shown in Table 1,
The performance data of product in 1 embodiment of the present invention 1~3 of table and comparative example 1
The detector for being deposited with DLC protective film in Examples 1 to 3 and comparative example 1 carries out adhesive force in accordance with the following methods
Test, uses cellotape paper (1/2 " width, model L-T-90I class).Adhesive tape is pasted on film surface, is then hung down rapidly
Straight cellotape paper of tearing, visual inspection, result are that the detector for being deposited with DLC protective film in Examples 1 to 3 passes through attached
Put forth effort to test, edge demoulding occurs in the product in comparative example 1 50%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the infrared focal plane array seeker with DLC protective film, comprising the following steps:
A) acetone and working solution is successively used to clean the window of infrared focal plane array seeker；
B) under vacuum conditions by the window of the infrared focal plane array seeker after cleaning, be passed through argon gas, carry out radio frequency etc. from
Son cleaning；
C it) is passed through carbon-source gas again, using radio-frequency plasma enhanced chemical vapor deposition method in infrared focal plane array seeker
Window surface deposit DLC protective film, obtain the infrared focal plane array seeker with DLC protective film；
The step C) radio-frequency power be 100~2500W, the step C) vacuum degree be 3 × 10-3~3 × 10-5Pa。
2. preparation method according to claim 1, which is characterized in that the window packet of the infrared focal plane array seeker
Include the ZnSe layer successively contacted, ZnS layers, Ge layers, ZnS layers and ZnSe layer；
The ZnSe layer is in contact with the DLC protective film.
3. preparation method according to claim 1, which is characterized in that the step B) in vacuum degree be 0.0013~
0.13Pa；
The step B) in argon gas flow be 30~90sccm；
The step B) in radio-frequency power be 300~700W.
4. preparation method according to claim 1, which is characterized in that the carbon-source gas is methane；
The flow of the carbon-source gas is 5~100sccm.
5. preparation method according to claim 1, which is characterized in that the step C) in deposit temperature be 20~200
℃；
The step C) in sedimentation time be 0.1~10min.
6. preparation method according to claim 1, which is characterized in that the step C) deposition process in made using argon gas
For carrier gas；
The flow of the argon gas is 100~200sccm.
7. preparation method according to claim 1, which is characterized in that the working solution is acetone, isopropanol and N- methyl
One or more of pyrrolidones.
8. a kind of infrared focal plane array seeker with DLC protective film, including infrared focal plane array seeker and deposition
In the DLC protective film of the detector window discharge surface；
The infrared focal plane array seeker with DLC protective film is according to preparation described in claim 1~7 any one
Method is prepared.
9. the infrared focal plane array seeker according to claim 8 with DLC protective film, which is characterized in that described
The service band of infrared focal plane array seeker with DLC protective film is 3~5 μm or 8~14 μm.
10. the infrared focal plane array seeker according to claim 8 with DLC protective film, which is characterized in that described
The refractive index of DLC protective film is 1.8~3.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910232823.XA CN109932064B (en) | 2019-03-26 | 2019-03-26 | Infrared focal plane array detector with DLC protective film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910232823.XA CN109932064B (en) | 2019-03-26 | 2019-03-26 | Infrared focal plane array detector with DLC protective film and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN109932064A true CN109932064A (en) | 2019-06-25 |
| CN109932064B CN109932064B (en) | 2020-11-03 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033653A (en) * | 1987-12-22 | 1989-07-05 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN101464528A (en) * | 2008-01-23 | 2009-06-24 | 四川大学 | DLC infrared anti-refiection protective film and method for producing the same |
| CN101736313A (en) * | 2008-11-26 | 2010-06-16 | 北京有色金属研究总院 | Method for preparing diamond-like film on germanium substrate |
| CN102997999A (en) * | 2012-11-26 | 2013-03-27 | 烟台睿创微纳技术有限公司 | Infrared focal plane array detector |
| US20160333186A1 (en) * | 2015-05-15 | 2016-11-17 | Sae Magnetics (H.K.) Ltd. | Article coated with dlc and manufacturing method thereof |
-
2019
- 2019-03-26 CN CN201910232823.XA patent/CN109932064B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033653A (en) * | 1987-12-22 | 1989-07-05 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN101464528A (en) * | 2008-01-23 | 2009-06-24 | 四川大学 | DLC infrared anti-refiection protective film and method for producing the same |
| CN101736313A (en) * | 2008-11-26 | 2010-06-16 | 北京有色金属研究总院 | Method for preparing diamond-like film on germanium substrate |
| CN102997999A (en) * | 2012-11-26 | 2013-03-27 | 烟台睿创微纳技术有限公司 | Infrared focal plane array detector |
| US20160333186A1 (en) * | 2015-05-15 | 2016-11-17 | Sae Magnetics (H.K.) Ltd. | Article coated with dlc and manufacturing method thereof |
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