CN105296926B - A kind of anti-reflection composite membrane optical window of hard and preparation method thereof - Google Patents
A kind of anti-reflection composite membrane optical window of hard and preparation method thereof Download PDFInfo
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- CN105296926B CN105296926B CN201510880620.3A CN201510880620A CN105296926B CN 105296926 B CN105296926 B CN 105296926B CN 201510880620 A CN201510880620 A CN 201510880620A CN 105296926 B CN105296926 B CN 105296926B
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Abstract
The invention discloses anti-reflection composite membrane optical windows of a kind of hard and preparation method thereof, belong to optical element film fabrication techniques field.The optical window has Sub | and HL membrane systems, wherein Sub are optical window substrate, and H is germanium binder course, and L is diamond-film-like.The present invention solves the problems, such as that diamond-film-like is mismatched with optical window thermal expansion system and adhesion is poor, realizes the deposition in optical window surface diamond-film-like by introducing germanium binder course between optical window and diamond-film-like；By using the compound of binder course and diamond-film-like, the transmissivity of optical window not only improved, but also improve window surface desertification erosion and weathering ability, while improve the environmental reliability of optical window superficial film, and extended the service life of optical window.
Description
Technical field
The invention belongs to optical element film fabrication techniques fields, and in particular to a kind of anti-reflection composite membrane optical window of hard
And preparation method thereof.
Background technology
In the field studies environment such as sea, space, optical window should not only have good optical characteristics, but also should have
The characteristics such as standby high rigidity, corrosion-resistant, impact resistance.Common optical window material can be ZnS, ZnSe, Si, SiO2、AS2S3、
KCl、CaF2Deng shape can be plate shaped, spherical and other shapes.Optical window use environment is severe, often wind-engaging
Husky and rainwater erosion can generate serious light scattering to incident light by the optical window surface of weathering and husky erosion, will drop
The transmissivity of low optical window, it is serious that optical system will be made ineffective, therefore, high rigidity need to be coated on optical window surface
And there is the film layer of antireflective effect to play protection and prolong the service life.
CN101231352A discloses a kind of infrared optical window HfON/BP anti-reflection protective films and preparation method thereof.It should
Anti-reflection protective film, BP films are inner layer film, are deposited on optical window surface, and HfON films are outer membrane, are deposited on BP films；BP films
Deposition enhances CVD technology using radio frequency plasma, and the deposition of HfON films uses reactive magnetron sputtering technique.This is anti-reflection guarantor
Cuticula has window anti-reflection effect, can improve case hardness, improve wearability.Due to BP films, the property of HfON membrane materials in itself
It influencing, the performances such as intensity, wearability, optical transmittance often have limitation, and its deposition method is more demanding, if
Deposition method is dealt with improperly, and big light reflection can be caused to lose.
Diamond-like (Diamond Like Carbon, DLC) film have the physics similar with diamond thin, chemistry,
Mechanical performance and higher hardness, impact resistance, radiation hardness, wear-resisting, corrosion-resistant, stable chemical performance, and from visible to remote red
Outer almost all band optical clear.DLC film is a kind of ideal optical window protection materials.(light laser and the particle such as Bai Ting
Beam, the 10th phase of volume 18 in October, 2006) a kind of broadband DLC film optical window is had developed, it is accurate using pulse
Molecular laser ablation graphite target deposited practical DLC film window on ZnS substrate materials, in main wave band
For transmitance more than 70%, the uniformity of film layer is better than 95%.
Optical window base material is mismatched with diamond-film-like coefficient of thermal expansion and adhesion is poor, can not be directly in optics
Diamond-film-like deposition on window, the optical property of the diamond-like protective film optical window of prior art preparation is generally relatively low,
Needing further to improve can just meet the requirements.
Invention content
The object of the present invention is to provide a kind of anti-reflection composite membrane optical windows of hard, so as to solve in the prior art, eka-gold
The problem of hard rock film is with optical window coefficient of thermal expansion mismatch and poor adhesion, is realized to the efficient anti-reflection of optical window, and
Improve optical window surface desertification erosion and weathering ability.
Second object of the present invention is to provide the preparation method of the anti-reflection composite membrane optical window of above-mentioned hard.
In order to achieve the goal above, the technical solution adopted in the present invention is：
A kind of anti-reflection composite membrane optical window of hard, the optical window have Sub | and HL membrane systems, wherein Sub are optical window
Substrate, H are germanium binder course, and L is diamond-film-like.
The anti-reflection composite membrane optical window of hard provided by the invention, by set gradually on optical window germanium binder course and
Diamond-like carbon film layer, germanium binder course play the role of connecting optical window and diamond-like carbon film layer, not only have high saturating
Rate is penetrated, and coefficient of thermal expansion, adhesiveness and optical window and diamond-like carbon film layer ensure that its is available all in controlled range
Existing optical thin film preparation process, such as the methods of physical vapour deposition (PVD), chemical vapor deposition, come prepare meet the requirements it is anti-reflection
Protective film.The hard is anti-reflection, and composite membrane optical window solves diamond-film-like and optical window coefficient of thermal expansion mismatch and glues
The problem of attached property difference, had not only improved the transmissivity of optical window, but also improved the surface desertification erosion of optical window and weathering ability.
The optical window substrate material therefor is zinc sulphide or zinc selenide.
The thickness of germanium binder course is 150~200nm；The thickness of diamond-like carbon film layer is 1180~1260nm.
The preparation method of the above-mentioned anti-reflection composite membrane optical window of hard, including using vacuum vapour deposition in optical window substrate
It is upper formation germanium binder course, then using radio frequency plasma method on the germanium binder course diamond-film-like deposition layer.
The vacuum vapour deposition includes the following steps：
1) under vacuum, heating optical window substrate keeps the temperature 1h to 160~200 DEG C；
2) optical window substrate RF radio frequency sources are bombarded into 5~8min；
3) germanium is deposited in optical window substrate, postcooling to room temperature is to get the optical window with germanium binder course；Vapor deposition
Process control vacuum degree is 1.5 × 10-3Pa, evaporation rate 0.3nm/s.
In step 1), before heating, optical window substrate is cleaned using the mixed liquor of alcohol and ether.
In step 3), the thickness of germanium binder course is controlled by crystal oscillator method.
The radio frequency plasma method includes the following steps：
A) under vacuum, there is 3~5min of optical window of germanium binder course using plasma bombardment；
B) using the mixed gas of argon gas and butane as reaction gas, maintenance pressure is 5~7Pa, is generated using radio frequency discharge
Plasma carries out deposition on the germanium binder course of optical window and is coated with, and postcooling to room temperature forms eka-gold on germanium binder course
Hard rock film to get；In the mixed gas, the flow-rate ratio of argon gas and butane is 20~30：160~200 (volume ratios)；Deposition plating
During system, radio-frequency power is 600~800W, and the time being coated with is 1200~1300s.
In step a), the plasma is generated by radio frequency discharge, and gases used is argon gas, and the flow of argon gas is 60
~80sccm, maintenance pressure are 2~4Pa；Radio-frequency power is 300~500W.
In the preparation method of the anti-reflection composite membrane optical window of hard provided by the present invention, germanium binder course is steamed by vacuum
Plating method is formed, and vacuum vapour deposition is that target is placed in vacuum to be evaporated or distil, and is allowed to what is be precipitated in workpiece surface deposition
Resistance heating, induction evaporation mode, electron beam and vacuum arc etc. can be used in process, evaporation source.Diamond-like carbon film layer is to utilize to penetrate
Frequency plasma deposition is formed.Radio frequency plasma belongs to one kind in plasma reinforced chemical vapour deposition, and plasma increases
Extensive chemical vapor deposition is at a certain temperature, to ionize reaction gas using direct current, radio frequency or microwave field, the plasma of generation
Body is directed on substrate under the action of back bias voltage and is reacted with surface, and required film is deposited in substrate surface, etc.
Gas ions can play facilitation to the decomposition of reaction gas and chemical combination, thermal energy can be replaced with electronics, so as in low temperature
Lower preparation large area, the simple substance of high quality or compound film material.
In the preparation method of the anti-reflection composite membrane optical window of hard provided by the present invention, germanium binder course passes through to optical window
The pretreatment of mouth substrate, makes optical window substrate obtain effective activation, is conducive to the formation of germanium binder course uniformly, stable；Pass through
Effective control to germanium joint thickness on the basis of optical transmittance is ensured, can take into account binder course and inside and outside two simultaneously
The binding force of layer.Using Radio frequency plasma in diamond-film-like deposition layer on being coated with the optical window of germanium binder course, pass through
Plasma cleaning (step a)), flow, pressure and the radio-frequency power of mixed gas and the control for being coated with the time, make diamond-like
Film layer and germanium binder course binding force enhance, and deposition gained film layer is fine and close, uniform, stress is small.
The preparation method of the anti-reflection composite membrane optical window of hard provided by the present invention, preparation process is simple, optical window
Substrate, germanium binder course, diamond-film-like interlayer binding force are high, and film layer is fine and close, uniform, stress is small；The selenium being coated with using the present invention
The peak transmission for changing the anti-reflection composite membrane of zinc optical window hard in 7.7~9.5 mu m wavebands is more than 93%, and average transmittance is more than
91%；Using the anti-reflection composite membrane of zinc sulphide optical window hard that is coated with of the present invention 7.7~9.5 mu m wavebands peak transmission
More than 92%, average transmittance is more than 90%, and environment and reliability are satisfied by optical thin film National Military Standard.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
The anti-reflection composite membrane optical window of hard of the present embodiment, the optical window have Sub | and HL membrane systems, wherein Sub are light
Window substrates are learned, H is germanium binder course, and L is diamond-film-like.
The preparation method of the anti-reflection composite membrane optical window of hard of the present embodiment, includes the following steps：
(1) vacuum vapour deposition is coated with germanium binder course in ZnS optical window substrates
1) using the mixed liquor of alcohol and ether, (volume ratio of alcohol and ether is 1:1) optical window substrate is cleaned, is removed
Remove surface irregularities, greasy dirt and auxiliary material；Optical window substrate is placed into vacuum chamber afterwards, is evacuated to 1 × 10-2Pa heats optical window
Mouth substrate keeps the temperature 1 hour to 180 DEG C；
2) optical window substrate RF radio frequency sources are bombarded into 6min；
3) germanium is deposited in optical window substrate, postcooling to room temperature is to get the optical window with germanium binder course；Vapor deposition
Process control vacuum degree is 1.5 × 10-3Pa, evaporation rate 0.3nm/s；Using crystal oscillator method control germanium binder course thickness be
160nm；
The optical window that step (1) obtains has Sub | and H membrane systems, Sub are optical window substrate, and H is germanium binder course；
(2) radio frequency plasma method diamond-film-like deposition on germanium binder course
A) optical window that gained is had germanium binder course places vacuum chamber, is evacuated to 1.5 × 10-3Pa；It is passed through argon gas,
Argon flow amount is 60sccm, and adjusting vacuum chamber valve makes pressure maintain 2.4Pa, opens radio frequency source, adjusts radio-frequency power and is
400w has the optical window 4min of germanium binder course using the plasma bombardment that radio frequency discharge generates；
B) mixed gas of argon gas and butane, argon flow amount 24sccm are passed through to vacuum chamber, the flow of butane is
180sccm, adjusting vacuum chamber valve makes pressure maintain 6Pa, opens radio frequency source, and adjusting radio-frequency power is 700W, utilizes radio frequency
Discharge the plasma generated, and deposition is carried out on the germanium binder course of optical window and is coated with, and the time being coated with is 1240s, is cooled down
To room temperature, formed on germanium binder course thickness for 1180nm diamond-film-likes to get；
The optical window that step (2) obtains has Sub | and HL membrane systems, wherein Sub are optical window substrate, and H is closed for germanium junction
Layer, L is diamond-film-like.
Embodiment 2
The anti-reflection composite membrane optical window of hard of the present embodiment, the optical window have Sub | and HL membrane systems, wherein Sub are light
Window substrates are learned, H is germanium binder course, and L is diamond-film-like.
The preparation method of the anti-reflection composite membrane optical window of hard of the present embodiment, includes the following steps：
(1) vacuum vapour deposition is coated with germanium binder course in ZnS optical window substrates
1) using the mixed liquor of alcohol and ether, (volume ratio of alcohol and ether is 1:1) optical window substrate is cleaned, is removed
Remove surface irregularities, greasy dirt and auxiliary material；Optical window substrate is placed into vacuum chamber afterwards, is evacuated to 1 × 10-2Pa heats optical window
Mouth substrate keeps the temperature 1 hour to 200 DEG C；
2) optical window substrate RF radio frequency sources are bombarded into 5min；
3) germanium is deposited in optical window substrate, postcooling to room temperature is to get the optical window with germanium binder course；Vapor deposition
Process control vacuum degree is 1.5 × 10-3Pa, evaporation rate 0.3nm/s；Using crystal oscillator method control germanium binder course thickness be
150nm；
The optical window that step (1) obtains has Sub | and H membrane systems, wherein Sub are optical window substrate, and H is germanium binder course；
(2) radio frequency plasma method diamond-film-like deposition on germanium binder course
A) optical window that gained is had germanium binder course places vacuum chamber, is evacuated to 1.5 × 10-3Pa；It is passed through argon gas,
Argon flow amount is 80sccm, and adjusting vacuum chamber valve makes pressure maintain 4Pa, opens radio frequency source, and adjusting radio-frequency power is 500w,
There is the optical window 3min of germanium binder course using the plasma bombardment that radio frequency discharge generates；
B) mixed gas of argon gas and butane, argon flow amount 30sccm are passed through to vacuum chamber, the flow of butane is
200sccm, adjusting vacuum chamber valve makes pressure maintain 5Pa, opens radio frequency source, and adjusting radio-frequency power is 600W, utilizes radio frequency
Discharge the plasma generated, and deposition is carried out on the germanium binder course of optical window and is coated with, and the time being coated with is 1300s, is cooled down
To room temperature, formed on germanium binder course thickness for 1200nm diamond-film-likes to get；
The optical window that step (2) obtains has Sub | and HL membrane systems, wherein Sub are optical window substrate, and H is closed for germanium junction
Layer, L is diamond-film-like.
Embodiment 3
The anti-reflection composite membrane optical window of hard of the present embodiment, the optical window have Sub | and HL membrane systems, wherein Sub are light
Window substrates are learned, H is germanium binder course, and L is diamond-film-like.
The preparation method of the anti-reflection composite membrane optical window of hard of the present embodiment, includes the following steps：
(1) vacuum vapour deposition is coated with germanium binder course in ZnSe optical window substrates
1) using the mixed liquor of alcohol and ether, (volume ratio of alcohol and ether is 1:1) optical window substrate is cleaned, is removed
Remove surface irregularities, greasy dirt and auxiliary material；Optical window substrate is placed into vacuum chamber afterwards, is evacuated to 1 × 10-2Pa heats optical window
Mouth substrate keeps the temperature 1 hour to 160 DEG C；
2) optical window substrate RF radio frequency sources are bombarded into 6min；
3) germanium is deposited in optical window substrate, postcooling to room temperature is to get the optical window with germanium binder course；Vapor deposition
Process control vacuum degree is 1.5 × 10-3Pa, evaporation rate 0.3nm/s；Using crystal oscillator method control germanium binder course thickness be
170nm；
The optical window that step (1) obtains has Sub | and H membrane systems, wherein Sub are optical window substrate, and H is germanium binder course；
(2) radio frequency plasma method diamond-film-like deposition on germanium binder course
A) optical window that gained is had germanium binder course places vacuum chamber, is evacuated to 1.5 × 10-3Pa；It is passed through argon gas,
Argon flow amount is 65sccm, and adjusting vacuum chamber valve makes pressure maintain 3Pa, opens radio frequency source, and adjusting radio-frequency power is 400w,
The plasma bombardment generated using radio frequency discharge is coated with the optical window 5min of germanium binder course；
B) mixed gas of argon gas and butane, argon flow amount 26sccm are passed through to vacuum chamber, the flow of butane is
170sccm, adjusting vacuum chamber valve makes pressure maintain 5.8Pa, opens radio frequency source, and adjustings radio-frequency power is 700W, using penetrating
The plasma that frequency electric discharge generates carries out deposition on the germanium binder course of optical window and is coated with, and the time being coated with is 1250s, cold
But to room temperature, formed on germanium binder course thickness for 1240nm diamond-film-likes to get；
The optical window that step (2) obtains has Sub | and HL membrane systems, wherein Sub are optical window substrate, and H is closed for germanium junction
Layer, L is diamond-film-like.
Embodiment 4
The anti-reflection composite membrane optical window of hard of the present embodiment, the optical window have Sub | and HL membrane systems, wherein Sub are light
Window substrates are learned, H is germanium binder course, and L is diamond-film-like.
The preparation method of the anti-reflection composite membrane optical window of hard of the present embodiment, includes the following steps：
(1) vacuum vapour deposition is coated with germanium binder course in ZnSe optical window substrates
1) using the mixed liquor of alcohol and ether, (volume ratio of alcohol and ether is 1:1) optical window substrate is cleaned, is removed
Remove surface irregularities, greasy dirt and auxiliary material；Optical window substrate is placed into vacuum chamber afterwards, is evacuated to 1 × 10-2Pa heats optical window
Mouth substrate keeps the temperature 1 hour to 160 DEG C；
2) optical window substrate RF radio frequency sources are bombarded into 8min；
3) germanium is deposited in optical window substrate, postcooling to room temperature is to get the optical window with germanium binder course；Vapor deposition
Process control vacuum degree is 1.5 × 10-3Pa, evaporation rate 0.3nm/s；Using crystal oscillator method control germanium binder course thickness be
200nm；
The optical window that step (1) obtains has Sub | and H membrane systems, wherein Sub are optical window substrate, and H is germanium binder course；
(2) radio frequency plasma method diamond-film-like deposition on germanium binder course
A) optical window that gained is coated with to germanium binder course places vacuum chamber, is evacuated to 1.5 × 10-3Pa；It is passed through argon gas,
Argon flow amount is 65sccm, and adjusting vacuum chamber valve makes pressure maintain 2Pa, opens radio frequency source, and adjusting radio-frequency power is 300w,
The plasma bombardment generated using radio frequency discharge is coated with the optical window 5min of germanium binder course；
B) mixed gas of argon gas and butane, argon flow amount 20sccm are passed through to vacuum chamber, the flow of butane is
170sccm, adjusting vacuum chamber valve makes pressure maintain 7Pa, opens radio frequency source, and adjusting radio-frequency power is 800W, utilizes radio frequency
Discharge the plasma generated, and deposition is carried out on the germanium binder course of optical window and is coated with, and the time being coated with is 1200s, is cooled down
To room temperature, formed on germanium binder course thickness for 1260nm diamond-film-likes to get；
The optical window that step (2) obtains has Sub | and HL membrane systems, wherein Sub are optical window substrate, and H is closed for germanium junction
Layer, L is diamond-film-like.
Test example
This test example to the hard of Examples 1 to 4 anti-reflection composite membrane optical window in the transmissivity of 7.7~9.5 mu m wavebands
It is detected, the transmissivity test of film layer is what is completed on the Spectrum GX type fourier spectrometers of PE companies production, is surveyed
100% correction is first carried out before examination to instrument, the sample that embodiment is coated with then is placed and measures.The results are shown in Table 1.
The transmissivity testing result of the anti-reflection composite membrane optical window of hard of 1 Examples 1 to 4 of table
| Serial number | Peak transmission | Average transmittance |
| Embodiment 1 | 92.4 | 90.5 |
| Embodiment 2 | 92.0 | 90.6 |
| Embodiment 3 | 93.5 | 91.3 |
| Embodiment 4 | 93.1 | 91.5 |
By the result of the test of table 1 it is found that the anti-reflection composite membrane of ZnS infrared optical window hard being coated with is in 7.7~9.5 μm of waves
The peak transmission of section is more than 92.0%, and average transmittance is more than 90.5%；The zinc selenide substrate optical window being coated with is hard
Matter is anti-reflection composite membrane 7.7~9.5 mu m wavebands peak transmission more than 93.0%, average transmittance is more than 91.3%.
The environment of the anti-reflection composite membrane optical window of hard of the present invention is satisfied by optical thin film National Military Standard with reliability.
Claims (7)
1. a kind of anti-reflection composite membrane optical window of hard, it is characterised in that：The optical window has Sub|HL membrane systems, wherein Sub
For optical window substrate, H is germanium binder course, and L is diamond-film-like；
The optical window substrate material therefor is zinc sulphide or zinc selenide；
The thickness of germanium binder course is 150~200nm；The thickness of diamond-like carbon film layer is 1180~1260nm；
The preparation method of the optical window, including：Germanium binder course is formed in optical window substrate using vacuum vapour deposition, then
Using radio frequency plasma method on the germanium binder course diamond-film-like deposition layer.
2. a kind of preparation method of the anti-reflection composite membrane optical window of hard as described in claim 1, it is characterised in that：Including：
Germanium binder course is formed in optical window substrate using vacuum vapour deposition, is then closed using radio frequency plasma method in the germanium junction
Diamond-film-like deposition layer on layer.
3. the preparation method of the anti-reflection composite membrane optical window of hard according to claim 2, it is characterised in that：The vacuum
Vapour deposition method includes the following steps：
1）Under vacuum, heating optical window substrate keeps the temperature 1h to 160~200 DEG C；
2）Optical window substrate RF radio frequency sources are bombarded into 5~8min；
3）Germanium is deposited in optical window substrate, postcooling to room temperature is to get the optical window with germanium binder course；Vapor deposition process
It is 1.5 × 10 to control vacuum degree-3Pa, evaporation rate 0.3nm/s.
4. the preparation method of the anti-reflection composite membrane optical window of hard according to claim 3, it is characterised in that：Step 1）
In, before heating, optical window substrate is cleaned using the mixed liquor of alcohol and ether.
5. the preparation method of the anti-reflection composite membrane optical window of hard according to claim 3, it is characterised in that：Step 3）
In, pass through the thickness of crystal oscillator method control germanium binder course.
6. the preparation method of the anti-reflection composite membrane optical window of hard according to claim 2, it is characterised in that：The radio frequency
Plasma method includes the following steps：
a）Under vacuum, there is 3~5min of optical window of germanium binder course using plasma bombardment；
b）Using the mixed gas of argon gas and butane as reaction gas, maintenance pressure be 5~7Pa, using radio frequency discharge generate etc. from
Daughter carries out deposition on the germanium binder course of optical window and is coated with, and postcooling to room temperature forms diamond-like on germanium binder course
Film to get；In the mixed gas, the flow-rate ratio of argon gas and butane is 20~30：160~200；During deposition is coated with, penetrate
Frequency power is 600~800W, and the time being coated with is 1200~1300s.
7. the preparation method of the anti-reflection composite membrane optical window of hard according to claim 6, it is characterised in that：Step a）
In, the plasma is generated by radio frequency discharge, and gases used is argon gas, and the flow of argon gas is 60~80sccm, is maintained
Pressure is 2~4Pa；Radio-frequency power is 300~500W.
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