CN105223634A - The high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage - Google Patents

The high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage Download PDF

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Publication number
CN105223634A
CN105223634A CN201510600064.XA CN201510600064A CN105223634A CN 105223634 A CN105223634 A CN 105223634A CN 201510600064 A CN201510600064 A CN 201510600064A CN 105223634 A CN105223634 A CN 105223634A
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CN
China
Prior art keywords
substrate
zinc sulfide
film
hafnium target
multispectral zinc
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CN201510600064.XA
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Chinese (zh)
Inventor
董茂进
王多书
熊玉卿
王田刚
王济洲
蔡宇宏
徐嶺茂
李凯朋
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无锡泓瑞航天科技有限公司
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Priority to CN201510600064.XA priority Critical patent/CN105223634A/en
Publication of CN105223634A publication Critical patent/CN105223634A/en

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Abstract

The present invention discloses the high low stress membrane thoroughly of a kind of 2.5-10um spectral coverage, described film is the HfON film being coated on multispectral zinc sulfide surface, described method for manufacturing thin film is: one, multispectral zinc sulfide substrate is adopted to deionized water rinsing respectively, analyzes pure acetone ultrasonic cleaning and analyze pure absolute ethyl alcohol ultrasonic cleaning, then cleaned by substrate surface; Two, at vacuum indoor location hafnium target, then multispectral zinc sulfide substrate is installed, between hafnium target and multispectral zinc sulfide substrate, baffle plate is set; Three, by vacuum chamber to 3.0 × 10-3 ~ 5.0 × 10-3Pa, and by substrate heating to 150 ~ 200 DEG C; Four, plasma bombardment is utilized to clean hafnium target 10 ~ 15 minutes; Five, after icon bombardment cleaning hafnium target, open baffle plate, adopt ion beam reaction technology, and pass into nitrogen and oxygen, preparation HfON film.The present invention provides the protective film of good physics, chemistry and Infrared grey image for base material.

Description

The high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage

Technical field

The present invention relates to field of optical films, be specifically related to the high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage.

Background technology

Infrared window, head-shield are the indispensable parts of infrared system, and its function is that protection thermal imaging system washes away lower normal work in high-speed flight and in various harsh environmental baseline.Along with the speed goes of aircraft (as high speed, round-the-clock fighter plane, guided missile etc.) is high, service condition is more and more harsher.Therefore, material of infrared window is except must having the good characteristics such as high infrared transmittivity, low absorption coefficient, also must have high physical strength, wear-resistant, the performance such as anti-blown sand weathering, resist chemical, and under the various harsh conditions such as high temperature, low temperature and radiation effects, its optics and physical and chemical performance have good stability.

But zinc sulphide (ZnS) infrared optical material used at present, required optics, thermal property and mechanical property can not be had simultaneously.It is the feasible solution solving infrared optical system window material problem that infrared window and radome fairing are coated with diaphragm; this rete with double effects is except must having infrared transparent, the absorption coefficient excellent optical property such as little; also should be able to heat shock resistance, high temperature resistant; adhere to well with substrate, the anti-rain-impact of the elements such as infrared window is protected in particularly harsh requirement.The diaphragm transmissivity of current existing ZnS infrared optical material is about 70%, and diaphragm stress is all greater than 0.1MPa.

Protective film for ZnS infrared optical material requires: good with substrate adhesion, to significantly improve original substrate transmitance, has high transmitance at explorer response spectral coverage; High rigidity and friction resistant, to the adaptability that environment for use has had; Will have good adhesiveness to various substrate, can deposit on large scale window, the phenomenons such as its internal stress is little, the demoulding that there will not be stress to cause greatly occur.

Summary of the invention

In view of this, the invention provides the high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage, for base material provides the protective film of good physics, chemistry and Infrared grey image, improve the thermodynamic property of base material.

Realize technical scheme of the present invention as follows:

The high low stress membrane thoroughly of a kind of 2.5-10um spectral coverage, described film is the HfON film being coated on multispectral zinc sulfide substrate by ion beam reaction technology, and film thickness is greater than 1 μm and is less than 2 μm.

The preparation method of described film comprises:

Step one, multispectral zinc sulfide substrate adopted respectively to deionized water rinsing, analyze pure acetone ultrasonic cleaning and analyze pure absolute ethyl alcohol ultrasonic cleaning, then substrate surface is cleaned;

Step 2, at vacuum indoor location hafnium target, then multispectral zinc sulfide substrate is installed, between hafnium target and multispectral zinc sulfide substrate, baffle plate is set;

Step 3, by vacuum chamber to 3.0 × 10 -3~ 5.0 × 10 -3pa, and by substrate heating to 150 ~ 200 DEG C;

Step 4, plasma bombardment is utilized to clean hafnium target 10 ~ 15 minutes;

After step 5, icon bombardment cleaning hafnium target, open baffle plate, adopt ion beam reaction technology, and pass into the mixed gas of nitrogen and oxygen, preparation HfON film.

Further, the throughput ratio that passes into of described nitrogen and oxygen is in the scope of 8:1 ~ 2:1.

Further, step one of the present invention is specially: by clean for multispectral zinc sulfide substrate deionized water rinsing, again with analyzing pure acetone by substrate Ultrasonic Cleaning 15min, then with analyzing pure absolute ethyl alcohol Ultrasonic Cleaning 15min, finally with analysis pure absolute ethyl alcohol, substrate is rinsed well, then by substrate wiping extremely surperficial no marking, scratch and drop remaining trace.

Beneficial effect:

The present invention be coated with the mechanical property that protective film can improve substrate, improve the spectral transmittance of substrate simultaneously.The diaphragm be coated with has high transmissivity at 2.5 ~ 10 μm of spectral coverages; the substrate hardness being coated with diaphragm is greater than 8Gpa and stress is less than 0.1Mpa; the diaphragm be coated with can withstand pull-out test and wipe test, meets the request for utilization of infrared window, head-shield etc.

Accompanying drawing explanation

Fig. 1 is membrane structure schematic diagram.

Fig. 2 is spectrum change before and after zinc sulphide (ZnS) substrate coating.

Embodiment

To develop simultaneously embodiment below in conjunction with accompanying drawing, describe the present invention.

As shown in Figure 1, the invention provides the high low stress membrane thoroughly of a kind of 2.5-10um spectral coverage, described film is the HfON film being coated on multispectral zinc sulfide substrate by ion beam reaction technology, and film thickness is greater than 1 μm and is less than 2 μm.

Preliminary work before film preparation:

Clean vacuum room: remove the rete come off in vacuum chamber with suction cleaner, then dip in absolute ethyl alcohol wiped clean vacuum chamber inwall with absorbent gauze, needs the partially manual polishing of polishing, to keep vacuum chamber clean.

The preparation method of described film comprises:

Step one, multispectral zinc sulfide substrate is put into glassware, clean with deionized water rinsing, again with analyzing pure acetone by substrate Ultrasonic Cleaning 15min, again with analyzing pure absolute ethyl alcohol Ultrasonic Cleaning 15min, finally rinse well with the pure absolute ethyl alcohol of analysis, with the wiping of special chipless cleansing tissue to surperficial no marking, scratch and drop remaining trace.

Step 2, at vacuum indoor location hafnium target (Hf), then multispectral zinc sulfide substrate is installed; Baffle plate is had between hafnium target and multispectral zinc sulfide substrate.

Step 3, open mechanical pump and take out in advance, then open cryopump and the vacuum tightness in vacuum chamber is evacuated to 3.0 × 10 -3~ 5.0 × 10 -3pa, and heated substrate is to 150 ~ 200 DEG C, vacuum tightness is too low affects rete compactness, and the time that too high needs are taken out is oversize, and the temperature range of 150 ~ 200 DEG C is applicable to coating growth.

Step 4, before opening baffle plate deposit film, utilize plasma bombardment hafnium target 10 ~ 15 minutes, be convenient to cleaning hafnium target surface and stable plasma, bombardment time too short hafnium target surface smoothness does not reach requirement, surface clean within 10 ~ 15 minutes, can be made clean, better do not improve more than 15 minutes cleaning performances.

After step 5, icon bombardment cleaning hafnium target, open baffle plate, adopt ion beam reaction technology, and pass into the mixed gas of nitrogen and oxygen, preparation HfON film.Thicknesses of layers is generally greater than 1 μm and is less than 2 μm, can not meet for window defencive function lower than 1 μm of diaphragm, and then rete can because internal stress be excessive, with substrate in conjunction with insecure to be greater than 2 μm.

The throughput ratio that passes into of described nitrogen and oxygen is in the scope of 8:1 ~ 2:1.Within the scope of this, gas flow can make HfON film have high transmissivity at 2.5um-10um, is greater than this scope and transmissivity can be made to reduce, and being less than this scope hardness can significantly decline.

After plated film terminates, test HfON film spectrum, hardness and stress.HfON film BGS6431 type electric thin stress distribution tester provided by the present invention records HfON membrane stress and is less than 0.1MPa, the hardness adopting the NHT nano-hardness tester of CSM company of Switzerland to record HfON film side is greater than 8Gpa, much larger than the hardness (2.5Gpa) of ZnS substrate, system2000 Fourier infrared spectrograph is adopted to test its spectrum, test zinc sulphide substrate is coated with the spectrum after HfON film, 2.5um-10um average transmittance is greater than 80%, if Fig. 2 is spectrum change before and after zinc sulphide (ZnS) substrate coating.Before plated film, transmissivity is approximately 74%, and after plated film, transmissivity is greater than 80%, and transmissivity is significantly improved.

In sum, these are only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (4)

1. the high low stress membrane thoroughly of 2.5-10um spectral coverage, it is characterized in that, described film is the HfON film being coated on multispectral zinc sulfide substrate by ion beam reaction technology, and film thickness is greater than 1 μm and is less than 2 μm.
2. the preparation method of the high low stress membrane thoroughly of a kind of 2.5-10um spectral coverage as claimed in claim 1, is characterized in that, comprise the following steps:
Step one, multispectral zinc sulfide substrate adopted respectively to deionized water rinsing, analyze pure acetone ultrasonic cleaning and analyze pure absolute ethyl alcohol ultrasonic cleaning, then substrate surface is cleaned;
Step 2, at vacuum indoor location hafnium target, then multispectral zinc sulfide substrate is installed, between hafnium target and multispectral zinc sulfide substrate, baffle plate is set;
Step 3, by vacuum chamber to 3.0 × 10 -3~ 5.0 × 10 -3pa, and by substrate heating to 150 ~ 200 DEG C;
Step 4, plasma bombardment is utilized to clean hafnium target 10 ~ 15 minutes;
After step 5, icon bombardment cleaning hafnium target, open baffle plate, adopt ion beam reaction technology, and pass into the mixed gas of nitrogen and oxygen, preparation HfON film.
3. the preparation method of the high low stress membrane thoroughly of a kind of 2.5-10um spectral coverage as claimed in claim 2, it is characterized in that, the throughput ratio that passes into of described nitrogen and oxygen is in the scope of 8:1 ~ 2:1.
4. the preparation method of the high low stress membrane thoroughly of a kind of 2.5-10um spectral coverage as claimed in claim 2, it is characterized in that, step one is specially: by clean for multispectral zinc sulfide substrate deionized water rinsing, again with analyzing pure acetone by substrate Ultrasonic Cleaning 15min, then with analyzing pure absolute ethyl alcohol Ultrasonic Cleaning 15min, finally with analysis pure absolute ethyl alcohol, substrate is rinsed well, then by substrate wiping extremely surperficial no marking, scratch and drop remaining trace.
CN201510600064.XA 2015-09-18 2015-09-18 The high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage CN105223634A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097753A (en) * 2018-08-30 2018-12-28 湖北久之洋红外系统股份有限公司 The preparation method of high adhesion force hard protective film on zinc sulphide window

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0564709A1 (en) * 1991-12-13 1993-10-13 Balzers Aktiengesellschaft Coated transparent substrate, use thereof, method and apparatus of manufacturing such coatings, and hafnium-oxynitride HfOxNy with 1.5 x/y 3 and 2.6 n 2.8
US20110281442A1 (en) * 2009-03-31 2011-11-17 Bevan Malcolm J Methods and apparatus for forming nitrogen-containing layers
CN102914807A (en) * 2012-11-13 2013-02-06 中国航天科技集团公司第五研究院第五一0研究所 Multi-spectral permeability-increasing protection film for zinc sulfide substrate
CN102912293A (en) * 2012-11-13 2013-02-06 中国航天科技集团公司第五研究院第五一0研究所 Multi-spectrum protective film and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0564709A1 (en) * 1991-12-13 1993-10-13 Balzers Aktiengesellschaft Coated transparent substrate, use thereof, method and apparatus of manufacturing such coatings, and hafnium-oxynitride HfOxNy with 1.5 x/y 3 and 2.6 n 2.8
US20110281442A1 (en) * 2009-03-31 2011-11-17 Bevan Malcolm J Methods and apparatus for forming nitrogen-containing layers
CN102914807A (en) * 2012-11-13 2013-02-06 中国航天科技集团公司第五研究院第五一0研究所 Multi-spectral permeability-increasing protection film for zinc sulfide substrate
CN102912293A (en) * 2012-11-13 2013-02-06 中国航天科技集团公司第五研究院第五一0研究所 Multi-spectrum protective film and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097753A (en) * 2018-08-30 2018-12-28 湖北久之洋红外系统股份有限公司 The preparation method of high adhesion force hard protective film on zinc sulphide window

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Application publication date: 20160106