CN110196460A - A kind of infrared stealth metal nanoparticle Meta Materials composite membrane compatible with visible light stealth and preparation method thereof - Google Patents
A kind of infrared stealth metal nanoparticle Meta Materials composite membrane compatible with visible light stealth and preparation method thereof Download PDFInfo
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- CN110196460A CN110196460A CN201910544936.3A CN201910544936A CN110196460A CN 110196460 A CN110196460 A CN 110196460A CN 201910544936 A CN201910544936 A CN 201910544936A CN 110196460 A CN110196460 A CN 110196460A
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
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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
- C23C14/3464—Sputtering using more than one target
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
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- G02B5/0808—Mirrors having a single reflecting layer
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Abstract
A kind of infrared stealth metal nanoparticle Meta Materials composite membrane compatible with visible light stealth and preparation method thereof, belongs to thin-film material infrared stealth technology field.The composite membrane is equably arranged in oxide base by the metal nanoparticle having a size of 5nm~20nm, and metal nanoparticle is size uniformity, and change in size is 1%~5%, and composite film thickness is 20nm~200nm.The alloy that the metal is the metals such as Al, Ti, Au, Ag, Cu and is made of these metals, the oxide are SiO2、SiO、Al3O2、TiO2Equal nonmetal oxides.Metal nanoparticle Meta Materials composite membrane prepared by the present invention can be realized metal nanoparticle size is controllable, gap is adjustable, arrangement is neat etc., when thickness is only 200nm, infrared band reflectivity is up to 99%, the reflectivity of visible waveband realizes the compatibility of visible light stealth and infrared stealth down to 30%.
Description
Technical field
The invention belongs to thin-film material infrared stealth technology fields, and in particular to a kind of compatible with visible light stealth infrared
Stealthy metal nanoparticle Meta Materials composite membrane and preparation method thereof.
Background technique
For all objects in nature, as long as its temperature is higher than absolute zero (0K), always object can be continuous
Thermal energy is become radiation energy by ground, to send out heat radiation.Most of infrared detection technique is by red between target and background
The difference of external radiation detects target, and especially at night, target object often shows more highlighted on infrared thermal imaging
Degree, to form sharp contrast with background.It is based on the above theory, infrared imaging detection technology answering in high-tech war
With also more and more extensive, such as thermal infrared imager known to us, it is exactly to be imaged using the heat radiation of object, detects object
The accurate location of body, meanwhile, detection range is remote, usage mode is hidden and anti-electromagnetic interference capability is strong, this make military equipment and
The safety of facility, existence are all received and are seriously threatened.Target survival ability in the complicated and severe electromagnetic environment is solved to ask
Topic, must just improve the infrared biological treatability of target.Therefore, various countries also increasingly pay attention to the development of infrared stealth technology.
Infrared stealth technology is to pass through the infrared signature for reducing target object, reduces its infrared spoke generated with background
The contrast penetrated reduces the probability itself being detected.For example, the positions such as engine of aircraft can outside radiations heat energy, generate
Infrared spray is let out, and is covered with Infrared stealthy materials if applied at the position that these are easy to produce heat radiation, by effective reduction aircraft
Infrared signature reduces its radiation thermal difference with sky, so that the risk that aircraft is detected is effectively reduced, to reach
The effect of " stealthy ".Infrared stealth film because its performance is high, effect is good, use when do not limited by target object shape the advantages that,
By it is believed that be most to have the stealthy means of development potentiality, and infrared stealth means being nowadays most widely used.According to this
Di Fen-Boltzmann law is it is found that we can be by reducing the infrared emittance of film surface and reducing target object surface
Achieve the purpose that reduce target object infrared energy in terms of temperature two.Due to large-scale military equipment need it is powerful
Power device is driven, and power drive can inevitably generate higher temperature, if passing through the method for control temperature
Large effect will obviously be generated to the performance of power device to reduce its infrared energy, therefore research prepares low-launch-rate
Coating becomes more fruitful method in Important Problems concerned by people and stealth technology.In recent years, low infrared emissivity
Material is widely used on civilian and military, such as industrial heat loss controls, military equipment is hidden, protection.Currently,
Although the domestic research in terms of infrared stealth technology reports the research of low-emissivity material also in the exploratory stage
Have very much.In past ten years, part metals and its oxide have become the important material for studying infrared low-emissivity film
Material.Wherein metal Al is due to itself having a lower emissivity and cheap and easy to get and be widely used, but its surface
High gloss keeps it very high to the reflectivity of visible light, is unfavorable for the compatibility of visible light stealth, this makes cheap metal Al again
Certain limitation is above provided in infrared stealth application.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of infrared stealth metal nanos compatible with visible light stealth
Particle Meta Materials composite membrane and preparation method thereof.Metal nanoparticle Meta Materials composite film thickness prepared by the present invention is 20nm
~200nm, infrared band reflectivity are up to 99%, and absorptivity 0 realizes infrared stealth function.At the same time, it can be seen that
The reflectivity of wave band realizes the compatibility of visible light stealth and infrared stealth down to 30%.
One aspect of the present invention provides a kind of metal nanoparticle Meta Materials composite membrane, and the composite membrane includes oxide base
The metal nanoparticle for being 5nm~20nm with the size being evenly arranged in the oxide base.
Based on above technical scheme, it is preferred that the metal is in the alloy of Al, Ti, Au, Ag, Cu or above-mentioned metal
It is at least one；
Based on above technical scheme, it is preferred that the oxide is SiO2、SiO、Al3O2、TiO2One of；
Metal nanoparticle is size uniformity in the present invention, and change in size is 1%~5%.
It is a further object of the present invention to provide a kind of infrared stealth metal nanoparticle super materials compatible with visible light stealth
Expect the preparation method of composite membrane, comprising the following steps: using pretreated quartz plate or monocrystalline silicon piece as substrate；With metallic target and base
Bottom oxide target be raw material cosputtering composite membrane, metallic target purity >=99.99%, the oxide target purity >=
99.999%；Sputtering parameter: the vacuum degree of coating chamber is superior or equal to 3.2 × 10-3Pa, Ar air pressure are 0.3Pa, splash-proofing sputtering metal by force
Dc source power 200W~400W, sputter radio-frequency power supply power 100W~400W of oxide；Cosputtering is to compound film thickness
Degree is 20nm~200nm；
The cosputtering: opening the DC power supply of splash-proofing sputtering metal, after metallic target starter, opens the radio frequency of sputtering oxide
Power supply slowly increases its incident power to oxide target material starter.When two targets are in ignition phase, metallic target is adjusted
The radio-frequency power supply power that the Dc source power and oxide target used uses is to setting value.Sample stage rotating turret is opened, then
Open the cosputtering that the baffle between sample stage and target carries out metal and oxide.
The metal is at least one of Al, Ti, Au, Ag, Cu or the alloy of above-mentioned metal；
The oxide is SiO2、SiO、Al3O2、TiO2One of；
Preferably, the pretreated quartz plate or monocrystalline silicon piece are the rotten-stone for selecting surface roughness to be less than 0.5nm
English piece or monocrystalline silicon piece are successively cleaned by ultrasonic 15min in acetone, deionized water and alcoholic solution, with the high pressure of high-purity argon gas
Spray gun drying.
The present invention a kind of the infrared stealth metal nanoparticle Meta Materials composite membrane and its preparation compatible with visible light stealth
Method, compared with prior art, beneficial effect is:
1, the present invention a kind of the infrared stealth metal nanoparticle Meta Materials composite membrane and its system compatible with visible light stealth
Preparation Method, prepares that metal nanoparticle size is controllable, gap is adjustable, arrangement is neat by metal and oxide cosputtering
Metal nanoparticle composite membrane, realize that the compatible performance of visible-infrared stealth is adjustable；
2, the compatible infrared stealth metal nanoparticle Meta Materials composite membrane of a kind of and visible light stealth of the invention, thickness
When for 20nm~200nm, infrared band reflectivity is up to 99%, and absorptivity 0 realizes the infrared stealth function of microthin coating
Energy；
3, the compatible infrared stealth metal nanoparticle Meta Materials composite membrane of a kind of and visible light stealth of the invention, red
While wave section reflectivity is up to 99%, it is seen that the reflectivity of wave band realizes visible light stealth and infrared hidden down to 30%
The compatibility of body；
4, the preparation method of the compatible infrared stealth metal nanoparticle Meta Materials composite membrane of visible light stealth of the invention,
Equipment is simply reproducible, and film growth controllability is good, and the composite membrane of preparation is with high purity, high-quality, low in cost.
Detailed description of the invention
Fig. 1 is the three dimensional structure diagram of composite membrane of the present invention.Wherein, 1- metal nanoparticle；2- oxide base；
Fig. 2 is Al-SiO prepared by the embodiment of the present invention 12Nano particle Meta Materials composite membrane cross-section TEM high-resolution and electricity
Sub- diffraction pattern；
Fig. 3 is Al-SiO prepared by the embodiment of the present invention 12The infrared transmission of nano particle Meta Materials composite membrane different-thickness
Rate spectrogram；
Fig. 4 is Al-SiO prepared by the embodiment of the present invention 12The infrared external reflection of nano particle Meta Materials composite membrane different-thickness
Rate spectrogram；
Transmission of visible light, reflectivity and absorptivity spectrogram when Fig. 5 is Al thickness of metal film 200nm；
Fig. 6 is Al-SiO prepared by the embodiment of the present invention 12It is visible when nano particle Meta Materials composite film thickness 200nm
Light transmission, reflectivity and absorptivity spectrogram.
Specific embodiment
Illustrate a specific embodiment of the invention with reference to the accompanying drawing.
Test method described in following embodiments is unless otherwise specified usual manner；Agents useful for same and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
Using DC power supply splash-proofing sputtering metal Al, SiO is sputtered using radio-frequency power supply2, Al-SiO2Nano particle Meta Materials are compound
The preparation method of film the following steps are included:
Step 1, substrate selection and pretreatment:
Select surface roughness be less than 0.5nm crystal orientation for (100) polished silicon slice, by silicon wafer successively in acetone, go
It is cleaned by ultrasonic 15min in ionized water and alcoholic solution, and is dried up with the high-pressure spray gun of high-purity argon gas；
Step 2, target prepares:
Metal Al target purity >=99.99% used, SiO used2Two kinds of targets are respectively put by target purity >=99.999%
In 2 target position, target baffle is closed；
Step 3, compound film preparation:
The substrate handled in step 1 is put on sample stage.When the vacuum degree of coating chamber is better than 3.2 × 10-3When Pa, it is passed through
Ar gas, pressure 0.3Pa open the DC power supply of sputtering Al, after metal Al target starter, open sputtering SiO2Radio frequency electrical
Source slowly increases its incident power to SiO2Target starter.When two targets are in ignition phase, adjust what Al target used
Dc source power is to 260W, SiO2The radio-frequency power supply power that target uses is to 200W.Sample stage rotating turret is opened, then opens sample
Baffle between sample platform and target carries out Al and SiO2Cosputtering to film thickness be 20nm~200nm；
Step 4, after plated film, baffle, shielding power supply and motor rotating switch are closed, is passed through sky after molecular pump shutdown
Gas opens cavity and takes out composite films.
The three-dimensional structure of metal nanoparticle Meta Materials composite films is made as shown in Figure 1, TEM figure is as shown in Figure 2；Its
Middle Fig. 2 can be seen that composite membrane by Al nano particle and the SiO for coating it2Composition, also, the size of Al nano particle is
5nm。
Al-SiO is made2Ir transmissivity, the reflectivity spectrogram of nano particle Meta Materials composite membrane different-thickness be respectively
Fig. 3 and 4 can be seen that the increase with composite film thickness by comparison, and ir transmissivity is gradually reduced, and reflectivity is gradually
Increase.Work as Al-SiO2When nano particle Meta Materials composite film thickness is 200nm, infrared reflectivity is up to 99%, and absorptivity is
0, realize infrared stealth function.Transmission of visible light, reflectivity and absorptivity spectrogram when Al thickness of metal film 200nm and
Al-SiO is made2Transmission of visible light, reflectivity and absorptivity spectrogram point when nano particle Meta Materials composite film thickness 200nm
Not Wei Figures 5 and 6, by comparison as can be seen that visible reflectance when simple Al thickness of metal film 200nm is up to
90%, and Al-SiO is made2It is hidden to realize visible light down to 30% for the reflectivity of nano particle Meta Materials composite membrane visible waveband
The compatibility of body and infrared stealth.
Embodiment 2
Using DC power supply splash-proofing sputtering metal Ti, SiO is sputtered using radio-frequency power supply2, Ti-SiO2Nano particle Meta Materials are compound
The preparation method of film the following steps are included:
Step 1, substrate selection and pretreatment:
Select surface roughness be less than 0.5nm crystal orientation for (100) polished silicon slice, by silicon wafer successively in acetone, go
It is cleaned by ultrasonic 15min in ionized water and alcoholic solution, and is dried up with the high-pressure spray gun of high-purity argon gas；
Step 2, target prepares:
Metal Ti target purity >=99.99% used, SiO used2Two kinds of targets are respectively put by target purity >=99.999%
In 2 target position, target baffle is closed；
Step 3, compound film preparation:
The substrate handled in step 1 is put on sample stage.When the vacuum degree of coating chamber is better than 3.2 × 10-3When Pa, it is passed through
Ar gas, pressure 0.3Pa open the DC power supply of sputtering Ti, after metal Ti target starter, open sputtering SiO2Radio frequency electrical
Source slowly increases its incident power to SiO2Target starter.When two targets are in ignition phase, adjust what Ti target used
Dc source power is to 200W, SiO2The radio-frequency power supply power that target uses is to 400W.Sample stage rotating turret is opened, then opens sample
Baffle between sample platform and target carries out Ti and SiO2Cosputtering to film thickness be 20nm~200nm；
Step 4, after plated film, baffle, shielding power supply and motor rotating switch are closed, is passed through sky after molecular pump shutdown
Gas opens cavity and takes out composite films.
Embodiment 3
Alloy TiAl is sputtered using DC power supply, SiO is sputtered using radio-frequency power supply2, TiAl-SiO2Nano particle Meta Materials
The preparation method of composite membrane the following steps are included:
Step 1, substrate selection and pretreatment:
Select surface roughness be less than 0.5nm crystal orientation for (100) polished silicon slice, by silicon wafer successively in acetone, go
It is cleaned by ultrasonic 15min in ionized water and alcoholic solution, and is dried up with the high-pressure spray gun of high-purity argon gas；
Step 2, target prepares:
Metal TiAl target purity >=99.99% used, SiO used2Target purity >=99.999% puts two kinds of targets respectively
Enter in 2 target position, closes target baffle；
Step 3, compound film preparation:
The substrate handled in step 1 is put on sample stage.When the vacuum degree of coating chamber is better than 3.2 × 10-3When Pa, it is passed through
Ar gas, pressure 0.3Pa open the DC power supply of sputtering TiAl, after metal TiAl target starter, open sputtering SiO2Radio frequency
Power supply slowly increases its incident power to SiO2Target starter.When two targets are in ignition phase, adjusting TiAl target makes
Dc source power is to 400W, SiO2The radio-frequency power supply power that target uses is to 100W.Sample stage rotating turret is opened, then is beaten
The baffle opened between sample stage and target carries out TiAl and SiO2Cosputtering to film thickness be 20nm~200nm；
Step 4, after plated film, baffle, shielding power supply and motor rotating switch are closed, is passed through sky after molecular pump shutdown
Gas opens cavity and takes out composite films.
Claims (9)
1. a kind of infrared stealth composite membrane compatible with visible light stealth, which is characterized in that the composite membrane includes oxide-base
Bottom and the metal nanoparticle being arranged in the oxide base；Composite film thickness is 20nm~200nm；The metal nano
The size of particle is 5nm~20nm.
2. composite membrane according to claim 1, which is characterized in that metal in the metal nanoparticle be Al, Ti,
The alloy of Au, Ag, Cu or above-mentioned metal.
3. composite membrane according to claim 1, which is characterized in that the oxide base is SiO2、SiO、Al3O2、TiO2。
4. the preparation method of the infrared multi-Functional Camouflage composite membrane of visible light-described in claim 1, which is characterized in that including following
Step: using pretreated quartz plate or monocrystalline silicon piece as substrate；Using metallic target and oxide target as raw material cosputtering composite membrane.
5. the preparation method according to claim 4, which is characterized in that cosputtering parameter: the vacuum degree of coating chamber be better than or
Equal to 3.2 × 10-3Pa, Ar air pressure are 0.3Pa by force, and Dc source power 200W~400W of splash-proofing sputtering metal sputters oxide
Radio-frequency power supply power 100W~400W；Cosputtering to composite film thickness is 20nm~200nm.
6. the preparation method according to claim 4, which is characterized in that metallic target purity >=99.99%, the oxidation
Object target purity >=99.999%.
7. preparation method according to claim 5, which is characterized in that the step of the cosputtering:
(1) DC power supply for opening splash-proofing sputtering metal opens the radio-frequency power supply of sputtering oxide after metallic target starter；
(2) increase radio-frequency power supply incident power and adjust gold when two targets are in ignition phase to oxide target material starter
Belong to the Dc source power that target uses and the radio-frequency power supply power that oxide target uses to setting value；
(3) sample stage rotating turret is opened, then opens baffle between sample stage and target and carries out splashing altogether for metal and oxide
It penetrates.
8. according to the method described in claim 4, it is characterized in that, the preprocessing process of the quartz plate or monocrystalline silicon piece are as follows:
Surface roughness is selected to be less than the polishing quartz plate or monocrystalline silicon piece of 0.5nm, successively in acetone, deionized water and alcoholic solution
After ultrasonic cleaning, dried up with the high-pressure spray gun of high-purity argon gas.
9. according to the method described in claim 4, it is characterized in that, closing baffle, sputtering after the cosputtering composite membrane
Power supply and motor rotating switch are passed through air after molecular pump shutdown, open cavity and take out the composite membrane.
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| CN113403594A (en) * | 2021-05-24 | 2021-09-17 | 西北工业大学 | High-temperature-resistant, water-oxygen-resistant and low-infrared-emissivity composite film for ceramic matrix composite and preparation method thereof |
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Application publication date: 20190903 |