CN114089448A - Infrared stealth flexible film and preparation method thereof - Google Patents

Infrared stealth flexible film and preparation method thereof Download PDF

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CN114089448A
CN114089448A CN202111372177.0A CN202111372177A CN114089448A CN 114089448 A CN114089448 A CN 114089448A CN 202111372177 A CN202111372177 A CN 202111372177A CN 114089448 A CN114089448 A CN 114089448A
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infrared stealth
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俞磊
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Optical Film Technology Co ltd
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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
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • 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
    • C23C14/0623—Sulfides, selenides or tellurides
    • C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses an infrared stealth flexible film which comprises a flexible substrate and a film coating layer on the surface, wherein the film coating layer is formed by alternately preparing a high-refractive-index material and a low-refractive-index material, and the average reflectivity of the film coating layer in a wave band of 8-14 mu m is more than 95%. The infrared stealth flexible film substrate prepared by the preparation method is soft, can be curled, can resist the high temperature of 300 ℃ per se, and can be applied to the environment below 300 ℃. The infrared emissivity is extremely low, the infrared stealth effect is good, the film layer is firm, and the preparation is simple.

Description

Infrared stealth flexible film and preparation method thereof
Technical Field
The invention relates to the field of film materials and infrared stealth, in particular to an infrared stealth flexible film and a preparation method thereof.
Background
Under normal atmospheric conditions, water vapor, carbon dioxide, ozone, particulate matter, etc. can absorb and scatter infrared radiation. Wherein, the transmission of infrared light in wave bands of 3-5 μm and 8-14 μm is high, so that the two wave bands are often used as infrared detection windows in military, wherein the wave band of 8-14 μm corresponds to the normal earth environment temperature, and the wave band of 3-5 μm corresponds to the high-temperature zone above 300 ℃.
In contrast to infrared detection, infrared stealth approaches also have emerged. According to Stefan-Boltzmann law, the total power E ═ sigma-T of radiation from an object4Wherein σ is a boltzmann constant, and ε is an emissivity of the object; t is the absolute temperature of the object. Maximum detection distance R of infrared detector varies from one to another1/2Thermal infrared imaging is a thermal image formed by receiving and distinguishing the difference between the target itself and the surrounding radiation, and its contrast: c ═ E (E-E)b)/Eb. In general, the temperature of the object to be detected is always higher than the ambient temperature, so E>EbTherefore, one of the principles of infrared stealth is to make the total radiation power E of the object to be measured approach the environmental radiation power E by reducing the emissivity epsilonb。
In recent years, there have been many researches on reducing the emissivity epsilon of an object, such as patent CN109233410A which mentions that the infrared radiation intensity and the identifiability thereof in the background are reduced by coating with a special paint, and patent CN104991291A achieves a low emissivity of 0.08 by magnetron sputtering coating on a Si substrate. But the coating is difficult to achieve the ultra-low emissivity achieved by coating, and the coating cannot be used on soft fabrics achieved by the coating. Thus limiting the application scenarios.
Disclosure of Invention
The technical problem solved by the invention is that a proper flexible substrate material is selected for an environment below 300 ℃, and the infrared radiation emissivity lower than 0.05 is realized in an infrared band of 8-14 mu m by reasonably designing a coating material, a film layer structure and a coating method, so that a practical infrared stealth flexible film is prepared.
The infrared stealth flexible film has a substrate made of a polyimide plastic film which is resistant to high temperature of 300 ℃ and soft, and is coated with a layer of high-refractive-index material and a layer of low-refractive-index material alternately. Wherein the high refractive index material is Ge and Si, and the low refractive index material is ZnS and ZnSe. For comprehensive cost and performance considerations, Ge and ZnS are preferred. Preferably, each layer is typically between 20 nm and 3 μm thick.
The film layer structure has the design effect that the average reflectivity is more than 95% in a wave band of 8-14 mu m. According to the law of conservation of energy, the absorption rate α, reflectance ρ and transmittance τ of an object to infrared rays have the following relationships: α + ρ + τ is 1, and for infrared opaque objects, τ is 0, and α is 1 — ρ. According to kirchhoff's law, the absorptivity of an object under thermal equilibrium conditions is equal to the emissivity: α ═ ε. From this, ε is 1- ρ. Therefore, the reflectivity rho can be used for calculating the emissivity epsilon, and the design and calculation process is simplified.
Related industry personnel can simply realize the purpose by adjusting the number of layers, the thickness and the material type of the film layer according to the required specific emissivity value.
The invention provides a preparation method of the infrared stealth flexible film, which comprises the following steps:
(1) the polyimide film substrate is unfolded and fixed on a film coating tool of a film coating machine
(2) Vacuumizing and heating
(3) Ion bombardment to remove adsorbed molecules and clean the substrate
(4) And heating the coating material by using electron beams or resistors, coating one layer to a set thickness, then coating the other layer, and alternately stacking the layers one by one until all designed film layers are coated.
In the preparation method, the coating machine is a vacuum evaporation coating machine.
In the above preparation method, the vacuum degree is greater than or equal to 1E10-3Pa, preferably 8E10-4Pa. The high vacuum degree can reduce the defects of the film layer and increase the bonding force of the film layer.
In the preparation method, the heating temperature is 150-200 ℃, and preferably 170 ℃.
In the preparation method, the ion source is a Hall ion source, argon is used as working gas, the power is 200-800W, preferably 400W, and the bombardment lasts for 4-10 minutes, preferably 8 minutes.
In the preparation method, the coating material is put in a crucible and heated and evaporated by electron beams, or put in a heat-resistant metal boat such as a molybdenum boat, a tungsten boat and the like and electrified and evaporated by resistance heating.
In the preparation method, the thickness of the film layer is controlled by a quartz crystal oscillator on a film plating machine, and the precision can reach within 10 nm.
Has the advantages that:
compared with the prior art, the infrared stealth flexible film has the following advantages that:
(1) the substrate is a polyimide film and can be used in a flexible printed circuit board, and the traditional film coating substrate such as a silicon wafer, a germanium sheet or glass is compared with a hard substrate, is soft and can be curled;
(2) the coating can resist the high temperature of 300 ℃ and can be applied to the environment below 300 ℃, the coated film layer is baked on a germanium substrate for 30 minutes at the temperature of 400 ℃, and the spectral change is less than 0.5 percent;
(3) the infrared emissivity is extremely low, and the infrared stealth effect is good;
(4) firm film layer, simple preparation, boiling in water for 30 minutes, and no falling off of the film layer.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of a vacuum evaporation coating structure of a polyimide film according to the present invention;
FIG. 2 is emissivity data for the infrared stealth film of example 1;
FIG. 3 is example 2 Infrared stealth film emissivity data.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
A strip-shaped infrared stealth flexible film.
A polyimide film strip with the width of 3cm and the length of 40cm is radially fixed on an umbrella stand at the top of a vacuum coating machine, and a thickness control crystal oscillator is arranged in the center of the umbrella stand. The left side and the right side of the bottom of the film plating machine are respectively provided with a Ge coating material and a ZnS coating material, wherein the Ge coating material is arranged in a crucible and heated by an electron gun, and the ZnS coating material is arranged in a molybdenum boat and heated by a resistor. The middle of the lower part is provided with an ion source, the opening of the ion source faces to the top tooling umbrella stand, and the whole structure is shown in figure 1. The coating machine is characterized in that a coating tool umbrella stand is arranged in a coating machine box body, a heating wire is arranged on the upper portion of the coating tool umbrella stand, an ion source is arranged in the coating tool umbrella stand and below a crystal oscillator and the coating tool umbrella stand, a coating material is arranged on the side face of the ion source, and a baffle is arranged above the coating material.
The film layer structure is as in table 1.
Figure BDA0003362709770000041
The film coating temperature is 170 ℃, and the vacuum degree is pumped to 8E10-4After Pa, the ion source is started, the power is 400W, and the bombardment time is 8 minutes. After the bombardment is finished, the electron gun is started to heat the Ge material, and the baffle is opened to start film coating. And when the crystal oscillator detects that the thickness reaches a set value, closing the electron gun and closing the baffle. And electrifying the molybdenum boat to heat the ZnS material, and opening the baffle to start coating. The above process is repeated in sequence until the 16 layers of film are completely plated.
The reflectivity is measured to calculate the emissivity, and the average emissivity in the 8-14 μm wave band is less than 2%, as shown in fig. 2.
The coated polyimide film and the uncoated polyimide film were attached to hot plates at 100 ℃ as shown in FIG. 3. The temperature was measured with an infrared thermometer, and the data obtained at room temperature and 23 ℃ are shown in Table 2:
table 2: measurement shielding effect of flexible film on infrared thermometer
Figure BDA0003362709770000042
Figure BDA0003362709770000051
The polyimide film after coating can shield the actual temperature of 98.3 ℃ to 33.8 ℃, and the temperature difference between the polyimide film and room temperature of 23 ℃ is greatly reduced, so that the infrared stealth effect is realized.
Example 2
This example produced a large area rectangular infrared stealth flexible film.
A polyimide film with the width of 40cm and the length of 60cm is unfolded and is attached to an umbrella stand at the top of a vacuum coating machine, and the central crystal oscillator is not required to be shielded. The left and the right sides of the bottom of the film plating machine are respectively provided with a Ge coating material and a ZnSe coating material, wherein the Ge is arranged in a crucible and is heated by an electron gun, and the ZnSe adopts a cake-shaped material and is also arranged in the crucible and is heated by the electron gun. The middle of the lower part is provided with an ion source, and the opening faces to the top tooling umbrella stand.
The film layer structure is as in table 3.
Table 3: ultra-low emissivity film structure 2
Figure BDA0003362709770000052
The coating temperature is 200 ℃, and the vacuum degree is pumped to 1E10-3After Pa, the ion source was turned on at 600W for 4 minutes of bombardment time. After the bombardment is finished, the electron gun is started to heat the Ge material, and the baffle is opened to start film coating. And when the crystal oscillator detects that the thickness reaches a set value, closing the electron gun and closing the baffle. And opening the electron gun on the other side to heat the ZnSe material, and opening the baffle to start coating. The above processes are repeated in sequence until the film is completely plated.
The reflectivity is measured to calculate the emissivity, and the average emissivity in the wave band of 8-14 μm is less than 5%, as shown in FIG. 3
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The infrared stealth flexible film is characterized by comprising a flexible substrate and a film coating layer on the surface, wherein the film coating layer is formed by alternately preparing a high-refractive-index material and a low-refractive-index material, and the average reflectivity of the film coating layer in a wave band of 8-14 mu m is more than 95%.
2. The infrared stealth flexible film of claim 1, wherein the flexible substrate is a polyimide family high temperature resistant plastic film.
3. The infrared stealth flexible film of claim 1, wherein said high index material is: ge or Si; the low-refractive-index material is as follows: ZnS or ZnSe.
4. A method of making an infrared stealth flexible film as recited in claim 1, comprising the steps of:
s1, spreading and fixing the substrate on a film coating tool of a film coating machine;
s2, vacuumizing and heating;
s3, removing adsorbed molecules by ion bombardment, and cleaning the substrate;
and S4, heating the coating materials by electron beams or resistors, coating one layer to a set thickness, then coating the other layer, and alternately overlapping the layers one by one until all designed film layers are coated.
5. The method of claim 4, wherein the coating vacuum is greater than or equal to 1E10-3Pa。
6. The method for preparing the infrared stealth flexible film according to claim 4, wherein the coating temperature is 150 to 200 ℃.
7. The method of claim 4, wherein the thickness of the material is controlled by a change in crystal frequency.
8. The method as claimed in claim 4, wherein the source of ions is a Hall ion source, and the working gas is argon gas with a power of 200 and 800W.
9. A method of making an infrared stealth flexible film according to claim 4, wherein the thickness of each layer in S4 is generally between 20 nm and 3 μm.
CN202111372177.0A 2021-11-18 2021-11-18 Infrared stealth flexible film and preparation method thereof Pending CN114089448A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114805898A (en) * 2022-05-05 2022-07-29 合肥中隐新材料有限公司 Infrared self-adaptive flexible bending stealth material and preparation method thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103233198A (en) * 2013-04-22 2013-08-07 兰州空间技术物理研究所 Method for improving adhesive force of long-wave infrared optical film and germanium substrate
CN104991291A (en) * 2015-06-26 2015-10-21 中国人民解放军国防科学技术大学 Infrared stealth film capable of achieving low emissivity in band range from 8 microns to 14 microns selectively, and preparation method for infrared stealth film
CN105388542A (en) * 2015-12-02 2016-03-09 中国建筑材料科学研究总院 Ge-As-Se infrared glass with anti-reflection film and preparation method thereof
CN110737035A (en) * 2019-10-22 2020-01-31 中国人民解放军国防科技大学 stealth materials compatible with selective infrared radiation and radar wave absorption and preparation method thereof
CN111722307A (en) * 2020-08-21 2020-09-29 上海米蜂激光科技有限公司 Infrared antireflection film with aspheric chalcogenide glass as substrate and preparation method thereof
CN112030115A (en) * 2020-11-06 2020-12-04 上海米蜂激光科技有限公司 Radar wave transmitting flexible substrate infrared filter film and preparation method thereof
CN112346160A (en) * 2020-10-20 2021-02-09 中国人民解放军国防科技大学 Nonmetal visible light laser infrared multiband compatible stealth film and preparation method thereof
CN112666637A (en) * 2020-12-29 2021-04-16 浙江大学 Lambert surface-based flexible thermal infrared stealth device and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103233198A (en) * 2013-04-22 2013-08-07 兰州空间技术物理研究所 Method for improving adhesive force of long-wave infrared optical film and germanium substrate
CN104991291A (en) * 2015-06-26 2015-10-21 中国人民解放军国防科学技术大学 Infrared stealth film capable of achieving low emissivity in band range from 8 microns to 14 microns selectively, and preparation method for infrared stealth film
CN105388542A (en) * 2015-12-02 2016-03-09 中国建筑材料科学研究总院 Ge-As-Se infrared glass with anti-reflection film and preparation method thereof
CN110737035A (en) * 2019-10-22 2020-01-31 中国人民解放军国防科技大学 stealth materials compatible with selective infrared radiation and radar wave absorption and preparation method thereof
CN111722307A (en) * 2020-08-21 2020-09-29 上海米蜂激光科技有限公司 Infrared antireflection film with aspheric chalcogenide glass as substrate and preparation method thereof
CN112346160A (en) * 2020-10-20 2021-02-09 中国人民解放军国防科技大学 Nonmetal visible light laser infrared multiband compatible stealth film and preparation method thereof
CN112030115A (en) * 2020-11-06 2020-12-04 上海米蜂激光科技有限公司 Radar wave transmitting flexible substrate infrared filter film and preparation method thereof
CN112666637A (en) * 2020-12-29 2021-04-16 浙江大学 Lambert surface-based flexible thermal infrared stealth device and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114805898A (en) * 2022-05-05 2022-07-29 合肥中隐新材料有限公司 Infrared self-adaptive flexible bending stealth material and preparation method thereof

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