CN110994189B - Heterogeneous material structured multilayer thin film wave absorber and manufacturing method thereof - Google Patents

Heterogeneous material structured multilayer thin film wave absorber and manufacturing method thereof Download PDF

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CN110994189B
CN110994189B CN201911345072.9A CN201911345072A CN110994189B CN 110994189 B CN110994189 B CN 110994189B CN 201911345072 A CN201911345072 A CN 201911345072A CN 110994189 B CN110994189 B CN 110994189B
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heterogeneous material
thickness
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CN110994189A (en
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刘卫国
葛少博
周顺
杨鹏飞
李世杰
阳志强
黄岳田
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Xian Technological University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
    • H01Q17/008—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems with a particular shape
    • 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
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a heterogeneous material structured multilayer film wave absorber and a manufacturing method thereof2Film and SiN x The films are sequentially laminated from bottom to top; the structured multilayer film is integrally a micro pyramid structure array. During preparation, the micro pyramid structure is directly formed in the heterogeneous material multilayer film by adopting a single-point diamond turning technology. The heterogeneous material structured multilayer film wave absorber provided by the invention has obvious wave absorbing characteristics on visible light waves and infrared wave waves, can realize the absorption of electromagnetic wave energy, has low preparation cost and high efficiency, and has important practical value in the photovoltaic and stealth fields.

Description

Heterogeneous material structured multilayer thin film wave absorber and manufacturing method thereof
Technical Field
The invention relates to the field of electromagnetic wave absorption, in particular to a heterogeneous material structured multilayer film wave absorber and a preparation method thereof.
Background
The wave-absorbing material is a material capable of effectively absorbing and losing electromagnetic wave energy irradiated on the surface of the wave-absorbing material. It is an important functional material. The wave-absorbing materials can be divided into coating type and structural type. The coating type wave-absorbing material is generally prepared by mixing absorbent such as powder and fiber with wave-absorbing performance with binder, curing agent and the like according to a certain proportion, and the coating type wave-absorbing material is used in stealth fighters such as F-117A, B-2, F-22 and the like at places with strong scattering sources of the fighter body. Compared with a coating type wave-absorbing material, the structural wave-absorbing material has the greatest advantage that the structural wave-absorbing material can be used as structural functional parts such as front edges and ventral fins of aircrafts while effectively absorbing incident waves, can be reasonably designed according to use scenes and mainly comprises a traditional structural type and a metamaterial type.
Common traditional structural wave-absorbing materials mainly comprise: jaumann absorber, geometric gradient absorber, etc. Although the preparation process is simple, the structure thickness is generally larger: each layer structure of the Jaumann absorber needs to satisfy d = lambda0/4（λ0A center operating wavelength); the thickness of the geometric gradient wave absorber is generally more than 400mm, even 600-750 mm, and the good absorption efficiency brings sharp increase of the structural thickness. The metamaterial wave-absorbing structure provides an ideal solution for miniaturization and integration of wave-absorbing devices. The electromagnetic response of the metamaterial is not only determined by the material of the metamaterial, but also related to the microstructure and arrangement mode of the resonant units. A perfect wave absorber (PMA) designed based on a metamaterial can realize nearly 100% absorption of electromagnetic waves with specific wavelengths by reasonably changing the microstructure parameters and arrangement mode of the resonant units. Most of the currently reported metamaterial wave absorbers are in the stage of theoretical calculation, and large-caliber preparation is difficult to realize.
Disclosure of Invention
The invention provides a polarization-insensitive heterogeneous material structured multilayer film wave absorber and a preparation method thereof, and aims to solve the problems that the wave absorber based on a traditional structural material is large in size and weight, and meanwhile, the wave absorber based on a metamaterial is narrow in bandwidth, high in manufacturing cost, low in efficiency and difficult to apply.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a heterogeneous material structured multi-layer film wave absorber comprises siliconThe silicon substrate is provided with 1-N multi-film-layer units on the top, and each multi-film-layer unit comprises an Ag thin film and an SiO thin film which are sequentially stacked from bottom to top2Film and SiN x And 1-N multi-film layer units of the film are integrally in a pyramid array structure.
Furthermore, the size of the silicon substrate is 4 microns, the overall height of the pyramid array structure is larger than 1 micron, the thickness of an Ag film in each multi-film-layer unit is 30-200 nm, and the thickness of an SiO film in each multi-film-layer unit is larger than that of the Ag film in each multi-film-layer unit2Film thickness of 200-800 nm, SiN x The thickness of the film is 200-800 nm; the thickness of the Ag film on the surface of the silicon substrate is not less than 120 nm.
A preparation method of a heterogeneous material structured multilayer thin film wave absorber comprises the following steps:
1) deposition of multilayer thin films
The preparation of the metal film layer on the silicon substrate is realized by adopting a magnetron sputtering deposition method, and the preparation of the dielectric film layer with low refractive index and the dielectric film layer with high refractive index is realized by adopting a plasma enhanced chemical deposition method;
2) single point diamond direct cutting shaping
And directly cutting the surface of the heterogeneous material multilayer film by adopting a single-point diamond cutting technology to realize the molding of the structural multilayer film wave absorber with the micro pyramid structure array.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention combines a structural wave absorber with a metamaterial wave absorber and provides a heterogeneous material structured multilayer film wave absorber insensitive to polarization. The whole structured optical film has pyramid-shaped textured surface appearance and has the characteristic of indistinct polarization. The structure is internally formed by superposing a metal film layer and a dielectric film layer with high and low refractive indexes, and the broadening of wave-absorbing wave bands can be realized by adjusting the thickness of the film layer.
2. The vibration-insensitive heterogeneous material structured multilayer film wave absorber provided by the invention integrates the heterogeneous material multilayer film in the three-dimensional pyramid structure, the characteristic dimension is micron order, the volume and the weight of the wave absorber are effectively reduced, and the planarization and the integration of a system are facilitated.
3. The manufacturing method of the polarization-insensitive heterogeneous material structured multilayer film wave absorber can effectively overcome the defects of low manufacturing efficiency and high processing cost of the conventional metamaterial wave absorber, can directly form a pyramid structure in the heterogeneous material multilayer film by adopting a single-point diamond cutting technology, has low manufacturing process cost and high manufacturing efficiency, has the cutting precision in the submicron order, can effectively realize the miniaturization, the light weight and the integration of a system, and can realize the mass production of large-caliber wave absorbers.
Drawings
FIG. 1 is a schematic design diagram of a heterogeneous material structured six-layer thin film wave absorber;
FIG. 2 is an effect graph of wave-absorbing characteristics (583 nm) of a heterogeneous material structured six-layer film;
FIG. 3 is a wave-absorbing characteristic (680 nm) effect diagram of a heterogeneous material structured six-layer film;
FIG. 4 is a schematic design diagram of a heterogeneous material structured nine-layer thin film wave absorber;
FIG. 5 is a wave-absorbing characteristic (5.5 μm) effect diagram of a heterogeneous material structured nine-layer film;
FIG. 6 is a wave-absorbing characteristic (13 μm) effect diagram of a heterogeneous material structured nine-layer film.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
the first embodiment is as follows:
as shown in fig. 1, the present invention provides a heterogeneous material structured multilayer thin film absorber, which is a six-layer thin film absorber and includes a silicon substrate, wherein 2 multi-film units, i.e., a metal-low refractive index layer-high refractive index layer (M-L-H), are disposed on the top of the silicon substrate, and each multi-film unit includes an Ag thin film and an SiO thin film sequentially stacked from bottom to top2Film and SiN x And the film and the 2 multi-film-layer units are integrally in a pyramid array structure. Wherein the size of the silicon substrate is 4 Mum multiplied by 4 Mum, 2 pyramid arrays integrally formed by multi-film layer unitsThe structure height was 2 μm. The film thickness of each multi-film unit is set as follows: as shown in FIG. 1, the thickness of the Ag film in the film layer unit is 40nm, and the SiO film2Film thickness 490nm, SiN x The thickness of the film was 490 nm. Because the thickness of the Ag film on the surface of the substrate is not less than 120nm, the Ag film with the thickness of 80nm can be deposited on the surface of the substrate in advance, and 2 multi-film-layer units are prepared on the deposited Ag film layer.
The preparation method of the six-layer film wave absorber comprises the following steps:
1. and depositing a metal film on the surface of the silicon substrate by adopting a magnetron sputtering technology, and controlling the deposition time to obtain the Ag film layer with the thickness of 120nm on the surface of the silicon substrate.
2. Depositing high and low refractive index dielectric film by adopting a plasma enhanced chemical vapor deposition method, and regulating and controlling reaction gas and deposition time to obtain SiO2Film thickness 490nm, SiN x The thickness of the film was 490nm,
then adopting magnetron sputtering technology to form SiN x Depositing a metal film on the surface of the film to obtain an Ag film layer with the thickness of 40nm, and preparing SiO with the thickness of 490nm on the Ag film layer2Film and SiN 490nm in thickness x Film, total 6 films.
3. And the direct cutting molding of the heterogeneous material structured multilayer film wave absorber is realized by adopting a single-point diamond cutting technology. The heterogeneous material multilayer film sample is fixed on the workbench, the single-point diamond sharp knife is assembled on the fly-cutting disc and rotates around the spindle rapidly, and accurate control of the size of the pyramid array structure formed by the 2 multi-film unit bodies in a whole can be realized by adjusting the cutting depth, the feeding speed and the rotating speed of the fly-cutting disc of the single-point diamond. After fly-cutting in one direction is completed, the sample is rotated 90 ° clockwise, and fly-cutting preparation in the other direction is completed using the same fly-cutting parameters.
And (4) finishing the preparation of the heterogeneous material structured six-layer thin film wave absorber by flying cutting twice.
Heterogeneous material structured six-layer film wave-absorbing materialThe wave absorbing effect of the device is shown in fig. 2 and fig. 3, wherein the X axis marks the bottom width of the structured multilayer film, the Y axis is the z direction of the space where the microstructure is located, and light waves vertically enter from top to bottom. As shown in FIG. 2, light with a wavelength of 583nm enters the six-layer structured thin film absorber at normal incidence and is confined to SiN with a high refractive index x Layer and a typical interference fringe distribution appears. The heterogeneous material structured six-layer film wave absorber can realize the wave absorbing effect on a plurality of wave bands through a single structure, as shown in figure 3, the wave with the wavelength of 680nm is vertically incident and is limited on the surface of a metal film layer.
Example two:
in the same way as in example 1, each wave-absorbing structure of metal-low refractive index layer-high refractive index layer (M-L-H) is designed as a multi-film-layer unit, in this example, 3 multi-film-layer units are disposed on the top of the silicon substrate, and the 3 multi-film-layer units are of a pyramid array structure as a whole. The silicon substrate size is 4 mu m multiplied by 4 mu m, and the pyramid array structure integrally formed by 3 multi-film layer units has the height of 1.8 mu m. The film thickness of each film unit is set as follows: the thickness of the Ag film layer is 200nm, and the SiO film layer2The thickness of the film was 200nm, SiN x The thickness of the film was 200nm as shown in FIG. 4.
The preparation method of the nine-layer film wave absorber comprises the following steps:
1. and depositing a metal film on the surface of the silicon substrate by adopting a magnetron sputtering technology, and controlling the deposition time to obtain the Ag film layer with the thickness of 200 nm.
2. Depositing a high-low refractive index dielectric film layer by adopting a plasma enhanced chemical vapor deposition method, and regulating and controlling reaction gas and deposition time to obtain SiO2The thickness of the film was 200nm, SiN x The thickness of the film was 200 nm.
The above operation is repeated twice, and the total of 3 film layer units is 9 heterogeneous material films.
3. And the direct cutting molding of the heterogeneous material structured multilayer film wave absorber is realized by adopting a single-point diamond cutting technology. By adjusting the cutting depth, the feeding speed and the rotating speed of the fly-cutting tool disk of the single-point diamond, the accurate control of the size of the micro pyramid structure unit can be realized. After fly-cutting in one direction is completed, the sample is rotated 90 ° clockwise, and fly-cutting preparation in the other direction is completed using the same fly-cutting parameters. And (4) finishing the preparation of the heterogeneous material structured nine-layer thin film wave absorber by flying cutting twice.
The wave absorbing effect of the heterogeneous material structured nine-layer film wave absorber is shown in fig. 5 and 6, wherein the bottom width of the structured multilayer film is marked on the X axis, the Y axis is the z direction of the space where the microstructure is located, and light waves vertically enter from top to bottom. Light waves with the wavelengths of 5.5 μm and 13 μm enter the structured multilayer thin film absorber at normal incidence, are confined inside the structured nine-layer thin film and are gradually absorbed. By adjusting the film layer, the heterogeneous material structured multilayer film wave absorber provided by the invention can realize broadening of wave absorbing wave bands, and the wave absorbing property is popularized to infrared wave bands.

Claims (2)

1. The utility model provides a heterogeneous material structurization multilayer film wave absorber which characterized in that, includes the silicon substrate, and the top of silicon substrate is provided with 1~ N many membranous layer units, and every many membranous layer unit includes from up stacking gradually Ag film, SiO down2Film and SiN x The film, 1-N multi-film layer units are integrally in a pyramid array structure;
the size of the silicon substrate is 4 microns multiplied by 4 microns, the overall height of the pyramid array structure is 1.8-2.0 microns, the thickness of an Ag thin film in each multi-film layer unit is 30-200 nm, and SiO is coated on the Ag thin film2Film thickness of 200-800 nm, SiN x The thickness of the film is 200-800 nm; the thickness of the Ag film on the surface of the silicon substrate is not less than 120nm, and when the thickness of the Ag film in the multi-film-layer unit does not reach 120nm, a layer of Ag film can be deposited on the surface of the silicon substrate to ensure that the thickness of the deposited Ag film is not less than 120nm when the deposited Ag film and the Ag film in the multi-film-layer unit are overlapped together.
2. The method for manufacturing a heterogeneous material structured multilayer thin film absorber according to claim 1, comprising the steps of:
1) deposition of multilayer thin films
Preparing Ag film layer on silicon substrate by magnetron sputtering deposition method, and preparing SiO film layer on Ag film layer surface by plasma enhanced chemical deposition method2Film layer and SiN x Preparing a film layer; repeating the above operation to alternately deposit Ag film and SiO 2 Film and SiN x Film, finish the deposition of the multilayer film;
2) single point diamond direct cutting shaping
Directly cutting the surface of the heterogeneous material multilayer film by adopting a single-point diamond cutting technology to realize the molding of the structural multilayer film wave absorber with the micro pyramid structure array;
the heterogeneous material multilayer film sample is fixed on a workbench, the single-point diamond sharp knife is assembled on the fly-cutting disc, and the precise control of the size of the micro pyramid structure array can be realized by adjusting the cutting depth, the feeding speed and the rotating speed of the fly-cutting disc of the single-point diamond;
after the fly-cutting in one direction is finished, rotating the sample clockwise by 90 degrees, and finishing the fly-cutting preparation in the other direction by adopting the same fly-cutting parameters;
and (4) finishing the preparation of the heterogeneous material structured multilayer film wave absorber by flying cutting twice.
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CN203132188U (en) * 2012-11-30 2013-08-14 中国科学院上海技术物理研究所 Color-adjustable solar energy selective absorption film system
CN104779447A (en) * 2015-04-08 2015-07-15 哈尔滨工业大学深圳研究生院 Structure of broadband wave absorber and preparation method
CN108515743B (en) * 2018-05-09 2020-07-28 同济大学 Metal/medium ultra-wideband absorption film and preparation method thereof

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CN102811595A (en) * 2012-07-31 2012-12-05 深圳光启创新技术有限公司 Broadband wave-absorbing material
CN110148637A (en) * 2019-06-02 2019-08-20 苏州腾晖光伏技术有限公司 A kind of solar battery antireflective membrane structure

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