CN113737134A - Thin film containing nested micro-trap structure and preparation method thereof - Google Patents

Thin film containing nested micro-trap structure and preparation method thereof Download PDF

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Publication number
CN113737134A
CN113737134A CN202111028756.3A CN202111028756A CN113737134A CN 113737134 A CN113737134 A CN 113737134A CN 202111028756 A CN202111028756 A CN 202111028756A CN 113737134 A CN113737134 A CN 113737134A
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China
Prior art keywords
layer material
film
material film
lower layer
substrate
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CN202111028756.3A
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Chinese (zh)
Inventor
胡忠强
赵亚楠
朱媛媛
刘明
何鋆
胡天存
张毅
崔万照
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Xian Jiaotong University
Xian Institute of Space Radio Technology
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Xian Jiaotong University
Xian Institute of Space Radio Technology
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Priority to CN202111028756.3A priority Critical patent/CN113737134A/en
Publication of CN113737134A publication Critical patent/CN113737134A/en
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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
    • C23C14/0605—Carbon
    • 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

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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)
  • Cold Cathode And The Manufacture (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

A film containing a nested micro-trap structure and a preparation method thereof comprise a lower layer material film, an upper layer material film and a substrate; the lower layer material film is arranged on the substrate, and the upper layer material film is arranged on the lower layer material film; the atom gaps of the lower layer material film are smaller than the atom gaps of the upper layer material film, and the atom gaps of the lower layer material film are embedded into the atom gaps of the upper layer material film to form a nested micro-trap structure. The invention utilizes magnetron sputtering technology to grow a film with a nested micro-trap structure, and then forms an upper layer film and a lower layer film with different densities by controlling sputtering power, wherein the lower layer film has small sputtering power, large material density, small atom spacing and small gaps among atoms; the upper layer of film has large sputtering power, small material density and large atom distance, large gaps exist among atoms, and the large gaps and the small gaps of the upper layer and the lower layer form a nested micro-trap structure.

Description

Thin film containing nested micro-trap structure and preparation method thereof
Technical Field
The invention belongs to the technical field of secondary electron emission inhibition, and particularly relates to a thin film containing a nested micro-trap structure and a preparation method thereof.
Background
The effective load of the spacecraft in China urgently needs to be developed towards integration and high power, however, in a severe space environment, special effects in the space are aggravated. The micro-discharge effect of the space high-power microwave component is the first problem. The space micro-discharge effect is also called secondary electron multiplication effect, and refers to a resonance discharge phenomenon generated when a high-power microwave component transmits a high-power microwave signal under the air pressure of 1 multiplied by 10 < -3 > Pa or lower. The microdischarge effect is a very important factor influencing the reliability of aerospace electronic equipment, and because the space electronic equipment is updated and developed at high speed, how to effectively inhibit secondary electron multiplication becomes a bottleneck problem restricting the development of space communication technology. The secondary electron multiplication effect can cause the standing-wave ratio of the microwave transmission system to be gradually increased, the reflected power to be increased and the noise level to be raised, so that the high-power microwave system can not normally work; the microdischarge also causes fluctuations in the intra-cavity tuning, parametric coupling, waveguide loss, phase constants, etc., generates harmonics that cause out-of-band interference and passive intermodulation products, and erodes the component surface, etc.
At present, most of suppression methods for Secondary Electron emission reduce SEY (Secondary Electron Yield) by changing surface topography, thereby realizing suppression of micro-discharge effect. In recent years, the european space agency has continuously conducted intensive and systematic research on surface topography control techniques through a plurality of projects, and the main research contents are various surface treatment techniques capable of effectively suppressing the secondary electron multiplication effect, including anti-electron multiplication coating, chemical etching, trench structure construction, and the like. However, the single way of changing the surface morphology of the material has a non-negligible effect on the performance of the material itself, and although playing a role in suppressing secondary electrons, the single way of changing the surface morphology of the material has an effect on the performance of the device in other respects.
Disclosure of Invention
The invention aims to provide a thin film containing a nested micro-trap structure and a preparation method thereof, so as to solve the problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a film containing a nested micro-trap structure comprises a lower layer material film, an upper layer material film and a substrate; the lower layer material film is arranged on the substrate, and the upper layer material film is arranged on the lower layer material film; the atom gaps of the lower layer material film are smaller than the atom gaps of the upper layer material film, and the atom gaps of the lower layer material film are embedded into the atom gaps of the upper layer material film to form a nested micro-trap structure.
Further, the lower layer material film and the upper layer material film are as follows: C. ag or Pb, and the upper and lower layers of film materials are in a nested structure in the growth process.
Further, the substrate is a silver-plated substrate made of Si, Al, Ag, Cu, Au, Fe, Co, Ni or aluminum alloy.
Further, a method for preparing a thin film containing a nested micro-trap structure comprises the following steps:
step 1: cleaning the substrate;
step 2: fixing the cleaned substrate on a magnetron sputtering tray, feeding the substrate into a magnetron sputtering cavity, and vacuumizing to 5 x 10-4Pa below;
and step 3: growing a lower layer material film under the argon atmosphere;
and 4, step 4: after the lower layer material film is grown, the upper layer material film is continuously grown.
Further, substrate cleaning: the substrate is surface cleaned with isopropanol and deionized water, and N is used2And (5) drying.
Further, the substrate is fixed by Kapton tape.
Further, in step 3, argon gas is introduced into the chamber, the pressure of the argon gas is 1Pa, the flow of the argon gas is 25sccm, and the lower material film is grown with a power of 10W for 20 s.
Further, in step 4, the power is increased to 60W, and the upper layer material film is grown continuously with the power of 60W for 20 s.
Compared with the prior art, the invention has the following technical effects:
the invention utilizes the magnetron sputtering technology to grow the film with the nested micro-trap structure, realizes that the upper layer and the lower layer of films with different densities are formed by controlling the sputtering power in a film coating mode on the premise of not changing the self structure of the material and influencing the self performance of the material, the lower layer of film has small sputtering power, large material density, small atom distance and small gaps among atoms; the upper layer of film has large sputtering power, small material density and large atom distance, large gaps exist among atoms, and the large gaps and the small gaps of the upper layer and the lower layer form a nested micro-trap structure. The surface appearance and the performance of the material of the device are not influenced, and the advantage of high secondary electron inhibition rate of the traditional changed surface appearance can be used.
The invention utilizes the control of the film coating power to manufacture two layers of films with different densities, and combines the film coating method with the surface topography method. Because the densities of the two layers of materials are different, the distances between atoms are also different, the upper layer of material is a material with large atomic distance, relatively large gaps are formed between atoms, the lower layer of material is a material with small atomic distance, small gaps are formed between atoms, and the large gaps and the small gaps form a nested micro-trap structure, so secondary electrons on the surface of the escaping material are subjected to general energy consumption similar to diffuse reflection in the small gaps, and the inhibiting effect is achieved when the energy is smaller than the surface work function of the coating material; the electrons with larger energy can be ejected out of the small gap and enter the large gap after being consumed in the small gap, and a new round of energy consumption is carried out. In the nested micro-trap structure consisting of the small gaps and the large gaps, after most of electron energy is consumed by two rounds, the energy is reduced to be lower than the surface work function of the coating material, and the purpose of greatly reducing the secondary electron emission coefficient is achieved.
Drawings
Fig. 1 is a front view of the macrostructures of this structure. A
FIG. 2 is a front view of the microstructure at the interface of the upper and lower material films.
FIG. 3 is a schematic diagram of a nested micro-trap structure consisting of large and small voids at the interface of an upper material film and a lower material film.
FIG. 4 is a top view of a schematic diagram of a nested micro-trap structure consisting of large and small voids at the interface of an upper and lower material films.
Fig. 5 shows the energy consumption process of the secondary electrons escaping from the surface of the material in the trap structure.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
referring to fig. 1 to 5, a thin film with nested micro-trap structures and a method for fabricating the same are disclosed, wherein the thin film with nested micro-trap structures is fabricated by magnetron sputtering.
The method comprises the following steps:
step 1: cleaning, surface cleaning a substrate with isopropyl alcohol and deionized water, and cleaning with N2And (5) drying.
Step 2: placing the substrate on a magnetron sputtering tray by using Kapton tape, feeding into a chamber, and vacuumizing to 5 × 10-4Pa or less.
And step 3: and introducing argon into the chamber, wherein the pressure of the argon is 1Pa, the flow of the argon is 25sccm, and growing the lower-layer material film by using the power of 10W for 20 s.
And 4, step 4: after the lower layer material film is grown, the power is increased to 60W, the upper layer material film is grown continuously with the power of 60W, and the growth lasts for 20 s.
Further, the substrate in the above step may be: si, Al, Ag, Cu, Au, Fe, Co, Ni and the like.
Further, the upper layer material and the lower layer material in the above steps may be: c, Ag, Pb and other materials with low secondary electron emission coefficients.
Implementation example:
in order to obtain a high-quality secondary electron suppression film with a nested micro-trap structure, a C material is selected as a lower layer material film, an Ag material is selected as an upper layer material film, the two materials are selected because the atomic radius of C is smaller, the covalent radius is smaller when the film is formed, the atomic radius of Ag atoms is larger relative to C atoms, the covalent radius is larger when the film is formed, thus the lower layer material film with smaller atomic gaps and the upper layer material film with larger atomic gaps are easier to prepare during film coating, and the formed nested micro-trap structure has higher quality. The substrate is made of aluminum alloy silver-plated material commonly used for space microwave material.
A preparation method of a thin film containing a nested micro-trap structure specifically comprises the following steps:
step 1: cleaning, namely performing ultrasonic surface cleaning on an aluminum alloy silver-plated substrate by using isopropanol and deionized water, and then using N2And (5) drying.
Step 2: clamping the cleaned substrate with tweezers, placing the substrate on a magnetron sputtering tray with Kapton tape, transferring into a chamber, and vacuumizing to 5 × 10-4Pa or less.
And step 3: and introducing argon into the chamber, wherein the pressure of the argon is 1Pa, the flow of the argon is 25sccm, and growing C with the power of 10W to be used as a lower layer material film for 20 s.
And 4, step 4: after the lower layer material film is grown, the power is increased to 60W, Ag continues to grow with the power of 60W, and the Ag is used as the upper layer material film to grow for 20 s.
Two layers of films with different densities are manufactured by controlling the film coating power, and the film coating method and the surface topography method are combined. Because the densities of the two layers of materials are different, the distances between atoms are also different, the upper layer of material is a material with large atomic distance, relatively large gaps are formed between atoms, the lower layer of material is a material with small atomic distance, small gaps are formed between atoms, and the large gaps and the small gaps form a nested micro-trap structure, so secondary electrons on the surface of the escaping material are subjected to general energy consumption similar to diffuse reflection in the small gaps, and the inhibiting effect is achieved when the energy is smaller than the surface work function of the coating material; the electrons with larger energy can be ejected out of the small gap and enter the large gap after being consumed in the small gap, and a new round of energy consumption is carried out. In the nested micro-trap structure consisting of the small gaps and the large gaps, after most of electron energy is consumed by two rounds, the energy is reduced to be lower than the surface work function of the coating material, and the purpose of greatly reducing the secondary electron emission coefficient is achieved.

Claims (8)

1. A film containing a nested micro-trap structure is characterized by comprising a lower layer material film, an upper layer material film and a substrate; the lower layer material film is arranged on the substrate, and the upper layer material film is arranged on the lower layer material film; the atom gaps of the lower layer material film are smaller than the atom gaps of the upper layer material film, and the atom gaps of the lower layer material film are embedded into the atom gaps of the upper layer material film to form a nested micro-trap structure.
2. The membrane with nested micro-trap structures of claim 1, wherein the lower layer material membrane and the upper layer material membrane are: C. ag or Pb, and the upper and lower layers of film materials are in a nested structure in the growth process.
3. The membrane containing nested micro-trap structures of claim 1, wherein the substrate is a silver-plated substrate of Si, Al, Ag, Cu, Au, Fe, Co, Ni or aluminum alloy.
4. A method for preparing a thin film containing a nested micro-trap structure, which is based on the thin film containing the nested micro-trap structure of any one of claims 1 to 3, and comprises the following steps:
step 1: cleaning the substrate;
step 2: fixing the cleaned substrate on a magnetron sputtering tray, feeding the substrate into a magnetron sputtering cavity, and vacuumizing to 5 x 10- 4Pa below;
and step 3: growing a lower layer material film under the argon atmosphere;
and 4, step 4: after the lower layer material film is grown, the upper layer material film is continuously grown.
5. The method of claim 4, wherein the substrate is cleaned by: the substrate is surface cleaned with isopropanol and deionized water, and N is used2And (5) drying.
6. A method according to claim 4, wherein the substrate is fixed by Kapton tape.
7. The method for preparing a thin film containing a nested micro-trap structure according to claim 4, wherein in step 3, argon gas is introduced into the chamber, the pressure of the argon gas is 1Pa, the flow of the argon gas is 25sccm, and the power of 10W is used for growing the thin film of the lower layer material for 20 s.
8. The method for preparing a thin film containing a nested micro-trap structure according to claim 4, wherein in the step 4, the power is increased to 60W, and the upper layer material thin film is grown for 20s by using the power of 60W.
CN202111028756.3A 2021-09-02 2021-09-02 Thin film containing nested micro-trap structure and preparation method thereof Pending CN113737134A (en)

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Application publication date: 20211203