CN116770267A - Film for inhibiting micro-discharge effect of satellite-borne microwave component and deposition process - Google Patents
Film for inhibiting micro-discharge effect of satellite-borne microwave component and deposition process Download PDFInfo
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- 230000000694 effects Effects 0.000 title claims abstract description 36
- 230000002401 inhibitory effect Effects 0.000 title claims abstract description 18
- 238000005137 deposition process Methods 0.000 title claims abstract description 13
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 41
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 15
- 239000010408 film Substances 0.000 claims description 106
- 238000006243 chemical reaction Methods 0.000 claims description 61
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 239000002243 precursor Substances 0.000 claims description 27
- 239000012159 carrier gas Substances 0.000 claims description 24
- HJUGFYREWKUQJT-UHFFFAOYSA-N tetrabromomethane Chemical compound BrC(Br)(Br)Br HJUGFYREWKUQJT-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010926 purge Methods 0.000 claims description 14
- 238000000427 thin-film deposition Methods 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 12
- 230000009471 action Effects 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000007736 thin film deposition technique Methods 0.000 claims description 5
- 230000005764 inhibitory process Effects 0.000 abstract description 7
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 238000010301 surface-oxidation reaction Methods 0.000 abstract description 2
- 238000007747 plating Methods 0.000 description 16
- 230000008021 deposition Effects 0.000 description 13
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- 229910052709 silver Inorganic materials 0.000 description 12
- 239000004332 silver Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000001629 suppression Effects 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
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- 238000000643 oven drying Methods 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
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Classifications
-
- 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
- C23C16/44—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 method of coating
- C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/26—Deposition of carbon only
-
- 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
Abstract
The invention provides a film for inhibiting micro-discharge effect of a satellite-borne microwave component and a deposition process, comprising the steps of preparing a titanium nitride film and an amorphous carbon film with target thickness on the surface of the satellite-borne microwave component in an atomic layer deposition mode, wherein the target thickness of the titanium nitride film is 15-20 nm; the target thickness of the amorphous carbon film is 5-8 nm. The titanium nitride film and the amorphous carbon film are sequentially deposited on the surface of the spaceborne microwave component, so that the inhibition of the micro discharge effect on the surface of the microwave component can be realized, and the microwave component has strong film base binding force, good surface oxidation resistance, complex microwave component surface shape retention and excellent electrical characteristics.
Description
Technical Field
The invention belongs to the technical field of space microwaves, and particularly relates to a film for inhibiting micro-discharge effect of a satellite-borne microwave component and a deposition process.
Background
The micro-discharge phenomenon refers to multiplication breakdown effect caused by exciting secondary electrons on the solid surface by free electrons under the action of a radio frequency field in a vacuum environment. In recent years, along with the stronger requirements of ultra-high-speed data transmission and ultra-large communication capacity in China on communication in higher frequency bands, the problem of micro-discharge of high-frequency high-power microwave components caused by miniaturization of microwave passive devices in the aerospace field is also more serious, the micro-discharge threshold is improved, and a new technology for inhibiting the micro-discharge effect is not yet found.
In a space payload system, microdischarge occurs primarily on both surfaces of a metallic resonant structure, and its necessary conditions for microdischarge include: the electron mean free path must be greater than the gap distance and the electron mean transit time an odd multiple of the half period of the radio frequency electric field. In addition, a secondary electron emission coefficient (Secondary Electron Yield, SEY) greater than 1 on the surface of the material is one of the fundamental reasons for inducing the micro-discharge effect. At present, there are two main trends in research on the micro-discharge suppression technology of the material surface, namely, surface roughening treatment, namely, forming a deeper hole array on the surface of a component, and manufacturing a trap to suppress the emission of secondary electrons so as to suppress the micro-discharge effect. However, the introduction of the "trap" structure may cause degradation of surface properties, especially electrical properties of the high frequency device, and increase of insertion loss, which affects normal operation of the device. The other is surface coating treatment, namely, directly carrying out low SEY material film plating on the surface of the base material, thereby inhibiting the micro-discharge effect and simultaneously effectively avoiding the deterioration of the electrical property of the surface of the component.
In the prior engineering application, the method for inhibiting the micro-discharge effect of the high-power microwave component coated with the low-SEY material film coating often has problems, such as: the coating film and the microwave component have weak adhesion and are easy to fall off or oxidize. These problems often make the micro-discharge effect suppression method of the thin film coating of the material coated with low SEY an obstacle in terms of model popularization and engineering application.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor performs intensive research, provides a film for inhibiting the micro-discharge effect of a satellite-borne microwave component based on an atomic layer deposition titanium nitride/amorphous carbon composite film and a deposition process thereof, solves the problems of weak adhesion between the film and the microwave component, easy falling or easy oxidation, and has the advantages of low SEY (styrene-ethylene-vinyl acetate copolymer), difficult oxidation of the surface, high diffractibility, strong binding force, good conductivity and the like in engineering application, thereby having great engineering application value and market prospect.
The technical scheme provided by the invention is as follows:
in a first aspect, a thin film deposition process for suppressing micro-discharge effects of a microwave component on board a satellite, comprising: and preparing a titanium nitride film and an amorphous carbon film with target thicknesses on the surface of the space-borne microwave component in an atomic layer deposition mode.
In a second aspect, a film for inhibiting micro-discharge effect of a satellite-borne microwave component comprises a titanium nitride film and an amorphous carbon film which are sequentially deposited on the surface of the satellite-borne microwave component, wherein the thickness of the titanium nitride film is 15-20 nm; the amorphous carbon film has a thickness of 5 to 8nm.
According to the film and the deposition process for inhibiting the micro-discharge effect of the satellite-borne microwave component, provided by the invention, the film and the deposition process have the following beneficial effects:
(1) According to the film and the deposition process for inhibiting the micro-discharge effect of the spaceborne microwave component, the titanium nitride film and the amorphous carbon film are sequentially deposited on the surface of the spaceborne microwave component, so that the problems that the titanium nitride film is easy to oxidize after being placed for a long time and the amorphous carbon film has poor bonding force on the surface of a substrate can be effectively solved, the inhibition of the micro-discharge effect on the surface of the microwave component can be realized, and the film has strong film base bonding force, good surface oxidation resistance, complex microwave component surface shape retention and excellent electrical characteristics;
(2) The invention provides a film for inhibiting micro-discharge effect of a satellite-borne microwave component and a deposition process, wherein the thickness of a titanium nitride film is 15-20 nm; the amorphous carbon film has the thickness of 5-8 nm, can realize the micro discharge inhibition of microwave components, can improve the micro discharge threshold by more than 3dB compared with the original aluminum alloy silver plating surface, can realize high-diffraction and high-uniformity film plating in components such as a cavity filter and the like no matter the components are flat, curved or high-depth-ratio surfaces with complex structures, has excellent electrical characteristics, and especially for high-frequency microwave components, the smaller the film thickness is, the more outstanding the advantages of the electrical characteristics after film plating are.
Drawings
FIG. 1 is a flow chart of a thin film deposition process for inhibiting micro-discharge effect of a satellite-borne microwave component;
FIG. 2 is a SEY curve of a silver-plated surface deposited with a 20nm titanium nitride film before and after long-term placement;
FIG. 3 is a SEY curve of a silver plating surface deposited 20nmTiN/C composite film before and after long-term placement;
FIG. 4 is a SEY curve of silver plated surface deposited with titanium nitride films of different thicknesses;
fig. 5 is a SEY curve of silver plated surface deposited amorphous carbon of varying thickness.
Detailed Description
The features and advantages of the present invention will become more apparent and clear from the following detailed description of the invention.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. Although various aspects of the embodiments are illustrated in the accompanying drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
According to a first aspect of the present invention, there is provided a thin film deposition process for suppressing micro-discharge effect of a satellite-borne microwave component, as shown in fig. 1, comprising the steps of:
step (1), thin film deposition technique and precursor determination: an atomic layer deposition technique was determined as a preparation method of the inhibition film, titanium tetrachloride and ammonia gas as precursors of the titanium nitride film, and tetrabromomethane and hydrogen gas as precursors of the amorphous carbon film.
In the step, the purity of titanium tetrachloride is not lower than 99.999%, the purity of ammonia is not lower than 99.999%, the purity of tetrabromomethane is not lower than 99.999%, and the purity of hydrogen is not lower than 99.999%.
Step (2), selecting and preprocessing a satellite-borne microwave component: and cleaning the surface of the selected spaceborne microwave component.
In this step, the selected on-board microwave components include filters, impedance transformers, antenna feeds, circulators, or switches, etc.
Cleaning treatments include, but are not limited to: sequentially ultrasonic cleaning with acetone, alcohol and isopropanol for 5min to remove oil, ultrasonic cleaning with deionized water for 5min, and oven drying at 50deg.C.
Step (3), determining a film deposition process: and sequentially depositing a titanium nitride film and an amorphous carbon film with target thicknesses on the surface of the space-borne microwave component.
Specifically, the thin film deposition process is as follows:
and 3.1, setting the temperature of a reaction cavity of the atomic layer deposition equipment, and heating the reaction cavity.
In this step, the temperature of the reaction chamber is set to 250 to 350 ℃, such as 300 ℃.
Step 3.2, when the temperature of the reaction cavity reaches the set temperature, transmitting the microwave component into the reaction cavity through the sample injection chamber, and vacuumizing the reaction cavity to 1e -6 Torr or less, and preheating.
In this step, the preheating time of the reaction chamber is 300 to 600 seconds, such as 600 seconds.
And 3.3, setting the circulation times, and alternately using two precursors of titanium tetrachloride and ammonia gas to perform atomic layer deposition reaction on the surface of the spaceborne microwave component to obtain the titanium nitride film with the target thickness.
In the step, the titanium nitride film deposition mode under each cycle comprises the following steps:
the carrier gas nitrogen pulse transmits the gas precursor titanium tetrachloride for 0.2-0.4 seconds, such as 0.3 seconds, to the reaction cavity, then the whole reaction cavity is purged with nitrogen for at least 8 seconds, then the gas precursor ammonia is introduced into the plasma device under the action of carrier gas argon, and enters the reaction cavity after glow reaction, and then argon is purged for at least 10 seconds. Wherein the purity of the carrier gas nitrogen is not lower than 99.999 percent, and the flow is 250-300 sccm, such as 300sccm; the purity of carrier gas argon is not lower than 99.999%, and the flow is 80-100 sccm, such as 100sccm; the flow rate of the precursor ammonia gas is 130-170 sccm, such as 150sccm.
In this step, the discharge power of the plasma device is 1500 to 2500W, such as 2000W, and the operating time is 13 to 17 seconds, such as 15 seconds.
In the step, the cycle times are 375-500 times, such as 375 times, and the thickness of the titanium nitride film in engineering application is 15-20 nm, such as 15nm.
And 3.4, setting the circulation times, and alternately using two precursors of tetrabromomethane and hydrogen to perform atomic layer deposition reaction on the titanium nitride film to obtain the amorphous carbon film with the target thickness.
In this step, the amorphous carbon film deposition method under each cycle includes:
and (3) introducing carrier gas nitrogen into the tetrabromomethane for 12-16 seconds, such as 15 seconds, to the reaction cavity, then carrying out nitrogen purging on the whole cavity for at least 8 seconds, then introducing gas precursor hydrogen into the plasma device under the action of carrier gas argon, entering the reaction cavity after glow reaction, and then carrying out argon purging for at least 8 seconds. Wherein the flow rate of carrier gas nitrogen is 250-300 sccm, such as 270sccm; the flow rate of the carrier gas argon is 90-110 sccm, such as 100sccm; the flow rate of the precursor hydrogen is 90-110 sccm, such as 100sccm.
In this step, the plasma apparatus has a discharge power of 250 to 450W, such as 400W, and an operating time of 1.5 to 3 seconds, such as 2 seconds.
In this step, the number of cycles is 250 to 400, such as 250, and the amorphous carbon film thickness for engineering applications is 5 to 8nm, such as 5nm.
According to a second aspect of the present invention, there is provided a film for suppressing micro-discharge effect of a microwave component on a satellite, the film comprising a titanium nitride film and an amorphous carbon film sequentially deposited on a surface of the microwave component on a satellite.
The space-borne microwave component is made of an aluminum alloy silver plating material, and a titanium nitride film and an amorphous carbon film are sequentially deposited on the surface of the space-borne microwave component, so that the problems that the titanium nitride film is easy to oxidize after being placed for a long time and the binding force of a carbon film on the surface of a substrate is poor can be effectively solved.
Preferably, the thickness of the titanium nitride film is 15 to 20nm such as 15nm; the amorphous carbon film has a thickness of 5 to 8nm, such as 5nm. The secondary electron emission characteristics of the titanium nitride film tend to saturate at 15nm, and the secondary electron emission characteristics of the amorphous carbon film tend to saturate at 5nm. Considering engineering application cost and reliability requirements, the thickness of the titanium nitride film is selected to be 15-20 nm, and the thickness of the amorphous carbon film is 5-8 nm.
Examples
The invention discloses a method for preparing a space-borne microwave component by using an aluminum alloy silver plating material. The Ku impedance transformer and the Ku narrow-band filter are commonly used spatial microwave components, and the micro-discharge suppression method according to the present invention will be described below by taking the Ku impedance transformer and the Ku narrow-band filter as examples.
Example 1Ku impedance transformer
1. A film deposition process for inhibiting micro-discharge effect of a satellite-borne microwave component comprises the following specific steps:
(1) Determination of thin film deposition technique and precursor: determining an atomic layer deposition technology as a preparation method of a TiN/C inhibition film, wherein titanium tetrachloride and ammonia are used as precursors, and tetrabromomethane and hydrogen are used as precursors of an amorphous carbon film; wherein the purity of the titanium tetrachloride is 99.999 percent, and the purity of the ammonia gas is 99.999 percent; the purity of tetrabromomethane is 99.999 percent, and the purity of hydrogen is 99.999 percent;
(2) Selecting and preprocessing a satellite-borne microwave component: selecting a Ku impedance converter as a deposition component, sequentially ultrasonically cleaning with acetone, alcohol and isopropanol for 5min to remove oil, ultrasonically cleaning with deionized water for 5min, and finally drying at 50 ℃ for later use;
(3) Determination of thin film deposition process:
setting the temperature of a reaction cavity of atomic layer deposition equipment to 300 ℃, and heating the reaction cavity;
secondly, when the temperature of the reaction cavity reaches the set temperature, the microwave component is transmitted into the reaction cavity through the sample injection chamber, and the reaction cavity is vacuumized to 1e -6 A preheating is performed for 600 seconds under Torr;
thirdly, firstly, carrying out nitrogen pulse transmission on a gas precursor titanium tetrachloride with purity of 99.999% and flow rate of 300sccm for 0.3 seconds to a reaction cavity by using carrier gas nitrogen with the temperature of 22 ℃, and then carrying out nitrogen purging on the whole cavity for 8 seconds; then under the action of carrier gas argon with the purity of 99.999 percent and the flow of 100sccm, introducing ammonia with the purity of 99.999 percent and the flow of 150sccm into a plasma device, entering a reaction cavity after glow reaction, wherein the discharge power of the plasma device is 2000W, the working time is 15 seconds, and then argon purging is carried out for 10 seconds to complete a cycle, thus 375 cycles are carried out; the average thickness of the titanium nitride film is 15nm;
step four, introducing tetrabromomethane into the reaction cavity for 15 seconds from carrier gas nitrogen with the flow rate of 270sccm, then carrying out nitrogen purging on the whole cavity for 8 seconds, then introducing precursor hydrogen with the flow rate of 100sccm into a plasma device under the action of carrier gas argon with the flow rate of 100sccm, entering the reaction cavity after glow reaction, wherein the discharge power of the plasma device is 400W, the working time is 2 seconds, and then carrying out argon purging for 8 seconds to complete a cycle, thus 250 cycles are carried out; the average thickness of the amorphous carbon film is 5nm;
(4) And conveying the Ku impedance transformer from the reaction cavity to the sample injection chamber, and taking out the sample after the sample is cooled and packaging and preserving the sample.
2. The comparative sample of the Ku impedance transformer was prepared by the same process, but only a 20nm titanium nitride film was plated in the third step. The micro-discharge experiment tests prove that the micro-discharge threshold of the Ku impedance transformer before and after film deposition is improved from 2000W to 5000W, which is improved by more than 3dB compared with the original micro-discharge threshold of the silver plating surface of the aluminum alloy, and the powerful inhibition effect is realized.
3. After the Ku impedance converter is subjected to film deposition in the steps, secondary electron emission characteristics of the surface of the Ku impedance converter before and after deposition are tested by using an SEY test platform, SEY curve results before and after the silver plating surface is deposited with a 20nm titanium nitride film for a long time are shown in FIG. 2, and a sample piece after the deposition of the 20nm titanium nitride film (TiN-original) has good secondary electron suppression characteristics compared with a sample piece (ag) before the deposition of a coating film. The samples were placed in a drying cabinet (# 1TiN-after 100 days) and a laboratory air environment (# 2TiN-after 100 days), respectively, and after a long-term storage for 100days, secondary electron emission characteristics were markedly deteriorated, surface titanium nitride was severely oxidized, and the SEY maximum values were deteriorated from 1.59 to 1.86 (# 1TiN-after 100 days) and 2.29 (# 2TiN-after 100 days), respectively.
The SEY curves before and after the deposition of the 20nmTiN/C composite film on the silver plating surface are shown in fig. 3, and the product after the deposition of the 20nmTiN/C composite film (TiN/C-original) has good secondary electron suppression characteristics compared with the product (ag) before the deposition of the plating film, and the effect is better than that of the deposition of the 20nm titanium nitride film on the silver plating surface.
The sample is placed in a drying cabinet (TiN/C-after 100 days), and no obvious deterioration appears after the sample is placed for 100days, so that the method provided by the invention is proved to solve the problems of oxidation of the titanium nitride film and carbon film falling off to a certain extent.
Example 2 narrow band Filter
1. A film deposition process for inhibiting micro-discharge effect of a satellite-borne microwave component comprises the following specific steps:
(1) Determination of thin film deposition technique and precursor: determining an atomic layer deposition technology as a preparation method of a TiN/C inhibition film, wherein titanium tetrachloride and ammonia are used as precursors, and tetrabromomethane and hydrogen are used as precursors of an amorphous carbon film; wherein the purity of the titanium tetrachloride is 99.999 percent, and the purity of the ammonia gas is 99.999 percent; the purity of tetrabromomethane is 99.999 percent, and the purity of hydrogen is 99.999 percent;
(2) Selecting and preprocessing a satellite-borne microwave component: selecting a Ku narrow-band filter as a deposition component, sequentially ultrasonically cleaning with acetone, alcohol and isopropanol for 5min to remove oil, ultrasonically cleaning with deionized water for 5min, and finally drying at 50 ℃ for later use;
(3) Determination of thin film deposition process:
setting the temperature of a reaction cavity to 300 ℃ and heating the reaction cavity;
secondly, when the temperature of the reaction cavity reaches the set temperature, the microwave component is transmitted into the reaction cavity through the sample injection chamber, and the reaction cavity is vacuumized to 1e -6 A preheating is performed for 600 seconds under Torr;
thirdly, firstly, carrying out nitrogen pulse transmission on a gas precursor titanium tetrachloride with purity of 99.999% and flow rate of 300sccm for 0.3 seconds to a reaction cavity by using carrier gas nitrogen with the temperature of 22 ℃, and then carrying out nitrogen purging on the whole cavity for 8 seconds; then under the action of carrier gas argon with the purity of 99.999 percent and the flow of 100sccm, introducing ammonia with the purity of 99.999 percent and the flow of 150sccm into a plasma device, entering a reaction cavity after glow reaction, wherein the discharge power of the plasma device is 2000W, the working time is 15 seconds, and then argon purging is carried out for 10 seconds to complete a cycle, thus 375 cycles are carried out; the thickness of the titanium nitride film is 20nm;
step four, introducing tetrabromomethane into the reaction cavity for 15 seconds from carrier gas nitrogen with the flow rate of 270sccm, then carrying out nitrogen purging on the whole cavity for 8 seconds, then introducing precursor hydrogen with the flow rate of 100sccm into a plasma device under the action of carrier gas argon with the flow rate of 100sccm, entering the reaction cavity after glow reaction, wherein the discharge power of the plasma device is 400W, the working time is 2 seconds, and then carrying out argon purging for 8 seconds to complete a cycle, thus 250 cycles are carried out; the thickness of the amorphous carbon film is 5nm;
(4) And conveying the Ku narrow-band filter from the reaction cavity to the sample injection chamber, and taking out the sample after the sample is cooled and packaging and preserving the sample.
After the Ku narrow-band filter is subjected to film deposition in the steps, the micro-discharge threshold is increased from 100W to 300W.
Experimental example 1 titanium nitride film thickness test
By adjusting the cycle times to 125, 250, 375, 500 and 750, titanium nitride films of 5nm, 10nm, 15nm, 20nm and 30nm were deposited by the titanium nitride film deposition method of example 1, respectively, and the secondary electron emission characteristics thereof are shown in fig. 4. As can be seen from fig. 4, compared with SEY curve of silver plating on the metal surface of the conventional microwave component, secondary electron emission coefficient is obviously reduced after TiN plating. And as the thickness of the titanium nitride film increases, the secondary electron emission coefficient gradually decreases and tends to be saturated at 15nm, the secondary electron emission coefficient is stabilized at about 1.6, and the secondary electron emission coefficient is reduced by about 31%. Therefore, the thickness of the titanium nitride film of the process is generally selected to be 15-20 nm in consideration of engineering application cost and reliability requirements.
Experimental example 2 amorphous carbon film thickness test
By adjusting the cycle times to 100, 150, 250 and 400, the amorphous carbon films of 2nm, 3nm, 5nm and 8nm were deposited respectively, using the amorphous carbon film deposition method of example 1, and the secondary electron emission characteristics thereof are shown in FIG. 5. As can be seen from fig. 5, compared with SEY curve of silver plating on the metal surface of the conventional microwave component, secondary electron emission coefficient is significantly reduced after amorphous carbon plating. As the thickness of the amorphous carbon film increases, the secondary electron emission coefficient gradually decreases, and the secondary electron emission coefficient of the 3nm amorphous carbon film is already lower than 1.4. The amorphous carbon film is mainly used as an oxidation resistant layer, and the thickness of the amorphous carbon film is generally selected to be 5-8 nm in consideration of the poor growth uniformity and the overall reliability requirement in the initial growth stage of atomic layer deposition.
The invention has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the invention. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, and these fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
What is not described in detail in the present specification is a well known technology to those skilled in the art.
Claims (10)
1. A film deposition process for inhibiting micro-discharge effect of a satellite-borne microwave component is characterized by comprising the following steps of: and sequentially depositing a titanium nitride film and an amorphous carbon film with target thicknesses on the surface of the space-borne microwave component.
2. The thin film deposition process for suppressing the micro-discharge effect of a microwave component on board according to claim 1, wherein the microwave component on board includes a filter, an impedance transformer, an antenna feed, a circulator, or a switch.
3. The thin film deposition process for suppressing the micro-discharge effect of a microwave component on a satellite as claimed in claim 1, wherein the surface of the microwave component on a satellite is cleaned before the titanium nitride thin film and the amorphous carbon thin film with target thicknesses are sequentially deposited on the surface of the microwave component on a satellite.
4. The thin film deposition process for suppressing the micro-discharge effect of a microwave component on a satellite as claimed in claim 1, wherein the step of sequentially depositing a titanium nitride thin film and an amorphous carbon thin film with target thicknesses on the surface of the microwave component on a satellite comprises:
setting the temperature of a reaction cavity of the atomic layer deposition equipment, and heating the reaction cavity;
when the temperature of the reaction cavity reaches the set temperature, the microwave component is transmitted into the reaction cavity through the sample injection chamber, the reaction cavity is vacuumized, and preheating is carried out;
setting the circulation times, and alternately using two precursors of titanium tetrachloride and ammonia gas to perform atomic layer deposition reaction on the surface of the spaceborne microwave component to obtain a titanium nitride film with target thickness;
setting the circulation times, and alternately using two precursors of tetrabromomethane and hydrogen to perform atomic layer deposition reaction on the titanium nitride film to obtain the amorphous carbon film with the target thickness.
5. The thin film deposition process for suppressing micro-discharge effect of a microwave component on a satellite as claimed in claim 4, wherein in the step of setting the temperature of the reaction chamber of the atomic layer deposition apparatus and heating the reaction chamber, the temperature of the reaction chamber is set to 250-350 ℃.
6. The thin film deposition process for suppressing micro-discharge effect of a microwave component on a satellite as claimed in claim 4, wherein when the temperature of the reaction chamber reaches a set temperature, the microwave component is transferred to the reaction chamber through the sample chamber, the reaction chamber is evacuated, and the preheating time of the reaction chamber is 300-600 seconds.
7. The thin film deposition process for suppressing micro-discharge effect of a microwave component on a satellite as claimed in claim 4, wherein the titanium nitride thin film deposition method under each cycle comprises:
the carrier gas nitrogen pulse transmits gas precursor titanium tetrachloride for 0.2-0.4 seconds to the reaction cavity, then nitrogen purging is carried out on the whole reaction cavity, then the gas precursor ammonia is introduced into the plasma device under the action of carrier gas argon, and enters the reaction cavity after glow reaction, and argon purging is carried out; preferably, the purity of carrier gas nitrogen is not lower than 99.999 percent, and the flow is 250-300 sccm; the purity of carrier gas argon is not lower than 99.999 percent, and the flow is 80-100 sccm; the flow of the precursor ammonia gas is 130-170 sccm.
8. The thin film deposition process for suppressing micro-discharge effect of a microwave component on a satellite as claimed in claim 4, wherein the amorphous carbon thin film deposition method under each cycle comprises:
introducing carrier gas nitrogen into tetrabromomethane for 12-16 seconds to a reaction cavity, then carrying out nitrogen purging on the whole cavity, then introducing gas precursor hydrogen into a plasma device under the action of carrier gas argon, entering the reaction cavity after glow reaction, and then carrying out argon purging; preferably, the flow rate of carrier gas nitrogen is 250-300 sccm; the flow rate of carrier gas argon is 90-110 sccm; the flow rate of the precursor hydrogen is 90-110 sccm.
9. The thin film deposition process for inhibiting micro-discharge effect of a satellite-borne microwave component according to claim 1, wherein the target thickness of the titanium nitride thin film is 15-20 nm; the target thickness of the amorphous carbon film is 5-8 nm.
10. The film for inhibiting the micro-discharge effect of the satellite-borne microwave component is characterized by comprising a titanium nitride film and an amorphous carbon film which are sequentially deposited on the surface of the satellite-borne microwave component, wherein the thickness of the titanium nitride film is 15-20 nm; the amorphous carbon film has a thickness of 5 to 8nm.
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