CN116005108A - Composite hydrogen-resistant coating processing method and composite hydrogen-resistant coating - Google Patents
Composite hydrogen-resistant coating processing method and composite hydrogen-resistant coating Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a processing method of a composite hydrogen-resistant coating and the composite hydrogen-resistant coating, wherein the third hydrogen-resistant layer obtained by the processing method has no crystal boundary defect of a crystal material, has excellent hydrogen-resistant performance, and can greatly increase the difficulty of penetrating a surface layer; the first hydrogen-resistant layer and the second hydrogen-resistant layer are processed by adopting a closed unbalanced magnetron sputtering process, so that the grain sizes of the first hydrogen-resistant layer and the second hydrogen-resistant layer are finer, the compactness of the coating is high, and the hydrogen-resistant performance of the first hydrogen-resistant layer and the second hydrogen-resistant layer can be greatly improved; the three hydrogen blocking layers are overlapped together, so that the permeation difficulty of hydrogen atoms to permeate into different layers is increased in geometric multiple. The method adopts relatively low process temperature, firstly, the crystal grains of the first hydrogen-resistant layer and the second hydrogen-resistant layer are not increased in a transitional way, so that a coating with small and compact crystal grains is obtained, secondly, the third hydrogen-resistant layer can be ensured to have enough hardness, and the problem that the substrate is easy to be deformed due to tempering caused by overhigh temperature, so that the first hydrogen-resistant layer, the second hydrogen-resistant layer and the third hydrogen-resistant layer are influenced to lose efficacy is avoided.
Description
Technical Field
The invention relates to the field of hydrogen-resistant materials, in particular to a composite hydrogen-resistant coating processing method and a composite hydrogen-resistant coating.
Background
The hydrogen energy is widely used in various industries at present because of the characteristics of safety, wide sources, high heat value, cleanness and the like. Hydrogen energy is generally stored in a liquid form in a metallic hydrogen storage container, and when hydrogen and isotopes permeate into a metallic material, the metallic material can be degraded in performance, and structural hydrogen damage occurs. Therefore, the covering of the hydrogen-resistant coating on the surface of the metal material is of great significance for solving the problem of hydrogen permeation.
For example, chinese patent application publication No. CN113122842a discloses a composite hydrogen barrier coating and a method for preparing the same, which includes alternating metal transition layers and oxide ceramic coatings of the corresponding metals.
For another example, chinese patent publication No. CN104561891B discloses a dual-component gradient hydrogen permeation resistant coating and a preparation method thereof, wherein the dual-component gradient hydrogen permeation resistant coating comprises a Cr coating, a Cr-O component gradient coating, a Cr-Al-O component gradient coating, an Al-O component gradient coating and an A306O3 coating which are sequentially arranged.
Although they all use a multi-layer composite structure to improve the hydrogen resistance, each layer of coating is composed of grains, and there is more or less a certain gap between the grains, which results in a certain limitation of the hydrogen resistance of each layer.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a processing method of a composite hydrogen-resistant coating and the composite hydrogen-resistant coating.
The aim of the invention is achieved by the following technical scheme:
the processing method of the composite hydrogen-resistant coating comprises the following steps:
s1, cleaning a substrate;
s2, depositing a first hydrogen resistance layer on the cleaned substrate by adopting a closed unbalanced magnetron sputtering process;
s3, depositing a second hydrogen resistance layer on the first hydrogen resistance layer by adopting a closed unbalanced magnetron sputtering process;
s4, depositing a third hydrogen resistance layer on the second hydrogen resistance layer, wherein the third hydrogen resistance layer is of an amorphous structure;
and controlling the deposition temperature not to exceed 200 ℃ when the first hydrogen resistance layer, the second hydrogen resistance layer and the third hydrogen resistance layer are deposited.
Preferably, in the processing method of the composite hydrogen-resistant coating, the thickness of the second hydrogen-resistant layer is between 2 and 20 micrometers.
Preferably, in the processing method of the composite hydrogen-resistant coating, the thickness of the third hydrogen-resistant layer is between 1 and 10 micrometers.
Preferably, in the processing method of the composite hydrogen-resistant coating, the third hydrogen-resistant layer is a diamond-like film, and the thickness of the third hydrogen-resistant layer is between 1 and 5 micrometers.
Preferably, in the processing method of the composite hydrogen-resistant coating, the deposition temperature is controlled to be not higher than 200 ℃ by alternately coating and cooling.
Preferably, in the processing method of the composite hydrogen-resistant coating, the deposition temperature is controlled between 100 ℃ and 150 ℃.
Preferably, in the processing method of the composite hydrogen-resistant coating, the time for each coating is 10-30 minutes, and the time for each cooling is 10-30 minutes.
Preferably, in the processing method of the composite hydrogen-resistant coating, the cooling is realized by introducing argon gas into a deposition furnace for circulating cooling and water for circulating cooling.
Preferably, in the processing method of the composite hydrogen-resistant coating, the temperature of the cooling water cooled by water circulation is controlled between 15 ℃ and 25 ℃.
The composite hydrogen-resistant coating is obtained by adopting any one of the processing methods.
The technical scheme of the invention has the advantages that:
according to the invention, the third hydrogen-resistant layer of the surface layer is of an amorphous structure, no crystal boundary defect of a crystal material exists, and the hydrogen-resistant layer has excellent hydrogen resistance, is arranged on the surface layer, so that the difficulty of breaking through the surface layer by hydrogen atoms is greatly increased, and the probability of hydrogen permeating into other layers can be reduced; the first hydrogen-resistant layer and the second hydrogen-resistant layer are processed by adopting a closed unbalanced magnetron sputtering process, so that the grain sizes of the first hydrogen-resistant layer and the second hydrogen-resistant layer are finer, the compactness of the coating is high, and the first hydrogen-resistant layer and the second hydrogen-resistant layer have higher hydrogen-resistant performance; the three hydrogen blocking layers are overlapped together, so that gaps of each layer can be made up, and the permeation difficulty of hydrogen atoms in each layer is greatly increased while the permeation difficulty between the layers is greatly increased. The method has the advantages that the relatively low process temperature is adopted, firstly, crystal grains of the first hydrogen-resistant layer and the second hydrogen-resistant layer can not be excessively increased, so that a compact coating with small crystal grains is obtained, secondly, the third hydrogen-resistant layer can be ensured to have enough hardness, the problem that the substrate is easy to deform due to tempering at too high temperature, and then the first hydrogen-resistant layer, the second hydrogen-resistant layer and the third hydrogen-resistant layer are influenced to lose efficacy is solved, and the stability of the structure is ensured.
The third hydrogen-resistant layer adopts the diamond-like carbon coating, and the thickness of the third hydrogen-resistant layer is controlled to be 1.5-2.5 microns, so that the surface layer can be effectively ensured to have enough hydrogen-resistant capability, and the problem that the stability of the coating is affected due to weakening of binding force caused by overlarge thickness of the diamond-like carbon coating is avoided.
According to the invention, through improvement of the deposition furnace, the deposition furnace not only can effectively improve the coating quality and compactness of closed unbalanced magnetron sputtering, but also can realize combination of different cleaning processes to improve the cleaning quality and effect.
According to the invention, the coating is performed in an alternating manner of coating and cooling, the coating temperature can be conveniently controlled, the deposition temperature is controlled to be between 100 ℃ and 150 ℃, the grain size can be prevented from being too large and the substrate can be prevented from being tempered, meanwhile, the cooling adopts two modes of argon circulation cooling and water circulation cooling, the cooling rate can be greatly improved, the overall deposition efficiency is improved, and the effective combination of grain size control, high efficiency and low cost can be realized.
Drawings
FIG. 1 is a schematic illustration of a composite hydrogen barrier coating of the present invention;
FIG. 2 is a cross-sectional profile view of a third hydrogen barrier layer of the present invention under SEM (electron scanning microscope);
FIG. 3 is a surface topography of the first hydrogen barrier layer of the present invention after 500 times magnification under SEM;
FIG. 4 is a schematic view of a deposition furnace of the present invention;
FIG. 5 is a schematic view of the structure of an anode layer ion source of the present invention;
fig. 6 is a surface structure diagram of a first hydrogen-resistant layer or a second hydrogen-resistant layer deposited in the deposition furnace of the present invention at coil current 5A, wherein the surface of the coating layer has a dense crystal structure with columnar crystals disappearing.
Detailed Description
The objects, advantages and features of the present invention are illustrated and explained by the following non-limiting description of preferred embodiments. These embodiments are only typical examples of the technical scheme of the invention, and all technical schemes formed by adopting equivalent substitution or equivalent transformation fall within the scope of the invention. In the description of the embodiments, it should be noted that the positional or positional relationship indicated by the terms such as "center", "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "inner", "outer", etc. are based on the positional or positional relationship shown in the drawings, are merely for convenience of description and simplification of description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in the specific orientation, and thus are not to be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The processing method of the composite hydrogen-resistant coating disclosed by the invention is described below with reference to the accompanying drawings, and comprises the following steps:
s1, cleaning a substrate 100;
s2, depositing a first hydrogen resistance layer 200 on the cleaned substrate 100 by adopting a closed unbalanced magnetron sputtering process;
s3, depositing a second hydrogen barrier layer 300 on the first hydrogen barrier layer 200 by adopting a closed unbalanced magnetron sputtering process;
and S4, depositing a third hydrogen-resistant layer 400 on the second hydrogen-resistant layer 300, wherein the third hydrogen-resistant layer 400 is of an amorphous structure, so as to obtain the composite hydrogen-resistant coating shown in the figure 1.
As shown in fig. 2, the third hydrogen barrier layer 400 of the present invention has an amorphous structure, which does not have grain boundary defects of crystalline materials, so that the coating layer has little void, thereby having excellent hydrogen barrier properties itself; the first hydrogen-resistant layer 200 and the second hydrogen-resistant layer 300 are obtained by adopting a closed unbalanced magnetron sputtering process, so that the grain sizes of the first hydrogen-resistant layer 200 and the second hydrogen-resistant layer 300 are smaller as shown in the figure 3, the compactness of the coating is effectively improved, and gaps among grains are reduced, so that the hydrogen-resistant performance of the first hydrogen-resistant layer 200 and the second hydrogen-resistant layer 300 is effectively improved; the three membrane layers with good hydrogen resistance are overlapped together, so that gaps of the membrane layers can be effectively compensated, and the permeation difficulty of hydrogen atoms to different membrane layers is increased in geometric multiple.
The first hydrogen-resistant layer 200 and the second hydrogen-resistant layer 300 are required to be deposited by adopting a closed unbalanced magnetron sputtering process, so that a deposition furnace used in the processing of the composite hydrogen-resistant coating can be a known closed unbalanced magnetron sputtering device, further, in consideration of the need of improving the cleaning quality of a substrate and the need of improving the compactness of a film layer to improve the hydrogen-resistant capability, in the embodiment, an ion beam source is added to the deposition furnace on the basis of the known closed unbalanced magnetron sputtering device to improve the cleaning effect, and an electromagnetic coil is added to optimize the closing degree of a magnetic field, so that the plasma density of magnetron sputtering is increased, and therefore, the crystal size of the first hydrogen-resistant layer and the second hydrogen-resistant layer prepared by adopting the deposition furnace is smaller, and the coating is more compact and has better hydrogen-resistant effect.
Specifically, as shown in fig. 4, the deposition furnace includes a furnace body 10, a turret 20, an ion beam source 30, a magnetron sputtering target 40, an electromagnetic coil 50, and a power supply assembly. The rotary frame 20 is arranged in the furnace body 10, and the rotary frame 20 is used for fixing a base material and can drive the base material to rotate at least one stage. The ion beam sources 30 are distributed around the turret 20, preferably in two numbers and symmetrically on opposite sides of the turret 20; the ion beam source 30 may be any of a variety of possible ion beam sources known in the art, with an anode layer ion source being preferred.
As shown in fig. 5, the anode layer ion source includes an inner cathode 301, an outer cathode 302, an anode 303, and a permanent magnet 304, the outer cathode 302 is located at the periphery of the inner cathode 301, and the anode 303 is disposed below the inner cathode 301 and the outer cathode 302 and opposite to the gap between the inner and outer cathodes. The permanent magnets 304 are located between the anodes 303 and below the inner cathode 301.
As shown in FIG. 5, the horizontal distance 305 between the inner and outer electrodes is set to be 4-8mm, and the distance 306 between the cathode and anode in the height direction is set to be 4-8mm, which is designed because: when the electrode spacing of the glow discharge is relatively close, breakdown easily occurs at a high operating pressure when the ion beam source 30 is operated at a voltage of 1500V to 2000V, resulting in unstable operation. The polar distance of glow discharge is enlarged, so that the occurrence of arcing condition can be effectively reduced, and the ion beam can stably work under higher air pressure. Furthermore, the anode layer ion source adopts a pulse power supply, the duty ratio of the pulse power supply is controlled within 40% when in work, and the phenomenon that the ion beam is arcing under the high voltage of 1500-2000V and the high air pressure of 0.6-1.5Pa can be effectively restrained, so that the ion beam can work more stably under higher working pressure. Therefore, the problem that the ion beam cleaning and the bias glow cleaning are difficult to clean simultaneously due to different working air pressures is effectively solved.
Further, the magnetic induction of the permanent magnet 304 is set between 450-550mT (millitesla), so designed because: the increase of the polar distance causes weakening of ion energy, resulting in poor cleaning effect, and the arrangement of the magnetic induction intensity of the permanent magnet 304 can effectively enhance ion energy, so as to ensure that the cleaning effect is achieved.
As shown in FIG. 4, the magnetron sputtering targets 40 are disposed around the rotating frame 20, the number of which can be designed according to the need, preferably, the magnetron sputtering targets 40 are 1-3 pairs, and each pair of the magnetron sputtering targets 40 is symmetrically disposed at both sides of the rotating frame 20. The magnetron sputtering target 40 can be any of a variety of known sputtering targets, preferably they are unbalanced magnetron sputtering targets 40 and form a closed magnetic trap 90.
As shown in fig. 4, the electromagnetic coils 50 are in one-to-one correspondence with the magnetron sputtering targets 40 and are arranged around the periphery of each magnetron sputtering target 40, so that the magnetic field closure performance can be enhanced, the electron escape is reduced, the plasma concentration in the workpiece area is increased, the bias current is increased, the film forming rate is improved, the obtained coated material grains are smaller and have higher density, and the gap of the film is effectively reduced, and the difficulty of hydrogen atom permeation is increased.
In the actual processing, in S1, in order to ensure the cleaning quality and efficiency of the substrate, the cleaning of the substrate 100 in this embodiment includes the following steps:
s11, placing the substrate 100 on a rotating frame in a deposition furnace.
S12, vacuumizing the deposition furnace to a preset vacuum degree, for example, 0.05Pa.
S13, filling argon into the deposition furnace until the air pressure in the deposition furnace is between 0.6 Pa and 1.5 Pa.
S14, turning on the bias power supply 60 and the ion beam source 30 to clean the substrate simultaneously with the bias glow cleaning and the ion beam cleaning, wherein the time for cleaning the substrate simultaneously with the bias glow cleaning and the ion beam cleaning is not more than 1 hour, more preferably not more than 45 minutes, and most preferably about 30 minutes.
In a specific operation, the bias power supply 60 is turned on first, and then the ion beam sources 30 are turned on one by one, wherein the voltage of the bias power supply 60 is 700-2000V, more preferably 800-2000V, and at this time, a large bias current (2-30A, more preferably 15-30A) can be obtained, so that a better cleaning effect can be obtained. The ion beam source 30 is operated at a voltage of between 300V and 2000V, and more preferably between 1500V and 2000V.
After the two cleaning modes are effectively combined, the large-area high-efficiency advantage of bias glow cleaning effectively overcomes the problems of small bias flow and low efficiency of ion beam cleaning, meanwhile, the large plasma energy and the directionality of the ion beam cleaning effectively overcome the defects that the plasma energy of the bias glow cleaning is insufficient and the high-quality cleaning can not be carried out on the corner areas and the opposite positions due to uneven glow distribution, and the perfect combination of the cleaning effect and the cleaning efficiency is realized.
The specific process of depositing the first hydrogen barrier layer and the second hydrogen barrier layer by adopting the unbalanced magnetron sputtering deposition process in S2 and S3 is a known technology, and will not be described herein. It should be noted that, during deposition, the current of the electromagnetic coil is controlled to be about 5A, so that the coating can be more dense, as shown in fig. 6.
In actual production, the inventors studied to find that: the metal materials such as titanium, nickel, chromium and the like have better binding force with the base material 100 during deposition, and the grains are refined. Therefore, in the step S2, the first hydrogen barrier layer 200 may be a titanium layer, a nickel layer or a chromium layer, and the specific thickness of the first hydrogen barrier layer 200 may be designed according to the bonding force to be achieved, which is not limited herein.
In the step S3, the second hydrogen blocking layer 300 may be a nitride or an oxide such as chromium nitride, titanium nitride, or tungsten carbide. The inventors further studied and found that: the titanium nitride has high melting point and good heat stability, and meanwhile, the crystal grains of the titanium can be thinned, so that the crystal structure is more compact, and a good hydrogen resistance effect is achieved. Therefore, the second hydrogen-blocking layer 300 is preferably a titanium nitride layer, and correspondingly, the first hydrogen-blocking layer 200 is a titanium layer. And, the thickness of the second hydrogen blocking layer 300 is preferably 2-20, more preferably 2.5-15 microns. Such thickness allows the second hydrogen blocking layer 300 to have a stable hydrogen blocking effect while providing sufficient support for the third hydrogen blocking layer 400 and ensuring the bonding force.
The third hydrogen barrier layer 400 is preferably a diamond-like film that can be prepared by ionizing hydrocarbon gas by a known anode layer ion beam; the diamond-like film can also be prepared by a mode of cathodic arc and elbow pipe filtration, wherein the method comprises the steps of evaporating and ionizing target molecules through arc discharge, and obtaining pure ion flow through elbow pipe filtration so as to prepare the diamond-like film; of course, the diamond-like film may also be deposited by PECVD.
The thickness of the third hydrogen blocking layer 400 is between 1 and 10 micrometers, more preferably, the thickness of the third hydrogen blocking layer 400 is between 1.5 and 5 micrometers, and most preferably between 1.5 and 2.5 micrometers, because the diamond-like thin film is a brittle material, the thickness of the diamond-like thin film is increased to easily cause the decrease of the binding force, and the binding force of the second hydrogen blocking layer 300 formed by titanium nitride is good, so that the thickness of the third hydrogen blocking layer 400 can be reduced and the thickness of the second hydrogen blocking layer 300 can be increased on the basis of ensuring sufficient hydrogen blocking capacity, thereby improving the hydrogen blocking effect of the whole coating and simultaneously having stable binding force.
When the first, second and third hydrogen-resistant layers are deposited, the deposition temperature of each layer is controlled to be not higher than 200 ℃, the first, second and third hydrogen-resistant layers are processed by adopting lower deposition temperature, and one of the first, second and third hydrogen-resistant layers can be effectively matched with a closed unbalanced magnetron sputtering process to enable the grains of the first hydrogen-resistant layer 200 and the second hydrogen-resistant layer 300 to be as small as possible and the coating to be more compact. Furthermore, the third hydrogen barrier layer 400 can be effectively ensured to have enough hardness to improve the structural stability and reduce the risk of damaging the surface layer by external force. More importantly, when the deposition temperature is too high, the substrate 100 is easy to temper and the hardness and strength are reduced, so that the substrate 100 is easy to deform to cause the bonding force with the coating to be poor, and finally the first hydrogen barrier layer 200, the second hydrogen barrier layer 300 and the third hydrogen barrier layer 400 are invalid, and the occurrence of the situation is effectively avoided by the lower process temperature.
The deposition temperature is controlled to be not higher than 200 ℃ by alternately performing film coating and cooling, taking the deposition of the first hydrogen-resistant layer 200 as an example, during deposition, the sputtering power supply 70 is turned on to perform film coating, the sputtering power supply 70 is turned off after 10-30 minutes of film coating, cooling is performed, the sputtering power supply 70 is turned on again after 10-30 minutes of cooling, the sputtering power supply 70 is turned off again after 10-30 minutes of film coating, cooling is performed, and the process is stopped when the thickness of the first hydrogen-resistant layer 200 reaches a target value.
The concrete cooling is realized by introducing argon gas into the deposition furnace for circulating cooling and water for circulating cooling. Argon gas circulation cooling is realized by continuously filling argon gas into the deposition furnace when coating is stopped every time and vacuumizing through a vacuumizing system. The water circulation cooling is realized by conveying cooling water to a water cooling plate at a proper position in the deposition furnace through a cooling water circulation system when each film coating is stopped. The specific location of the cooling plate may be designed as desired and is not limited herein. The specific structure of the cooling water circulation system is known technology, and the cooling water temperature supplied to the water cooling plate is controlled between 15 ℃ and 25 ℃ without description.
Combining the two cooling modes can increase the cooling rate to achieve the target cooling temperature in as short a time as possible, which is advantageous for increasing the overall deposition rate. More preferably, when each layer is deposited, the deposition temperature is more preferably controlled between 100 ℃ and 150 ℃, so that the cooling time can be effectively shortened, the cooling cost is reduced, and the perfect combination of low cost, high aging and good coating quality is realized.
Example 2
The embodiment discloses a composite hydrogen-resistant coating, which is obtained by processing the composite hydrogen-resistant coating by adopting the processing method of the embodiment. The composite hydrogen barrier coating may be used in a variety of applications where prevention of hydrogen permeation is desired, such as in hydrogen storage vessels.
Example 3
The embodiment discloses a hydrogen storage container, which comprises a substrate 100, wherein a first hydrogen-resistant layer 200, a second hydrogen-resistant layer 300 and a third hydrogen-resistant layer 400 are sequentially arranged on the substrate 100 from inside to outside, the third hydrogen-resistant layer 400 is of an amorphous structure, and particularly a diamond-like film layer, and the thickness of the diamond-like film layer is 1.5-5 microns.
The invention has various embodiments, and all technical schemes formed by equivalent transformation or equivalent transformation fall within the protection scope of the invention.
Claims (10)
1. The processing method of the composite hydrogen-resistant coating is characterized by comprising the following steps of: the method comprises the following steps:
s1, cleaning a substrate;
s2, depositing a first hydrogen resistance layer on the cleaned substrate by adopting a closed unbalanced magnetron sputtering process;
s3, depositing a second hydrogen resistance layer on the first hydrogen resistance layer by adopting a closed unbalanced magnetron sputtering process;
s4, depositing a third hydrogen resistance layer on the second hydrogen resistance layer, wherein the third hydrogen resistance layer is of an amorphous structure;
and controlling the deposition temperature not to exceed 200 ℃ when the first hydrogen resistance layer, the second hydrogen resistance layer and the third hydrogen resistance layer are deposited.
2. The method for processing the composite hydrogen-resistant coating according to claim 1, wherein: the thickness of the second hydrogen-blocking layer is between 2 and 20 micrometers.
3. The method for processing the composite hydrogen-resistant coating according to claim 1, wherein: the thickness of the third hydrogen-blocking layer is between 1 and 10 micrometers.
4. The method for processing the composite hydrogen-resistant coating according to claim 1, wherein: the third hydrogen-blocking layer is a diamond-like film having a thickness of between 1 and 5 microns.
5. The method for processing the composite hydrogen-resistant coating according to claim 1, wherein: the control of the deposition temperature not exceeding 200 ℃ is achieved by alternately coating and cooling.
6. The method for processing the composite hydrogen-resistant coating according to claim 5, wherein: the deposition temperature is controlled between 100-150 ℃.
7. The method for processing the composite hydrogen-resistant coating according to claim 5, wherein: the time for each coating is 10-30 minutes, and the time for each cooling is 10-30 minutes.
8. The method for processing the composite hydrogen-resistant coating according to claim 5, wherein: the cooling is realized by introducing argon gas into the deposition furnace for circulating cooling and water for circulating cooling.
9. The method for processing the composite hydrogen-resistant coating according to claim 8, wherein: the temperature of the cooling water cooled by water circulation is controlled between 15 ℃ and 25 ℃.
10. The composite hydrogen-resistant coating is characterized in that: processed by the processing method according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117967964A (en) * | 2024-02-21 | 2024-05-03 | 江苏兴邦能源科技有限公司 | Stacked hydrogen storage tank made of hydrogen storage materials |
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| JP2013180501A (en) * | 2012-03-02 | 2013-09-12 | Hyomen Kino Design Kenkyusho Kk | Hydrogen permeation prevention coating |
| CN104711527A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院大连化学物理研究所 | Method for magnetron sputtering low-temperature preparation of TiN film |
| CN105525273A (en) * | 2015-12-02 | 2016-04-27 | 北京天瑞星光热技术有限公司 | Silicon carbide hydrogen permeation barrier coating for stainless steel and preparation method for silicon carbide hydrogen permeation barrier coating |
| JP2017090370A (en) * | 2015-11-16 | 2017-05-25 | アズビル株式会社 | Hydrogen permeation prevention film |
| DE102020212869A1 (en) * | 2020-10-12 | 2021-11-04 | Carl Zeiss Smt Gmbh | Method of forming a hydrogen protective layer |
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| JP2013180501A (en) * | 2012-03-02 | 2013-09-12 | Hyomen Kino Design Kenkyusho Kk | Hydrogen permeation prevention coating |
| CN104711527A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院大连化学物理研究所 | Method for magnetron sputtering low-temperature preparation of TiN film |
| JP2017090370A (en) * | 2015-11-16 | 2017-05-25 | アズビル株式会社 | Hydrogen permeation prevention film |
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