CN109680254A - A kind of magnesium alloy carries hydrogen thin-film material and preparation method thereof - Google Patents

A kind of magnesium alloy carries hydrogen thin-film material and preparation method thereof Download PDF

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Publication number
CN109680254A
CN109680254A CN201910152281.5A CN201910152281A CN109680254A CN 109680254 A CN109680254 A CN 109680254A CN 201910152281 A CN201910152281 A CN 201910152281A CN 109680254 A CN109680254 A CN 109680254A
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magnesium alloy
hydrogen
film material
thin
sputtering
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CN109680254B (en
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王亮
唐舵
吉祥波
王窈
李勇
邢宗仁
覃文志
高原
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Institute of Chemical Material of CAEP
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3457Sputtering using other particles than noble gas ions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0031Intermetallic compounds; Metal alloys; Treatment thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F42AMMUNITION; BLASTING
    • F42CAMMUNITION FUZES; ARMING OR SAFETY MEANS THEREFOR
    • F42C19/00Details of fuzes
    • F42C19/08Primers; Detonators
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/32Hydrogen storage

Abstract

The invention discloses a kind of magnesium alloys to carry hydrogen thin-film material, including magnesium alloy film, and the ratio of magnesium atom and aluminium atom is between 9:1 to 1:9 in the magnesium alloy film;Hydrogen atom proportion is less than or equal to 20%.The Laser Driven improved efficiency principle that magnesium alloy carries hydrogen thin-film material is: metal hydrogen storage material is under light laser ablation effect, discharge rapidly out hydrogen, hydrogen participates in and enhances laser ablation reaction, so that photo plasma temperature and electron density increase, and then promotes plasma drive efficiency.Preparation method includes the following steps 1: choosing the substrate with high laser transmittance, is cleaned up and be dried for standby;Step 2: step 1 gained substrate and magnesium alloy target being put into sputtering chamber, vacuumized after installation is fixed;Step 3: passing through magnetron sputtering magnesium alloy film.

Description

A kind of magnesium alloy carries hydrogen thin-film material and preparation method thereof
Technical field
It is that a kind of magnesium alloy carries hydrogen thin-film material and its system specifically the present invention relates to hydrogen thin film technique field is carried Preparation Method.
Background technique
With the networking and informationization of modern war, electromagnetic compatible environment will be more inside future battlefield and weapon system It is complicated and harsh.Priming system originates element as the function of weapon system, decides the essential safety of ammunition.For this purpose, Los Alamos, Sandia are equal to the eighties in last century, and the Laser Driven Flyer Plates technology with anti-strong electromagnetic ability is answered For detonating charge.Laser Driven Flyer Plates technology, which is developed so far, achieves numerous significant achievements, however, still there is many critical issues It needs to be studied, more outstanding is laser and the lower problem of film flying energy coupling efficiency.All the time, film flying is as solution Certainly the key of energy coupling efficiency has obtained extensive research.In early days, film flying mainly uses single-layer metal film, and energy coupling efficiency is not Foot 20%;In recent years, film flying uses composite structure, which includes absorbed layer, ablation layer, thermal insulation layer and film flying layer.It is multiple It closes in film flying, the main function of absorbed layer is enhancing laser absorption rate, usually C or Ti;Ablation layer is transducing layer, usually The metal materials such as Al, Ge, Cu form high pressure plasma under laser excitation, to shear film flying layer material, make its acquisition Higher speed impacts detonating charge;Thermal insulation layer main function is to reduce ablation layer energy loss, usually Al2O3, CuO etc..C/ Al/Al2O3/ Al is presently most common and efficient compound film flying structure, and driving efficiency has compared to fine aluminium film flying substantially to be mentioned It rises, energy coupling efficiency is up to 47.4%.Nevertheless, the related application of Laser Driven Flyer Plates is to raising conversion efficiency and acquisition The demand of higher flyer velocity is still urgent.
Currently, hydrogen storage film obtains extensive concern as a kind of new energy material.The invention discloses one kind to be suitable for Magnesium alloy as ablation layer carries hydrogen thin-film material, under laser irradiation effect, due to introducing the quick violent of hydrogen Reaction, enhances laser induced plasma effect, causes flyer velocity and conversion efficiency to significantly improve, to Laser Driven Flyer Plates Application be of great significance.
Summary of the invention
The purpose of the present invention is to provide a kind of magnesium alloys to carry hydrogen thin-film material and preparation method thereof, existing for solving Laser and the low problem of film flying energy coupling efficiency in technology.
The present invention is solved the above problems by following technical proposals:
A kind of magnesium alloy carries hydrogen thin-film material, including magnesium alloy film, in the magnesium alloy film magnesium atom and The ratio of aluminium atom is between 9:1 to 1:9;Hydrogen atom proportion is less than or equal to 20%.Magnesium alloy carries hydrogen thin-film material Laser Driven improved efficiency principle is: metal hydrogen storage material discharges rapidly out hydrogen under light laser ablation effect, and hydrogen participates in simultaneously Enhance laser ablation reaction, so that photo plasma temperature and electron density increase, and then promotes plasma drive efficiency.
Preferably, with a thickness of nanometer scale to micron dimension.
Preferably, the magnesium alloy thin-film material has good hydrogen absorption property.
A kind of magnesium alloy carries the preparation method of hydrogen thin-film material, and described method includes following steps:
Step 1: choosing the substrate with high laser transmittance, cleaned up and be dried for standby;
Step 2: step 1 gained substrate and magnesium alloy target being put into sputtering chamber, vacuumized after installation is fixed;
Step 3: passing through magnetron sputtering magnesium alloy film.
Preferably, it cleans and includes the following steps: in the step 1
Step 1.1: substrate being cleaned by ultrasonic in acetone 15 minutes;
Step 1.2: step 1.1 gained substrate is cleaned by ultrasonic 15 minutes in dehydrated alcohol;
Step 1.3: step 1.2 gained substrate is cleaned by ultrasonic 15 minutes in deionized water;
Step 1.4: step 1.3 gained substrate is cleaned 15 minutes in plasma cleaner.
Preferably, sputtering technology in the step 3 are as follows: back end vacuum is less than 4 × 10-4Pa;Operating air pressure 0.6Pa;Sputtering Power 100W, sputtering current 325mA, sputtering voltage 310V;Argon gas and hydrogen, argon gas and hydrogen volume ratio are passed through when sputtering simultaneously For between 3:1 to 1:1.
Preferably, it is 3:1,3:2 or 1:1 that sputtering, which is the ratio for the argon gas and hydrogen being passed through,.
Preferably, the vacuum degree after vacuumizing in the step 2 is better than 4 × 10-4Pa。
Compared with prior art, the present invention have the following advantages that and the utility model has the advantages that
(1) magnesium alloy carries hydrogen film and can greatly improve Laser Driven Flyer Plates efficiency in the present invention, can be used as laser-impact The ablation layer material of piece class priming system.
(2) preparation method preparation process of the present invention is simple, low in cost, reproducible, environmental-friendly, practical, institute Material is obtained to have broad application prospects in the fields such as priming system transductive material and hydrogen storage film material.
Detailed description of the invention
The surface topography map of magnesium alloy film in the embodiment of the present invention that Fig. 1 measures for scanning electron microscope;
The energy spectrum diagram of magnesium alloy film in the embodiment of the present invention that Fig. 2 measures for scanning electron microscope;
Fig. 3 be the neutron reflection measurement data of magnesium alloy film in the embodiment of the present invention that measures of neutron reflection spectrometer, Fitting data and fitting result figure;
Fig. 4 be the neutron reflection measurement data of magnesium alloy film in the embodiment of the present invention that measures of neutron reflection spectrometer, The fitting result figure of fitting data.
Specific embodiment
The present invention is described in further detail below with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1:
A kind of magnesium alloy carries hydrogen thin-film material, including magnesium alloy film, in the magnesium alloy film magnesium atom and The ratio of aluminium atom is between 9:1 to 1:9;Hydrogen atom proportion is less than or equal to 20%;It is with a thickness of nanometer scale to micron Magnitude, and material has good hydrogen absorption property.
Above-mentioned material can be prepared via a method which that a kind of magnesium alloy carries the preparation method of hydrogen thin-film material, including such as Lower step:
Step 1: the substrate of high laser transmittance is chosen, there are commonly the substrate of the materials such as sapphire, quartz, K9 glass, The present embodiment uses quartz substrate, is cleaned up and is dried for standby, cleaning process is as follows:
Step 1.1: substrate being cleaned by ultrasonic in acetone 15 minutes;
Step 1.2: step 1.1 gained substrate is cleaned by ultrasonic 15 minutes in dehydrated alcohol;
Step 1.3: step 1.2 gained substrate is cleaned by ultrasonic 15 minutes in deionized water;
Step 1.4: step 1.3 gained substrate is cleaned 15 minutes in plasma cleaner;
Step 2: step 1 gained substrate and magnesium alloy target are put into sputtering chamber, the atomic ratio of magnalium is 1:1, It is vacuumized after installation is fixed, vacuum degree is better than 4 × 10-4Pa;
Step 3: passing through magnetron sputtering magnesium alloy film, sputtering technology are as follows: back end vacuum is less than 4 × 10-4Pa;Work gas Press 0.6Pa;Sputtering power 100W, sputtering current 325mA, sputtering voltage 310V;Argon gas and hydrogen, argon gas are passed through when sputtering simultaneously With hydrogen volume ratio between 3:1 to 1:1.
According to above-mentioned steps, a kind of magnesium alloy hydrogen storage film material, the magnalium being grown in quartz glass substrate are prepared Alloy firm:
Step 1: quartz substrate is chosen, is cleaned up and is dried for standby, cleaning process is as follows:
Step 1.1: substrate being cleaned by ultrasonic in acetone 15 minutes;
Step 1.2: step 1.1 gained substrate is cleaned by ultrasonic 15 minutes in dehydrated alcohol;
Step 1.3: step 1.2 gained substrate is cleaned by ultrasonic 15 minutes in deionized water;
Step 1.4: step 1.3 gained substrate is cleaned 15 minutes in plasma cleaner;
Step 2: step 1 gained substrate and magnesium alloy target are put into sputtering chamber, the atomic ratio of magnalium is 1:1, It is vacuumized after installation is fixed, vacuum degree is better than 4 × 10-4Pa;
Step 3: passing through magnetron sputtering magnesium alloy film, sputtering technology are as follows: back end vacuum is less than 4 × 10-4Pa;Work gas Press 0.6Pa;Sputtering power 100W, sputtering current 325mA, sputtering voltage 310V;Argon gas and hydrogen, argon gas are passed through when sputtering simultaneously It is 3:1 with hydrogen volume ratio.
Embodiment 2:
On the basis of embodiment 1, a kind of magnesium alloy hydrogen storage film material is prepared, is grown in quartz glass substrate Magnesium alloy film:
Step 1: quartz substrate is chosen, is cleaned up and is dried for standby, cleaning process is as follows:
Step 1.1: substrate being cleaned by ultrasonic in acetone 15 minutes;
Step 1.2: step 1.1 gained substrate is cleaned by ultrasonic 15 minutes in dehydrated alcohol;
Step 1.3: step 1.2 gained substrate is cleaned by ultrasonic 15 minutes in deionized water;
Step 1.4: step 1.3 gained substrate is cleaned 15 minutes in plasma cleaner;
Step 2: step 1 gained substrate and magnesium alloy target being put into sputtering chamber, vacuumized after installation is fixed, vacuum Degree is better than 4 × 10-4Pa;
Step 3: passing through magnetron sputtering magnesium alloy film, sputtering technology are as follows: back end vacuum is less than 4 × 10-4Pa;Work gas Press 0.6Pa;Sputtering power 100W, sputtering current 325mA, sputtering voltage 310V;Argon gas and hydrogen, argon gas are passed through when sputtering simultaneously It is 3:2 with hydrogen volume ratio.
Embodiment 3:
On the basis of embodiment 1, a kind of magnesium alloy hydrogen storage film material is prepared, is grown in quartz glass substrate Magnesium alloy film:
Step 1: quartz substrate is chosen, is cleaned up and is dried for standby, cleaning process is as follows:
Step 1.1: substrate being cleaned by ultrasonic in acetone 15 minutes;
Step 1.2: step 1.1 gained substrate is cleaned by ultrasonic 15 minutes in dehydrated alcohol;
Step 1.3: step 1.2 gained substrate is cleaned by ultrasonic 15 minutes in deionized water;
Step 1.4: step 1.3 gained substrate is cleaned 15 minutes in plasma cleaner;
Step 2: step 1 gained substrate and magnesium alloy target are put into sputtering chamber, the atomic ratio of magnalium is 1:1, It is vacuumized after installation is fixed, vacuum degree is better than 4 × 10-4Pa;
Step 3: passing through magnetron sputtering magnesium alloy film, sputtering technology are as follows: back end vacuum is less than 4 × 10-4Pa;Work gas Press 0.6Pa;Sputtering power 100W, sputtering current 325mA, sputtering voltage 310V;Argon gas and hydrogen, argon gas are passed through when sputtering simultaneously With hydrogen volume ratio between 3:1 to 1:1, the tantalum of one layer of 10nm thickness is finally sputtered in film surface, plays passivation, with Prevent film oxidation and liberation of hydrogen under the conditions of hydrogen storage.
The resulting film of embodiment is detected in conjunction with shown in attached drawing 1-4, can be seen that in Fig. 1, in 100,000 times of amplifications Also more uniform, it is microcosmic to show fine cracks;Fig. 2 shows mainly to have magnalium element and is attached to the protection materials tantalum on surface; Fig. 3 and Fig. 4 shows the ratio of hydrogen atom in magnesium alloy film up to 20%.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application Within scope and spirit.

Claims (9)

1. a kind of magnesium alloy carries hydrogen thin-film material, including magnesium alloy film, it is characterised in that: in the magnesium alloy film The ratio of magnesium atom and aluminium atom is between 9:1 to 1:9;Hydrogen atom proportion is less than or equal to 20%.
2. magnesium alloy according to claim 1 carries hydrogen thin-film material, it is characterised in that: it is with a thickness of nanometer scale to micro- Rice magnitude.
3. magnesium alloy according to claim 1 carries hydrogen thin-film material, it is characterised in that: the magnesium alloy thin-film material With good hydrogen absorption property.
4. the preparation method that a kind of magnesium alloy carries hydrogen thin-film material, which is characterized in that described method includes following steps:
Step 1: choosing the substrate with high laser transmittance, cleaned up and be dried for standby;
Step 2: step 1 gained substrate and magnesium alloy target being put into sputtering chamber, vacuumized after installation is fixed;
Step 3: passing through magnetron sputtering magnesium alloy film.
5. the preparation method that magnesium alloy according to claim 4 carries hydrogen thin-film material, which is characterized in that the step 1 Middle cleaning includes the following steps:
Step 1.1: substrate being cleaned by ultrasonic in acetone 15 minutes;
Step 1.2: step 1.1 gained substrate is cleaned by ultrasonic 15 minutes in dehydrated alcohol;
Step 1.3: step 1.2 gained substrate is cleaned by ultrasonic 15 minutes in deionized water;
Step 1.4: step 1.3 gained substrate is cleaned 15 minutes in plasma cleaner.
6. the preparation method that magnesium alloy according to claim 4 carries hydrogen thin-film material, which is characterized in that the step 3 Middle sputtering technology are as follows: back end vacuum is less than 4 × 10-4Pa;Operating air pressure 0.6Pa;Sputtering power 100W, sputtering current 325mA, splashes Radio presses 310V;Argon gas and hydrogen are passed through simultaneously when sputtering, and the volume ratio of argon gas and hydrogen is between 3:1 to 1:1.
7. the preparation method that magnesium alloy according to claim 4 carries hydrogen thin-film material, which is characterized in that sputtering is to be passed through Argon gas and hydrogen ratio be 3:1,3:2 or 1:1.
8. the preparation method that magnesium alloy according to claim 4 carries hydrogen thin-film material, which is characterized in that the step 2 In vacuumize after vacuum degree better than 4 × 10-4Pa。
9. the preparation method that magnesium alloy according to claim 4 carries hydrogen thin-film material, which is characterized in that the step 3 Magnesium alloy thin film sputtering sputters the tantalum of one layer of 10nm thickness above it after completing.
CN201910152281.5A 2019-02-28 2019-02-28 Magnesium-aluminum alloy hydrogen-carrying thin film material and preparation method thereof Active CN109680254B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112930018A (en) * 2021-01-26 2021-06-08 中科超睿(青岛)技术有限公司 Magnesium-containing neutron target based on multi-principal-element design and preparation method thereof

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CN112930018A (en) * 2021-01-26 2021-06-08 中科超睿(青岛)技术有限公司 Magnesium-containing neutron target based on multi-principal-element design and preparation method thereof

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