CN109680254B - Magnesium-aluminum alloy hydrogen-carrying thin film material and preparation method thereof - Google Patents

Magnesium-aluminum alloy hydrogen-carrying thin film material and preparation method thereof Download PDF

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CN109680254B
CN109680254B CN201910152281.5A CN201910152281A CN109680254B CN 109680254 B CN109680254 B CN 109680254B CN 201910152281 A CN201910152281 A CN 201910152281A CN 109680254 B CN109680254 B CN 109680254B
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aluminum alloy
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film material
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CN109680254A (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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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3457—Sputtering using other particles than noble gas ions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible 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
    • C01B3/001—Reversible 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
    • C01B3/0031—Intermetallic compounds; Metal alloys; Treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F42—AMMUNITION; BLASTING
    • F42C—AMMUNITION FUZES; ARMING OR SAFETY MEANS THEREFOR
    • F42C19/00—Details of fuzes
    • F42C19/08—Primers; Detonators
    • 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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Abstract

The invention discloses a magnesium-aluminum alloy hydrogen-carrying film material which comprises a magnesium-aluminum alloy film, wherein the ratio of magnesium atoms to aluminum atoms in the magnesium-aluminum alloy film is 9:1 to 1: 9; the proportion of hydrogen atoms is less than or equal to 20 percent. The principle of improving the laser driving efficiency of the magnesium-aluminum alloy hydrogen-carrying thin film material is as follows: the metal hydrogen storage material can rapidly release hydrogen under the action of strong laser ablation, and the hydrogen participates in and enhances the laser ablation reaction, so that the temperature and the electron density of the photoinduced plasma are increased, and the driving efficiency of the plasma is further improved. The preparation method comprises the following steps of 1: selecting a substrate with high laser transmittance, cleaning and drying the substrate for later use; step 2: putting the substrate obtained in the step (1) and a magnesium-aluminum alloy target material into a sputtering chamber, and vacuumizing after mounting and fixing; and step 3: the magnesium-aluminum alloy film is sputtered by magnetron sputtering.

Description

Magnesium-aluminum alloy hydrogen-carrying thin film material and preparation method thereof
Technical Field
The invention relates to the technical field of hydrogen-carrying films, in particular to a magnesium-aluminum alloy hydrogen-carrying film material and a preparation method thereof.
Background
With the networking and informatization of modern war, the electromagnetic compatibility environment inside the battlefield and weapon system in the future is bound to be more complex and harsh. The initiating explosive device, as a functional initiating element of the weapon system, determines the intrinsic safety of the ammunition.For this reason, LosAlamos, Sandia, equal to the beginning of the 80 th century, applied the laser-driven flyer technology with strong electromagnetic interference resistance to the initiation of explosives. The development of the laser-driven flyer technology has achieved a lot of remarkable results so far, however, many key problems still remain to be studied deeply, and what is more prominent is the problem of low energy coupling efficiency of laser and flyer. Flyers have been widely studied as a key to solving the problem of energy coupling efficiency. In the early stage, the flyer mainly adopts a single-layer metal film, and the energy coupling efficiency is less than 20%; in recent years, flyer sheets have adopted a composite structure including an absorption layer, an ablation layer, a thermal insulation layer, and a flyer layer. In the composite flyer, the absorption layer mainly plays a role in enhancing the laser absorptivity, and is usually C or Ti; the ablation layer is an energy conversion layer, is usually made of metal materials such as Al, Ge, Cu and the like, and forms high-pressure plasma under the excitation of laser so as to shear the material of the flyer layer and enable the flyer layer to obtain high-speed impact detonating explosive; the primary function of the thermal barrier layer is to reduce the energy loss of the ablative layer, typically Al2O3CuO, and the like. C/Al2O3the/Al is the most commonly used and efficient composite flyer structure at present, the driving efficiency of the composite flyer structure is greatly improved compared with that of a pure aluminum flyer, and the energy coupling efficiency can reach 47.4%. Nevertheless, the related application of laser driven flyers still requires increased transduction efficiency and higher flyer velocity.
At present, hydrogen storage films are widely spotlighted as a new energy material. The invention discloses a magnesium-aluminum alloy hydrogen-carrying film material suitable for serving as an ablation layer, which is characterized in that under the action of laser irradiation, the rapid and violent reaction of hydrogen is introduced, so that the laser-induced plasma effect is enhanced, the speed and the energy conversion efficiency of a flyer are obviously improved, and the magnesium-aluminum alloy hydrogen-carrying film material has important significance for the application of laser-driven flyers.
Disclosure of Invention
The invention aims to provide a magnesium-aluminum alloy hydrogen-carrying thin film material and a preparation method thereof, which are used for solving the problem of low energy coupling efficiency of laser and flyer in the prior art.
The invention solves the problems through the following technical scheme:
a magnesium-aluminum alloy hydrogen-carrying film material comprises a magnesium-aluminum alloy film, wherein the ratio of magnesium atoms to aluminum atoms in the magnesium-aluminum alloy film is 9:1 to 1: 9; the proportion of hydrogen atoms is less than or equal to 20 percent. The principle of improving the laser driving efficiency of the magnesium-aluminum alloy hydrogen-carrying thin film material is as follows: the metal hydrogen storage material can rapidly release hydrogen under the action of strong laser ablation, and the hydrogen participates in and enhances the laser ablation reaction, so that the temperature and the electron density of the photoinduced plasma are increased, and the driving efficiency of the plasma is further improved.
Preferably, the thickness is on the order of nanometers to micrometers.
Preferably, the magnesium aluminum alloy thin film material has good hydrogen adsorption performance.
A preparation method of a magnesium-aluminum alloy hydrogen-carrying film material comprises the following steps:
step 1: selecting a substrate with high laser transmittance, cleaning and drying the substrate for later use;
step 2: putting the substrate obtained in the step (1) and a magnesium-aluminum alloy target material into a sputtering chamber, and vacuumizing after mounting and fixing;
and step 3: the magnesium-aluminum alloy film is sputtered by magnetron sputtering.
Preferably, the step 1 of washing comprises the following steps:
step 1.1: ultrasonically cleaning the substrate in acetone for 15 minutes;
step 1.2: ultrasonically cleaning the substrate obtained in the step 1.1 in absolute ethyl alcohol for 15 minutes;
step 1.3: ultrasonically cleaning the substrate obtained in the step 1.2 in deionized water for 15 minutes;
step 1.4: and (4) cleaning the substrate obtained in the step 1.3 in a plasma cleaner for 15 minutes.
Preferably, the sputtering process in step 3 is as follows: vacuum of the back bottom is less than 4 x 10-4Pa; the working air pressure is 0.6 Pa; the sputtering power is 100W, the sputtering current is 325mA, and the sputtering voltage is 310V; argon and hydrogen are simultaneously introduced during sputtering, and the volume ratio of the argon to the hydrogen is 3:1 to 1: 1.
Preferably, the sputtering is carried out with argon and hydrogen in a ratio of 3:1, 3:2 or 1: 1.
Preferably, the vacuum degree after the vacuum pumping in the step 2 is better than 4 multiplied by 10-4Pa。
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the magnesium-aluminum alloy hydrogen-carrying film can greatly improve the efficiency of laser driving flyer and can be used as an ablation layer material of a laser shock piece initiating explosive device.
(2) The preparation method disclosed by the invention is simple in preparation process, low in cost, good in repeatability, environment-friendly and strong in practicability, and the obtained material has a wide application prospect in the fields of initiating explosive device transduction materials, hydrogen storage thin film materials and the like.
Drawings
FIG. 1 is a surface topography map of a magnesium-aluminum alloy film in an embodiment of the invention measured by a scanning electron microscope;
FIG. 2 is a graph of an energy spectrum of a magnesium aluminum alloy thin film in an embodiment of the invention measured by a scanning electron microscope;
FIG. 3 is a graph of neutron reflection measurement data, fitting data and fitting results of the magnesium-aluminum alloy thin film in the embodiment of the invention measured by a neutron reflection spectrometer;
fig. 4 is a graph of fitting results of neutron reflection measurement data and fitting data of the magnesium-aluminum alloy thin film in the embodiment of the invention measured by a neutron reflection spectrometer.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
a magnesium-aluminum alloy hydrogen-carrying film material comprises a magnesium-aluminum alloy film, wherein the ratio of magnesium atoms to aluminum atoms in the magnesium-aluminum alloy film is 9:1 to 1: 9; the proportion of hydrogen atoms is less than or equal to 20 percent; the thickness of the material is nano-scale to micron-scale, and the material has good hydrogen adsorption performance.
The material can be prepared by the following method, and the preparation method of the magnesium-aluminum alloy hydrogen-carrying film material comprises the following steps:
step 1: the method comprises the following steps of selecting a substrate with high laser transmittance, wherein the substrate is made of materials such as sapphire, quartz, K9 glass and the like, the quartz substrate is adopted in the embodiment, the substrate is cleaned and dried for later use, and the cleaning process is as follows:
step 1.1: ultrasonically cleaning the substrate in acetone for 15 minutes;
step 1.2: ultrasonically cleaning the substrate obtained in the step 1.1 in absolute ethyl alcohol for 15 minutes;
step 1.3: ultrasonically cleaning the substrate obtained in the step 1.2 in deionized water for 15 minutes;
step 1.4: cleaning the substrate obtained in the step 1.3 in a plasma cleaning machine for 15 minutes;
step 2: putting the substrate obtained in the step 1 and a magnesium-aluminum alloy target material into a sputtering chamber, wherein the atomic ratio of magnesium to aluminum is 1:1, and vacuumizing after mounting and fixing, wherein the vacuum degree is better than 4 multiplied by 10-4Pa；
And step 3: the magnesium-aluminum alloy film is sputtered by magnetron sputtering, and the sputtering process comprises the following steps: vacuum of the back bottom is less than 4 x 10-4Pa; the working air pressure is 0.6 Pa; the sputtering power is 100W, the sputtering current is 325mA, and the sputtering voltage is 310V; argon and hydrogen are simultaneously introduced during sputtering, and the volume ratio of the argon to the hydrogen is 3:1 to 1: 1.
Preparing a magnesium-aluminum alloy hydrogen storage film material according to the steps, wherein a magnesium-aluminum alloy film growing on a quartz glass substrate comprises the following steps:
step 1: selecting a quartz substrate, cleaning and drying the quartz substrate for later use, wherein the cleaning process comprises the following steps:
step 1.1: ultrasonically cleaning the substrate in acetone for 15 minutes;
step 1.2: ultrasonically cleaning the substrate obtained in the step 1.1 in absolute ethyl alcohol for 15 minutes;
step 1.3: ultrasonically cleaning the substrate obtained in the step 1.2 in deionized water for 15 minutes;
step 1.4: cleaning the substrate obtained in the step 1.3 in a plasma cleaning machine for 15 minutes;
step 2: putting the substrate obtained in the step 1 and a magnesium-aluminum alloy target material into a sputtering chamber, wherein the atomic ratio of magnesium to aluminum is 1:1, and vacuumizing after mounting and fixing, wherein the vacuum degree is better than 4 multiplied by 10-4Pa；
And step 3: the magnesium-aluminum alloy film is sputtered by magnetron sputtering, and the sputtering process comprises the following steps: vacuum of the back bottom is less than 4 x 10-4Pa; the working air pressure is 0.6 Pa; the sputtering power is 100W, the sputtering current is 325mA, and the sputtering voltage is 310V; argon and hydrogen are simultaneously introduced during sputtering, and the volume ratio of the argon to the hydrogen is 3: 1.
Example 2:
on the basis of example 1, a magnesium-aluminum alloy hydrogen storage film material is prepared, a magnesium-aluminum alloy film grown on a quartz glass substrate:
step 1: selecting a quartz substrate, cleaning and drying the quartz substrate for later use, wherein the cleaning process comprises the following steps:
step 1.1: ultrasonically cleaning the substrate in acetone for 15 minutes;
step 1.2: ultrasonically cleaning the substrate obtained in the step 1.1 in absolute ethyl alcohol for 15 minutes;
step 1.3: ultrasonically cleaning the substrate obtained in the step 1.2 in deionized water for 15 minutes;
step 1.4: cleaning the substrate obtained in the step 1.3 in a plasma cleaning machine for 15 minutes;
step 2: putting the substrate obtained in the step 1 and a magnesium-aluminum alloy target material into a sputtering chamber, installing and fixing the substrate and then vacuumizing the chamber, wherein the vacuum degree is better than 4 multiplied by 10-4Pa；
And step 3: the magnesium-aluminum alloy film is sputtered by magnetron sputtering, and the sputtering process comprises the following steps: vacuum of the back bottom is less than 4 x 10-4Pa; the working air pressure is 0.6 Pa; the sputtering power is 100W, the sputtering current is 325mA, and the sputtering voltage is 310V; argon and hydrogen are simultaneously introduced during sputtering, and the volume ratio of the argon to the hydrogen is 3: 2.
Example 3:
on the basis of example 1, a magnesium-aluminum alloy hydrogen storage film material is prepared, a magnesium-aluminum alloy film grown on a quartz glass substrate:
step 1: selecting a quartz substrate, cleaning and drying the quartz substrate for later use, wherein the cleaning process comprises the following steps:
step 1.1: ultrasonically cleaning the substrate in acetone for 15 minutes;
step 1.2: ultrasonically cleaning the substrate obtained in the step 1.1 in absolute ethyl alcohol for 15 minutes;
step 1.3: ultrasonically cleaning the substrate obtained in the step 1.2 in deionized water for 15 minutes;
step 1.4: cleaning the substrate obtained in the step 1.3 in a plasma cleaning machine for 15 minutes;
step 2: putting the substrate obtained in the step 1 and a magnesium-aluminum alloy target material into a sputtering chamber, wherein the atomic ratio of magnesium to aluminum is 1:1, and vacuumizing after mounting and fixing, wherein the vacuum degree is better than 4 multiplied by 10-4Pa；
And step 3: the magnesium-aluminum alloy film is sputtered by magnetron sputtering, and the sputtering process comprises the following steps: vacuum of the back bottom is less than 4 x 10-4Pa; the working air pressure is 0.6 Pa; the sputtering power is 100W, the sputtering current is 325mA, and the sputtering voltage is 310V; and during sputtering, simultaneously introducing argon and hydrogen, wherein the volume ratio of the argon to the hydrogen is 3:1 to 1:1, and finally sputtering a layer of tantalum with the thickness of 10nm on the surface of the film to play a passivation role so as to prevent the film from being oxidized and hydrogen from being separated out under the hydrogen storage condition.
The films obtained in the examples are detected by combining the drawings of fig. 1-4, and as can be seen in fig. 1, the films are relatively uniform under the magnification of 10 ten thousand times, and microscopically show fine cracks; FIG. 2 shows the predominance of elemental magnesium and aluminum with the protective material tantalum adhered to the surface; fig. 3 and 4 show that the proportion of hydrogen atoms in the magnesium-aluminum alloy film reaches 20%.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.

Claims (6)

1. A magnesium-aluminum alloy hydrogen-carrying film material comprises a magnesium-aluminum alloy film, and is characterized in that: the ratio of magnesium atoms to aluminum atoms in the magnesium-aluminum alloy film is 9:1 to 1: 9; the hydrogen atom accounts for less than or equal to 20 percent, and the thickness is from nanometer magnitude to micrometer magnitude;
the preparation method of the magnesium-aluminum alloy hydrogen-carrying film material comprises the following steps:
step 1: selecting a substrate with high laser transmittance, cleaning and drying the substrate for later use;
step 2: putting the substrate obtained in the step (1) and a magnesium-aluminum alloy target material into a sputtering chamber, and vacuumizing after mounting and fixing;
and step 3: carrying out magnetron sputtering on a magnesium-aluminum alloy film;
the sputtering process in the step 3 comprises the following steps: vacuum of the back bottom is less than 4 x 10-4Pa; the working air pressure is 0.6 Pa; the sputtering power is 100W, the sputtering current is 325mA, and the sputtering voltage is 310V; argon and hydrogen are simultaneously introduced during sputtering, and the volume ratio of the argon to the hydrogen is 3:1 to 1: 1.
2. The magnesium aluminum alloy hydrogen-carrying thin film material as claimed in claim 1, wherein: the magnesium-aluminum alloy thin film material has good hydrogen adsorption performance.
3. The magnesium aluminum alloy hydrogen-carrying thin film material as claimed in claim 1, wherein the step 1 of cleaning comprises the following steps:
step 1.1: ultrasonically cleaning the substrate in acetone for 15 minutes;
step 1.2: ultrasonically cleaning the substrate obtained in the step 1.1 in absolute ethyl alcohol for 15 minutes;
step 1.3: ultrasonically cleaning the substrate obtained in the step 1.2 in deionized water for 15 minutes;
step 1.4: and (4) cleaning the substrate obtained in the step 1.3 in a plasma cleaner for 15 minutes.
4. The magnesium aluminum alloy hydrogen-carrying thin film material as claimed in claim 1, wherein the ratio of argon gas and hydrogen gas introduced in sputtering is 3:1, 3:2 or 1: 1.
5. The magnesium-aluminum alloy hydrogen-carrying thin film material as claimed in claim 1, wherein the degree of vacuum after the vacuum pumping in the step 2 is better than 4 x 10-4Pa。
6. The magnesium aluminum alloy hydrogen-carrying thin film material as claimed in claim 1, wherein the step 3 is to sputter a layer of tantalum with a thickness of 10nm on the magnesium aluminum alloy thin film after the sputtering is completed.
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