AU2021102207A4 - Magnesium nanowire film, and preparation method and use thereof - Google Patents
Magnesium nanowire film, and preparation method and use thereof Download PDFInfo
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- 239000011777 magnesium Substances 0.000 title claims abstract description 162
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 137
- 239000002070 nanowire Substances 0.000 title claims abstract description 128
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000000758 substrate Substances 0.000 claims abstract description 70
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 55
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000003860 storage Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000011343 solid material Substances 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000013077 target material Substances 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 84
- 238000009792 diffusion process Methods 0.000 abstract description 12
- 239000010409 thin film Substances 0.000 abstract description 12
- 238000005137 deposition process Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 16
- 238000004626 scanning electron microscopy Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000004544 sputter deposition Methods 0.000 description 7
- 125000004429 atom Chemical group 0.000 description 6
- 238000004088 simulation Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 241000566146 Asio Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005274 electronic transitions Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3402—Gas-filled discharge tubes operating with cathodic sputtering using supplementary magnetic fields
- H01J37/3405—Magnetron sputtering
- H01J37/3408—Planar magnetron sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B3/0026—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 of one single metal or a rare earth metal; Treatment thereof
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
Abstract
The present disclosure relates to the technical field of metal thin films and
provides a method for preparing a magnesium nanowire film. In the present
disclosure, the morphology of the magnesium nanowire film is controlled by
controlling an inclination angle and a temperature of a substrate. When the
magnetron sputtering is conducted at an inclination angle of 600 < a < 890 relative
to the substrate, namely, oblique incidence, during the deposition process, the
diffusion of magnesium atoms occurs in the direction of the projection of the
magnetron sputtering beam on the surface of a film, and the diffusion in the
direction parallel to the surface of the film is only determined by the incidence
angle, which allows growing magnesium nanowires to have a uniform diameter and
a uniform distribution. When the substrate has a temperature of 250 C to 1000 C,
well-separated magnesium nanowires can be obtained. Experimental results show
that, when the substrate has a temperature of 250 C and an inclination angle of 850,
magnesium nanowires in an obtained magnesium nanowire film are well dispersed
and have a diameter of 25 nm to 50 nm, which can be used as a solid material for
hydrogen storage.
1/5
FIG. 1
FIG. 2
FIG. 3
Description
1/5
FIG. 1
FIG. 2
FIG. 3
The present disclosure relates to the technical field of metal thin films, and in
particular to a magnesium nanowire film, and a preparation method and use
thereof.
With the aggravation of global warming and the increase of fossil fuel
consumption, traditional fuels are gradually replaced by renewable energy sources
such as hydropower, solar power, and wind power. Compared with fossil fuels,
hydrogen has higher chemical energy, which leads to an exhaust gas of water
vapor in a fuel cell, without any other greenhouse gases or harmful emissions.
Therefore, compared with traditional fuels, hydrogen has huge application
potential. However, before hydrogen can be used as an economical and feasible
fuel, it is necessary to solve the problems of hydrogen production, distribution and
storage, especially the problem of hydrogen storage. Since solid materials have a
higher bulk density and are safer than gases or liquids, solid materials are often
used to store hydrogen, thus solving the problem of hydrogen storage.
Among the solid materials for hydrogen storage, magnesium has the
characteristics of abundance, low cost, low density, low toxicity, high hydrogen
storage capacity, and reversibility, which allows magnesium to be a
commonly-used solid material for hydrogen storage. However, this material has
the defects of high desorption temperature, low hydrogen absorption power, and
easy oxidization of magnesium by oxygen, making it difficult for hydrogen to
diffuse in the material. Over the years, various studies have been devoted to
solving the above-mentioned problems. For example, in Energy Rev. 2017, 72,
523-534, the size of Mg/MgH 2 (less than 1 pm) particles was reduced by
mechanical ball milling in the presence (or absence) of a catalyst material, thereby
significantly improving the adsorption kinetics of the solid material. However, the
Mg/MgH 2 particles obtained by this method still have a relatively-large size, which
can only improve the adsorption kinetics of the solid material, but not the
thermodynamic parameters. Therefore, it is necessary to obtain Mg/MgH 2 particles
with a smaller size to simultaneously solve the problems of high desorption
temperature, low hydrogen absorption power, and easy oxidation of magnesium by
oxygen existing in a magnesium material for hydrogen storage.
The present disclosure is intended to provide a magnesium nanowire film, and
a preparation method and use thereof. In the magnesium nanowire film prepared
by the present disclosure, magnesium nanowires have a small size, with a
diameter of 25 nm to 50 nm.
To achieve the objective of the present disclosure, the present disclosure
provides the following technical solutions.
The present disclosure provides a method for preparing a magnesium nanowire
film, including: using magnetron sputtering to deposit the magnesium nanowire
film on a substrate, where,
a target material for the magnetron sputtering is an Mg target;
there is a distance of 60 mm to 80 mm between the Mg target and the
substrate;
the magnetron sputtering is conducted under the protection of argon;
during the magnetron sputtering, the substrate has a temperature of 250 C to
100°C; and
during the magnetron sputtering, the substrate has an inclination angle of
600< a < 890.
Preferably, the substrate may include a conductive silicon wafer, aSiO 2 wafer, or an A 20 3 wafer.
Preferably, the Mg target may have a purity of 99.99 wt% or more.
Preferably, during the magnetron sputtering, the substrate may have a
temperature of 250 C to 800 C.
Preferably, the magnetron sputtering may be conducted at power of 20 W
tolo W.
Preferably, the magnetron sputtering may be conducted at a working voltage of
0.13 Pa to 1.3 Pa.
Preferably, the magnetron sputtering may be conducted for 10 min to 60 min.
The present disclosure also provides a magnesium nanowire film prepared by
the preparation method according to the above technical solution, and magnesium
nanowires in the magnesium nanowire film have a diameter of 20 nm to 100 nm.
The present disclosure also provides use of the magnesium nanowire film
according to the above technical solution as a solid material for hydrogen storage.
The present disclosure provides a method for preparing a magnesium nanowire
film. In the present disclosure, magnetron sputtering is used to deposit the
magnesium nanowire film on a substrate, where, a target material for the
magnetron sputtering is defined as a Mg target; there is a distance of 60 mm to 80
mm between the Mg target and the substrate; the magnetron sputtering is
conducted under the protection of argon; during the magnetron sputtering, the
substrate has a temperature of 250 C to 100°C; and during the magnetron
sputtering, the substrate has an inclination angle of 600< a < 890. In the present
disclosure, during the magnetron sputtering, the morphology of the magnesium
nanowire film is controlled by controlling an inclination angle and a temperature of
a substrate. When the magnetron sputtering is conducted at an inclination angle of
600 < a < 890 relative to the substrate, namely, oblique incidence, during the deposition process, the diffusion of magnesium atoms occurs in the direction of the projection of the magnetron sputtering beam on the surface of a film, and the diffusion in the direction parallel to the surface of the film is only determined by the incidence angle, which allows growing magnesium nanowires to have a uniform diameter and a uniform distribution. When the substrate has a temperature of
0 C to 100 0 C, well-separated magnesium nanowires can be obtained.
Experimental results show that, when the substrate has a temperature of 250 C and
an inclination angle of 850, magnesium nanowires in an obtained magnesium
nanowire film are well dispersed and have a diameter of 25 nm, which can be used
as a solid material for hydrogen storage.
FIG. 1 is a scanning electron microscopy (SEM) image of the magnesium
nanowire film prepared in Example 1 of the present disclosure;
FIG. 2 is an SEM image of the magnesium nanowire film prepared in Example
2 of the present disclosure;
FIG. 3 is an SEM image of the magnesium nanowire film prepared in Example
3 of the present disclosure;
FIG. 4 is an SEM image of the magnesium nanowire film prepared in Example
4 of the present disclosure;
FIG. 5 is an SEM image of the magnesium nanowire film prepared in Example
of the present disclosure;
FIG. 6 is an SEM image of the magnesium nanowire film prepared in
Comparative Example 1 of the present disclosure;
FIG. 7 illustrates the growth simulation of the magnesium nanowire film
prepared in Example 6 of the present disclosure;
FIG. 8 is an X-ray photoelectron spectroscopy (XPS) spectrum of the
magnesium nanowire film prepared in Example 6 of the present disclosure;
FIG. 9 shows SEM images of the magnesium nanowire films prepared in
Examples 7 to 13 of the present disclosure;
FIG. 10 shows kMC simulation results for the influence of the deposition angle
a of the magnesium nanowire films prepared in Examples 7 to 13 of the present
disclosure on the inclination angle P of the magnesium nanowires;
FIG. 11 shows SEM images of the magnesium nanowire films prepared in
Examples 14 to 17 of the present disclosure; and
FIG. 12 shows the Monte Carlo kinetic simulation for the magnesium nanowire
films prepared in Examples 14 to 17 of the present disclosure.
The present disclosure provides a method for preparing a magnesium nanowire
film, including: using magnetron sputtering to deposit the magnesium nanowire
film on a substrate, where,
a target material for the magnetron sputtering is an Mg target;
there is a distance of 60 mm to 80 mm between the Mg target and the
substrate;
the magnetron sputtering is conducted under the protection of argon;
during the magnetron sputtering, the substrate has a temperature of 250 C to
100 °C; and
during the magnetron sputtering, the substrate has an inclination angle of
600< a < 890.
The present disclosure adopts magnetron sputtering to deposit a magnesium
nanowire film on a substrate. The present disclosure has no specific limitations on
a device for the magnetron sputtering, and a magnetron sputtering device well
known to those skilled in the art may be adopted. In the present disclosure, a
device for the magnetron sputtering may preferably be a cylindrical stainless steel
reaction chamber.
In the present disclosure, a target material for the magnetron sputtering is an
Mg target. In the present disclosure, the Mg target may have a purity preferably of
99.99 wt% or more and more preferably of 99.999 wt% or more. In the present
disclosure, when the Mg target has a purity in the above range, it is more conducive
to obtaining a magnesium nanowire film with high purity.
The present disclosure has no specific limitations on a size of the Mg target, and
the size can be adjusted according to an actual situation. In the present disclosure,
the Mg target may have a size preferably of 2 inches in diameter and 0.25 inch in
thickness.
In the present disclosure, there is a distance preferably of 60 mm to 80 mm,
more preferably of 75 mm to 80 mm, and most preferably of 80 mm between the
Mg target and the substrate. In the present disclosure, a distance between the Mg
target and the substrate affects a carrier concentration and mobility. When a
distance between the Mg target and the substrate is in the above range, it is more
conducive to obtaining a magnesium nanowire film with high quality.
In the present disclosure, the substrate may preferably include a
single-side-polished conductive silicon wafer (100), an A 20 3 wafer, or aSiO 2 wafer.
The present disclosure has no specific limitations on a source of the substrate, and
a commercially available product well known to those skilled in the art may be
adopted.
In the present disclosure, the substrate may preferably be cleaned before
magnetron sputtering. The present disclosure has no specific limitations on a
method for the cleaning, and a cleaning method well known to those skilled in the
art may be adopted. In the present disclosure, an agent reagent for the cleaning
may preferably be ultrapure water (UPW). In the present disclosure, the cleaning is
conducted to remove impurities on the surface of the substrate.
In the present disclosure, before magnetron sputtering, a vacuum degree in the reaction chamber may be adjusted preferably to 1.6 x 10-4 to 1.6 x 10-6 Pa, and more preferably to 1.6 x 10-5 to 1.6 x 10-6 Pa. In the present disclosure, when the vacuum degree during the magnetron sputtering is in the above range, air in the reaction chamber can be removed.
The present disclosure has no specific limitations on a device for adjusting the
vacuum degree during magnetron sputtering, and a device for adjusting the
vacuum degree well known to those skilled in the art may be adopted. In the
present disclosure, the device for adjusting the vacuum degree may preferably be
a turbomolecular pump (TMP).
In the present disclosure, the magnetron sputtering is conducted under the
protection of argon. The present disclosure adopts argon as a working gas, which
can prevent the oxidation of magnesium during magnetron sputtering. The present
disclosure has no specific limitations on a flow rate of the argon, and the flow rate
can be adjusted according to an actual experimental process.
In the present disclosure, during the magnetron sputtering, the substrate has
a temperature of 25 0 C to 100 0 C and preferably of 25 0C to 80 0 C. In the present
disclosure, during the magnetron sputtering, the temperature of the substrate
determines a diameter of magnesium nanowires in the magnesium nanowire film.
When the temperature of the substrate is in the above range during the magnetron
sputtering, it can ensure that the magnesium nanowires in the magnesium
nanowire film have a diameter of 25 nm to 100 nm.
In the present disclosure, during the magnetron sputtering, the substrate may
have an inclination angle of 600< a < 890 and preferably of 650 < a < 850. In the
present disclosure, during the sputtering process, a glancing angle deposition
(GLAD) system is used to control the inclination angle of the substrate. When the
inclination angle of the substrate is in the above range, it can ensure that the
magnesium nanowires in the magnesium nanowire film have a diameter of 25 nm to 100 nm.
In the present disclosure, the magnetron sputtering may be conducted at a
working voltage preferably of 0.13 Pa to 1.3 Pa and more preferably of 0.2 Pa to
0.26 Pa. In the present disclosure, when the magnetron sputtering is conducted at
a working voltage in the above range, the morphology of magnesium nanowires in
the magnesium nanowire film can be further controlled.
In the present disclosure, the magnetron sputtering may be conducted at
power preferably of 20 W to 100 W, more preferably of 30 W to 50 W, and most
preferably of 50 W. In the present disclosure, when the magnetron sputtering is
conducted at power in the above range, the morphology of magnesium nanowires
in the magnesium nanowire film can be further controlled.
In the present disclosure, the magnetron sputtering may be conducted
preferably for 10 min to 60 min and more preferably for 15 min to 30 min. In the
present disclosure, when the magnetron sputtering is conducted for a time period
in the above range, the morphology of magnesium nanowires in the magnesium
nanowire film can be further controlled.
The present disclosure uses magnetron sputtering to deposit a nanostructured
magnesium thin film on a substrate and controls the morphology of the magnesium
nanowire film by controlling an inclination angle and a temperature of the substrate
during magnetron sputtering, so that magnesium nanowires are well dispersed in
the magnesium nanowire film and can have a size much lower than that of
magnesium nanowires in the prior art.
The present disclosure also provides a magnesium nanowire film prepared by
the preparation method according to the above technical solution, and magnesium
nanowires in the magnesium nanowire film have a diameter of 25 nm to 100 nm.
The magnesium nanowires in the magnesium nanowire film provided by the
present disclosure may have a diameter of 25 nm to 100 nm and are well dispersed in the magnesium nanowire film.
The present disclosure also provides use of the magnesium nanowire film
according to the above technical solution as a solid material for hydrogen storage.
The present disclosure has no specific limitations on a method for the use of the
magnesium nanowire film as a solid material for hydrogen storage, and a use
method as a solid material for hydrogen storage well known to those skilled in the
art may be adopted.
The technical solutions of the present disclosure will be clearly and completely
described below with reference to examples of the present disclosure. Apparently,
the described examples are merely some rather than all of the examples of the
present disclosure. All other examples obtained by a person of ordinary skill in the
art based on the examples of the present disclosure without creative efforts shall
fall within the protection scope of the present disclosure.
Example 1
This experiment was conducted in a cylindrical stainless steel reaction chamber
(height: 60 cm and diameter: 42 cm). The reaction chamber was evacuated by a
TMP, and a magnetron cathode was installed on the top of the reaction chamber. An
Mg target (purity: 99.99 wt%) with a diameter of 2 inches and a thickness of 0.25
inches was used. A conductive silicon wafer (100) was used as a substrate, and the
substrate was located at 80 mm below the Mg target. A GLAD system was used to
control an inclination angle of the substrate, and the inclination angle a was
controlled at 85 0 C. The substrate was cleaned with UPW before deposition.
The magnesium target was sputtered in a direct current mode at an argon
atmosphere. During the sputtering process, magnetron sputtering was conducted
under the following conditions to obtain a magnesium nanowire film: power: 50 W;
voltage: 0.26 Pa; time: 20 min; vacuum degree: 1.6 x 10-5 Pa; and substrate
temperature: 250 C.
The magnesium nanowire film prepared in Example 1 was scanned with SEM to
obtain an SEM image shown in FIG. 1. It can be seen from FIG. 1 that, when the
substrate has a temperature of 250 C and an inclination angle a of 850, magnesium
nanowires in an obtained magnesium nanowire film have an inclination angle of
220 and a diameter of 25 nm to 50 nm, and the magnesium nanowires are well
separated.
Example 2
The operations in this example were the same as example 1 except that the
substrate had a temperature of 400C.
The magnesium nanowire film prepared in Example 2 was scanned with SEM to
obtain an SEM image shown in FIG. 2. It can be seen from FIG. 2 that, when the
substrate has a temperature of 400 C and an inclination angle a of 850, magnesium
nanowires in an obtained magnesium nanowire film have an inclination angle of
220 and a diameter of 45 nm to 65 nm, and the magnesium nanowires are well
separated. Compared with nanowires prepared at 25 0 C, the nanowires have a
reduced inclination angle due to the increase in the substrate temperature and the
enhancement in atomic diffusion.
Example 3
The operations in this example were the same as example 1 except that the
substrate had a temperature of 600 C.
The magnesium nanowire film prepared in Example 3 was scanned with SEM to
obtain an SEM image shown in FIG. 3. It can be seen from FIG. 3 that, when the
substrate has a temperature of 600 C and an inclination angle a of 850, magnesium
nanowires in an obtained magnesium nanowire film have an inclination angle of
210 and a diameter of 60 nm to 75 nm, and the magnesium nanowires are well
separated. It can be known that the width of the nanowires is slightly increased,
and as the substrate temperature increases, the atomic diffusion continues to increase. Example 4 The operations in this example were the same as example 1 except that the substrate had a temperature of 800 C. The magnesium nanowire film prepared in Example 4 was scanned with SEM to obtain an SEM image shown in FIG. 4. It can be seen from FIG. 4 that, when the substrate has a temperature of 800 C and an inclination angle a of 850, magnesium nanowires in an obtained magnesium nanowire film have an inclination angle of 210 and a diameter of 65 nm to 100 nm, and the magnesium nanowires are well separated. The diameter of the nanowires continues to increase. Example 5 The operations in this example were the same as example 1 except that the substrate had a temperature of 1000 C. The magnesium nanowire film prepared in Example 5 was scanned with SEM to obtain an SEM image shown in FIG. 5. It can be seen from FIG. 5 that, when the substrate has a temperature of 1000 C and an inclination angle a of 850, obtained magnesium nanowires have an inclination angle of 00 and are not clearly separated, and magnesium of a block structure appears on the top. This is because the atomic diffusion overcomes the shadowing effect, and the temperature effect is dominant. Comparative Example 1 The operations in this example were the same as example 1 except that the substrate had a temperature of 2000 C. The magnesium nanowire film prepared in Comparative Example 1 was scanned with SEM to obtain an SEM image shown in FIG. 6. It can be seen from FIG. 6 that, when the substrate has a temperature of 2000 C and an inclination angle a of 850, obtained nanowires have an inclination angle of 00, and the nanowire structure disappears completely. The cross-sectional morphology of the magnesium thin film characterized by the SEM totally shows magnesium of a block structure.
It can be proved from Examples 1 to 5 and Comparative Example 1 that the
morphology of the magnesium thin film is completely controlled by a temperature,
and when the temperature is not in the range of 250 C to 1000 C, a magnesium
nanowire film cannot be obtained.
Example 6
The magnesium nanowire film in this example was prepared by the same
method as in Example 1 except that the following conditions were adopted:
sputtering power: 50 W; a = 00; and Pot = 0.26 Pa.
The Monte Carlo software was used to simulate the growth of the magnesium
thin film prepared in Example 6, as shown in FIG. 7. It can be seen from FIG. 7 that,
as the energy of the right or left diffusion of magnesium atoms increases, the pore
in the magnesium thin film decreases in size and the width of the magnesium
nanowires increases. However, as the energy of the upward movement of
magnesium atoms increases, both the pore in the magnesium thin film and the
width of the magnesium nanowires remain unchanged. Therefore, the morphology
of the magnesium thin film is mainly determined by the left and right parallel
diffusion of magnesium atoms.
An X-ray photoelectron spectrometer was used to detect the magnesium
nanowire film prepared in Example 6, and an obtained XPS spectrum was shown in
FIG. 8. It can be seen from FIG. 8 that the electronic transitions of Mg, 0, and C in
the thin film are at 49.5 eV (Mg2p), 285 eV (Cs), and 530 eV (01s), respectively.
Further quantitative analysis for these signals reveals that the thin film includes
about 50% of oxygen atoms and 10% of carbon atoms. The presence of carbon
atoms may be related to surface contamination occurring during the transport of
the sample from the reaction chamber to an XPS instrument.
Example 7
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 60
during GLAD.
Example 8
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 700
during GLAD.
Example 9
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 800
during GLAD.
Example 10
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 82.50
during GLAD.
Example 11
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 850
during GLAD.
Example 12
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 870
during GLAD.
Example 13
The magnesium nanowire film in this example was prepared by the same
operations as Example 1 except that the substrate had an inclination angle of 890 during GLAD.
The magnesium nanowire films prepared in Examples 7 to 13 were scanned
with SEM to obtain SEM images shown in FIG. 9. It can be seen from FIG. 9 that,
when an incident angle is of 600 < a < 890, the inclination angle P of nanowires in
the magnesium nanowire film strongly depends on a. At a large incident angle
(greater than 600), the shadowing mechanism is enhanced, thus forming a column
inclined toward the magnesium target. As a increases, P increases significantly,
and when a > 850, P remains stable. This is because when an incident direction of
sputtered atoms is perpendicular to the surface of a deposited film, a diffusion
distance of the atoms is only equivalent to a few atoms in each direction, and a
magnesium thin film with nanotopography will not be obtained. However, when
atoms are sputtered obliquely at a given angle to the substrate, during the
deposition process, the diffusion of atoms occurs in the direction of the projection
of a sputtering beam on the surface of a film, and the diffusion in the direction
parallel to the surface of the film is only determined by the incidence angle.
Therefore, when the incident angle is 600 < a < 890, a magnesium nanowire film
with well-separated nanowires of a diameter of 20 nm to 50 nm may be obtained.
The magnesium nanowire films prepared in Examples 7 to 13 were analyzed to
obtain kMC simulation results illustrating the influence of the deposition angle a on
the inclination angle P of the magnesium nanowires, as shown in FIG. 10. It can be
seen from FIG. 10 that the inclination angle P of nanowires in the magnesium
nanowire film strongly depends on a.
Example 14
The operations in this example were the same as Example 1 except that the
sputtering power was fixed at 50 W, the inclination angle a was fixed at 850, and
the Pot was 0.13 Pa.
Example 15
This example differs from Example 14 in that that the Pot was 0.26 Pa, and the
operations in this example were the same as example 14.
Example 16
This example differs from Example 14 in that that the Pot was 0.65 Pa, and the
operations in this example were the same as example 14.
Example 17
This example differs from Example 14 in that that the Pot was 1.3 Pa, and the
operations in this example were the same as example 14.
The magnesium nanowire films prepared in Examples 14 to 17 were detected
with SEM to obtain SEM images shown in FIG. 11. According to FIG. 11, when Pot
is 0.13 Pa, 0.26 Pa, 0.65 Pa, and 1.3 Pa, magnesium nanowires in obtained
magnesium nanowire films have inclination angles of 51 ±1.00, 44 ±1.00, 24
1.00, and 5 ±0.50, respectively.
The Monte Carlo kinetic simulation was conducted for the magnesium nanowire
films prepared in Examples 14 to 17, as shown in FIG. 12. It can be seen from FIG.
12 that the inclination angle P of magnesium nanowires is used as a variable of the
PTot function, where, 0.13 Pa is the minimum value required to maintain the
discharge of the magnetron. FIG. 12 shows that, with the increase of Pot, @
decreases rapidly, from P = 51 ±1.00 at 0.13 Pa to @ = 5 ±0.50 at 1.3 Pa. This
indicates that the change of the inclination angle of the magnesium nanowires can
be attributed to the increase of Pot, and this may be because the decrease of
incident particle flux leads to the increase of collision probability.
It can be seen from the test results of the foregoing examples that the
preparation method provided by the present disclosure can be used to prepare a
magnesium nanowire film with well-separated magnesium nanowires of a diameter
of 25 nm to 100 nm, which can be used as a solid material for hydrogen storage.
The above descriptions are merely preferred implementations of the present disclosure. It should be noted that a person of ordinary skill in the art may further make several improvements and modifications without departing from the principle of the present disclosure, but such improvements and modifications should be deemed as falling within the protection scope of the present disclosure.
Claims (5)
1. A method for preparing a magnesium (Mg) nanowire film, comprising: using
magnetron sputtering to deposit the magnesium nanowire film on a substrate,
wherein,
a target material for the magnetron sputtering is an Mg target;
there is a distance of 60 mm to 80 mm between the Mg target and the
substrate;
the magnetron sputtering is conducted under the protection of argon;
during the magnetron sputtering, the substrate has a temperature of 250 C to
100°C; and
during the magnetron sputtering, the substrate has an inclination angle of
600< a < 890.
2. The preparation method according to claim 1, wherein, the substrate
comprises a conductive silicon wafer, a SiO 2 wafer, or an A1 2 0 3 wafer;
wherein, the Mg target has a purity of 99.99 wt% or more.
3. The preparation method according to claim 1, wherein, during the
magnetron sputtering, the substrate has a temperature of 250 C to 80°C;
wherein, the magnetron sputtering is conducted at power of 20 W tolOO W;
wherein, the magnetron sputtering is conducted at a working voltage of 0.13
Pa to 1.3 Pa;
wherein, the magnetron sputtering is conducted for 10 min to 60 min.
4. A magnesium nanowire film prepared by the preparation method according
to any one of claims 1 to 3, wherein, magnesium nanowires in the magnesium
nanowire film have a diameter of 20 nm to 100 nm.
5. Use of the magnesium nanowire film according to claim 4 as a solid material
for hydrogen storage.
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