CN108265275B - ZnO-Ga2O3Preparation method of core-shell nanowire - Google Patents

ZnO-Ga2O3Preparation method of core-shell nanowire Download PDF

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CN108265275B
CN108265275B CN201810057491.1A CN201810057491A CN108265275B CN 108265275 B CN108265275 B CN 108265275B CN 201810057491 A CN201810057491 A CN 201810057491A CN 108265275 B CN108265275 B CN 108265275B
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nanowire
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徐春祥
游道通
张炜
赵杰
石增良
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Southeast University
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • 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
    • C23C14/08—Oxides
    • 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
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • C23C14/24—Vacuum evaporation

Abstract

The invention discloses ZnO-Ga2O3The preparation method of the core-shell nanowire comprises a ZnO core layer and Ga2O3The shell layer is formed by the following preparation steps: 1) mixing and grinding ZnO powder and carbon powder, filling the mixture into a container, placing the container at the closed end of a quartz tube with an opening at one end, and placing a cleaned growth substrate at the position of the opening of the quartz tube; then placing the quartz tube in a tube furnace, sealing the tube furnace, vacuumizing, introducing argon and oxygen, and growing a ZnO nanowire array on a growth substrate after the reaction is finished; 2) putting the ZnO nanowire array obtained in the step 1) into a magnetron sputtering instrument, and sputtering a layer of Ga on the surface of the ZnO nanowire2O3A sheath film to obtain ZnO-Ga2O3Core-shell nanowires; the invention grows Ga with different thickness, uniform size and uniform distribution on the ZnO nanowire by a simple gas phase transmission method and a magnetron sputtering method2O3And (5) a shell layer film.

Description

ZnO-Ga2O3Preparation method of core-shell nanowire
Technical Field
The invention relates to ZnO-Ga2O3A preparation method of core-shell structure nano-wire belongs to the field of preparation method of nano-wire.
Background
In the design of a nano structure, the semiconductor nano heterojunction has potential application in the fields of ultraviolet detection, light-emitting devices, catalysis, gas sensitivity and the like because of containing different components. The properties of materials are influenced by their composition, morphology and size, and therefore growing nano-heterojunctions of different composition, morphology and size is of great interest. As wide bandgap semiconductor materials, ZnO and Ga2O3The material has excellent performance in the fields of ultraviolet detection, luminescent devices, catalysis, gas sensitivity and the like. ZnO-Ga-in comparison with a single component2O3The composite material nano heterojunction is used in ultraviolet detecting, light emitting device,The catalysis and gas sensitivity show more excellent performance, and the synergistic effect between the catalysis and the gas sensitivity greatly improves the performance of the material.
ZnO-Ga now adopted2O3Core-shell composites are generally prepared by a process comprising: surface reaction, seed deposition, microemulsion, hydrothermal, self-assembly, sol-gel, electrodeposition, templating, displacement, sonochemical, and the like. For ZnO-Ga2O3For the core-shell structure material, in order to achieve a uniform and compact coating effect of the shell material, a sol-gel method, a template method and other means are generally adopted, but the solution preparation environment is complex, the process stability is poor, large-area growth and industrial popularization and application are difficult to carry out, and a ZnO substrate is soaked in an aqueous solution for many times or for a long time, so that more ZnO surface defects are introduced in the process.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide ZnO-Ga2O3The preparation method of the core-shell structure nanowire is simple and easy to operate, strong in repeatability, and capable of growing Ga with different thicknesses, uniform sizes and uniform distribution2O3And (5) a shell layer film.
The technical scheme is as follows: the invention provides ZnO-Ga2O3The preparation method of the core-shell nanowire comprises the following steps of preparing a ZnO core layer and Ga2O3The shell layer is formed by the following preparation steps:
1) preparing a ZnO nanowire array: mixing and grinding ZnO powder and carbon powder until no particle sense exists, filling the mixture into a container, then placing the container at the closed end of a quartz tube with an opening at one end, and then placing a cleaned growth substrate at the position of a tube opening in the quartz tube; then placing the quartz tube in a tube furnace, sealing the tube furnace, vacuumizing, introducing argon and oxygen, and growing a ZnO nanowire array on a growth substrate after the reaction is finished;
2)ZnO-Ga2O3preparing a core-shell nanowire: putting the ZnO nanowire array obtained in the step 1) into a magnetron sputtering instrument, and sputtering a layer of Ga on the surface of the ZnO nanowire2O3The sheath layer is thinFilm to obtain ZnO-Ga2O3Core-shell nanowires;
wherein:
the purities of the ZnO powder and the carbon powder in the step 1) are respectively 99.97-99.99 wt%; the ZnO powder and the carbon powder are mixed and ground, and the mass ratio of the ZnO powder to the carbon powder is 1: 1-1: 3.
mixing and grinding the ZnO powder and the carbon powder in the step 1) until no granular sensation exists, wherein the grinding time is 15-25 min.
The container in the step 1) is a ceramic boat.
The clean growth substrate in the step 1) is a growth substrate which is subjected to ultrasonic cleaning by acetone, absolute ethyl alcohol and deionized water in sequence and is dried by nitrogen, wherein the growth substrate is a sapphire substrate, a silicon substrate or a silicon dioxide substrate;
the size of the growth substrate is 1-3 cm multiplied by 1-3 cm.
The quartz tube with the opening at one end is 20-30 cm long and 1-3 cm in diameter.
The step of placing the cleaned growth substrate at the position of the pipe orifice in the quartz pipe refers to the step of placing the growth substrate in the quartz pipe at a position 3-8 cm away from the pipe orifice of the quartz pipe.
The closed tube type furnace is vacuumized, argon and oxygen are introduced, the flow of the argon is 130-180 sccm, and the flow of the oxygen is 13-18 sccm.
The ZnO nanowire array grows on the growth substrate after the reaction is finished, namely the ZnO nanowire array grows on the growth substrate after the reaction is carried out for 10-60 min at the temperature of 1000-1200 ℃; and then closing the air valve and the vacuum pump, introducing air into the tubular furnace, and opening the tubular furnace to take out the sample when the air pressure in the furnace is atmospheric pressure.
Putting the ZnO nanowire array obtained in the step 1) into a magnetron sputtering instrument, and sputtering a layer of Ga on the surface of the ZnO nanowire2O3The sputtering conditions of the sheath film were: the sputtering target material is Ga2O3A target material, wherein the air pressure of the cavity is 1-4 Pa, the flow of argon is 30-60 sccm, the flow of oxygen is 5-30 sccm, the sputtering power is 80-150W,the sputtering time is 5-60 min.
Said Ga being2O3The target specification is 60X 3 mm.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1) the ZnO-Ga provided by the invention2O3The preparation method of the core-shell structure nanowire is simple and easy to operate, strong in repeatability, and capable of growing Ga with different thicknesses, uniform size and uniform distribution2O3A shell layer film;
2) ZnO-Ga prepared by the invention2O3The core-shell structure nanowire can be widely applied to the fields of ultraviolet detection, luminescent devices, catalysis, gas sensitivity and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a ZnO nanowire array synthesized in example 1 of the present invention;
FIG. 2 shows ZnO-Ga of the present invention2O3A transmission electron microscope image of the core-shell structure nanowire;
FIG. 3 shows ZnO-Ga prepared in example 1 of the present invention2O3And (3) analyzing a full spectrogram by using the X-ray photoelectron spectroscopy of the core-shell structure nanowire.
Detailed Description
ZnO-Ga2O3The preparation method of the core-shell structure nanowire comprises the following steps:
1) ZnO powder with the purity of 99.97-99.99 wt% and carbon powder are mixed according to the mass ratio of 1: 1-1: 3, mixing and grinding for 15-25 min until no granular sensation exists, and filling the mixture into a ceramic boat; cutting the growth substrate into 1-3 cm multiplied by 1-3 cm, carrying out ultrasonic cleaning on acetone, absolute ethyl alcohol and deionized water in sequence, blow-drying the substrate by using nitrogen, taking the substrate as a growth substrate, placing the substrate into a closed end of a quartz tube with an opening at one end, and placing the cleaned growth substrate into the quartz tube at a position 3-8 cm away from a tube opening; pushing the quartz tube into a tube furnace horizontally for high-temperature reaction, closing the tube furnace, vacuumizing, introducing argon and oxygen, closing an air valve and a vacuum pump after the reaction time, introducing air, opening the tube furnace when the air pressure in the tube furnace is atmospheric pressure, and taking out a sample;
2) putting the ZnO nanowire array grown on the growth substrate into a magnetron sputtering instrument, and sputtering a layer of Ga2O3A sheath film;
the growth substrate in the step 1) is a sapphire substrate, a silicon substrate or a silicon dioxide substrate;
the temperature of the high-temperature reaction in the step (1) is 1000-1200 ℃, the flow of argon is 130-180 sccm, the flow of oxygen is 13-18 sccm, and the reaction time is 10-60 min.
The sputtering target in the step (2) is Ga2O3The target material has the specification of 60 multiplied by 3mm, the air pressure of a cavity is 1-4 Pa, the flow of argon is 30-60 sccm, the flow of oxygen is 5-30 sccm, the sputtering power is 80-150W, and the sputtering time is 5-60 min.
Example 1:
the first step is as follows: mixing and grinding ZnO powder with the purity of 99.99 wt% and carbon powder according to the mass ratio of 1:1 for 20min until no granular sensation exists, and filling the mixture into a ceramic boat; cutting the sapphire substrate into 1.5cm multiplied by 1cm, carrying out ultrasonic cleaning on the sapphire substrate by acetone, absolute ethyl alcohol and deionized water in sequence, drying the sapphire substrate by using nitrogen to be used as a growth substrate, placing the growth substrate into a quartz tube with an opening at one end, a closed end of the quartz tube and a diameter of 3cm, and placing the cleaned sapphire substrate into the quartz tube at a position 5cm away from the tube opening. Pushing the quartz tube into a horizontal tube furnace with the set temperature of 1050 ℃, sealing the tube furnace, vacuumizing, introducing argon flow of 150sccm and oxygen flow of 15sccm, and reacting for 20min to grow a ZnO nanowire array on a growth substrate; then closing the air valve and the vacuum pump, introducing air, opening the tube furnace when the air pressure in the furnace is atmospheric pressure, and taking out a sample, wherein the appearance of the sample is shown in figure 1;
the second step is that: putting the ZnO nanowire array grown on the sapphire substrate into a magnetron sputtering instrument, and sputtering a layer of Ga2O3A sheath film to obtain the ZnO-Ga2O3The core-shell structure nanowire has the following sputtering conditions: with Ga2O3The target material is a sputtering source with the specification of 60 multiplied by 3mm, the air pressure of the cavity is 2Pa, the argon flow is 55sccm, the oxygen flow is 15sccm, the sputtering power is 100W, and the sputtering time is 8min; synthetic ZnO-Ga2O3The core-shell structure nanowire has a morphology structure as shown in fig. 2, and chemical elements and valence state distribution as shown in fig. 3.
Example 2:
the first step is as follows: mixing and grinding ZnO powder with the purity of 99.99 wt% and carbon powder according to the mass ratio of 1:1 for 25min until no granular sensation exists, and filling the mixture into a ceramic boat; cutting the silicon substrate into 2cm multiplied by 2cm, carrying out ultrasonic cleaning on the silicon substrate by acetone, absolute ethyl alcohol and deionized water in sequence, drying the silicon substrate by using nitrogen, using the silicon substrate as a growth substrate, placing the silicon substrate as a growth substrate into a quartz tube with an opening at one end, a length of 30cm and a diameter of 3cm, and placing the cleaned sapphire substrate into a quartz tube at a position 6cm away from the tube opening. The quartz tube was pushed into a horizontal tube furnace set at 1000 ℃ as a whole, the tube furnace was closed, evacuated, and argon flow of 180sccm and oxygen flow of 18sccm were introduced. After 30min reaction, growing a ZnO nanowire array on the growth substrate; then closing the air valve and the vacuum pump, introducing air, and opening the tube furnace when the air pressure in the furnace is atmospheric pressure to take out a sample;
the second step is that: putting the ZnO nanowire array grown on the sapphire substrate into a magnetron sputtering instrument, and sputtering a layer of Ga2O3A sheath film to obtain the ZnO-Ga2O3The core-shell structure nanowire has the following sputtering conditions: with Ga2O3The target material is a sputtering source with the specification of 60 multiplied by 3mm, the air pressure of the cavity is 4Pa, the flow of argon is 30sccm, the flow of oxygen is 5sccm, the sputtering power is 150W, and the sputtering time is 5 min.
Example 3:
the first step is as follows: mixing and grinding ZnO powder with the purity of 99.98 wt% and carbon powder according to the mass ratio of 1:2 for 15min until no granular sensation exists, and filling the mixture into a ceramic boat; cutting the silicon dioxide substrate into 1.5cm multiplied by 1.5cm, carrying out ultrasonic cleaning on the silicon dioxide substrate by acetone, absolute ethyl alcohol and deionized water in sequence, drying the silicon dioxide substrate by using nitrogen, using the silicon dioxide substrate as a growth substrate, placing the silicon dioxide substrate into a quartz tube with an opening at one end, a length of 30cm and a diameter of 3cm, and placing the cleaned sapphire substrate into the quartz tube at a position 8cm away from the tube opening. The quartz tube was pushed into a horizontal tube furnace set at 1100 ℃ as a whole, the tube furnace was closed, vacuum was applied, and argon flow of 130sccm and oxygen flow of 13sccm were introduced. After 10min reaction, growing a ZnO nanowire array on a growth substrate; then closing the air valve and the vacuum pump, introducing air, and opening the tube furnace when the air pressure in the furnace is atmospheric pressure to take out a sample;
the second step is that: putting the ZnO nanowire array grown on the sapphire substrate into a magnetron sputtering instrument, and sputtering a layer of Ga2O3A sheath film to obtain the ZnO-Ga2O3The core-shell structure nanowire has the following sputtering conditions: with Ga2O3The target material is a sputtering source with the specification of 60 multiplied by 3mm, the air pressure of the cavity is 2Pa, the flow of argon is 60sccm, the flow of oxygen is 30sccm, the sputtering power is 80W, and the sputtering time is 60 min.
Example 4:
the first step is as follows: mixing and grinding ZnO powder with the purity of 99.97 wt% and carbon powder according to the mass ratio of 1:3 for 20min until no granular sensation exists, and filling the mixture into a ceramic boat; cutting the silicon substrate into 2cm multiplied by 2cm, carrying out ultrasonic cleaning on the silicon substrate by acetone, absolute ethyl alcohol and deionized water in sequence, drying the silicon substrate by using nitrogen, using the silicon substrate as a growth substrate, placing the silicon substrate as a growth substrate into a quartz tube with an opening at one end, a closed end of the quartz tube with the length of 30cm and the diameter of 3cm, and placing the cleaned sapphire substrate into the quartz tube at the position 3cm away from the tube opening. The quartz tube was pushed into a horizontal tube furnace set at 1200 ℃ as a whole, the tube furnace was closed, vacuum was applied, and argon flow 140sccm and oxygen flow 14sccm were introduced. After 60min reaction, growing a ZnO nanowire array on the growth substrate; then closing the air valve and the vacuum pump, introducing air, and opening the tube furnace when the air pressure in the furnace is atmospheric pressure to take out a sample;
the second step is that: putting the ZnO nanowire array grown on the sapphire substrate into a magnetron sputtering instrument, and sputtering a layer of Ga2O3A sheath film to obtain the ZnO-Ga2O3The core-shell structure nanowire has the following sputtering conditions: with Ga2O3The target is a sputtering source with the specification of 60 multiplied by 3mm, the air pressure of the cavity is 1Pa, the flow of argon is 40sccm, the flow of oxygen is 15sccm, the sputtering power is 100W, and the sputtering time is 40 min.
While the invention has been shown and described with respect to the preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the scope of the invention as defined in the following claims.

Claims (7)

1. ZnO-Ga2O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: the nano-wire with the core-shell structure consists of a ZnO core layer and Ga2O3The shell layer is formed by the following preparation steps:
1) preparing a ZnO nanowire array: mixing and grinding ZnO powder and carbon powder until no particle sense exists, filling the mixture into a container, then placing the container at the closed end of a quartz tube with an opening at one end, and then placing a cleaned growth substrate at the position of a tube opening in the quartz tube; then placing the quartz tube in a tube furnace, sealing the tube furnace, vacuumizing, introducing argon and oxygen, and growing a ZnO nanowire array on a growth substrate after the reaction is finished;
2)ZnO-Ga2O3preparing a core-shell nanowire: putting the ZnO nanowire array obtained in the step 1) into a magnetron sputtering instrument, and sputtering a layer of Ga on the surface of the ZnO nanowire2O3A sheath film to obtain ZnO-Ga2O3Core-shell nanowires;
wherein: the purities of the ZnO powder and the carbon powder in the step 1) are respectively 99.97-99.99 wt%; the ZnO powder and the carbon powder are mixed and ground, and the mass ratio of the ZnO powder to the carbon powder is 1: 1-1: 3;
the ZnO nanowire array is grown on the growth substrate after the reaction is finished, namely the ZnO nanowire array is grown on the growth substrate after the reaction is carried out for 10-60 min at the temperature of 1000-1200 ℃.
2. ZnO-Ga according to claim 12O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: mixing and grinding the ZnO powder and the carbon powder in the step 1) until no granular sensation exists, wherein the grinding time is 15-25 min.
3. As claimed in claim 1ZnO-Ga2O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: the container in the step 1) is a ceramic boat.
4. ZnO-Ga according to claim 12O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: the clean growth substrate in the step 1) is a growth substrate which is sequentially subjected to ultrasonic cleaning by acetone, absolute ethyl alcohol and deionized water and blow-drying by nitrogen, wherein the growth substrate is a sapphire substrate, a silicon substrate or a silicon dioxide substrate.
5. ZnO-Ga according to claim 12O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: the step of placing the cleaned growth substrate at the position of the pipe orifice in the quartz pipe refers to the step of placing the growth substrate in the quartz pipe at a position 3-8 cm away from the pipe orifice of the quartz pipe.
6. ZnO-Ga according to claim 12O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: the closed tube type furnace is vacuumized, argon and oxygen are introduced, the flow of the argon is 130-180 sccm, and the flow of the oxygen is 13-18 sccm.
7. ZnO-Ga according to claim 12O3The preparation method of the core-shell nanowire is characterized by comprising the following steps: putting the ZnO nanowire array obtained in the step 1) into a magnetron sputtering instrument, and sputtering a layer of Ga on the surface of the ZnO nanowire2O3The sputtering conditions of the sheath film were: sputtering target Ga2O3The target material has a cavity pressure of 1-4 Pa, an argon flow of 30-60 sccm, an oxygen flow of 5-30 sccm, a sputtering power of 80-150W, and a sputtering time of 5-60 min.
CN201810057491.1A 2018-01-22 2018-01-22 ZnO-Ga2O3Preparation method of core-shell nanowire Active CN108265275B (en)

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