CN108265275A - A kind of ZnO-Ga2O3The preparation method of core-shell nano line - Google Patents
A kind of ZnO-Ga2O3The preparation method of core-shell nano line Download PDFInfo
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- CN108265275A CN108265275A CN201810057491.1A CN201810057491A CN108265275A CN 108265275 A CN108265275 A CN 108265275A CN 201810057491 A CN201810057491 A CN 201810057491A CN 108265275 A CN108265275 A CN 108265275A
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
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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
- C23C14/06—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
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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
- C23C14/24—Vacuum evaporation
Abstract
The invention discloses a kind of ZnO Ga2O3The preparation method of core-shell nano line, the core-shell nano line are by ZnO stratum nucleares and Ga2O3Shell is formed, and preparation process is as follows：1) by ZnO powder and carbon dust mixed grinding, the blind end for the quartz ampoule for being placed in one end open is inserted in container, the growth substrate cleaned up is positioned at quartz ampoule nozzle position；Then the quartz ampoule is placed in tube furnace, is vacuumized after closing tube furnace and is passed through argon gas and oxygen, growth has ZnO nanowire array in growth substrate after reaction；2) step 1) is obtained ZnO nanowire array to be put into magnetic control sputtering device, one layer of Ga is sputtered on ZnO nano-wire surface2O3Sheath layer film obtains ZnO Ga2O3Core-shell nano line；The present invention grows different-thickness, size uniformity, the Ga being evenly distributed by simple Vapor Transport and magnetically controlled sputter method on ZnO nano-wire2O3Blanket films.
Description
Technical field
The present invention relates to a kind of ZnO-Ga2O3The preparation method of nuclear shell structure nano line belongs to the preparation method neck of nano wire
Domain.
Background technology
In nano-structure design, semiconductor nano hetero-junctions, since it contains different ingredients, in ultraviolet detection, hair
The fields such as optical device, catalysis and air-sensitive have potential application.The performance of material is influenced by its ingredient, pattern and size, because
The nano heterojunction of this growth heterogeneity, pattern and size causes the great interest of people.As wide bandgap semiconductor material
Material, ZnO and Ga2O3Excellent performance is all presented in fields such as ultraviolet detection, luminescent device, catalysis and air-sensitives.With it is single into
Split-phase ratio, ZnO-Ga2O3Composite material nanometer hetero-junctions shows superior in ultraviolet detection, luminescent device, catalysis and air-sensitive
Performance, between the two synergistic effect substantially increase the performance of material.
The ZnO-Ga used now2O3Core-shell composite material preparation method generally comprises：Surface reaction method, seed deposition method,
Microemulsion method, hydro-thermal method, self-assembly method, sol-gal process, electrodeposition process, template, displacement method, sonochemical method etc..For
ZnO-Ga2O3Core-shell structure material for, Shell Materials to be made to reach uniform, fine and close covered effect, are generally required using molten
Means such as sol-gel, template, but prepared by solution environment is complicated, technology stability is poor, it is difficult to carry out large area deposition and
Industrial application, and zno-based piece repeatedly or is for a long time impregnated in aqueous solution, this process will introduce more
ZnO surface defects.
Invention content
Technical problem：The object of the present invention is to provide a kind of ZnO-Ga2O3The preparation method of nuclear shell structure nano line, the party
Method operation is simple, repeatable strong, can grow different-thickness, size uniformity, the Ga being evenly distributed2O3Blanket films.
Technical solution：The present invention provides a kind of ZnO-Ga2O3The preparation method of core-shell nano line, the nucleocapsid are received
Rice noodles are by ZnO stratum nucleares and Ga2O3Shell is formed, and preparation process is as follows：
1) preparation of ZnO nanowire array：ZnO powder and carbon dust mixed grinding are inserted into container after no granular sensation
It is interior, which is placed in the blind end of the quartz ampoule of one end open later, the growth substrate cleaned up is positioned over stone later
At nozzle position inside English pipe；Then the quartz ampoule is placed in tube furnace, is vacuumized, and be passed through argon gas after closing tube furnace
And oxygen, growth has ZnO nanowire array in growth substrate after reaction；
2)ZnO-Ga2O3The preparation of core-shell nano line：Step 1) is obtained ZnO nanowire array to be put into magnetic control sputtering device,
One layer of Ga is sputtered on ZnO nano-wire surface2O3Sheath layer film, obtains ZnO-Ga2O3Core-shell nano line；
Wherein：
The purity of ZnO powder and carbon dust described in step 1) is 99.97wt%~99.99wt%；It is described by ZnO
The mass ratio of powder and carbon dust mixed grinding, ZnO powder and carbon dust is 1：1~1：3.
Described in step 1) by ZnO powder and carbon dust mixed grinding up to no granular sensation milling time for 15~
25min。
Container described in step 1) is ceramic boat.
The growth substrate that cleans up described in step 1) refers to pass through acetone, absolute ethyl alcohol, deionized water ultrasound successively clearly
The growth substrate washed and dried up with nitrogen, wherein the growth substrate is Sapphire Substrate, silicon substrate or silicon dioxide liner
Bottom；
The size of the growth substrate is 1~3cm × 1~3cm.
The length of the quartz ampoule of the one end open is 20~30cm, a diameter of 1~3cm.
Refer to be positioned over distance at the nozzle position that the growth substrate cleaned up is positioned over inside quartz ampoule
In quartz ampoule at 3~8cm of quartz ampoule nozzle.
Vacuumized, and be passed through argon gas and oxygen after the closing tube furnace, the argon flow amount for 130~
180sccm, oxygen flow are 13~18sccm.
Described being grown in growth substrate after reaction has ZnO nanowire array to refer to that in temperature be 1000~1200
Under the conditions of DEG C, growth has ZnO nanowire array in growth substrate after 10~60min of reaction；Air valve and vacuum pump are closed later,
Air is passed through to tube furnace, when air pressure is atmospheric pressure in stove, tube furnace is opened, takes out sample.
It is described step 1) is obtained into ZnO nanowire array to be put into magnetic control sputtering device, sputter one on ZnO nano-wire surface
Layer Ga2O3The sputtering condition of sheath layer film is：Sputtering target material is Ga2O3Target, cavity air pressure be 1~4Pa, argon flow amount 30
~60sccm, oxygen flow are 5~30sccm, and sputtering power is 80~150W, and sputtering time is 5~60min.
The Ga2O3Target specification is 60 × 3mm.
Advantageous effect：Compared with prior art, the present invention has the following advantages：
1) ZnO-Ga provided by the invention2O3The preparation method operation of nuclear shell structure nano line is simple, repeats by force, can give birth to
Long different-thickness, size uniformity, the Ga being evenly distributed2O3Blanket films；
2) ZnO-Ga prepared by the present invention2O3Nuclear shell structure nano line can be with ultraviolet detection, luminescent device, catalysis and air-sensitive
It is used widely in the fields of grade.
Description of the drawings
Fig. 1 is the ZnO nanowire array scanning electron microscope diagram that the embodiment of the present invention 1 synthesizes；
Fig. 2 is the ZnO-Ga of the present invention2O3Nuclear shell structure nano line transmission electron microscope figure；
Fig. 3 is ZnO-Ga prepared by the embodiment of the present invention 12O3Nuclear shell structure nano line X-ray photoelectron spectroscopic analysis is composed entirely
Figure.
Specific embodiment
A kind of ZnO-Ga2O3The preparation method of nuclear shell structure nano line, includes the following steps：
1) by purity be 99.97wt%~99.99wt% ZnO ends and carbon dust according to mass ratio 1：1~1：3 mixing
After grinding 15~25min to no granular sensation, insert in ceramic boat；Growth substrates are cut into 1~3cm × 1~3cm, are carried out successively
Acetone, absolute ethyl alcohol, deionized water are cleaned by ultrasonic, and are dried up with nitrogen, as growth substrate, are put into the quartz ampoule of one end open
Blind end, cleaned growth substrates are placed away from the quartz ampoule at 3~8cm of nozzle positions；By quartz ampoule integral level
The reaction of tube furnace high temperature is pushed into, tube furnace is closed, vacuumizes, and be passed through argon gas and oxygen, after the reaction time, closes gas
Valve and vacuum pump, are passed through air, when air pressure is atmospheric pressure in stove, open tube furnace, take out sample；
2) ZnO nanowire array that will have been grown in growth substrates is put into magnetic control sputtering device, sputters one layer of Ga2O3Sheaths
Film；
Growth substrate described in step 1) is Sapphire Substrate, silicon substrate or silicon dioxide substrates；
The temperature of step (1) described pyroreaction is 1000~1200 DEG C, and the argon flow amount is 130~180sccm
It is 13~18sccm with oxygen flow, the reaction time is 10~60min.
Sputtering target material described in step (2) is Ga2O3Target, specification be 60 × 3mm, cavity air pressure be 1~4Pa, argon gas
Flow is 30~60sccm, and oxygen flow is 5~30sccm, and sputtering power is 80~150W, and sputtering time is 5~60min.
Embodiment 1：
The first step：By purity be 99.99wt% ZnO ends and carbon dust according to mass ratio 1:1 mixed grinding 20min is extremely
After granular sensation, insert in ceramic boat；Sapphire Substrate is cut into 1.5cm × 1cm, successively carry out acetone, absolute ethyl alcohol, go from
Sub- water is cleaned by ultrasonic, and is dried up with nitrogen, as growth substrate, is put into the length 30cm of one end open, the quartz ampoule of diameter 3cm
Blind end places cleaned Sapphire Substrate away from the quartz ampoule at nozzle 5cm positions.Quartz ampoule is integrally pushed into setting
Temperature is in 1050 DEG C of horizontal pipe furnace, closes tube furnace, vacuumizes, and be passed through argon flow amount 150sccm and oxygen flow
15sccm, after 20min reacts, being grown in growth substrate has ZnO nanowire array；Air valve and vacuum pump are closed later,
Air is passed through, when air pressure is atmospheric pressure in stove, tube furnace is opened, takes out sample, sample topography is as shown in Figure 1；
Second step：Grown on Sapphire Substrates good ZnO nanowire array is put into magnetic control sputtering device, sputters one layer
Ga2O3Sheath layer film obtains the ZnO-Ga2O3Nuclear shell structure nano line, sputtering condition are：With Ga2O3Target is sputtering
Source, specification are 60 × 3mm, and cavity air pressure is 2Pa, argon flow amount 55sccm, oxygen flow 15sccm, and sputtering power is
100W, sputtering time 8min；The ZnO-Ga of synthesis2O3Nuclear shell structure nano line appearance structure as shown in Fig. 2, chemical element and
Valence distribution is as shown in Figure 3.
Embodiment 2：
The first step：By purity be 99.99wt% ZnO ends and carbon dust according to mass ratio 1:1 mixed grinding 25min is extremely
After granular sensation, insert in ceramic boat；Silicon substrate is cut into 2cm × 2cm, acetone, absolute ethyl alcohol, deionized water is carried out successively and surpasses
Sound cleans, and is dried up with nitrogen, as growth substrate, is put into the length 30cm of one end open, the quartzy duct occlusion of diameter 3cm
End places cleaned Sapphire Substrate away from the quartz ampoule at nozzle 6cm positions.Quartz ampoule is integrally pushed into set temperature
In 1000 DEG C of horizontal pipe furnaces, to close tube furnace, vacuumizing, and be passed through argon flow amount 180sccm and oxygen flow
18sccm.After 30min reacts, being grown in growth substrate has ZnO nanowire array；Air valve and vacuum pump are closed later,
Air is passed through, when air pressure is atmospheric pressure in stove, tube furnace is opened, takes out sample；
Second step：Grown on Sapphire Substrates good ZnO nanowire array is put into magnetic control sputtering device, sputters one layer
Ga2O3Sheath layer film obtains the ZnO-Ga2O3Nuclear shell structure nano line, sputtering condition are：With Ga2O3Target is sputtering
Source, specification are 60 × 3mm, and cavity air pressure is 4Pa, argon flow amount 30sccm, oxygen flow 5sccm, and sputtering power is
150W, sputtering time 5min.
Embodiment 3：
The first step：By purity be 99.98wt% ZnO ends and carbon dust according to mass ratio 1:2 mixed grinding 15min are extremely
After granular sensation, insert in ceramic boat；Silicon dioxide substrates are cut into 1.5cm × 1.5cm, successively carry out acetone, absolute ethyl alcohol,
Deionized water is cleaned by ultrasonic, and is dried up with nitrogen, as growth substrate, is put into the length 30cm of one end open, the stone of diameter 3cm
English duct occlusion end places cleaned Sapphire Substrate away from the quartz ampoule at nozzle 8cm positions.Quartz ampoule is integrally pushed into
Set temperature is in 1100 DEG C of horizontal pipe furnace, closes tube furnace, vacuumizes, and be passed through argon flow amount 130sccm and oxygen
Flow 13sccm.After 10min reacts, being grown in growth substrate has ZnO nanowire array；Air valve and vacuum are closed later
Pump, is passed through air, when air pressure is atmospheric pressure in stove, opens tube furnace, takes out sample；
Second step：Grown on Sapphire Substrates good ZnO nanowire array is put into magnetic control sputtering device, sputters one layer
Ga2O3Sheath layer film obtains the ZnO-Ga2O3Nuclear shell structure nano line, sputtering condition are：With Ga2O3Target is sputtering
Source, specification are 60 × 3mm, and cavity air pressure is 2Pa, argon flow amount 60sccm, oxygen flow 30sccm, and sputtering power is
80W, sputtering time 60min.
Embodiment 4：
The first step：By purity be 99.97wt% ZnO ends and carbon dust according to mass ratio 1:3 mixed grinding 20min are extremely
After granular sensation, insert in ceramic boat；Silicon substrate is cut into 2cm × 2cm, acetone, absolute ethyl alcohol, deionized water is carried out successively and surpasses
Sound cleans, and is dried up with nitrogen, as growth substrate, is put into the length 30cm of one end open, the quartzy duct occlusion of diameter 3cm
End places cleaned Sapphire Substrate away from the quartz ampoule at nozzle 3cm positions.Quartz ampoule is integrally pushed into set temperature
In 1200 DEG C of horizontal pipe furnaces, to close tube furnace, vacuumizing, and be passed through argon flow amount 140sccm and oxygen flow
14sccm.After 60min reacts, being grown in growth substrate has ZnO nanowire array；Air valve and vacuum pump are closed later,
Air is passed through, when air pressure is atmospheric pressure in stove, tube furnace is opened, takes out sample；
Second step：Grown on Sapphire Substrates good ZnO nanowire array is put into magnetic control sputtering device, sputters one layer
Ga2O3Sheath layer film obtains the ZnO-Ga2O3Nuclear shell structure nano line, sputtering condition are：With Ga2O3Target is sputtering
Source, specification are 60 × 3mm, and cavity air pressure is 1Pa, argon flow amount 40sccm, oxygen flow 15sccm, and sputtering power is
100W, sputtering time 40min.
Although the present invention is illustrated and has been described with regard to preferred embodiment, it is understood by those skilled in the art that
Without departing from scope defined by the claims of the present invention, variations and modifications can be carried out to the present invention.
Claims (9)
1. a kind of ZnO-Ga2O3The preparation method of core-shell nano line, it is characterised in that：The nano wire of the nucleocapsid is by ZnO cores
Layer and Ga2O3Shell is formed, and preparation process is as follows：
1) preparation of ZnO nanowire array：ZnO powder and carbon dust mixed grinding are inserted after no granular sensation in container,
The container is placed in the blind end of the quartz ampoule of one end open later, the growth substrate cleaned up is positioned over quartz ampoule later
At internal nozzle position；Then the quartz ampoule is placed in tube furnace, is vacuumized, and be passed through argon gas and oxygen after closing tube furnace
Gas, growth has ZnO nanowire array in growth substrate after reaction；
2)ZnO-Ga2O3The preparation of core-shell nano line：Step 1) is obtained ZnO nanowire array to be put into magnetic control sputtering device,
ZnO nano-wire surface sputters one layer of Ga2O3Sheath layer film, obtains ZnO-Ga2O3Core-shell nano line.
2. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：Step 1) is described
ZnO powder and the purity of carbon dust be 99.97wt%~99.99wt%；Described mix ZnO powder and carbon dust is ground
The mass ratio of mill, ZnO powder and carbon dust is 1：1~1：3.
3. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：Step 1) is described
By ZnO powder and carbon dust mixed grinding up to the milling time of no granular sensation is 15~25min.
4. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：Step 1) is described
Container be ceramic boat.
5. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：Step 1) is described
Clean up growth substrate refer to successively by acetone, absolute ethyl alcohol, deionized water is cleaned by ultrasonic and the life that is dried up with nitrogen
Long substrate, wherein the growth substrate is Sapphire Substrate, silicon substrate or silicon dioxide substrates.
6. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：Described will be clear
The growth substrate of wash clean, which is positioned at the nozzle position inside quartz ampoule, to be referred to be positioned at 3~8cm of quartz ampoule nozzle
Quartz ampoule in.
7. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：The closing
Vacuumized after tube furnace, and be passed through argon gas and oxygen, the argon flow amount is 130~180sccm, oxygen flow be 13~
18sccm。
8. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：The reaction
After in growth substrate growth there is ZnO nanowire array to refer in temperature under the conditions of 1000~1200 DEG C, reaction 10~
Growth has ZnO nanowire array in growth substrate after 60min.
9. a kind of ZnO-Ga as described in claim 12O3The preparation method of core-shell nano line, it is characterised in that：Described will step
It is rapid 1) to obtain ZnO nanowire array and be put into magnetic control sputtering device, sputter one layer of Ga on ZnO nano-wire surface2O3Sheath layer film splashes
The condition of penetrating is：Sputtering target material Ga2O3Target, cavity air pressure are 1~4Pa, and argon flow amount is 30~60sccm, oxygen flow for 5~
30sccm, sputtering power are 80~150W, and sputtering time is 5~60min.
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Cited By (1)
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| CN110323303A (en) * | 2019-07-09 | 2019-10-11 | 北京镓族科技有限公司 | A kind of Ga2O3- CuSCN nucleocapsid hetero-junctions solar blind ultraviolet detector and preparation method thereof |
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