CN106637404A - Method for growing large-area mono-crystal vanadium dioxide thin film by utilizing tubular furnace - Google Patents
Method for growing large-area mono-crystal vanadium dioxide thin film by utilizing tubular furnace Download PDFInfo
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- CN106637404A CN106637404A CN201611107754.2A CN201611107754A CN106637404A CN 106637404 A CN106637404 A CN 106637404A CN 201611107754 A CN201611107754 A CN 201611107754A CN 106637404 A CN106637404 A CN 106637404A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
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Abstract
The invention discloses a method for growing a large-area mono-crystal vanadium dioxide thin film by utilizing a tubular furnace. The thin film grows on an experiment substrate with a certain thickness of SiO2/Si, Si3N4/Si, silicon, quartz, sapphires and the like by adopting a gas-solid manner. A growth surface of the experiment substrate is subjected to strict polishing treatment, and a reaction source vanadium pentaoxide powder is uniformly put at the bottom of a quartz boat; the experiment substrate is put into the quartz boat and the growth surface of the substrate is put downward. The large-area mono-crystal vanadium dioxide thin film is prepared through controlling a temperature rising speed, temperature, air pressure, gas flow size and reaction time in a vacuum environment of the tubular furnace. Compared with a common vanadium dioxide thin film, the large-area mono-crystal vanadium dioxide thin film prepared by the method has more excellent performances, the process is simple and the film forming quality is high; after the prepared mono-crystal vanadium dioxide thin film is subjected to insulator-metal phase change, the changing amplitude of the electrical conductivity reaches 4 to 5 orders of magnitude; the mono-crystal vanadium dioxide thin film is a mono-crystal material thin film and has wide application prospects in photo-electric, infrared and gas sensing aspects and the like.
Description
Technical field
The present invention relates to a kind of oxide semiconductor material growing method, more particularly to it is a kind of using the big face of tube furnace growth
Product monocrystalline vanadium dioxide film method.
Background technology
Vanadium dioxide is a kind of transition metal oxide with unique properties, occurs insulator to gold in 340K or so
The thermal induced phase transition of category state.This phase transformation of vanadium dioxide not only can be realized by heating, by other such as illumination, power-up
The modes such as field are likely to cause.Vanadium dioxide film with thermal induced phase transition property is in lasing safety, ultrafast switch and infrared
Thermal imaging aspect has potential using value, thus vanadium dioxide film is referred to as " smart membranes " by image.
General vanadium dioxide film material preparation method mainly has vacuum vapour deposition, sputtering method, chemical vapour deposition technique, thing
Physical vapor deposition and pulsed laser deposition etc..Japan musashi open country electrical communication use for laboratory pulsed laser deposition is in TiO2Substrate
On prepare vanadium dioxide film;U.S. Robert Webster research center is obtained difference using magnetron sputtering method in the pressure of different oxygen
The vanadium dioxide of stoichiometric proportion±xSeries thin film.These preparation method techniques are more ripe, can growing film area it is big, and film
Thickness is controllable, but these films are the film of polycrystalline structure, and change in resistance typically can only achieve 2~3 numbers during its phase transformation
Performance in terms of magnitude, electricity-optics thus be also affected.
The content of the invention
In the deficiency of aspect of performance, the present invention proposes a kind of profit to the vanadium dioxide film material prepared for conventional method
With the method for tube furnace growing large-area monocrystalline vanadium dioxide film, to solve above-mentioned background technology in shortcoming.
To solve above-mentioned technical problem, one kind of the present invention utilizes tube furnace growing large-area monocrystalline vanadium dioxide film side
Method, using tube furnace vanadium dioxide film is grown, and the tube furnace includes tubular type furnace control system and quartz ampoule, and quartz ampoule one end is
Air inlet, arranges vacuum meter on the pipeline of air inlet, experiment substrate and quartz boat, experiment substrate and quartz boat are put in quartz ampoule
In be put into vanadium pentoxide powder, the quartz ampoule other end is gas outlet.
Experiment substrate selects SiO2/Si、Si3N4/ Si, silicon, quartz or sapphire.Experiment is by controlling intensification during growth
Speed, keeping temperature, rate of temperature fall and gas flow are realizing.
In the present invention, testing substrate aufwuchsplate need to be through polishing;Vanadium pentoxide powder used is pure in experiment
Spend for 99.99%, and nodeless mesh particle;Used carrier gas in experiment is argon gas, and its purity is 99.9999%.
One kind utilizes tube furnace growing large-area monocrystalline vanadium dioxide film method, comprises the following steps that:
(1) experiment substrate and quartz boat are respectively cleaned by ultrasonic respectively with acetone, absolute ethyl alcohol, it is ensured that experiment substrate and quartz
Boat surface is clean, without grease and pollutant;Substrate and quartz boat, removal of oil and grease and oxide, acetone are tested using solvent clean
Also can be replaced with isopropanol.
(2) vanadium pentoxide powder is put in the experiment substrate and quartz boat of acquisition in step (1), and is put in order
To in quartz ampoule, experiment every time needs to use three quartz boats, and first quartz boat is placed in the middle of the inner side warm area of quartz ampoule;The
Two quartz boats are positioned in the middle of the outside warm area of quartz ampoule;3rd quartz boat is positioned over the upstream distance of second quartz boat
Its 5~10mm.Vanadium pentoxide powder is uniformly placed in quartz boat, and experiment substrate puts into first and second quartz
In boat, experiment substrate growth placed face down tests the height and following powder 1~3mm of distance of substrate, wherein the 3rd stone
Substrate is not placed on Ying Zhou;Be in 3rd quartz boat do not test substrate only put powder, the powder in second quartz boat
It is considerably less, to prevent the quality of the excessive film for affecting to grow into substrate surface of powder, the powder of the 3rd quartz boat from somewhat comparing
First boat is more, because the 3rd quartz boat is without powder boat is individually placed, in order to provide the 3rd quartz boat
The environment powder of one good growing film of upper substrate is somewhat more.
(3) after the quartz boat placed in step (2), envelope chamber is carried out to quartz ampoule, is evacuated to 50~80mTorr,
Argon gas is then passed to, flow is 5~20SCCM, the temperature of outside warm area and inner side warm area is raised to into 800~1000 DEG C, the used time 40
~100 minutes, the air pressure valve of vacuum orifice is adjusted in time by the change of quartzy intraductal atmospheric pressure in observation temperature-rise period so as to stone
English intraductal atmospheric pressure is controlled in the range of 200~900mTorr, and in 10~20 DEG C/min, temperature reaches 800 to control heating rate
~1000 DEG C of laggard trip temperatures keep, and the retention time is 180~360 minutes, then control 1~2 DEG C/min of rate of temperature fall, work as temperature
Degree opens quartz ampoule after showing less than 30 DEG C, take out experiment substrate.
The vanadium pentoxide powder and that vanadium pentoxide powder that first quartz boat is placed with, second quartz boat are placed with
The mass ratio of the vanadium pentoxide powder being placed with three quartz boats is 1.5~3:1~2:1.5~6.
Outside warm area and inner side warm area temperature are raised to 900~1000 DEG C and 800~900 DEG C from room temperature respectively.According to each
Different experiment substrates may be used in experiment, the substrate for needing high growth temperature temperature outside is put into into, it would be desirable to low-temperature epitaxy
Substrate is put into inner side warm area.
Generally tube furnace is all used for the growth of vanadium dioxide nanowire, and the present invention is used by adjusting vanadium pentoxide powder
The influence factors such as amount, substrate placement position, heating rate, temperature hold-time, rate of temperature fall, carrier gas flux, realize big face
The vanadium dioxide film growth of product monocrystalline.This growth and raw material vanadium pentoxide powder, substrate placement position, the growth for being adopted
Temperature etc. is all closely related.Pressure in experimentation in quartz ampoule and the size from type of substrate difference to growing film
Have an impact, this is relevant with Crystal surface structure and growth rate.
Beneficial effects of the present invention:
1st, the vanadium dioxide film of present invention growth, after a liter high-temperature reaches transformation temperature, produces obvious sudden change of resistivity
Characteristic, can reach the change of 4~5 orders of magnitude;
2nd, the rate of film build of the vanadium dioxide film of present invention growth is high, due to surface void it is less, charge carrier transport efficiency
It is higher, so as to be conducive to improving material photoelectric properties;
3rd, the vanadium dioxide film of present invention growth is obtained using tube furnace growth, growth apparatus are simple, preparation technology into
Ripe, reproducible, low cost, the film thickness of generation is suitable, uniformity is good, controllability is strong, so as to be conducive to the industry of material
Change and popularization and application.
Description of the drawings
Fig. 1 is the structural representation of the vanadium dioxide film tube furnace of the present invention.
Fig. 2 is to test position and powder position of the substrate in quartz ampoule in vanadium dioxide film growth course of the present invention to show
It is intended to.
Fig. 3 is to heat process chart using tube furnace growing large-area monocrystalline vanadium dioxide film.
Fig. 4 is the present invention in 1000nm SiO2The vanadium dioxide film scanning electron microscope diagram grown on/Si substrates.
Fig. 5 is the present invention in 200nm Si3N4The vanadium dioxide film scanning electron microscope diagram grown on/Si substrates.
Fig. 6 is the vanadium dioxide film scanning electron microscope diagram that the present invention grows on a silicon substrate.
Fig. 7 is the resistance variation with temperature curve map of vanadium dioxide film of the present invention.
Fig. 8 is the resistance variation with temperature X-ray diffractogram of vanadium dioxide film of the present invention.
In figure, 1, air inlet, 2, vacuum meter, 3, quartz ampoule, 4, quartz boat, 5, gas outlet, 6, tubular type furnace control system, 7,
Vanadium pentoxide powder, 8, experiment substrate.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, should
Embodiment is only used for the explanation present invention, does not constitute the restriction to protection scope of the present invention.
As shown in figure 1, one kind of the present invention utilizes tube furnace growing large-area monocrystalline vanadium dioxide film method, using pipe
Formula stove grows vanadium dioxide film, and the tube furnace includes tubular type furnace control system 6 and quartz ampoule 3, and the one end of quartz ampoule 3 is air inlet
1, arrange on the pipeline of air inlet 1 and experiment substrate 8 and quartz boat 4 are put in vacuum meter 2, quartz ampoule 3, test substrate 8 and quartz
Vanadium pentoxide powder 7 is put in boat 4, the other end of quartz ampoule 3 is gas outlet 5.
Experiment substrate 8 selects SiO2/Si、Si3N4/ Si, silicon, quartz or sapphire.Experiment is by controlling intensification during growth
Speed, keeping temperature, rate of temperature fall and gas flow are realizing.
In the present invention, testing substrate aufwuchsplate need to be through polishing;Vanadium pentoxide powder used is pure in experiment
Spend for 99.99%, and nodeless mesh particle;Used carrier gas in experiment is argon gas, and its purity is 99.9999%.
Embodiment 1
As shown in figure 1, the quartz ampoule 3 for being grown in strict closing of vanadium dioxide film is interior complete, at the two ends of quartz ampoule 3 point
It is not air inlet 1 and gas outlet 5;The gentle rate of temperature fall of liter of experiment is set by tubular type furnace control system 6;It is high-quality in order to prepare
The monocrystalline vanadium dioxide film of amount, before tube furnace begins to warm up, to being filled with 1~2 argon gas in quartz ampoule 3, then allows it again
It is evacuated to vacuum state.
A kind of method of utilization tube furnace growing large-area monocrystalline vanadium dioxide film method, it is comprised the following steps:
It is 10 × 10mm from sizes of substrate2SiO2/ Si tests substrate 8, and it with silicon is substrate at it that this experiment substrate 8 is
One layer of 500~1000nm SiO of superficial growth2Film;First to SiO used2/ Si experiment substrates 8 are cleaned, and will test substrate
8 are put in the cleaning gaily decorated basket, experiment substrate 8 is inserted into and cleans placed side by side in gaily decorated basket groove, and each experiment substrate 8 keeps one
Fixed spacing, in order to avoid the inter-adhesive damaging substrate surface between substrate and substrate when ultrasonic wave is cleaned;The first step will be clear
Wash the gaily decorated basket to be put into beaker and pour appropriate acetone into, be put in supersonic wave cleaning machine and clean 10 minutes, until the ultrasound of acetone it is clear
Wash end;Substrate after second step is directly cleaned with acetone is put in the beaker equipped with absolute ethyl alcohol together with the cleaning gaily decorated basket
It is put into again in supersonic wave cleaning machine and cleans 10 minutes.
Cleaned experiment substrate 8 is dried up with nitrogen gun, it is ensured that the clean without grease spot in experiment substrate 8 surface and
Particulate matter.Quartz boat 4 is finally cleaned, quartz boat 4 is put into quartz beaker the inside, first pour appropriate acetone into inside, ultrasound
Cleaning took out quartz boat 4 from quartz beaker the inside after 5 minutes, and directly quartz boat 4 is put in the beaker equipped with absolute ethyl alcohol
Face ultrasound 5 minutes;
As shown in Fig. 2 the purity of the raw material vanadium pentoxide powder 7 used in experiment is 99.99%, due to five oxidations
The inner vanadium oxide particles that there are some crystallizations of two vanadium powder 7, must be processed vanadium pentoxide powder 7 before experiment,
Vanadium pentoxide powder 7 is put into mortar the inside, with alms bowl pestle the vanadium pentoxide powder 7 of crystallization is ground.Experiment every time needs to use
To three quartz boats 4, the vanadium pentoxide powder 7 of 0.1~0.2g is placed with first quartz boat 4, is placed on the interior of quartz ampoule 3
In the middle of the warm area of side, the vanadium pentoxide powder 7 that second quartz boat 4 is placed with 0.07~0.15g is positioned over the outside temperature of quartz ampoule 3
In the middle of area, the vanadium pentoxide powder 7 that 0.1~0.4g is placed with the 3rd quartz boat 4 is positioned over the upstream of second quartz boat 4
Apart from its 5~10mm.Vanadium pentoxide powder 7 is uniformly placed in quartz boat 4, and experiment substrate 8 puts into first and the
In two quartz boats 4, the experiment growth placed face down of substrate 8 tests the height and following vanadium pentoxide powder 7 of substrate 8
Apart from 2mm, wherein not placing experiment substrate 8 on the 3rd quartz boat 4.
As shown in figure 3, a kind of heat technological process using tube furnace growing large-area monocrystalline vanadium dioxide film.To quartz
Pipe 3 carries out envelope chamber, is evacuated to 50~80mTorr, then passes to argon gas, and flow is 10SCCM, by outside warm area and inner side temperature
Area's temperature is raised to 1000 DEG C and 900 DEG C from room temperature respectively, and the heating-up time is all 100 minutes.Quartz in by observing temperature-rise period
The change of air pressure in pipe 3 adjusts in time the air pressure valve of gas outlet 5 so as to which air pressure is controlled 200~700mTorr's in quartz ampoule 3
In the range of, reach the laggard trip temperature of temperature and keep, keep duration 360 minutes, growth is lowered the temperature after terminating, the drop of both sides warm area
The warm time is 600 minutes, and when temperature could open quartz ampoule 3 less than 30 DEG C experiment substrate 8 is taken out.
As shown in figure 4, being using SiO after tube furnace growth experiment2The scanning electron microscope diagram piece of/Si substrates 8.Can in figure
To observe that the vanadium dioxide film rate of film build for preparing is good and surface free from admixture.
Embodiment 2
From 200nm Si3N4/ Si does experiment substrate 8, and its membrane-film preparation process is as described in Example 1;It is evacuated to 50~
80mTorr, then passes to argon gas, and flow is 15SCCM, and respectively outside warm area and inner side warm area temperature are raised to into 900 DEG C from room temperature
With 800 DEG C, the heating-up time all be 40 minutes.The experimental temperature slightly difference that different materials is adopted, general range is 40~80
Between DEG C.The change of air pressure adjusts in time the air pressure valve of gas outlet 5 in quartz ampoule 3 in by observing temperature-rise period so as to quartz
Air pressure is controlled in the range of 300~500mTorr in pipe 3, is reached the laggard trip temperature of temperature and is kept, and the retention time is 200 points
Clock, then controls temperature fall time 360 minutes, and quartz ampoule 3 is opened after temperature is shown less than 30 DEG C, takes out experiment substrate 8.
As shown in figure 5, being using Si after tube furnace growth experiment3N4/ Si substrate scan electron microscope pictures.From picture
In it can be seen that Si3N4/ Si experiment substrate 8 can also growing large-area vanadium dioxide film, but its surface void has one
Fixed space, without SiO2The large area vanadium dioxide film effect that/Si experiment substrates 8 grow out is good, and this is due to difference
The difference reason such as substrate lattice constant, lattice atoms is caused.
Embodiment 3
Experiment substrate 8 is done from silicon, its membrane-film preparation process is as described in Example 1;50~80mTorr is evacuated to, so
After be passed through argon gas, flow is 20SCCM, and respectively outside warm area and inner side warm area temperature are raised to into 950 DEG C and 850 DEG C from room temperature, is risen
The warm time is all 70 minutes.The experimental temperature slightly difference that different materials is adopted, general range is between 40~100 DEG C.It is logical
The change for crossing air pressure in quartz ampoule 3 in observation temperature-rise period adjusts in time the air pressure valve of gas outlet 5 so as to air pressure in quartz ampoule 3
Control reaches the laggard trip temperature of temperature and keeps in the range of 200~400mTorr, and the retention time is 100 minutes, is then controlled
Temperature fall time 500 minutes, opens quartz ampoule 3 after temperature is shown less than 30 DEG C, takes out experiment substrate 8.
As shown in fig. 6, being using silicon chip scanning electron microscope diagram piece after tube furnace growth experiment.Can be with from picture
Find out silicon experiment substrate 8 can also growing large-area vanadium dioxide film, but its surface void has certain space, does not have
There is SiO2The large area vanadium dioxide film effect that/Si experiment substrates 8 grow out is good, and this is because substrates of different lattice is normal
The difference reason such as number, lattice atoms is caused;
Fig. 7 varies with temperature knot for present invention one kind using tube furnace growing large-area monocrystalline vanadium dioxide film resistance
Really.After vanadium dioxide film occurs insulator-metal phase transition at 68 DEG C, resistivity can occur drastically to change, and amplitude of variation reaches 4
Individual most magnitudes, considerably beyond the change in resistance of general polycrystal film material.
As shown in figure 8, for the X-ray diffractogram of vanadium dioxide, it is possible to obtain the composition of material, material internal atom or point
The structure of son.As can be seen from Fig. the film is vanadium dioxide monocrystal thin films, and the natural width of the close instrument of halfwidth, crystal is tied
Brilliant degree is high, and monocrystalline quality is good.A kind of method of utilization tube furnace growing large-area monocrystalline vanadium dioxide film of the present invention overcomes
Said method prepares the deficiency of thin-film material quality, and the change of phase change resistor rate can reach 4~5 orders of magnitude, electricity, optical
Very big lifting can be there has also been.The large area monocrystalline vanadium dioxide film of this utilization tube furnace growth, for expansion vanadium dioxide
Phase-change material application has positive effect.
Claims (5)
- It is 1. a kind of to utilize tube furnace growing large-area monocrystalline vanadium dioxide film method, it is characterised in that:Comprise the following steps that:(1) substrate will be tested and quartz boat will be cleaned by ultrasonic respectively with acetone, absolute ethyl alcohol, it is ensured that experiment substrate and quartz boat surface Totally, without grease and pollutant;(2) vanadium pentoxide powder is put in the experiment substrate and quartz boat of acquisition in step (1), and puts into stone in order In English pipe, experiment every time needs to use three quartz boats, and first quartz boat is placed in the middle of the inner side warm area of quartz ampoule;Second Quartz boat is positioned in the middle of the outside warm area of quartz ampoule;The upstream of second quartz boat is positioned in 3rd quartz boat;Five oxygen Change two vanadium powders to be uniformly placed in quartz boat, experiment substrate is put in first and second quartz boat;(3) after the quartz boat placed in step (2), envelope chamber is carried out to quartz ampoule, is evacuated to 50~80mTorr, then It is passed through argon gas, flow is 5~20SCCM, the temperature of outside warm area and inner side warm area is raised to into 800~1000 DEG C, the used time 40~ 100 minutes, adjusting the air pressure valve of vacuum orifice made its quartzy intraductal atmospheric pressure control in the range of 200~900mTorr, control In 10~20 DEG C/min, temperature reaches 800~1000 DEG C of laggard trip temperatures and keeps heating rate, and the retention time is 180~360 points Clock, then controls 1~2 DEG C/min of rate of temperature fall, and after temperature is shown less than 30 DEG C quartz ampoule is opened, and takes out experiment substrate.
- 2. according to claim 1 a kind of using tube furnace growing large-area monocrystalline vanadium dioxide film method, its feature It is:The tube furnace includes tubular type furnace control system and quartz ampoule, and described quartz ampoule one end is air inlet, the pipe of the air inlet Vacuum meter is set on road, experiment substrate and quartz boat are put in the quartz ampoule, in the experiment substrate and quartz boat five are put into V 2 O powder, the quartz ampoule other end is gas outlet.
- 3. according to claim 1 a kind of using tube furnace growing large-area monocrystalline vanadium dioxide film method, its feature It is:The vanadium pentoxide powder and the 3rd that vanadium pentoxide powder that first quartz boat is placed with, second quartz boat are placed with The mass ratio of the vanadium pentoxide powder being placed with individual quartz boat is 1.5~3:1~2:1.5~6.
- 4. according to claim 1 a kind of using tube furnace growing large-area monocrystalline vanadium dioxide film method, its feature It is:Experiment substrate selects SiO2/Si、Si3N4/ Si, silicon, quartz or sapphire.
- 5. according to claim 1 a kind of using tube furnace growing large-area monocrystalline vanadium dioxide film method, its feature It is:Outside warm area and inner side warm area temperature are raised to 900~1000 DEG C and 800~900 DEG C from room temperature respectively.
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CN111893569A (en) * | 2020-07-13 | 2020-11-06 | 暨南大学 | Vanadium dioxide crystal with good appearance and strong crystallinity, and preparation and application thereof |
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CN112938893A (en) * | 2021-02-09 | 2021-06-11 | 南方科技大学 | Vanadium dioxide single crystal driver and preparation method and application thereof |
CN112981530B (en) * | 2021-02-09 | 2022-04-05 | 南方科技大学 | Vanadium dioxide single crystal micro-nanowire and preparation method and application thereof |
CN112981530A (en) * | 2021-02-09 | 2021-06-18 | 南方科技大学 | Vanadium dioxide single crystal micro-nanowire and preparation method and application thereof |
CN112938893B (en) * | 2021-02-09 | 2023-10-17 | 南方科技大学 | Vanadium dioxide monocrystal driver and preparation method and application thereof |
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CN114086251B (en) * | 2021-12-02 | 2024-05-31 | 中国电子科技集团公司第四十六研究所 | Preparation method of CdS polycrystalline material with high electrical uniformity and low resistance |
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