CN109023297A - A kind of preparation method of large scale single layer selenium subregion doping tungsten disulfide thin-film material - Google Patents
A kind of preparation method of large scale single layer selenium subregion doping tungsten disulfide thin-film material Download PDFInfo
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- CN109023297A CN109023297A CN201810944786.0A CN201810944786A CN109023297A CN 109023297 A CN109023297 A CN 109023297A CN 201810944786 A CN201810944786 A CN 201810944786A CN 109023297 A CN109023297 A CN 109023297A
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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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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Abstract
The present invention relates to a kind of preparation method of large scale single layer selenium subregion doping tungsten disulfide thin-film material, preparation process is as follows: by Al2O3Substrate is placed on the quartz boat for filling tungsten source, and the quartz boat is placed in the high-temperature region of double temperature-area tubular furnaces;The quartz boat for filling sulphur source and selenium source is placed in double temperature-area tubular furnace low-temperature spaces, wherein the mass ratio S:Se of sulphur source and selenium source is 0.25-4, and double temperature-area tubular furnaces are encapsulated;Make the pressure normal pressure of reaction chamber under an argon atmosphere, the rate of heat addition that low-temperature space in double temperature-area tubular furnaces is arranged is 7-8 DEG C/min, rises to 240-280 DEG C of reaction temperature after 30-40min, and maintain this reaction temperature 15-20min;The rate of heat addition that double temperature-area tubular furnace high temperature areas are arranged is 20-22.5 DEG C/min, rises to 900-1000 DEG C of reaction temperature after 40-50min, and maintain this reaction temperature 5-10min;Deng being down to room temperature naturally after reaction.
Description
Technical field
The present invention relates to a kind of preparation methods of large scale single layer selenium subregion doping tungsten disulfide thin-film material, belong to and partly lead
Film material preparation field.
Background technique
With the rise of the two-dimensional layers such as graphene nano materials research upsurge in recent years, a kind of novel two-dimensional layer
It closes object-class graphene transient metal chalcogenide compound (TDMCs) and causes the wide of the various fields researcher such as physics, chemistry
General concern.The general formula of molecular structure of this kind of materials is expressed as MX2, wherein M is transition metal, such as IV race's element (Ti), V
Race's element (V etc.) and VI race's element (Mo, W etc.);X is chalcogenide, such as S, Se and Te etc.;Typical compound has tungsten disulfide
(WS2), two tungsten selenide (WSe2) etc..Such compound all has " sandwich folder by what the single-layer or multi-layer of hexagonal crystal system formed
The two dimensional crystal material of the heart " layer structure is sandwiched in two layers wherein one layer of metallic molecule forms hexaplanar and keeps apart to obtain chalcogen
Among molecule, the crystal for forming bulk is combined between adjacent atomic layer by faint model ylid bloom action power;Due to layer and layer it
Between way of stacking it is different with interatomic coordination mode, the crystal of transient metal chalcogenide compound can be divided into hexagonal by its symmetry
Crystallographic system and orthorhombic system.
Different from the graphene with two-dimensional layered structure, class graphene transient metal chalcogenide compound has special energy
Band structure, compared to zero band gap of graphene, such compound usually possesses the natural band-gap energy of 1.0-2.0eV.Single layer two
The band gap of tungsten sulfide reaches 2.0eV due to quantum confined effect;And the band gap of two tungsten selenide of single layer reaches 1.7eV.Due to
Its big band gap and relatively high carrier mobility its possess in field of photovoltaic materials and be widely applied.
In order to improve class graphene transient metal chalcogenide compound in the performance of photoelectric device, the band gap for adjusting the material is
One important solution is also a bottleneck, because seldom there is nature band gap in nature in the natural of 1.0-2.0eV
Ore compound, and can be obtained by simply removing intercalation method.Many modes can be realized to two-dimensional layer material band gap
Adjustment, such as chemical doping, ion implanting and on the surface of the material introduce functional group.Recently, theoretical calculation and experimental study be all
Demonstrate the preparation of the adjustable two-dimensional layer semiconductor material of achievable band gap.Chemical vapor deposition method must can effectively pass through
Change sulphur/selenium element ratio and prepares the adjustable selenium doping tungsten disulfide of band gap.
Only single layer or few layer just have the performance in terms of the excellent photoelectricity of above structure, therefore primary and important task
It is to prepare single layer or few adjustable material of this kind of band gap of layer.The ruler for the selenium doping tungsten disulfide film reported in recent document
Very little all smaller, large-sized selenium doping tungsten disulfide film also obtains not successfully, it is therefore desirable to study larger sized selenium and mix
Miscellaneous tungsten disulfide film, while having that high quality, uniformity be good, the single layer selenium doping tungsten disulfide film material of selenium subregion doping
Material;It realizes a large amount of preparations, can achieve the requirement of industrial mass production.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of large scale single layer selenium subregion doping tungsten disulfide thin-film material
Method obtains large scale single layer selenium subregion by aumospheric pressure cvd legal system and adulterates tungsten disulfide thin-film material, and size reaches
1000-2000 square micron, while having many advantages, such as that high quality, single layer, uniformity be good, good crystallinity, this method operation letter
Single, less energy consumption has reached the requirement of large-scale production.The present invention is realized by the following technical scheme, and passes through selection
Tungsten source, sulphur source and selenium source issue biochemical reaction in the double temperature-area tubular furnace high temperature condition of normal pressure of chemical vapor deposition, then sink
Product arrives growth substrate surface, ultimately generates large scale single layer selenium subregion doping tungsten disulfide thin-film material.
A kind of preparation method of large scale single layer selenium subregion doping tungsten disulfide thin-film material, it is heavy using atmospheric chemical vapor
Area method and double temperature-area tubular furnaces, with Al2O3For growth substrate, using WO3As tungsten source, the sulphur powder that distils is as sulphur source, selenium grain conduct
Selenium source obtains the single layer selenium subregion doping tungsten disulfide thin-film material having a size of 1000-2000 square micron, and preparation process is such as
Under:
(1) by Al2O3Substrate is placed on the quartz boat for filling tungsten source, and the quartz boat is placed in double temperature-area tubular furnaces
High-temperature region;The quartz boat for filling sulphur source and selenium source is placed in double temperature-area tubular furnace low-temperature spaces, wherein the mass ratio of sulphur source and selenium source
S:Se is 0.25-4, and double temperature-area tubular furnaces are encapsulated;
(2) make the pressure normal pressure of reaction chamber under an argon atmosphere, the heating of low-temperature space in double temperature-area tubular furnaces is set
Rate is 7-8 DEG C/min, rises to 240-280 DEG C of reaction temperature after 30-40min, and maintain this reaction temperature 15-20min;If
The rate of heat addition for setting double temperature-area tubular furnace high temperature areas is 20-22.5 DEG C/min, rises to reaction temperature 900- after 40-50min
1000 DEG C, and maintain this reaction temperature 5-10min;Deng being down to room temperature naturally after reaction.
Before step (1), the preprocess method of growth substrate Al2O3 can be such that respectively in deionized water, third
Ultrasonic mode cleans the organic substance impurity of removal substrate surface in ketone, chloroform and aqueous isopropanol, is used again using preceding
Deionized water rinses substrate, and is dried up with nitrogen gun.
The present invention is using aumospheric pressure cvd method and double temperature-area tubular furnaces, with Al2O3For growth substrate, using WO3Make
For tungsten source, the sulphur powder that distils is used as sulphur source, selenium grain as selenium source, it is available with high quality, uniformity is good, selenium subregion of single layer
Adulterate tungsten disulfide thin-film material.Preparation method of the present invention is simple and easy to operate, the time is short, reproducible, to instrument and equipment requirement
It is low.The single layer that high quality, the uniformity obtained by chemical vapour deposition technique is good, size can reach 1000-2000 square micron
Selenium subregion adulterates tungsten disulfide thin-film material, for other methods for preparing selenium doping tungsten disulfide, thin-film material
Size increases an order of magnitude, there is apparent advantage, prepares obtained thin-film material and is expected to be applied to photoswitch, photoelectricity crystalline substance
The fields such as body pipe, optical detector.
Detailed description of the invention:
Fig. 1 is the experiment easy device figure that selenium subregion prepared by embodiment 1 adulterates tungsten disulfide thin-film material.Sulphur source and selenium
Source is placed in low-temperature space, and reaction temperature is set as 280 DEG C;Tungstic acid is placed in high-temperature region, and reaction temperature is set as 1000 DEG C;
Carrier gas argon gas enters high-temperature region from the low-temperature space of double temperature-area tubular furnaces.
Fig. 2 is the light microscopic figure that selenium subregion prepared by embodiment 1 adulterates tungsten disulfide thin-film material.The upper left corner is baseplate material
Al2O3Piece, other regions are that selenium subregion adulterates tungsten disulfide thin-film material, and good film-forming property, integrity degree is high, the ruler of thin-film material
It is very little to can achieve 1000 square microns.
Fig. 3 is the AFM figure that selenium subregion prepared by embodiment 1 adulterates tungsten disulfide thin-film material.Photo shows selenium obtained
Subregion adulterate tungsten disulfide thin-film material with a thickness of 0.75nm (shown in right part of flg), be single layer structure.
Fig. 4 is the TEM figure that selenium subregion prepared by embodiment 2 adulterates tungsten disulfide thin-film material.Photo shows selenium obtained
It is single layer that subregion, which adulterates tungsten disulfide thin-film material,.
Fig. 5 is the TEM figure that selenium subregion prepared by embodiment 3 adulterates tungsten disulfide thin-film material, by picture it is found that selenium is to two
Tungsten sulfide has carried out subregion doping, and tungsten disulfide and two tungsten selenide subregions are present in film.
Fig. 6 (1), (2) and (3) is the XPS figure that selenium subregion prepared by embodiment 1,2 and 3 adulterates tungsten disulfide thin-film material,
Peak-fit processing has been done to S element respectively.By picture it is found that having prepared different selenium doping tungsten disulfide thin-film materials, implement
Corresponding S:Se is respectively 0.54,0.96 and 3.98 in film prepared by example 1,2 and 3.
Specific embodiment
Technology path of the invention is as follows:
(1) growth substrate used in this experiment is Al2O3Piece, by respectively in deionized water, acetone, chloroform
The impurity such as the organic substance of removal substrate surface are cleaned with mode ultrasonic in aqueous isopropanol, are rushed again with deionized water using preceding
Substrate is washed, and spare with nitrogen gun drying.By treated, growth substrate is placed on the quartz boat for filling tungsten source, and by the stone
Ying Zhou is placed in the high-temperature region of double temperature-area tubular furnaces, for carrier gas, positioned at the outlet side of tube furnace;To fill sulphur source and
The quartz boat of selenium source is placed in the low-temperature space of double temperature-area tubular furnaces, for carrier gas, positioned at the inlet end of tube furnace, wherein
The original quality of sulphur source and selenium source ratio (S:Se) is 0.25-4, and double temperature-area tubular furnaces are encapsulated.
(2) when reaction starts, by the inert gas argon gas access tube formula furnace of 500-1000sccm, using mechanical pump to reaction
Chamber carries out pumping process, so that the pressure of reaction chamber is extracted into low pressure 1turr, is arranged by the way of ventilating while being evacuated
Air in net double temperature-area tubular furnaces, prevents the air impact selenium in pyroreaction in tube furnace from adulterating tungsten disulfide film
It generates and deposits.Sulphur/selenium source will shift to an earlier date tungsten source 10min and reach sublimation temperature, when double temperature-area tubular furnaces are begun to warm up, adjust argon gas
Flow be 50sccm.The rate of heat addition that double temperature-area tubular furnace low-temperature spaces are arranged is 7-8 DEG C/min, rises to reaction after 30-40min
240-280 DEG C of temperature, and maintain this reaction temperature 15-20min.The rate of heat addition that double temperature-area tubular furnace high temperature areas are arranged is
20-22.5 DEG C/min, 900-1000 DEG C of reaction temperature is risen to after 40-50min, and maintain this reaction temperature 5-10min;Deng anti-
Naturally room temperature is down to after answering.
(3) temperature is cooled to room temperature, and substrate is taken out from double temperature-area tubular furnaces, has just obtained the single layer selenium of oversize
Subregion adulterates tungsten disulfide thin-film material.
3 embodiments of the invention are given below, are that rather than model of the invention is limited to further explanation of the invention
It encloses.
Embodiment 1
Weigh 5mg tungsten trioxide powder, 100mg sulphur powder and 400mg selenium powder (mass ratio of sulphur source and selenium source is 0.25) point
It is not placed in 30 × 60mm pottery quartz boat, the growth substrate (Al that will be handled well2O3) it is respectively placed in deionized water, acetone, three chloromethanes
Alkane and each ultrasound 20min of isopropanol rinse base with deionized water again using preceding with impurity such as the organic substances that removes substrate surface
Plate, and dried up with nitrogen gun.By treated, substrate is placed on the quartz boat for filling tungsten source, and the quartz boat is placed in dual temperature
The lower warm area (for carrier gas, positioned at the outlet side of tube furnace) of area's tube furnace, will fill the quartz boat of sulphur source and selenium source
It is placed in the upper warm area (for carrier gas, positioned at the inlet end of tube furnace) of double temperature-area tubular furnaces, finally encapsulates tube furnace.It will
The inert gas argon gas access tube formula furnace of 1000sccm carries out pumping process to reaction chamber using mechanical pump, makes reaction chamber
Pressure be extracted into low pressure 1turr, the air in double temperature-area tubular furnaces is emptied by the way of ventilating while being evacuated, is prevented
The generation and deposition of air impact selenium doping tungsten disulfide film in pyroreaction in tube furnace.Sulphur/selenium source will shift to an earlier date tungsten
Source 10min reaches sublimation temperature, and when double temperature-area tubular furnaces are begun to warm up, the flow for adjusting argon gas is 50sccm.Dual temperature area is set
The rate of heat addition of warm area is 7 DEG C/min on tube furnace, rises to 280 DEG C of reaction temperature after 40min, keeps temperature 15min;Setting
The rate of heat addition of warm area is 20 DEG C/min under double temperature-area tubular furnaces, rises to 1000 DEG C of reaction temperature after 50min, keeps the temperature
5min;It is down to room temperature naturally after reaction.It is down to room temperature naturally after reaction.Temperature is cooled to room temperature, by substrate from pipe
It is taken out in formula furnace, has just obtained the selenium doping tungsten disulfide thin-film material of the good oversize of uniformity.It can be obtained from Fig. 6 (1)
Out, the S:Se in the thin-film material is 0.54.The size of the tungsten disulfide thin-film material of selenium subregion doping simultaneously can achieve
1000 square microns.
Embodiment 2
5mg tungsten trioxide powder, 250mg sulphur powder and 250mg selenium powder (mass ratio of sulphur source and selenium source is 1) is weighed to set respectively
In the substrate (Al that in the pottery quartz boat of 30 × 60mm, will be handled well2O3) it is respectively placed in deionized water, acetone, chloroform and different
Each ultrasound 20min of propyl alcohol rinses substrate with deionized water again using preceding with impurity such as the organic substances that removes substrate surface, and
It is dried up with nitrogen gun.By treated, substrate is placed on the quartz boat for filling tungsten source, and the quartz boat is placed in dual temperature area pipe
The lower warm area (for carrier gas, positioned at the outlet side of tube furnace) of formula furnace, the quartz boat for filling sulphur source and selenium source is placed in
The upper warm area (for carrier gas, positioned at the inlet end of tube furnace) of double temperature-area tubular furnaces, finally encapsulates tube furnace.It will
The inert gas argon gas access tube formula furnace of 750sccm carries out pumping process to reaction chamber using mechanical pump, makes reaction chamber
Pressure is extracted into low pressure 1turr, and the air in double temperature-area tubular furnaces is emptied by the way of ventilating while being evacuated, is prevented
The generation and deposition of air impact selenium doping tungsten disulfide film in pyroreaction in tube furnace.Sulphur/selenium source will shift to an earlier date tungsten source
10min reaches sublimation temperature, and when double temperature-area tubular furnaces are begun to warm up, the flow for adjusting argon gas is 50sccm.Dual temperature area is arranged to manage
The rate of heat addition of warm area is 7.5 DEG C/min on formula furnace, rises to 270 DEG C of reaction temperature after 36min, keeps temperature 17.5min;If
The rate of heat addition for setting warm area under double temperature-area tubular furnaces is 21 DEG C/min, rises to 750 DEG C of reaction temperature after 46min;Keep the temperature
7.5min;It is down to room temperature naturally after reaction.As can be drawn from Figure 2, which adulterates tungsten disulfide thin-film material
Size can achieve 1500 square microns.As can be drawn from Figure 6, which is single thin film;It should can be with from Fig. 6 (2)
It obtains, S:Se is 0.96 in the thin-film material.
Embodiment 3
5mg tungsten trioxide powder, 400mg sulphur powder and 100mg selenium powder (mass ratio of sulphur source and selenium source is 4) is weighed to set respectively
In the substrate (Al that in the pottery quartz boat of 30 × 60mm, will be handled well2O3) it is respectively placed in deionized water, acetone, chloroform and different
Each ultrasound 20min of propyl alcohol rinses substrate with deionized water again using preceding to remove the impurity and organic substance of substrate surface, and
It is dried up with nitrogen gun.By treated, substrate is placed on the quartz boat for filling tungsten source, and the quartz boat is placed in dual temperature area pipe
The high-temperature region (for carrier gas, positioned at the outlet side of tube furnace) of formula furnace, the quartz boat for filling sulphur source and selenium source is placed in
The low-temperature space (for carrier gas, positioned at the inlet end of tube furnace) of double temperature-area tubular furnaces, finally encapsulates tube furnace.It will
The inert gas argon gas access tube formula furnace of 500sccm carries out pumping process to reaction chamber using mechanical pump, makes reaction chamber
Pressure is extracted into low pressure 1turr, and the air in double temperature-area tubular furnaces is emptied by the way of ventilating while being evacuated, is prevented
The generation and deposition of air impact selenium doping tungsten disulfide film in pyroreaction in tube furnace.Sulphur/selenium source will shift to an earlier date tungsten source
10min reaches sublimation temperature, and when double temperature-area tubular furnaces are begun to warm up, the flow for adjusting argon gas is 50sccm.Dual temperature area is arranged to manage
The rate of heat addition of formula furnace low-temperature space is 8 DEG C/min, rises to 240 DEG C of reaction temperature after 30min;Keep temperature 20min;Setting is double
The rate of heat addition of temperature-area tubular furnace high-temperature region is 22.5 DEG C/min, rises to 900 DEG C of reaction temperature after 40min;Keep the temperature
10min;It is down to room temperature naturally after reaction.From Fig. 6 (3), it can be concluded that, S:Se is 3.98 in the thin-film material.The selenium simultaneously
The size of subregion doping tungsten disulfide thin-film material can achieve 2000 square microns.
Claims (2)
1. a kind of preparation method of large scale single layer selenium subregion doping tungsten disulfide thin-film material, using aumospheric pressure cvd
Method and double temperature-area tubular furnaces, with Al2O3For growth substrate, using WO3As tungsten source, the sulphur powder that distils is as sulphur source, and selenium grain is as selenium
Source obtains the single layer selenium subregion doping tungsten disulfide thin-film material having a size of 1000-2000 square micron, and preparation process is as follows:
(1) by Al2O3Substrate is placed on the quartz boat for filling tungsten source, and the quartz boat is placed in the high temperature of double temperature-area tubular furnaces
Area;The quartz boat for filling sulphur source and selenium source is placed in double temperature-area tubular furnace low-temperature spaces, wherein the mass ratio S:Se of sulphur source and selenium source
For 0.25-4, and double temperature-area tubular furnaces are encapsulated;
(2) make the pressure normal pressure of reaction chamber under an argon atmosphere, the rate of heat addition of low-temperature space in double temperature-area tubular furnaces is set
For 7-8 DEG C/min, 240-280 DEG C of reaction temperature is risen to after 30-40min, and maintain this reaction temperature 15-20min;Setting is double
The rate of heat addition in temperature-area tubular furnace high temperature area is 20-22.5 DEG C/min, rises to 900-1000 DEG C of reaction temperature after 40-50min,
And maintain this reaction temperature 5-10min;Deng being down to room temperature naturally after reaction.
2. preparation method according to claim 1, which is characterized in that before step (1), to growth substrate Al2O3's
Preprocess method is as follows: mode ultrasonic in deionized water, acetone, chloroform and aqueous isopropanol cleans removal base respectively
The organic substance impurity of plate surface rinses substrate with deionized water again using preceding, and is dried up with nitrogen gun.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110257906A (en) * | 2019-07-23 | 2019-09-20 | 西北工业大学 | A kind of two dimension Transition-metal dichalcogenide crystal and its preparation method and application |
CN110734092A (en) * | 2019-10-28 | 2020-01-31 | 华南师范大学 | monoatomic layer tungsten disulfide two-dimensional material and preparation method and application of reverse physical vapor deposition thereof |
CN111218717A (en) * | 2020-02-17 | 2020-06-02 | 燕山大学 | Growing Fe-doped single-layer WS2Method for two-dimensional crystallization |
CN113122819A (en) * | 2021-04-09 | 2021-07-16 | 安徽大学 | Preparation method of tantalum-doped large-area two-dimensional niobium disulfide material |
CN113278949A (en) * | 2021-04-16 | 2021-08-20 | 中国计量大学 | Preparation method for single-layer molybdenum selenide sulfide alloy with adjustable components |
CN114540956A (en) * | 2021-12-29 | 2022-05-27 | 杭州电子科技大学 | Preparation method of niobium-doped two-dimensional tungsten sulfide crystal material |
CN114835090A (en) * | 2022-05-08 | 2022-08-02 | 中国科学院重庆绿色智能技术研究院 | Electrochemical sensor manufacturing method based on tungsten diselenide with vertical structure |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20150075594A1 (en) * | 2013-09-17 | 2015-03-19 | National Tsing Hua University | W18o49-type tungsten oxide nanomaterial and applications thereof in light sensor, mosfet and solar cell |
CN104649326A (en) * | 2015-02-11 | 2015-05-27 | 中国科学技术大学 | Selenium doped transition metal sulfide single-layer film and preparation method thereof |
CN105624643A (en) * | 2016-01-06 | 2016-06-01 | 天津大学 | Preparation method for large-area selenium doped molybdenum disulfide thin film material |
CN106007796A (en) * | 2016-05-23 | 2016-10-12 | 浙江师范大学 | Preparation method of tungsten disulfide single-layer thin film |
CN108365092A (en) * | 2018-01-18 | 2018-08-03 | 南京大学 | A kind of high temperature resistant memristor based on two-dimensional atomic crystal |
-
2018
- 2018-08-19 CN CN201810944786.0A patent/CN109023297A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20150075594A1 (en) * | 2013-09-17 | 2015-03-19 | National Tsing Hua University | W18o49-type tungsten oxide nanomaterial and applications thereof in light sensor, mosfet and solar cell |
CN104649326A (en) * | 2015-02-11 | 2015-05-27 | 中国科学技术大学 | Selenium doped transition metal sulfide single-layer film and preparation method thereof |
CN105624643A (en) * | 2016-01-06 | 2016-06-01 | 天津大学 | Preparation method for large-area selenium doped molybdenum disulfide thin film material |
CN106007796A (en) * | 2016-05-23 | 2016-10-12 | 浙江师范大学 | Preparation method of tungsten disulfide single-layer thin film |
CN108365092A (en) * | 2018-01-18 | 2018-08-03 | 南京大学 | A kind of high temperature resistant memristor based on two-dimensional atomic crystal |
Non-Patent Citations (2)
Title |
---|
YANG L ET AL.: ""Large-area synthesis of monolayered MoS2(1−x)Se2x with a tunable band gap and its enhanced electrochemical catalytic activity"", 《NANOSCALE》 * |
YINGJIE CAO ET AL: ""Morphology engineering of monolayer MoS2 by adjusting chemical environment during growth"", 《PHYSICA E》 * |
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