CN109999850A - A kind of orthorhombic phase group-III chalcogenide catalysis material and preparation method - Google Patents
A kind of orthorhombic phase group-III chalcogenide catalysis material and preparation method Download PDFInfo
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- CN109999850A CN109999850A CN201910329977.0A CN201910329977A CN109999850A CN 109999850 A CN109999850 A CN 109999850A CN 201910329977 A CN201910329977 A CN 201910329977A CN 109999850 A CN109999850 A CN 109999850A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 23
- 150000004770 chalcogenides Chemical class 0.000 title claims abstract description 15
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 34
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 6
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910005543 GaSe Inorganic materials 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004518 low pressure chemical vapour deposition Methods 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 3
- -1 chalcogenide compounds Chemical class 0.000 abstract 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910021389 graphene Inorganic materials 0.000 description 10
- 239000011669 selenium Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 150000001787 chalcogens Chemical class 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of group-III chalcogenide catalysis material and preparation methods, including silver foil substrate is carried out ultrasonic cleaning and the high temperature anneal, and III-VI compounds of group thin slice of uniform size is synthesized using the method for low-pressure chemical vapor deposition.It is kept for 10-20 minutes at the reaction temperatures, until cooled to room temperature, simultaneously closes off and be passed through argon gas and hydrogen, group-III chalcogenide compounds thin-layer sample of uniform size can be obtained in silver foil substrate.The chemical vapour deposition technique that this method uses can be realized on a large scale, and the group-III chalcogenide compounds thin slice of high quality, preparation process is simple, can scale volume production.
Description
Technical field
The invention belongs to field of semiconductor materials, and in particular to a kind of preparation method of the chemical vapor deposition under low pressure,
Preparation has the thin slice of the group-III chalcogenide of potential photocatalysis characteristic in silver foil substrate.
Background technique
From two scientists of Univ Manchester UK An Deliehaimu in 2004 and Constantine Nuo Woxiao love
Two-dimentional carbon nanomaterial graphene is successfully separated, excellent optics, electricity, mechanical characteristic are other class graphene-structureds
Solid foundation is established.This defect of zero band gap of graphene seriously limits it in certain fields, especially in photocatalysis field
Using.In order to increase the chemistry and catalytic activity of graphene, generally require to carry out graphene various chemical modifications to graphene
Nearby density of electronic states carries out modulation to fermi level, enhances the catalytic activity of graphene.But these methods are big to a certain extent
The earth improves the degree-of-difficulty factor of device preparation, and scale application is even more extremely difficult.Two-dimentional chalkogenide has many similar
The even better than characteristic of graphene, such as possess structure similar with graphene and superior physicochemical properties, also
With the unexistent suitable band gap of graphene, typical semiconductor energy band structure is presented, in addition it is in transistor, lithium-ion electric
The application prospect of pond, sensor and photocatalysis etc. is also very wide.And unlike graphene, two-dimentional chalkogenide is also
It can be directly as the catalyst much reacted.Therefore sight has gradually been turned to the moderate chalcogen semiconductor material of band gap by people
Research to adapt to the demand of catalysis material.
Realize above-mentioned application prospect research premise is that preparation is extensive, the two-dimentional chalkogenide of high quality.Wherein,
Two-dimentional III-VI compounds of group as rising in recent years two-dimensional semiconductor material and be concerned.Orthorhombic phase two dimension III-VI at present
There has been no cost-effective methods to obtain for the preparation of compounds of group.Therefore III-VI compounds of group of orthorhombic phase two dimension how is realized
On a large scale, the problem of preparation of validation is current urgent need to resolve.
Summary of the invention
The present invention provides one kind in silver foil substrate, is synthesized using the method for low-pressure chemical vapor deposition of uniform size
The preparation method of III-VI race's catalysis material.Preparation method used of the invention can scale, cost-effective side can be passed through
The group-III chalcogenide of formula acquisition high quality.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of group-III chalcogenide catalysis material, the described method comprises the following steps:
(1) predecessor and pretreated silver foil substrate are successively individually positioned in three-temperature-zone tube furnace according to airflow direction
In;
(2) vacuum degree of reaction chamber is evacuated to 6KPa, is passed through hydrogen and argon gas and the reaction chamber of high temperature process furnances is cleaned;
(3) it is passed through argon gas and hydrogen, while heating the high temperature process furnances of three-temperature-zone, reaction generates the chalcogenide object light of group-III and urges
Change material, is deposited in silver foil substrate.
(4) hydrogen and argon gas are simultaneously closed off after cooled to room temperature, it is chalcogenide group-III can be obtained in substrate
Object thin-layer sample.
Silver foil substrate pretreatment method described in step (1) are as follows: silver foil substrate is put into the NaOH solution of 0.5 mol/L
Middle cleaning, after carried out in deionized water solution ultrasonic cleaning 5 minutes;High annealing of the substrate that cleaning is finished at 900 DEG C
High temperature pre-anneal treatment is carried out in furnace, annealing time is 2 hours.
Step (1) predecessor is for any one in the source S and the source Se with any one in the source In and the source Ga according to matter
Amount is mixed than 1:1-5;The source S is S powder;The source Se is Se powder;The source In is powder In2O3;The source Ga
It is triethyl-gallium.
Carrier gas described in step (2) is the argon gas of flow velocity 50-60sccm and the hydrogen of 10-30sccm.
The heating temperature in the source S described in step (3) is 180-210 DEG C;The heating temperature in the source Se is 250-280
℃;The heating temperature in the source In is 620-650 DEG C;The heating temperature in the source Ga is 70-100 DEG C;The silver foil base
650-700 DEG C of heating temperature of bottom region.
The reaction time of the step (3) is 10-20 minutes.
The method is specifically included that S/Se powder, powder In2O3It is successively placed respectively with silver foil substrate according to airflow direction
In the tube furnace of three-temperature-zone.
The method specifically includes that, by liquid triethyl-gallium, S/Se powder and silver foil substrate are successively distinguished according to airflow direction
It is placed in the tube furnace of three-temperature-zone.
Further, group-III chalcogenide catalysis material, the catalysis material are prepared using the preparation method
Including any one in InSe, InS, GaSe or GaS.
The beneficial effects of the present invention are: it provides a kind of chemical vapour deposition technique and prepares group-III chalcogenide material
Material, compared to other preparation methods, preparation process is simple, is easy to scale.And with traditional III-VI race of hexagonal phase two dimension
Compound is compared, and orthorhombic phase structure also has anisotropic characteristic in addition to having conventional photoelectric property.This special property
A possibility that mass-energy let us obtains the property of significant difference on from different directions, increase as catalysis material.Therefore, institute
Obtained group-III chalcogenide is expected to apply each field, especially photocatalysis field in future.
Detailed description of the invention
Fig. 1 is the preparation flow figure of InSe;
Fig. 2 is the XRD diagram of 1 gained InSe of embodiment;
The SEM that Fig. 3 is 1 gained InSe of embodiment schemes;
Fig. 4 is the absorption coefficient of light figure of 1 gained InSe of embodiment;
Fig. 5 is the XRD diagram of embodiment 2-4 resulting materials.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
A method of two dimension InSe being prepared using Low Pressure Chemical Vapor Deposition, preparation flow figure is as shown in Figure 1, specific steps
It is as follows:
(1) silver foil is placed in sodium hydroxide (0.5mol/L) solution and is cleaned, be subsequently placed in deionized water and be cleaned by ultrasonic 5 points
Clock.By the silver foil after cleaning through row pre-anneal treatment in 900 DEG C of high-temperature annealing furnace, annealing time is 2 hours;
(2) by the selenium powder of 1g, the indium oxide of 2g and 10 silver foil substrates are respectively placed in three-temperature-zone tubular type according to airflow direction
In furnace, wherein the spacing of silver foil substrate is 1cm;
(3) vacuum degree of tube furnace is evacuated to 6KPa, argon gas and hydrogen is passed through simultaneously with the flow velocity of 50sccm and 20sccm, cleaned
Reaction chamber;
(4) it is continually fed into gas, heats the temperature of three-temperature-zone tube furnace to 270 DEG C, 630 DEG C and 680 simultaneously in 20min
DEG C, stop heating after 15min is kept under the action of air-flow;
(5) cooled to room temperature simultaneously closes off argon gas and hydrogen, obtains InSe.
XRD diagram, SEM figure and the absorption coefficient of light figure for the InSe being prepared are distinguished as shown in Figure 2,3, 4.The XRD diagram of Fig. 2
There are two apparent diffraction maximums.The SEM image of Fig. 3 can be evident that InSe is in gill shape film two-dimensional material.Fig. 4
Absorption coefficient of light figure show apparent anisotropy, and in visible light and UV light region, InSe material is all showed
Good smooth capture ability out.
Embodiment 2
A method of two dimension InS is prepared using Low Pressure Chemical Vapor Deposition, the specific steps are as follows:
(1) silver foil is placed in sodium hydroxide (0.5mol/ L) solution and is cleaned, be subsequently placed in deionized water and be cleaned by ultrasonic 5
Minute.By the silver foil after cleaning through row pre-anneal treatment in 900 DEG C of high-temperature annealing furnace, annealing time is 2 hours;
(2) by 1g sulphur powder, the indium oxide of 4g and 10 silver foil substrates are respectively placed in three-temperature-zone tube furnace according to airflow direction
In, wherein the spacing of silver foil substrate is 1cm;
(3) vacuum degree of tube furnace is evacuated to 6Kpa, argon gas and hydrogen is passed through simultaneously with the flow velocity of 50sccm and 10sccm, cleaned
Reaction chamber;
(4) it is continually fed into gas, heats the temperature of three-temperature-zone tube furnace to 200 DEG C, 630 DEG C and 670 simultaneously in 20min
DEG C, stop heating after 15min is kept under the action of air-flow;
(5) cooled to room temperature simultaneously closes off argon gas and hydrogen, obtains InS.
Embodiment 3
A method of two dimension GaSe is prepared using Low Pressure Chemical Vapor Deposition, the specific steps are as follows:
(1) silver foil is placed in sodium hydroxide (0.5mol/ L) solution and is cleaned, be subsequently placed in deionized water and be cleaned by ultrasonic 5
Minute.By the silver foil after cleaning through row pre-anneal treatment in 900 DEG C of high-temperature annealing furnace, annealing time is 2 hours;
(2) by 2g triethyl-gallium, 1g selenium powder and 10 silver foil substrates are respectively placed in three-temperature-zone tube furnace according to airflow direction
In, wherein the spacing of silver foil substrate is 1cm;
(3) vacuum degree of tube furnace is evacuated to 6KPa, argon gas and hydrogen is passed through simultaneously with the flow velocity of 60sccm and 20sccm, cleaned
Reaction chamber;
(4) it is continually fed into gas, heats the temperature of three-temperature-zone tube furnace to 100 DEG C, 250 DEG C and 690 simultaneously in 20min
DEG C, stop heating after 15min is kept under the action of air-flow;
(5) cooled to room temperature simultaneously closes off argon gas and hydrogen, obtains GaSe.
Embodiment 4
A method of two dimension GaS is prepared using Low Pressure Chemical Vapor Deposition, the specific steps are as follows:
(1) silver foil is placed in sodium hydroxide (0.5mol/ L) solution and is cleaned, be subsequently placed in deionized water and be cleaned by ultrasonic 5
Minute.By the silver foil after cleaning through row pre-anneal treatment in 900 DEG C of high-temperature annealing furnace, annealing time is 2 hours;
(2) by 5g triethyl-gallium, 1g sulphur powder and 10 silver foil substrates are respectively placed in three-temperature-zone tube furnace according to airflow direction
In, wherein the spacing of silver foil substrate is 1cm;
(3) vacuum degree of tube furnace is evacuated to 6KPa, argon gas and hydrogen is passed through simultaneously with the flow velocity of 60sccm and 30sccm, cleaned
Reaction chamber;
(4) it is continually fed into gas, heats the temperature of three-temperature-zone tube furnace to 70 DEG C, 210 DEG C and 700 simultaneously in 20min
DEG C, stop heating after 15min is kept under the action of air-flow;
(5) cooled to room temperature simultaneously closes off argon gas and hydrogen, obtains GaS.
The XRD diagram of embodiment 2-4 resulting materials is as shown in Figure 5.
Claims (9)
1. a kind of preparation method of orthorhombic phase group-III chalcogenide catalysis material, which is characterized in that the method includes
Following steps:
(1) predecessor and pretreated silver foil substrate are successively individually positioned in three-temperature-zone tube furnace according to airflow direction
In;
(2) vacuum degree of reaction chamber is evacuated to 6KPa, is passed through hydrogen and argon gas and the reaction chamber of high temperature process furnances is cleaned;
(3) it is passed through argon gas and hydrogen, while heating the high temperature process furnances of three-temperature-zone, reaction generates the chalcogenide object light of group-III
Catalysis material is deposited in silver foil substrate;
(4) hydrogen and argon gas are simultaneously closed off after cooled to room temperature, the chalcogenide materialization of group-III can be obtained in substrate
Close object thin-layer sample.
2. preparation method according to claim 1, which is characterized in that silver foil substrate pretreatment method described in step (1)
Are as follows: silver foil substrate is put into the NaOH solution of 0.5 mol/L and is cleaned, after carried out in deionized water solution ultrasonic cleaning 5 points
Clock;The substrate that cleaning finishes is subjected to high temperature pre-anneal treatment in 900 DEG C of high-temperature annealing furnace, annealing time is 2 hours.
3. preparation method according to claim 1, which is characterized in that step (1) predecessor is in the source S and the source Se
Any one is mixed with any one in the source In and the source Ga according to mass ratio 1:1-5;The source S is S powder;The source Se is
Se powder;The source In is powder In2O3;The source Ga is triethyl-gallium.
4. requiring the preparation method according to right 1, which is characterized in that carrier gas described in step (2) is flow velocity 50-60sccm
Argon gas and 10-30sccm hydrogen.
5. preparation method according to claim 1, which is characterized in that the heating temperature in the source S described in step (3) is 180-
210℃;The heating temperature in the source Se is 250-280 DEG C;The heating temperature in the source In is 620-650 DEG C;Described
The heating temperature in the source Ga is 70-100 DEG C;650-700 DEG C of heating temperature of the silver foil basal region.
6. preparation method according to claim 1, which is characterized in that the reaction time of the step (3) is 10-20 points
Clock.
7. preparation method according to claim 1-6, which is characterized in that the method is specifically included that S/Se
Powder, powder In2O3It is successively individually positioned in the tube furnace of three-temperature-zone with silver foil substrate according to airflow direction.
8. preparation method according to claim 1-6, which is characterized in that the method is specifically included that liquid
Triethyl-gallium, S/Se powder and silver foil substrate are successively individually positioned in the tube furnace of three-temperature-zone according to airflow direction.
9. the group-III chalcogenide catalysis material being prepared using preparation method described in claim 1, the light
Catalysis material includes any one in InSe, InS, GaSe or GaS.
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Cited By (2)
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CN110983297A (en) * | 2019-12-23 | 2020-04-10 | 重庆大学 | Method for preparing uniform material layer based on chemical vapor deposition |
CN113445025A (en) * | 2021-06-03 | 2021-09-28 | 东北林业大学 | Preparation of wafer-level two-dimensional In by chemical vapor deposition2Se3Method for making thin film |
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CN103194729A (en) * | 2013-03-27 | 2013-07-10 | 中国科学院物理研究所 | Method for preparing metal chalcogenide film |
CN105887045A (en) * | 2015-02-16 | 2016-08-24 | 炬力奈米科技有限公司 | Method And Apparatus For Fabricating Two-Dimensional Layered Chalcogenide Film |
CN107815663A (en) * | 2017-10-19 | 2018-03-20 | 深圳大学 | A kind of effectively lifting individual layer two dimension Transition-metal dichalcogenide yield, the method for quality |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110983297A (en) * | 2019-12-23 | 2020-04-10 | 重庆大学 | Method for preparing uniform material layer based on chemical vapor deposition |
CN113445025A (en) * | 2021-06-03 | 2021-09-28 | 东北林业大学 | Preparation of wafer-level two-dimensional In by chemical vapor deposition2Se3Method for making thin film |
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