CN105734529B - A kind of synthetic method of molybdenum disulfide nano wall - Google Patents
A kind of synthetic method of molybdenum disulfide nano wall Download PDFInfo
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- CN105734529B CN105734529B CN201610147322.8A CN201610147322A CN105734529B CN 105734529 B CN105734529 B CN 105734529B CN 201610147322 A CN201610147322 A CN 201610147322A CN 105734529 B CN105734529 B CN 105734529B
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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
- C23C16/22—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
- 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
- C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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Abstract
A kind of synthetic method of molybdenum disulfide nano wall, is related to a kind of synthetic method of molybdenum disulfide nano material.The problem of the present invention is to solve the preparation methods of existing molybdenum disulfide nano material there are intake and stop time point that solid-state sulphur source not can control sulphur source, and gaseous state sulphur source can bring impurity, reduce purity, easily cause security risk.Method: one, cleaning silicon chip；Two, it by silicon wafer and is respectively provided with the quartz boat of molybdenum trioxide powder and sulphur powder and is put into the quartz ampoule of chemical vapor deposition unit, start vacuum pump, be passed through argon gas or nitrogen, heats up, it maintains, stop heating, improves gas flow rate, it is cooling, close vacuum pump, restore normal pressure, takes out silicon wafer, that is, complete the growth of molybdenum disulfide nano wall.This method does not introduce impurity element into system, guarantees sample degree of purity.It can be very good the intake and stop time point of control sulphur source, method is simple, easy to operate.The present invention is used for the growth of molybdenum disulfide nano wall.
Description
Technical field
The present invention relates to a kind of synthetic methods of molybdenum disulfide nano material.
Background technique
Molybdenum disulfide (molybdenum disulfide) is typical layer structure, between layers with weaker model moral
Wa Ersili is combined；Each molybdenum atom is surrounded by six sulphur atoms.Molybdenum disulfide because its special layer structure and it is each to
The opposite sex, application in the industry are growing, and are applied to friction, lubrication, catalytic refining, electron probe, hydrogen storage material, electrode material
The numerous areas such as material and PhotoelectrochemicalSystem System for Hydrogen Production catalyst.It is considered as class grapheme material, be constantly subjected to from physics, material and
The generally favor of the different fields researcher such as chemistry.
There are many acquisition modes, such as mechanical force removing, electrochemical stripping, chemical vapor deposition for nanostructure molybdenum disulfide
Growth etc., the molybdenum disulfide of more different structures can be grown using chemical vapor deposition method, and more at present is to utilize
Chemical vapor deposition method grows single layer or few layer molybdenum disulfide nano thin slice.By experimental study, molybdenum disulfide has on surface
There is stronger chemical inertness, just there is higher chemical activity in the region for exposing Mo-S key only at section.
Sulphur source generallys use solid-state and two kinds of gaseous state, solid-state sulphur source in the preparation method of existing molybdenum disulfide nano material
For sulphur powder etc., solid-state sulphur source not can control the intake and stop time point of sulphur source；Gaseous state sulphur source is carbon disulfide, hydrogen sulfide
Deng.Gaseous state sulphur source can bring impurity, reduce the purity of molybdenum disulfide, and gaseous state sulphur source is inflammable and explosive, causes security risk.
Summary of the invention
The present invention is to solve the preparation method of existing molybdenum disulfide nano material, there are solid-state sulphur sources not can control sulphur source
Intake and stop time point, gaseous state sulphur source can bring impurity, reduce purity, the problem of easily causing security risk, provide one
The synthetic method of kind molybdenum disulfide nano wall.
The synthetic method of molybdenum disulfide nano wall of the present invention, sequentially includes the following steps:
One, prepare: successively silicon wafer being cleaned by ultrasonic using acetone, dehydrated alcohol and deionized water, ultrasound is clear every time
Washing the time is 10min~15min, silicon wafer after being cleaned；Weigh the molybdenum trioxide powder and 0.12g~0.18g of 4mg~8mg
Sulphur powder, be respectively put into respective quartz boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at 3~5cm of quartz boat equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 10~20mL/min leads to flow velocity
Enter argon gas or nitrogen, and start heating system simultaneously, by temperature from room temperature to 600 DEG C~700 DEG C, and is 600 in temperature
DEG C~700 DEG C at maintain 10min~20min, be then shut off heating system, and improve argon gas or nitrogen flow rate to 200~
500mL/min, cooled to room temperature close vacuum pump, until quartzy intraductal pressure reaches normal pressure, taking out surface growth has two
The silicon wafer of molybdenum sulfide nm wall completes the growth of molybdenum disulfide nano wall.
The principle of the present invention:
Solid-state sulphur source (sulphur powder) is placed in the quartz ampoule outside stove by the method for the present invention, and stove is warming up to 600 DEG C~700
DEG C when, the optimal evaporation temperature (150 DEG C or so) of sulphur powder can be reached just by placing the temperature at sulphur powder, and silicon wafer is in chemical gas
Mutually at the optimum position temperature of deposition, sulphur powder distillation at this time is sulphur steam, and sulphur steam passes through carrier gas hydrogen or argon gas, and oxidation
Molybdenum steam, which meets, to react and deposits to base silicon on piece, and reaction principle schematic diagram is as shown in Figure 3.The method of the present invention is by being put into sulphur
The intake of the quality control sulphur source of powder, after completion of the reaction, sulphur can be taken away by increasing carrier gas flux, not toward depositing in substrate,
To control stop time point.
Beneficial effects of the present invention:
1, the present invention uses sulphur powder as sulphur source, it is ensured that does not introduce impurity element into system, guarantees sample degree of purity.
Since the distillation of solid-state sulphur source is become sulphur steam by the method for the present invention, intake and the deadline of control sulphur source can be very good
Point solves the problems, such as solid-state sulphur source not and can control the intake and stop time point of sulphur source；
2, the method for the present invention operating procedure is simple, is easily operated by the personnel of no professional knowledge, it is easier to realize industrialization.
3, the growth area for the molybdenum disulfide nano wall that the method for the present invention obtains is big and uniform, and molybdenum disulfide nano wall has
Bigger specific surface area, and exposure more multi-section, this feature make it capacitor, lithium battery, in terms of have very
Good prospect, is conducive to application industrially.
4, the method for the present invention equipment is simple, reduces production cost.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph for the silicon wafer substrate that surface growth prepared by embodiment 1 has molybdenum disulfide nano wall；
Fig. 2 is the Raman spectrum testing result of molybdenum disulfide nano wall prepared by embodiment 1；
Fig. 3 is the schematic illustration of the method for the present invention；1 is stove in figure, and 2 be quartz ampoule, and 3 be molybdenum trioxide, and 4 be sulphur
Powder, 5 be silicon wafer, and arrow indicates inert gas flows direction.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: the synthetic method of present embodiment molybdenum disulfide nano wall, sequentially includes the following steps:
One, prepare: successively silicon wafer being cleaned by ultrasonic using acetone, dehydrated alcohol and deionized water, after obtaining cleaning
Silicon wafer；The molybdenum trioxide powder of 4mg~8mg and the sulphur powder of 0.12g~0.18g are weighed, is respectively put into respective quartz boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at 3~5cm of quartz boat equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being passed through argon gas or nitrogen, and simultaneously
Start heating system, by temperature from room temperature to 600 DEG C~700 DEG C, and maintains 10min at being 600 DEG C~700 DEG C in temperature
~20min is then shut off heating system, and improves argon gas or nitrogen flow rate to 200~500mL/min, cooled to room temperature,
Vacuum pump is closed, until quartzy intraductal pressure reaches normal pressure, the silicon wafer that surface growth has molybdenum disulfide nano wall is taken out, that is, completes
The growth of molybdenum disulfide nano wall.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: ultrasound is clear every time in step 1
Washing the time is 10min~15min.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: 5mg is weighed in step 1
The molybdenum trioxide powder of~7mg and the sulphur powder of 0.14g~0.16g.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: will in step 2
Silicon wafer is placed in the quartz ampoule in stove close to vacuum pump side, at the quartz boat 4cm equipped with molybdenum trioxide.It is other with it is specific
One of embodiment one to three is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: leading in step 2
The flow velocity for entering argon gas or nitrogen is 10~20mL/min.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: being mentioned in step 2
High argon gas or nitrogen flow rate are to 300~400mL/min.It is other identical as one of specific embodiment one to five.
Using following verification experimental verifications effect of the present invention:
Embodiment 1:
The growing method of the present embodiment molybdenum disulfide nano wall, is specifically realized by the following steps:
One, prepare: successively utilizing acetone, dehydrated alcohol and deionized water are cleaned by ultrasonic silicon wafer, and ultrasound is clear every time
10min is washed, silicon wafer after being cleaned；The molybdenum trioxide powder of 4mg and the sulphur powder of 0.12g are weighed, and is respectively put into respective quartz
In boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at the quartz boat 3cm equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 10mL/min is passed through argon with flow velocity
Gas, and start heating system simultaneously, it is 700 DEG C from room temperature to temperature by temperature, and maintained at being 700 DEG C in temperature
10min is then shut off heating system, and improves argon gas flow velocity to 200mL/min, and cooled to room temperature closes vacuum pump, to
Reach normal pressure to quartzy intraductal pressure, takes out the silicon wafer that surface growth has molybdenum disulfide nano wall, i.e. completion molybdenum disulfide nano
The growth of wall.
The silicon wafer that surface growth has molybdenum disulfide nano wall is obtained using scanning electron microscope observation 1 step 2 of embodiment
Substrate is as shown in Figure 1, go out molybdenum disulfide nano wall in silicon wafer substrate surface successful growth as shown in Figure 1, and molybdenum disulfide is received
The scale of rice wall is about in 100nm.
Carry out Raman spectrum detection to the molybdenum disulfide nano wall that 1 step 2 of embodiment obtains, as shown in Fig. 2, Fig. 2 is
Raman spectrogram, curve indicates the Raman spectrum curve for the molybdenum disulfide nano wall that 1 step 2 of embodiment obtains in figure, passes through figure
2 it can be seen that there is apparent molybdenum disulfide characteristic peak, it is known that in substrate surface success at having grown molybdenum disulfide nano wall.
Embodiment 2:
The growing method of the present embodiment molybdenum disulfide nano wall, is specifically realized by the following steps:
One, prepare: successively utilizing acetone, dehydrated alcohol and deionized water are cleaned by ultrasonic silicon wafer, and ultrasound is clear every time
Wash 10min；Silicon wafer after being cleaned；The molybdenum trioxide powder of 4mg and the sulphur powder of 0.12g are weighed, and is respectively put into respective quartz
In boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at the quartz boat 3cm equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 10mL/min is passed through argon with flow velocity
Gas, and start heating system simultaneously, it is 650 DEG C from room temperature to temperature by temperature, and maintained at being 650 DEG C in temperature
10min is then shut off heating system, and improves argon gas flow velocity to 200mL/min, and cooled to room temperature closes vacuum pump, to
Reach normal pressure to quartzy intraductal pressure, takes out the silicon wafer that surface growth has molybdenum disulfide nano wall, i.e. completion molybdenum disulfide nano
The growth of wall.
Embodiment 3:
The growing method of the present embodiment molybdenum disulfide nano wall, is specifically realized by the following steps:
One, prepare: successively utilizing acetone, dehydrated alcohol and deionized water are cleaned by ultrasonic silicon wafer, and ultrasound is clear every time
Wash 10min；Silicon wafer after being cleaned；The molybdenum trioxide powder of 4mg and the sulphur powder of 0.12g are weighed, and is respectively put into respective quartz
In boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at the quartz boat 3cm equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 10mL/min is passed through nitrogen with flow velocity
Gas, and start heating system simultaneously, it is 700 DEG C from room temperature to temperature by temperature, and maintained at being 700 DEG C in temperature
10min is then shut off heating system, and improves nitrogen flow rate to 200mL/min, and cooled to room temperature closes vacuum pump, to
Reach normal pressure to quartzy intraductal pressure, takes out the silicon wafer that surface growth has molybdenum disulfide nano wall, i.e. completion molybdenum disulfide nano
The growth of wall.
Embodiment 4:
The growing method of the present embodiment molybdenum disulfide nano wall, is specifically realized by the following steps:
One, prepare: successively utilizing acetone, dehydrated alcohol and deionized water are cleaned by ultrasonic silicon wafer, and ultrasound is clear every time
Wash 10min；Silicon wafer after being cleaned；The molybdenum trioxide powder of 4mg and the sulphur powder of 0.12g are weighed, and is respectively put into respective quartz
In boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at the quartz boat 3cm equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 20mL/min is passed through argon with flow velocity
Gas, and start heating system simultaneously, it is 650 DEG C from room temperature to temperature by temperature, and maintained at being 650 DEG C in temperature
10min is then shut off heating system, and improves argon gas flow velocity to 200mL/min, and cooled to room temperature closes vacuum pump, to
Reach normal pressure to quartzy intraductal pressure, takes out the silicon wafer that surface growth has molybdenum disulfide nano wall, i.e. completion molybdenum disulfide nano
The growth of wall.
Embodiment 5:
The growing method of the present embodiment molybdenum disulfide nano wall, is specifically realized by the following steps:
One, prepare: successively utilizing acetone, dehydrated alcohol and deionized water are cleaned by ultrasonic silicon wafer, and ultrasound is clear every time
Wash 10min；Silicon wafer after being cleaned；The molybdenum trioxide powder of 4mg and the sulphur powder of 0.12g are weighed, and is respectively put into respective quartz
In boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at the quartz boat 3cm equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 20mL/min is passed through argon with flow velocity
Gas, and start heating system simultaneously, it is 650 DEG C from room temperature to temperature by temperature, and maintained at being 650 DEG C in temperature
10min is then shut off heating system, and improves argon gas flow velocity to 200mL/min, and cooled to room temperature closes vacuum pump, to
Reach normal pressure to quartzy intraductal pressure, takes out the silicon wafer that surface growth has molybdenum disulfide nano wall, i.e. completion molybdenum disulfide nano
The growth of wall.
Embodiment 6:
The growing method of the present embodiment molybdenum disulfide nano wall, is specifically realized by the following steps:
One, prepare: successively utilizing acetone, dehydrated alcohol and deionized water are cleaned by ultrasonic silicon wafer, and ultrasound is clear every time
Wash 10min；Silicon wafer after being cleaned；The molybdenum trioxide powder of 4mg and the sulphur powder of 0.17g are weighed, and is respectively put into respective quartz
In boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into
In the quartz ampoule of chemical vapor deposition unit, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove,
Quartz boat equipped with sulphur powder is placed in the quartz ampoule outside stove and puts silicon wafer at stove 2cm close to gas galvanometer side
Close to vacuum pump side in quartz ampoule in stove, at the quartz boat 3cm equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being that 10mL/min is passed through argon with flow velocity
Gas, and start heating system simultaneously, it is 700 DEG C from room temperature to temperature by temperature, and maintained at being 700 DEG C in temperature
10min is then shut off heating system, and improves argon gas flow velocity to 200mL/min, and cooled to room temperature closes vacuum pump, to
Reach normal pressure to quartzy intraductal pressure, takes out the silicon wafer that surface growth has molybdenum disulfide nano wall, i.e. completion molybdenum disulfide nano
The growth of wall.
Claims (5)
1. a kind of synthetic method of molybdenum disulfide nano wall, it is characterised in that this method sequentially includes the following steps:
One, prepare: successively silicon wafer being cleaned by ultrasonic using acetone, dehydrated alcohol and deionized water, silicon wafer after being cleaned；
The molybdenum trioxide powder of 4mg~8mg and the sulphur powder of 0.12g~0.18g are weighed, is respectively put into respective quartz boat；
Two, it grows molybdenum disulfide nano wall: silicon wafer and the quartz boat for being respectively provided with molybdenum trioxide powder and sulphur powder is put into chemistry
In the quartz ampoule of vapor phase growing apparatus, specific laying method are as follows: the quartz boat equipped with molybdenum trioxide is placed among stove, will be filled
There is the quartz boat of sulphur powder to be placed in the quartz ampoule outside stove close to Ar/N2Silicon wafer is placed on by air inlet side at stove 2cm
Close to Ar/N in quartz ampoule in stove2Gas outlet side, at 3~5cm of quartz boat equipped with molybdenum trioxide；
Start vacuum pump, pressure will be evacuated in quartz ampoule and reaches 0.1Pa hereinafter, being passed through argon gas or nitrogen, argon gas or nitrogen
Flow velocity be 10~20mL/min, and start heating system simultaneously, by temperature from room temperature to 600 DEG C~700 DEG C, and in temperature
Degree is that 10min~20min is maintained at 600 DEG C~700 DEG C, is then shut off heating system, and improve argon gas or nitrogen flow rate to 200
~500mL/min, cooled to room temperature close vacuum pump, until quartzy intraductal pressure reaches normal pressure, taking out surface growth has
The silicon wafer of molybdenum disulfide nano wall completes the growth of molybdenum disulfide nano wall.
2. a kind of synthetic method of molybdenum disulfide nano wall according to claim 1, it is characterised in that in step 1 every time
The ultrasonic cleaning time is 10min~15min.
3. a kind of synthetic method of molybdenum disulfide nano wall according to claim 1, it is characterised in that weighed in step 1
The molybdenum trioxide powder of 5mg~7mg and the sulphur powder of 0.14g~0.16g.
4. a kind of synthetic method of molybdenum disulfide nano wall according to claim 1, it is characterised in that by silicon in step 2
Piece is placed in the quartz ampoule in stove close to vacuum pump side, at the quartz boat 4cm equipped with molybdenum trioxide.
5. a kind of synthetic method of molybdenum disulfide nano wall according to claim 1, it is characterised in that improved in step 2
Argon gas or nitrogen flow rate are to 300~400mL/min.
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| CN106830082B (en) * | 2017-01-10 | 2019-03-01 | 四川大学 | A kind of method that controllable magnanimity prepares molybdenum disulfide nano band |
| CN109487231B (en) * | 2018-12-30 | 2023-08-22 | 金堆城钼业股份有限公司 | Device and method for preparing triangular molybdenum disulfide film |
| CN109868505B (en) * | 2019-03-19 | 2020-06-23 | 中南大学 | Molybdenum dioxide @ molybdenum disulfide core-shell nanorod growing along crystal direction less than 010 and preparation method thereof |
| CN110436525B (en) * | 2019-07-22 | 2021-09-28 | 金堆城钼业股份有限公司 | Preparation method of micro/nano molybdenum disulfide |
| CN110357162B (en) * | 2019-07-22 | 2021-11-09 | 金堆城钼业股份有限公司 | Method for efficiently synthesizing high-purity molybdenum disulfide |
| CN110422846B (en) * | 2019-08-13 | 2022-06-07 | 哈尔滨工业大学 | Synthesis method of molybdenum carbide nano material |
| CN113279058B (en) * | 2021-04-13 | 2023-03-24 | 中国科学院上海技术物理研究所 | Controllable preparation method of low-symmetry layered material Te |
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| CN105063573A (en) * | 2015-07-15 | 2015-11-18 | 中国电子科技集团公司第四十六研究所 | Process for manufacturing molybdenum disulfide thin film through two-step method |
| CN105161576A (en) * | 2015-10-20 | 2015-12-16 | 华中科技大学 | Preparation method of Schottky solar cell based on molybdenum disulfide |
| CN105272358A (en) * | 2015-06-01 | 2016-01-27 | 湘潭大学 | Preparation method for a large-area single-layer or few-layer molybdenum disulfide film |
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2016
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN103757602A (en) * | 2014-01-13 | 2014-04-30 | 清华大学 | Method for preparing single-layer molybdenum disulfide film |
| CN104058458A (en) * | 2014-07-07 | 2014-09-24 | 中国科学技术大学 | Method for preparing high-quality single/double-layer controllable molybdenum disulfide |
| CN105272358A (en) * | 2015-06-01 | 2016-01-27 | 湘潭大学 | Preparation method for a large-area single-layer or few-layer molybdenum disulfide film |
| CN105063573A (en) * | 2015-07-15 | 2015-11-18 | 中国电子科技集团公司第四十六研究所 | Process for manufacturing molybdenum disulfide thin film through two-step method |
| CN105161576A (en) * | 2015-10-20 | 2015-12-16 | 华中科技大学 | Preparation method of Schottky solar cell based on molybdenum disulfide |
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