CN108118395A - A kind of method that chemical vapor deposition prepares two tungsten selenide monocrystal thin films - Google Patents
A kind of method that chemical vapor deposition prepares two tungsten selenide monocrystal thin films Download PDFInfo
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- CN108118395A CN108118395A CN201711354238.4A CN201711354238A CN108118395A CN 108118395 A CN108118395 A CN 108118395A CN 201711354238 A CN201711354238 A CN 201711354238A CN 108118395 A CN108118395 A CN 108118395A
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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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
Abstract
The invention discloses a kind of method that chemical vapor deposition prepares two tungsten selenide monocrystal thin films, this method includes：Using the oxide powder, halide salt, selenium powder of tungsten as raw material, inert gas is carrier gas, and raw material is flashed to gaseous state and is transported to deposition on substrate two selenizing W films of growth.By the way that the means such as raw material proportioning, growth temperature, growth time, carrier gas flux is controlled to control film thickness.Using the present invention, more than 50um, two controllable selenizing W films of the number of plies can be grown under 600 800 degrees Celsius under hydrogen free environment.
Description
Technical field
The invention belongs to the techniques of production of thin film by chemical gas-phase deposition, have been provided in particular in a kind of hydrogen-free, low temperature, normal pressure
The method that chemical vapour deposition technique prepares two tungsten selenide monocrystal thin films, is related to a kind of transient metal chalcogenide compound film of uniqueness
Preparation.
Background technology
Two tungsten selenides（WSe2）It is a kind of p-type semiconductor material, there is preferable energy gap, is 1.3 electron-volts, reason
Field-effect transistor by estimated two tungsten selenides not only has up to 500 square centimeters often to lie prostrate carrier mobility per second, more can
Obtain 108High on-off ratio, and its thermal conductivity is minimum in material, can reduce the energy loss of electronic device.The opposing party
Face, two selenizing W film of individual layer are a kind of direct band-gap semicondictors, and energy gap is 1.6-1.7 electron-volts, compared to indirect belt
The body material of gap has efficient fluorescence efficiency.Secondly, the strong Quantum geometrical phase effect of transition metal element d orbital electron,
So that two tungsten selenide of individual layer generates energy valley quantum state.Therefore, this New Two Dimensional material similar with graphene, can not only be
Future semiconductor, micro-nano field of electronic devices are widely used, while also following condensed state physics and photoelectronics are led
The research in domain has important meaning.
Preparing the method for two selenizing W films at present mainly includes：Mechanical stripping method, chemical stripping method, physical vapour deposition (PVD)
Method and chemical vapour deposition technique.Two tungsten selenide film dimensions of individual layer prepared by mechanical stripping method and chemical stripping method are small, and the number of plies
It is uneven, the requirement of microelectronics integrated technique can not be met.Vapour deposition process is considered as that a kind of two tungsten selenides of effectively growth are thin
The method of film.Although physical vaporous deposition can grow the diaphragm of large-size, need more than 0.1 support vacuum degree and
960 degrees Celsius are used as growth conditions.Chemical vapour deposition technique can then realize it is lower than physical vapour deposition (PVD) at a temperature of grown junction
Crystalloid amount height, large-sized two tungsten selenides diaphragm.Current chemical vapour deposition technique uses pure tungsten oxide powder and selenium more
Powder is auxiliary gas as raw material, hydrogen, obtains two selenizing W films in 0.1 support more than high vacuum and 925 degrees Celsius of depositions, to the greatest extent
Pipe is declined compared to physical deposition temperature, but still needs to high depositing temperature and hydrogen assisted reaction, causes forming thin film area
Small, the shortcomings of number of plies is uneven, crystalline quality is not high.How to realize and obtained in the case of reduction depositing temperature and without hydrogen catalysis
Two controllable selenizing W films of crystalline quality height, large scale, the number of plies have become current two-dimensional semiconductor Material Field research
One of emphasis.The breakthrough of this technology can not only drive the two-dimensional material of analogous crystalline structure, such as large scale individual layer tungsten disulfide
Etc. the breakthrough of preparation processes and following novel semiconductor material, the important propulsive force of microelectronics integration field development.Therefore,
The growing technology of two controllable selenizing W films of crystalline quality height, large scale, the number of plies has huge market prospects.
The content of the invention
To solve the above-mentioned problems, the object of the present invention is to provide a kind of cleaning method, tungsten by controlling growth substrates
Source mixture ratio, the means such as flow of inert gas control nucleation rate, by controlling growth temperature, growth time, hydrogen
The means such as flow control film thickness and mass growth condition efficient growth crystalline quality is high, large-sized chemical vapor deposition system
The method of standby two tungsten selenide monocrystal thin films.
The present invention solves the technical solution of above-mentioned technical problem, and a kind of chemical vapor deposition prepares two tungsten selenide monocrystal thin films
Method, this method is using the oxide powder, halide salt, selenium powder of tungsten as raw material, and inert gas is carrier gas, using chemical vapor deposition
Area method, dual temperature area heat growth realize the high selenizing W film of no hydrogen catalysis, growth at atmosphere crystalline quality.
Further, this method concretely comprises the following steps：
The processing of step 1. growth substrates：Growth substrates are successively put into acetone, ethyl alcohol, deionized water, in each above-mentioned solution
It is each to be cleaned by ultrasonic after twenty minutes, it takes out, nitrogen drying；
It is prepared by step 2. tungsten source：Example weighs the oxide powder of tungsten and halide salt mixing in mass ratio, with mortar by mixed-powder
It grinds and is uniformly mixed, compound particles characteristic size is 0.5-2 microns；
Step 3. inert gas shielding：First to being vacuumized in quartz ampoule, then protective gas is passed through to exclude quartzy inner air tube,
Recover normal pressure in pipe；
Two selenizing W film of step 4. is grown：Using dual temperature area heat growth, it is former higher than 99.9% solid that the first warm area places purity
Expect selenium powder, the second warm area places the tungsten source described in step 2, and by step 1, treated that substrate is placed in tungsten source downstream 1-3 centimeters,
The first warm area is heated to 265-400 degrees Celsius with certain rate of heat addition, is delivered to the selenium steam of heating using inert gas
Second warm area, then the second warm area is heated to 600-800 degrees Celsius with certain rate of heat addition, soaking time 5-30 minutes, lazy
Property atmosphere under 30-50 degrees Celsius per minute be cooled to 400 degrees Celsius, complete growth to get to two tungsten selenide monocrystal thin films.
Further, the substrate in the step 1 includes titanium dioxide silicon chip, mica sheet, graphite flake and sapphire sheet.
Further, halide in the step 2：The mass ratio of tungsten oxide powder is 1:6-20.
Further, tungsten oxide powder includes green tungsten trioxide powder or black-and-blue tungsten oxide powder in the step 2；
The halide salt includes sodium chloride, potassium chloride, sodium bromide, potassium bromide, sodium iodide and potassium iodide.
Further, the middle protective gas flow using 30 millimeters of caliber quartz ampoules of the step 3 is 200-500
Standard milliliters are per minute, and the protective gas flow using 60 millimeters of caliber quartz ampoules is 10 standard milliliters per minute -100
Standard milliliters are per minute.
Further, the protective gas in the step 3 is high-purity argon gas or high pure nitrogen；
Further, the first warm area rate of heat addition is 15-20 degrees Celsius per minute.
Further, the second warm area rate of heat addition is with 20-35 degrees Celsius per minute.
Beneficial effects of the present invention：Preparation method of the present invention by using different tungsten sources, to chemical vapor deposition mistake
Growth temperature, time in journey, gas flow are adjusted, and energy-efficient that measured two tungsten selenide of crystalline is prepared is thin
Film.This method can obtain two selenizing W films of extensive batch using the growth substrates of different type and size, without
Hydrogen, without 800 degrees Celsius or more high temperature, without high vacuum environment.Two high selenizing W films of crystalline quality can be prepared into
Novel and multifunctional opto-electronic device.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, embodiment will be described below
Needed in attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description be only the present invention some
Embodiment, for those of ordinary skill in the art, without creative efforts, can also be attached according to these
Figure obtains other attached drawings.
Fig. 1 show the two tungsten selenide individual layer triangular form Film Optics photos grown on typical silicon-on-insulator.Single two
The size of tungsten selenide monocrystalline has 60 microns, and edge crystallinity is very good.
Fig. 2 show the Raman spectrum of the two tungsten selenide individual layer triangular form films grown on typical silicon-on-insulator.Raman
Excitation wavelength is 514 nanometers, and the feature that the Raman vibration peak in spectrum at 250 wave numbers and at 259 wave numbers corresponds to two tungsten selenides is drawn
Graceful vibration frequency.
Fig. 3 show the photoluminescence spectrum of the two tungsten selenide individual layer triangular form films grown on typical silicon-on-insulator, light
It is 514 nanometers to cause excitation wavelength, and the spike in spectrum near 760 nanometers is the exciton stimulated luminescence of two tungsten selenide of individual layer.Individual layer
Two tungsten selenides compared with block two tungsten selenides, due to band structure from indirect band gap transitions be direct band gap, photoluminescence intensity
It significantly improves, glow peak blue shift.
Specific embodiment
Technical scheme is described in detail with reference to example, it is clear that described example is only this
The example of small part rather than whole in invention.Based on the example in the present invention, those skilled in the art are not making wound
The every other example obtained under the premise of the property made work, belongs to the scope of protection of the invention.
The method that chemical vapor deposition of the present invention prepares two tungsten selenide monocrystal thin films, this method concretely comprise the following steps：
The processing of step 1. growth substrates：Growth substrates are successively put into acetone, ethyl alcohol, deionized water, in each above-mentioned solution
It is each to be cleaned by ultrasonic after twenty minutes, it takes out, nitrogen drying；
It is prepared by step 2. tungsten source：Example weighs the oxide powder of tungsten and halide salt mixing in mass ratio, with mortar by mixed-powder
It grinds and is uniformly mixed, compound particles characteristic size is 0.5-2 microns；
Step 3. inert gas shielding：First to being vacuumized in quartz ampoule, then protective gas is passed through to exclude quartzy inner air tube,
Recover normal pressure in pipe；
Two selenizing W film of step 4. is grown：Using dual temperature area heat growth, it is former higher than 99.9% solid that the first warm area places purity
Expect selenium powder, the second warm area places the tungsten source described in step 2, and by step 1, treated that substrate is placed in tungsten source downstream 1-3 centimeters,
The first warm area is heated to 265-400 degrees Celsius with certain rate of heat addition, is delivered to the selenium steam of heating using inert gas
Second warm area, then the second warm area is heated to 600-800 degrees Celsius with certain rate of heat addition, soaking time 5-30 minutes, lazy
Property atmosphere under with 30-50 degrees Celsius per minute be cooled to 400 degrees Celsius, complete growth to get to two tungsten selenide monocrystal thin films.
The substrate in the step 1 includes titanium dioxide silicon chip, mica sheet, graphite flake and sapphire sheet.
Halide in the step 2：The mass ratio of tungsten oxide powder is 1:6-20.
Tungsten oxide powder includes green tungsten trioxide powder or black-and-blue tungsten oxide powder in the step 2；The halogen
Salt dissolving includes sodium chloride, potassium chloride, sodium bromide, potassium bromide, sodium iodide and potassium iodide.
The middle protective gas flow using 30 millimeters of caliber quartz ampoules of the step 3 is 200-500 standards milli
Liter Per Minute is 10 standard milliliters -100 standard milli per minute using the protective gas flow of 60 millimeters of caliber quartz ampoules
Liter Per Minute.
The middle protective gas of the step 3 is high-purity argon gas or high pure nitrogen.
The first warm area rate of heat addition is 15-20 degrees Celsius per minute.
The second warm area rate of heat addition is with 20-35 degrees Celsius per minute.
Embodiment 1
Using insulating silicon as growth substrates, substrate cleaning is as follows：Insulating silicon is successively put into acetone, ethyl alcohol, deionized water, above-mentioned every
Respectively it is cleaned by ultrasonic in kind solution after twenty minutes, takes out, nitrogen drying；Prepare tungsten source, in mass ratio example potassium chloride powder：Green three
Tungsten oxide powder=1:8 mixing, by powder mull and are uniformly mixed, 0.7 micron of compound particles particle size using mortar.It grew
Journey is as follows：The protective gas of 30 minutes is passed through to exclude quartzy inner air tube, is excluded empty in clean 60 millimeters of quartz ampoules of diameter
After gas, it is per minute that argon stream is adjusted to 80 standard milliliters, the first warm area places selenium powder in stove, adds with 15 centigrade per minutes
For heat to 320 degrees Celsius, the second warm area places the mixed-powder of green tungsten trioxide powder and potassium chloride, and the second warm area is Celsius with 30
Spend it is per minute be heated to 700 degrees Celsius, silicon-on-insulator is vertically arranged in 1 centimeters of mixed-powder downstream, after reaching temperature, reaction life
It is long to continue 10min, 400 degrees Celsius are cooled to 30-50 degrees Celsius per minute under inert gas shielding after heat preservation, is completed
Growth.
Embodiment 2
Using mica as growth substrates.Substrate cleaning is as follows：Clean growth substrates：Growth substrates successively be put into acetone, ethyl alcohol, go from
Sub- water is respectively cleaned by ultrasonic after twenty minutes in each above-mentioned solution, takes out, nitrogen drying；Prepare tungsten source, in mass ratio example chlorination
Sodium powder end：Black-and-blue tungsten oxide powder=1:12 mixing, by powder mull and are uniformly mixed, compound particles particle size 2 using mortar
Micron.Growth course is as follows：The protective gas of 30 minutes is passed through to exclude the quartzy inner air tube of 60 millimeters of diameter, is excluded clean
After inner air tube, it is per minute that argon stream is adjusted to 100 standard milliliters, selenium is placed in the first warm area position in argon gas atmosphere stove
Powder is heated to 300 degrees Celsius with 15 centigrade per minutes, and the second warm area places the mixed of black-and-blue tungsten oxide powder and sodium chloride
Powder is closed, 780 degrees Celsius are heated to 30 centigrade per minutes, mica sheet is vertically arranged in 2 centimeters of mixed-powder downstream, reaches
After temperature, reaction growth continues 30 minutes, is cooled to after heat preservation under inert gas shielding with 30-50 degrees Celsius per minute
400 degrees Celsius, complete growth.
The above description is merely a specific embodiment, but protection scope of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can readily occur in change or replacement, should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Embodiment 3
Using insulating silicon as growth substrates, substrate cleaning is as follows：Insulating silicon is successively put into acetone, ethyl alcohol, deionized water, above-mentioned every
Respectively it is cleaned by ultrasonic in kind solution after twenty minutes, takes out, nitrogen drying；Prepare tungsten source, in mass ratio example potassium chloride powder：Green three
Tungsten oxide powder=1:20 mixing, by powder mull and are uniformly mixed, 1 micron of compound particles particle size using mortar.Growth course
It is as follows：The protective gas of 30 minutes is passed through to exclude quartzy inner air tube, excludes the clean quartzy inner air tube of 30 millimeters of diameter
Afterwards, that argon stream is adjusted to 200 standard milliliters is per minute, and the first warm area places selenium powder in stove, is added with 15 centigrade per minutes
For heat to 290 degrees Celsius, the second warm area places the mixed-powder of green tungsten trioxide powder and potassium chloride, and the second warm area is Celsius with 20
Spend it is per minute be heated to 685 degrees Celsius, silicon-on-insulator is vertically arranged in 2 centimeters of mixed-powder downstream, after reaching temperature, reaction life
Length continues 15 minutes, and 400 degrees Celsius are cooled under inert gas shielding with 30-50 degrees Celsius per minute after heat preservation, complete
Into growth.
The above description is merely a specific embodiment, but protection scope of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can readily occur in change or replacement, should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (9)
1. a kind of method that chemical vapor deposition prepares two tungsten selenide monocrystal thin films, it is characterised in that：This method is with the oxidation of tungsten
Object powder, halide salt, selenium powder are raw material, and inert gas is carrier gas, and using chemical vapour deposition technique, dual temperature area heat growth is real
Now without the high selenizing W film of hydrogen catalysis, growth at atmosphere crystalline quality.
2. according to the method described in claim 1, it is characterized in that, this method concretely comprises the following steps：
The processing of step 1. growth substrates：Growth substrates are successively put into acetone, ethyl alcohol, deionized water, in each above-mentioned solution
It is each to be cleaned by ultrasonic after twenty minutes, it takes out, nitrogen drying；
It is prepared by step 2. tungsten source：Example weighs the oxide powder and halide salt of tungsten in mass ratio, is ground mixed-powder with mortar
And be uniformly mixed, compound particles characteristic size is 0.5-2 microns；
Step 3. inert gas shielding：First to being vacuumized in quartz ampoule, then protective gas is passed through to exclude quartzy inner air tube,
Recover normal pressure in pipe；
Two selenizing W film of step 4. is grown：Using dual temperature area heat growth, it is former higher than 99.9% solid that the first warm area places purity
Expect selenium powder, the second warm area places the tungsten source described in step 2, and by step 1, treated that substrate is placed in tungsten source downstream 1-3 centimeters,
The first warm area is heated to 265-400 degrees Celsius with certain rate of heat addition, is delivered to the selenium steam of heating using inert gas
Second warm area, then the second warm area is heated to 600-800 degrees Celsius with certain rate of heat addition, soaking time 5-30 minutes, lazy
Property atmosphere under with 30-50 degrees Celsius per minute be cooled to 400 degrees Celsius, complete growth to get to two tungsten selenide monocrystal thin films.
3. according to the method described in claim 2, it is characterized in that, the substrate in the step 1 include titanium dioxide silicon chip,
Mica sheet, graphite flake and sapphire sheet.
4. according to the method described in claim 2, it is characterized in that, halide in the step 2：The quality of tungsten oxide powder
Ratio is 1:6-20.
5. according to the method described in claim 2, it is characterized in that, tungsten oxide powder includes green three oxygen in the step 2
Change tungsten powder or black-and-blue tungsten oxide powder；The halide salt include sodium chloride, potassium chloride, sodium bromide, potassium bromide, sodium iodide and
Potassium iodide.
6. according to the method described in claim 2, it is characterized in that, the step 3 it is middle using 30 millimeters of caliber quartz ampoules
The protective gas flow is per minute for 200-500 standard milliliters, uses the protectiveness gas of 60 millimeters of caliber quartz ampoules
Body flow is per minute for 10 standard milliliters -100 standard milliliters per minute.
7. according to the method described in claim 2, it is characterized in that, the middle protective gas of the step 3 for high-purity argon gas or
High pure nitrogen.
8. according to the method described in claim 2, it is characterized in that, the first warm area rate of heat addition is taken the photograph for 15-20 per minute
Family name's degree.
9. according to the method described in claim 2, it is characterized in that, the second warm area rate of heat addition is with 20-35 per minute
Degree Celsius.
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