CN110344023A - A kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film - Google Patents

A kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film Download PDF

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CN110344023A
CN110344023A CN201910728337.7A CN201910728337A CN110344023A CN 110344023 A CN110344023 A CN 110344023A CN 201910728337 A CN201910728337 A CN 201910728337A CN 110344023 A CN110344023 A CN 110344023A
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powder
low
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sio
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CN110344023B (en
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李宁
刘明
薛超瑞
胡胜亮
常青
王慧奇
李莹
张锦芳
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North University of China
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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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Abstract

The present invention relates to a kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, it is therefore an objective to provide a kind of using SiO2/ Si substrate, the single layer WS of one-step synthesis high coverage rate, size uniformity2Film, technical solution of the present invention is the following steps are included: by WO3Powder is pressed into WO3Powder thin slice；Clean SiO2/ Si substrate；Weigh sulphur powder；By the SiO after cleaning2/ Si substrate is put into cuboid pyroceram crucible centre, then by WO3Powder thin slice is placed on SiO2Right above/Si substrate；Sulphur powder and tungsten source obtained sample are put into CVD furnace, reacted, the single layer WS of low-temp low-pressure vapor deposition high coverage rate is obtained2Film.The present invention under the conditions of low-pressure low-temperature, a step generate size uniformity, high coverage rate, length be 10-50um single layer WS2Film, preparation method is simple, the reaction time is short, cost of labor is low, product purity is high, solves single layer WS2The technical problem of field of film preparation.

Description

A kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film
Technical field
The invention belongs to inorganic nano membrane material preparation technical fields, and in particular to a kind of low-temp low-pressure vapor deposition height covers The preparation method of the single layer WS2 film of lid rate.
Background technique
It is well known that graphene is the single layer nano material of current most study, but since its band gap is zero, limitation Its application in terms of optical property.And single layer WS2Film is a type graphene-structured, and body phase WS2Optical band gap It is indirect band gap, single layer WS2Optical band gap be direct band gap, this makes single layer WS2Nano material is largely paid close attention to.Its It is (W-S-W) in layer, is extremely strong covalent bonding, and be between layers weaker Van der Waals force, is extremely easily peeled off.One Step synthesis single layer WS2Film is hot subject of today, but the single layer WS of high coverage rate2Preparation method it is less.Due to SiO2/ Si substrate is to single layer WS2Local area limit, it more difficult to grow the single layer WS of high coverage rate2, therefore, using SiO2/ Si lining Bottom, the single layer WS of one-step synthesis high coverage rate, size uniformity2It is a big technical problem.
Summary of the invention
The purpose of the invention is to provide a kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation of film Method, using SiO2/ Si substrate, the single layer WS of one-step synthesis high coverage rate2。
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, comprising the following steps:
(1) WO is prepared3Powder thin slice: the WO of 1-2g is weighed3Powder is put it into the round tablet mold of diameter 17mm, It is pressed into WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 10-25min, ultrasonic power 50-60W, supersonic frequency 40kHz；
(3) 200-800mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, tungsten source sample is obtained Product；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 30-50cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 500-800 DEG C, sets the anti-of sulphur powder Answering temperature is 180-200 DEG C, and heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, makes sulphur powder ratio Tungsten source sample shifts to an earlier date 6-10min and reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, protects Reaction 6-10min is held, reaction pressure is 5 × 104Pa, argon gas flow velocity are 50-80sccm, hydrogen flow rate 2-10sccm makes Obtain the single layer WS of low-temp low-pressure vapor deposition high coverage rate2Film.
Further, WO is suppressed in the step (1)3The intensity of pressure of powder thin slice is 10-20MPa, and the dwell time is 3-5min。
Further, WO in the step (4)3Powder thin slice and SiO2The vertical distance of/Si substrate is 1-10mm.
The beneficial effects of the present invention are:
(1) preparation method of the invention is by by WO3Powder suppresses flakiness, passes through pressure change WO3The reunion feelings of powder Condition makes WO3Powder is compact to reunite together, and in WO3It is a kind of soft-agglomerated state between powder, such soft-agglomerated state changes Distillation and the diffusion way for having become tungsten source, in high temperature distillation, WO3Molecule is single with a kind of slow but uniform state distillation Layer WS2Film large area deposition provides advantage.
(2) of the invention by WO3Thin slice and SiO2/ Si substrate transverse is placed, and the diffusion length of the two, WO can be greatly shortened3 Diffusional deposition directly down is easier after distillation, this kind, which is provided with, to be conducive to grow single layer WS under cryogenic2Film passes through tune Whole air pressure controls WO3Molecule is uniformly spread downwards, to grow the WS of high coverage rate under conditions of low-temp low-pressure2It is thin Film.
(3) present invention is under the conditions of low-pressure low-temperature, a step generate size uniformity, high coverage rate, length be 10-50um Single layer WS2Film, preparation method is simple, the reaction time is short, cost of labor is low, product purity is high, solves single layer WS2Film system The technical problem in standby field.
Detailed description of the invention
Fig. 1 is single layer WS prepared by the present invention2The optical microscope of film；
Fig. 2 is single layer WS prepared by the present invention2The x-ray diffraction map of film；
Fig. 3 is single layer WS prepared by the present invention2The x-ray photoelectron spectroscopy analysis chart of film；
Fig. 4 is present invention preparation WS2WO when film3Powder thin slice and SiO2The position view of/Si substrate.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawings and examples.
The single layer WS of one of the present embodiment low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, including Following steps:
(1) WO is prepared3Powder thin slice: the WO of 1-2g is weighed3Powder is put it into the round tablet mold of diameter 17mm, Suppress WO3The intensity of pressure of powder thin slice is 10-20MPa, dwell time 3-5min；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 10-25min, ultrasonic power 50-60W, supersonic frequency 40kHz；
(3) 200-800mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, the WO3Powder is thin Piece and SiO2The vertical distance of/Si substrate is 1-10mm, obtains tungsten source sample；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 30-50cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 500-800 DEG C, sets the anti-of sulphur powder Answering temperature is 180-200 DEG C, and heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, makes sulphur powder ratio Tungsten source sample shifts to an earlier date 6-10min and reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, protects Reaction 6-10min is held, reaction pressure is 5 × 104Pa, argon gas flow velocity are 50-80sccm, hydrogen flow rate 2-10sccm makes Obtain the single layer WS of low-temp low-pressure vapor deposition high coverage rate2Film.
To single layer WS obtained above2Film is characterized substantially, and Fig. 1 is single layer WS2The optical microscope of film, by Fig. 1 can be seen that WS obtained2Film dimensions are uniform, and size is uniform, and single layer WS2The yield of film is higher.Fig. 2 is obtained Single layer WS2The x-ray diffraction map of film, Fig. 3 are single layer WS obtained2The x-ray photoelectron spectroscopy of film is analyzed, by Fig. 2 and Fig. 3 is it is found that obtain is pure WS2.Fig. 4 is to prepare WS2WO when film3Powder thin slice and SiO2Illustrate the position of/Si substrate Figure, by by WO3Powder thin slice is placed on SiO2Right above/Si substrate, make its vertical distance 1-10mm, shortens WO3Diffusion Distance makes WO3It is easier diffusional deposition directly down after distillation, is conducive to the single layer for growing high coverage rate under cryogenic WS2Film.
Embodiment 1
The single layer WS of one of the present embodiment low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, including Following steps:
(1) WO is prepared3Powder thin slice: the WO of 1.5g is weighed3Powder is put it into the round tablet mold of diameter 17mm, Suppress WO3The intensity of pressure of powder thin slice is 10MPa, and dwell time 3min is pressed into WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 10min, ultrasonic power 60W, supersonic frequency 40kHz；
(3) 500mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, make WO3Powder thin slice With SiO2The vertical distance of/Si substrate is 4mm, obtains tungsten source sample；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 30cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 720 DEG C, set the reaction temperature of sulphur powder as 180 DEG C, heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, shifts to an earlier date sulphur powder than tungsten source sample 6min reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, keeps reaction 10min, instead Answering pressure is 5 × 104Pa, argon gas flow velocity are 50sccm, hydrogen flow rate 6sccm, obtain low-temp low-pressure vapor deposition height and cover The single layer WS of lid rate2Film.
Embodiment 2
The single layer WS of one of the present embodiment low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, including Following steps:
(1) WO is prepared3Powder thin slice: the WO of 1.0g is weighed3Powder is put it into the round tablet mold of diameter 17mm, Suppress WO3The intensity of pressure of powder thin slice is 20MPa, and dwell time 4min is pressed into WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 15min, ultrasonic power 55W, supersonic frequency 40kHz；
(3) 200mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, make WO3Powder thin slice With SiO2The vertical distance of/Si substrate is 1mm, obtains tungsten source sample；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 40cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 700 DEG C, set the reaction temperature of sulphur powder as 190 DEG C, heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, shifts to an earlier date sulphur powder than tungsten source sample 8min reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, keeps reaction 6min, reaction Pressure is 5 × 104Pa, argon gas flow velocity are 60sccm, hydrogen flow rate 3sccm, obtain the high covering of low-temp low-pressure vapor deposition The single layer WS of rate2Film.
Embodiment 3
The single layer WS of one of the present embodiment low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, including Following steps:
(1) WO is prepared3Powder thin slice: the WO of 2.0g is weighed3Powder is put it into the round tablet mold of diameter 17mm, Suppress WO3The intensity of pressure of powder thin slice is 15MPa, and dwell time 5min is pressed into WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 25min, ultrasonic power 50W, supersonic frequency 40kHz；
(3) 800mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, make WO3Powder thin slice With SiO2The vertical distance of/Si substrate is 10mm, obtains tungsten source sample；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 50cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 750 DEG C, set the reaction temperature of sulphur powder as 200 DEG C, heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, shifts to an earlier date sulphur powder than tungsten source sample 10min reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, keeps reaction 8min, instead Answering pressure is 5 × 104Pa, argon gas flow velocity are 80sccm, hydrogen flow rate 4sccm, obtain low-temp low-pressure vapor deposition height and cover The single layer WS of lid rate2Film.
Embodiment 4
The single layer WS of one of the present embodiment low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, including Following steps:
(1) WO is prepared3Powder thin slice: the WO of 1.8g is weighed3Powder is put it into the round tablet mold of diameter 17mm, Suppress WO3The intensity of pressure of powder thin slice is 15MPa, and dwell time 5min is pressed into WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 25min, ultrasonic power 50W, supersonic frequency 40kHz；
(3) 700mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, make WO3Powder thin slice With SiO2The vertical distance of/Si substrate is 7mm, obtains tungsten source sample；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 50cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 800 DEG C, set the reaction temperature of sulphur powder as 200 DEG C, heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, shifts to an earlier date sulphur powder than tungsten source sample 10min reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, keeps reaction 8min, instead Answering pressure is 5 × 104Pa, argon gas flow velocity are 80sccm, hydrogen flow rate 10sccm, obtain low-temp low-pressure vapor deposition height and cover The single layer WS of lid rate2Film.
Embodiment 5
The single layer WS of one of the present embodiment low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, including Following steps:
(1) WO is prepared3Powder thin slice: the WO of 1.0g is weighed3Powder is put it into the round tablet mold of diameter 17mm, Suppress WO3The intensity of pressure of powder thin slice is 20MPa, and dwell time 4min is pressed into WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate use respectively acetone soln, ethanol solution, Deionized water is cleaned by ultrasonic 15min, ultrasonic power 55W, supersonic frequency 40kHz；
(3) 400mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is put into cuboid pyroceram Crucible centre, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, make WO3Powder thin slice With SiO2The vertical distance of/Si substrate is 3mm, obtains tungsten source sample；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, is made Sulphur powder is 40cm at a distance from the sample of tungsten source, sets the reaction temperature of tungsten source sample as 500 DEG C, set the reaction temperature of sulphur powder as 190 DEG C, heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, shifts to an earlier date sulphur powder than tungsten source sample 8min reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, keeps reaction 6min, reaction Pressure is 5 × 104Pa, argon gas flow velocity are 60sccm, hydrogen flow rate 2sccm, obtain the high covering of low-temp low-pressure vapor deposition The single layer WS of rate2Film.

Claims (3)

1. a kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film, which is characterized in that including following Step:
(1) WO is prepared3Powder thin slice: the WO of 1-2g is weighed3Powder is put it into the round tablet mold of diameter 17mm, compacting At WO3Powder thin slice；
(2)SiO2The cleaning of/Si substrate: a 9*13mm is taken2SiO2/ Si substrate respectively with acetone soln, ethanol solution, go from Sub- water is cleaned by ultrasonic 10-25min, ultrasonic power 50-60W, supersonic frequency 40kHz；
(3) 200-800mg sulphur powder is weighed；
(4) preparation of tungsten source sample: by the SiO after cleaning in step (2)2/ Si substrate is being put into cuboid pyroceram crucible just Center, then the WO that step (1) is suppressed3Powder thin slice is placed on SiO2Right above/Si substrate, tungsten source sample is obtained；
(5) vulcanization reaction: tungsten source sample made from the weighed sulphur powder of step (3) and step (4) is put into CVD furnace, sulphur powder is made With at a distance from the sample of tungsten source be 30-50cm, set the reaction temperature of tungsten source sample as 500-800 DEG C, set the reaction temperature of sulphur powder Degree is 180-200 DEG C, and heating rate is 10 DEG C/min, controls the heating time of tungsten source sample and sulphur powder, makes sulphur powder than tungsten source Sample shifts to an earlier date 6-10min and reaches the reaction temperature respectively set, after system temperature reaches the reaction temperature of setting, keeps anti- 6-10min is answered, reaction pressure is 5 × 104Pa, argon gas flow velocity are 50-80sccm, and hydrogen flow rate 2-10sccm is obtained low The single layer WS of warm low pressure gas phase deposition high coverage rate2Film.
2. a kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate according to claim 12The preparation method of film, It is characterized by: suppressing WO in the step (1)3The intensity of pressure of powder thin slice is 10-20MPa, dwell time 3-5min.
3. a kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate according to claim 12The preparation method of film, It is characterized by: WO in the step (4)3Powder thin slice and SiO2The vertical distance of/Si substrate is 1-10mm.
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