CN110451564A - Vulcanize the preparation method of pretreated single layer molybdenum disulfide based on substrate - Google Patents
Vulcanize the preparation method of pretreated single layer molybdenum disulfide based on substrate Download PDFInfo
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Abstract
The invention belongs to two-dimensional semiconductor field of material technology, specially vulcanize the preparation method of pretreated single layer molybdenum disulfide based on substrate.The present invention is using silicon wafer as growth substrates, in substrate after over cleaning, places it in quartz test tube and carries out vulcanizing treatment in the environment of containing sulfur vapor, then prepares single layer molybdenum disulfide using the method for chemical vapor deposition.The present invention passes through the temperature of optimization substrate vulcanizing treatment, time, prepares the single layer molybdenum disulfide monocrystalline and large area continuous film of high quality.This method process is simple, without expensive vulcanization source and growth source.Prepared high quality monolayer molybdenum disulfide can be used for preparing the opto-electronic device and micro-nano electronic device of the specific function with more high-fluorescence quantum yield, more excellent performance.
Description
Technical field
The invention belongs to two-dimensional semiconductor field of material technology, and in particular to the preparation method of single layer molybdenum disulfide.
Technical background
Molybdenum disulfide (MoS2) it is a kind of typical New Two Dimensional semiconductor material, there is excellent optically and electrically property
Matter.Single layer molybdenum disulfide has the interlayer structure of sandwich, wherein clipping one layer of molybdenum atom between two layers of sulphur atom, each molybdenum is former
6 sulphur atoms are dispersed with around sub, 3 molybdenum atoms are dispersed with around each sulphur atom, they are with strong Covalent bonding together.
Block molybdenum disulfide is combined by Van der Waals force between layers, and with the reduction of the number of plies, band gap can be by the indirect of multilayer
Band gap becomes the direct band-gap semicondictor of single layer.The band gap of single layer molybdenum disulfide is about 1.8eV, has good carrier defeated
Performance is transported, as the New Two Dimensional semiconductor material complementary with graphene, transistor has up to 108Current on/off ratio,
And have lower energy loss, it is considered to be in next generation's integrated circuit substituted for silicon continue Moore's Law important materials it
One.Therefore, the preparation of high quality molybdenum disulfide seems especially for its application in fields such as photoelectric device, field effect transistors
It is important.
In general, the single layer molybdenum disulfide of chemical vapor deposition growth and the molybdenum disulfide of mechanical stripping are generally existing non-
Metallic element sulphur vacancy, these sulphur vacancy defects can reduce the optical quality and electric property of molybdenum disulfide.It has been proposed that using
Chemical reagent handles molybdenum disulfide to achieve the purpose that repair sulphur vacancy.For example, being handled using bis- (fluoroform) sulfimides
The single layer molybdenum disulfide of mechanical stripping, can be such that its fluorescence quantum efficiency reaches close to 100%.Other chemical reagent such as 3- mercapto
Propyl trimethoxy silicane is also used to repair the sulphur vacancy in single layer molybdenum disulfide, to improve the electricity of molybdenum disulfide device
Performance.However the method for chemical reagent processing can introduce pollution impurity absorption in defect empty place, and in repair process also
It needs to carry out high-temperature process to single layer molybdenum disulfide, these lengthy and jumbled steps limit molybdenum disulfide in field of optoelectronic devices
Using.Chemical vapour deposition technique is to prepare large area molybdenum disulfide most efficient method, in order to improve the light based on molybdenum disulfide
The performance of electronic device and micro-nano electronic device needs to prepare the single-layer molybdenum disulfide film of high quality.How directly passing through
The method of vapor deposition is learned to prepare the weight that the single layer molybdenum disulfide of high quality has become the research of two-dimensional semiconductor Material Field
One of point problem.The breakthrough of this unquestionable technology will promote the technology of preparing of other two-dimentional Transition-metal dichalcogenides
It breaks through, to prepare miscellaneous high quality two dimension Transition-metal dichalcogenide semiconductor material, pushes New Two Dimensional
Application of the semiconductor material in integrated circuit fields.
Substrate vulcanization is the key factor for effectively improving the quality that chemical vapor deposition prepares molybdenum disulfide.Silicon wafer is selected to make
For growth substrates, since silicon wafer has natural conductive layer and insulating medium layer, the single layer molybdenum disulfide sample grown can
It is directly used in late device technique, needs not move through transfer process, to reduce process flow, reduces the processing cost of device.
The present invention proposes a kind of preparation method for vulcanizing pretreated high quality monolayer molybdenum disulfide based on substrate, with solid elemental sulfur work
For sulphur source, silicon wafer will form the sulfuric horizon of chemical bonding during sulfur vapor is heat-treated, then pass through chemical vapor deposition
Grown above silicon single layer molybdenum disulfide of the method after vulcanizing treatment.By control silicon chip substrate vulcanizing treatment temperature, when
Between etc. means, to control the quality of the molybdenum disulfide of chemical vapor deposition growth.It can be in existing chemical gas using the present invention
On the basis of phase deposition growing molybdenum disulfide, the high quality monolayer molybdenum disulfide that optical quality is good, sulphur vacancy defect is few is prepared.
Summary of the invention
The object of the present invention is to be led for the generally existing sulphur vacancy of the single layer molybdenum disulfide of chemical vapour deposition technique preparation
The problems such as its luminous efficiency is lower, electric property is poor is caused, a kind of preparation method of the single layer molybdenum disulfide of high quality is proposed.
The preparation method of single layer molybdenum disulfide provided by the invention, be based on substrate vulcanize it is pretreated, specific steps are such as
Under:
(1) carry out vulcanizing treatment to silicon chip substrate: sulphur simple substance solid and silicon chip substrate are respectively placed in quartz test tube, and (internal diameter can be with
In 20-25 mm), to adjust sulphur source and substrate to suitable position, in the double temperature-area tubular furnaces for being continually fed into nitrogen protection gas
Respectively to sulphur simple substance and silicon, under sulfur vapor environment, the sulfuric horizon that chemical bond is formed with sulphur is formed in substrate surface;
(2) on the substrate handled through step (1) 50-100 μm of ol/L of spin coating 3,4,9,10 ,-pyrene tetracarboxylic acid acid potassium salt
(PTAS) solution, to promote the nucleation and growth of molybdenum disulfide;
(3) using elemental sulfur and molybdenum source (molybdenum trioxide powder) as growth source, substrate and elemental sulfur, molybdenum source to suitable position are adjusted
It sets, grows single layer molybdenum disulfide on the substrate handled through step (2) using chemical vapour deposition technique to get optical quality is arrived very
Good single layer molybdenum disulfide.
In step (1) of the present invention, the silicon wafer contains 300 ± 10 nm thick oxide layers, before carrying out vulcanizing treatment to it also
Include the steps that cleaning it, to remove the impurity of silicon chip surface, the specific method is as follows: successively with acetone, isopropanol, ultrapure water
Each ultrasound 25-30min, is then dried up with high pure nitrogen.
In step (1) of the present invention, the suitable distance of elemental sulfur and substrate is 22-24 cm.To elemental sulfur and silicon
Before, step (1) further includes being taken away the air in quartz ampoule using mechanical pump, is arrived when vacuum degree reaches 3-5Pa Shi Zaitong nitrogen
In quartz ampoule, to quartzy intraductal pressure to normal pressure, which repeats 2-4 times to reduce the oxygen and steam in quartz ampoule as far as possible.
In step (1) of the present invention, the temperature to sulphur simple substance heating is 170-200 DEG C, and the heating temperature to substrate is 200-
700 DEG C, substrate curing time is 0.5-1 h.The heating schedule for then terminating tube furnace, is down to room temperature naturally to furnace body and takes
Silicon wafer out.
In step (2) of the present invention, PTAS is dissolved in isopropanol, on the silicon wafer that vulcanizing treatment is crossed is placed on sol evenning machine and drips
3-5 μ L PTAS solution carries out spin coating, and control spin coating machine speed is 1000-2000 r/min, and spin-coating time is 1-3 min.
In step (3) of the present invention, the dosage for controlling elemental sulfur is 120-200 mg, and the dosage of molybdenum trioxide is 2-5 mg,
The distance of elemental sulfur and substrate is 20-24 cm, and the distance of substrate and molybdenum source is 0.5-1 cm, and substrate is placed upward.
In step (3) of the present invention, the purity of sulphur simple substance is 99.99%, and the purity of molybdenum trioxide is 99.9%.Adjust growth
Behind source and the position of substrate, use nitrogen as carrier gas.Before to growth source and silicon, step (3) further includes utilizing machine
Tool pump takes the air in quartz ampoule away, when vacuum degree reaches 3-5Pa Shi Zaitong nitrogen into quartz ampoule, to quartzy intraductal pressure
To normal pressure, which repeats 2-4 times to reduce the oxygen and steam in quartz ampoule as far as possible.Then use aumospheric pressure cvd
Method grow molybdenum disulfide, the heating temperature of sulphur source and molybdenum source risen to respectively in 35-40 min 160-190 DEG C and
650-700 DEG C, the control reaction time is 3-5 min.In heat growth source and growth molybdenum disulfide all processes, the flow of nitrogen
For 10-50 sccm.Stop heating after having grown molybdenum disulfide, waits tube furnace to be down to room temperature naturally and take out silicon wafer, then in light
Learning can be observed have a large amount of single layer molybdenum disulfide on silicon wafer under microscope.
The high quality monolayer molybdenum disulfide that the present invention is prepared, including monocrystalline and continuous film.
Beneficial effects of the present invention: the present invention under sulfur vapor by carrying out vulcanizing treatment to silicon wafer, then using chemistry
The method of vapor deposition prepares single layer molybdenum disulfide.By optimizing temperature, the time of substrate vulcanizing treatment, high quality is prepared
Single layer molybdenum disulfide monocrystalline and large area continuous film.This method process is simple, without expensive vulcanization source and growth source.
Prepared high quality monolayer molybdenum disulfide can be used for preparing the special function with more high-fluorescence quantum yield, more excellent performance
The opto-electronic device and micro-nano electronic device of energy.
Detailed description of the invention
Fig. 1 is the schematic device of silicon chip substrate vulcanizing treatment experiment.
Fig. 2 is the single layer molybdenum disulfide photoluminescence image prepared in embodiment 1 and embodiment 2.Wherein, (a) is substrate
Resulting single layer molybdenum disulfide is prepared without vulcanizing treatment, (b) prepares resulting single layer two after 600 DEG C of processing for substrate
Molybdenum sulfide.
Fig. 3 is the single layer molybdenum disulfide photoluminescence spectra prepared in embodiment 1 and embodiment 2.Wherein, thin curve is lining
Bottom prepares the photoluminescence spectra of resulting single layer molybdenum disulfide without vulcanizing treatment, and bold curve is that substrate passes through 600 DEG C of sulphur
Change the photoluminescence spectra that processing prepares resulting single layer molybdenum disulfide.
Specific embodiment
Embodiment 1
The experimental method of silicon chip substrate vulcanization, including the following steps:
1, cleaning silicon chip is successively used acetone, isopropanol, each ultrasonic 20 min of ultrapure water, is then dried up with high pure nitrogen.
2,500 mg sulphur simple substance solids are weighed to be placed in quartz ampoule, the silicon chip substrate cleaned up is respectively placed in another stone
In English test tube, the position for adjusting sulphur source and substrate is 22 cm.Then the air in quartz ampoule is taken away with mechanical pump, works as vacuum
Degree reaches 3-5Pa Shi Zaitong nitrogen into quartz ampoule, and to quartzy intraductal pressure to normal pressure, which is repeated 3 times to drop as far as possible
Oxygen and steam in low quartz pipe.Then in the double temperature-area tubular furnaces for being continually fed into nitrogen protection gas respectively to sulphur simple substance and
Silicon, wherein the heating temperature of sulphur source is 200 DEG C, and the heating temperature of silicon chip substrate is 600 DEG C, under sulfur vapor environment
To growth substrates SiO2/ Si carries out vulcanizing treatment 1h, and substrate surface is made to form the sulfuric horizon for forming chemical bond with sulphur.
3, to 3,4,9,10 of 5 100 μm of ol/L of μ L of spin coating on substrate described above ,-pyrene tetracarboxylic acid acid potassium salt
(PTAS) solution is to promote the nucleation and growth of molybdenum disulfide, and control spin coating machine speed is 1000r/min, and spin-coating time is
1min。
4,150 mg sulphur simple substances are weighed and 3 mg molybdenum trioxides are placed in quartz boat, the distance for adjusting elemental sulfur and substrate is
The distance of 22 cm, substrate and molybdenum source is 1 cm, and substrate is placed upward.Then the air in quartz ampoule is taken away with mechanical pump,
When vacuum degree reaches 3-5Pa Shi Zaitong nitrogen into quartz ampoule, to quartzy intraductal pressure to normal pressure, which is repeated 3 times with to the greatest extent
It may be decreased the oxygen and steam in quartz ampoule.Nitrogen is used to grow molybdenum disulfide using the method for normal pressure as carrier gas, 35
The heating temperature of sulphur source and molybdenum source is risen to 170 DEG C and 680 DEG C respectively, the control reaction time is 5 min in min.Heating life
In long source and growth molybdenum disulfide all processes, the flow of nitrogen is 10 sccm.Stop heating after having grown molybdenum disulfide, etc.
It is down to room temperature naturally to tube furnace and takes out silicon wafer, then can be observed have a large amount of two sulphur of single layer on silicon wafer under an optical microscope
Change molybdenum.
Embodiment 2-7 mainly investigates substrate vulcanizing treatment temperature and prepares resulting single layer molybdenum disulfide to chemical vapor deposition
The influence of quality.With embodiment 1, difference is to change the temperature of substrate vulcanizing treatment specific implementation process.
1 embodiment of the present invention of table:
。
It is obtained by experimental result, optimum cure treatment temperature is 600 DEG C, is embodied in and prepares resulting single layer curing
Molybdenum has stronger luminous intensity and preferable electric property.The luminous intensity of resulting molybdenum disulfide is prepared slightly more than the temperature
There is decline.When being lower than 400 DEG C of curing temperature, it is almost unchanged to prepare resulting single layer molybdenum disulfide luminous intensity, then with
The raising of molybdenum sulfide treatment temperature, molybdenum disulfide luminous intensity enhancing.
The present invention is grinding for the basic research of New Two Dimensional material and the potential application of related two-dimensional material opto-electronic device
Study carefully and provides the reliable means of high quality sample preparation.
Claims (7)
1. a kind of preparation method for vulcanizing pretreated single layer molybdenum disulfide based on substrate, which is characterized in that specific step is as follows:
(1) vulcanizing treatment is carried out to silicon chip substrate: sulphur simple substance solid and silicon chip substrate is respectively placed in quartz test tube, adjusted
Sulphur source and substrate are to suitable position, respectively to sulphur simple substance and substrate in the double temperature-area tubular furnaces for being continually fed into nitrogen protection gas
Heating forms the sulfuric horizon that chemical bond is formed with sulphur in substrate surface under sulfur vapor environment;
(2) on the substrate handled through step (1) 50-100 μm of ol/L of spin coating 3,4,9,10 ,-pyrene tetracarboxylic acid acid potassium salt
Solution, to promote the nucleation and growth of molybdenum disulfide;
(3) using elemental sulfur and molybdenum source molybdenum trioxide powder as growth source, substrate and elemental sulfur, molybdenum source to suitable position are adjusted,
Grow single layer molybdenum disulfide on the substrate handled through step (2) using chemical vapour deposition technique to get fine to optical quality
Single layer molybdenum disulfide.
2. preparation method according to claim 1, which is characterized in that silicon wafer described in step (1) contains 300 ± 10 nm
Thick oxide layer needs to clean before carrying out vulcanizing treatment to it, to remove the impurity of silicon chip surface.
3. preparation method according to claim 2, which is characterized in that elemental sulfur described in step (1) and substrate it is suitable
Distance 22-24 cm;Before to elemental sulfur and silicon, the air in quartz ampoule is taken away using mechanical pump, when vacuum degree reaches
To 3-5Pa Shi Zaitong nitrogen into quartz ampoule, to quartzy intraductal pressure to normal pressure, which repeats 2-4 times to reduce as far as possible
Oxygen and steam in quartz ampoule.
4. preparation method according to claim 3, which is characterized in that in step (1), the temperature to sulphur simple substance heating is
170-200 DEG C, the heating temperature to substrate is 200-700 DEG C, and substrate curing time is 0.5-1 h.
5. preparation method according to claim 1,2 or 3, which is characterized in that the detailed process of step (2) are as follows: by PTAS
It being dissolved in isopropanol, the silicon wafer that vulcanizing treatment is crossed is placed on sol evenning machine and drips 3-5 μ L 3, and 4,9,10 ,-pyrene tetrabasic carboxylic acid
Potassium salt soln carries out spin coating, and control spin coating machine speed is 1000-2000 r/min, spin-coating time 1-3min.
6. preparation method according to claim 5, which is characterized in that in step (3), the dosage for controlling elemental sulfur is
120-200 mg, the dosage of molybdenum trioxide are 2-5 mg, and the distance of elemental sulfur and substrate is 20-24 cm, substrate and molybdenum source away from
From for 0.5-1 cm, and substrate is placed upward.
7. preparation method according to claim 5, which is characterized in that in step (3), adjust growth source and substrate
Behind position, use nitrogen as carrier gas;Before to growth source and silicon, the air in quartz ampoule is taken out first with mechanical pump
It walks, when vacuum degree reaches 3-5Pa Shi Zaitong nitrogen into quartz ampoule, to quartzy intraductal pressure to normal pressure, which is repeated 2-4 times
To reduce the oxygen and steam in quartz ampoule as far as possible;Molybdenum disulfide, In are then grown using the method for aumospheric pressure cvd
The heating temperature of sulphur source and molybdenum source is risen into 160-190 DEG C and 650-700 DEG C respectively in 35-40 min, when control is reacted
Between be 3-5 min;In heat growth source and growth molybdenum disulfide all processes, control nitrogen flow is 10-50 sccm.
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CN112079386A (en) * | 2020-09-16 | 2020-12-15 | 长春理工大学 | MoS2Preparation method for regulating and controlling S vacancy defects of two-dimensional material |
CN113046692A (en) * | 2021-03-17 | 2021-06-29 | 四川大学 | Preparation method of single-crystal tungsten diselenide monolayer film |
CN113511681A (en) * | 2020-04-09 | 2021-10-19 | 北京大学 | Method for locally growing transition metal chalcogenide with assistance of chalcogenide wafer |
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CN112079386A (en) * | 2020-09-16 | 2020-12-15 | 长春理工大学 | MoS2Preparation method for regulating and controlling S vacancy defects of two-dimensional material |
CN113046692A (en) * | 2021-03-17 | 2021-06-29 | 四川大学 | Preparation method of single-crystal tungsten diselenide monolayer film |
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