CN105002476B - A kind of method of the chemical vapor deposition growth large scale single-layer molybdenum disulfide film of substrate modification - Google Patents
A kind of method of the chemical vapor deposition growth large scale single-layer molybdenum disulfide film of substrate modification Download PDFInfo
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Abstract
The present invention proposes a kind of method of the chemical gas-phase method growing large-size individual layer molybdenum disulfide of substrate modification.To vulcanize ammonia as substrate surface dressing agent, by the means such as the concentration, soak time, cleaning method of controlled modification agent control nucleation rate, the means control film thickness such as growth temperature, growth time, throughput by controlling chemical vapor deposition.Can be on the basis of original growth chemical vapor depsotition equipment, under the conditions of relatively low growth temperature, efficient growing large-size single-layer molybdenum disulfide film using the present invention.The growing method for the large scale individual layer molybdenum disulfide that the present invention is provided is applied to the similar two-dimensional semiconductor material of structure, such as growth of large scale individual layer tungsten disulfide, two selenizing molybdenums and two tungsten selenides.
Description
Technical field
The present invention relates to the method that chemical vapor deposition prepares film, especially a kind of chemical vapor deposition of substrate modification
The method of growing large-size single-layer molybdenum disulfide film.
Background of invention
Individual layer molybdenum disulfide (MoS2) is a kind of new two-dimensional semiconductor material, with a preferable band gap
(1.8eV), the FET (FET) based on it can not only obtain 108High on-off ratio, and damaged with relatively low energy
Consumption.On the other hand, crystal of molybdenum disulfide single layer structure is a kind of direct band-gap semicondictor, and the change of band structure can be effective
Improve fluorescence efficiency and the photoabsorption cross-section of individual layer molybdenum disulfide.Molybdenum atom and sulphur in the alveolate texture of individual layer molybdenum disulfide
Atom alternately occupies adjacent lattice-site position, and the center inverting that macroscopical crystal has symmetrically is destroyed；Meanwhile, transition metal
The strong SO coupling effect of d electronics, causes individual layer molybdenum disulfide to have a kind of new electronic state --- energy valley quantum
State.Thus, it could be seen that individual layer molybdenum disulfide is as the new material complementary with graphene, not only future will be in sophisticated semiconductor, micro-
Nanometer electronic device field has highly important application prospect, and to the research pair of the physical characteristics such as its band structure, energy valley
Condensed state physics and opto-electronics have important value.
Preparing the method for individual layer molybdenum disulfide at present mainly includes：Mechanical stripping method, chemical stripping method and vapour deposition.Machine
Single-layer molybdenum disulfide film size prepared by tool and chemical peeling is smaller, it is impossible to meet extensive microelectronics preparation technology's
It is required that.Chemical gaseous phase depositing process (CVD) is considered as a kind of method of effective growth single-layer molybdenum disulfide film, and it utilizes height
The vulcanization reaction of gaseous sulfur and molybdenum oxide under the conditions of temperature, realizes deposition growing monocrystalline on various substrates/polycrystalline individual layer molybdenum disulfide.
It is in conventional chemical vapor deposition process to use silicon-silica as growth substrates more, using silicon-silica as growth substrates one
Aspect is conducive to growing the follow-up observation of sample, and on the other hand, silicon-silicon dioxide substrates have natural conductive layer and medium
Layer, grow obtained sample directly can process using late device, reduce technological process reduction and prepare cost.However, at present
Chemical vapor deposition growth molybdenum disulfide is present, and film forming area is small, the shortcomings of thickness of sample is difficult to control.How big chi is obtained
Very little, single-layer molybdenum disulfide film growth has become one of emphasis and focus of current two-dimensional semiconductor Material Field research.
Certainly the breakthrough of this technology can not only drive similar two-dimensional semiconductor material, such as large scale individual layer tungsten disulfide, two selenium
Change molybdenum and two tungsten selenides etc., the breakthrough of preparation technology, and by be novel semiconductor material, integrated circuit fields development it is important
Motive force.Therefore, large scale, the growing technology of single-layer molybdenum disulfide film have huge market prospects.
Substrate surface modification technique is that one kind can effectively improve epitaxial growth nucleation rate, is realized in low temperature and low saturation
The method of sample grown under state, and select economical and efficient substrate modification agent be the Technique Popularizing key factor.The present invention
A kind of silicon-silicon dioxide growth substrate surface modification, the method for chemical gas-phase method growing large-size individual layer molybdenum disulfide are proposed, is led to
The means such as the concentration, soak time, cleaning method of controlled modification agent control nucleation rate is crossed, during by controlling growth temperature, growth
Between, the means such as throughput control film thickness.Using the present invention can it is original growth chemical vapor depsotition equipment on the basis of,
Under the conditions of relatively low growth temperature, efficient growing large-size single-layer molybdenum disulfide film.
The content of the invention
The purpose of the present invention is to overcome current chemical vapor deposition growth molybdenum disulfide film size smaller, film thickness
Uppity shortcoming, proposes a kind of side of the chemical vapor deposition growth large scale individual layer molybdenum disulfide of substrate surface modification
Method.
The technical scheme is that, the side of the chemical vapor deposition growth large scale single-layer molybdenum disulfide film of substrate modification
Method, comprises the following steps：1) in vulcanization ammonia solution, surface modification is carried out to epitaxial growth substrate so that substrate surface is formed
The sulfuric horizon of one layer of chemical bonding；2) in the heating furnace for going back protective gas is continually fed into, to being put into step 1 wherein) in institute
The substrate annealing after surface modification is stated, the sulphur simple substance of excess surface is eliminated；3) using chemical vapour deposition technique in step 2) in institute
State and molybdenum disulfide film is grown on the substrate surface of annealing, that is, obtain the large scale single-layer molybdenum disulfide film；The annealing
The annealing temperature of processing is 100-500 DEG C, and annealing time is 10min-60min.In above-mentioned preparation method, step 1) in, it is described
The step of epitaxial growth substrate also includes cleaning it before surface modification processing, to change to its surface hydrophilicity
Property, comprise the following steps that：It is cleaned by ultrasonic 10 minutes respectively through acetone, ethanol and deionized water first, recycles sulfuric acid and mistake
Hydrogen oxide volume ratio is (3-5)：1 mixed solution is cleaned 30 minutes at 160 DEG C, then is cleaned by ultrasonic 5 points by deionized water
Clock removes the concentrated sulfuric acid of excess surface.
In above-mentioned preparation method, step 1) in, the concentration of the vulcanization ammonia is 40-44wt%, during the immersion of growth substrate
Between be 24 hours.
In above-mentioned preparation method, step 1) in, including the substrate after surface modification is cleaned by ultrasonic, cleaning agent is goes
Ionized water, scavenging period is 2min, high pure nitrogen drying.
In above-mentioned preparation method, step 1) in, also including by the substrate after processing, being dried under vacuum environment, removing surface
Remaining organic matter.The epitaxial growth substrate concretely silicon-silicon dioxide substrates, quartz substrate, alundum (Al2O3) substrate,
The epitaxial growth substrate is that the thickness of silica in commercially produced product, the silicon-silicon dioxide substrates is about 10nm-
500nm, the quartz substrate, the aufwuchsplate of alundum (Al2O3) substrate can be [100], a variety of crystal faces such as [111].
In above-mentioned preparation method, step 2) in, the protective gas concretely high pure nitrogen.
The flow for going back protective gas is 10sccm-300sccm.
In above-mentioned preparation method, step 3) in, in the chemical vapour deposition technique, using height dual temperature area heating means,
The low-temperature space places solid material sulphur, and the sulphur powder purity is not less than 99.9%, and heating-up temperature is 400 DEG C, the high-temperature region
Solid material molybdenum trioxide solid powder is placed, the molybdenum trioxide purity is not less than 99.9%, and reaction temperature is 700-900
DEG C, the reaction time is 5-30min, and current-carrying gas flow is 20sccm-100sccm, the pressure growth at atmosphere of reaction system.
It is available to be spliced by monocrystalline individual layer triangular form molybdenum disulfide when the reaction time of the reaction is more than 10min
Continuous molybdenum disulfide film.
In above-mentioned preparation method, step 3) in, including to being pumped the air in quartz ampoule using oil-sealed rotary pump, take seriously
Reciprocal of duty cycle reaches leads to high-purity nitrogen again during 1.0*10-3Torr, the process is repeated 3 times, oxygen and water vapour in reduction quartz ampoule
Influence.
In above-mentioned preparation method, step 3) in, including to the different growth temperature controlled processes of warm area.Aoxidized first to three
Molybdenum warm area is heated, and heating rate control is heated to 800 DEG C for 20 DEG C/min；When the heating-up temperature of molybdenum trioxide reaches 400 DEG C,
Solid sulfur is begun to warm up, and the rate of heat addition is heated to 400 DEG C for 40 DEG C/min；When low temperature and high-temperature region reach the peak of setting
When, current-carrying gas is opened, the flow of current-carrying gas is 100sccm；Growth continues 5~20 minutes.
In above-mentioned preparation method, step 3) in, also including to growing the obtained thin progress of large scale individual layer molybdenum disulfide
Sample specifically can be moved to room temperature region by the step of fast cooling, the cooling from high-temperature region, rapid to terminate the of molybdenum disulfide
Two layers deposition, or raw material molybdenum trioxide growth.
The present invention is by above-mentioned preparation method preparation-obtained monocrystalline individual layer triangular form molybdenum disulfide and its is spliced
Continuous molybdenum disulfide film belongs to protection scope of the present invention.
The coating material similar to vulcanization ammonia belongs to protection scope of the present invention in described above-mentioned preparation method.
Beneficial effects of the present invention：Preparation method of the present invention is given birth to by the chemical vapor deposition modified substrate surface
Growth temperature, time and gas flow are adjusted in long molybdenum disulfide growth course, can be efficiently prepared large size
Single-layer molybdenum disulfide film, this method can use different type, and various sizes of growth substrates obtain extensive batch
Molybdenum disulfide film, without higher growth temperature, without expensive coating material, without longer preparation time.
Large scale single-layer molybdenum disulfide film can be prepared into the electronic device of specific function.
Brief description of the drawings
Fig. 1 is the optical photograph for the single-layer molybdenum disulfide film that embodiment 1 grows in silicon-silicon dioxide substrates；
Fig. 2 is the Raman spectrogram for the single-layer molybdenum disulfide film that embodiment 1 grows in silicon-silicon dioxide substrates；
Fig. 3 is the fluorescence spectra for the single-layer molybdenum disulfide film that embodiment 1 grows in silicon-silicon dioxide substrates.
Embodiment
Embodiment 1
Using silicon-silicon dioxide substrates as growth substrates, the thickness of the wherein silicon dioxide layer of silicon face heat treatment is
300nm.Substrate processes are as follows：Silicon-silicon dioxide substrates are cleaned first, by acetone, ethanol and deionized water
Ultrasound is respectively washed 10 minutes, and it is 3 with hydrogen peroxide volume ratio to recycle sulfuric acid:1 mixed solution cleans 30 points at 160 DEG C
Clock, then it is cleaned by ultrasonic the concentrated sulfuric acid for removing excess surface for 5 minutes by deionized water；Silicon-silica after finishing will be cleaned
Substrate, which is put into 40-44wt% vulcanization ammonia solution, to be soaked 24 hours, and silicon-silicon dioxide substrates after immersion are finally in deionization
It is cleaned by ultrasonic 2 minutes in water, substrate is dried up with high pure nitrogen；Silicon after drying-silicon dioxide substrates vacuum is preserved 24 hours,
Remove remaining organic matter.By above-mentioned 300 DEG C of annealing 30min of substrate in nitrogen atmosphere stove.Use above-mentioned silicon-silicon dioxide substrates
Molybdenum disulfide film is grown in vacuum tube furnace.Growth course is as follows：Using growth raw material be high-purity molybdenum trioxide and sulphur,
Current-carrying gas is high-purity nitrogen, and growth furnace is dual temperature area tubular type growth furnace, and solid sulfur is placed on low-temperature space, molybdenum trioxide and silicon
Piece is placed on the reaction zone of high temperature jointly, and silicon chip is 2 centimetres with molybdenum trioxide distance, and carrier gas flow direction is bin cure to three
Molybdenum oxide；First, the air in quartz ampoule is pumped using oil-sealed rotary pump, when vacuum reaches 1.0*10-3Lead to again during Torr
High-purity nitrogen, the process is repeated 3 times；Molybdenum disulfide film epitaxial growth is growth at atmosphere, and growth course reaction zone adds first
Heat, 20 DEG C/min is heated to 800 DEG C；When the heating-up temperature of molybdenum trioxide reaches 400 DEG C, solid sulfur is begun to warm up, heating speed
Rate is heated to 400 DEG C for 40 DEG C/min；When low temperature and high-temperature region reach the peak of setting, current-carrying gas, current-carrying are opened
The flow of gas is 100sccm；Growth continues 5~20 minutes；After growth terminates, electric furnace is cooled to room temperature automatically, and the process begins
Current-carrying gas is passed through eventually.
Fig. 1 show the molybdenum disulfide single thin film optical photograph grown in typical silicon-silicon dioxide substrates.Single two
The size of vulcanization molybdenum single crystal triangle can reach 100um, after these monocrystalline triangles mutually splice, and it is several that can form size
The polycrystal film of millimeter, polycrystal film surfacing, crystal boundary is not obvious.
Fig. 2 is the Raman spectrum of the molybdenum disulfide single thin film grown in typical silicon-silicon dioxide substrates.Raman excitation
Wavelength is 382cm in 514nm, spectrum-1The Raman vibration peak at place is the E of molybdenum disulfide1 2gRaman Vibration Mode, 402cm-1Place
Raman vibration peak is the A of molybdenum disulfidel gRaman Vibration Mode.The wherein E of molybdenum disulfide1 2gAnd Al gThe difference of mode vibration frequency
It is related to the thickness of film, their difference on the frequency can be calculated from figure for 20cm-1For the feature of individual layer molybdenum disulfide.
Fig. 3 is the fluorescence emission spectrum of the molybdenum disulfide single thin film grown in typical silicon-silicon dioxide substrates.It is glimmering
Light excitation wavelength is 514nm, and the big ripple bag in spectrum near 680nm is individual layer molybdenum disulfide exciton fluorescence.Individual layer molybdenum disulfide
Compared with block molybdenum disulfide, because band structure from indirect band gap transitions is direct band gap, photoluminescence intensity significantly improves.
Embodiment 2
With alundum (Al2O3) (Al2O3) substrate be growth substrates, wherein thin film deposition face be alundum (Al2O3) (100) face.
Substrate processes are as follows：Alundum (Al2O3) substrate is cleaned first, by acetone, ethanol and deionized water ultrasound respectively
Cleaning 10 minutes, it is 3 with hydrogen peroxide volume ratio to recycle sulfuric acid:1 mixed solution is cleaned 30 minutes at 160 DEG C, then is passed through
Cross deionized water and be cleaned by ultrasonic the concentrated sulfuric acid for removing excess surface for 5 minutes；The alundum (Al2O3) substrate cleaned after finishing is put into
Soaked 24 hours in 40-44wt% vulcanization ammonia solution, the alundum (Al2O3) substrate after immersion is last ultrasonic in deionized water
Cleaning 2 minutes, substrate is dried up with high pure nitrogen；Alundum (Al2O3) substrate vacuum after drying is preserved 24 hours, removed remaining
Organic matter..By above-mentioned 300 DEG C of annealing 30min of substrate in nitrogen atmosphere stove.Using above-mentioned alundum (Al2O3) substrate in vacuum tube
Growth molybdenum disulfide film in formula stove.Growth course is as follows：The use of growth raw material is high-purity molybdenum trioxide and sulphur, current-carrying gas
For high-purity nitrogen, growth furnace is dual temperature area tubular type growth furnace, and solid sulfur is placed on low-temperature space, molybdenum trioxide and alundum (Al2O3)
Substrate is placed on the reaction zone of high temperature jointly, and alundum (Al2O3) substrate is 2 centimetres, carrier gas flow side with molybdenum trioxide distance
To being bin cure to molybdenum trioxide；First, the air in quartz ampoule is pumped using oil-sealed rotary pump, when vacuum reaches 1.0*
10-3Lead to high-purity nitrogen during Torr again, the process is repeated 3 times；Molybdenum disulfide film epitaxial growth is growth at atmosphere, growth course
Reaction zone is heated first, and 20 DEG C/min is heated to 800 DEG C；When the heating-up temperature of molybdenum trioxide reaches 400 DEG C, solid sulfur starts
Heating, the rate of heat addition is heated to 400 DEG C for 40 DEG C/min；When low temperature and high-temperature region reach the peak of setting, open and carry
Gas body, the flow of current-carrying gas is 100sccm；Growth continues 5~20 minutes；After growth terminates, electric furnace is cooled to room automatically
Temperature, the process is passed through current-carrying gas all the time.
The implementation of the present invention does not have the restriction present invention, and any simple modifications based on the present invention are not departing from the present invention
Claimed scope.
Claims (10)
1. a kind of method of the chemical vapor deposition growth large scale single-layer molybdenum disulfide film of substrate surface modification, it is characterized in that
Comprise the following steps：1) in vulcanization ammonia solution, surface modification is carried out to epitaxial growth substrate so that one layer of substrate surface formation
The sulfuric horizon of chemical bonding；2) in the heating furnace of protective gas is continually fed into, to being put into step 1 wherein) described in surface
Substrate annealing after modification, eliminates the sulphur simple substance of excess surface；3) using chemical vapour deposition technique in step 2) described in anneal
Substrate surface on grow molybdenum disulfide film, that is, obtain the large scale single-layer molybdenum disulfide film；The annealing
Annealing temperature is 100-500 DEG C, and annealing time is 10min-60min.
2. according to the method described in claim 1, it is characterized in that, step 1) in, the epitaxial growth substrate is at surface modification
The step of also including cleaning it before reason, to be modified to its surface hydrophilicity, comprise the following steps that：Distinguish first
It is cleaned by ultrasonic 10 minutes by acetone, ethanol and deionized water, it is 3-5 with hydrogen peroxide volume ratio to recycle sulfuric acid：1 mixing
Solution is cleaned 30 minutes at 160 DEG C, then is cleaned by ultrasonic the concentrated sulfuric acid for removing excess surface for 5 minutes by deionized water.
3. method according to claim 2, it is characterized in that, step 1) in, the concentration of the vulcanization ammonia is 40-44wt%, raw
The soak time of long substrate is 24 hours.
4. method according to claim 3, it is characterized in that, step 1) in, including the substrate after surface modification surpassed
Sound is cleaned, and cleaning agent is deionized water, and scavenging period is 2min, high pure nitrogen drying.
5. method according to claim 4, it is characterized in that, step 1) in, also including by the substrate after processing, vacuum environment
Lower drying, removes the organic matter of surface residual.
6. the method according to one of claim 1-5, it is characterized in that, the epitaxial growth substrate is silicon-titanium dioxide silicon substrate
Piece, quartz substrate, alundum (Al2O3) substrate, the epitaxial growth substrate are commercially produced product, in the silicon-silicon dioxide substrates
The thickness of silica is 10nm-500nm, and the quartz substrate, the aufwuchsplate of alundum (Al2O3) substrate are [100] or [111]
Crystal face.
7. the method according to one of claim 1-5, it is characterized in that, step 2) in, the protective gas is high pure nitrogen；
The flow of the protective gas is 10sccm-300sccm.
8. the method according to one of claim 1-5, it is characterized in that, in the above method, step 3) in, the chemical gaseous phase
In sedimentation, using height dual temperature area heating means, low-temperature space places solid material sulphur, and sulphur powder purity is not less than 99.9%, plus
Hot temperature is 400 DEG C, and solid material molybdenum trioxide solid powder is placed in high-temperature region, and the molybdenum trioxide purity is not less than
99.9%, reaction temperature is 700-900 DEG C, and the reaction time is 5-30min, and current-carrying gas flow is 20sccm-100sccm, instead
The pressure for answering system is normal pressure.
9. method according to claim 8, it is characterized in that, when the reaction time of the reaction is more than 10min, obtain by list
The continuous molybdenum disulfide film that brilliant individual layer triangular form molybdenum disulfide is spliced.
10. method according to claim 8, it is characterized in that, step 3) in, using oil-sealed rotary pump by quartz ampoule
Air pump, when vacuum reaches 1.0*10-3Lead to high-purity nitrogen during Torr again, the process is repeated 3 times, in reduction quartz ampoule
The influence of oxygen and water vapour；To the different growth temperature controlled processes of warm area：Molybdenum trioxide warm area is heated first, heating speed
Rate control is heated to 800 DEG C for 20 DEG C/min；When the heating-up temperature of molybdenum trioxide reaches 400 DEG C, solid sulfur is begun to warm up, plus
Hot speed is heated to 400 DEG C for 40 DEG C/min；When low temperature and high-temperature region reach the peak of setting, current-carrying gas is opened,
The flow of current-carrying gas is 100sccm；Growth continues 5 ~ 20 minutes；Step 3) in, the large scale individual layer two obtained to growing
Vulcanize molybdenum film and carry out fast cooling, the cooling is that sample is moved into room temperature region from high-temperature region, and molybdenum disulfide is terminated rapidly
The second layer deposition, or raw material molybdenum trioxide growth.
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