CN105002476A - Method for growing substrate-modified large-size monolayer molybdenum disulfide film through chemical vapor deposition - Google Patents
Method for growing substrate-modified large-size monolayer molybdenum disulfide film through chemical vapor deposition Download PDFInfo
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Abstract
The invention proposes a method for growing a substrate-modified large-size monolayer molybdenum disulfide film through chemical vapor deposition. Ammonium sulfide serves as a substrate surface modifying agent; a nucleation rate is controlled through such methods as control of a concentration of the modifying agent, a dipping time and a cleaning method; and a film thickness is controlled through such methods as control of a growing temperature, a growing time and an air flow of the chemical vapor deposition. The method can efficiently grow the large-size monolayer molybdenum disulfide film under the condition of a relatively lower growing temperature on the basis of traditional growth chemical vapor deposition equipment. The method for growing large-size monolayer molybdenum disulfide, provided by the invention, is suitable for the growth of large-size monolayer tungsten disulfide, molybdenum diselenide, tungsten diselenide and the like similar to two-dimensional semiconductor materials in structure.
Description
Technical field
The present invention relates to the method that film is prepared in chemical vapour deposition, especially a kind of method of chemical vapor deposition growth large size single-layer molybdenum disulfide film of substrate modification.
Background of invention
Individual layer molybdenumdisulphide (MoS2) is a kind of novel two-dimensional semiconductor material, and have a desirable band gap (1.8eV), the field effect transistor (FET) based on it can not only obtain 10
8high on-off ratio, and there is lower energy waste.On the other hand, crystal of molybdenum disulfide single layer structure is a kind of direct band-gap semicondictor, and the change of energy band structure effectively can improve fluorescence efficiency and the photoabsorption cross-section of individual layer molybdenumdisulphide.In the polynuclear plane of individual layer molybdenumdisulphide, molybdenum atom and sulphur atom alternately occupy adjacent lattice point position, and the center inverting symmetry that macroscopical crystal has is destroyed; Meanwhile, the strong SO coupling effect of transition metal d electronics, causes individual layer molybdenumdisulphide to have a kind of new electronic state---energy valley quantum state.Therefore visible, individual layer molybdenumdisulphide is as the type material with Graphene complementation, not only following have very important application prospect by sophisticated semiconductor, micro-nano field of electronic devices, and have important value to the research of its physical property such as energy band structure, energy valley to condensed state physics and opto-electronics.
The method preparing individual layer molybdenumdisulphide at present mainly comprises: mechanically peel method, chemical stripping method and vapour deposition.Single-layer molybdenum disulfide film size prepared by machinery and chemical peeling is less, cannot meet the requirement of extensive microelectronics preparation technology.Chemical gaseous phase depositing process (CVD) is considered to a kind of method of effective growth single-layer molybdenum disulfide film, and it utilizes the vulcanization reaction of gaseous sulfur and molybdenum oxide under hot conditions, realizes deposition growing monocrystalline on various substrates/polycrystalline individual layer molybdenumdisulphide.Adopt silicon-silicon-dioxide as growth substrates in conventional chemical vapor deposition method more, with silicon-silicon-dioxide for growth substrates is conducive to the follow-up observation growing sample on the one hand, on the other hand, silicon-silicon dioxide substrates has natural conductive layer and medium layer, grow the sample obtained and directly can apply late device processing, reduce technical process and reduce preparation cost.But current chemical vapor deposition growth molybdenumdisulphide exists, the shortcomings such as film forming area is little, and thickness of sample is wayward.How to obtain large size, the growth of single-layer molybdenum disulfide film become current two-dimensional semiconductor Material Field research one of emphasis and focus.Certainly the breakthrough of this technology not only can drive similar two-dimensional semiconductor material, as large size individual layer tungsten disulfide, two selenizing molybdenums and two tungsten selenide etc., the breakthrough of preparation technology, and will be the important impetus of novel semiconductor material, integrated circuit fields development.Therefore, the growing technology of large size, single-layer molybdenum disulfide film has huge market outlook.
Substrate surface modification technique is that one effectively can improve epitaxy nucleation rate, realizes the method for sample grown under low temperature and low saturation state, and selects the substrate modification agent of economical and efficient to be the key factor of this technology popularization.The present invention proposes the method for a kind of silicon-silicon dioxide growth substrate surface modification, chemical gas-phase method growing large-size individual layer molybdenumdisulphide, controlling nucleation rate by the means such as concentration, soak time, purging method of controlled modification agent, controlling film thickness by controlling the means such as growth temperature, growth time, airshed.Utilize the present invention can on the basis of original growth chemical vapor depsotition equipment, under relatively low growth temperature condition, efficient growing large-size single-layer molybdenum disulfide film.
Summary of the invention
The object of the invention is, overcome current chemical vapor deposition growth molybdenum disulfide film size less, the uppity shortcoming of film thickness, propose the method for the chemical vapor deposition growth large size individual layer molybdenumdisulphide that a kind of substrate surface is modified.
Technical solution of the present invention is, the method of the chemical vapor deposition growth large size single-layer molybdenum disulfide film of substrate modification, comprise the steps: 1) in sulfuration ammonia solution, finishing is carried out to epitaxial growth substrate, make substrate surface form the sulfuric horizon of one deck chemical bonding; 2) go back in the process furnace of shielding gas, to putting into step 1 wherein continuing to pass into) described in substrate annealing after finishing, eliminate the sulphur simple substance of excess surface; 3) adopt chemical Vapor deposition process in step 2) described in annealing substrate surface on grow molybdenum disulfide film, namely obtain described large size single-layer molybdenum disulfide film; The annealing temperature of described anneal is 100-500 DEG C, and annealing time is 10min-60min.In above-mentioned preparation method, step 1) in, described epitaxial growth substrate also comprised the step of cleaning it before finishing process, to carry out modification to its surface hydrophilicity, concrete steps are as follows: first respectively through acetone, ethanol and deionized water ultrasonic cleaning 10 minutes, recycling sulfuric acid is (3-5) with hydrogen peroxide volume ratio: the mixing solutions of 1 cleans 30 minutes at 160 DEG C, then within 5 minutes, removes the vitriol oil of excess surface through deionized water ultrasonic cleaning.
In above-mentioned preparation method, step 1) in, the concentration of described sulfuration ammonia is 40-44wt%, and the soak time of growth substrate is 24 hours.
In above-mentioned preparation method, step 1) in, the substrate comprised after effects on surface modification carries out ultrasonic cleaning, and clean-out system is deionized water, and scavenging period is 2min, and high pure nitrogen dries up.
In above-mentioned preparation method, step 1) in, also comprise the substrate after by process, dry under vacuum environment, remove the organism of surface residual.Described epitaxial growth substrate specifically can be silicon-silicon dioxide substrates, quartz substrate, aluminium sesquioxide substrate, described epitaxial growth substrate is commercially produced product, in described silicon-silicon dioxide substrates, the thickness of silicon-dioxide is about 10nm-500nm, the aufwuchsplate of described quartz substrate, aluminium sesquioxide substrate can be [100], multiple crystal faces such as [111].
In above-mentioned preparation method, step 2) in, described protective gas specifically can be high pure nitrogen.
The described flow going back protective gas is 10sccm-300sccm.
In above-mentioned preparation method, step 3) in, in described chemical Vapor deposition process, adopt the two warm area heating means of height, solid material sulphur is placed in described cold zone, and described sulphur powder purity is not less than 99.9%, and Heating temperature is 400 DEG C, solid material molybdic oxide pressed powder is placed in described high-temperature zone, described molybdic oxide purity is not less than 99.9%, and temperature of reaction is 700-900 DEG C, and the reaction times is 5-30min, current-carrying gas flow is 20sccm-100sccm, the pressure growth at atmosphere of reaction system.
The reaction times of described reaction, when being greater than 10min, can obtain the continuous molybdenum disulfide film be spliced by monocrystalline individual layer triangular form molybdenumdisulphide.
In above-mentioned preparation method, step 3) in, comprise utilizing oil-sealed rotary pump to be pumped by the air in silica tube, the nitrogen logical high-purity again when vacuum tightness reaches 1.0*10-3Torr, this process repeats 3 times, reduces the impact of oxygen and water vapor in silica tube.
In above-mentioned preparation method, step 3) in, comprise the temperature controlled process of difference growth warm area.First to the heating of molybdic oxide warm area, it is that 20 DEG C/min is heated to 800 DEG C that temperature rise rate controls; When the Heating temperature of molybdic oxide reaches 400 DEG C, solid sulfur starts heating, and heating rate is that 40 DEG C/min is heated to 400 DEG C; When low temperature and high-temperature zone all reach the maximum of setting, open current-carrying gas, the flow of current-carrying gas is 100sccm; Growth continues 5 ~ 20 minutes.
In above-mentioned preparation method, step 3) in, also comprise to grow the thin step of carrying out fast cooling of large size individual layer molybdenumdisulphide obtained, sample specifically can be moved to room temperature region from high-temperature zone by described cooling, the second layer deposition of rapid termination molybdenumdisulphide, or the growth of raw material molybdic oxide.
The present invention all belongs to protection scope of the present invention by above-mentioned preparation method preparation-obtained monocrystalline individual layer triangular form molybdenumdisulphide and the continuous molybdenum disulfide film that is spliced thereof.
In described above-mentioned preparation method, the coating materials similar to sulfuration ammonia all belongs to protection scope of the present invention.
Beneficial effect of the present invention: preparation method of the present invention is regulated by growth temperature, time and gas flow in the chemical vapor deposition growth molybdenumdisulphide process of growth of modifying substrate surface, can efficiently prepare large size single-layer molybdenum disulfide film, the method can use dissimilar, the growth substrates of different size obtains the molybdenum disulfide film of extensive batch, without the need to higher growth temperature, without the need to expensive coating materials, without the need to longer preparation time.Large size single-layer molybdenum disulfide film can be prepared into the electron device of specific function.
Accompanying drawing explanation
Fig. 1 is the optical photograph of the single-layer molybdenum disulfide film that embodiment 1 grows in silicon-silicon dioxide substrates;
Fig. 2 is the Raman spectrogram of the single-layer molybdenum disulfide film that embodiment 1 grows in silicon-silicon dioxide substrates;
Fig. 3 is the fluorescence spectrum figure of the single-layer molybdenum disulfide film that embodiment 1 grows in silicon-silicon dioxide substrates.
Embodiment
Embodiment 1
With silicon-silicon dioxide substrates for growth substrates, wherein the thickness of the heat treated silicon dioxide layer of silicon face is 300nm.Substrate processes is as follows: first clean silicon-silicon dioxide substrates, through the ultrasonic cleaning respectively of acetone, ethanol and deionized water 10 minutes, recycling sulfuric acid cleans 30 minutes than the mixing solutions for 3:1 with hydrogen peroxide volume at 160 DEG C, then within 5 minutes, removes the vitriol oil of excess surface through deionized water ultrasonic cleaning; Sulfuration ammonia solution silicon-silicon dioxide substrates after cleaning being put into 40-44wt% soaks 24 hours, and the silicon-silicon dioxide substrates after immersion is ultrasonic cleaning 2 minutes in deionized water finally, dries up substrate with high pure nitrogen; Silicon-silicon dioxide substrates vacuum after drying up is preserved 24 hours, removes remaining organism.By above-mentioned substrate 300 DEG C annealing 30min in nitrogen atmosphere stove.Above-mentioned silicon-silicon dioxide substrates is used to grow molybdenum disulfide film in vacuum tube furnace.Process of growth is as follows: use growth raw material to be high-purity molybdic oxide and sulphur, current-carrying gas is high-purity nitrogen, growth furnace is two warm area tubular type growth furnace, solid sulfur is placed on cold zone, molybdic oxide and silicon chip are placed on the reaction zone of high temperature jointly, silicon chip and molybdic oxide distance are 2 centimetres, and carrier gas flow direction is that bin cure is to molybdic oxide; First, oil-sealed rotary pump is utilized to be pumped by the air in silica tube, when vacuum tightness reaches 1.0*10
-3nitrogen logical high-purity again during Torr, this process repeats 3 times; Molybdenum disulfide film epitaxy is growth at atmosphere, and first process of growth reaction zone heats, and 20 DEG C/min is heated to 800 DEG C; When the Heating temperature of molybdic oxide reaches 400 DEG C, solid sulfur starts heating, and heating rate is that 40 DEG C/min is heated to 400 DEG C; When low temperature and high-temperature zone all reach the maximum of setting, open current-carrying gas, the flow of current-carrying gas is 100sccm; Growth continues 5 ~ 20 minutes; After growth terminates, electric furnace is cooled to room temperature automatically, and this process passes into current-carrying gas all the time.
Figure 1 shows that the molybdenumdisulphide single thin film optical photograph that typical silicon-silicon dioxide substrates grows.The size of single molybdenumdisulphide monocrystalline triangle can reach 100um, and after these monocrystalline triangles splice mutually, can form the polycrystal film being of a size of several millimeters, polycrystal film surfacing, crystal boundary is not obvious.
Fig. 2 is the Raman spectrum of the molybdenumdisulphide single thin film that typical silicon-silicon dioxide substrates grows.Raman excitation wavelength is 514nm, 382cm in spectrum
-1the Raman vibration peak at place is the E of molybdenumdisulphide
1 2graman Vibration Mode, 402cm
-1the Raman vibration peak at place is the A of molybdenumdisulphide
l graman Vibration Mode.The wherein E of molybdenumdisulphide
1 2gand A
l gthe difference of mode vibration frequency is relevant to the thickness of film, and the difference on the frequency that can calculate them from figure is 20cm
-1for the feature of individual layer molybdenumdisulphide.
The fluorescence emission spectrum of molybdenumdisulphide single thin film of Fig. 3 for typical silicon-silicon dioxide substrates grows.Fluorescence exciting wavelength is 514nm, and the large ripple bag in spectrum near 680nm is individual layer molybdenumdisulphide exciton fluorescence.Individual layer molybdenumdisulphide is compared with block molybdenumdisulphide, and because energy band structure is direct band gap from indirect band gap transitions, photoluminescence intensity significantly improves.
Embodiment 2
With aluminium sesquioxide (Al
2o
3) substrate is growth substrates, wherein thin film deposition face is (100) face of aluminium sesquioxide.Substrate processes is as follows: first clean aluminium sesquioxide substrate, through the ultrasonic cleaning respectively of acetone, ethanol and deionized water 10 minutes, recycling sulfuric acid cleans 30 minutes than the mixing solutions for 3:1 with hydrogen peroxide volume at 160 DEG C, then within 5 minutes, removes the vitriol oil of excess surface through deionized water ultrasonic cleaning; Sulfuration ammonia solution aluminium sesquioxide substrate after cleaning being put into 40-44wt% soaks 24 hours, and the last ultrasonic cleaning in deionized water of the aluminium sesquioxide substrate after immersion 2 minutes, dries up substrate with high pure nitrogen; Aluminium sesquioxide substrate vacuum after drying up is preserved 24 hours, removes remaining organism.。By above-mentioned substrate 300 DEG C annealing 30min in nitrogen atmosphere stove.Above-mentioned aluminium sesquioxide substrate is used to grow molybdenum disulfide film in vacuum tube furnace.Process of growth is as follows: use growth raw material to be high-purity molybdic oxide and sulphur, current-carrying gas is high-purity nitrogen, growth furnace is two warm area tubular type growth furnace, solid sulfur is placed on cold zone, molybdic oxide and aluminium sesquioxide substrate are placed on the reaction zone of high temperature jointly, aluminium sesquioxide substrate and molybdic oxide distance are 2 centimetres, and carrier gas flow direction is that bin cure is to molybdic oxide; First, oil-sealed rotary pump is utilized to be pumped by the air in silica tube, when vacuum tightness reaches 1.0*10
-3nitrogen logical high-purity again during Torr, this process repeats 3 times; Molybdenum disulfide film epitaxy is growth at atmosphere, and first process of growth reaction zone heats, and 20 DEG C/min is heated to 800 DEG C; When the Heating temperature of molybdic oxide reaches 400 DEG C, solid sulfur starts heating, and heating rate is that 40 DEG C/min is heated to 400 DEG C; When low temperature and high-temperature zone all reach the maximum of setting, open current-carrying gas, the flow of current-carrying gas is 100sccm; Growth continues 5 ~ 20 minutes; After growth terminates, electric furnace is cooled to room temperature automatically, and this process passes into current-carrying gas all the time.
Enforcement of the present invention does not limit the present invention, does not anyly exceed the scope of protection of present invention based on simple modifications of the present invention.
Claims (10)
1. the method for the chemical vapor deposition growth large size single-layer molybdenum disulfide film of a substrate surface modification, it is characterized in that comprising the steps: 1) in sulfuration ammonia solution, finishing is carried out to epitaxial growth substrate, makes substrate surface form the sulfuric horizon of one deck chemical bonding; 2) go back in the process furnace of shielding gas, to putting into step 1 wherein continuing to pass into) described in substrate annealing after finishing, eliminate the sulphur simple substance of excess surface; 3) adopt chemical Vapor deposition process in step 2) described in annealing substrate surface on grow molybdenum disulfide film, namely obtain described large size single-layer molybdenum disulfide film; The annealing temperature of described anneal is 100-500 DEG C, and annealing time is 10min-60min.
2. method according to claim 1, it is characterized in that, step 1) in, described epitaxial growth substrate also comprised the step of cleaning it before finishing process, to carry out modification to its surface hydrophilicity, concrete steps are as follows: first respectively through acetone, ethanol and deionized water ultrasonic cleaning 10 minutes, recycling sulfuric acid is (3-5) with hydrogen peroxide volume ratio: the mixing solutions of 1 cleans 30 minutes at 160 DEG C, then within 5 minutes, removes the vitriol oil of excess surface through deionized water ultrasonic cleaning.
3. method according to claim 2, is characterized in that, step 1) in, the concentration of described sulfuration ammonia is 40-44wt%, and the soak time of growth substrate is 24 hours.
4. method according to claim 3, is characterized in that, step 1) in, the substrate comprised after effects on surface modification carries out ultrasonic cleaning, and clean-out system is deionized water, and scavenging period is 2min, and high pure nitrogen dries up.
5. method according to claim 4, is characterized in that, step 1) in, also comprise the substrate after by process, dry under vacuum environment, remove the organism of surface residual.
6. according to the method one of claim 1-5 Suo Shu, it is characterized in that, described epitaxial growth substrate specifically can be silicon-silicon dioxide substrates, quartz substrate, aluminium sesquioxide substrate, described epitaxial growth substrate is commercially produced product, in described silicon-silicon dioxide substrates, the thickness of silicon-dioxide is about 10nm-500nm, the aufwuchsplate of described quartz substrate, aluminium sesquioxide substrate is [100], multiple crystal faces such as [111].
7., according to the method one of claim 1-5 Suo Shu, it is characterized in that, step 2) in, described protective gas specifically can be high pure nitrogen; The described flow going back protective gas is 10sccm-300sccm.
8. according to the method one of claim 1-5 Suo Shu, it is characterized in that, in above-mentioned preparation method, step 3) in, in described chemical Vapor deposition process, adopt the two warm area heating means of height, solid material sulphur is placed in described cold zone, described sulphur powder purity is not less than 99.9%, Heating temperature is 400 DEG C, solid material molybdic oxide pressed powder is placed in described high-temperature zone, described molybdic oxide purity is not less than 99.9%, temperature of reaction is 700-900 DEG C, reaction times is 5-30min, current-carrying gas flow is 20sccm-100sccm, the pressure growth at atmosphere of reaction system.
9. method according to claim 8, is characterized in that, when the reaction times of described reaction is greater than 10min, obtains the continuous molybdenum disulfide film be spliced by monocrystalline individual layer triangular form molybdenumdisulphide.
10. method according to claim 8, is characterized in that, step 3) in, comprise utilizing oil-sealed rotary pump to be pumped by the air in silica tube, the nitrogen logical high-purity again when vacuum tightness reaches 1.0*10-3Torr, this process repeats 3 times, reduces the impact of oxygen and water vapor in silica tube; To the temperature controlled process of difference growth warm area: first to the heating of molybdic oxide warm area, it is that 20 DEG C/min is heated to 800 DEG C that temperature rise rate controls; When the Heating temperature of molybdic oxide reaches 400 DEG C, solid sulfur starts heating, and heating rate is that 40 DEG C/min is heated to 400 DEG C; When low temperature and high-temperature zone all reach the maximum of setting, open current-carrying gas, the flow of current-carrying gas is 100sccm; Growth continues 5 ~ 20 minutes; Step 3) in, to grow the thin step of carrying out fast cooling of large size individual layer molybdenumdisulphide obtained, sample specifically can be moved to room temperature region from high-temperature zone by described cooling, stops rapidly the second layer deposition of molybdenumdisulphide, or the growth of raw material molybdic oxide.
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| CN115011925B (en) * | 2022-05-19 | 2023-08-08 | 甘肃省科学院传感技术研究所 | Low-dimensional layered molybdenum disulfide film material and preparation method thereof |
| CN115231616A (en) * | 2022-07-19 | 2022-10-25 | 南京大学 | Method for preparing molybdenum disulfide micropore pattern without mask |
| CN115231616B (en) * | 2022-07-19 | 2023-06-16 | 南京大学 | Method for preparing molybdenum disulfide micropore pattern without mask |
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