CN108341431A - A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap - Google Patents
A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap Download PDFInfo
- Publication number
- CN108341431A CN108341431A CN201810092998.0A CN201810092998A CN108341431A CN 108341431 A CN108341431 A CN 108341431A CN 201810092998 A CN201810092998 A CN 201810092998A CN 108341431 A CN108341431 A CN 108341431A
- Authority
- CN
- China
- Prior art keywords
- nanometer sheet
- temperature
- molybdenum dioxide
- molybdenum
- band gap
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap.It is an object of the invention to carry out sulfur doping to molybdenum dioxide nanometer sheet to adjust the technique study of band gap, the nanometer sheet of different band gap is obtained, and then micro-nano electronic device manufacturing field can be applied to, and obtain the electronic device haveing excellent performance.The disadvantage that it is an object of the invention to overcome molybdenum dioxide band gap excessive, the band gap of the molybdenum dioxide nanometer sheet of preparation is adjusted, in order to realize the purpose, a kind of method that molybdenum dioxide nanometer sheet band gap is adjusted is we disclosed, the sulfur doping degree of the control and regulation nanometer sheet of the ratio and growth temperature of presoma sulphur powder and molybdenum trioxide powder is passed through.Finally in the molybdenum dioxide nanometer sheet for obtaining different band gap.Processing step disclosed in this invention is simple, easily-controlled reaction conditions, is suitable for industrialized production, and product has excellent electrical properties, has huge application value in micro-nano electronics device field.
Description
Technical field
The present invention relates to the preparation methods that a kind of sulfur doping adjusts molybdenum dioxide nanometer plate shape and band gap, belong to new material
Preparing technical field.
Background technology
Molybdenum dioxide is a kind of wide bandgap semiconductor, has the superiority such as excellent optics, electricity, catalysis, electrochromism
Can, these performances make molybdenum dioxide have in catalyst, flat-panel monitor, sensor, electrochromic device and lithium battery etc.
Very big application value.
Semiconductor material with wide forbidden band has broad-band gap, high critical breakdown electric field, high heat conductance, high carrier saturation drift speed
The features such as spending has huge application potential in high temperature, high frequency, high-power, photoelectron and radioresistance etc..In addition titanium dioxide
Molybdenum preparation method of nano material is various, and cost is relatively low, and therefore, molybdenum dioxide prepares the excellent candidate material research of micro-nano electronic device
Persons prepare the nano material of two-dimentional molybdenum dioxide using various methods, but mostly exist low output, complex process, purity it is low,
The shortcomings of band gap is unadjustable, the research being applied to also only are in laboratory stage, to realize the application of related device, need
Preparation method and property are advanced optimized.
Invention content
It is an object of the invention to overcome prepare low output, technique in prepared by molybdenum dioxide nanometer sheet is cumbersome, band gap can not
The problem of adjusting, studies preparation method, so as to obtain the ultra-thin titanium dioxide of different shape and band gap on a large scale
Molybdenum nanometer sheet, and then molybdenum dioxide can be applied to micro-nano electronic device manufacturing field.
The method disclosed in the present uses simple and practicable chemical vapour deposition technique, by the way of thermal evaporation vulcanization,
By selecting different preparation parameters, the nanometer sheet of different shape and band gap can be respectively obtained.Operation is simple, and reaction condition is easy
In grasp, raw material is non-toxic, has good industrial production prospect.We use preparation side disclosed in this invention simultaneously
Method, by the way that different growth parameter(s)s is arranged, to obtain the molybdenum dioxide nanometer flake products of two kinds of different shapes and band gap.
Technical scheme of the present invention
A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap, the preparation method be with
Sulphur powder is presoma with molybdenum trioxide powder, and argon gas is carrier gas, passes through the ratio for controlling presoma and the height for adjusting growth temperature
Obtain the molybdenum dioxide nanometer sheet of different shape and band gap;Wherein, the mass ratio of sulphur powder and molybdenum trioxide powder is 20:1~20:3;
Growth temperature is 700 DEG C~800 DEG C.
The present invention prepares the molybdenum dioxide nanometer sheet of different shape and different band gap by control variate method, we are particularly
It is open to use following two different modes:
First way is to change the ratio of presoma, 700 DEG C of the high-temperature region temperature, the matter of sulphur powder and molybdenum trioxide powder
Amount is respectively 100mg:5mg, 100mg:10mg and 100mg:15mg(20:1~20:3), other parameters are the same.Prepare triangle,
The molybdenum dioxide nanometer sheet of pentagon and diamond shape.
The second way is to adjust the height of growth temperature, and the sulphur powder and the quality of molybdenum trioxide powder are respectively 100mg:
5mg, 700 DEG C, 750 DEG C and 800 DEG C of high-temperature region temperature, other parameters are the same.Also the dioxy of triangle, pentagon and diamond shape is prepared
Change molybdenum nanometer sheet.
Further, we have refined the preparation method of molybdenum dioxide nanometer sheet, include the following steps:Substrate treatment, medicine
Product weigh and equipment debugging, specifically grow three parts.Prepare product molybdenum dioxide nanometer sheet, specific growth step:
(1) Substrate treatment.By SiO2/ Si substrate bases each ultrasound 10min under deionized water, acetone and isopropanol, goes
Except the impurity and organic matter on surface;Again in Piranha washing lotion (H2SO4:H2O2=3:1) 90min is impregnated in;It is super with deionized water again
Sound 15min finally uses argon gas rifle to dry up;
(2) drug weighing and equipment debugging.Weigh sulphur powder and molybdenum trioxide powder in proportion with high Accuracy Electronic Balance, respectively
It is put in two quartz boats, sulphur powder is put in close to the low-temperature space at air inlet, molybdenum trioxide is put in the high temperature close to exhaust outlet
Area, while SiO2/ Si substrates are positioned over the top of molybdenum trioxide powder, and polishing is face-down.Set the heating and heat preservation of high-temperature region
Program, 50 DEG C/min of heating rate control the temperature of high-temperature region at 700 DEG C~800 DEG C;Adjust the temperature of heating tape, heating
10 DEG C/min of rate controls the temperature at low-temperature space, ensures the stabilization of two warm area temperature;
(3) specific growth opens mechanical pump and takes the air in chamber, pipeline and mixing chamber away to vacuum degree about 0.1MPa,
15min is kept, vacuum system is closed, being passed through Ar with the rate of 200sccm fills up chamber, and gas washing 15min opens temperature program,
Ar throughputs are adjusted to 100sccm;When high-temperature region, temperature reaches preset temperature, low-temperature space will also reach default temperature simultaneously
Degree.Ar throughputs are 100sccm, and heat preservation 10min stops heating after the completion of to be grown, it is cold to 200sccm acceleration to adjust Ar flows
But;It waits for that high-temperature region is cooled to 100 DEG C or less and can be taken off sample, upgrowth situation is observed with scanning electron microscope.
Invention also provides the ultra-thin molybdenum dioxide nanometer sheets of above method acquisition in micro-nano field of electronic devices
Using the application especially in preparing transistor device.
The advantages of the present invention:
The present invention has studied the growth of ultra-thin molybdenum dioxide nanometer sheet, and the growth technique based on chemical meteorology deposition method is ground
Study carefully the influence of temperature and presoma ratio for preparation, optimization has obtained the adjustable molybdenum dioxide nanometer of band gap of high quality
Piece, and the optical property of the nanometer sheet of growth is studied, find the band gap to the control and regulation nanometer sheet of growth parameter(s).
Make its being more widely applied in luminescent device and micro-nano field of electronic devices.
Compared with prior art, the present invention one is simple controllable, the material non-toxic inexpensive of preparation process;Second is that the nanometer prepared
The band gap of piece is adjustable, good conductivity, Photoluminescence are good;;Third, preparation time is short, it is suitable for industrialized production, and gained
Product has huge application value in micro-nano field of electronic devices.
Description of the drawings
Fig. 1 is molybdenum dioxide (MoO prepared by the embodiment of the present invention 12) nanometer sheet scanning electron microscope sem figure, a MoO2-1
Sample, b MoO2- 2 samples, c MoO2- 3 samples.
Fig. 2 is the scanning electron microscope sem figure of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2, a MoO2- 4 samples, b
For MoO2- 5 samples, c MoO2- 6 samples.
Fig. 3 is the scanning electron microscope sem figure of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2, a MoO2- 4 samples, b
For MoO2- 5 samples, c MoO2- 6 samples.
Fig. 4 is the atomic force microscope figure of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2, a MoO2- 4 samples
Product, b MoO2- 4 samples, c MoO2- 5 samples, d MoO2- 5 samples, e MoO2- 6 samples, f MoO2- 6 samples.
Fig. 5 is the Raman spectrogram of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2.
Fig. 6 is the energy-dispersive spectroscopy EDS figures of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2, a MoO2- 4 samples
Product, b MoO2- 4 samples, c MoO2- 5 samples, d MoO2- 5 samples, e MoO2- 6 samples, f MoO2- 6 samples.
Fig. 7 is the uv-visible absorption spectroscopy of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2, a MoO2-4
Sample, b MoO2- 5 samples, c MoO2- 6 samples.
Fig. 8 is the photoluminescence spectra of molybdenum dioxide nanometer sheet prepared by the embodiment of the present invention 2, a MoO2- 4 samples, b
For MoO2- 5 samples, c MoO2- 6 samples.
Specific implementation mode
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are only the characteristics of further illustrating the present invention and advantage, rather than to the claims in the present invention
Limitation.
Embodiment 1
Molybdenum dioxide nanometer sheet is prepared according to method provided by the invention:Molybdenum trioxide powder 5mg, sulphur powder 100mg, high temperature
Area's growth temperature (700 DEG C, 750 DEG C and 800 DEG C), 50 DEG C/min of heating rate;150 DEG C of low-temperature space growth temperature, heating rate
10℃/min;Argon gas 100sccm, soaking time 10min postcoolings take out sample after dropping to room temperature.Obtain product MoO2- 1,
MoO2- 2 and MoO2- 3 are used for subsequent analysis and characterization.
Specific preparation process is as follows:
(1) Substrate treatment, by SiO2/ Si substrate bases each ultrasound 10min under deionized water, acetone and isopropanol, goes
Except the impurity and organic matter on surface;Again in H2SO4:H2O2=3:90min is impregnated in 1 Piranha washing lotion;It is super with deionized water again
Sound 15min finally uses argon gas rifle to dry up;
(2) drug weighing and equipment debugging, molybdenum trioxide powder 5mg, sulphur powder 100mg are weighed with high Accuracy Electronic Balance,
It is put in two quartz boats, sulphur powder is put in close to the low-temperature space at air inlet, molybdenum trioxide powder is put in close to exhaust outlet respectively
High-temperature region, while SiO2/ Si substrates are positioned over the top of molybdenum trioxide powder, and polishing is face-down.Set the heating of high-temperature region
And heat preservation program, 50 DEG C/min of heating rate control the temperature (700 DEG C, 750 DEG C, 800 DEG C) of high-temperature region;Adjust heating tape
Temperature, control the temperature at low-temperature space, 150 DEG C of low-temperature space growth temperature, heating rate 10 DEG C/min ensures two warm area temperature
The stabilization of degree;
(3) specific growth opens mechanical pump and takes the air in chamber, pipeline and mixing chamber away to vacuum degree 0.1MPa, protects
15min is held, mechanical pump is closed, being passed through Ar with the rate of 200sccm fills up chamber, and gas washing 15min opens temperature program, by Ar
Throughput is adjusted to 100sccm;When high-temperature region, temperature reaches preset temperature, low-temperature space will also reach preset temperature simultaneously.Ar
Throughput is 100sccm, keeps the temperature 10min, stops heating after the completion of to be grown, adjusts Ar flows and accelerate to cool down to 200sccm;It waits for
High-temperature region is cooled to 100 DEG C or less and can be taken off sample, and upgrowth situation is observed with scanning electron microscope.The results are shown in Figure 1,
A is MoO2- 1 sample, b MoO2- 2 samples, c MoO2- 3 samples, three kinds of triangle illustrated, pentagon and diamond shape shapes
The molybdenum dioxide nanometer sheet of shape.Wherein diamond shape nanometer sheet is the appearance of the monoclinic crystal of standard, meets the crystallographic system of molybdenum dioxide.
Embodiment 2
Molybdenum dioxide nanometer sheet is prepared according to method provided by the invention:700 DEG C of high-temperature region growth temperature, heating rate 50
℃/min;150 DEG C of low-temperature space growth temperature, 10 DEG C/min of heating rate;Molybdenum trioxide powder (5mg, 10mg, 15mg),;Sulphur powder
100mg, argon gas 100sccm, soaking time 10min;Soaking time 10min postcoolings take out sample after dropping to room temperature.It is produced
Product MoO2- 4, MoO2- 5 and MoO2- 6 are used for subsequent analysis and characterization.
(1) Substrate treatment, by SiO2/ Si substrate bases each ultrasound 10min under deionized water, acetone and isopropanol, goes
Except the impurity and organic matter on surface;Again in Piranha washing lotion (H2SO4:H2O2=3:1) 90min is impregnated in;It is super with deionized water again
Sound 15min finally uses argon gas rifle to dry up;
(2) drug weighing and equipment debugging weigh sulphur powder and three oxidations with high Accuracy Electronic Balance by above-mentioned usage ratio
Molybdenum powder, molybdenum trioxide powder (5mg, 10mg, 15mg), sulphur powder 100mg are put in two quartz boats, S are put in close to air inlet respectively
Low-temperature space at mouthful, molybdenum trioxide powder are put in the high-temperature region close to exhaust outlet, while SiO2/ Si substrates are positioned over molybdenum trioxide powder
Top, polishing is face-down.High-temperature region is controlled in the heating and heat preservation program, 50 DEG C/min of heating rate for setting high-temperature region
700 DEG C of the temperature of molybdenum trioxide powder;The temperature of heating tape is adjusted, the temperature at low-temperature space, low-temperature space growth temperature 150 are controlled
DEG C, 10 DEG C/min of heating rate ensures the stabilization of two warm area temperature;
(3) specific growth opens mechanical pump and takes the air in chamber, pipeline and mixing chamber away to vacuum degree about 0.1MPa,
15min is kept, mechanical pump is closed, being passed through Ar with the rate of 200sccm fills up chamber, and gas washing 15min opens temperature program, will
Ar throughputs are adjusted to 100sccm;When high-temperature region, temperature reaches preset temperature, low-temperature space will also reach preset temperature simultaneously.
Ar throughputs are 100sccm, keep the temperature 10min, stop heating after the completion of to be grown, adjust Ar flows and accelerate to cool down to 200sccm;
It waits for that high-temperature region is cooled to 100 DEG C or less and can be taken off sample, upgrowth situation is observed with scanning electron microscope.As a result such as Fig. 2 institutes
Show, a MoO2- 4 samples, b MoO2- 5 samples, c MoO2- 6 samples illustrate to obtain three kinds of triangle, pentagon and diamond shape shapes
The molybdenum dioxide nanometer sheet of shape.Wherein diamond shape nanometer sheet is the appearance of the monoclinic crystal of standard, meets the crystallographic system of molybdenum dioxide.
Embodiment 3
By Examples 1 and 2, we prepare three kinds of triangle, pentagon and diamond shape shape dioxies under the conditions of two kinds
Change molybdenum nanometer sheet, we respectively measure its angle.As shown in figure 3, a is MoO2- 4 samples, b MoO2- 5 samples, c are
MoO2The apex angle of -6 samples, triangle, pentagon and diamond shape is all 80 °, wherein the adjacent angle of the apex angle both sides of pentagon and diamond shape
It all it is 100 °, the angle wherein at the small angle of triangle also there are one 100 ° is unobvious, wherein 80 ° and 100 ° are the two of standard
The angle of molybdenum oxide monoclinic crystal, therefore we tentatively judge that three kinds of nanometer sheet main compositions are all molybdenum dioxide, only
Reaction process and growth rate is inconsistent results in three kinds of shapes.
Embodiment 4
By product MoO2- 4, MoO2- 5 and MoO2- 6 are respectively adopted atomic force microscope (AFM), Raman spectrum and energy color
Dispersive spectrometer (EDS) detects.As shown in Figure 4, a and b is MoO2- 4 samples, c and d are MoO2- 5 samples, e and f are MoO2- 6 samples
Product, it can be seen that triangle, three kinds of shapes of pentagon and diamond shape molybdenum dioxide nanometer sheet be ultrathin nanometer piece, surface roughness
Extremely low, the height relief of whole surface is little, and thickness is each about 10nm.Triangle, pentagon and the diamond shape that we grow
The Raman spectrum of molybdenum dioxide nanometer sheet is as shown in figure 5, a is MoO2- 4 samples, b MoO2- 5 samples, c MoO2- 6 samples, three
Corresponding to the peak position offset variation very little of molybdenum dioxide in a sample in Raman peaks can almost ignore.It has also been found that other be not belonging to two
The peak position of molybdenum oxide includes the vibration peak position of Mo-S and S-S, and following we are further analyzed.Correspond in nanometer sheet
The Raman peaks strength difference of the vibration peak position of Mo-S and S-S is very big, as shown in figure 5, again to diamond shape from triangle to pentagon,
Its peak intensity weakens successively to disappearance.We are according to EDS collection of illustrative plates, as shown in fig. 6, as shown in Figure 4, a and b are MoO2- 4 samples, c
It is MoO with d2- 5 samples, e and f are MoO2- 6 samples are further verified from triangle to pentagon again to sulphur in diamond shape nanometer sheet
Constituent content gradually disappears until reducing.We judge there is sulfur doping generation when sulphur powder is excessive relative to molybdenum trioxide powder, adjoint
Molybdenum trioxide increases sulfur doping and is gradually reduced to disappearance, finally prepares pure molybdenum dioxide nanometer sheet.
Embodiment 5
Using ultrasonic method SiO2The product MoO prepared on/Si substrates2- 4, MoO2- 5 and MoO2The collection of -6 nanometer sheets is being gone
In ionized water, using ultraviolet-visible spectrophotometer to product MoO2- 4, MoO2- 5 and MoO2- 6 nanometer sheets are tested.To eliminate
The influence of solvent uses the deionized water for being not added with product to be calibrated as blank when being tested.When analyzing product test, light
Scanning range is composed from 200-800nm.Gained scanning result is as shown in fig. 7, a is MoO2- 4 samples, b MoO2- 5 samples, c are
MoO2- 6 samples.As can be seen from the figure the molybdenum dioxide nanometer sheet prepared has strong suction in the ultraviolet light range of 200-300nm
Take-up, absorptivity is more than 90% at certain wavelength.By the triangle, pentagon and diamond shape molybdenum dioxide obtained in Fig. 7 illustrations
The E of nanometer sheetgValue is about 3.75eV, 3.97eV and 4.25eV.
SiO2The product MoO of/Si substrate surfaces2- 4, MoO2- 5 and MoO2- 6 nanometer sheets are surveyed under sepectrophotofluorometer
Examination.Fig. 8 is photoluminescence spectra (PL) test result that nanometer sheet is excited using the exciter of 220nm wavelength.In order to keep away
Exempt from SiO2Influence of/Si the substrates to its luminescent properties, experiment will single cleaning SiO2/ Si substrates are tested as a contrast, it can be found that
Substrate does not have glow peak, can exclude the glow peak of substrate, i.e. transmitting of the gained glow peak entirely from product.Such as Fig. 8 institutes
Show, a MoO2- 4 samples, b MoO2- 5 samples, c MoO2- 6 samples, triangle made from chemical vapour deposition technique in this method
Shape, pentagon and diamond shape molybdenum dioxide nanometer sheet are respectively in 328.57nm (3.77eV), 312.2nm (3.97eV) and 294.3nm
There is stronger glow peak at (4.21eV), illustrates that this substance has good UV-light luminous property.Glow peak is by electronics
It is generated in conduction band and valence band-to-band transition, and the band gap of the movement of its product molybdenum dioxide nanometer sheet luminous peak position is related.
The above results show that the obtained ultra-thin molybdenum dioxide nanometer sheet of the present invention is a kind of good micro-nano electronic device
Material, especially with adjust test parameters adjust the obtained sulfur doping molybdenum dioxide nanometer sheet of band gap can be used as it is a kind of micro- well
Nanometer electronic device material is highly suitable for making high conductivity, high stability, high-power and High Density Integration electronic device.
Claims (8)
1. the preparation method of molybdenum dioxide nanometer sheet is adjusted in a kind of sulfur doping shape and band gap, which is characterized in that preparation method
Using molybdenum trioxide powder and sulphur powder as presoma, argon gas is carrier gas, the height of ratio and control growth temperature by changing presoma
It is low, using chemical vapour deposition technique in SiO2The molybdenum dioxide nanometer sheet of different shape and band gap is prepared on/Si substrates:;Wherein,
The mass ratio of sulphur powder and molybdenum trioxide powder is 20:1~20:3;Growth temperature is 700 DEG C~800 DEG C.
2. the preparation method of molybdenum dioxide nanometer sheet according to claim 1, characterized in that first to SiO2/ Si substrates into
Row processing, each ultrasound 10min, removes the impurity and organic matter on surface under deionized water, acetone and isopropanol;Again in H2SO4:
H2O2=3:90min is impregnated in 1 Piranha washing lotion;Deionized water ultrasound 15min is used again, finally argon gas rifle is used to dry up.
3. the preparation method of molybdenum dioxide nanometer sheet according to claim 1, characterized in that include the following steps:
Sulphur powder and molybdenum trioxide powder is separated, while SiO2/Si substrates being positioned over to the top of molybdenum trioxide powder, burnishing surface
Downward, sulphur powder is warming up to 150 DEG C and with the speed of 50 DEG C/min by molybdenum trioxide powder 700-800 with the speed of 10 DEG C/min
DEG C, 10min is kept the temperature, heating is stopped, high-temperature region is naturally cooling to room temperature, takes out SiO2/ Si substrates obtain product molybdenum dioxide and receive
Rice piece.
4. the preparation method of molybdenum dioxide nanometer sheet according to claim 3, characterized in that prepared by control variate method
The molybdenum dioxide nanometer sheet of different shape and different band gap, two kinds shift gears:Mode one, 700 DEG C of the high-temperature region temperature, sulphur
The quality of powder and molybdenum trioxide powder is respectively 100mg:5mg, 100mg:10mg and 100mg:15mg.Mode two, the sulphur powder with
The quality of molybdenum trioxide powder is 100mg:5mg, high-temperature region temperature are respectively 700 DEG C, 750 DEG C and 800 DEG C.
5. the preparation method of molybdenum dioxide nanometer sheet according to claim 3, characterized in that open mechanical pump vacuum degree and take out
To 0.1MPa, 15min is kept, closes mechanical pump, being passed through argon gas with the rate of 200sccm fills up chamber, and gas washing 15min is opened
Ar throughputs are adjusted to 100sccm by temperature program.
6. the preparation method of molybdenum dioxide nanometer sheet according to claim 3, characterized in that when high-temperature region, temperature reaches pre-
If when temperature, low-temperature space will also reach preset temperature simultaneously;Ar throughputs are 100sccm, 10min are kept the temperature, after the completion of to be grown
Stop heating, adjusts Ar flows and accelerate to cool down to 200sccm.
7. the ultra-thin molybdenum dioxide nanometer sheet that the preparation method according to any one of claim 1-6 obtains.
8. the ultra-thin molybdenum dioxide nanometer sheet described in claim 7 is especially being prepared in the application of micro-nano field of electronic devices
Application in transistor device.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810092998.0A CN108341431A (en) | 2018-01-31 | 2018-01-31 | A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810092998.0A CN108341431A (en) | 2018-01-31 | 2018-01-31 | A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108341431A true CN108341431A (en) | 2018-07-31 |
Family
ID=62961744
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810092998.0A Pending CN108341431A (en) | 2018-01-31 | 2018-01-31 | A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108341431A (en) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104477995A (en) * | 2014-11-26 | 2015-04-01 | 济南大学 | MoO2 nanosheets and preparation method thereof |
CN105854901A (en) * | 2016-04-21 | 2016-08-17 | 国家纳米科学中心 | Preparation method of molybdenum trioxide and molybdenum disulfide composite material |
CN106238077A (en) * | 2016-07-28 | 2016-12-21 | 中国地质大学(北京) | A kind of carbon fiber@molybdenum disulfide nano sheet core-shell structure and preparation method thereof |
CN106830082A (en) * | 2017-01-10 | 2017-06-13 | 四川大学 | A kind of method that controllable magnanimity prepares molybdenum disulfide nano band |
CN106865616A (en) * | 2017-03-30 | 2017-06-20 | 华南师范大学 | The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density |
CN107162058A (en) * | 2017-06-30 | 2017-09-15 | 华南理工大学 | A kind of molybdenum dioxide hexagonal nano-flake and preparation method thereof |
-
2018
- 2018-01-31 CN CN201810092998.0A patent/CN108341431A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104477995A (en) * | 2014-11-26 | 2015-04-01 | 济南大学 | MoO2 nanosheets and preparation method thereof |
CN105854901A (en) * | 2016-04-21 | 2016-08-17 | 国家纳米科学中心 | Preparation method of molybdenum trioxide and molybdenum disulfide composite material |
CN106238077A (en) * | 2016-07-28 | 2016-12-21 | 中国地质大学(北京) | A kind of carbon fiber@molybdenum disulfide nano sheet core-shell structure and preparation method thereof |
CN106830082A (en) * | 2017-01-10 | 2017-06-13 | 四川大学 | A kind of method that controllable magnanimity prepares molybdenum disulfide nano band |
CN106865616A (en) * | 2017-03-30 | 2017-06-20 | 华南师范大学 | The method for preparing the porous two-dimentional molybdenum disulfide nano sheet of high density |
CN107162058A (en) * | 2017-06-30 | 2017-09-15 | 华南理工大学 | A kind of molybdenum dioxide hexagonal nano-flake and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Zhang et al. | Anisotropic photoresponse of layered 2D SnS-based near infrared photodetectors | |
Wan et al. | Observation of reduced phase transition temperature in N-doped thermochromic film of monoclinic VO2 | |
Szekeres et al. | Spectroscopic ellipsometry study of CVD molybdenum oxide films: effect of temperature | |
Souissi et al. | Thickness effect on VOC sensing properties of sprayed In 2 S 3 films | |
Neimash et al. | Microstructure of thin Si–Sn composite films | |
Tark et al. | Effect of a hydrogen ratio in electrical and optical properties of hydrogenated Al-doped ZnO films | |
Ma et al. | Preparations and characterizations of polycrystalline PbSe thin films by a thermal reduction method | |
Muffler et al. | ILGAR–A novel thin-film technology for sulfides | |
Amor et al. | Effect of substrate temperature on microstructure and optical properties of hydrogenated nanocrystalline Si thin films grown by plasma enhanced chemical vapor deposition | |
Fan et al. | Structural development and dynamic process in sulfurizing precursors to prepare Cu2ZnSnS4 absorber layer | |
Haque et al. | Conversion of h-BN into c-BN for tuning optoelectronic properties | |
Mulmi et al. | Effect of annealing on optical properties of zinc oxide thin films prepared by homemade spin coater | |
Calvo-Mola et al. | Temperature dependence of Raman and photoluminescence spectra of pure and high-quality MoO3 synthesized by hot wall horizontal thermal evaporation | |
CN108341431A (en) | A kind of preparation method of sulfur doping shape and the adjustable molybdenum dioxide nanometer sheet of band gap | |
Su et al. | Effects of carbon concentration on properties of nano-diamond films | |
Dong et al. | Size dependence of optical and mechanical properties of Si 3 N 4 nanobelts controlled by flow rates | |
Benítez-Lara et al. | Silicon rich oxide powders by HWCVD: Its optical and morphological properties | |
Reidy et al. | Kinetic control for planar oxidation of MoS $ _2$ | |
Kim et al. | Cone-shaped structures of GeO2 fabricated by a thermal evaporation process | |
Ali et al. | Morphological, luminescence and structural properties of nanocrystalline silicon thin films | |
Cahyono et al. | Reduced energy bandgap of a-Si: H films deposited by PECVD at elevating temperatures | |
Wang et al. | Effect of N2 addition in Ar plasma on the development of microstructure of ultra-nanocrystalline diamond films | |
Baribeau et al. | Low-temperature Si growth on Si (001): Impurity incorporation and limiting thickness for epitaxy | |
Calta et al. | Impact of sublayer thickness and annealing on silicon nanostructures formation in a-Si: H/a-SiNx: H superlattices for photovoltaics | |
Su et al. | Synthesis and luminescent properties of ternary Si–Ge–N nanowires |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180731 |