CN108179399A - A kind of method that chemical vapour deposition technique prepares tantalum disulfide - Google Patents
A kind of method that chemical vapour deposition technique prepares tantalum disulfide Download PDFInfo
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- CN108179399A CN108179399A CN201810064973.XA CN201810064973A CN108179399A CN 108179399 A CN108179399 A CN 108179399A CN 201810064973 A CN201810064973 A CN 201810064973A CN 108179399 A CN108179399 A CN 108179399A
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
The invention discloses a kind of method that chemical vapour deposition technique prepares tantalum disulfide, including：The business goldleaf of purchase is subjected to cleaning and high temperature pre-anneal treatment；It is put into cleaning in high temperature process furnances with the goldleaf after preannealing, carries out the growth of tantalum disulfide nanometer sheet using the method for aumospheric pressure cvd, the method for utilizing low-pressure chemical vapor deposition carries out the growth of the uniform thin layer tantalum disulfide film of cm size.After growth, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen, you can obtains the different-thickness tantalum disulfide nanometer sheet and thin layer tantalum disulfide film sample on goldleaf.The use of chemical vapor deposition method can realize the batch controllable preparation of the adjustable tantalum disulfide sample of large area, high quality, thickness；It can realize the exploration of its microscopic appearance and electronic structure；The tantalum disulfide sample of different-thickness/coverage can be prepared by regulating and controlling growth time.
Description
Technical field
The invention belongs to Material Field, in particular it relates to using the growing method of aumospheric pressure cvd,
The adjustable metallicity tantalum disulfide nanometer sheet of controllable preparation thickness on goldleaf substrate；Utilize the growth side of low-pressure chemical vapor deposition
Method, the uniform large area thin layer tantalum disulfide film of controllable preparation cm size on goldleaf substrate.
Background technology
Using graphene and molybdenum disulfide as the rise of the two-dimensional layer nano material of representative so that other New Two Dimensional atoms
Crystalline material has gradually come into the visual field of people.Two-dimensional gold attribute transient metal sulfide has charge density wave phase transition, surpasses
The novel physical characteristic such as orderly, iron/anti-ferromagnetism is led, and then has greatly pushed the spy of condensed state physics basic problem
Rope.Metallic transition metals sulfide is other than having the physical characteristic of above-mentioned novelty, in electronics device and energy field
Also there is the application prospect of very abundant.It is well known that realize the high effect of semiconductive transient metal sulfide electronics device
One maximum bottleneck is exactly the high contact resistance between the material and metal electrode, and work content between the two mismatches
It causes between interface there are great Schottky barrier, so as to hinder carrying for semiconductive transient metal sulfide mobility
It rises.There is quite similar lattice structure in view of metallic transition metals sulfide and semiconductive transient metal sulfide,
The two is integrated with may construct full transient metal sulfide field-effect transistor (metallic alloy as contact electrode, partly lead
Body material is as conducting channel).Metallic transition metals sulfide is in addition to being used as connecing for semiconductive transient metal sulfide
Other than touched electrode, itself or a kind of very excellent energy and material.It is analysed in ultracapacitor, lithium ion battery and electro-catalysis
The fields such as hydrogen reaction have very extensive application prospect.
The precondition for realizing above-mentioned physical property research and explorative research is to prepare the controllable metallicity of high quality, thickness
Transient metal sulfide.It should be pointed out that tantalum disulfide is in recent years by a kind of metallic transition metals sulphur of extensive concern
Compound has the charge density wave phase transition and superconducting characteristic of very abundant, is for studying charge density wave phase transition and surpassing
Lead the ideal material system of state relationship.At present it has been reported that tantalum disulfide material be mainly by mechanically pulling off and molecular beam epitaxy
Method obtain.The tantalum disulfide material thickness of mechanical stripping preparation strategy acquisition is uncontrollable, farmland area size is small, preparation efficiency
It is low, it can not realize scale application.It is simultaneously a kind of sub- associated material system of forceful electric power in view of tantalum disulfide, between layers
Interaction force is stronger, and mechanical stripping method is difficult to obtain the sample of thin layer.The growth strategy of molecular beam epitaxy is introduced into two
In the preparation for vulcanizing tantalum, although realizing the accurate control of tantalum disulfide thickness, and the tantalum disulfide sample of individual layer/few layer is obtained
Product, but this preparation method operation exception is complicated, manufacturing cost is higher, the tantalum disulfide sample obtained can only carry out substantially
Physical property research, can not realize industrial applications.Therefore, both the above preparation method seriously hinders two-dimensional gold attribute two
The novel physical characteristic exploration for vulcanizing tantalum and the practical application in electronics device/energy field.
Invention content
It is controllable using the growing method of aumospheric pressure cvd the object of the present invention is to provide one kind on goldleaf substrate
Prepare the adjustable metallicity tantalum disulfide nanometer sheet of thickness；Utilize the method controllable preparation cm size of low-pressure chemical vapor deposition
Uniform thin layer tantalum disulfide film.It should be pointed out that the adjustable tantalum disulfide nanometer sheet of thickness can be used to study thickness dependence
Charge density wave phase transition and the novel physical characteristic such as superconducting state.The preparation of thin layer tantalum disulfide film provides a research
Under two-dimensional confinement between charge density wave phase transition and superconducting state relationship platform.What is more important, prepared curing
Tantalum shows superpower electrocatalytic hydrogen evolution activity, comparable with the catalytic performance of common noble metal platinum.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
A kind of method that chemical vapour deposition technique prepares tantalum disulfide, the described method comprises the following steps：
1) goldleaf substrate is subjected to cleaning and high temperature pre-anneal treatment；
2) by treated, goldleaf substrate is placed in the high temperature process furnances of three-temperature-zone, according to the suitable of gas routing upstream to downstream
Sequence is sequentially placed sulphur powder, tantalic chloride and goldleaf substrate；
3) argon gas and hydrogen are passed through into the reaction chamber of high temperature process furnances, reaction chamber is cleaned；
4) increase respectively sulphur powder, tantalic chloride and goldleaf substrate temperature to 280~300 DEG C, 300~350 DEG C and 700~
750 DEG C, carry out the growth of tantalum disulfide；
5) after tantalum disulfide growth, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen, you can obtains goldleaf substrate
On tantalum disulfide sample.
Further, in step 3), vacuum degree in reaction chamber is first evacuated to 1Pa hereinafter, again to the anti-of high temperature process furnances
Intracavitary is answered to be passed through argon gas and hydrogen, reaction chamber is cleaned.
Preferably, the size of the goldleaf substrate is 1 centimetre of 1 cm x, and thickness is 25 microns.
Preferably, in the step 1), goldleaf substrate is sequentially placed into sodium hydroxide solution and deionized water and is carried out clearly
It washes, is then cleaned by ultrasonic in acetone, dried up with nitrogen, complete the cleaning of goldleaf substrate.
Preferably, in the step 2), the quality of sulphur powder and tantalic chloride is respectively 100~120mg and 3~5mg；Pentachloro-
It is respectively 5~7cm and 3~4cm to change tantalum with the distance between goldleaf and sulphur powder.
Preferably, in the step 3), the flow of argon gas and hydrogen is respectively 100~150sccm and 10~15sccm.
Preferably, in the step 4), growth time is 5 to 30 minutes.
More specifically：
First, aumospheric pressure cvd prepares the adjustable tantalum disulfide nanometer sheet of thickness on goldleaf substrate, the method includes
Following steps：
1. the business goldleaf of purchase is cleaned by ultrasonic, then the goldleaf substrate after cleaning is carried out at high temperature preannealing
Reason, Pre-annealing Temperature are set as 1000 DEG C, and annealing time is 3 hours；
2. the goldleaf after annealing is placed in the high temperature process furnances of three-temperature-zone, according to the sequence of gas routing upstream to downstream, according to
Secondary placement sulphur powder, tantalic chloride and goldleaf；
3. being passed through argon gas and hydrogen into reaction chamber, reaction chamber is cleaned, discharges air remaining in cavity, cleaning
Time is 30 minutes；
4. the temperature for setting sulphur powder, tantalic chloride and goldleaf respectively is 280 DEG C, 300 DEG C and 700 DEG C, two sulphur are then carried out
Change the growth of tantalum, growth time 5 to 30 minutes is adjustable；
After 5. tantalum disulfide is grown, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen, you can obtains on goldleaf
Tantalum disulfide sample.
In the present invention, the size of the goldleaf is 1 centimetre of 1 cm x, and thickness is 25 microns.
In the step 1, goldleaf is sequentially placed into sodium hydroxide (0.5mol/l) solution and deionized water and is cleaned,
Then it is cleaned by ultrasonic 10 minutes in acetone, is dried up with nitrogen, completes the cleaning of goldleaf substrate.
In the step 2, the quality of sulphur powder and tantalic chloride is respectively 100mg and 3mg.Tantalic chloride and goldleaf and sulphur powder
The distance between be respectively 5cm and 3cm.
In the step 3, the flow of argon gas and hydrogen is respectively 100sccm and 10sccm.
In the step 4, growth time is respectively 5,10,20 and 30 minutes.
The advantage of the invention is that：1) use of aumospheric pressure cvd method can realize large area, high quality two
Vulcanize the batch controllable preparation of tantalum sample；2) it is micro- that the tantalum disulfide sample prepared on goldleaf can directly be scanned tunnel
Mirror/micro- stave sign, and then can realize the exploration of its microscopic appearance and electronic structure；3) it can be made by regulating and controlling growth time
The tantalum disulfide sample of standby different-thickness.
2nd, low-pressure chemical vapor deposition prepares the uniform thin layer tantalum disulfide film of cm size on goldleaf substrate, described
Method includes the following steps：
1. the business goldleaf of purchase is cleaned by ultrasonic, high temperature pre-anneal treatment then is carried out to the goldleaf after cleaning,
Pre-annealing Temperature is set as 1000 DEG C, and annealing time is 3 hours；
2. the goldleaf after annealing is placed in the high temperature process furnances of three-temperature-zone, according to the sequence of gas routing upstream to downstream, according to
Secondary placement sulphur powder, tantalic chloride and goldleaf；
3. vacuum degree in reaction chamber is evacuated to 1Pa hereinafter, the air in reaction chamber is drained using vacuum pump；
4. being passed through argon gas and hydrogen into reaction chamber, the temperature for setting sulphur powder, tantalic chloride and goldleaf respectively is 280 DEG C,
300 DEG C and 700 DEG C, the growth of tantalum disulfide is then carried out, growth time 5 to 20 minutes is adjustable；
After 5. tantalum disulfide is grown, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen, you can obtains on goldleaf
Thin layer tantalum disulfide sample.
In the present invention, the size of the goldleaf is 1 centimetre of 1 cm x, and thickness is 25 microns.
In the step 1, goldleaf is sequentially placed into sodium hydroxide (0.5mol/l) solution and deionized water and is cleaned,
Then it is cleaned by ultrasonic 10 minutes in acetone, is dried up with nitrogen, completes the cleaning of goldleaf substrate.
In the step 2, the quality of sulphur powder and tantalic chloride is respectively 100mg and 3mg.Tantalic chloride and goldleaf and sulphur powder
The distance between be respectively 5cm and 3cm.
In the step 4, the flow of argon gas and hydrogen is respectively 100sccm and 10sccm.
In the step 4, growth time is respectively 5,10 and 20 minutes.
The advantage of the invention is that：1) use of low-pressure chemical vapor deposition method reduces the feed speed of predecessor,
And then it can realize the controllable preparation of thin layer tantalum disulfide sample on goldleaf；2) tantalum disulfide prepared on goldleaf can directly into
Row scanning tunneling microscope/micro- stave sign, and then can realize the exploration of its microscopic appearance and electronic structure；3) pass through regulation and control
Growth time can prepare the thin layer tantalum disulfide sample of different coverages and tantalum disulfide film.
Description of the drawings
Fig. 1 be embodiment 1 corresponding to aumospheric pressure cvd prepare different-thickness tantalum disulfide nanometer sheet pattern,
Element, lattice structure and thickness result；
Low-pressure chemical vapor depositions of the Fig. 2 corresponding to embodiment 2 prepares the pattern, element, lattice of thin layer tantalum disulfide
Structure and thickness result；
Fig. 3 is the atomic structure of corresponding tantalum disulfide nanometer sheet/film in embodiment 1 and embodiment 2；
Fig. 4 is application of the tantalum disulfide nanometer sheet corresponding to embodiment 1 in electrocatalytic hydrogen evolution reaction.
Specific embodiment
With the drawings and specific embodiments, the present invention is described in further detail below.
Embodiment 1
The business goldleaf (area is 1 centimetre of 1 cm x) of purchase is sequentially placed in sodium hydroxide (0.5mol/l) solution
It is cleaned with carrying out 5 minutes in deionized water, is then cleaned by ultrasonic 10 minutes in acetone, is dried up with nitrogen.By the gold after cleaning
Foil, which is put into 1000 DEG C of high-temperature annealing furnace, carries out pre-anneal treatment, and annealing time is 3 hours.Long-time high temperature pre-anneal treatment
Be conducive to reconstructing again for goldleaf surface, and then obtain bigger crystal face size.Goldleaf substrate after annealing is placed in high temperature process furnances
In, according to the sequence of gas routing upstream to downstream, it is sequentially placed into sulphur powder, tantalic chloride and goldleaf.The matter of sulphur powder and tantalic chloride
Amount is respectively 100mg and 3mg.The distance of tantalic chloride and sulphur powder is 3cm, and the distance between tantalic chloride and goldleaf are ranging from
5cm.Then to argon gas (100sccm) and hydrogen (10sccm) is passed through in reaction chamber, reaction chamber is cleaned, is discharged in cavity
Remaining air, scavenging period are 30 minutes.The temperature of sulphur powder, tantalic chloride and goldleaf is then increased respectively to 280 DEG C, 300
DEG C and 700 DEG C.The reactivity species of tantalum disulfide are transported to gold by argon gas (100sccm) and hydrogen (10sccm) as carrier gas
The growth of tantalum disulfide is realized on foil substrate, the growth time 5 to 30 minutes of tantalum disulfide is adjustable, can be obtained under different growth times
Obtain different-thickness and the tantalum disulfide sample of farmland area size.After growth, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen
Gas opens a position and takes out sample.
Gained tantalum disulfide sample is scanned electron microscope, x-ray photoelectron spectroscopy, X ray single crystal diffraction and original
Sub- force microscope test, as a result as shown in Fig. 1 a, Fig. 1 b, Fig. 1 c and Fig. 1 d.By scanning electron microscope data can be seen that with
The increase of growth time, the farmland area size of tantalum disulfide sample constantly increases, this shows to obtain by regulating and controlling growth time
The tantalum disulfide sample of different farmland areas size, as shown in Figure 1a.X-ray photoelectron spectroscopy characterization display combine can 22.7eV and
24.7eV corresponds to Ta respectively4+4f7/2And 4f5/2, and combine energy 162.1eV and 163.2eV and then correspond to S respectively2-2p3/2With
2p1/2, as shown in Figure 1 b.In addition, the element ratio that Ta and S can be also obtained using x-ray photoelectron spectroscopy is 1:2.08 and then
It demonstrates goldleaf surface and forms tantalum disulfide, and the tantalum disulfide obtained is highly stable, does not aoxidize.Further
X ray single crystal diffraction characterization find that all characteristic peaks of tantalum disulfide correspond to hexagonal lattice structure well, utilization
Rietica softwares can obtain its lattice constantSo as to prove to utilize atmospheric pressure
It is 2H phase structures to learn the tantalum disulfide that the growing method being vapor-deposited is prepared on goldleaf, as illustrated in figure 1 c.Atomic force microscope
Characterize data is shown, with the increase of growth time, the thickness of tantalum disulfide constantly increases, as shown in Figure 1 d.This illustrates normal pressure
Chemical vapor deposition growth tantalum disulfide follows the pattern of Volmer-Weber (VW).
Embodiment 2
The business goldleaf (area is 1 centimetre of 1 cm x) of purchase is sequentially placed in sodium hydroxide (0.5mol/l) solution
It is cleaned with carrying out 5 minutes in deionized water, is then cleaned by ultrasonic 10 minutes in acetone, is dried up with nitrogen.By the gold after cleaning
Foil, which is put into 1000 DEG C of high-temperature annealing furnace, carries out pre-anneal treatment, and annealing time is 3 hours.Long-time high temperature preannealing is advantageous
In reconstructing again for goldleaf surface, and then obtain bigger crystal face size.Goldleaf substrate after annealing is placed in high temperature process furnances, is pressed
According to the sequence of gas routing upstream to downstream, it is sequentially placed into sulphur powder, tantalic chloride and goldleaf.Sulphur powder and the quality of tantalic chloride difference
For 100mg and 3mg.The distance of tantalic chloride and sulphur powder is 3cm, the distance between tantalic chloride and goldleaf ranging from 5cm.It opens
Vacuum degree in reaction chamber is evacuated to 1Pa hereinafter, discharging air remaining in cavity by vacuum pump.Then to being passed through argon in reaction chamber
Gas (100sccm) and hydrogen (10sccm), while the temperature of sulphur powder, tantalic chloride and goldleaf is increased respectively to 280 DEG C, 300 DEG C
With 700 DEG C.The reactivity species of tantalum disulfide are transported to goldleaf by argon gas (100sccm) and hydrogen (10sccm) as carrier gas
The growth of tantalum disulfide is realized on substrate, the growth time 5 to 20 minutes of tantalum disulfide is adjustable, can be obtained under different growth times
The thin layer tantalum disulfide sample of different coverages.After growth, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen, opens a position
Take out sample.
Gained tantalum disulfide sample is scanned electron microscope, x-ray photoelectron spectroscopy, X ray single crystal diffraction, atom
Force microscope and light microscope test, as a result as shown in Fig. 2 a, Fig. 2 b, Fig. 2 c, Fig. 2 d and Fig. 2 e.By scanning electron microscope
Data can be seen that the increase with growth time, and the farmland area size of tantalum disulfide sample constantly increases, and can finally obtain full layer
Tantalum disulfide film, this shows that by regulating and controlling growth time the tantalum disulfide sample of different farmland areas size can be obtained, such as Fig. 2 a institutes
Show.X-ray photoelectron spectroscopy characterization display combines energy 22.7eV and 24.7eV and corresponds to Ta respectively4+4f7/2And 4f5/2, and combine
Energy 162.1eV and 163.2eV then corresponds to S respectively2-2p3/2And 2p1/2, as shown in Figure 2 b.Also may be used using x-ray photoelectron spectroscopy
The element ratio for obtaining Ta and S is 1:2.08, and then demonstrate goldleaf surface and form tantalum disulfide, and two sulphur obtained
It is highly stable to change tantalum, does not aoxidize.Further X-ray diffraction characterization finds that all characteristic peaks of tantalum disulfide are very
Good correspondence hexagonal lattice structure, can obtain its lattice constant using Rietica softwares is respectively So as to which the tantalum disulfide that the growing method proved using low-pressure chemical vapor deposition is prepared on goldleaf is that 2H phases are tied
Structure, as shown in Figure 2 c.AFM data is shown, with the increase of growth time, the thickness of tantalum disulfide does not occur
Change, as shown in Figure 2 d, this shows in low-pressure chemical vapor deposition growth course, and tantalum disulfide follows Frank-van der
Merwe (FM) growth pattern.Light microscope characterization shows under cm size that tantalum disulfide film thickness is uniform, such as Fig. 2 e institutes
Show.
Embodiment 3
The different-thickness tantalum disulfide nanometer sheet prepared on goldleaf is transferred to progress transmission electron microscope table on copper mesh
Sign.Transfer process is as follows：(macromolecule membrane is thick for tantalum disulfide/goldleaf surface spin coating polymethyl methacrylate macromolecule membrane
Spend for 500nm), and heated at 180 DEG C and dry (time is 10 minutes), it is subsequently placed into (etchant composition in goldleaf etching agent
Respectively potassium iodide, iodine and water, mass ratio 1：4：40) etching of goldleaf substrate, is carried out, etch period is 3 hours, Ran Houyong
Copper mesh pulls polymethyl methacrylate macromolecule membrane/tantalum disulfide sample out, and is dried at 100 DEG C 10 minutes so that
Sample comes into full contact with copper mesh.Finally polymethyl methacrylate macromolecule membrane/tantalum disulfide/copper mesh is put into acetone and removed
Remove polymethyl methacrylate macromolecule membrane (time is 30 minutes), you can obtain tantalum disulfide/copper mesh specimen.Transmitted electron
Accelerating potential used is 200kV during microscopic characterization.
Obtained sample carries out transmission electron microscope and selected diffraction characterization, as a result as Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d,
Fig. 3 e, Fig. 3 f, shown in Fig. 3 g and Fig. 3 h.Low amplification factor transmission electron microscope characterize data shows that low pressure chemical phase sinks
Tantalum disulfide sample layer thickness prepared by product is highly uniform (Fig. 3 a), is further found to being amplified characterization at film tuck, low
Tantalum disulfide thickness prepared by pressure chemical vapor deposition is 4 layers (Fig. 3 b).It chooses electronic diffraction characterization and only shows a set of six
The diffraction spot of weight symmetry, tantalum disulfide film prepared by this explanation have higher crystalline quality.In addition, the selection electronics spreads out
It penetrates and presents only the corresponding Bragg diffraction of Ta atoms, do not observe what charge density wave superlattices reflected between emptying
Diffraction spot, it was demonstrated that the charge density wave phase of the tantalum disulfide of 4 thickness receives apparent inhibition, as shown in Figure 3c.Then
More deep Atomic Resolution transmission electron microscope characterization result shows that tantalum disulfide film has gem-pure cellular
Lattice structure, lattice constant 0.33nm is consistent with lattice constant in the face of body phase tantalum disulfide, illustrates low pressure chemical phase
Tantalum disulfide prepared by deposition has very high crystal quality, as shown in Figure 3d.Then to aumospheric pressure cvd prepare compared with
Thick tantalum disulfide nanometer sheet carries out the transmission electron microscope characterization of system, as shown in Figure 3 e, sharp keen triangle farmland area side
Boundary shows that the sample has higher crystal quality and single crystal characteristics.It chooses electronic diffraction characterization to find, the tantalum disulfide farmland area
Only a set of symmetrical Bragg diffraction spot of sixfold (yellow circle marks in Fig. 3 f), it was confirmed that the tantalum disulfide triangle nanometer
Piece is single crystal domains area.In addition, other than Bragg diffraction spot, extremely complex satellite is presented around the diffraction spot of center
Diffraction spot (Blue circles mark in Fig. 3 f), illustrates there is non-commensurability charge density wave phase in thicker tantalum disulfide sample.
Further Atomic Resolution transmission electron microscope characterization finds that the tantalum disulfide nanometer sheet has the honeycomb crystal lattice of high quality
Structure (Fig. 3 g).And in Fourier transformation image other than Bragg diffraction spot, also present and obviously defend
Star diffraction spot.Inversefouriertransform filtering is carried out to the satellite diffraction spot, finds corresponding Atomic Resolution transmission electron microscope
Occur unordered superstructure in figure, as illustrated in figure 3h, again demonstrate the two thicker sulphur of aumospheric pressure cvd preparation
Changing tantalum sample has obviously non-commensurability charge density wave phase.
Embodiment 4
Prepared tantalum disulfide/goldleaf directly carries out electro-chemical test as working electrode using in embodiment 1.It is all
Electro-chemical test be to be carried out on the three-electrode system of electrochemical workstation (CHI660D).Made with tantalum disulfide/goldleaf
For working electrode, platinum foil is used as to electrode, and saturation calomel is used as with reference to electrode, and electrolyte is the dilution heat of sulfuric acid of 0.5mol/l.
All potentials are calibrated to reversible hydrogen electrode (RHE).It is tested using linear sweep voltammetry, sweep speed 5mV/s, such as
Shown in Fig. 4 a.When cathode-current density is 10mA/cm2When, the overpotential of tantalum disulfide only has 65~150mV, far below tradition
The respective value of semiconductor phase transient metal sulfide, this shows that tantalum disulfide can be realized electricity under lower extra electric field and urge
Change evolving hydrogen reaction.Tafel curve in Fig. 4 b has obtained the Ta Feier of tantalum disulfide nanometer sheet by further linear fit
Slope be 33~42mV/dec, the numerical value will be far below it has been reported that conventional semiconductors phase transient metal sulfide numerical value,
Show that tantalum disulfide has faster electrocatalytic hydrogen evolution reaction speed.It should be noted that the Tafel slope of tantalum disulfide with
The Tafel slope of noble metal platinum is very close, this shows that the reaction of tantalum disulfide electrocatalytic hydrogen evolution follows Volmer-Tafel machines
System.In addition, the method extrapolated using Tafel curve, the exchange current density that tantalum disulfide nanometer sheet has been calculated is 100
~179.47 μ A/cm2, this be it has been reported that transient metal sulfide material in highest numerical value, reconfirmed curing
The efficient electrocatalytic hydrogen evolution response characteristic of tantalum, as illustrated in fig. 4 c.
It should be noted last that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted.Although ginseng
The present invention is described in detail according to embodiment, it will be apparent to an ordinarily skilled person in the art that the technical side to the present invention
Case is modified or replaced equivalently, and without departure from the spirit and scope of technical solution of the present invention, should all be covered in the present invention
Right in.
Claims (7)
1. a kind of method that chemical vapour deposition technique prepares tantalum disulfide, the described method comprises the following steps：
1) goldleaf substrate is subjected to cleaning and high temperature pre-anneal treatment；
2) will treated that goldleaf substrate is placed in the high temperature process furnances of three-temperature-zone, according to the sequence of gas routing upstream to downstream, according to
Secondary placement sulphur powder, tantalic chloride and goldleaf substrate；
3) argon gas and hydrogen are passed through into the reaction chamber of high temperature process furnances, reaction chamber is cleaned；
4) sulphur powder, tantalic chloride and goldleaf substrate temperature are increased respectively to 280~300 DEG C, 300~350 DEG C and 700~750
DEG C, carry out the growth of tantalum disulfide；
5) after tantalum disulfide growth, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen, you can obtains on goldleaf substrate
Tantalum disulfide sample.
2. the method that chemical vapour deposition technique according to claim 1 prepares tantalum disulfide, which is characterized in that in step 3)
In, vacuum degree in reaction chamber is first evacuated to 1Pa hereinafter, argon gas and hydrogen are passed through into the reaction chamber of high temperature process furnances again, to anti-
Chamber is answered to be cleaned.
3. the method that chemical vapour deposition technique according to claim 1 or 2 prepares tantalum disulfide, which is characterized in that described
The size of goldleaf substrate is 1 centimetre of 1 cm x, and thickness is 25 microns.
4. the method that chemical vapour deposition technique according to claim 1 or 2 prepares tantalum disulfide, which is characterized in that described
In step 1), goldleaf substrate is sequentially placed into sodium hydroxide solution and deionized water and is cleaned, it is then ultrasonic in acetone
Cleaning, is dried up with nitrogen, completes the cleaning of goldleaf substrate.
5. the method that chemical vapour deposition technique according to claim 1 or 2 prepares tantalum disulfide, which is characterized in that described
In step 2), the quality of sulphur powder and tantalic chloride is respectively 100~120mg and 3~5mg；Tantalic chloride and goldleaf and sulphur powder it
Between distance be respectively 5~7cm and 3~4cm.
6. the method that chemical vapour deposition technique according to claim 1 or 2 prepares tantalum disulfide, which is characterized in that described
In step 3), the flow of argon gas and hydrogen is respectively 100~150sccm and 10~15sccm.
7. the method that chemical vapour deposition technique according to claim 1 or 2 prepares tantalum disulfide, which is characterized in that described
In step 4), growth time is 5 to 30 minutes.
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| CN108970624A (en) * | 2018-08-10 | 2018-12-11 | 清华-伯克利深圳学院筹备办公室 | A kind of carbon/tantalum disulfide heterojunction material and its preparation method and application |
| CN109371469A (en) * | 2018-12-18 | 2019-02-22 | 南方科技大学 | A kind of monocrystal material, and its preparation method and application |
| CN109999848A (en) * | 2019-04-23 | 2019-07-12 | 福州大学 | III-VI race's catalysis material of Ca orthorhombic phase is mixed in a kind of preparation of chemical vapour deposition technique |
| CN112442674A (en) * | 2019-09-03 | 2021-03-05 | Asm Ip私人控股有限公司 | Method and apparatus for depositing chalcogenide films and structures including films |
| CN113122819A (en) * | 2021-04-09 | 2021-07-16 | 安徽大学 | Preparation method of tantalum-doped large-area two-dimensional niobium disulfide material |
| CN113215551A (en) * | 2021-04-01 | 2021-08-06 | 浙江工业大学 | Method for preparing TaC |
| CN113725360A (en) * | 2021-09-02 | 2021-11-30 | 中国人民解放军国防科技大学 | Thermal field transistor based on tantalum disulfide charge density wave phase change and preparation method thereof |
| CN114318297A (en) * | 2021-12-09 | 2022-04-12 | 天津理工大学 | Method for preparing tantalum disulfide by atmospheric pressure chemical vapor deposition |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108970624A (en) * | 2018-08-10 | 2018-12-11 | 清华-伯克利深圳学院筹备办公室 | A kind of carbon/tantalum disulfide heterojunction material and its preparation method and application |
| CN108970624B (en) * | 2018-08-10 | 2021-07-30 | 清华-伯克利深圳学院筹备办公室 | Carbon/tantalum disulfide heterojunction material and preparation method and application thereof |
| CN109371469A (en) * | 2018-12-18 | 2019-02-22 | 南方科技大学 | A kind of monocrystal material, and its preparation method and application |
| CN109999848A (en) * | 2019-04-23 | 2019-07-12 | 福州大学 | III-VI race's catalysis material of Ca orthorhombic phase is mixed in a kind of preparation of chemical vapour deposition technique |
| CN112442674A (en) * | 2019-09-03 | 2021-03-05 | Asm Ip私人控股有限公司 | Method and apparatus for depositing chalcogenide films and structures including films |
| CN113215551A (en) * | 2021-04-01 | 2021-08-06 | 浙江工业大学 | Method for preparing TaC |
| CN113215551B (en) * | 2021-04-01 | 2023-05-23 | 浙江工业大学 | Method for preparing TaC |
| CN113122819A (en) * | 2021-04-09 | 2021-07-16 | 安徽大学 | Preparation method of tantalum-doped large-area two-dimensional niobium disulfide material |
| CN113725360A (en) * | 2021-09-02 | 2021-11-30 | 中国人民解放军国防科技大学 | Thermal field transistor based on tantalum disulfide charge density wave phase change and preparation method thereof |
| CN114318297A (en) * | 2021-12-09 | 2022-04-12 | 天津理工大学 | Method for preparing tantalum disulfide by atmospheric pressure chemical vapor deposition |
| CN114318297B (en) * | 2021-12-09 | 2024-03-26 | 天津理工大学 | Method for preparing tantalum disulfide by normal pressure chemical vapor deposition |
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Application publication date: 20180619 |