CN110095505A - A kind of method of Transition-metal dichalcogenide energy gap regulation - Google Patents
A kind of method of Transition-metal dichalcogenide energy gap regulation Download PDFInfo
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Abstract
A kind of method of Transition-metal dichalcogenide energy gap adjustment, the generation device of its pressure is diamond anvil cell, by integrating vanderburg electrode on diamond anvil, in situ under the effect of measurement pressure, according to change in resistance rule, detect Transition-metal dichalcogenide energy gap regulating effect, pressure stepping accuracy is high, it is continuously adjustable for the compression of Transition-metal dichalcogenide energy gap, sample resistivity is measured using vanderburg method, and relationship is varied with temperature according to resistivity data and resistivity and judges Transition-metal dichalcogenide energy gap closure situation, it is applicable not only to single crystal samples and also effective to polycrystal powder sample, the scope of application is wider, strong operability, effect is good.
Description
Technical field
The present invention relates to high-pressure physics technologies and semiconducting electonic structure field, more particularly to a kind of transition metal sulfur family
The method of compound energy gap adjustment.
Background technique
Transition-metal dichalcogenide is the inorganic semiconductor material of a quasi-tradition, and chemical general formula often uses MX2It indicates, M
=Mo, W etc., X=S, Se, Te.TMDs has typical layer structure, and each layer is all the form of sandwich X-M-X, i.e. transition
Metal is in centre, and up and down respectively by the atom of covalently key connection chalcogen, the layer of sandwich structure relies on Van der Waals
Power is stacked with the lattice structure of shape bodies.
Transition-metal dichalcogenide has semiconductor properties, and the increase of pressure makes its structure cell become smaller, Brillouin zone also by
Compression, energy gap narrow, and the electronics in valence band is easier to transit to conduction band participation conduction, and macroscopically energy gap, which narrows, shows as sample electricity
Resistance rate reduces.Temperature, which increases, can make the impurity energy level in energy level or energy gap in valence band enter conduction band participation conduction, so half
The resistivity of conductor is reduced with the raising of temperature.Its band structure is similar to metal after energy gap closure, and the raising of temperature can make
Atomic kernel vibrates aggravation near its equilbrium position, and the collision opportunity between free electron and atomic kernel is bigger, also more hinders
Hinder the directed movement of electronics, therefore after energy gap closure, the resistivity of material is increased with the raising of temperature.
2004, graceful Geim group, Chester university was successfully separated out graphite material-graphene of monoatomic layer
(graphene), two-dimensional material is proposed, transition metal as graphite material-graphene of monoatomic layer is successfully separated
Chalcogenide the means such as is easy to be by mechanically pulling off and obtains valuable two-dimensional material.Two-dimensional material graphene possesses superior
Electronic transmission performance, optical characteristics, thermal characteristic have very huge potentiality in energy field, but essentially
It is semimetal, there is no energy gap in band structure, this practical application to graphene in electronic field and photoelectric field is brought
Very big obstacle.
Transition-metal dichalcogenide is semiconductor properties, has biggish energy gap, also has both the superiority of two-dimensional material
Can, it can be competent at the purposes in terms of electronics and photoelectricity.In certain application scenarios, the energy gap of Transition-metal dichalcogenide is needed
Width is adjustable, and the constituent material of photovoltaic device is Transition-metal dichalcogenide, and the model of spectrum can be absorbed in the variation of energy gap
It encloses and extends to designated band, improve photoelectric conversion efficiency.
The electronic structure tuning of Transition-metal dichalcogenide is mainly the following mode:
1, extra electric field disturbance electron spin, change electronic degree of freedom；
2, the sample number of plies is reduced, keeps the quantum effect of two-dimensional material significant, quantum confinement is carried out to electronic structure；
3, by bending to material, stretch or introduce the modes such as substrate stress is applied to lattice, to change electronics knot
Structure.
The specific conditions such as electric field, stress are required when tuning energy gap using these means, generate the device of these conditions very
Harshness, this usage mode that will lead to them are restricted very much, and current technology means are extremely difficult to the manipulation of single layer atom, only
Stress could be generated to influence electronic structure on the bending of monocrystal thin films sample or stretching, and many application examples require sample
Form is polycrystal powder.
Summary of the invention
The present invention aiming at the problems existing in the prior art, according to Transition-metal dichalcogenide after by pressure resistivity become
Law, situ high pressure conduct the detection method of activation energy, and creativeness proposes a kind of Transition-metal dichalcogenide energy gap tune
Whole method can make Transition-metal dichalcogenide energy gap all continuously adjustable to closed state, be suitable for powder Polycrystalline.
The technical scheme adopted by the invention is that: a kind of method of Transition-metal dichalcogenide energy gap adjustment, feature
Be, it the following steps are included:
(1) start diamond anvil, impression is generated on gasket, through-hole is set at impression center, it will be on gasket
Through-hole is as pressure chamber；
(2) diamond anvil cell is subjected to chemical cleaning, removes the grease and dust on its surface；
(3) on upper diamond anvil cell anvil face, in the way of radio-frequency sputtering, the metal molybdenum film of 0.3 micron of deposition
As conductive layer；
(4) the metal molybdenum film on upper diamond anvil cell anvil face is processed into using the method for photoetching and chemical attack
The figure of vanderburg electrode, the position of electrode arrangements are determined by accurate litho machine console completely；
(5) 1.5 microns -2.5 microns of aluminum oxide film is deposited to diamond pair using the method for radio-frequency sputtering
In the molybdenum electrode for pushing up anvil anvil face, as insulating layer；
(6) on the insulating layer, expose electrode detector window with photoetching and chemical corrosion method；
(7) diamond anvil is assembled, the gasket with through-hole is arranged on lower diamond anvil cell anvil face, in pressure bottom of chamber
Ruby is placed in portion, Transition-metal dichalcogenide powder Polycrystalline is then filled up pressure chamber, by the upper gold of integrated microelectrode
Hard rock opposed anvils are assembled on press；
(8) Transition-metal dichalcogenide powder Polycrystalline resistivity is measured using vanderburg method, firstly, in upper Buddha's warrior attendant
Exciting current I is given at stone opposed anvils microelectrode first end 1,2 both ends of microelectrode second end12, at microelectrode third end 3, microelectrode
Voltage U is surveyed at four ends, 4 both ends34, obtain resistance R1=U34/I12；Then it is given at microelectrode second end 2,3 both ends of microelectrode third end
Exciting current I23, voltage U is surveyed at the 4th end 4 of microelectrode, 1 both ends of microelectrode first end41, obtain resistance R2=U41/I23, by R1
And R2Bring the electric rent rate value ρ that vanderburg equation calculation goes out sample into:
Wherein d is the thickness of sample, is measured in experiment by micrometer, realizes Transition-metal dichalcogenide powder polycrystalline sample
The in situ measurement of product resistivity；
(9) uniformly slowly adjustment press continuously presses, according to ruby fluorescence peak R1Line is true with the frequency shift property of pressure
Recognize pressure size, intracavitary Transition-metal dichalcogenide powder Polycrystalline will be pressed to be compacted, while using repeatedly according in step 8
Vanderburg method measures sample resistivity；
(10) diamond anvil gradually presses since normal pressure, realize pressure increase continuously, and according to resistivity data with
And resistivity varies with temperature relationship and judges Transition-metal dichalcogenide energy gap closure situation.
In the step (1), the diamond anvil face diameter is 400 microns, is set at gasket impression center
Setting diameter is 200 microns of through-holes as pressure chamber, and diamond anvil is able to achieve the pressure from normal pressure to 80GPa and continuously adjusts.
A kind of method of Transition-metal dichalcogenide energy gap adjustment of the present invention has the beneficial effect that:
1, a kind of method of Transition-metal dichalcogenide energy gap adjustment, pressure production method is scientific and reasonable, pressure stepping
Precision is high, and pressure limit is also high, continuously adjustable for the compression of Transition-metal dichalcogenide energy gap, and suppressed range is big, not only
Suitable for single crystal samples and also effective to polycrystal powder sample, the scope of application is wider, strong operability, and effect is good；
2, a kind of method of Transition-metal dichalcogenide energy gap adjustment, realizes that pressure increases continuously, using vanderburg method
Sample resistivity is measured, and relationship is varied with temperature according to resistivity data and resistivity and judges Transition-metal dichalcogenide
Energy gap closure situation.Measurement means are reasonable, and operation is accurate, simple and reliable.
Detailed description of the invention
Fig. 1 is the pressure apparatus schematic diagram used in a kind of method of Transition-metal dichalcogenide energy gap adjustment；
Fig. 2 is the upper diamond anvil cell A direction view of pressure apparatus in Fig. 1；
Fig. 3 is integrated microcircuit method schematic diagram on the upper diamond anvil cell anvil face of the pressure apparatus in Fig. 1；
Fig. 4 is the method effect through a kind of adjustment of Transition-metal dichalcogenide energy gap, WSe2The change in resistance of sample
Regular schematic diagram；
Fig. 5 is WSe2The resistivity alternating temperature curve of sample energy band closure front and back；
Fig. 6 is pressure to WSe2Band structure impact effect schematic diagram；
Fig. 7 is the WSe that Fig. 4 and Fig. 5 are shown2The conduction activation energy of material and the linear relationship chart of pressure；
Fig. 8 is pressure to WS2, WSe2, MoS2, MoSe2Energy gap regulating effect schematic diagram；
In figure: 1. microelectrode first ends, 2. microelectrode second ends, 3. microelectrode third ends, the 4th end of 4. microelectrode, 5. samples
Product, diamond anvil cell on 6., 7. lower diamond anvil cells, 8. rubies, 9. gaskets, 10. copper conductors, 11. aluminium oxide,
12. molybdenum.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, invention is further described in detail, specific reality described herein
Mode is applied only to explain the present invention, is not intended to limit the present invention.
Referring to attached drawing 1 to attached drawing 3,
(1) selecting anvil face diameter is 400 microns of diamond anvil, and T301 steel is depressed into 40 microns as gasket 9 in advance, and
Use laser the center of impression burn a diameter be 200 microns hole as press chamber；
(2) diamond anvil cell sulfuric acid and nitric acid volume ratio 4:1 are subjected to chemical cleaning, get rid of surface grease and
Dust, to improve adhesive force of the conductive metal film on diamond anvil；
(3) in the way of radio-frequency sputtering, on upper diamond anvil cell anvil face, deposited metal molybdenum film is as conductive
Layer, sedimentation time are 4 minutes, 0.3 micron of molybdenum film thickness；
(4) method for utilizing photoetching and chemical attack, by metal molybdenum processing film at the figure of vanderburg electrode；
(5) it recycles the method for radio-frequency sputtering on 1.5 microns -2.5 microns of deposited aluminum oxide thin film to molybdenum electrode, makees
For insulating layer；
(6) then expose electrode detector window with photoetching and chemical corrosion method, draw copper conductor；
(7) ruby is placed in pressure bottom of chamber portion, by WSe2Powder crystal inserts sample cavity, by the diamond of integrated microelectrode
Anvil is assembled on Mao-Bell press；
(8) Transition-metal dichalcogenide powder Polycrystalline resistivity is measured using vanderburg method, firstly, in upper Buddha's warrior attendant
Exciting current I is given at stone opposed anvils microelectrode first end 1,2 both ends of microelectrode second end12, at microelectrode third end 3, microelectrode
Voltage U is surveyed at four ends, 4 both ends34, obtain resistance R1=U34/I12；Then it is given at microelectrode second end 2,3 both ends of microelectrode third end
Exciting current I23, voltage U is surveyed at the 4th end 4 of microelectrode, 1 both ends of microelectrode first end41, obtain resistance R2=U41/I23, by R1
And R2Bring the electric rent rate value ρ that vanderburg equation calculation goes out sample into:
Wherein d is the thickness of sample, is measured in experiment by micrometer, realizes Transition-metal dichalcogenide powder polycrystalline sample
The in situ measurement of product resistivity；
(9) with spanner, uniformly slowly rotation compression screw applies pressure to sample；According to ruby fluorescence peak R1Line with
The frequency shift property of pressure confirms pressure size, and intracavitary Transition-metal dichalcogenide powder Polycrystalline will be pressed to be compacted, while anti-
It is multiple that sample resistivity is measured using vanderburg method according in step (8)；
(10) diamond anvil gradually presses since normal pressure, realizes that pressure increases continuously, and continuous to measure, pressure can make original
The distance between son is close, and electron orbit wave function overlapping degree increases, and energy band broadening, energy gap narrows, and finally makes conductive energy
Power changes, i.e., can determine whether energy gap closure situation with Pressure Variation according to resistivity.
Referring to attached drawing 4, WSe is compareed2Sample change in resistance rule, from normal pressure be raised to 35.7GPa during WSe2Resistance
Rate gently linearly reduces by 5 orders of magnitude with the increase of pressure.In 38.1GPa resistivity with pressure change curve occur
One inflection point declined suddenly, it means that WSe2Energy gap be closed.
Referring to attached drawing 5 and attached drawing 6, by resistivity variation with temperature relationship under high pressure it is found that energy gap is closed preceding WSe2
Resistivity reduce as the temperature rises, it was demonstrated that WSe2Semiconductor pass property, WSe after 38GPa2Energy gap closure,
Resistivity increases with temperature and is increased, this illustrates WSe2It is changed into conductivity of metals, conduction band bottom under the effect of the pressure
It is in identical energy with top of valence band, remains at different Brillouin zone K points, the two is directly overlapping there is no occurring.
Referring to attached drawing 6 and attached drawing 7, according to Arrhenius formula ρ=ρ0exp(Et/ 2kT), by the temperature-independent of resistivity
Relationship can calculate the conduction activation energy Et of carrier.Et is reduced with the increase of pressure with the rate of 9.29meV/GPa.Et
Level off to 0eV when, all impurity energy levels are all excited, all carriers can arrive conduction band participate in conduction, at this moment carrier will satisfy
With resistivity will not change as the temperature increases.The unexpected decline for continuing growing piezoresistive rate is then due to energy band
It is indirectly overlapping caused.The distance of W atom and Se atom reduce with the increase of pressure so that near Fermi surface WState, 5dXYThe 4p state degree of coupling of state and Se increase, and are progressively smaller until closed state so as to cause energy gap.
Referring to attached drawing 8, a kind of method adjusted using Transition-metal dichalcogenide energy gap, pressure is to WS2, WSe2,
MoS2, MoSe2Energy gap regulating effect is as shown in the figure.
The above is only preferred embodiment of the invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
This is considered as protection scope of the present invention.
Claims (2)
1. a kind of method of Transition-metal dichalcogenide energy gap adjustment, characterized in that it the following steps are included:
(1) start diamond anvil, impression is generated on gasket, through-hole is set at impression center, by the through-hole on gasket
As pressure chamber；
(2) diamond anvil cell is subjected to chemical cleaning, removes the grease and dust on its surface；
(3) on upper diamond anvil cell anvil face, in the way of radio-frequency sputtering, the metal molybdenum film conduct of 0.3 micron of deposition
Conductive layer；
(4) the metal molybdenum film on upper diamond anvil cell anvil face is processed into model moral using the method for photoetching and chemical attack
The figure of fort electrode, the position of electrode arrangements are determined by accurate litho machine console completely；
(5) 1.5 microns -2.5 microns of aluminum oxide film is deposited to diamond anvil cell using the method for radio-frequency sputtering
In the molybdenum electrode of anvil face, as insulating layer；
(6) on the insulating layer, expose electrode detector window with photoetching and chemical corrosion method；
(7) diamond anvil is assembled, the gasket with through-hole is arranged on lower diamond anvil cell anvil face, is put in pressure bottom of chamber portion
Ruby is set, Transition-metal dichalcogenide powder Polycrystalline is then filled up into pressure chamber, by the upper diamond of integrated microelectrode
Opposed anvils are assembled on press；
(8) Transition-metal dichalcogenide powder Polycrystalline resistivity is measured using vanderburg method, firstly, in upper diamond pair
Exciting current I is given at top anvil microelectrode first end (1), microelectrode second end (2) both ends12, at microelectrode third end (3), microelectrode
Voltage U is surveyed at 4th end (4) both ends34, obtain resistance R1=U34/I12；Then in microelectrode second end (2), microelectrode third end
(3) exciting current I is given at both ends23, voltage U is surveyed at the 4th end (4) of microelectrode, microelectrode first end (1) both ends41, obtain resistance R2
=U41/I23, by R1And R2Bring the electric rent rate value ρ that vanderburg equation calculation goes out sample into:
Wherein d is the thickness of sample, is measured in experiment by micrometer, realizes Transition-metal dichalcogenide powder Polycrystalline electricity
The in situ measurement of resistance rate；
(9) uniformly slowly adjustment press continuously presses, according to ruby fluorescence peak R1Line confirms pressure with the frequency shift property of pressure
Size will press intracavitary Transition-metal dichalcogenide powder Polycrystalline to be compacted, while use model moral according to step (8) is middle repeatedly
Fort method measures sample resistivity；
(10) diamond anvil gradually presses since normal pressure, realizes that pressure increases continuously, and according to resistivity data and electricity
Resistance rate varies with temperature relationship and judges Transition-metal dichalcogenide energy gap closure situation.
2. a kind of method of Transition-metal dichalcogenide energy gap adjustment according to claim 1, characterized in that described
The step of (1) in, the diamond anvil face diameter be 400 microns, gasket impression center setting diameter be 200 microns
Through-hole is able to achieve the pressure from normal pressure to 80GPa and continuously adjusts as pressure chamber, diamond anvil.
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Cited By (5)
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| CN112147414A (en) * | 2020-09-27 | 2020-12-29 | 中国科学院地球化学研究所 | Method for measuring resistivity of metallic iron under ultrahigh pressure |
| CN112415055A (en) * | 2020-10-10 | 2021-02-26 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
| CN112782211A (en) * | 2020-12-28 | 2021-05-11 | 东北电力大学 | Water phase change detection method |
| CN113267683A (en) * | 2021-05-07 | 2021-08-17 | 武汉理工大学 | In-situ measurement method for metal resistivity at high temperature and high pressure |
| CN116251536A (en) * | 2023-03-16 | 2023-06-13 | 吉林大学 | Iridium telluride powder material with orthogonal structure and preparation method thereof |
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| CN112415055A (en) * | 2020-10-10 | 2021-02-26 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
| CN112415055B (en) * | 2020-10-10 | 2023-06-13 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
| CN112782211A (en) * | 2020-12-28 | 2021-05-11 | 东北电力大学 | Water phase change detection method |
| CN112782211B (en) * | 2020-12-28 | 2023-11-21 | 东北电力大学 | Water phase change detection method |
| CN113267683A (en) * | 2021-05-07 | 2021-08-17 | 武汉理工大学 | In-situ measurement method for metal resistivity at high temperature and high pressure |
| CN113267683B (en) * | 2021-05-07 | 2023-05-12 | 武汉理工大学 | In-situ measurement method for metal resistivity at high temperature and high pressure |
| CN116251536A (en) * | 2023-03-16 | 2023-06-13 | 吉林大学 | Iridium telluride powder material with orthogonal structure and preparation method thereof |
| CN116251536B (en) * | 2023-03-16 | 2024-05-17 | 吉林大学 | Iridium telluride powder material with orthogonal structure and preparation method thereof |
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