CN114725187A - alpha-GeTe two-dimensional material and PVD (physical vapor deposition) preparation method and application thereof - Google Patents
alpha-GeTe two-dimensional material and PVD (physical vapor deposition) preparation method and application thereof Download PDFInfo
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- CN114725187A CN114725187A CN202210278701.6A CN202210278701A CN114725187A CN 114725187 A CN114725187 A CN 114725187A CN 202210278701 A CN202210278701 A CN 202210278701A CN 114725187 A CN114725187 A CN 114725187A
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- 229910005900 GeTe Inorganic materials 0.000 title claims abstract description 114
- 239000000463 material Substances 0.000 title claims abstract description 83
- 238000005240 physical vapour deposition Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000000758 substrate Substances 0.000 claims abstract description 69
- 239000002135 nanosheet Substances 0.000 claims abstract description 56
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 239000012159 carrier gas Substances 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 230000005669 field effect Effects 0.000 claims description 43
- 238000000151 deposition Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 11
- 239000010445 mica Substances 0.000 claims description 6
- 229910052618 mica group Inorganic materials 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000010894 electron beam technology Methods 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000005457 optimization Methods 0.000 claims 1
- 229910003090 WSe2 Inorganic materials 0.000 description 34
- 230000003287 optical effect Effects 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 22
- GPMBECJIPQBCKI-UHFFFAOYSA-N germanium telluride Chemical compound [Te]=[Ge]=[Te] GPMBECJIPQBCKI-UHFFFAOYSA-N 0.000 description 20
- 238000010586 diagram Methods 0.000 description 18
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 9
- 238000005229 chemical vapour deposition Methods 0.000 description 9
- 229910052681 coesite Inorganic materials 0.000 description 9
- 229910052906 cristobalite Inorganic materials 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 9
- 229910052682 stishovite Inorganic materials 0.000 description 9
- 229910052905 tridymite Inorganic materials 0.000 description 9
- 238000011160 research Methods 0.000 description 8
- 229910052573 porcelain Inorganic materials 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 229910020039 NbSe2 Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000002055 nanoplate Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- SDDGNMXIOGQCCH-UHFFFAOYSA-N 3-fluoro-n,n-dimethylaniline Chemical compound CN(C)C1=CC=CC(F)=C1 SDDGNMXIOGQCCH-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910016001 MoSe Inorganic materials 0.000 description 1
- 229910016021 MoTe2 Inorganic materials 0.000 description 1
- 229910004214 TaSe2 Inorganic materials 0.000 description 1
- 229910004202 TaTe2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0657—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C—CHEMISTRY; METALLURGY
- 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 belongs to the field of two-dimensional material preparation, and particularly discloses a PVD (physical vapor deposition) preparation method of an alpha-GeTe two-dimensional material, which comprises the steps of heating and volatilizing a GeTe raw material at the temperature of 600-380 ℃, and carrying a hydrogen-containing carrier gas to carry out physical vapor deposition on the surface of a substrate without a dangling bond to prepare the alpha-GeTe two-dimensional material; the hydrogen-containing carrier gas is a mixed gas of hydrogen and protective atmosphere, wherein the flow of the hydrogen is 1-10sccm, and the flow of the protective atmosphere is 70-90 sccm. The invention also discloses a material prepared by the preparation method and application. The technical scheme of the invention can extend the alpha-GeTe 2D metal nanosheets with thin atomic levels in a two-dimensional mode; the controllable preparation of the alpha-GeTe nanosheet with the atomic-level thickness is realized for the first time.
Description
Technical Field
The invention belongs to the field of preparation of two-dimensional materials, and particularly relates to the field of preparation of alpha-GeTe two-dimensional materials.
Technical Field
Two-dimensional (2D) materials have become a new generation of atomically thin devices due to their wide range of physical and chemical propertiesA new material platform for basic research and potential applications. Is widely applied to the field of electronic devices1-3Photoelectric field4,5Valley electronics and spintronics6,7Sensor8,9And energy storage10,11And the like. While most efforts have focused on graphene and 2D semiconductors, 2D metallic materials (e.g., TaS)2 12， TaSe2 13，NbSe2 14，Td-MoTe2 15And VS and2 16) Considerable attention has been paid to it due to its particular physical properties. Reported that NbSe2Shows thickness-dependent superconducting properties, and the transition temperature increases from 1.0K to 4.56K as the number of layers increases from a single layer to 10 layers17。VS2Excellent conductivity of the nanosheets (3X 105S m)-1) Apply it in the next generation electronic field18,19. Two-dimensional PtTe2The single crystal has strong thickness-adjustable electrical property20And NiTe2Has similar conductivity change trend21. As a new member of the 2D material family, MTMD has abundant physical properties and exciting application potential in future electronic, spintronics and catalytic applications.
Chemical Vapor Deposition (CVD) is well controllable and easy to fabricate in large quantities, in addition to mechanically peeling sheets of limited size and scalability. CVD has been widely used for two-dimensional TMDC materials, and in particular, various 2D-TMD semiconductors (e.g., MoSe) have been successfully prepared by using different forms of CVD methods2 22，WSe2 23And) heterostructures thereof24. In addition, CVD for preparing metallic two-dimensional materials is also widely reported. PtSe as thickness decreases2And TaTe2A metal to semiconductor transition occurs25,26. The appearance of two-dimensional metal materials solves the contact problem of two-dimensional materials in the construction of electronic and optoelectronic devices. The two-dimensional metal material can form an ideal vdW interface and can strongly inhibit metal-induced gap states formed in a semiconductor. Two-dimensional semiconductor materials in electronics and opticsAn important step in practical applications in electronic devices. However, the resulting thickness 2D-MTMD is typically in the range of a few nanometers to a few tens of nanometers. Especially the growth of single-layer MTMD, which is crucial for the basic research and potential technical applications of such new materials limited by 2D, remains a major challenge.
Citations
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Disclosure of Invention
In order to fill the gap of the preparation of the alpha-GeTe two-dimensional material, the invention provides a PVD (physical vapor deposition) synthesis method of the alpha-GeTe two-dimensional material, and aims to successfully prepare the alpha-GeTe two-dimensional material which is pure in phase and has an ultrathin structure and is two-dimensional and non-layered.
The second purpose of the invention is to provide the alpha-GeTe two-dimensional material prepared by the preparation method and the application of the alpha-GeTe two-dimensional material in micro-nano electronic devices.
The third purpose of the invention is to provide a micro-nano electronic device containing the alpha-GeTe two-dimensional material.
The industry provides some CVD preparation reports of metal telluride two-dimensional materials such as V, Nb, Ta and the like, but no preparation report of alpha-GeTe two-dimensional materials exists. In addition, it is well known in the industry that materials of different elements have different properties, and the technical scheme is difficult to simply convert and the conversion effect is difficult to expect. For example, for the preparation of a GeTe two-dimensional material, the material has low activity and is difficult to successfully prepare, in addition, GeTe has multi-phase forms of alpha, beta, gamma and the like, and the phase purity, the thickness, the morphology and the performance of a product prepared by the existing preparation method are not ideal, so that the invention provides the following scheme for filling the blank of the preparation of the alpha-GeTe two-dimensional material and improving the preparation effect:
a PVD preparation method of an alpha-GeTe two-dimensional material comprises the steps of volatilizing a GeTe raw material at 600-700 ℃, and carrying out physical vapor deposition on the volatilized raw material on the surface of a substrate without dangling bonds at the deposition temperature of 340-380 ℃ in the presence of a hydrogen-containing carrier gas to prepare the alpha-GeTe two-dimensional material;
the carrier gas containing the hydrogen is a mixed gas of the hydrogen and the protective atmosphere, wherein the flow of the hydrogen is 1-10sccm, and the flow of the protective atmosphere is 70-90 sccm.
The invention firstly proposes to synthesize the alpha-GeTe two-dimensional material by adopting a PVD mode, and researches show that the alpha-GeTe two-dimensional material synthesized by adopting PVD is easy to have the problems of higher vertical growth rate than transverse growth rate, difficult transverse deposition, unsatisfactory crystallinity, unsatisfactory phase purity, poorer morphology uniformity and the like. Aiming at the problems in the alpha-GeTe PVD preparation process, the research of the invention finds that for the preparation of the alpha-GeTe two-dimensional material, a hydrogen-assisted PVD preparation idea is innovatively adopted, and the combined control of a suspension-free substrate, a deposition temperature and a carrier gas flow rate is matched, so that the transverse growth and the vertical growth of the alpha-GeTe can be unexpectedly and effectively induced, in addition, an alpha phase can be effectively induced, and thus the ultrathin alpha-GeTe single-crystal two-dimensional material with excellent crystallinity, phase purity and uniform appearance can be prepared.
In the invention, the PVD preparation method without a suspended substrate and under the assistance of hydrogen atmosphere, and the combined control of the atmosphere and temperature in the PVD deposition process are adopted as the key points for cooperatively solving the problems of difficulty in preparation, multiple impurity phases, easiness in vertical growth, poor morphology uniformity and the like of a GeTe two-dimensional material.
In the invention, the substrate without dangling bonds is mica without dangling bonds or a two-dimensional material substrate, and is preferably a two-dimensional material substrate. The research of the invention finds that the two-dimensional material substrate can be further cooperated with the hydrogen-assisted PVD process, and the two-dimensional material has better cooperative performance in the aspects of successfully preparing the alpha-GeTe two-dimensional material and improving the phase, the appearance and the thickness of the alpha-GeTe two-dimensional material.
The two-dimensional material substrate is deposited with MX2A substrate of two-dimensional material.
Preferably, M is a transition metal element, and more preferably at least one of Mo and W;
preferably, said X is at least one of S, Se;
preferably, the substrate without dangling bonds has a flat surface.
Preferably, in the two-dimensional material substrate, the plane size of the two-dimensional material is greater than or equal to 50 um; preferably greater than or equal to 200 um.
In the present invention, the purity of the GeTe raw material is 99% or more, and more preferably 99.9% or more.
In the invention, the volatilization temperature of the GeTe raw material is 620-675 ℃, and the preferable temperature is 620-630 ℃.
In the invention, in the hydrogen-containing carrier gas, the protective atmosphere is at least one of nitrogen and inert gas.
In the invention, the hydrogen-assisted PVD is adopted, so that the transverse growth of alpha-GeTe can be effectively improved, the alpha phase can be induced, the morphology of the material can be regulated, and the material with high phase purity, uniform morphology and atomic-scale thickness can be prepared.
The research of the invention finds that under the hydrogen-assisted PVD preparation process, the combination control of the atmosphere and the PVD temperature is further matched, so that the alpha phase, the high crystallinity, the uniform morphology and the atomic-scale thickness of the alpha-GeTe two-dimensional material can be further improved in a synergistic manner.
In the invention, the flow rate of the hydrogen in the hydrogen-containing carrier gas is 2-8 sccm, preferably 4-8 sccm. The flow rate of the protective atmosphere is 75-85 sccm.
In the invention, the temperature of the physical vapor deposition is 340-360 ℃, and preferably 340-350 ℃.
It was found that at the preferred carrier gas and PVD deposition temperatures, further synergistic improvement in alpha phase purity was achieved, facilitating atomic scale thickness of the material.
In the invention, the time of physical vapor deposition is 5-15 min, preferably 8-12 min.
The invention also provides the alpha-GeTe two-dimensional material prepared by the preparation method.
The invention also provides an application of the alpha-GeTe two-dimensional material prepared by the preparation method, and the alpha-GeTe two-dimensional material is used for preparing micro-nano electronic devices;
the micro-nano device electric device is a field effect transistor, for example.
In the invention, the alpha-GeTe two-dimensional material can be prepared into a required micro-nano electronic device based on the existing method. For example, the steps of preparing the field effect transistor by using the prepared alpha-GeTe two-dimensional nanosheet are as follows:
marking a sample on the surface of the alpha-GeTe two-dimensional nanosheet of the substrate without the dangling bond by using electron beam exposure, and then depositing metal on the surface of the sample to obtain a field effect transistor;
preferably, depositing metal on the surface of the alpha-GeTe nanosheet by a vacuum coating machine;
preferably, the metal is Cr and Au.
The invention also provides a field effect transistor device which comprises the alpha-GeTe two-dimensional material prepared by the preparation method or is prepared from the alpha-GeTe two-dimensional material.
Advantageous effects
1. The invention provides an alpha-GeTe two-dimensional material.
2. The invention innovatively adopts a hydrogen-assisted PVD preparation idea, is matched with the combined control of a suspension-free substrate, deposition temperature and carrier gas flow, can unexpectedly and effectively induce the transverse growth and the vertical growth of the alpha-GeTe, and can also effectively induce an alpha-phase, so that the ultrathin alpha-GeTe two-dimensional material with excellent crystallinity, phase purity and uniform appearance can be prepared. The preparation method disclosed by the invention is ultrathin, particularly the growth of MTMD (molecular weight distribution) with atomic-scale thickness, which is very important for basic research and potential technical application of new materials limited by 2D (two-dimensional).
The thickness of the germanium telluride nanosheet prepared by the method can reach atomic level, the size can reach 2-30 mu m, the germanium telluride nanosheet has regular hexagonal or triangular shapes, the crystallinity is good, and the quality is high.
3. The alpha-GeTe two-dimensional material prepared by the invention has good semiconductor performance. For example, the method can be used for preparing the metal germanium telluride contact WSe2A field effect transistor.
Drawings
FIG. 1 is a schematic view of an atmospheric pressure chemical vapor deposition apparatus for preparing germanium telluride nanosheets;
FIG. 2 shows the WSe of example 1-12An optical schematic diagram of a germanium telluride nanosheet prepared on a substrate;
FIG. 3 shows the WSe of example 1-12An X-ray energy spectrum of the germanium telluride nanosheet prepared on the substrate;
FIG. 4 shows the WSe of example 1-12A statistical thickness chart of the germanium telluride nanosheets prepared on the substrate;
FIG. 5 is an optical schematic of germanium telluride nanoplates made in examples 1-2 on a mica substrate;
FIG. 6 is a statistical plot of the thickness of germanium telluride nanoplates made on mica substrates for examples 1-2;
FIG. 7 shows comparative example 1-1 on SiO2Optical schematic of the product produced on a Si substrate;
FIG. 8 shows comparative example 1-1 on SiO2A statistical thickness map of the product produced on a Si substrate;
FIG. 9 shows WSe of comparative examples 1-22An optical schematic of the product produced on the substrate;
FIG. 10 shows WSe of comparative examples 1-22A thickness histogram of the product produced on the substrate;
FIG. 11 shows examples 1-2 in WSe2An optical schematic diagram of a germanium telluride nanosheet prepared on a substrate;
FIG. 12 shows examples 1-2 in WSe2A thickness statistical graph of the germanium telluride nanosheets prepared on the substrate;
FIG. 13 shows examples 1 to 3 in WS2An optical schematic diagram of a germanium telluride nanosheet prepared on a substrate;
FIG. 14 shows examples 1-3 in WSe2A thickness statistical chart of the germanium telluride nanosheets prepared on the substrate;
FIG. 15 shows examples 1-4 in WSe2An optical diagram of a germanium telluride nanosheet produced on a substrate;
FIG. 16 shows examples 1-4 in WSe2A thickness statistical graph of the germanium telluride nanosheets prepared on the substrate;
FIG. 17 shows examples 1-5 in WSe2An optical diagram of a germanium telluride nanosheet produced on a substrate;
FIG. 18 shows examples 1-5 at WSe2A thickness statistical graph of the germanium telluride nanosheets prepared on the substrate;
FIG. 19 shows examples 1-6 in WSe2An optical diagram of a germanium telluride nanosheet produced on a substrate;
FIG. 20 shows examples 1-6 at WSe2A thickness statistical graph of the germanium telluride nanosheets prepared on the substrate;
FIG. 21 shows comparative examples 1 to 3 on SiO2Optical diagram of the product produced on a Si substrate;
FIG. 22 shows comparative examples 1 to 4 on SiO2Optical diagram of the product produced on Si substrate;
FIG. 23 shows example 2-1 in WSe2An optical schematic of a GeTe device fabricated on a substrate;
FIG. 24 is an output curve of the α -GeTe field effect transistor of example 2-1;
FIG. 25 is a transfer curve of the α -GeTe field effect transistor of example 2-1;
FIG. 26 is a graph showing the relationship between the conductivity and the thickness of the α -GeTe field effect transistor of example 2-1;
FIG. 27 is a breakdown curve of the α -GeTe field effect transistor of example 2-1;
FIG. 28 shows WSe of example 2-2. alpha. -GeTe nanosheets as metal electrodes2A field effect transistor schematic;
FIG. 29 shows WSe of example 2-2. alpha. -GeTe nanosheet as metallic electrode2A field effect transistor optical picture;
FIG. 30 shows WSe of example 2-2. alpha. -GeTe nanosheets as metallic electrodes2A field effect transistor output curve;
FIG. 31 shows WSe of example 2-2. alpha. -GeTe nanosheets as metal electrodes2A field effect transistor transfer curve;
FIG. 32 is a WSe with comparative example 2-1Cr/Au as a metal electrode2A field effect transistor schematic;
FIG. 33 is a WSe with comparative example 2-1Cr/Au as a metal electrode2A field effect transistor optical schematic;
FIG. 34 shows WSe of comparative example 2-1Cr/Au as a metal electrode2A field effect transistor output curve;
FIG. 35 shows WSe of comparative example 2-1 in which Cr/Au is a metal electrode2A field effect transistor output curve;
the specific implementation method comprises the following steps:
the present invention will be further described below by way of examples, but the present invention is not limited to the following.
In the following cases of the invention, dangling bond-free two-dimensional material substrates are treated with WSe2The nanoplatelets substrate is exemplified and can be obtained on the basis of conventional means, for example, in the present case, the preparation steps are: 100mg of tungsten selenide feedstock was first placed in the center of a tube furnace, purged with 1200sccm Ar gas to remove oxygen, and then blown upstream from the heated zone with an Ar gas flow rate of 80sccm (reverse flow: 285nm SiO. RTM.) instead2Si substrate to raw material), setting temperature-raising program at 40min, heating to 1180 ℃, keeping constant temperature for two minutes, changing the direction of Ar gas to growth from upstream to downstream for three minutes (positive gas flow: raw material to 285nm SiO2a/Si substrate), naturally cooling to 285nm SiO2Deposition on Si substrate to obtain WSe2Nanosheets. It should be noted that the substrate and preparation are only exemplary of the embodiments of the present invention, and do not constitute the present inventionThe necessary technical definition of the method.
In the following cases, the purity of the GeTe raw material was 99.99% or more.
1. Preparing an alpha-GeTe nano sheet on a two-dimensional material substrate:
examples 1 to 1
The experimental setup diagram of α -GeTe nanosheets is shown in fig. 1. FIG. 1 is a WSe2The preparation device of the nano-sheet substrate can prepare WSe by adopting the existing method2Nanosheet substrate (also referred to herein as WSe)2Two-dimensional material substrates, or WSe2A substrate). Placing the porcelain boat containing GeTe powder in a constant temperature region 1 of a tube furnace, wherein a piece of the porcelain boat is grown with WSe2285nm SiO of nanosheet2the/Si as the growth substrate of germanium telluride was placed on another porcelain boat and placed in the constant temperature zone 2 of the tube furnace to obtain the proper crystal growth temperature. Before heating, the atmosphere in the quartz tube was purged with a large flow rate (600 sccm) of argon gas. Under the action of reverse carrier gas flow (constant temperature region 2 to constant temperature region 1), the temperature of constant temperature region 1 and constant temperature region 2 is raised to 625 deg.C (volatilization temperature) and 340 deg.C (physical vapor deposition temperature), and then converted into forward carrier gas (constant temperature region 1 to constant temperature region 2), and the volatilized raw materials are subjected to WSe2Surface physical vapor deposition of the nano-sheets, wherein the carrier gas is Ar-H2The flow rate of argon is 80sccm, the flow rate of hydrogen is 7.8sccm, and the time of physical vapor deposition is 10 min.
In WSe2The substrate will have single crystal alpha-GeTe nano-sheet. The optical photograph of the prepared alpha-GeTe nanosheet is shown in FIG. 2.
FIG. 2 is an optical schematic diagram of an α -GeTe nanosheet prepared in the present example, in which the position 1 represents SiO2[ Si ], WSe at 2 in the figure2In the figure, 2 represents the grown alpha-GeTe, and figure 3 is an XRD pattern showing that the alpha-GeTe has good crystallinity (figure 3), the thickness reaches the atomic level, the distribution is 1.2-5 nm, and the size is 2-30 μm. The scale in FIG. 2 is 5 μm. FIG. 4 is a thickness histogram.
Examples 1 to 2
The only difference compared to example 1-1 is that mica was used as the PVD deposition substrate, instead of the growth described with WSe2285nm SiO of nanosheet2and/Si. The other operations and parameters were the same as in example 1.
FIG. 5 is an optical schematic diagram of an α -GeTe nanosheet prepared on a mica substrate, the α -GeTe nanosheet obtained under the conditions has good crystallinity, thin thickness, distribution of 40-160 nm and size of 2-30 μm. The scale in FIG. 5 is 10 μm. FIG. 6 is a thickness histogram.
Comparative examples 1 to 1
Compared with example 1-1, the difference is only that SiO is used2(ii)/Si (for suspended substrate) as PVD substrate, instead of said growth with WSe2285nm SiO of nanosheet2and/Si. The other operations and parameters were the same as in example 1. FIG. 7 is a schematic representation of SiO2Optical schematic of the product prepared on a/Si substrate, in which 1 denotes SiO2and/Si, wherein a position 2 in the figure represents alpha-GeTe, and the alpha-GeTe nano-sheet obtained under the condition has poor crystallinity, thicker thickness and smaller size, and the scale in figure 7 is 10 mu m. FIG. 8 is a thickness histogram.
Comparative examples 1 to 2
The difference from example 1-1 is only that no hydrogen gas was added to the carrier gas. The flow rate of the carrier gas is: ar flow rate of 80sccm, H 20 sccm. The other operations and parameters were the same as in example 1.
FIG. 9 shows a WSe2The optical schematic diagram of the product prepared on the substrate, the thickness of the nanosheet obtained under the condition is 40-160 nm, and the size is 2-30 μm. The scale in FIG. 9 is 10 μm. Fig. 10 is a thickness statistical chart.
Examples 1 to 2
Compared with example 1-1, the difference is that GeTe volatilization temperature (constant temperature zone 1) is 650 ℃, WSe2The temperature of the substrate (constant temperature region 2) is 350 ℃, the flow rate of Ar in the carrier gas is 80sccm, and H27.8sccm, and the deposition time is 10 min. FIG. 11 shows a WSe2The alpha-GeTe nanosheet prepared on the substrate has an optical schematic diagram, and the alpha-GeTe nanosheet obtained under the condition has good crystallinity, is slightly thick and reaches an atomic level, is distributed at 5-15 nm and has the size of 2-30 mu m. The scale in FIG. 11 is 10 μm. FIG. 12 is a thickness histogram.
Examples 1 to 3
Compared with example 1-1, the difference is that GeTe volatilization temperature is 675 ℃, WSe2The temperature of the substrate (constant temperature zone 2) is 360 ℃, the flow rate of Ar in the carrier gas is 80sccm, and H27.8sccm, and the deposition time is 10 min. FIG. 13 shows WSe2The alpha-GeTe nanosheet prepared on the substrate has an optical schematic diagram, and the alpha-GeTe nanosheet obtained under the condition has good crystallinity, is slightly thick and reaches the atomic level, is distributed at-30 nm and has the size of 2-30 mu m. The scale in FIG. 13 is 10 μm. FIG. 14 is a thickness histogram.
Examples 1 to 4
Compared with example 1-1, the only difference is that H in the carrier gas2The flow rate was 2 sccm. FIG. 15 shows a WSe2The alpha-GeTe nanosheet prepared on the substrate has an optical schematic diagram, and the alpha-GeTe nanosheet obtained under the condition has good crystallinity, is slightly thick and reaches an atomic level, is distributed at 30-60 nm and has the size of 2-30 mu m. The scale in FIG. 15 is 10 μm. FIG. 16 is a thickness histogram.
Examples 1 to 5
Compared with example 1-1, the difference is only that H in the carrier gas2The flow rate was 4 sccm. FIG. 17 shows WSe2The alpha-GeTe nanosheet prepared on the substrate has an optical schematic diagram, and the alpha-GeTe nanosheet obtained under the condition has good crystallinity, is slightly thick and reaches an atomic level, is distributed at 1-5 nm and has the size of 2-30 mu m. The scale in FIG. 17 is 10 μm. FIG. 18 is a thickness histogram.
Examples 1 to 6
Compared with example 1-1, the difference is only that H in the carrier gas2The flow rate was 8 sccm. FIG. 19 shows a WSe2The alpha-GeTe nanosheet prepared on the substrate has good crystallinity, is slightly thick and reaches atomic level, is distributed at 3-12 nm and has the size of 2-30 mu m. The scale in FIG. 19 is 10 μm. FIG. 20 is a thickness histogram.
Comparative examples 1 to 3
The difference from example 1-1 is only that the temperature of the constant temperature region 1 was 710 ℃, the Ar flow rate in the carrier gas was 80sccm, and H was20sccm, and a deposition time of 10 min. Optical schematic of the product obtained in FIG. 21As shown in the figure, the prepared material has no regulation and fails to be prepared.
Comparative examples 1 to 4:
compared with the example 1-1, the difference is only that the CVD method is adopted for preparation, and the steps are as follows:
the same two-temperature zone tube furnace as in example 1-1 was used, in which the raw materials of (50mg) tellurium powder and (50mg) germanium powder were mixed and placed in a porcelain boat 1, and the porcelain boat was set in the heating zone (constant temperature zone 1) at the upstream, and WSe was deposited thereon2The two-dimensional material is placed in a deposition zone (constant temperature zone 2) and is located downstream of the carrier gas flow. The temperature of the area of the porcelain boat 1 is controlled at 625 ℃ under the reverse airflow (from the constant temperature area 2 to the constant temperature area 1), the temperature of the constant temperature area 2 is controlled at 340 ℃, and then the carrier gas is changed and the volatilized Te and Ge raw materials are carried to the WSe at the downstream under the carrying of the carrier gas2Performing chemical vapor deposition on the surface of the two-dimensional material, wherein the carrier gas is Ar-H2(ii) a The flow rates are Ar 80sccm and H respectively28sccm, and the time for chemical deposition is 10 min.
The optical diagram is shown in 22, and the alpha-GeTe nano-sheet prepared by CVD has multiphase coexistence and the vertical dimension is far larger than the transverse dimension. The scale in FIG. 22 is 10 μm.
2. Preparation of field effect transistor and two-dimensional material
Example 2-1
The preparation method of the alpha-GeTe field effect transistor comprises the step of depositing metal Cr (10nm)/Au (50nm) on alpha-GeTe nanosheets (materials prepared in the embodiment 1-1) prepared by a PVD method by using electron beam exposure to obtain the alpha-GeTe field effect transistor.
Examples 2 to 2
α-GeTe/WSe2Method for preparing field effect transistor, depositing metal Cr (10nm)/Au (50nm) on alpha-GeTe nanosheet (material prepared in example 1-1) prepared by PVD method by exposing with electron beam to obtain alpha-GeTe contact WSe2A field effect transistor.
Comparative example 2-1
WSe2A method of producing a field effect transistor, which is different from that of example 2-1 only in that WSe is not used2Forming alpha-GeTe on the surface of two-dimensional material directlyIn the WSe2And (5) carrying out transistor preparation on the surface. Other device preparations and parameters were the same as in example 2-1.
FIG. 23 is a schematic view of an α -GeTe field effect transistor in accordance with example 2-1;
FIG. 24 is an output curve of an α -GeTe field effect transistor of an embodiment 2-1;
FIG. 25 is a graph of the transfer curve for the α -GeTe field effect transistor of example 2-1;
FIG. 26 is a graph of conductivity statistics for an implementation of 2-1 α -GeTe field effect transistor;
FIG. 27 is a graph of breakdown voltage for a field effect transistor embodying 2-1 α -GeTe;
FIG. 28 is a WSe of example 2-2. alpha. -GeTe as a metal electrode2A field effect transistor schematic;
FIG. 29 shows WSe of example 2-2. alpha. -GeTe as a metal electrode2A field effect transistor optical diagram;
FIG. 30 is a WSe of a comparative example 2-2. alpha. -GeTe as a metal electrode2A field effect transistor output curve;
FIG. 31 is a WSe of comparative example 2-2. alpha. -GeTe as a metal electrode2A field effect transistor transfer curve;
FIG. 32 is a WSe with comparative example 2-1Cr/Au as a metal electrode2A field effect transistor schematic;
FIG. 33 is a WSe with comparative example 2-1Cr/Au as a metal electrode2A field effect transistor optical schematic;
FIG. 34 shows WSe with comparative example 2-1Cr/Au as metal electrode2A field effect transistor output curve;
FIG. 35 shows WSe of comparative example 2-1 in which Cr/Au is a metal electrode2A field effect transistor output curve;
the electric research of the field effect transistor proves that the alpha-GeTe has good conductivity and ultrahigh breakdown voltage. By comparing example 2-2 and comparative example 2-1, the field effect transistor using α -GeTe as a metal electrode has a large improvement in performance, in which the on-state current density is increased from 7.83 μ A/μm to 23.86 μ A/μm and the electron mobility is 16.5cm2 V- 1S-1Increased to 75.0cm2 V-1S-1) Proves that alpha-GeTe is used as the metal electrode pair WSe2Enhancement of field effect transistor performance.
Claims (10)
1. A PVD preparation method of an alpha-GeTe two-dimensional material is characterized by comprising the following steps: volatilizing the GeTe raw material at the temperature of 600-700 ℃; carrying out physical vapor deposition on the volatilized raw materials on the surface of a substrate without dangling bonds at the deposition temperature of 380 ℃ along with hydrogen-containing carrier gas to prepare the alpha-GeTe two-dimensional material;
the hydrogen-containing carrier gas is a mixed gas of hydrogen and protective atmosphere, wherein the flow of the hydrogen is 1-10sccm, and the flow of the protective atmosphere is 70-90 sccm.
2. The PVD method of producing an α -GeTe two-dimensional material of claim 1, wherein: the volatilization temperature of the GeTe raw material is 620-675 ℃, and the preferable temperature is 620-630 ℃;
preferably, the purity of the GeTe raw material is greater than or equal to 99%, and more preferably greater than or equal to 99.9%.
3. A PVD method for producing α -GeTe two-dimensional material according to claim 1, wherein: in the hydrogen-containing carrier gas, the protective atmosphere is at least one of nitrogen and inert gas.
4. A PVD method for producing α -GeTe two-dimensional material according to claim 1, wherein: in the hydrogen-containing carrier gas, the flow rate of hydrogen is 2-8 sccm, preferably 4-8 sccm;
the flow rate of the protective atmosphere is preferably 75-85 sccm.
5. The PVD method of producing an α -GeTe two-dimensional material of claim 1, wherein: the temperature of the heating volatilization area is 620-675 ℃, and the further optimization is 620-630 ℃.
6. A PVD method for producing α -GeTe two-dimensional material according to claim 1, wherein: the temperature of the physical vapor deposition area is 340-360 ℃, and the preferable temperature is 340-350 ℃;
preferably, the time of physical vapor deposition is 5-15 min.
7. The PVD method of producing an α -GeTe two-dimensional material of claim 1, wherein: mica or two-dimensional material substrate without dangling bonds;
the two-dimensional material substrate is deposited with MX2A substrate of two-dimensional material;
preferably, M is a transition metal element, and more preferably at least one of Mo and W;
preferably, said X is at least one of S, Se;
preferably, said substrate free of dangling bonds has a flat surface;
preferably, in the two-dimensional material substrate, the plane size of the two-dimensional material is greater than or equal to 50 um; preferably greater than or equal to 200 um.
8. An alpha-GeTe two-dimensional material prepared by the preparation method of any one of claims 1 to 7.
9. The application of the alpha-GeTe two-dimensional material prepared by the preparation method of any one of claims 1 to 7 is characterized in that the alpha-GeTe two-dimensional material is used for preparing micro-nano electronic devices;
preferably, the micro-nano electronic device is a field effect transistor;
preferably, the field effect transistor is prepared by the following steps:
marking a sample on the surface of an alpha-GeTe two-dimensional nanosheet of a substrate without dangling bonds by electron beam exposure, and then depositing metal on the surface of the sample to obtain a field effect transistor;
preferably, depositing metal on the surface of the alpha-GeTe nanosheet by a vacuum coating machine;
preferably, the metal is Cr and Au.
10. A field effect transistor device, comprising or prepared from the α -GeTe two-dimensional material prepared by the preparation method of any one of claims 1 to 7.
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| CN118480761A (en) * | 2024-07-09 | 2024-08-13 | 湘潭大学 | Preparation method and application of wafer-level tellurium-selenium alloy film |
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| CN116121865A (en) * | 2023-02-22 | 2023-05-16 | 湘潭大学 | Method for preparing tungsten selenide/indium selenide two-dimensional vertical heterojunction |
| CN118480761A (en) * | 2024-07-09 | 2024-08-13 | 湘潭大学 | Preparation method and application of wafer-level tellurium-selenium alloy film |
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