CN114477105B - Two-dimensional BiCuSeO nanosheet, preparation method thereof and semiconductor device - Google Patents
Two-dimensional BiCuSeO nanosheet, preparation method thereof and semiconductor device Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 74
- 229910002903 BiCuSeO Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000004065 semiconductor Substances 0.000 title claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 58
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000010949 copper Substances 0.000 claims abstract description 31
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 29
- 229910052802 copper Inorganic materials 0.000 claims abstract description 28
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001301 oxygen Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000011669 selenium Substances 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 21
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 18
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000001103 potassium chloride Substances 0.000 claims description 9
- 235000011164 potassium chloride Nutrition 0.000 claims description 9
- 239000005751 Copper oxide Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910000431 copper oxide Inorganic materials 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- IRPLSAGFWHCJIQ-UHFFFAOYSA-N selanylidenecopper Chemical compound [Se]=[Cu] IRPLSAGFWHCJIQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 2
- 239000002064 nanoplatelet Substances 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims description 2
- FBGGJHZVZAAUKJ-UHFFFAOYSA-N bismuth selenide Chemical compound [Se-2].[Se-2].[Se-2].[Bi+3].[Bi+3] FBGGJHZVZAAUKJ-UHFFFAOYSA-N 0.000 claims 3
- 239000002055 nanoplate Substances 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 description 24
- OMEPJWROJCQMMU-UHFFFAOYSA-N selanylidenebismuth;selenium Chemical compound [Se].[Bi]=[Se].[Bi]=[Se] OMEPJWROJCQMMU-UHFFFAOYSA-N 0.000 description 15
- 230000005641 tunneling Effects 0.000 description 15
- 238000002844 melting Methods 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000004907 flux Effects 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 239000010445 mica Substances 0.000 description 7
- 229910052618 mica group Inorganic materials 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 238000011144 upstream manufacturing Methods 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000000089 atomic force micrograph Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
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- 238000000879 optical micrograph Methods 0.000 description 3
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- 238000010900 secondary nucleation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- ZZEMEJKDTZOXOI-UHFFFAOYSA-N digallium;selenium(2-) Chemical compound [Ga+3].[Ga+3].[Se-2].[Se-2].[Se-2] ZZEMEJKDTZOXOI-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000005619 thermoelectricity Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- JMMCWGSOHCBMNQ-UHFFFAOYSA-N [O].[Se].[Cu].[Bi] Chemical compound [O].[Se].[Cu].[Bi] JMMCWGSOHCBMNQ-UHFFFAOYSA-N 0.000 description 1
- CTNCAPKYOBYQCX-UHFFFAOYSA-N [P].[As] Chemical compound [P].[As] CTNCAPKYOBYQCX-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 239000011888 foil Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 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
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
Abstract
The invention discloses a two-dimensional BiCuSeO nanosheet, a preparation method thereof and a semiconductor device, wherein the preparation method comprises the following steps: providing a reaction device, wherein the reaction device comprises a low-pressure reaction chamber, and the reaction chamber is provided with a first area and a second area which are sequentially arranged at intervals; placing a selenium-containing precursor in a first area, and placing a copper-containing precursor and an oxygen-containing precursor in a second area; the growth substrate is placed in the two areas and is reversely buckled above the copper-containing precursor and the oxygen-containing precursor; and (4) performing heat treatment, namely evaporating and reacting the selenium-containing precursor, the copper-containing precursor and the oxygen-containing precursor, and obtaining the BiCuSeO nano sheet on the surface of the growth substrate. The invention realizes the preparation of the two-dimensional BiCuOSe nanosheet with the minimum thickness of 7.6nm and the maximum transverse dimension of 270 mu m by a Chemical Vapor Deposition (CVD) method.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a two-dimensional BiCuSeO nanosheet, a preparation method thereof and a semiconductor device.
Background
Due to the rapidly evolving demands of microelectronics, the size of conventional silicon-based transistors is continuously shrinking following moore's law. As transistors shrink to their physical limits, a series of problems develop, such as the power consumption of the devices increasing significantly. In order to reduce the power consumption of a CMOS transistor, one effective method is to reduce the applied voltage when the transistor is turned from an off state to an on state. The minimum value of this applied voltage is determined by the size of the thermionic barrier across the source when carriers are injected into the channel. Thus, for a conventional transistor, the minimum value of the sub-threshold swing (SS) at room temperature is 60mV/dec, i.e., the Boltzmann limit. Due to the boltzmann limit, the power consumption of the integrated circuit is greatly increased, reducing the performance (on-state current and on-off ratio) of the transistor. To make the SS of the transistor less than 60mV/dec, two common approaches are to utilize a heterojunction-based tunneling transistor (T-FET) and a ferroelectric gate-based negative capacitance transistor (NC-FET). Different from the common MOSFET which crosses a potential barrier to form current by means of carrier thermal injection, the tunneling transistor for realizing carrier transportation based on band-band tunneling is not limited by the Boltzmann limit, and has the advantages of low subthreshold swing and high on-off ratio. For a T-FET, the realization of a tunneling effect needs to regulate and control a Fermi level through a grid voltage, and a traditional semiconductor transistor has an obvious Fermi pinning effect due to factors such as doping, interface defects and the like, so that the regulation and control of the grid voltage on the concentration of carriers are limited. Therefore, it is difficult to realize a conventional semiconductor transistor having an SS value lower than 60mV/dec and a high on-off ratio at room temperature. Compared with the traditional semiconductor material, the two-dimensional material has the unique advantages of thickness of atomic level, natural dangling bond-free interface, ultrahigh mobility, no influence of lattice mismatch on stacking and the like. In recent years, a tunneling transistor with low power consumption and high switching ratio based on a two-dimensional material 2D-2D heterojunction and a 3D-2D composite structure is gradually a hot spot of research.
So far, there are many reports based on various two-dimensional material heterojunction tunneling transistors. However, for a 2D-2D tunneling transistor formed by a heterojunction built in a two-dimensional material, although the SS value can be reduced to a certain extent, it is still difficult to break through the boltzmann limit at room temperature. And there are two possible reasons for this.
First, there is a shortage of p-type two-dimensional material. So far, the most common carrier types of two-dimensional materials are electrons, the p-type two-dimensional materials are rarely selected, and the p-type two-dimensional materials commonly used for experimental research comprise black phosphorus(BP), black arsenic phosphorus (b-AsP), tellurium (Te), gallium selenide (GaSe), and some bipolar two-dimensional materials WSe 2 、MoTe 2 And so on, to a limited extent. Moreover, most of the materials are unstable in air (such as BP), and great limitation is brought to the construction of heterojunction for realizing tunneling by energy band matching.
Second, the two-dimensional material itself is generally low in carrier concentration and difficult to dope. The two-dimensional material of the atomic layer thickness makes it difficult to controllably optimize the carrier concentration and type by modulation doping as in conventional semiconductors. Controllable doping of two-dimensional materials has been one of the limiting factors for their widespread use. Although the two-dimensional material can be adjusted to some extent by applying a gate voltage, the carrier concentration of the two-dimensional material itself is low (less than 10) 18 cm -3 ) It is difficult to realize heavy doping by gate voltage regulation. And due to the limitation of the carrier concentration, a high electric field is difficult to form between the channel and the source and the drain of the tunneling heterojunction, and the probability of carrier tunneling into the channel is reduced.
The method is characterized in that a p-type two-dimensional material with intrinsic heavy doping is searched by combining the factors, and the method is very important for constructing a 2D-2D heterojunction tunneling transistor and realizing the preparation of a low-SS and high-on-off ratio tunneling transistor device. BiCuSeO is a thermoelectric material with excellent performance, and the appropriate energy band gap (0.4-0.9 eV), intrinsic p-type heavy doping and stable chemical properties provide possibility for the construction of a 2D-2D heterojunction tunneling transistor. So far, biCuSeO can mostly prepare single crystal blocks only by a solid-phase reaction method and a fluxing agent method. However, due to the electrostatic force existing between atomic layers of BiCuSeO itself, it is difficult to obtain a nanosheet with a single atomic layer or several atomic layers by mechanical exfoliation like graphene. Although BiCuSeO can obtain nanosheets with thicknesses of only a few atomic layers through a solution method, the nanosheets are small in lateral size (smaller than 1 μm), random and irregular in shape, and cannot meet the requirements of a semiconductor device preparation process.
Disclosure of Invention
The invention aims to provide a two-dimensional BiCuSeO nanosheet, a preparation method thereof and a semiconductor device, which can solve the problems of small transverse size and random and irregular shape in the prior art.
In order to achieve the above object, an embodiment of the present invention further provides a preparation method of a two-dimensional BiCuSeO nanosheet, including:
providing a reaction device, wherein the reaction device comprises a low-pressure reaction chamber, and the reaction chamber is provided with a first area and a second area which are sequentially arranged at intervals;
placing a selenium-containing precursor in a first area, placing a copper-containing precursor, an oxygen-containing precursor and a growth substrate in a second area, and inversely covering the growth substrate above the copper-containing precursor and the oxygen-containing precursor;
and (4) performing heat treatment, namely evaporating and reacting the selenium-containing precursor, the copper-containing precursor and the oxygen-containing precursor, and obtaining the BiCuSeO nano sheet on the surface of the growth substrate.
In one or more embodiments of the present invention, the selenium-containing precursor is selected from one or more of bismuth selenide, copper selenide, elemental selenium powder, or elemental selenium bulk; the oxygen-containing precursor is selected from one or more of bismuth oxide and copper oxide; the copper-containing precursor is selected from one or more of copper oxide, copper selenide, elemental copper powder and elemental copper foil.
In one or more embodiments of the present invention, the selenium-containing precursor is bismuth selenide, the copper-containing precursor is copper powder, and the oxygen-containing precursor is bismuth oxide.
In one or more embodiments of the invention, the mass ratio of copper, bismuth selenide and bismuth oxide is 1 (10-50) to (50-100).
In one or more embodiments of the present invention, the present invention further includes a flux disposed in the second region, wherein the flux is one or more of potassium chloride, sodium chloride, and copper chloride.
In one or more embodiments of the invention, the distance between the first and second regions is from 5cm to 15cm.
In one or more embodiments of the present invention, the heat treatment includes: heating to 600-720 ℃ within 20-30 min, and keeping the temperature for 5-30 min.
In one or more embodiments of the invention, the vaporized precursor is delivered to the growth substrate during the heat treatment by continuously flowing 50-150sccm of inert gas.
In order to achieve the above object, an embodiment of the present invention further provides a two-dimensional BiCuSeO nanosheet, which is prepared by the preparation method, and the thickness of the nanosheet is 7.6nm to 100nm; the lateral dimension is 5 μm to 270 μm.
In order to achieve the above object, an embodiment of the present invention further provides a semiconductor device, including the two-dimensional BiCuSeO nanosheet.
Compared with the prior art, the preparation method disclosed by the invention realizes the preparation of the two-dimensional BiCuOSe nanosheet with the minimum thickness of 7.6nm and the maximum transverse dimension of 270 mu m by a simple Chemical Vapor Deposition (CVD) method. And the characteristic of intrinsic p-type heavy doping is verified. The method has important significance for the preparation and research of semiconductor devices in the future.
Drawings
FIG. 1 is a schematic view of a reaction apparatus according to an embodiment of the present invention;
fig. 2a and b show an optical microscope image of a two-dimensional BiCuSeO nanosheet and its corresponding Atomic Force Microscope (AFM) image provided in embodiment 1 of the present invention, fig. 2c and d show an optical microscope image of a two-dimensional BiCuSeO nanosheet and its corresponding Atomic Force Microscope (AFM) image provided in embodiment 2 of the present invention, and fig. 2e and f show an optical microscope image of a two-dimensional BiCuSeO nanosheet and its corresponding Atomic Force Microscope (AFM) image provided in embodiment 3 of the present invention;
fig. 3 shows a Scanning Electron Microscope (SEM) image of a two-dimensional bicusseo nanosheet provided in example 1 of the present invention;
fig. 4 shows a spherical aberration electron microscope (STEM) atomic image and an element distribution scan (mapping) map of a two-dimensional bicusseo nanosheet provided in embodiment 1 of the present invention, wherein a is a low-power high-angle annular dark field image of the bicusseo nanosheet, b is a high-power high-angle annular dark field image, and c-f are distribution scan maps of Bi, cu, se, and O elements in the bicusseo nanosheet, respectively;
FIG. 5 is an elemental analysis chart of a two-dimensional BiCuSeO nanosheet in example 1 of the present invention;
fig. 6 shows an X-ray diffraction (XRD) pattern of a two-dimensional BiCuSeO nanosheet provided in example 3 of the present invention;
fig. 7 a shows a test chart of lateral resistance of a two-dimensional bicuiseo nanosheet hall device provided in embodiment 1 of the present invention changing with a magnetic field, fig. 7b shows a test chart of resistance of a corresponding hall device changing with a changing temperature, and fig. 7 c shows a fourier infrared spectroscopy (FTIR) test chart of the two-dimensional bicuiseo nanosheet provided in embodiment 3.
Detailed Description
The solid-phase reaction method is the most common method for preparing BiCuSeO (copper bismuth selenide oxide) at present, but the reaction period is long, the obtained product is impure and easy to generate impurities, only bulk materials with uncontrollable appearance can be synthesized, and a two-dimensional BiCuSeO nanosheet cannot be obtained. The flux method can obtain pure-phase BiCuSeO bulk materials, but cannot obtain two-dimensional nanosheets with the thickness of less than 100 nm. The BiCuSeO nanosheet can be obtained by a solution method, but the BiCuSeO nanosheet is small in transverse size (smaller than 1 mu m), and the shape of the obtained nanosheet is not controllable, so that the BiCuSeO nanosheet cannot be used for preparation and related research of semiconductor devices.
In order to solve the technical problem, the invention provides a preparation method of a two-dimensional BiCuSeO nanosheet, which comprises the steps of placing a growth substrate and a precursor in a quartz tube by a Chemical Vapor Deposition (CVD) growth method, and vacuumizing to synthesize the two-dimensional BiCuSeO nanosheet under a low-pressure condition. The low-melting-point selenium source is placed at the upstream of the tube furnace, the high-melting-point copper source and the oxygen source are placed at the center of the tube furnace, the mica substrate is reversely buckled on the high-melting-point source, and inert gas is introduced to convey the precursor. And then heating the tube furnace to a certain temperature, preserving the temperature, evaporating the precursor, reacting to generate BiCuSeO, and depositing, nucleating and epitaxially growing on a growth substrate to form a two-dimensional BiCuSeO nanosheet. The preparation method provided by the embodiment of the invention has the advantages of low raw material price, low production equipment cost, simplicity and safety in operation, high controllability and strong repeatability, and the obtained BiCuSeO nanosheets are uniform and controllable in thickness, are suitable for large-area production of two-dimensional BiCuSeO, and meet research requirements and industrialization requirements in practical application.
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations such as "comprises" or "comprising", etc., will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
A two-dimensional BiCuSeO nanosheet according to a preferred embodiment of the present invention, having a thickness of from 7.6nm to 100nm, preferably from 7.6nm to 50nm; the lateral dimension is 5 μm to 270 μm.
In the technical scheme, the thickness of the two-dimensional nanosheet is less than 100nm, the transverse size of the two-dimensional nanosheet is greater than 5 microns, the two-dimensional nanosheet can be used for preparing a semiconductor device, and particularly the two-dimensional nanosheet is of great importance for constructing a 2D-2D heterojunction (heterojunction formed by stacking two-dimensional materials and two-dimensional materials) tunneling transistor and realizing the preparation of a tunneling transistor device with low SS (sub-threshold swing) and high on-off ratio.
The embodiment of the invention also provides a preparation method of the two-dimensional BiCuSeO nanosheet, which comprises the following steps:
referring to fig. 1, a reaction device 100 is provided, where the reaction device 100 includes a low-pressure reaction chamber 11, and the reaction chamber 11 has a first region 111 and a second region 112 arranged at intervals in sequence;
placing a selenium-containing precursor 12 in a first region 111, placing a copper-containing precursor and an oxygen-containing precursor 13, and placing a growth substrate 14 in a second region 112, wherein the growth substrate 14 is inverted over the copper-containing precursor and the oxygen-containing precursor 13;
and (4) performing heat treatment, namely evaporating and reacting the selenium-containing precursor 12, the copper-containing precursor and the oxygen-containing precursor 13, and obtaining the BiCuSeO nanosheet on the surface of the growth substrate 14.
In the embodiment, the two-dimensional BiCuSeO single crystal nanosheet with controllable thickness and size is successfully prepared by a simple Chemical Vapor Deposition (CVD) method, and the method can be widely applied to the related fields of thermoelectricity, semiconductor devices and the like. Compared with the prior art, the chemical vapor deposition method has the advantages of simple operation, safe raw materials, simple equipment, low cost, good repeatability, high crystallinity, high quality, smooth surface, uniform thickness and the like.
In an actual manufacturing process, the "low-pressure reaction chamber" may be an inner cavity of a quartz tube for heating reaction, which is directly placed in a heating cavity of a heating device, such as a tube furnace.
It should be noted that the vacuum-tight reaction chamber includes, but is not limited to, the above-described implementation manner, and may be any growth apparatus or growth container of a vacuum-tight reaction chamber capable of implementing the two-dimensional BiCuSeO nanosheet growth.
In some embodiments, the selenium-containing precursor includes, but is not limited to, one or more of bismuth selenide, copper selenide, and the like, or even elemental selenium powder (bulk), which can be thermally decomposed to produce selenium.
In some embodiments, the oxygen-containing precursor includes, but is not limited to, one or more of bismuth oxide, copper oxide, and the like, which can be thermally decomposed to generate oxygen.
In some embodiments, the copper-containing precursor includes, but is not limited to, copper oxide, copper selenide, and one or more of the compounds that can decompose to form copper upon heating, and even elemental copper powder (foil).
In some embodiments, the growth substrate may include, but is not limited to, a silicon dioxide sheet, a fluorophlogopite sheet, a quartz sheet, a sapphire sheet, and the like.
In a specific embodiment, the selenium-containing precursor is bismuth selenide, the copper-containing precursor is copper powder, and the oxygen-containing precursor is bismuth oxide. In the embodiment, the mass ratio of the copper to the bismuth selenide to the bismuth oxide is 1 (10-50) to 50-100.
In some embodiments, the flux is disposed in the second region, and the flux includes, but is not limited to, any one or more of low melting point chlorides such as potassium chloride, sodium chloride, copper chloride, and the like.
In some embodiments, the distance between the first region and the second region is 5cm-15cm. The temperature difference between the first zone and the second zone is in the range of 50-200 ℃. When the distance is too small, the selenium source temperature is high, the evaporation amount is large, and other products such as Cu are easily generated 2 And (5) Se. If the distance is too far, the temperature of the selenium source is low, the evaporation capacity is too small, and the BiCuSeO cannot be generated due to insufficient selenium source.
The second area is located in a temperature area with higher temperature in the vacuum-sealed reaction chamber, and the first area is located in a temperature area with lower temperature in the vacuum-sealed reaction chamber. The temperature in the direction from the second region to the first region varies in a gradient, i.e. the temperature in the second region > the temperature in the first region.
In some embodiments, the heat treating comprises: heating to 600-720 ℃ within 20-30 min, and keeping the temperature for 5-30 min.
In some embodiments, the vaporized precursor is delivered to the growth substrate during the thermal treatment by continuously flowing 50-150sccm of an inert gas. Transport inert gases include, but are not limited to, argon, nitrogen, and the like.
The embodiment of the invention also provides a semiconductor device which comprises the two-dimensional BiCuSeO nanosheet or the two-dimensional BiCuSeO nanosheet prepared by the method. In one embodiment, the semiconductor device may be a transistor.
Example 1
Selecting a plurality of pieces of clean mica as growth substrates for later use. Selecting bismuth selenide (Bi) 2 Se 3 ) As a selenium source, bismuth oxide (Bi) 2 O 3 ) As an oxygen source, copper oxide (CuO) was used as a copper source, and potassium chloride (KCl) was used as a flux. The mass ratio of the copper oxide to the bismuth selenide to the bismuth oxide is 1.
The low melting point bismuth selenide is placed at the upstream of the tube furnace (10 cm from the center), the high melting point copper oxide, bismuth oxide and potassium chloride are placed at the center of the tube furnace, and the mica substrate is reversely buckled on the high melting point source. And opening a vacuum pump to vacuumize to below 1Pa, and repeatedly introducing 100-200sccm argon gas to carry out gas washing so as to remove oxygen in the quartz tube.
And (3) raising the temperature of the tubular furnace to 660 ℃ within 25min, keeping the temperature for 10min after raising the maximum temperature, and naturally cooling to room temperature. In the whole process of temperature rise, heat preservation and cooling, 100sccm argon is continuously introduced to be used as transport and protective gas.
The two-dimensional BiCuSeO nanosheet obtained in the embodiment is shown in FIG. 2a, the nanosheet is rectangular, and the maximum transverse size can reach 84 μm; FIG. 2b is a corresponding AFM characterization, with a thickness of 7.6nm.
Fig. 3 is an SEM representation of the two-dimensional BiCuSeO nanosheet obtained in this example, and it can be seen that the surface thereof is uniform and has no significant secondary nucleation.
Fig. 4 and fig. 5 are spherical aberration electron microscope representations of the two-dimensional bicusseo nanosheets obtained in this example, which illustrate the high quality and high crystallinity (no obvious defect) of the two-dimensional nanosheets, and the two-dimensional nanosheets contain Bi, cu, se and O and are uniformly distributed.
The two-dimensional BiCuSeO nanosheet obtained by the implementation case is large in transverse size, thin and uniform in thickness, and free of obvious secondary nucleation on the surface, and a material foundation is laid for the preparation of the Hall device. Therefore, the hall device test based on this embodiment is as shown in fig. 7 a, b: in fig. 7, a illustrates that the carrier type of the two-dimensional BiCuSeO nanosheet obtained by the present invention is a hole; in fig. 7, b indicates that the BiCuSeO nanosheet resistance increases with increasing temperature, and becomes metallic.
Example 2
Selecting a plurality of pieces of clean mica as growth substrates for standby. Selecting bismuth selenide (Bi) 2 Se 3 ) As a selenium source, bismuth oxide (Bi) 2 O 3 ) As an oxygen source, copper powder (Cu) was used as a copper source, and potassium chloride (KCl) was used as a flux. The mass ratio of the copper powder to the bismuth selenide to the bismuth oxide is 1.
The low-melting point bismuth selenide is placed at the upstream of the tube furnace (15 cm away from the center), the high-melting point copper powder, bismuth oxide and potassium chloride are placed at the center of the tube furnace, the mica substrate is reversely buckled on the high-melting point source, and 100-200sccm argon is repeatedly introduced for gas scrubbing to remove oxygen in the quartz tube.
And (3) heating the tube furnace to 700 ℃ within 25min, keeping the temperature for 30min after the maximum temperature is raised, and naturally cooling to room temperature. In the whole process of temperature rise, heat preservation and cooling, 100sccm argon is continuously introduced to be used as transport and protective gas.
The two-dimensional BiCuSeO nanosheet obtained in this embodiment is shown in fig. 2 c. Due to the higher temperature of the embodiment, the nano-sheet with the transverse dimension of 277 mu m can be obtained. Meanwhile, the excessively evaporated precursor can further react and deposit on the nanosheet, so that obvious secondary nucleation and growth exist on the nanosheet, and the edge of the nanosheet has a phenomenon of laminated growth. Figure 2d is a corresponding AFM characterization, illustrating that the thickness of the nanoplatelets is 17.4nm.
Example 3
Selecting a plurality of pieces of clean mica as growth substrates for later use. Selecting bismuth selenide (Bi) 2 Se 3 ) As a selenium source, bismuth oxide (Bi) 2 O 3 ) As an oxygen source, copper powder (Cu) was used as a copper source, and potassium chloride (KCl) was used as a flux. The mass ratio of the copper powder to the bismuth selenide to the bismuth oxide is 1.
The low melting point bismuth selenide is placed at the upstream of the tube furnace (5 cm away from the center), the high melting point copper, bismuth oxide and potassium chloride are placed at the center of the tube furnace, and the mica substrate is reversely buckled on the high melting point source. And opening a vacuum pump to vacuumize to below 1Pa, and repeatedly introducing 100-200sccm argon gas to carry out gas washing so as to remove oxygen in the quartz tube.
And (3) heating the tubular furnace to 620 ℃ within 25min, keeping the temperature for 10min after the temperature is raised to the highest temperature, and naturally cooling to room temperature. During the whole process of temperature rise, heat preservation and cooling, 100sccm argon is continuously introduced as transport and protective gas.
The two-dimensional BiCuSeO nanosheet obtained by the embodiment and AFM characterization thereof are shown in FIGS. 2e and 2 f. The relative content of the copper source is higher, so that the nucleation density is increased; the growth temperature of the system is low, the transverse transportation of the precursor on the substrate is limited, and only a sample with high nucleation density, transverse size smaller than 20 mu m and thickness larger than 50nm can be obtained. High density nucleation growth provides conditions for testing XRD and FTIR: as shown in fig. 6, the two-dimensional BiCuSeO nanosheet obtained in this example is illustrated, and its exposed crystal plane is the (100) crystal plane family; as shown in c in fig. 7, FTIR test gave a band gap of 0.45eV for BiCuSeO nanosheets. The test results of the hall devices a and 7b in fig. 7 of example 1 are combined to demonstrate that the synthesized two-dimensional BiCuSeO nanosheet is a p-type heavily doped semiconductor.
In summary, the embodiment of the invention successfully prepares the two-dimensional BiCuSeO single crystal nanosheet with controllable thickness and size by a simple Chemical Vapor Deposition (CVD) method, and the two-dimensional BiCuSeO single crystal nanosheet can be widely applied to the related fields of thermoelectricity, semiconductor devices and the like. The chemical vapor deposition method has the advantages of simple operation, safe raw materials, simple equipment, low cost and good repeatability, and the prepared nanosheet has the advantages of high crystallinity, high quality, smooth surface, uniform thickness and the like.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (6)
1. A preparation method of a two-dimensional BiCuSeO nanosheet is characterized by comprising the following steps:
providing a reaction device, wherein the reaction device comprises a low-pressure reaction chamber, the reaction chamber is provided with a first area and a second area which are sequentially arranged at intervals, and the distance between the first area and the second area is 5cm-15cm;
placing a selenium-containing precursor in a first region, placing a copper-containing precursor, an oxygen-containing precursor and a growth substrate in a second region, and reversely covering the growth substrate above the copper-containing precursor and the oxygen-containing precursor, wherein the selenium-containing precursor is selected from one or more of bismuth selenide, copper selenide, elemental selenium powder or elemental selenium block, the oxygen-containing precursor is selected from one or more of bismuth oxide and copper oxide, the copper-containing precursor is selected from one or more of copper oxide, copper selenide, elemental copper powder and elemental copper foil, and the growth substrate also comprises a fluxing agent, the fluxing agent is arranged in the second region, and the fluxing agent is one or more of potassium chloride, sodium chloride and copper chloride;
placing the reaction device in a tubular furnace, starting a vacuum pump to vacuumize to below 1Pa, and introducing 100-200sccm argon gas to wash gas so as to remove oxygen in the reaction device;
and (3) performing heat treatment, namely evaporating and reacting the selenium-containing precursor, the copper-containing precursor and the oxygen-containing precursor, and obtaining the BiCuSeO nanosheet on the surface of the growth substrate, wherein the temperature of the second region is higher than that of the first region, the temperature difference range of the first region and the second region is 50-200 ℃, in the heat treatment process, 50-150sccm inert gas is continuously introduced, and the evaporated precursor is conveyed to the growth substrate.
2. The method of making two-dimensional BiCuSeO nanosheets of claim 1, wherein the selenium-containing precursor is bismuth selenide, the copper-containing precursor is copper powder, and the oxygen-containing precursor is bismuth oxide.
3. The preparation method of the two-dimensional BiCuSeO nanosheet as defined in claim 2, wherein the mass ratio of the copper to the bismuth selenide to the bismuth oxide is 1 (10-50) to (50-100).
4. A method of making two-dimensional BiCuSeO nanoplates as in claim 1, wherein the thermal treatment comprises: heating to 600-720 ℃ within 20-30 min, and keeping the temperature for 5-30 min.
5. Two-dimensional BiCuSeO nanoplatelets produced by the method of production according to any one of claims 1 to 4, having a thickness of 7.6nm to 100nm and a transverse dimension of 5 μm to 270 μm.
6. A semiconductor device comprising the two-dimensional BiCuSeO nanosheet of claim 5.
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