CN114373828A - Method for heterointegration of single-crystal two-dimensional semiconductor molybdenum telluride film and random lattice mismatch single crystal substrate - Google Patents

Method for heterointegration of single-crystal two-dimensional semiconductor molybdenum telluride film and random lattice mismatch single crystal substrate Download PDF

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CN114373828A
CN114373828A CN202110370754.6A CN202110370754A CN114373828A CN 114373828 A CN114373828 A CN 114373828A CN 202110370754 A CN202110370754 A CN 202110370754A CN 114373828 A CN114373828 A CN 114373828A
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single crystal
film
crystal substrate
molybdenum
molybdenum telluride
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潘宇
徐晓龙
李艳平
叶堉
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Peking University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/0237—Materials
    • H01L21/02373—Group 14 semiconducting materials
    • H01L21/02381—Silicon, silicon germanium, germanium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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    • H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
    • H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by at least one potential-jump barrier or surface barrier, e.g. phototransistors
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    • H01L31/102—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier or surface barrier
    • H01L31/109—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier or surface barrier the potential barrier being of the PN heterojunction type
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Abstract

The invention discloses a method for heterointegration of a single-crystal two-dimensional semiconductor molybdenum telluride film and an arbitrary lattice mismatch single-crystal substrate. The invention breaks through the necessary condition of heterogeneous integration of different single crystal materials in the traditional epitaxial process, namely lattice matching, and utilizes the 2H-MoTe prepared by the chemical vapor deposition method2The method has a special growth mechanism of lateral epitaxial phase change, and enables the single-crystal two-dimensional semiconductor molybdenum telluride film to be directly grown and integrated with any single-crystal substrate without the limitation of lattice matching by controlling the temperature and time. The heterogeneous integrated structure obtained by the method can simultaneously utilize the semiconductor characteristics of molybdenum telluride and the physical characteristics of a substrate, and improve the performance of the deviceAnd enhanced device functionalization. The method is suitable for large-area preparation, can realize the preparation of integrated photoelectric device arrays, provides a foundation for realizing wafer-level and industrialized chip manufacture, and provides a foundation for the application of two-dimensional semiconductor materials in the aspects of integrated circuits and photoelectric chips.

Description

Method for heterointegration of single-crystal two-dimensional semiconductor molybdenum telluride film and random lattice mismatch single crystal substrate
Technical Field
The invention relates to the field of semiconductors, in particular to a method for preparing a two-dimensional semiconductor material film on a single crystal substrate with highly mismatched lattice structures by large-area epitaxy.
Background
In order to expand the functions of chips or improve the performance thereof, the semiconductor industry and related research fields need to heterointegrate high-quality single crystal materials with different physical properties into chips. Epitaxial technology has been developed for many semiconductors as a mature, high quality crystal growth method, and is widely used in silicon-based semiconductor manufacturing processes, such as bipolar heterojunction transistors and advanced Complementary Metal Oxide Semiconductors (CMOS). Epitaxy is also particularly important for compound semiconductors, such as the realization of two-dimensional electron gases (2DEG) in the gallium arsenide system. However, the integration of different kinds of single crystal materials by heteroepitaxy is limited by lattice matching in the same chip, and only two kinds of single crystal materials with similar lattice structures and lattice constants can be subjected to epitaxial growth, or a buffer layer is added between a substrate and an epitaxial layer to realize heterointegration, but the buffer layer has high technical cost and complex process. Thus, the limitation of lattice matching results in many single crystal materials not being integrated together by heteroepitaxy, thereby hindering the development of related devices.
The two-dimensional layered semiconductor phase molybdenum telluride thin film has many special physical characteristics, including a vdW interface between layers and no dangling bond on the surface, and a carrier has a quantum confinement effect when being transmitted in the layer, so that the scattering of the surface carrier and the defect state of a heterogeneous interface are reduced; the material has a narrow band gap structure (about 1eV), and is suitable for near-infrared photoelectric devices; the molybdenum telluride film can be grown and prepared on a large scale and at a wafer level, is beneficial to being compatible with the traditional mature semiconductor technology, and has practical and commercial prospects.
Disclosure of Invention
Aiming at the problems of the heteroepitaxy technology, the invention provides a method for preparing a monocrystalline material heteroepitaxy growth of a monocrystalline two-dimensional semiconductor molybdenum telluride film mismatched with other lattice structures in a large area.
The invention discloses a research hairTwo-dimensional semiconductor molybdenum telluride thin film (2H-MoTe) prepared by Chemical Vapor Deposition (CVD) method2) The method has a special growth mechanism of lateral epitaxial phase transition, by which a large-area single-crystal semiconductor molybdenum telluride film can be grown by controlling temperature and time, and the single-crystal semiconductor molybdenum telluride film grown by the method can be integrated with single-crystal materials of any lattice structure without the limitation of lattice matching.
Based on the discovery, the invention provides a method for heterointegration of a single-crystal two-dimensional semiconductor molybdenum telluride film and any lattice mismatch single-crystal substrate, which comprises the following steps:
(1) depositing a layer of molybdenum film with the thickness of 1-5nm on the surface of any single crystal substrate;
(2) putting the sample with the molybdenum film into a furnace, adding a tellurium simple substance (Te source), pretreating the molybdenum film by a chemical vapor deposition method, and forming a metal phase molybdenum telluride film (1T' -MoTe) on a single crystal substrate2)；
(3) 1T' -MoTe2Putting into a furnace together with Te source for chemical vapor deposition, heating at high temperature to promote 1T' -MoTe2Appearance of 2H-MoTe in thin films2Nucleation centers and, with increasing heating time, 2H-MoTe2Domain along 2H-MoTe2And 1T' -MoTe2The interface is gradually extended outwards in the plane for phase change growth to finally form 2H-MoTe2And the film and the single crystal substrate are in a heterogeneous integrated structure.
The three-dimensional single crystal substrate silicon, gallium nitride, sapphire, quartz, silicon carbide and other single crystal substrates can be selected as the single crystal substrate in the step (1).
The method for depositing the molybdenum film on the single crystal substrate in the step (1) can be a magnetron sputtering method, an electron beam thermal evaporation method or an atomic layer deposition method.
And (3) putting the single crystal substrate with the molybdenum film grown on the surface and a proper amount of Te source (powder or particles) into a quartz boat, and putting the quartz boat into the furnace for chemical vapor deposition, wherein the furnace in the step (2) is a normal-pressure tube furnace or a box furnace.
The temperature for the chemical vapor deposition in the step (2) is controlled to 49The temperature is 0-510 ℃ and the time is 5-20 min, and the polycrystal 1T' -MoTe is obtained2A film.
And (4) controlling the temperature of the chemical vapor deposition in the step (3) to be 600-700 ℃ and the time to be 1-3 h to obtain the monocrystalline two-dimensional semiconductor molybdenum telluride film. In this step, the two-dimensional semiconductor molybdenum telluride film is laterally phase-change epitaxially grown from a nucleation center, so that the crystal lattice orientation of the film is consistent with that of the nucleation center, and the single crystallinity is maintained. Furthermore, since the growth of the single-crystal two-dimensional semiconductor molybdenum telluride thin film is confined within the pre-grown 1T' -phase molybdenum telluride thin film, it is not affected by the lattice structure of the single-crystal substrate from the vertical direction.
The steps (2) and (3) can also be continuously carried out, the single crystal substrate sample with the molybdenum film deposited on the surface and the Te source are put into a furnace, and then the furnace is directly heated from the room temperature environment to 600-700 ℃ (the heating rate is generally within the range of 20-40 ℃/min, preferably 30 ℃/min) to form 2H-MoTe2And the film and the single crystal substrate are in a heterogeneous integrated structure.
Further, the two-dimensional semiconductor phase molybdenum telluride film obtained in the step (3) and a heterogeneous integrated sample of a three-dimensional single crystal substrate are subjected to device design and process processing, so that a functional photoelectric device array can be prepared. If other three-dimensional single crystal materials with special physical properties are replaced and integrated with the two-dimensional semiconductor molybdenum telluride, the functional types of the device can be expanded, and the performance of the device can be improved.
The advantages of the invention are as follows:
the method of the invention breaks through the necessary conditions of heterogeneous integration of different types of single crystal materials in the traditional epitaxial process: lattice matching.
Due to lattice mismatch among different single crystal materials, some single crystal materials and traditional semiconductor materials (such as silicon, gallium nitride and silicon carbide) cannot be heterointegrated directly through epitaxial growth, and the special growth mechanism of the epitaxial semiconductor molybdenum telluride film in the plane by utilizing the phase change technology enables the single crystal molybdenum telluride film to be integrated with any single crystal substrate directly without the limitation of lattice matching. Meanwhile, the performance of the device can be improved and the device functionalization can be enhanced by utilizing the semiconductor characteristics of the molybdenum telluride and the physical characteristics of the substrate. The method is suitable for large-area preparation, can realize the preparation of an integrated photoelectric device array, provides a foundation for realizing wafer-level and industrialized chip manufacture, and provides a foundation for the application of two-dimensional semiconductor materials in the aspects of integrated circuits and photoelectric chips.
Drawings
FIG. 1 is a schematic diagram of a method of growing a semiconductor phase molybdenum telluride and a metal phase molybdenum telluride by chemical vapor deposition in an embodiment of the present invention, wherein: 1-tube furnace, 2-quartz tube, 3-quartz boat, 4-tellurium powder, 5-monocrystalline silicon substrate;
FIG. 2 shows a schematic growth mechanism (a), an optical micrograph (b), a Raman spectrum characterization image (c) and an electron back-scattering diffraction mapping spectrum (d, e) of the sample in step (3) of the example of the present invention, in which 1T 'represents a metal phase molybdenum telluride thin film (1T' -MoTe)2) And 2H denotes a semiconductor phase molybdenum telluride thin film (2H-MoTe)2)。
FIG. 3 shows a pn junction device structure design (a) of a p-type semiconductor phase molybdenum telluride thin film and an n-type single crystal silicon substrate, an optical micrograph (b) of a device array and a current-voltage performance curve (c) of 20 devices in an embodiment of the present invention.
Detailed Description
The invention will be further elucidated by means of specific embodiments in the following with reference to the drawing.
In the embodiment, the pn junction device formed by heterogeneously integrating the two-dimensional semiconductor molybdenum telluride thin film and various lattice mismatch three-dimensional single crystal materials is prepared by the following steps:
(1) a three-dimensional single crystal substrate material is prepared, in order to show the advantage that a two-dimensional single crystal semiconductor molybdenum telluride film can be directly grown on a single crystal material with lattice structure mismatching, a single crystal silicon material different from the molybdenum telluride film (hexagonal lattice structure) is selected as a substrate (cubic lattice structure), and the crystal face is [001 ]. The semiconductor molybdenum telluride has a lattice constant a-b of 0.352nm and the single crystal silicon has a lattice constant a-b of 0.543nm, with a 35% lattice mismatch.
(2) A layer of molybdenum film with the thickness of about 2nm is evaporated on a monocrystalline silicon substrate by a magnetron sputtering method.
(3) Referring to fig. 1, tellurium powder 4 and a single crystal silicon substrate 5 on which a molybdenum thin film is evaporated are placed in a quartz boat 3, and then placed in a quartz tube 2 of a tube furnace 1. After 20min of temperature rise, the tubular furnace temperature zone is heated to 700 ℃, the temperature is naturally reduced after 2h of temperature rise, and the gas flow of 7sccm hydrogen and 5sccm argon is kept in the period. The growth mechanism of the two-dimensional single-crystal semiconductor molybdenum telluride thin film is shown in a diagram in FIG. 2, when 2H MoTe appears in the thin film2After the nucleation center, tellurium atoms are continuously supplemented, and the two-dimensional single crystal semiconductor molybdenum telluride film is transversely and epitaxially grown, and the atomic structure of the two-dimensional single crystal semiconductor molybdenum telluride film keeps the same single crystallinity as the nucleation center. A circular single crystal semiconductor molybdenum telluride thin film of about 2.5mm in diameter was obtained on a single crystal silicon substrate by this method, as shown in the b-diagram in FIG. 2.
(4) And performing Raman spectrum and EBSD crystal lattice orientation characterization on the grown single crystal semiconductor molybdenum telluride film. As shown in the c diagram in FIG. 2, it was confirmed that a semiconductor molybdenum telluride thin film was obtained on the surface of the single-crystal silicon substrate, and the periphery of the circular single-crystal semiconductor molybdenum telluride was 1T' -MoTe which had not been phase-changed yet2. Electron Back Scattering Diffraction (EBSD) analysis of the sample determined the circular semiconductor molybdenum telluride film as a single crystal, as shown by d and e in fig. 2.
(5) The large-area continuous semiconductor phase molybdenum telluride thin film growing on the monocrystalline silicon substrate is subjected to photoetching, etching, electron beam evaporation coating, stripping and other steps to obtain the molybdenum telluride/silicon pn junction device, the structural design of the device is shown as a in figure 3, and the optical micrograph of the prepared device is shown as b in figure 3.
The obtained molybdenum telluride/silicon pn junction device and the photodetector are subjected to electrical measurement at room temperature, and the measurement result of 20 pn junction devices as shown in c in figure 3 shows that the device obtained by the method has relatively high current on-off ratio.
Finally, it is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.

Claims (10)

1. A method for heterointegration of a single-crystal two-dimensional semiconductor molybdenum telluride film and an arbitrary lattice mismatch single-crystal substrate comprises the following steps:
1) depositing a layer of molybdenum film with the thickness of 1-5nm on the surface of the single crystal substrate;
2) taking a tellurium simple substance as a Te source, pretreating the molybdenum film on the single crystal substrate by a chemical vapor deposition method, and forming a metal phase molybdenum telluride film on the single crystal substrate;
3) and (3) taking a tellurium simple substance as a Te source, and processing the metal phase molybdenum telluride film on the single crystal substrate by a chemical vapor deposition method to form a heterogeneous integrated structure of the single crystal two-dimensional semiconductor molybdenum telluride film and the single crystal substrate.
2. The method according to claim 1, wherein the single crystal base in step 1) is selected from the group consisting of three-dimensional single crystal substrate silicon, gallium nitride, sapphire, quartz, silicon carbide, and other single crystal substrates.
3. The method of claim 1, wherein the method of depositing the molybdenum thin film in step 1) is a magnetron sputtering method, an electron beam thermal evaporation method, or an atomic layer deposition method.
4. The method according to claim 1, wherein the step 2) comprises placing a single crystal substrate sample having a molybdenum thin film deposited on the surface thereof and an elemental tellurium into a furnace for chemical vapor deposition; raising the temperature in the step 3) to promote the 2H-MoTe to appear in the metal phase molybdenum telluride film2Nucleation center, 2H-MoTe2The crystal domain grows in a transverse epitaxial mode in a plane to form a single crystal two-dimensional semiconductor molybdenum telluride film.
5. The method according to claim 1, wherein the chemical vapor deposition in step 2) is carried out at 490 to 510 ℃ for 5 to 20min to obtain polycrystalline 1T' -MoTe2A film.
6. The method of claim 1, wherein the chemical vapor deposition in step 3) is performed at a temperature of 600 to 700 ℃ for 1 to 3 hours to obtain the single crystal two-dimensional semiconductor molybdenum telluride film.
7. The method according to claim 1, wherein the step 2) and the step 3) are continuously carried out, and the single crystal substrate sample with the molybdenum film deposited on the surface and the tellurium simple substance are placed into a furnace for chemical vapor deposition, and the temperature is heated from room temperature to 600-700 ℃ to form a heterogeneous integrated structure of the single crystal two-dimensional semiconductor molybdenum telluride film and the single crystal substrate.
8. The method according to claim 7, wherein the steps 2) and 3) are continuously performed at a temperature increase rate of 20 to 40 ℃/min.
9. A hetero-integrated structure of a single-crystal two-dimensional semiconductor molybdenum telluride thin film prepared by the method of any one of claims 1 to 8 and an arbitrary lattice mismatch single-crystal substrate.
10. Use of the heterointegrated structure of a single-crystal two-dimensional semiconductor molybdenum telluride film as claimed in claim 9 with any lattice mismatched single crystal substrate in the manufacture of optoelectronic devices.
CN202110370754.6A 2021-04-07 2021-04-07 Method for heterointegration of single-crystal two-dimensional semiconductor molybdenum telluride film and random lattice mismatch single crystal substrate Pending CN114373828A (en)

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