CN111261492A - Nano thin film material - Google Patents

Nano thin film material Download PDF

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Publication number
CN111261492A
CN111261492A CN201811450387.5A CN201811450387A CN111261492A CN 111261492 A CN111261492 A CN 111261492A CN 201811450387 A CN201811450387 A CN 201811450387A CN 111261492 A CN111261492 A CN 111261492A
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nise
film
nano
nano film
foil
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陈莉芳
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Yuyao Jingpeng Photovoltaic Power Generation Co Ltd
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Yuyao Jingpeng Photovoltaic Power Generation Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor 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
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02367Substrates
    • H01L21/0237Materials
    • H01L21/02425Conductive materials, e.g. metallic silicides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02518Deposited layers
    • H01L21/02521Materials
    • H01L21/02551Group 12/16 materials
    • H01L21/0256Selenides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02617Deposition types
    • H01L21/02631Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/34Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
    • H01L21/46Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
    • H01L21/477Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
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    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor 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
    • H01L31/0248Semiconductor 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
    • H01L31/0256Semiconductor 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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    • H01L31/032Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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Abstract

The invention discloses a nano film material, which comprises the steps of preparation of a NiSe nano film, transfer of the NiSe nano film, construction of a NiSe nano film photodetector and the like. The NiSe nano film with a non-laminated structure, which is grown by a solid-phase reaction method, has good quality, large grain size and small quantity of grain boundaries; the photoelectric current obtained by the photoelectric detector prepared based on the high-quality NiSe nano film is improved by 4 orders of magnitude compared with the NiSe nano crystal film; the preparation method has the advantages of simple preparation process, low cost and good practical value, and the method can be used for preparing other non-laminated structure material nano films compatible with the traditional planar process.

Description

Nano thin film material
Technical Field
The invention belongs to the field of semiconductor film materials, and relates to a method for preparing a nano film material by a solid-phase reaction method.
Background
Due to their unique structures and properties, graphene and other two-dimensional materials, including hexagonal phase boron nitride and transition metal sulfides, have attracted considerable attention. Particularly, the high-quality large-area two-dimensional film can be prepared on a specific substrate by methods such as chemical vapor deposition and the like, which remarkably accelerates the application development of the two-dimensional material. Inspired by the two-dimensional material with the layered structure, the nano film of the non-layered structure material is compatible with the traditional planar process, and is more beneficial to the application compared with other dimensions. Moreover, compared with the film composed of the nanocrystalline, the prepared non-laminated structure nano film with large-size crystal grains has more excellent performance, because the grain boundary can cause the scattering of electrons. The layered structure material has strong lateral chemical bonds within the layers and weak van der waals forces between the layers, which make it easier for atoms to grow into a two-dimensional film during nucleation and growth. The non-laminated structure material has strong atomic bonds in three directions, so that the material lacks intrinsic anisotropic growth driving force, and the growth of the non-laminated structure nano film is difficult to realize. Two-dimensional ultrathin nanosheets and non-lamellar structured nanofilms of non-lamellar structured materials have been prepared by wet chemical templating and exfoliation methods, respectively, but are limited in size to only a few hundred nanometers and a few micrometers, respectively. The nano film of the large-area non-laminated structure material can be obtained by epitaxial growth on a single crystal substrate by a molecular beam epitaxy method, but the cost is higher.
Disclosure of Invention
The invention aims to provide a nano thin film material. The growth method of the nano film provided by the invention has the advantages of simple process, low cost and strong practical value, and can be used for preparing other non-laminated structure material nano films compatible with the traditional planar process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nano-film material comprising the steps of:
(1) preparing the NiSe nano film: selecting a Ni foil with the thickness of 50 mu m and the purity of 99.99 percent, and annealing at the temperature of 450-550 ℃ for 25-35min in a low-pressure atmosphere with 10sccmH2 and 20sccmAr to remove oxides on the surface of the Ni foil; after annealing, depositing a ZnSe film on the surface of the Ni foil by using an electron beam evaporation method, wherein the vacuum degree is kept at 1 x 10 < -4 > to 3 x 10 < -4 > Pa in the whole deposition process; annealing the ZnSe/Ni foil at the vacuum degree of 1.5 × 10-4-2.5 × 10-4Pa at 650-;
(2) and (3) transferring the NiSe nano film: the NiSe nano film obtained on the surface of the Ni foil with the thickness of 50 mu m is spin-coated with PMMA with the concentration of 80-120mg/ml, and the spin-coating conditions are as follows: firstly, spin-coating and spin-coating for 5-7s at the rotation speed of 400-; after the spin coating is finished, placing the mixture on a heating table and baking the mixture for 4 to 6min at the temperature of between 70 and 90 ℃; then putting the PMMA/NiSe/Ni foil into a solution of 2.0mol/LFeCl3 to etch the Ni foil; after the Ni foil is etched, the PMMA/NiSe film is placed in deionized water to clean FeCl3 etching liquid remained on the surface of the PMMA/NiSe film; then, fishing out the NiSe nano film supported by the PMMA from the SiO2/Si substrate; after the materials are completely air-dried, placing PMMA/NiSe/SiO2/Si in a low-pressure atmosphere with 10sccmH2 and 20sccmAr, and annealing at 350-450 ℃ for 1-3h to remove PMMA, thereby obtaining the NiSe nano film transferred to the SiO2/Si substrate;
(3) constructing a NiSe nano film photodetector: after the NiSe nano film is transferred to the SiO2/Si substrate, a channel with the length of 5 mu m and the width of 10 mu m is constructed by utilizing a photoetching method; the electrodes were fabricated by depositing 10/35nmCr/Au by a high vacuum thermal evaporation system.
The invention has the beneficial effects that:
(1) the NiSe nano film with a non-laminated structure, which is grown by a solid-phase reaction method, has the advantages of good quality, large grain size and small quantity of grain boundaries.
(2) The photoelectric current obtained by the photoelectric detector prepared based on the high-quality NiSe nano film is improved by 4 orders of magnitude compared with the NiSe nano crystal film.
(3) The preparation method has the advantages of simple preparation process, low cost and good practical value, and the method can be used for preparing other non-laminated structure material nano films compatible with the traditional planar process.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The invention will be further described with reference to the following examples, but the scope of the invention is not limited to these examples.
A nano-film material comprising the steps of:
(1) preparing the NiSe nano film: selecting a Ni foil with the thickness of 50 mu m and the purity of 99.99 percent, and annealing for 30min at 500 ℃ in a low-pressure atmosphere with 10sccm H2 and 20sccm Ar to remove oxides on the surface of the Ni foil; after annealing, depositing a ZnSe film on the surface of the Ni foil by using an electron beam evaporation method, wherein the vacuum degree is kept at 2 x 10 < -4 > Pa in the whole deposition process; annealing the ZnSe/Ni foil at the vacuum degree of 2 x 10 < -4 > Pa and the temperature of 700 ℃ for 30min to obtain a NiSe nano film;
(2) and (3) transferring the NiSe nano film: PMMA with the concentration of 100mg/ml is spin-coated on the NiSe nano film obtained on the surface of the Ni foil with the thickness of 50 microns, and the spin-coating conditions are as follows: firstly, spin coating and spin coating for 6s at the rotating speed of 500r/min, and then spin coating for 40s at the rotating speed of 2000 r/min; after the spin coating is finished, placing the mixture on a heating table and baking the mixture for 5min at the temperature of 80 ℃; then putting the PMMA/NiSe/Ni foil into a solution of 2.0mol/L FeCl3 to etch the Ni foil; after the Ni foil is etched, the PMMA/NiSe film is placed in deionized water to clean FeCl3 etching liquid remained on the surface of the PMMA/NiSe film; then, fishing out the NiSe nano film supported by the PMMA from the SiO2/Si substrate; after the materials are completely air-dried, placing PMMA/NiSe/SiO2/Si in a low-pressure atmosphere with 10sccm H2 and 20sccm Ar, and annealing at 400 ℃ for 2H to remove PMMA, so that the NiSe nano film transferred to the SiO2/Si substrate is obtained;
(3) constructing a NiSe nano film photodetector: after the NiSe nano film is transferred to the SiO2/Si substrate, a channel with the length of 5 mu m and the width of 10 mu m is constructed by utilizing a photoetching method; the electrodes were fabricated by depositing 10/35nmCr/Au by a high vacuum thermal evaporation system.
The vapor phase method is widely applied to crystal growth, and a certain supersaturation degree is required for realizing the growth of the crystal by the vapor phase method. After undergoing a gas-solid transition process, atoms or molecules begin to nucleate and grow. In this non-equilibrium dynamic process, the supply rate of the gas source is much greater than the rate of crystal growth at supersaturation levels corresponding to film growth, so that the product morphology determined by the dynamic process generally exhibits isolated island structures rather than continuous nanofilms, which is caused by the three-dimensional growth behavior resulting from the non-layered structure. Based on the consideration of molecular beam epitaxial growth of single crystal non-layered structure nano thin film, the control of the relative rate between the gas source supply and the crystal growth is a key element of the growth of the non-layered structure nano thin film. Taking NiSe on Ni foil as an example, a method for epitaxially growing a non-laminated structure nano film in an interface limited domain is invented through the introduction of a solid-phase reaction method. At a specific temperature, NiSe nucleates at the ZnSe-Ni interface after forming NiSe by interdiffusion of Zn and Ni atoms. During this thermodynamic equilibrium without gas-solid transition, the rate of NiSe growth is believed to be determined by diffusion and reaction rates. This allows the NiSe to form coherent interfaces ((102) NiSe/(111) Ni and (110) NiSe/(200) Ni) with the Ni substrate during the relaxation time, i.e., the epitaxial growth of NiSe on the surface of the Ni foil is achieved, resulting in a lower energy NiSe-Ni interface. At the same time, Zn and Ni atoms diffuse along the ZnSe-NiSe interface, and the NiSe reactant then grows epitaxially on the NiSe-Ni steps or on the upper surface of the NiSe nucleation sites. Thus, the NiSe grains grow further by depletion of the ZnSe source and the NiSe-ZnSe interface advancing in the transverse and longitudinal directions. When the ZnSe film above the NiSe nucleation point is consumed before the transverse ZnSe film, the growth of the NiSe crystal grains can be continued only by the transverse propulsion of the NiSe-ZnSe interface, and finally the continuous NiSe nano film is formed by mutual splicing of the crystal grains.
The NiSe nano film with a non-laminated structure, which is grown by a solid-phase reaction method, has good quality, large grain size and small quantity of grain boundaries; the photoelectric current obtained by the photoelectric detector prepared based on the high-quality NiSe nano film is improved by 4 orders of magnitude compared with the NiSe nano crystal film; the preparation method has the advantages of simple preparation process, low cost and good practical value, and the method can be used for preparing other non-laminated structure material nano films compatible with the traditional planar process.
Finally, it should be noted that: therefore, although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that the present invention may be modified or substituted with equivalents without departing from the spirit and scope of the present invention, and all such modifications and improvements are intended to be covered by the following claims.

Claims (1)

1. A nano-film material, comprising the steps of: (1) preparing the NiSe nano film: selecting a Ni foil with the thickness of 50 mu m and the purity of 99.99 percent, and annealing at the temperature of 450-550 ℃ for 25-35min in a low-pressure atmosphere with 10sccmH2 and 20sccmAr to remove oxides on the surface of the Ni foil; after annealing, depositing a ZnSe film on the surface of the Ni foil by using an electron beam evaporation method, wherein the vacuum degree is kept at 1 x 10 < -4 > to 3 x 10 < -4 > Pa in the whole deposition process; annealing the ZnSe/Ni foil at the vacuum degree of 1.5 × 10-4-2.5 × 10-4Pa at 650-; (2) and (3) transferring the NiSe nano film: the NiSe nano film obtained on the surface of the Ni foil with the thickness of 50 mu m is spin-coated with PMMA with the concentration of 80-120 mg/ml.
CN201811450387.5A 2018-11-30 2018-11-30 Nano thin film material Pending CN111261492A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111863378A (en) * 2020-07-28 2020-10-30 安徽智磁新材料科技有限公司 Soft magnetic particle film with high-temperature magnetic stability and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111863378A (en) * 2020-07-28 2020-10-30 安徽智磁新材料科技有限公司 Soft magnetic particle film with high-temperature magnetic stability and preparation method thereof
CN111863378B (en) * 2020-07-28 2021-09-24 安徽智磁新材料科技有限公司 Soft magnetic particle film with high-temperature magnetic stability and preparation method thereof

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