CN111261492A - Nano thin film material - Google Patents
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- 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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- 239000000463 material Substances 0.000 title claims abstract description 24
- 239000010409 thin film Substances 0.000 title description 5
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002120 nanofilm Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000011888 foil Substances 0.000 claims description 23
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 15
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 11
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 5
- 238000005137 deposition process Methods 0.000 claims description 3
- 238000005566 electron beam evaporation Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000003746 solid phase reaction Methods 0.000 abstract description 5
- 239000002159 nanocrystal Substances 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- 239000010408 film Substances 0.000 description 15
- 239000013078 crystal Substances 0.000 description 9
- 238000004528 spin coating Methods 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfides Chemical class 0.000 description 1
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- 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
- H01L21/02425—Conductive materials, e.g. metallic silicides
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- 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
- H01L21/02551—Group 12/16 materials
- H01L21/0256—Selenides
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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- H01L21/04—Manufacture 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
- H01L21/34—Manufacture 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
- H01L21/46—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
- H01L21/477—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
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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
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.
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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 |
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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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