CN108546995B - Preparation method for directionally growing tellurium-zinc-cadmium film on graphene substrate - Google Patents

Preparation method for directionally growing tellurium-zinc-cadmium film on graphene substrate Download PDF

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CN108546995B
CN108546995B CN201810204992.8A CN201810204992A CN108546995B CN 108546995 B CN108546995 B CN 108546995B CN 201810204992 A CN201810204992 A CN 201810204992A CN 108546995 B CN108546995 B CN 108546995B
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cdznte
substrate
graphene
copper foil
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CN108546995A (en
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黄健
谷青苗
周新雨
杨帆
邹天宇
唐可
黄浩斐
王林军
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University of Shanghai for Science and Technology
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
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    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08—Etching
    • C30B33/10—Etching in solutions or melts

Abstract

The invention discloses a preparation method for directionally growing a tellurium-zinc-cadmium film on a graphene substrate. According to the method, the scheme of preparing the film by close-space sublimation by setting the distance between the substrate and the sublimation source is adopted, the graphene material is used as the substrate structure, the lattice matching degree with the target CdZnTe film is high, and therefore the preparation of the CdZnTe film with good directionality is realized. The invention aims to prepare the oriented CdZnTe film on a graphene substrate by adopting a space-entering sublimation method, so that the transmission loss of current carriers between an upper electrode and a lower electrode is low when a device is manufactured, the current carrier transmission speed of the device is increased, and the transmission speed of the device is increased. Compared with CdZnTe single crystal, the method has the advantages of simple growth process, lower cost, large-area preparation and high feasibility of batch growth.

Description

Preparation method for directionally growing tellurium-zinc-cadmium film on graphene substrate
Technical Field
The invention relates to a preparation method of a cadmium zinc telluride material, in particular to a preparation method of a cadmium zinc telluride film, and also relates to a preparation method of a large-area cadmium zinc telluride material, belonging to the technical field of inorganic non-metal material manufacturing processes.
Background
CdZnTe is an important II-VI group compound semiconductor, and can be widely applied to the preparation of high-energy nuclear radiation detectors because of higher average atomic number, excellent carrier transmission performance and larger forbidden bandwidth. Due to good photoelectric property, the method has great superiority in the aspects of environmental monitoring, nuclear physics technology, ray analysis, safety detection, medical imaging and space science research. However, because of the inherent physical characteristics of CdZnTe, the crystal grown by the melt method has many defects of non-uniformity of components, grain boundary, twin crystal, dislocation, inclusion phase and precipitation and the like, and the prepared crystal structure has high cost, long time and complex process, and the CdZnTe single crystal material is not suitable for a large-area flat panel detector. Therefore, a method which is suitable for preparing a large-area CdZnTe film and has low cost is sought.
Compared with a single crystal growth process, the film preparation process is simple, the cost is lower, the batch growth feasibility is high, and the film preparation process is suitable for preparing a large-area flat panel detector based on the planar characteristics of the film. At present, the research on the CdZnTe film detector is still in the initial stage internationally. The CdZnTe film can be prepared by a chemical method or can be obtained by physical vapor deposition. Among these thin film preparation methods, the near-space sublimation method is the most promising method, and the method has low cost, high speed and good quality, and is suitable for large-area deposition of thin films. At present, the close space sublimation method is used for preparing the CdTe thin film, but the preparation of the CdZnTe thin film is less.
The CdZnTe thin film prepared by the near-space sublimation method is a polycrystalline thin film, the growth of the thin film is generally disoriented and disorderly, and relatively speaking, the thin film is difficult to realize high resistance and low defect, which affects the application of the thin film on a high-performance radiation detector. The preparation process can be carried out on different substrates, and the lattice matching degree of the substrate and the CdZnTe structure can affect the prepared film to different degrees. How to prepare the CdZnTe thin-film material which has few defects and high resistivity and is suitable for manufacturing a radiation detector becomes a technical problem to be solved urgently.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to overcome the defects in the prior art, and provides a preparation method for directionally growing a tellurium-zinc-cadmium film on a graphene substrate. The film prepared by the method has high directionality, and the transfer loss of current carriers between the upper electrode and the lower electrode is less when the film is manufactured into a device.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method for directionally growing a cadmium zinc telluride film on a graphene substrate comprises the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 100-600 mTorr, introducing hydrogen gas at the flow rate of 10-50 sccm, heating to 500-2000 ℃, keeping the temperature for 10-60 min, then removing oxides on the surface of the copper foil, continuously keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 1-20 sccm for 10-30 min, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 10-80%, and obtaining a product, namely a graphene film, generated on the copper foil; then stopping introducing methane, and naturally cooling the graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use; preparing a single-layer graphene film on a copper foil as a substrate for later use by adopting a CVD (chemical vapor deposition) method and preferably;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to pump vacuum, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be not more than 10 mm; heating the sublimation source and the substrate to 400-650 ℃ and 200-550 ℃ respectively, and growing CdZnTe for 10-500 min to obtain a product generated on the graphene film, namely a CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature; growing CdZnTe for 120-180 min preferably by adopting a near-space sublimation method, wherein the product generated on the graphene film is the CdZnTe film;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 0.03-1 mu m as a polishing material, polishing the CdZnTe film sample by adopting a manual polishing method, and then putting the polished CdZnTe film sample in CdCl2Annealing treatment is carried out for 20-60 minutes at 300-450 ℃ in the atmosphere; and then preparing a bromomethanol solution with the bromine mass concentration of 0.1-0.5%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 10-60 s, thereby obtaining the CdZnTe film with the columnar structure prepared on the graphene substrate. The Close Space Sublimation (CSS) method is a practical film growth process, and has been applied to the preparation of CdTe films. In order to adapt to the application of a high-energy radiation detector, the preparation of the high-quality CdZnTe film with columnar oriented growth on the graphene substrate can obviously make up for the defects of the polycrystalline film. Compared with CdZnTe films grown on other substrates, the CdZnTe film with the columnar structure grown on the graphene substrate has the advantages of few defects, high resistivity and the like, and is suitable for manufacturing radiation detectors. Preferably, the CdZnTe film with the thickness of 10-500 mu m prepared on the graphene substrate is obtained. And preferably obtaining the CdZnTe thin film with the thickness of 150-250 mu m prepared on the graphene substrate.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. compared with CdZnTe films grown on other substrates, the columnar CdZnTe film grown on the graphene substrate prepared by the invention has fewer crystal boundary defects and higher resistivity, and the carrier transmission speed is high and the loss is less when the device is prepared;
2. compared with the CdZnTe single crystal growth process, the preparation method has the advantages of simple process, lower cost, large-area preparation and high feasibility of batch growth by adopting the CdZnTe film preparation process by the near-space sublimation method;
3. the invention aims to prepare the oriented CdZnTe film on the graphene substrate by adopting a space-entering sublimation method, so that the transmission loss of current carriers between an upper pole and a lower pole is low when a device is manufactured, the transmission speed of the current carriers of the device is improved, and the transmission speed of the device is improved.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this embodiment, a method for preparing a cadmium zinc telluride thin film directionally grown on a graphene substrate includes the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 340mTorr, introducing hydrogen gas at the flow rate of 20sccm, heating to 1050 ℃ and keeping the temperature for 30min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 8sccm for 20min respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 50%, and obtaining a product generated on the copper foil, namely a single-layer graphene film; then stopping introducing methane, and naturally cooling the single-layer graphene film in the CVD reaction chamber in the non-oxidation protective atmosphere environment of the argon and the hydrogen for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the single-layer graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to vacuumize, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 4 mm; heating the sublimation source and the substrate to 600 ℃ and 400 ℃ respectively, and growing CdZnTe for 120min to obtain a product generated on the graphene film, namely the CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 0.05 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2Annealing at 400 ℃ for 30 minutes in the atmosphere; and then preparing a bromomethanol solution with the bromine mass percentage concentration of 0.1%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 40s, thereby obtaining the CdZnTe film which is prepared on the graphene substrate and has a columnar structure and the thickness of 150 mu m.
Experimental test analysis:
the CdZnTe thin film with the thickness of 150 μm and the columnar structure prepared on the graphene substrate and prepared in the embodiment is used as a sample to carry out experimental tests, and the resistivity of the CdZnTe thin film prepared in the embodiment is measured to be 5.9 multiplied by 109Omega cm. The Close Space Sublimation (CSS) method is a practical film growth process, and has been applied to the preparation of CdTe films. In order to adapt to the application of a high-energy radiation detector, the preparation of the high-quality CdZnTe film with columnar oriented growth on the graphene substrate can obviously make up for the defects of the polycrystalline film. The CdZnTe film with the columnar structure growing on the graphene substrate and other substratesCompared with the CdZnTe film which grows upwards, the CdZnTe film has the advantages of few defects, high resistivity and the like, and is suitable for manufacturing a radiation detector.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for preparing a cadmium zinc telluride thin film directionally grown on a graphene substrate includes the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 340mTorr, introducing hydrogen gas at the flow rate of 20sccm, heating to 1050 ℃ and keeping the temperature for 30min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 8sccm for 20min respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 50%, and obtaining a product generated on the copper foil, namely a single-layer graphene film; then stopping introducing methane, and naturally cooling the single-layer graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the single-layer graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to vacuumize, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 4 mm; heating the sublimation source and the substrate to 600 ℃ and 400 ℃ respectively, and growing CdZnTe for 150min to obtain a product generated on the graphene film, namely the CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 0.05 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2Annealing at 400 ℃ for 30 minutes in the atmosphere; and then preparing a bromomethanol solution with the bromine mass percentage concentration of 0.1%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 40s, thereby obtaining the CdZnTe film which is prepared on the graphene substrate and has a columnar structure and the thickness of 200 mu m.
Experimental test analysis:
the CdZnTe thin film with a columnar structure and a thickness of 200 μm prepared on the graphene substrate in this example was used as a sample for experimental tests, and the resistivity of the CdZnTe thin film prepared in this example was measured to be 5.9 × 109Omega cm. The Close Space Sublimation (CSS) method is a practical film growth process, and has been applied to the preparation of CdTe films. In order to adapt to the application of a high-energy radiation detector, the preparation of the high-quality CdZnTe film with columnar oriented growth on the graphene substrate can obviously make up for the defects of the polycrystalline film. Compared with CdZnTe films grown on other substrates, the CdZnTe film with the columnar structure grown on the graphene substrate has the advantages of few defects, high resistivity and the like, and is suitable for manufacturing radiation detectors.
Example three:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a cadmium zinc telluride thin film directionally grown on a graphene substrate includes the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 340mTorr, introducing hydrogen gas at the flow rate of 20sccm, heating to 1050 ℃ and keeping the temperature for 30min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 8sccm for 20min respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 50%, and obtaining a product generated on the copper foil, namely a single-layer graphene film; then stopping introducing methane, and naturally cooling the single-layer graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the single-layer graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to vacuumize, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 4 mm; heating the sublimation source and the substrate to 600 ℃ and 400 ℃ respectively, and growing CdZnTe for 180min to obtain a product generated on the graphene film, namely the CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 0.05 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2Annealing at 400 ℃ for 30 minutes in the atmosphere; and then preparing a bromomethanol solution with the bromine mass percent concentration of 0.1%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 40s, thereby obtaining the CdZnTe film with the thickness of 250 μm and a columnar structure prepared on the graphene substrate.
Experimental test analysis:
the CdZnTe thin film with a thickness of 250 μm prepared on the graphene substrate and having a columnar structure prepared in this example was used as a sample for experimental tests, and the resistance of the CdZnTe thin film prepared in this example was measuredThe ratio was 5.9X 109Omega cm. The Close Space Sublimation (CSS) method is a practical film growth process, and has been applied to the preparation of CdTe films. In order to adapt to the application of a high-energy radiation detector, the preparation of the high-quality CdZnTe film with columnar oriented growth on the graphene substrate can obviously make up for the defects of the polycrystalline film. Compared with CdZnTe films grown on other substrates, the CdZnTe film with the columnar structure grown on the graphene substrate has the advantages of few defects, high resistivity and the like, and is suitable for manufacturing radiation detectors.
Example four:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a cadmium zinc telluride thin film directionally grown on a graphene substrate includes the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 100mTorr, introducing hydrogen gas at the flow rate of 10sccm, heating to 500 ℃ and keeping the temperature for 60min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 1sccm for 30min respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 10%, and obtaining a product generated on the copper foil, namely a graphene film; then stopping introducing methane, and naturally cooling the graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to pump vacuum, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 10 mm; heating the sublimation source and the substrate to 400 ℃ and 200 ℃ respectively, and growing CdZnTe for 500min to obtain a product generated on the graphene film, namely a CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 0.03 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2Annealing at 300 ℃ for 60 minutes in the atmosphere; and then preparing a bromomethanol solution with the bromine mass percent concentration of 0.5%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 10s, thereby obtaining the CdZnTe film with the thickness of 500 mu m and a columnar structure prepared on the graphene substrate.
Experimental test analysis:
the CdZnTe film with a columnar structure prepared on the graphene substrate and prepared in the embodiment is used as a sample to carry out experimental tests, and the resistivity of the CdZnTe film prepared in the embodiment is 5 multiplied by 10^10 omega cm. The Close Space Sublimation (CSS) method is a practical film growth process, and has been applied to the preparation of CdTe films. In order to adapt to the application of a high-energy radiation detector, the preparation of the high-quality CdZnTe film with columnar oriented growth on the graphene substrate can obviously make up for the defects of the polycrystalline film. Compared with CdZnTe films grown on other substrates, the CdZnTe film with the columnar structure grown on the graphene substrate has the advantages of few defects, high resistivity and the like, and is suitable for manufacturing radiation detectors.
Example five:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a cadmium zinc telluride thin film directionally grown on a graphene substrate includes the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 600mTorr, introducing hydrogen gas at the flow rate of 50sccm, heating to 2000 ℃ and keeping the temperature for 10min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 20sccm for 10min, respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 80%, and obtaining a product generated on the copper foil, namely a graphene film; then stopping introducing methane, and naturally cooling the graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to pump vacuum, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 4 mm; heating the sublimation source and the substrate to 650 ℃ and 550 ℃ respectively, and growing CdZnTe for 10min to obtain a product generated on the graphene film, namely a CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 1 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2Annealing at 450 ℃ for 20 minutes in the atmosphere; then preparing a bromomethanol solution with the bromine mass percent concentration of 0.1%, immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 60s, and thus obtaining the preparation on the graphene substrateThe thickness of the columnar structure of (2) is 10 mu m of CdZnTe film.
Experimental test analysis:
the CdZnTe film with a columnar structure prepared on the graphene substrate and prepared in the embodiment is used as a sample to carry out experimental tests, and the resistivity of the CdZnTe film prepared in the embodiment is 5 multiplied by 10^10 omega cm. The Close Space Sublimation (CSS) method is a practical film growth process, and has been applied to the preparation of CdTe films. In order to adapt to the application of a high-energy radiation detector, the preparation of the high-quality CdZnTe film with columnar oriented growth on the graphene substrate can obviously make up for the defects of the polycrystalline film. Compared with CdZnTe films grown on other substrates, the CdZnTe film with the columnar structure grown on the graphene substrate has the advantages of few defects, high resistivity and the like, and is suitable for manufacturing radiation detectors.
In summary, in the embodiments of the present invention, the CVD method is adopted to prepare the graphene on the copper foil, and then the graphene is used as the substrate to prepare the directional tellurium-zinc-cadmium thin film by the near-space sublimation method. According to the embodiment, the scheme of preparing the film by close-space sublimation by setting the distance between the substrate and the sublimation source is adopted, the graphene material is used as the substrate structure, the lattice matching degree with the target CdZnTe film is high, and therefore the preparation of the CdZnTe film with good directionality is realized. In the embodiment, the directional CdZnTe film is prepared on the graphene substrate by adopting a space-entering sublimation method, so that the transmission loss of current carriers between an upper pole and a lower pole is low when a device is manufactured, the current carrier transmission speed of the device is increased, and the transmission speed of the device is increased.
The embodiments of the present invention have been described above, but the present invention is not limited to the above embodiments, and various changes and modifications can be made according to the purpose of the invention, and all changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitution ways, so long as the invention meets the purpose of the present invention, and the technical principle and inventive concept of the method for preparing the tellurium-zinc-cadmium film directionally growing on the graphene substrate of the present invention shall not depart from the scope of the present invention.

Claims (2)

1. A preparation method for directionally growing a tellurium-zinc-cadmium film on a graphene substrate is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 100mTorr, introducing hydrogen gas at the flow rate of 10sccm, heating to 500 ℃ and keeping the temperature for 60min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 1sccm for 30min respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 10%, and obtaining a product generated on the copper foil, namely a graphene film; then stopping introducing methane, and naturally cooling the graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to pump vacuum, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 10 mm; heating the sublimation source and the substrate to 400 ℃ and 200 ℃ respectively, and growing CdZnTe for 500min to obtain a product generated on the graphene film, namely a CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 0.03 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2In the atmosphere 30Annealing at 0 ℃ for 60 minutes; and then preparing a bromomethanol solution with the bromine mass percent concentration of 0.5%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 10s, thereby obtaining the CdZnTe film with the thickness of 500 mu m and a columnar structure prepared on the graphene substrate.
2. A preparation method for directionally growing a tellurium-zinc-cadmium film on a graphene substrate is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing and pretreating a substrate:
the CVD method is adopted to prepare the substrate, and the specific method is as follows:
cleaning a copper foil by using an acetone solution to remove organic impurities on the surface of the copper foil, then placing the cleaned copper foil into a CVD growth chamber, introducing argon gas to control the pressure to be 600mTorr, introducing hydrogen gas at the flow rate of 50sccm, heating to 2000 ℃ and keeping the temperature for 10min, then removing oxides on the surface of the copper foil, keeping the temperature unchanged, introducing mixed gas of methane and hydrogen gas at the flow rate of 20sccm for 10min, respectively, controlling the volume fraction of the hydrogen gas in the mixed gas in the CVD growth chamber to be 80%, and obtaining a product generated on the copper foil, namely a graphene film; then stopping introducing methane, and naturally cooling the graphene film in the CVD reaction chamber in the argon and hydrogen environment for later use;
(2) the growth process of the CdZnTe film is as follows:
a near space sublimation method is adopted, dustless cloth is dipped in alcohol to wipe and clean the reaction cavity, and impurities in the reaction cavity are removed; grinding tellurium-zinc-cadmium single crystal into powder serving as a sublimation source, placing the powder into a reaction cavity, taking the graphene film prepared in the step (1) as a near-space sublimed substrate, placing the substrate into the reaction cavity, starting a mechanical pump to pump vacuum, and pumping the air pressure in the reaction cavity to be below 5 Pa; adjusting the distance between the substrate and the sublimation source to be 4 mm; heating the sublimation source and the substrate to 650 ℃ and 550 ℃ respectively, and growing CdZnTe for 10min to obtain a product generated on the graphene film, namely a CdZnTe film, so as to obtain a CdZnTe film sample; then closing the heating source, turning off the mechanical pump, and taking out the CdZnTe film sample after the CdZnTe film sample is cooled to room temperature;
(3) polishing, corroding and annealing the CdZnTe film:
adopting alumina with the granularity of 1 mu m as a polishing material, adopting a manual polishing method to polish the CdZnTe film sample, and then putting the polished CdZnTe film sample in CdCl2Annealing at 450 ℃ for 20 minutes in the atmosphere; and then preparing a bromomethanol solution with the bromine mass percent concentration of 0.1%, and immersing the annealed CdZnTe film sample into the bromomethanol solution for corrosion treatment for 60s, so as to obtain the CdZnTe film with the thickness of 10 μm and a columnar structure prepared on the graphene substrate.
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