CN113471303A - High-detection-efficiency self-supporting CdZnTe thick film structure, detection device, preparation method and application thereof - Google Patents
High-detection-efficiency self-supporting CdZnTe thick film structure, detection device, preparation method and application thereof Download PDFInfo
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- H01L31/0264—Inorganic materials
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Abstract
The invention discloses a self-supporting CdZnTe thick film structure with high detection efficiency, a detection device, a preparation method and application thereof. The preparation method of the self-supporting CdZnTe thick film gamma ray detector with high detection efficiency provided by the invention comprises four main steps of substrate pretreatment, a growth process of a CdZnTe film, a stripping process of the CdZnTe film and electrode manufacturing of the self-supporting CdZnTe thick film gamma ray detector. The method of the invention grows the CdZnTe thick film on the single crystal film substrate with high thermal conductivity, the high thermal conductivity of the substrate can promote the nucleation of CZT crystal grains, and further the CdZnTe thick film with large area and low defect concentration is obtained.
Description
Technical Field
The invention relates to a film composite material of a semiconductor, a preparation process and application thereof, in particular to a cadmium zinc telluride film device and a preparation process thereof, which are applied to the technical fields of inorganic non-metallic material manufacturing and optical functional devices.
Background
In recent years, the development of semiconductor nuclear radiation detectors has been fairly rapid. Such detectors have been widely used in many fields such as nuclear physics, X-ray and gamma ray astronomy, and nuclear medicine. Compared with a gas detector and a scintillator detector, the semiconductor detector has more excellent imaging performance and stronger energy spectrum resolution capability, and simultaneously, the whole detection system can be more compact in structure.
Semiconductor materials conventionally used for nuclear radiation detectors are silicon (Si) and germanium (Ge). Detectors based on these two materials are widely used for low energy X-ray and alpha particle detection due to their excellent carrier transport properties. However, with the change of the detection demand and the continuous increase of the detection demand, the compound semiconductor material is rapidly developed. The compound semiconductor material has the advantage that the physical properties of the material can be changed by adjusting the chemical composition and the growth process of the material according to different application environments so as to meet different detection requirements. The compound semiconductor is mainly derived from elements of groups IIIA and VA in the periodic table, typically GaAs, and elements of groups IIA and VIA, CdTe. In addition to these binary compounds, there are ternary compounds such as CdZnTe, HgCdTe and CdMnTe. Among these compound semiconductor materials, cadmium zinc telluride (CdZnTe) is a very competitive X-ray and gamma-ray detecting material. Its emergence has largely driven the development of high resolution room temperature semiconductor detectors. Some energy spectrometers adopting CdZnTe not only have high energy resolution, but also have wide energy dynamic range of measurement.
CdZnTe is a compound semiconductor material with relatively high average atomic number, and because Zn is doped, CdZnTe crystal has larger forbidden bandwidth and higher resistivity than CdTe, and the dislocation density is smaller, thus ensuring smaller leakage current and noise of the detector under the condition of room temperature, the CdZnTe crystal is particularly suitable for being prepared into a room temperature gamma ray detector and is also widely used for nondestructive detection, analysis and on-site investigation of nuclear materials. The forbidden band width is about 1.57eV, so that the material is very suitable for being used as a room-temperature nuclear radiation detection material without a liquid nitrogen cooling system. Meanwhile, CdZnTe also has relatively high resistivity, the leakage current of the body is low under the condition of high electric field, and the noise is also inhibited. In addition, the higher atomic number makes the CdZnTe material have higher quantum efficiency to gamma rays. Further research finds that the CdZnTe material has excellent high-energy radiation detection characteristics. For hard X-rays and gamma rays, the cut-off capability and the detection quantum efficiency of CdZnTe are high, the method is suitable for detecting photons with energy of 10 keV-1.5 MeV, and especially in the energy range of 10 keV-100 keV, the energy detection efficiency can even reach more than 90%. The continuously mature CdZnTe growth method, the continuously optimized detector structure and the continuously perfect signal processing technology all enable the performance of the CdZnTe detector to be more and more excellent, play more and more important roles in the field of nuclear radiation detection, become hot spots in the field of room-temperature semiconductor radiation detection at present, and are highly valued by countries in the world.
At present, several commonly used CdZnTe is named as CZT for short, the epitaxial substrate materials of the film comprise FTO, ITO, glass and GaAs, the FTO, the ITO and the glass are low in price, the bonding force between the FTO, the ITO and the glass and the epitaxial CZT film is strong, the radiation resistance and the high-temperature stability are poor, and the film is not suitable for working in the severe environment of nuclear radiation detection or ultraviolet detection. GaAs has low thermal conductivity and poor heat dissipation capability, and is not suitable for manufacturing high-power devices. A large amount of latent heat of crystallization is released in the CZT nucleation process, so that the temperature distribution of each part of the surface of the substrate is uneven, and the uniformity and the growth quality of the CZT film are influenced. AlN has the characteristics of wide direct band gap, high thermal conductivity, high chemical inertness, good thermal stability and the like, is used as a substrate for growing the CZT film, is more favorable for the nucleation of CZT grains, the crystallinity of the grown CZT film is better, the number of interface defects and holes is less, and the CZT film with good quality is more favorable for being manufactured into a nucleation radiation detector to be used in various environments.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art and provide a self-supporting CdZnTe thick film structure with high detection efficiency, a detection device, a preparation method and an application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-detection-efficiency self-supporting CdZnTe thick film structure peeled off from an AlN substrate is characterized in that a CdZnTe thick film is firstly grown and prepared on the AlN substrate to obtain a CdZnTe/AlN composite structure combining the CdZnTe thick film and the AlN substrate, and the CdZnTe thick film is separated from the AlN substrate for at least 5min by an ultrasonic method to obtain the self-supporting CdZnTe thick film structure.
Preferably, the thickness of the CdZnTe film is not more than 600 μm, and the thickness of the selected AlN substrate is not more than 500 nm.
The invention relates to a preparation method of a high-detection-efficiency self-supporting CdZnTe thick film structure stripped on an AlN substrate, which comprises the following steps:
a. substrate pretreatment:
respectively ultrasonically cleaning the AlN substrate by using acetone, alcohol and deionized water for at least 30 minutes, washing off impurities and organic matters on the surface of the AlN substrate, blow-drying by using nitrogen, and putting into a magnetron sputtering reaction chamber to be used as a substrate for later use;
and b, growth process of the CdZnTe film:
opening a close-space sublimation cavity, putting the AlN substrate pretreated in the step a into the cavity, starting a mechanical pump to pump vacuum, pumping the air pressure in the sublimation chamber to be not higher than 5Pa, then starting a halogen lamp, and respectively heating the sublimation source and the substrate to be not lower than 670 ℃ and not lower than 490 ℃ at the heating rate of not higher than 50 ℃/min;
then adopting a near space sublimation method, continuously growing the CdZnTe film material on the surface of the AlN substrate for at least 180mins, then closing the halogen lamp, after the CdZnTe film material growing on the substrate is cooled to room temperature, closing the mechanical pump, taking out the AlN substrate loaded with the CdZnTe film material, and thus obtaining the CdZnTe/AlN composite structure combined by the CdZnTe film and the AlN substrate
c, stripping the CdZnTe film:
and (3) carrying out ultrasonic treatment on the CdZnTe/AlN composite structure for at least 5 minutes by an ultrasonic method to obtain a self-supporting CdZnTe thick film structure separated from the AlN substrate.
A gamma ray detector is characterized in that a gold electrode layer with the thickness not more than 100nm is prepared on a self-supporting CdZnTe thick film interface stripped on an AlN substrate to form a CdZnTe/Au structural device which is used as a self-supporting CdZnTe thick film gamma ray detector.
The invention relates to a preparation method of a gamma ray detector, which comprises the following steps:
preparing a gold electrode layer with the thickness of not more than 100nm on the surface and the interface of the self-supporting CdZnTe thick film by adopting an evaporation method to obtain an Au/CdZnTe/Au structural device; then in N2In the atmosphere and under the condition of the annealing temperature not lower than 400 ℃, the Au/CdZnTe/Au structural device is subjected to rapid annealing treatment for at least 100s, so that the Au/CdZnTe/Au structural device forms ohmic contact on the connection interface of the functional layer, and the self-supporting CdZnTe thick-film gamma-ray detector is prepared.
The self-supporting CdZnTe thick film gamma ray detector is utilized, and has high cut-off capacity and high detection quantum efficiency on gamma rays; within the energy range of 10-100 keV, the energy detection efficiency of the self-supporting CdZnTe thick-film gamma-ray detector is not lower than 90%. The self-supporting CdZnTe thick-film gamma-ray detector can realize higher detection efficiency on gamma rays.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the self-supporting CdZnTe thick-film gamma-ray detector has relatively high resistivity, low leakage current and suppressed noise under the condition of high electric field;
2. the gamma-ray detector has high gamma-ray cut-off capability and detection quantum efficiency, particularly the energy detection efficiency can even reach more than 90% within the energy range of 10-100 keV, and the gamma-ray detector has excellent high-energy radiation detection characteristics.
Drawings
FIG. 1 is an XRD pattern of a self-supporting CdZnTe thick film structure material stripped on an AlN substrate according to a preferred embodiment of the invention.
FIG. 2 is an XRD pattern of a free-standing CdZnTe thick film structured material exfoliated on a comparative example glass substrate.
FIG. 3 is an SEM image of the surface of a self-supporting CdZnTe thick film structure stripped on an AlN substrate according to a preferred embodiment of the invention.
FIG. 4 is an I-T curve diagram of the Au/CdZnTe/Au composite structure device stripped from the AlN substrate under the irradiation of ultraviolet light in a 254nm solar dead zone in the preferred embodiment of the invention.
FIG. 5 is an I-T curve diagram of an Au/CdZnTe/Au composite structure device stripped on a glass substrate of a comparative example under the irradiation condition of ultraviolet light in a 254nm solar dead zone.
FIG. 6 shows 60KeV according to a preferred embodiment of the present invention241Pulse height spectrum of the self-supporting CdZnTe thick-film radiation detector stripped from the Am gamma-ray source AlN substrate.
FIG. 7 shows comparative example 60KeV241Pulse height spectrum of self-supporting CdZnTe thick film radiation detector stripped from Am gamma ray source glass substrate.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example one
In this embodiment, a self-supporting CdZnTe thick film structure peeled off from an AlN substrate is prepared by first epitaxially growing a CdZnTe film on the surface of the AlN substrate to obtain a CdZnTe/AlN composite structure in which the CdZnTe film and the AlN substrate are combined. And separating the CZT thick film from the AlN substrate for 5min by using an ultrasonic method to obtain a self-supporting CdZnTe thick film structure. The CdZnTe film has a thickness of 600 μm and the AlN substrate has a thickness of 500 nm.
In this embodiment, the preparation method of the self-supporting CdZnTe thick film structure component with AlN substrate lift-off in this embodiment includes the following steps:
a. substrate pretreatment:
respectively ultrasonically cleaning an AlN substrate with the thickness of 500nm for 30min by using acetone, alcohol and deionized water, removing impurities and organic matters on the surface of the AlN substrate, blow-drying by using nitrogen, and putting into a magnetron sputtering reaction chamber to serve as a substrate for later use;
and b, growth process of the CdZnTe film:
opening a close-space sublimation cavity, putting the AlN substrate pretreated in the step a into the cavity, starting a mechanical pump to vacuumize, pumping the air pressure in the sublimation chamber to 5Pa, then starting a halogen lamp, and respectively heating the sublimation source and the substrate to 670 ℃ and 490 ℃ at the heating rate of 50 ℃/min;
then adopting a near space sublimation method, continuously growing the CdZnTe film material on the surface of the AlN substrate for 180mins, then closing the halogen lamp, cooling the CdZnTe film material growing on the substrate to room temperature, closing the mechanical pump, and taking out the AlN substrate loaded with the CdZnTe film material with the thickness of 600 mu m, thereby obtaining a CdZnTe/AlN composite structure combined by the CdZnTe film and the AlN substrate;
c, stripping the CdZnTe film:
and (3) carrying out ultrasonic treatment on the CdZnTe/AlN composite structure for 5min by an ultrasonic method to obtain a self-supporting CdZnTe thick film structure separated from the AlN substrate.
In this embodiment, a structural device is formed by combining a gold electrode layer with a thickness of 100nm on the surface and the interface of the self-supporting CdZnTe thick film in this embodiment, so as to form an Au/CdZnTe/Au composite structural device, which is used as a gamma ray detector for the self-supporting CdZnTe thick film.
In this embodiment, the method for manufacturing a composite structure device in this embodiment includes the following steps:
preparing a gold electrode layer with the thickness of 100nm on the surface and the interface of the self-supporting CdZnTe thick film by adopting an evaporation method to obtain an Au/CdZnTe/Au structural device; then in N2In the atmosphere and under the condition of the annealing temperature of 400 ℃, the Au/CdZnTe/Au structural device is annealed for 100s, so that the functional layer connecting interface of the Au/CdZnTe/Au structural device forms ohmic contact, and the self-supporting CdZnTe/thick-film gamma-ray detector is prepared. The method for preparing the high-quality self-supporting CdZnTe thick-film gamma-ray detector is used for preparing the high-quality self-supporting CdZnTe thick-film structural component. Realizes the forming and the rapid preparation of the large-size CdZnTe thick film, improves the production efficiency and saves the production cost.
In this embodiment, a device with the structure of this embodiment is applied, and the gamma-ray detector with the self-supporting CdZnTe thick film peeled off from the AlN substrate has a relatively high resistivity, low leakage current under high electric field conditions, suppressed noise, and high gamma-ray cut-off capability and quantum efficiency. In the embodiment, the self-supporting CdZnTe thick-film gamma ray detector is utilized, so that the gamma ray detector has high cut-off capability and high detection quantum efficiency; within the energy range of 10-100 keV, the energy detection efficiency of the self-supporting CdZnTe thick-film gamma-ray detector is not lower than 90%.
Comparative example:
in the comparative example, the self-supporting CdZnTe thick film structure device stripped from the Glass substrate firstly epitaxially grows a CdZnTe film on the surface of the Glass substrate to obtain a CdZnTe/Glass composite structure combining the CdZnTe film and the Glass substrate. And separating the CZT thick film from the glass substrate for 5min by using an ultrasonic method to obtain a self-supporting CdZnTe thick film structure. The CdZnTe film has a thickness of about 400 μm and the AlN substrate has a thickness of 500 nm. And combining a gold electrode layer with the thickness of 100nm on the surface and the interface of the self-supporting CdZnTe thick film stripped on the glass substrate of the comparative example to form an Au/CdZnTe/Au composite structure device which is used as a self-supporting CdZnTe thick film gamma ray detector stripped on the glass substrate.
Experimental test analysis:
with reference to the above examples and comparative examples, the self-supporting CdZnTe/thick film gamma ray detector peeled off from the AlN substrate prepared in the examples and the self-supporting CdZnTe/thick film gamma ray detector peeled off from the glass substrate prepared in the comparative examples are illustrated in the drawings obtained by testing with an experimental instrument as follows:
FIG. 1 is an XRD pattern of a self-supporting CdZnTe thick film structure material stripped from an AlN substrate according to an embodiment of the invention. It can be seen that the CdZnTe peak position is 23.879 degrees, which is the (111) peak of CdZnTe, and the CdZnTe has better preferred orientation along the (111) crystal plane and a full width at half maximum of 0.180 degrees.
FIG. 2 is an XRD pattern of a free-standing CdZnTe thick film structured material exfoliated on a comparative example glass substrate. 23.800 DEG is the (111) peak of CdZnTe, has a full width at half maximum of 0.207 DEG, and has relatively poor preferred orientation.
FIG. 3 is an SEM image of the surface of a self-supporting CdZnTe thick film structure stripped on an AlN substrate according to an embodiment of the invention. The CdZnTe film grows well on the AlN substrate, the particles are formed, the size of the crystal particles is larger, and the average particle size is 100 mu m.
FIG. 4 is an I-T curve diagram of an Au/CdZnTe/Au composite structure device stripped on an AlN substrate under the irradiation of ultraviolet light in a 254nm solar dead zone in the embodiment of the invention. It can be seen that the current is periodically changed with the light-dark condition, the light-dark current ratio reaches nearly 1000 times, and the body leakage current of the Au/CdZnTe/Au composite structure device is lower.
FIG. 5 is an I-T curve diagram of an Au/CdZnTe/Au composite structure device stripped on a glass substrate of a comparative example under the irradiation condition of ultraviolet light in a 254nm solar dead zone. The light dark current is relatively small and is about 4.5 times, and the bulk leakage current of the Au/CdZnTe/Au composite structure device is relatively high.
FIG. 6 shows 60KeV according to an embodiment of the present invention241Pulse height spectrum of the self-supporting CdZnTe thick-film radiation detector stripped from the Am gamma-ray source AlN substrate. The detector has a good response with an energy resolution of about 13.6%.
FIG. 7 shows comparative example 60KeV241Pulse height spectrum of self-supporting CdZnTe thick film radiation detector stripped from Am gamma ray source glass substrate. The figure shows only one strong noise peak, and the response peak of the thick film radiation detector is not found.
In summary, the embodiments of the present invention provide a self-supporting CdZnTe thick film gamma ray detector with high detection efficiency and being peeled off from an AlN substrate and a method for manufacturing the same, in which a CdZnTe film is grown on the AlN substrate and a self-supporting CdZnTe thick film gamma ray detector is manufactured, so that high detection efficiency for gamma rays is achieved. The preparation method of the self-supporting CdZnTe thick film gamma ray detector with high detection efficiency stripped from the AlN substrate provided by the embodiment of the invention comprises four main steps of substrate pretreatment, growth process of the CdZnTe thick film, stripping process of the CdZnTe thick film and electrode manufacturing of the self-supporting CdZnTe thick film gamma ray detector. The method of the embodiment of the invention can quickly grow the high-quality CdZnTe film with large area and low defect density on the AlN substrate, and the gamma ray detector prepared by the high-detection-efficiency self-supporting CdZnTe thick film structure stripped on the AlN substrate has lower leakage current and noise under the room temperature condition and higher cut-off capability and detection quantum efficiency on gamma rays.
In a word, the preparation method of the self-supporting CdZnTe thick film gamma ray detector with high detection efficiency comprises four main steps of substrate pretreatment, a growth process of a CdZnTe film, a stripping process of the CdZnTe film and electrode manufacturing of the self-supporting CdZnTe thick film gamma ray detector. The method of the invention grows the CdZnTe thick film on the single crystal film substrate with high thermal conductivity, the high thermal conductivity of the substrate can promote the nucleation of CZT crystal grains, and further the CdZnTe thick film with large area and low defect concentration is obtained.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.
Claims (6)
1. The utility model provides a high detection efficiency self-supporting CdZnTe thick film structure of peeling off on AlN basement which characterized in that: firstly, growing and preparing a CdZnTe thick film on an AlN substrate to obtain a CdZnTe/AlN composite structure combining the CdZnTe thick film and the AlN substrate, and separating the CdZnTe thick film from the AlN substrate for at least 5min by using an ultrasonic method to obtain a self-supporting CdZnTe thick film structure.
2. The high detection efficiency self-supporting CdZnTe thick film structure exfoliated on AlN substrate according to claim 1, wherein: the deposition thickness of the CdZnTe thick film is not more than 600 mu m.
3. A preparation method of the high detection efficiency self-supporting CdZnTe thick film structure stripped on the AlN substrate according to claim 1, which is characterized by comprising the following steps:
a. substrate pretreatment:
respectively ultrasonically cleaning the AlN substrate by using acetone, alcohol and deionized water for at least 30 minutes, washing off impurities and organic matters on the surface of the AlN substrate, blow-drying by using nitrogen, and putting into a magnetron sputtering reaction chamber to be used as a substrate for later use;
and b, growth process of the CdZnTe film:
opening a close-space sublimation cavity, putting the AlN substrate pretreated in the step a into the cavity, starting a mechanical pump to pump vacuum, pumping the air pressure in the sublimation chamber to be not higher than 5Pa, then starting a halogen lamp, and respectively heating the sublimation source and the substrate to be not lower than 670 ℃ and not lower than 490 ℃ at the heating rate of not higher than 50 ℃/min;
then adopting a near space sublimation method, continuously growing a CdZnTe film material on the surface of the AlN substrate for at least 180mins, then closing the halogen lamp, cooling the CdZnTe film material growing on the substrate to room temperature, closing the mechanical pump, and taking out the AlN substrate loaded with the CdZnTe film material, thereby obtaining a CdZnTe/AlN composite structure combined by the CdZnTe film and the AlN substrate;
c, stripping the CdZnTe film:
and (3) carrying out ultrasonic treatment on the CdZnTe/AlN composite structure for at least 5 minutes by an ultrasonic method to obtain a self-supporting CdZnTe thick film structure separated from the AlN substrate.
4. A gamma ray detection device, characterized by: preparing a gold electrode layer with the thickness of not more than 100nm on the self-supporting CdZnTe thick film interface stripped on the AlN substrate according to claim 1 to form a CdZnTe/Au structural device which is used as a self-supporting CdZnTe thick film gamma ray detector.
5. A method for preparing a gamma ray detector device according to claim 4, comprising the steps of:
preparing a gold electrode layer with the thickness of not more than 100nm on the surface and the interface of the self-supporting CdZnTe thick film by adopting an evaporation method to obtain an Au/CdZnTe/Au structural device; then in N2In the atmosphere and under the condition of the annealing temperature not lower than 400 ℃, the Au/CdZnTe/Au structural device is subjected to rapid annealing treatment for at least 100s, so that the Au/CdZnTe/Au structural device forms ohmic contact on the connection interface of the functional layer, and the self-supporting CdZnTe thick-film gamma-ray detector is prepared.
6. The use of the gamma-ray detector device as claimed in claim 4, wherein the self-supporting CdZnTe thick-film gamma-ray detector has high cut-off capability and high detection quantum efficiency for gamma rays; within the energy range of 10-100 keV, the energy detection efficiency of the self-supporting CdZnTe thick-film gamma-ray detector is not lower than 90%.
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