CN113151901A - CZT crystal and post-processing method thereof, CZT wafer, nuclear radiation detection device and preparation method thereof - Google Patents
CZT crystal and post-processing method thereof, CZT wafer, nuclear radiation detection device and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The invention relates to a CZT crystal and a post-processing method thereof, a CZT wafer, a nuclear radiation detection device and a preparation method thereof. The post-processing method of the CZT crystal comprises the following steps: growing CZT crystal by using a moving heater method; the CZT crystal is firstly annealed in situ for 50-70 h at 870-930 ℃, then cooled to 400-420 ℃ within 50-80 h, and finally kept warm for 40-50 h at 400-420 ℃. According to the CZT crystal post-processing method, a thermal migration mechanism is utilized to eliminate thermal stress, Te inclusion and Te precipitation are reduced, the obtained CZT crystal is high in quality, the density of relevant defects such as Te inclusion is reduced, and the photoelectric performance of the CZT crystal when used for a detector is finally improved.
Description
Technical Field
The invention relates to the field of CZT crystal manufacturing, in particular to a CZT crystal and a post-processing method thereof, a CZT wafer, a nuclear radiation detection device and a preparation method thereof.
Background
Cadmium zinc telluride (CdZnTe), hereinafter referred to as CZT, is an important compound semiconductor material that can be used to detect high energy particle rays, such as gamma rays and X-rays, due to its high average atomic number. Compared with common semiconductor materials such as silicon (Si), germanium (Ge) and the like, CZT has higher intrinsic resistivity and larger forbidden bandwidth, and is the most ideal semiconductor material for manufacturing room-temperature ray and ray detectors and equal infrared thin film epitaxial substrates. The ideal room-temperature nuclear radiation semiconductor material is concerned in many fields, is suitable for the fields of celestial body physics, safety inspection, ecological environmental protection, nuclear medicine, clinical medicine and the like, and becomes an upgrading and updating product for replacing the traditional detector and the scintillator detector.
CZT is used as a II-VI compound semiconductor material, although the growing method is many, due to the fact that the CZT crystal has a high melting point, large thermal stress and high component vapor pressure at the melting point, and due to various reasons that the CZT crystal has low thermal conductivity, a growing interface is difficult to control, a Zn component is segregated and the like, the CZT crystal quality is difficult to guarantee, particularly the CZT crystal with high quality and large size is difficult to grow, the wide application of a CZT nuclear radiation detector is limited by crystal performance and growing cost, and therefore the CZT crystal preparation technology needs to be further developed and perfected.
Defects in CZT crystals have great influence on CZT crystal quality and CZT nuclear radiation detectors prepared from CZT wafers, particularly Te related Te inclusion and Te precipitation can affect the performance of the CZT nuclear radiation detectors, and a large amount of large-size Te inclusion or Te precipitation can cause reduction of energy resolution and reduction of electron mobility life product and drift distance. Therefore, the preparation of CZT crystal with less Te inclusion, less Te precipitation and high crystal quality has important significance.
Disclosure of Invention
Based on this, it is necessary to provide a post-treatment method of CZT crystals, which can reduce the amount of Te inclusions and Te precipitates in the CZT crystals and improve the crystal quality.
In addition, a CZT crystal, a CZT wafer and a preparation method thereof, and a CZT nuclear radiation detection device and a preparation method thereof are also needed to be provided.
A post-processing method of CZT crystal comprises the following steps:
growing CZT crystal by using a moving heater method;
the CZT crystal is firstly subjected to in-situ annealing treatment for 50-70 h at 870-930 ℃, then the temperature is reduced to 400-420 ℃ within 50-80 h, and finally the temperature is kept for 40-50 h at 400-420 ℃.
In one embodiment, the growing the CZT crystal using a moving heater method comprises:
cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material;
placing seed crystals, the Te-rich polycrystalline material and the CZT polycrystalline material in a reaction container from bottom to top in sequence;
and growing for 400-450 h at 850-950 ℃ by adopting a moving heater method to obtain the CZT crystal.
In one embodiment, the reaction vessel is a quartz vessel with a carbon film plated inner surface.
A CZT crystal is obtained after being processed by the CZT crystal post-processing method.
A preparation method of a CZT wafer comprises the following steps:
obtaining the CZT crystal;
and selecting single crystals in the CZT crystal, and slicing to prepare the CZT wafer.
In one embodiment, the method further comprises the step of mechanically and chemically polishing the CZT wafer.
In one embodiment, the step of mechanically polishing comprises: and respectively polishing the CZT wafer by using a polishing solution containing magnesium oxide with the particle size of 0.5 mu m and a polishing solution containing aluminum oxide with the particle size of 0.05 mu m for 20-30 min, and then washing and drying by using water.
In one embodiment, the step of chemically polishing comprises: and (3) placing the CZT wafer after mechanical polishing treatment in a bromomethanol solution with the mass percentage concentration of 2% and a bromoethylene glycol solution with the mass percentage concentration of 2% in sequence for chemical polishing for 2-3 min, and then cleaning and drying with methanol.
A CZT wafer is prepared by the preparation method of the CZT wafer.
In one embodiment, the CZT wafer has dimensions of 10mm by 2 mm.
The utility model provides a nuclear radiation detection device, includes CZT wafer, gold electrode and circuit assembly, gold electrode deposition is in CZT wafer both sides, circuit assembly with the gold electrode electricity is connected, CZT wafer is foretell CZT wafer.
In one embodiment, the thickness of the gold electrode on one side of the CZT wafer is 70nm to 100 nm.
A preparation method of a nuclear radiation detection device comprises the following steps:
depositing gold electrodes on two sides of the CZT wafer, wherein the CZT wafer is the CZT wafer;
and electrically connecting the gold electrode with a circuit component to prepare the nuclear radiation detection device.
In one embodiment, the gold electrodes are deposited on both sides of the CZT wafer by electron beam evaporation.
In one embodiment, the step of depositing gold electrodes on both sides of the CZT wafer further comprises: and sequentially carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone, and then cleaning the CZT wafer for 2-5 times by using deionized water.
According to the CZT crystal post-processing method, the CZT crystal grown by the moving heater method is subjected to in-situ annealing treatment, then is subjected to gradient cooling, is kept at a low temperature for a certain time, the temperature and the time in each step are controlled, the thermal stress is eliminated by using a thermal migration mechanism, Te inclusion and Te precipitation are reduced, the obtained CZT crystal is high in quality, the density of relevant defects such as Te inclusion is reduced, and the photoelectric performance of the CZT crystal when used for a detector is finally improved.
Drawings
FIG. 1 is a process flow diagram of a method for post-processing CZT crystals in accordance with one embodiment;
FIG. 2 is a schematic diagram of a CZT crystal grown by a moving heater method and a schematic diagram of a temperature field;
FIG. 3 is a temperature profile during the preparation and post-treatment of CZT crystals of example 1;
FIG. 4 is a graph of Te inclusion distribution of CZT wafers of example 1 and comparative example 1, as scanned under an infrared transmission optical microscope;
fig. 5 is a graph of voltage current data for nuclear radiation detection devices prepared in example 1 and comparative example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings. The detailed description sets forth the preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In order to solve the problem that the performance of a nuclear radiation detector is influenced by more Te inclusions and Te precipitates in CZT crystals in the traditional technology, the invention provides a post-processing method of CZT crystals, so as to obtain uniform CZT crystals with high quality, high resistance and high single crystal rate.
Specifically, referring to fig. 1, a post-processing method of CZT crystal according to an embodiment includes the following steps:
step S110: and growing the CZT crystal by adopting a moving heater method.
In one embodiment, step S110 specifically includes:
cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material;
putting seed crystals, a Te-rich polycrystalline material and a CZT polycrystalline material into a reaction vessel from bottom to top in sequence;
growing for 400-450 h at 850-950 ℃ by adopting a moving heater method to obtain CZT crystal.
Specifically, In-element is doped In the synthesized CZT polycrystalline material and Te-rich polycrystalline material to compensate Cd vacancy defect generated by deviation of stoichiometric ratio In the crystal growth process.
In one embodiment, the step of synthesizing the CZT polycrystalline material comprises: and (3) packaging Cd, Zn, Te and In according to a certain stoichiometric ratio under a vacuum condition to prepare the CZT polycrystal material.
The step of synthesizing the Te-rich polycrystalline material comprises: and (3) packaging the CZT polycrystal material and high-purity Te under a vacuum condition to synthesize the Te-rich polycrystal material.
It is understood that in the present embodiment, the method for synthesizing CZT polycrystalline material and Te-rich polycrystalline material may be a method commonly used in the art, and will not be described herein.
Specifically, in the present embodiment, the reaction vessel used is a quartz vessel having an inner surface coated with a carbon film. The reaction between the high-temperature CZT crystal melt and the quartz container can be effectively blocked by plating the carbon film on the inner surface of the quartz container, and the growth of complete and high-quality single crystals is facilitated. Further, the reaction vessel is a high-purity (6N) quartz vessel, which is washed sequentially with acetone and aqua regia to remove organic and inorganic impurities on the surface, and then rinsed with deionized water and plated with a carbon film to serve as the reaction vessel in the present embodiment. Further, the reaction vessel was a quartz crucible having an inner surface coated with a carbon film.
Referring to fig. 2, fig. 2 is a schematic diagram of CZT crystal growth by a moving heater method and a schematic diagram of a temperature field. The moving heater method is a method for growing high-quality single crystals, and can grow high-quality single crystals with high purity, good component uniformity and low defect density at a temperature far lower than the melting point of the crystals. In the process of growing CZT crystals, CZT polycrystalline material, Te-rich polycrystalline material and seed crystals are sequentially placed in a crucible from top to bottom. The growth temperature field is shown on the right side of fig. 1 with a symmetrical and sharp peak to meet the requirement of equal temperature at the growth interface and the dissolution interface. Ideally, when the heater is at rest, the temperature at the growth interface and the dissolution interface are equal, the corresponding solute concentrations are also equal, the system is in an equilibrium state, and growth does not occur. When the heater moves upwards at a certain speed, the temperature at the growth interface at the lower end deviates to the low temperature direction, and the temperature at the dissolution interface at the upper end deviates to the high temperature direction, so that the solute concentration at the two solid-liquid interfaces changes, the concentration difference is caused, the balance of the system is broken, and the growth starts. Along with the slow movement of the heater, the CZT solute is continuously dissolved in the dissolution interface, enters the Te-rich melting zone and is transported to the lower growth interface for crystallization, so that the continuous growth of CZT crystals is realized.
Step S120: the CZT crystal is firstly annealed in situ for 50-70 h at 870-930 ℃, then the temperature is reduced to 400-420 ℃ within 50-80 h, and finally the temperature is preserved for 40-50 h at 400-420 ℃.
In one embodiment, the temperature of the in-situ annealing process is 870 ℃ to 930 ℃. For example, the temperature of the in-situ annealing treatment is 870 ℃, 900 ℃ or 930 ℃. The time of the in-situ annealing treatment is 50h, 60h or 70 h. According to the CZT crystal post-processing method, the CZT crystal grown by the moving heater method is subjected to in-situ annealing treatment, then is subjected to gradient cooling, and finally is kept at a low temperature for a certain time, thermal stress is eliminated by using a thermal migration mechanism, Te inclusion and Te precipitation are reduced, the obtained CZT crystal is high in quality, the density of relevant defects such as Te inclusion is reduced, and the photoelectric performance of the CZT crystal when used for a detector is finally improved. The prepared CZT crystal material has important significance and application prospect in the aspects of safety monitoring and radiation protection in the fields of public safety, military, nuclear industry, nuclear medicine, scientific research, aerospace and the like.
The invention also provides CZT crystal of an embodiment, which is obtained by processing the CZT crystal of the embodiment by the post-processing method. The CZT crystal has high quality, the density of relevant defects such as Te inclusion and the like is reduced, and the photoelectric performance of the CZT crystal when used for a detector is finally improved.
In one embodiment, the CZT crystal is 41mm in diameter and 135mm in height.
The invention also provides a method for preparing a CZT wafer, which comprises the following steps:
obtaining the CZT crystal;
and selecting single crystals in the CZT crystal, and carrying out slicing and scribing to prepare the CZT wafer.
Specifically, the CZT wafer has dimensions of 10mm × 10mm × 2 mm.
In one embodiment, the step of selecting a single crystal in the CZT crystal, and slicing and scribing specifically comprises: and taking the CZT crystal out of the reaction vessel. And observing the distribution condition of the crystal grains on the surface of the CZT crystal, determining the cutting direction of the wafer to be cut, using an inner circle slicer to cut the wafer, and scribing the wafer obtained by cutting into the size of 10mm multiplied by 2mm through a scribing machine.
Further, the preparation method of the CZT wafer further comprises the step of carrying out mechanical polishing and chemical polishing on the CZT wafer.
Specifically, the step of mechanically polishing comprises: and respectively polishing the CZT wafer by using a polishing solution containing magnesium oxide with the particle size of 0.5 mu m and a polishing solution containing aluminum oxide with the particle size of 0.05 mu m for 20-30 min, and then washing and drying by using water. The CZT wafer surface is flattened through the mechanical polishing, and surface defects such as tool marks, mechanical damage and the like left in the slicing and scribing process are eliminated.
In one embodiment, in the step of washing with water, ultrasonic washing is adopted. And in the drying step, a drying mode in a nitrogen atmosphere is adopted.
Specifically, the step of chemically polishing comprises: and (3) placing the CZT wafer after mechanical polishing treatment in a bromomethanol solution with the mass percentage concentration of 2% and a bromoethylene glycol solution with the mass percentage concentration of 2% in sequence for chemical polishing for 2-3 min, and then cleaning and drying with methanol.
And removing a damaged layer on the surface of the wafer caused by mechanical polishing through chemical polishing treatment. Residual bromine and other impurities on the surface of the CZT wafer can be removed by methanol cleaning. And in the drying step, a drying mode in a nitrogen atmosphere is adopted.
The invention also provides an embodiment of a CZT wafer. The CZT wafer is prepared by the method for preparing a CZT wafer according to the above embodiment. In one embodiment, the CZT wafer has dimensions of 10mm by 2 mm. The CZT wafer has high crystal quality and low density of relevant defects such as Te inclusion, and can be used for preparing a nuclear radiation detection device and improving the photoelectric property of the nuclear radiation detection device.
The invention also provides a nuclear radiation detection device of an embodiment, which comprises a CZT wafer, gold electrodes and a circuit assembly, wherein the gold electrodes are deposited on two sides of the CZT wafer, and the circuit assembly is electrically connected with the gold electrodes. The CZT wafer is the CZT wafer according to the above embodiment.
Specifically, on one side of the CZT crystal, the thickness of the gold electrode is 70nm to 100 nm.
In one embodiment, gold electrodes are deposited on both sides of the CZT wafer by electron beam evaporation.
Further, high-purity gold with the purity of 99.99999% is selected as the evaporation material of the gold electrode.
The CZT wafer of the nuclear radiation detection device has high crystal quality and low density of relevant defects such as Te inclusion, so that the nuclear radiation detection device has good photoelectric performance.
The invention also provides a preparation method of the nuclear radiation detection device, which comprises the following steps:
depositing gold electrodes on two sides of the CZT wafer;
and electrically connecting the gold electrode with the circuit component to prepare the nuclear radiation detection device.
Specifically, before the step of depositing gold electrodes on two sides of the CZT wafer, the method further comprises the following steps: and cleaning the CZT wafer. In one embodiment, the step of cleaning comprises: and (3) carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone in sequence, and then cleaning for 2-5 times by using deionized water.
Specifically, gold electrodes are deposited on both sides of the CZT wafer by means of electron beam evaporation. On one side of the CZT crystal, the thickness of the gold electrode is 70 nm-100 nm. Further, high-purity gold with the purity of 99.99999% is selected as the evaporation material of the gold electrode.
The preparation method of the nuclear radiation detection device is simple in process, and the CZT wafer which is high in crystal quality and small in density of relevant defects such as Te inclusion and the like is used as the raw material, so that the prepared nuclear radiation detection device is excellent in photoelectric performance.
The following are specific examples:
example 1
The post-treatment process of the CZT crystal in the embodiment is specifically as follows:
(1) cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material; placing seed crystals, a Te-rich polycrystalline material and a CZT polycrystalline material in a crucible from bottom to top in sequence; and growing for 400h at 900 ℃ by adopting a moving heater method to obtain the CZT crystal.
(2) And then heating the CZT crystal to 930 ℃ in situ for annealing treatment for 50h, then cooling the CZT crystal to 400 ℃ at a constant speed within 50h, and finally preserving heat at 400 ℃ for 40h, and cooling to obtain the post-treated CZT crystal.
Specifically, the temperature profile during the preparation and post-treatment of the CZT crystal of the present example is shown in fig. 3.
The process for preparing the CZT wafer of the present example is specifically as follows:
(1) and taking the post-processed CZT crystal out of the crucible, observing the distribution condition of crystal grains on the surface of the crystal, selecting a single crystal with the largest crystal grain size in the CZT crystal, determining the cutting direction of a wafer to be sliced, slicing by using an internal diameter slicer, and scribing the wafer obtained by cutting into the size of 10mm multiplied by 2mm by using a dicing saw.
(2) Polishing the scribed CZT wafer with polishing solution containing magnesium oxide with particle size of 0.5 μm and polishing solution containing aluminum oxide with particle size of 0.05 μm for 25min until the surface is flat, ultrasonically cleaning the surface with deionized water, and performing N-phase polishing2And (5) drying in the atmosphere.
(3) The CZT wafer after mechanical polishing treatment is sequentially placed in a 2 mass percent bromomethanol solution and a 2 mass percent bromoethylene glycol solution for chemical polishing for 3min, then the CZT wafer is cleaned by methanol to remove bromine and other impurities remained on the surface, and finally N is added2And drying in the atmosphere to obtain the CZT wafer.
The preparation process of the nuclear radiation detector of the embodiment is specifically as follows:
(1) and (3) carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone in sequence, and then cleaning the CZT wafer for 5 times by using deionized water until the CZT wafer is clean.
(2) High-purity gold with the purity of 99.99999 percent is selected as a raw material, and gold electrodes with the thickness of 93nm are respectively deposited on the two sides of the CZT wafer in an electron beam evaporation deposition mode.
(3) And electrically connecting the gold electrode with the circuit component to prepare the nuclear radiation detection device.
Example 2
The post-treatment process of the CZT crystal in the embodiment is specifically as follows:
(1) cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material; placing seed crystals, a Te-rich polycrystalline material and a CZT polycrystalline material in a crucible from bottom to top in sequence; and growing for 400h at 900 ℃ by adopting a moving heater method to obtain the CZT crystal.
(2) Then carrying out in-situ annealing treatment on the CZT crystal at 870 ℃ for 60h, then reducing the temperature to 420 ℃ at a constant rate within 70h, finally carrying out heat preservation at 420 ℃ for 50h, and reducing the temperature to obtain the post-treated CZT crystal.
The process for preparing the CZT wafer of the present example is specifically as follows:
(1) and taking the post-processed CZT crystal out of the crucible, observing the distribution condition of crystal grains on the surface of the crystal, selecting a single crystal with the largest crystal grain size in the CZT crystal, determining the cutting direction of a wafer to be sliced, slicing by using an internal diameter slicer, and scribing the wafer obtained by cutting into the size of 10mm multiplied by 2mm by using a dicing saw.
(2) Polishing the scribed CZT wafer with polishing solution containing magnesium oxide with particle size of 0.5 μm and polishing solution containing aluminum oxide with particle size of 0.05 μm for 25min until the surface is flat, ultrasonically cleaning the surface with deionized water, and performing N-phase polishing2And (5) drying in the atmosphere.
(3) The CZT wafer after mechanical polishing treatment is sequentially placed in a 2 mass percent bromomethanol solution and a 2 mass percent bromoethylene glycol solution for chemical polishing for 3min, then the CZT wafer is cleaned by methanol to remove bromine and other impurities remained on the surface, and finally N is added2And drying in the atmosphere to obtain the CZT wafer.
The preparation process of the nuclear radiation detector of the embodiment is specifically as follows:
(1) and (3) carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone in sequence, and then cleaning the CZT wafer for 5 times by using deionized water until the CZT wafer is clean.
(2) High-purity gold with the purity of 99.99999 percent is selected as a raw material, and gold electrodes with the thickness of 93nm are respectively deposited on the two sides of the CZT wafer in an electron beam evaporation deposition mode.
(3) And electrically connecting the gold electrode with the circuit component to prepare the nuclear radiation detection device.
Example 3
The post-treatment process of the CZT crystal in the embodiment is specifically as follows:
(1) cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material; placing seed crystals, a Te-rich polycrystalline material and a CZT polycrystalline material in a crucible from bottom to top in sequence; and growing for 400h at 900 ℃ by adopting a moving heater method to obtain the CZT crystal.
(2) And then carrying out in-situ annealing treatment on the CZT crystal at 900 ℃ for 70h, then reducing the temperature to 450 ℃ at a constant rate within 80h, and finally carrying out heat preservation at 450 ℃ for 60h, and reducing the temperature to obtain the post-treated CZT crystal.
The process for preparing the CZT wafer of the present example is specifically as follows:
(1) and taking the post-processed CZT crystal out of the crucible, observing the distribution condition of crystal grains on the surface of the crystal, selecting a single crystal with the largest crystal grain size in the CZT crystal, determining the cutting direction of a wafer to be sliced, slicing by using an internal diameter slicer, and scribing the wafer obtained by cutting into the size of 10mm multiplied by 2mm by using a dicing saw.
(2) Polishing the scribed CZT wafer with polishing solution containing magnesium oxide with particle size of 0.5 μm and polishing solution containing aluminum oxide with particle size of 0.05 μm for 25min until the surface is flat, ultrasonically cleaning the surface with deionized water, and performing N-phase polishing2And (5) drying in the atmosphere.
(3) The CZT wafer after mechanical polishing treatment is sequentially placed in a 2 mass percent bromomethanol solution and a 2 mass percent bromoethylene glycol solution for chemical polishing for 3min, then the CZT wafer is cleaned by methanol to remove bromine and other impurities remained on the surface, and finally N is added2And drying in the atmosphere to obtain the CZT wafer.
The preparation process of the nuclear radiation detector of the embodiment is specifically as follows:
(1) and (3) carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone in sequence, and then cleaning the CZT wafer for 5 times by using deionized water until the CZT wafer is clean.
(2) High-purity gold with the purity of 99.99999 percent is selected as a raw material, and gold electrodes with the thickness of 93nm are respectively deposited on the two sides of the CZT wafer in an electron beam evaporation deposition mode.
(3) And electrically connecting the gold electrode with the circuit component to prepare the nuclear radiation detection device.
Comparative example 1
The CZT crystal of comparative example 1 was prepared as follows:
cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material; placing seed crystals, a Te-rich polycrystalline material and a CZT polycrystalline material in a crucible from bottom to top in sequence; and growing for 400h at 900 ℃ by adopting a moving heater method to obtain the CZT crystal.
The CZT wafer of comparative example 1 was prepared as follows:
(1) taking the prepared CZT crystal out of the crucible, selecting the single crystal with the largest crystal grain size in the CZT crystal by observing the distribution condition of crystal grains on the surface of the crystal, determining the cutting direction of a wafer to be cut, cutting the wafer by using an inner circle slicer, and cutting the wafer obtained by cutting into the size of 10mm multiplied by 2mm by using a dicing saw.
(2) Polishing the scribed CZT wafer with polishing solution containing magnesium oxide with particle size of 0.5 μm and polishing solution containing aluminum oxide with particle size of 0.05 μm for 25min until the surface is flat, ultrasonically cleaning the surface with deionized water, and performing N-phase polishing2And (5) drying in the atmosphere.
(3) The CZT wafer after mechanical polishing treatment is sequentially placed in a 2 mass percent bromomethanol solution and a 2 mass percent bromoethylene glycol solution for chemical polishing for 3min, then the CZT wafer is cleaned by methanol to remove bromine and other impurities remained on the surface, and finally N is added2And drying in the atmosphere to obtain the CZT wafer.
The preparation process of the nuclear radiation detecting device of comparative example 1 is specifically as follows:
(1) and (3) carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone in sequence, and then cleaning the CZT wafer for 5 times by using deionized water until the CZT wafer is clean.
(2) And respectively depositing gold electrodes with the thickness of 93nm on two sides of the CZT wafer by adopting an electron beam evaporation deposition mode.
(3) And electrically connecting the gold electrode with the circuit component to prepare the nuclear radiation detection device.
The following are test sections:
the physically mechanically polished and chemically etched CZT wafers of example 1 and comparative example 1 were scanned using an infrared transmission optical microscope to obtain high resolution and sharp images of defects in transmission mode, with a 5mm x 5mm area of the in vivo inclusion scan mosaic at 200 x, as shown in fig. 4. The distribution of inclusions can be clearly seen from the images, and the software can be used to analyze the size of the inclusions, count and calculate the density of the inclusions to obtain experimental data as shown in table 1, wherein the average density is the number of Te inclusions with a certain size in a unit area.
In order to clearly observe the distribution characteristics of inclusions and etch pits, the magnification of the infrared transmission optical microscope was set at 200 times, and the field of view was 5mm × 5 mm. In fig. 4A, B, C, D is the Te inclusion distribution for the CZT wafers of comparative example 1 and E, F, G, H is the Te inclusion distribution for the CZT wafers of example 1. It can be more clearly seen from fig. 4 that the large size Te inclusion density of the CZT wafer of example 1 is significantly lower than that of the CZT wafer of comparative example 1.
TABLE 1 comparison of mean density of Te inclusions in CZT wafers of examples and comparative examples
| Te of less than or equal to 6 mu m is mixed with the average density | Mean density of Te inclusions > 6 μm | |
| Example 1 | 100cm-2 | 9.7cm-2 |
| Comparative example 1 | 388cm-2 | 1.9cm-2 |
As can be seen from table 1 and fig. 4, the post-treatment method of CZT crystal in example 1, which is used to perform in-situ annealing heat treatment, gradient heat treatment and low-temperature constant-temperature heat treatment after growth of CZT crystal, enables the average density of Te inclusions after orientation, slicing, scribing, physical polishing and chemical etching of the prepared CZT crystal to be significantly lower than the density of Te inclusions of CZT wafers prepared in comparative example 1 without post-treatment.
The photoelectric properties of the nuclear radiation detecting devices prepared in example 1 and comparative example 1 were measured by a voltage-current test (I-V) method, and the experimental data shown in fig. 5 below were obtained.
As can be seen from FIG. 5, the leakage current passing through example 1 is smaller than that of comparative example 1, and meets the requirement that the CdZnTe nuclear radiation detector has small leakage current for CdZnTe crystals.
Compared with the traditional growth mode, the in-situ annealing heat treatment, the gradient heat treatment and the low-temperature constant-temperature treatment processes after the crystal growth adopted in the embodiment reduce the density of the Te inclusions of the CZT wafer, and finally improve the photoelectric performance of the detector. The CZT crystal material prepared by the embodiment has important significance and application prospect in the aspects of safety monitoring and radiation protection in the fields of public safety, military, nuclear industry, nuclear medicine, scientific research, aerospace and the like.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (15)
1. A post-processing method of CZT crystal is characterized by comprising the following steps:
growing CZT crystal by using a moving heater method;
the CZT crystal is firstly subjected to in-situ annealing treatment for 50-70 h at 870-930 ℃, then the temperature is reduced to 400-420 ℃ within 50-80 h, and finally the temperature is kept for 40-50 h at 400-420 ℃.
2. The method of post-processing CZT crystals according to claim 1, wherein the step of growing CZT crystals using a moving heater method comprises:
cd, Zn, Te and In with the purity not lower than 99.99999 percent are used as raw materials to synthesize a CZT polycrystal material and a Te-rich polycrystal material;
placing seed crystals, the Te-rich polycrystalline material and the CZT polycrystalline material in a reaction container from bottom to top in sequence;
and growing for 400-450 h at 850-950 ℃ by adopting a moving heater method to obtain the CZT crystal.
3. The method of post-processing CZT crystal according to claim 2, wherein the reaction vessel is a quartz vessel having an inner surface coated with a carbon film.
4. A CZT crystal obtained by the post-treatment method of a CZT crystal according to any one of claims 1 to 3.
5. A method for preparing a CZT wafer is characterized by comprising the following steps:
obtaining the CZT crystal of claim 4;
and selecting single crystals in the CZT crystal, and slicing to prepare the CZT wafer.
6. The method of manufacturing a CZT wafer according to claim 5, further comprising the step of mechanically and chemically polishing the CZT wafer.
7. The method of manufacturing a CZT wafer according to claim 6, wherein the step of mechanically polishing comprises: and respectively polishing the CZT wafer by using a polishing solution containing magnesium oxide with the particle size of 0.5 mu m and a polishing solution containing aluminum oxide with the particle size of 0.05 mu m for 20-30 min, and then washing and drying by using water.
8. The method for preparing a CZT wafer according to claim 6 or 7, wherein the step of chemically polishing comprises: and (3) sequentially placing the CZT wafer after mechanical polishing treatment in a bromomethanol solution with the mass percentage concentration of 2% and a bromoethylene glycol solution with the mass percentage concentration of 2% for chemical polishing for 2-3 min, and then cleaning and drying with methanol.
9. A CZT wafer prepared by the method of any one of claims 5 to 8.
10. The CZT wafer of claim 9, wherein the CZT wafer has dimensions of 10mm x 2 mm.
11. A nuclear radiation detection device comprising a CZT wafer, gold electrodes deposited on both sides of the CZT wafer, and a circuit assembly electrically connected to the gold electrodes, wherein the CZT wafer is the CZT wafer of claim 9 or claim 10.
12. The nuclear radiation detection device of claim 11, wherein the gold electrode has a thickness of 70nm to 100nm on one side of the CZT wafer.
13. A preparation method of a nuclear radiation detection device is characterized by comprising the following steps:
depositing gold electrodes on both sides of a CZT wafer, said CZT wafer being a CZT wafer according to claim 9 or 10;
and electrically connecting the gold electrode with a circuit component to prepare the nuclear radiation detection device.
14. The method of claim 13, wherein the gold electrodes are deposited on both sides of the CZT wafer by electron beam evaporation.
15. The method for fabricating a nuclear radiation detection device according to claim 13, wherein the step of depositing gold electrodes on both sides of the CZT wafer further comprises: and sequentially carrying out ultrasonic cleaning on the CZT wafer by using alcohol and acetone, and then cleaning the CZT wafer for 2-5 times by using deionized water.
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