CN114808133A - Doping method for optimizing vacancy defect in compound semiconductor crystal - Google Patents
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Abstract
The invention provides a doping method for optimizing vacancy defects In compound semiconductor crystals, which solves the technical problem of poor optimization effect of vacancy defects In the existing compound semiconductor crystals.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a doping method for optimizing a vacancy defect in a compound semiconductor crystal.
Background
Semiconductor nuclear radiation detectors, which can provide a compact configuration and excellent resolution of radiation signals, have been widely used in the fields of environmental monitoring, medical imaging, industrial nondestructive testing, security anti-terrorism, celestial physics, and high-energy physics. Among semiconductor radiation detectors developed in recent years, compound semiconductor cadmium zinc telluride (CdZnTe or CZT) crystals and CdTe crystals have very excellent photoelectric properties and are considered as the most promising room-temperature X-ray and gamma-ray detector materials.
Both CZT and CdTe crystals generally require high resistivity, large carrier mobility and lifetime in order to achieve good detection performance. These factors are closely related to the deviation of the stoichiometric ratio of the elements, doping, and impurities. The unavoidable deviation of the melt stoichiometry due to an excessively high Cd partial pressure during growth introduces Cd vacancies (V) Cd - ) Isodefect, usually using In element doped In ppb to ppm level to compensate Cd vacancy, producing donor In with shallow energy level Cd + To balance the V of primary ionization Cd - Thereby achieving high resistance.
In is taken as the most appropriate CdTe and CZT crystal doping element, the key performances such as the resistivity, the carrier concentration, the mobility life and the like of the crystal can be obviously improved theoretically, however, the doping efficiency of In is limited by the existing doping mode, the defects such as Cd vacancy and the like are still too high, and the ideal doping performance cannot be obtained, so that controversial still exists for the effect of In doping CZT and CdTe crystals. Such as: the literature "Bassani F., Tatarenko S., Saminadayar K., et al 1-x Zn x Te by molecular-beam epitaxy:Uniformly and planar-doped layers,quantum wells,and superlattices[J]Journal of Applied Physics, "doping In into CdTe and CZT polycrystals to epitaxially grow CZT and CdTe thin films, indicates that low In doped crystals cannot achieve satisfactory performance due to residual acceptor impurities (e.g., Cd vacancies), whereas at high In doping concentrations, more neutral In can occur due to defect reactions Cd + -V Cd - The equi-composite defects (collectively referred to as a-centers) greatly reduce the effective doping amount of In atoms and reduce the doping effect. Similarly, the documents "m.fielderle, a.fauler, j.konrath, v.babentsov, j.franc and r.b.james," compatibility of unaided and coped high resistance CdTe and (Cd, Zn) Te detector Crystals, "In IEEE Transactions on Nuclear science," adopt the briding of Cd, Zn, Te, In, etc. raw materials, and grow CdTe and CZT Crystals with high resistivity by the bridgman melt method, which also indicates that In doping needs to reduce Cd vacancies while avoiding excessive a-center concentration to increase the electrical mobility lifetime product, thereby increasing the electrical mobility lifetime productMore excellent radiation detection performance can be obtained.
In view of the above, it is necessary to provide an optimized doping method to overcome the vacancy defect.
Disclosure of Invention
The invention aims to solve the technical problem of poor optimization effect of vacancy defects in the existing compound semiconductor crystal, and provides a doping method for optimizing the vacancy defects in the compound semiconductor crystal, in particular to a method for solving the overhigh Cd vacancy defect in CZT and CdTe crystals, which is also a novel doping method for a semiconductor for radiation detection.
The conception of the invention is as follows:
through the analysis of the prior art, it can be seen that when the conventional In doping method is adopted, i.e. In is directly mixed into raw materials such as Cd, Zn, Te and the like, or In is added into CdTe and CZT polycrystalline materials, the optimal In doping effect cannot be obtained, and the In doping efficiency is not high. This is because the doping efficiency and effect of In is closely related to the actual concentration of In doping into the crystal to replace Cd vacancies. The low In doping concentration can not well neutralize Cd vacancy defect, the main point defect In the crystal is Cd vacancy, and the Cd vacancy still exists In the CZT and CdTe crystal with high In doping concentration, because In shows strong self-compensation action during the doping process to form an In-related defect complex (A-center), and the doping efficiency of In element is limited. In is still an impurity atom In theory, defects generated by too high doping concentration can form trapping centers of electrons or holes In the crystal, which easily causes the increase of scattering degree of carriers In the crystal when moving In an electric field, thereby deteriorating performance. Therefore, In order to obtain CZT and CdTe crystals for detectors with good resistivity and carrier transport performance, the doping mode of the doping element In needs to be controlled, the doping efficiency of In is improved, and the concentration of defects such as Cd vacancy and the like In the crystals is reduced under the condition of low In doping concentration.
In order to achieve the purpose, the technical solution provided by the invention is as follows:
a doping method for optimizing vacancy defects in a compound semiconductor crystal is characterized by comprising the following steps:
1) preparing a Te and In uniform combination raw material according with a metering ratio according to the ratio of Te to In the grown In-doped CZT crystal or In-doped CdTe crystal;
2) weighing Cd, Zn and the Te and In uniform combination raw material obtained In the step 1) according to the stoichiometric ratio of the In-doped CZT crystal or the In-doped CdTe crystal to prepare a CZT polycrystal material or a CdTe polycrystal material;
3) filling the CZT polycrystal material or CdTe polycrystal material obtained in the step 2) into a growth container, sealing, and placing the growth container into crystal growth equipment for growth to obtain CZT crystals or CdTe crystals.
Further, the specific steps (step of preparing Te and In uniform combination raw materials according with the stoichiometric ratio) In the step 1) are as follows:
1.1) weighing proper amount of Te raw material and In raw material according to the determined Te and In proportion (different proportions according to requirements) In the grown In-doped CZT crystal or In-doped CdTe crystal and the space size of a material mixing container In ten-thousand to hundred-grade clean room environment, filling the materials into the material mixing container, uniformly mixing, and sealing the material mixing container;
1.2) placing the material mixing container sealed In the step 1.1) In a high-temperature furnace, raising the temperature to uniformly heat the material mixing container to 20-50 ℃ above the melting point of Te, namely, within the range of 472-502 ℃, so that In and Te are mixed and combined uniformly In a liquid state; wherein, the melt fluidity is not good at the lower overheating temperature, which is not beneficial to the uniform mixing, while the overheating temperature is too high, which leads to higher vapor pressure and raw material-crucible reaction, therefore, the melting point of Te is selected to be 20-50 ℃ above;
1.3) after the uniform combination, closing the high-temperature furnace, cooling to room temperature, and crushing the material mixing container In a clean room to obtain the uniform combination raw material of Te and In.
Further, In the step 1.1), the material mixing container adopts a quartz crucible, Te raw material and In raw material are filled In the position 4-10cm away from the sealing opening of the quartz crucible, so that the raw material is prevented from being ablated during sealing, and the quartz crucible is sealed by oxyhydrogen flame.
Further, in the step 1.2), the high-temperature furnace is a multi-temperature-zone swinging furnace, the material mixing container is uniformly heated by adjusting the temperature of each part of the multi-temperature zone, and a furnace body of the high-temperature furnace can swing within +/-30-60 degrees to fully convect the melt, so that the uniform mixing of the high-temperature furnace and the melt is facilitated;
the material mixing container slowly swings for 12-24h at the speed of 1-2r/min In the high-temperature furnace body, and the melt swings for a long time to ensure that Te and In are fully and uniformly mixed.
Further, the step 2) is specifically as follows:
2.1) weighing uniformly combined raw materials of Cd, Zn, Te and In according to the stoichiometric proportion of the grown In-doped CdTe crystal or In-doped CZT crystal In a ten-thousand to one-hundred grade clean room environment, putting the uniformly combined raw materials into a material mixing container, uniformly mixing, and sealing the material mixing container;
2.2) placing the sealed material mixing container in a high-temperature swing furnace, slowly heating (the heating rate is 10-50 ℃/min) to the melting point of CdTe or CZT, preserving heat for 24-48h to ensure full melting, and then swinging the material mixing container at the speed of 0.5-2r/min for 12-24h in the heat preservation state to ensure full and uniform mixing; the slow heating mode can ensure the slow combination reaction of Te and Zn and Cd, and the excessive reaction temperature and rate can cause a great deal of heat release of the combination reaction, which can cause the crushing of a material mixing container.
2.3) closing the high-temperature swinging furnace, cooling to room temperature, crushing the material mixing container, and taking out the CZT polycrystal material or the CdTe polycrystal material.
Further, in the step 2.1), the size of each raw material is controlled to be 0.1-2cm 3 Within the range, the small-sized charged raw material size can stabilize the reaction rate of the melted raw materials and ensure more sufficient mixing; the material mixing container adopts a quartz crucible.
Further, in the step 3), the crystal growth equipment is Bridgman crystal growth equipment.
In addition, the invention also provides a CZT crystal or CdTe crystal, which is characterized in that: the preparation method is adopted.
A CdTe or CZT wafer for radiation detection, characterized by: the raw material is CZT crystal or CdTe crystal prepared by the method.
A preparation method of CdTe wafer or CZT wafer for radiation detection is characterized in that: cutting, grinding and polishing the CZT crystal or CdTe crystal prepared by the method, and selecting a proper area for sampling to prepare the CZT crystal or CdTe crystal.
The invention has the advantages that:
on the basis of the existing charging and crystal growth method, the invention abandons the method of directly adding the doping element In into the raw materials of Cd, Zn, Te and the like or CdTe, CZT polycrystal materials, but the In and Te elements with the calculated doping proportion are reacted and combined at high temperature In advance, then the materials are charged according to the proportion of each element In the crystal, and are uniformly mixed at high temperature to obtain CZT or CdTe polycrystal materials, and finally CZT and CdTe monocrystal crystals are prepared by adopting crystal growth equipment. In generally occupies a Cd position In CdTe and CZT crystals, the doping element In can occupy the Cd position In advance by the uniform combination and mixing of the doping element In and the main component Te In advance, so that the excessive formation of the compound defect of In and Cd In the doping process can be avoided as much as possible, the compensation efficiency and compensation effect of In on the Cd vacancy are improved, the doping efficiency of In is improved, the key performances of the crystal such as resistivity, carrier concentration, mobility, service life and the like and the radiation detection performance are improved, and the photoelectric performance of the CZT and CdTe crystals is optimized; in addition, the doping amount of the In element is generally extremely trace (between about 100ppb and 100 ppm), a large amount of uniform combination raw materials of In and Te are prefabricated In advance, the workload is not increased In the production process, the lower limit of In weighing can be improved, the weighing precision is effectively improved, the error is reduced, and the requirements of equipment such as a balance and the like and the operation precision are reduced.
Drawings
FIG. 1 is a spectrum of energy of example 1-1: ( 241 Am) with an energy resolution of 5.81% (@59.5 keV).
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
the research team of the application analyzes the actual effect of the conventional In doping method In the existing CdTe and CZT crystals, and finds that the optimal In doping effect cannot be obtained by directly mixing In raw materials such as Cd, Zn and Te or adding In into CdTe and CZT polycrystalline materials, the In element can show strong self-compensation behavior for the existing defects In the chemical combination process of the crystals to form an In related defect complex, so that the In doping efficiency is greatly reduced, and a large amount of defects such as Cd vacancy and the like still exist In the crystals.
Aiming at the problem, the invention provides the method for mixing the doping element In and the main element Te uniformly In advance In a high-temperature melt state, and the advanced combination of the In and the Te can lead the In to occupy the Cd position In advance, thereby avoiding the formation of the compound defect of the In and the Cd In the doping process as much as possible, improving the compensation effect of the In on the Cd position, improving the doping efficiency of the In and improving the performances of CdTe and CZT crystals.
The method comprises the following specific steps:
step 1: according to the proportion of Te and In the grown In-doped CZT and CdTe crystals, preparing a Te and In uniform combination raw material which meets the metering ratio;
wherein the step of preparing Te and In mixed raw materials (homogeneous combination) which accord with the metering ratio is as follows:
step 1.1: weighing appropriate amount of Te and In raw materials according to the determined Te and In proportion In the grown crystal and the space size of a material mixing container In a ten-thousand to one-hundred grade clean room environment, filling the raw materials into the material mixing container, uniformly mixing, and sealing the material mixing container; the material mixing container is preferably a quartz crucible, and the sealed quartz crucible is generally fused by oxyhydrogen flame;
step 1.2: and (3) placing the sealed material mixing container In a high-temperature furnace, preferably a multi-temperature zone swinging furnace, raising the temperature to uniformly heat the temperature of the container to be 20-50 ℃ above the melting point of Te, namely within the range of 472-.
Step 2: weighing Cd, Zn, Te and In uniformly combined raw materials according to the stoichiometric ratio of the In-doped CZT crystal or the In-doped CdTe crystal to prepare a CZT or CdTe polycrystal material;
the preparation method of the CZT or CdTe polycrystalline material comprises the following steps:
step 2.1: according to the chemical transformation of the grown CdTe or CZT crystal in ten-thousand to hundred-hundred grade clean room environmentWeighing Cd, Zn, Te and In uniformly combined raw materials according to a stoichiometric proportion, putting the raw materials into a material mixing container, uniformly mixing, and sealing the material mixing container; preferably, the size of each raw material is controlled to be 0.1-2cm 3 Within the range, so that the reaction rate of the melted raw materials is stable, and more sufficient mixing is ensured;
step 2.2: slowly heating the raw materials in a high-temperature swing furnace to the melting point of CdTe or CdTe polycrystalline material, preserving heat for 24 hours, slowly swinging the material mixing container for 12-24 hours at the speed of 0.5-2r/min in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container, and taking out the CZT polycrystalline material or CdTe polycrystalline material.
And step 3: filling the CZT polycrystal material or the CdTe polycrystal material into a growth container, sealing, and placing the growth container in a crystal growth device for growth to obtain CdTe crystals or CZT crystals;
of course, after obtaining the above raw materials, the raw materials are further applied to radiation detection equipment, for example, the taken crystal needs to be cut, ground and polished to prepare a CdTe wafer or a CZT wafer for radiation detection.
The following detailed description of embodiments of the invention is intended to be illustrative, and not to be construed as limiting the invention.
Comparative example 1:
step 1: weighing Cd, Zn, Te and In raw materials according to the stoichiometric ratio of In-doped CZT to prepare a CZT polycrystal material;
the method for preparing the CZT polycrystal material comprises the following steps:
step 1.1: in a hundred-grade clean room environment, weighing Cd, Zn, Te and In raw materials according to the stoichiometric proportion of the grown CZT crystal, putting the raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 1.2: slowly heating the raw material in a high-temperature swing furnace to the melting point of CZT, preserving heat for 24 hours, slowly swinging the material mixing container at the speed of 1r/min for 24 hours in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container, and taking out the CZT polycrystal material.
Step 2: the polycrystalline material is filled into a quartz crucible for growth and sealed, the crucible is placed in an ACRT Bridgman method crystal growth device for growth to obtain CZT crystals, the crystals are taken out for cutting, grinding and polishing, and two CZT wafers are prepared by sampling in the head and middle regions of the crystals as comparative examples 1-1 and comparative examples 1-2.
And testing a thermally stimulated current spectrum (TSC) of the comparative example 1-1, wherein the TSC is one of analysis means aiming at the characterization of the deep level defects of the high-resistance sample at present, the TSC spectrum can be subjected to spectrum decomposition by using a simultaneous multi-peak method (SIMPA) technology to obtain the level and the concentration of each type of defect in the crystal, and the TSC spectrum decomposition data of the comparative example 1-1 is shown in Table 1.
Comparative examples 1-1 and 1-2 were tested for resistivity, electron mobility lifetime, and energy resolution ((R)) 241 Am @59.5keV) as shown in table 2.
Example 1:
step 1: preparing a Te and In uniform combination raw material which accords with the metering ratio according to the ratio of Te to In the grown In-doped CZT crystal;
the preparation method of the Te and In uniform combination raw material according with the metering ratio comprises the following steps:
step 1.1: weighing Te and In raw materials In a hundred-grade clean room environment, putting the Te and In raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 1.2: and (3) placing the sealed crucible In a multi-temperature-zone swinging furnace, raising the temperature to uniformly heat the temperature of the container to 487 ℃, swinging the crucible at a high temperature, introducing forced convection to uniformly mix the raw materials In a molten state, cooling the high-temperature furnace to room temperature, and crushing a growth container In a clean room to obtain the Te and In uniformly-combined raw materials.
Step 2: weighing Cd, Zn and uniformly combined Te and In raw materials according to the stoichiometric ratio of the In-doped CZT crystal to prepare a CZT polycrystal material;
the preparation method of the CZT polycrystal material comprises the following steps:
step 2.1: weighing Cd, Zn, Te and In uniformly combined raw materials according to the stoichiometric proportion of the grown CZT crystal In a hundred-grade clean room environment, putting the raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 2.2: slowly heating the raw material in a high-temperature swing furnace to the melting point of CZT, preserving heat for 24 hours, slowly swinging a material mixing container at the speed of 1r/min for 24 hours in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container, and taking out CZT polycrystal material;
and step 3: the CZT polycrystal material was charged into a quartz crucible for growth and sealed, and the crucible was placed in an ACRT Bridgman method crystal growth apparatus to grow CZT crystals, the CZT crystals were taken out to cut, grind and polish, and two CZT wafers were prepared by sampling the head and middle regions of the crystals as examples 1-1 and 1-2 (the sampling positions were the same as in comparative example 1).
The TSC spectra of example 1-1 were tested and the data of the solutions are shown In Table 1, and it was found that, as compared with comparative example 1-1, the composite defects A-center.1 and A-center.2 and Cd vacancy defect V of CZT crystal grown by mixing In and Te In combination and uniformly In advance and charging them were compared with the case where In was directly doped into the raw material Cd - Are all greatly reduced, wherein V Cd - The concentration is reduced by five times, which shows that the In doping efficiency can be obviously improved by the In and Te advanced doping, the composite defects of In and Cd formed In the doping process are reduced, and the compensation effect of the In on Cd vacancy is improved.
Examples 1-1 and 1-2 were tested for resistivity, electron mobility lifetime, and energy resolution: ( 241 Am @59.5keV) as shown in table 2. As can be seen by comparing with comparative examples 1-1 and 1-2, the resistivity, the electron mobility life span and the energy resolution of the CZT crystal grown by mixing In and Te uniformly In advance and then charging are greatly improved, wherein the energy resolution is up to 5.81%, as shown In figure 1.
Example 2:
step 1: preparing a Te and In uniform combination raw material which accords with the metering ratio according to the ratio of Te to In the grown In-doped CZT;
the preparation method of the Te and In uniform combination raw material according with the metering ratio comprises the following steps:
step 1.1: weighing Te and In raw materials In a hundred-grade clean room environment, putting the Te and In raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 1.2: and (3) placing the sealed crucible In a multi-temperature-zone swinging furnace, raising the temperature to uniformly heat the temperature of the container to 472 ℃, swinging the crucible at a high temperature, introducing forced convection to uniformly mix the raw materials In a molten state, cooling the high-temperature furnace to room temperature, and crushing the growth container In a clean room to obtain the Te and In uniformly combined raw materials.
Step 2: weighing Cd, Zn and uniformly combined Te and In raw materials according to the stoichiometric ratio of In-doped CZT to prepare a CZT polycrystal material;
the method for preparing the CZT polycrystal material comprises the following steps:
step 2.1: weighing Cd, Zn, Te and In uniformly combined raw materials according to the stoichiometric proportion of the grown CZT crystal In a hundred-grade clean room environment, putting the raw materials into a quartz crucible, uniformly mixing the raw materials, and sealing the quartz crucible by oxyhydrogen flame;
step 2.2: slowly heating the raw material in a high-temperature swing furnace to the melting point of CZT, preserving heat for 24h, slowly swinging the material mixing container at the speed of 1r/min for 24h in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container, and taking out CZT polycrystal material.
And step 3: polycrystalline material is filled into a quartz crucible for growth and sealed, CZT crystal is grown in a Bridgman crystal growth device in which the crucible is placed, the crystal is taken out to be cut, ground and polished, and two pieces of CZT wafer are prepared by sampling in the head and middle regions of the crystal as example 2-1 and example 2-2 (the sampling positions are the same as in comparative example 1 and example 1).
Examples 2-1 and 2-2 were tested for resistivity, electron mobility and energy resolution ((C)) 241 Am @59.5keV) as shown in table 2. As can be seen by comparing with comparative examples 1-1 and 1-2, the resistivity, the electron mobility lifetime and the energy resolution of the CZT crystal grown by mixing In and Te uniformly and charging are all improved greatly.
Example 3:
step 1: preparing a Te and In uniform combination raw material which accords with the metering ratio according to the ratio of Te to In the grown In-doped CZT;
the preparation method of the Te and In uniform combination raw material according with the metering ratio comprises the following steps:
step 1.1: weighing Te and In raw materials In a hundred-grade clean room environment, putting the Te and In raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 1.2: and (3) placing the sealed crucible In a multi-temperature-zone swinging furnace, raising the temperature to uniformly heat the temperature of the container to 502 ℃, swinging the crucible at high temperature, introducing forced convection to uniformly mix the raw materials In a molten state, cooling the high-temperature furnace to room temperature, and crushing the growth container In a clean room to obtain the Te and In uniformly combined raw materials.
Step 2: weighing Cd, Zn and uniformly combined Te and In raw materials according to the stoichiometric ratio of In-doped CZT to prepare a CZT polycrystal material;
the method for preparing the CZT polycrystal material comprises the following steps:
step 2.1: weighing Cd, Zn, Te and In uniformly combined raw materials according to the stoichiometric proportion of the grown CZT crystal In a hundred-grade clean room environment, putting the raw materials into a quartz crucible, uniformly mixing the raw materials, and sealing the quartz crucible by oxyhydrogen flame;
step 2.2: slowly heating the raw material in a high-temperature swing furnace to the melting point of CZT, preserving heat for 24h, slowly swinging the material mixing container at the speed of 1r/min for 24h in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container, and taking out CZT polycrystal material.
And step 3: polycrystalline material is filled into a quartz crucible for growth and sealed, CZT crystal is obtained by placing the crucible in Bridgman crystal growth equipment for growth, the crystal is taken out for cutting, grinding and polishing, and two pieces of CZT wafers of example 3-1 and example 3-2 are prepared by sampling in the head and middle regions of the crystal (the sampling positions are the same as those of comparative example 1 and examples 1 and 2).
Examples 3-1 and 3-2 were tested for resistivity, electron mobility and energy resolution ((C)) 241 Am @59.5keV) as shown in table 2. As can be seen from comparison with comparative examples 1-1 and 1-2, the resistivity and electron mobility of CZT crystal grown by mixing In and Te In combination and charging In advanceThe service life of the electron mobility and the energy resolution are greatly improved.
Table 1: TSC resolution Spectrum data of comparative example 1-1 and example 1-1
Table 2: comparison of the Main Properties of comparative example 1, example 2 and example 3
| Resistivity (omega cm) | Electron mobility (cm) 2 /V/s) | Electron mobility lifetime product (cm) 2 /v) | Energy resolution @59.5keV | |
| Comparative examples 1 to 1 | 1.02*10 10 | 848 | 0.70*10 -3 | 8.5％ |
| Comparative examples 1 to 2 | 0.93*10 10 | 868 | 0.73*10 -3 | 8.2％ |
| Examples 1 to 1 | 1.76*10 10 | 1148 | 1.16*10 -3 | 5.81％ |
| Examples 1 to 2 | 1.58*10 10 | 1090 | 0.96 * 10 -3 | 6.2％ |
| Example 2-1 | 1.61*10 10 | 968 | 0.83*10 -3 | 7.4％ |
| Examples 2 to 2 | 1.72*10 10 | 1035 | 0.92*10 -3 | 7.1％ |
| Example 3-1 | 1.54*10 10 | 955 | 0.81*10 -3 | 7.7％ |
| Examples 3 to 2 | 1.63*10 10 | 1076 | 0.94*10 -3 | 7.0％ |
Comparative example 2:
step 1: weighing Cd, Te and In raw materials according to the stoichiometric ratio of In doped CdTe to prepare a CdTe polycrystal material;
the preparation method of the CdTe polycrystalline material comprises the following steps:
step 1.1: in a hundred-grade clean room environment, weighing Cd, Te and In raw materials according to the stoichiometric proportion of a grown CdTe crystal, putting the raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 1.2: slowly heating the raw materials in a high-temperature swing furnace to the melting point of CdTe, preserving heat for 24 hours, slowly swinging the material mixing container at the speed of 1r/min for 24 hours in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container and taking out the CdTe polycrystal material.
Step 2: filling the polycrystal material into a quartz crucible for growth, sealing, placing the crucible in an ACRT Bridgman method crystal growth device for growth to obtain CdTe crystals, taking out the crystals, cutting, grinding and polishing, and sampling in the head and middle regions of the crystals to obtain two CdTe wafers serving as a comparative example 2-1 and a comparative example 2-2.
Comparative examples 2-1 and 2-2 were tested for resistivity, electron mobility lifetime, and energy resolution ((R)) 241 Am @59.5keV) as shown in table 3.
Example 4:
step 1: preparing a Te and In uniform combination raw material which meets the metering ratio according to the proportion of Te and In the grown In-doped CdTe;
the preparation method of the Te and In mixed raw material according with the metering ratio comprises the following steps:
step 1.1: weighing Te and In raw materials In a hundred-grade clean room environment, putting the Te and In raw materials into a quartz crucible, uniformly mixing, and sealing the quartz crucible by oxyhydrogen flame;
step 1.2: and (3) placing the sealed crucible In a multi-temperature-zone swinging furnace, raising the temperature to uniformly heat the temperature of the container to 487 ℃, swinging the crucible at a high temperature, introducing forced convection to uniformly mix the raw materials In a molten state, cooling the high-temperature furnace to room temperature, and crushing the growth container In a clean room to obtain uniformly combined Te and In raw materials.
Step 2: weighing Cd and uniformly combined Te and In raw materials according to the stoichiometric ratio of In doped CdTe to prepare a CdTe polycrystal material;
the preparation method of the CdTe polycrystalline material comprises the following steps:
step 2.1: in a hundred-grade clean room environment, Cd, Te and In raw materials which are uniformly combined are weighed according to the stoichiometric proportion of a grown CdTe crystal, the raw materials are put into a quartz crucible and are uniformly mixed, and the quartz crucible is sealed by oxyhydrogen flame;
step 2.2: slowly heating the raw materials in a high-temperature swing furnace to the melting point of CdTe, preserving heat for 24 hours, slowly swinging the material mixing container at the speed of 1r/min for 24 hours in the heat preservation state, finally closing the furnace body, cooling to the room temperature, crushing the material mixing container and taking out the CdTe polycrystal material.
And 3, step 3: polycrystalline material is filled into a quartz crucible for growth and sealed, the crucible is placed in an ACRT Bridgman method crystal growth device to grow CdTe crystals, the crystals are taken out to be cut, ground and polished, and two CdTe wafers are prepared by sampling the head and the middle area of the crystals as an example 4-1 and an example 4-2 (the sampling position is the same as the comparative example 2).
Examples 4-1 and 4-2 were tested for resistivity, electron mobility, and energy resolution ((C)) 241 Am @59.5keV) as shown in table 3. Compared with the comparative examples 2-1 and 2-2, the resistivity, the electron mobility life and the energy resolution of the CdTe crystal grown by mixing In and Te evenly In advance and then charging are all greatly improved, wherein the energy resolution is up to 10.8 percent.
Table 3: comparison of the Main Properties of comparative example 2 and example 4
| Resistivity (omega cm) | Electron mobility (cm) 2 /V/s) | Energy resolution @59.5keV | |
| Comparative example 2-1 | 3.7*10 9 | 854 | 15.2％ |
| Comparative examples 2 to 2 | 3.4*10 9 | 678 | 16.6％ |
| Example 4-1 | 4.2*10 9 | 1070 | 11.7％ |
| Example 4 to 2 | 4.5*10 9 | 1340 | 10.8％ |
Therefore, the method provided by the invention can improve the In doping efficiency, improve the key performances of the crystal such as resistivity, carrier concentration, mobility life and the like, and the radiation detection performance, and optimize the photoelectric performance of the CZT and CdTe crystals.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications or substitutions can be easily made by those skilled in the art within the technical scope of the present disclosure.
Claims (10)
1. A doping method for optimizing vacancy defects in a compound semiconductor crystal is characterized by comprising the following steps:
1) preparing a Te and In uniform combination raw material according with a metering ratio according to the ratio of Te to In the grown In-doped CZT crystal or In-doped CdTe crystal;
2) weighing Cd, Zn and the Te and In uniform combination raw material obtained In the step 1) according to the stoichiometric ratio of the In-doped CZT crystal or the In-doped CdTe crystal to prepare a CZT polycrystal material or a CdTe polycrystal material;
3) filling the CZT polycrystal material or CdTe polycrystal material obtained in the step 2) into a growth container, sealing, and placing the growth container into crystal growth equipment for growth to obtain CZT crystals or CdTe crystals.
2. The method for optimizing the doping of vacancy defects in a compound semiconductor crystal according to claim 1, wherein the step 1) comprises the following specific steps:
1.1) weighing Te raw materials and In raw materials according to the given Te and In proportion In grown In-doped CZT crystals or In-doped CdTe crystals and the space size of a material mixing container In a ten-thousand to one-hundred grade clean room environment, filling the materials into the material mixing container, uniformly mixing, and sealing the material mixing container;
1.2) placing the material mixing container sealed In the step 1.1) In a high-temperature furnace, heating to ensure that the temperature of the material mixing container is uniformly heated to be 20-50 ℃ above the melting point of Te, and mixing and uniformly combining In and Te In a liquid state;
1.3) after the uniform combination, closing the high-temperature furnace, cooling to room temperature, and crushing the material mixing container In a clean room to obtain the uniform combination raw material of Te and In.
3. The method of optimizing the doping of vacancy defects in a compound semiconductor crystal according to claim 2, characterized in that:
in the step 1.1), the material mixing container adopts a quartz crucible, Te raw materials and In raw materials are filled In a position 4-10cm away from a sealing opening of the quartz crucible, and oxyhydrogen flame is used for sealing the quartz crucible.
4. The method of optimizing the doping of vacancy defects in a compound semiconductor crystal according to claim 3, characterized in that:
in the step 1.2), the high-temperature furnace is a multi-temperature-zone swinging furnace, the material mixing container is uniformly heated by adjusting the temperature of each part of the multi-temperature zone, and the furnace body of the high-temperature furnace can swing within +/-30-60 degrees;
the material mixing container swings for 12-24h in the high-temperature furnace body at the speed of 1-2 r/min.
5. The method for optimizing the doping of a vacancy defect in a compound semiconductor crystal according to any one of claims 1 to 4, wherein the step 2) is specifically:
2.1) weighing uniformly combined raw materials of Cd, Zn, Te and In according to the stoichiometric proportion of the grown In-doped CdTe crystal or In-doped CZT crystal In a ten-thousand to one-hundred grade clean room environment, putting the uniformly combined raw materials into a material mixing container, uniformly mixing, and sealing the material mixing container;
2.2) placing the sealed material mixing container in a high-temperature swing furnace, heating to the melting point of CdTe or CZT, preserving heat for 24-48h, and then swinging the material mixing container at the speed of 0.5-2r/min for 12-24h in the heat preservation state;
2.3) closing the high-temperature swinging furnace, cooling to room temperature, crushing the material mixing container, and taking out the CZT polycrystal material or the CdTe polycrystal material.
6. The method of optimizing the doping of vacancy defects in a compound semiconductor crystal according to claim 5, wherein:
in the step 2.1), the size of each raw material is controlled to be 0.1-2cm 3 Within the range; the material mixing container adopts a quartz crucible.
7. The method of optimizing the doping of vacancy defects in a compound semiconductor crystal according to claim 6, characterized in that:
in the step 3), the crystal growth equipment is Bridgman crystal growth equipment.
8. A CZT crystal or CdTe crystal characterized by: prepared by the process of any one of claims 1 to 7.
9. A CdTe or CZT wafer for radiation detection, characterized by: the raw material is CZT crystal or CdTe crystal prepared by the method of any one of claims 1-7.
10. A method for preparing a CdTe wafer or CZT wafer for radiation detection, characterized in that: cutting, grinding and polishing the CZT or CdTe crystal obtained by the method of any one of claims 1-7, and sampling the appropriate area.
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