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CN116334759A - Seed crystal dissolving method and device for growing tellurium-zinc-cadmium crystals based on THM - Google Patents

Seed crystal dissolving method and device for growing tellurium-zinc-cadmium crystals based on THM Download PDF

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Publication number
CN116334759A
CN116334759A CN202310259350.9A CN202310259350A CN116334759A CN 116334759 A CN116334759 A CN 116334759A CN 202310259350 A CN202310259350 A CN 202310259350A CN 116334759 A CN116334759 A CN 116334759A
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tellurium
zinc
cadmium
seed crystal
growing
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张继军
卢伟
徐哲人
曹祥智
刘昊
祁永武
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/46Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003Heating or cooling of the melt or the crystallised material
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006Controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/14Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention relates to a seed crystal dissolving method and a device for growing tellurium-zinc-cadmium crystals based on THM, wherein the device comprises a growth crucible, an adiabatic bracket for placing the growth crucible, a SiC heat conduction rod arranged at the bottom of the growth crucible and a thermocouple for monitoring the temperature of the tellurium-zinc-cadmium single crystal seed crystal, and the seed crystal dissolving method comprises the following steps: s1, preprocessing tellurium-zinc-cadmium single crystal seed crystal and first tellurium-zinc-cadmium polycrystal ('false seed crystal'), sequentially placing the first tellurium-zinc-cadmium polycrystal, the tellurium-zinc-cadmium single crystal seed crystal, the tellurium-rich solvent zone material and the third tellurium-zinc-cadmium polycrystal from bottom to top, vacuumizing, heating, and preserving heat; s2, downwards moving a heater to heat and dissolve part of components of the tellurium-zinc-cadmium monocrystal seed crystal; s3, moving the heater upwards to enable tellurium-zinc-cadmium crystals to start to continuously grow. Compared with the prior art, the invention reduces the size requirement on tellurium-zinc-cadmium single crystal seed crystal, enhances the release of crystallization latent heat during the fusion growth, and improves the quality of tellurium-zinc-cadmium crystal.

Description

Seed crystal dissolving method and device for growing tellurium-zinc-cadmium crystals based on THM
Technical Field
The invention relates to the technical field of photoelectric material preparation, in particular to a seed crystal dissolving method and device for growing tellurium-zinc-cadmium crystals based on THM.
Background
Cadmium zinc telluride (CdZnTe) is a II-VI compound semiconductor, and has the advantages that: the high-energy particle beam has higher average atomic number and can be used for detecting high-energy particle beams such as gamma rays, X rays and the like; and cadmium zinc telluride has higher intrinsic resistivity and larger forbidden bandwidth than common semiconductor materials such as silicon (Si), germanium (Ge) and the like, and is more suitable for manufacturing room-temperature ray and ray detectors and infrared film epitaxial substrates. Cadmium zinc telluride is becoming an ideal material for manufacturing novel detectors in the fields of astrophysics, safety inspection, ecological environmental protection, nuclear medicine, clinical medicine and the like. The current mainstream methods for growing tellurium-zinc-cadmium crystals comprise a vertical Bridgman method, a vertical gradient condensation method, a moving heater method and the like.
When tellurium-zinc-cadmium crystals are used as substrate materials, the crystal orientation is very critical. The directional seeding growth technology of tellurium-zinc-cadmium crystal seed crystals can effectively improve the utilization rate of the crystals. However, the conventional vertical Bridgman method (VB) has the defects that the seed crystal is extremely easy to be completely melted due to high growth temperature, and the seeding success rate of the tellurium-zinc-cadmium seed crystal is not high.
The mobile heater method (Traveling Heater Method) is hereinafter abbreviated as THM and has the advantages of low growth temperature, uniform components, high crystal purity and the like. The main stream of THM at present generally adopts equal diameter seed crystal for growing tellurium-zinc-cadmium. The isodiametric seed crystal is one with single crystal orientation, and has the advantages of easy availability, simple growth device and the like. But the growth result shows that the crystal orientation of the subsequent growth is uncontrollable and the single crystal rate is low. Is unfavorable for improving the quality of tellurium-zinc-cadmium crystals.
In order to improve the crystal quality, single crystal fine seed crystals can be adopted for seeding growth. However, the use of single crystal fine seeds has several disadvantages: 1. the large-size single crystal fine seed crystal is difficult to obtain, the obtained seed crystal is short in length and difficult to inoculate. 2. Because THM is a solvent method, the tellurium-zinc-cadmium solution has high solubility, and is extremely easy to be completely dissolved at a certain temperature. 3. The crystal seed crystal is small in size in the middle and later growth stages, so that the crystallization latent heat in the growth process is difficult to release, and the crystal quality in the growth stage is drastically reduced. Therefore, for the THM growth process, the control of the dissolution of the single crystal seed is extremely important.
Disclosure of Invention
The invention aims to overcome the defects of the THM growth process in the process of single crystal seed crystal grafting control, and provides a seed crystal grafting method and device based on THM growth tellurium-zinc-cadmium crystal.
The aim of the invention can be achieved by the following technical scheme:
one of the technical schemes of the invention is to provide a seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on THM, which comprises the following steps:
s1, preprocessing tellurium-zinc-cadmium single crystal seed crystal and first tellurium-zinc-cadmium polycrystal ('false seed crystal', namely a small-sized mechanically polished and corroded polycrystal (cut from a grown tellurium-zinc-cadmium ingot)), sequentially placing the first tellurium-zinc-cadmium polycrystal, the tellurium-zinc-cadmium single crystal seed crystal, a tellurium-zinc-rich solvent zone material and the third tellurium-zinc-cadmium polycrystal from bottom to top, vacuumizing, heating and preserving heat;
s2, downwards moving a heater to heat and dissolve part of components of the tellurium-zinc-cadmium monocrystal seed crystal;
s3, moving the heater upwards to enable tellurium-zinc-cadmium crystals to start to continuously grow.
In the step S1, the seed crystal of the tellurium-zinc-cadmium single crystal and the first tellurium-zinc-cadmium polycrystal are pretreated by cutting and soaking the seed crystal of the tellurium-zinc-cadmium single crystal and the first tellurium-zinc-cadmium polycrystal respectively in HNO 3 Adding the mixture into an etching solution prepared by the volume ratio of the mixture to HF of 2:1, taking out, grinding and polishing, etching for 4min by using 2% bromomethanol by mass fraction, ultrasonically cleaning for 5min by using absolute ethyl alcohol, and finally using N 2 And (5) drying by air.
Further, in the step S1, the tellurium-rich solvent zone material comprises pure tellurium and a second tellurium-zinc-cadmium polycrystal, the quality of the pure tellurium and the second tellurium-zinc-cadmium polycrystal being determined in terms of mole percent with respect to Te-Cd on the CdTe T-X phase diagram.
Further, in the step S1, the temperature is kept when the temperature is raised and heating is continued to the melting point of the tellurium-rich solvent zone material, and at the moment, the tellurium-rich solvent zone material starts to melt.
Further, in the step S1, the heat preservation is continued until the tellurium-rich solvent zone material is completely melted and the third tellurium-zinc-cadmium polycrystal above the tellurium-rich solvent zone material is dissolved so as to saturate tellurium, and the heat preservation is ended.
Further, in the step S2, the speed of moving the heater downwards is 0.1mm/h, and the time of moving the heater downwards is enough to heat and dissolve about 50% of tellurium-zinc-cadmium single crystal seed crystals.
Further, in the step S3, the speed of upward moving the heater is 0.12mm/h in the seed crystal seeding stage and the shoulder growing stage of the tellurium-zinc-cadmium crystal; and in the equal diameter growth stage of the tellurium-zinc-cadmium crystal, the upward moving speed of the heater is 0.2mm/h, and the growth gradient is 20 ℃/cm.
The second technical scheme of the invention is to provide a device for implementing the seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on THM according to the first technical scheme, which comprises a growth crucible for reaction, an adiabatic bracket for placing the growth crucible, a SiC heat conduction rod arranged at the bottom of the growth crucible and used for releasing the bottom temperature of the growth crucible, and a thermocouple arranged on the growth crucible and used for monitoring the seed crystal temperature of the tellurium-zinc-cadmium single crystals.
Further, the two thermocouples are respectively arranged at the upper end and the lower end of the growth crucible for placing tellurium-zinc-cadmium monocrystal seed crystals.
Further, a supporting rod is arranged outside the SiC heat conduction rod.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts tellurium-zinc-cadmium monocrystal seed crystal to grow tellurium-zinc-cadmium crystals, the subsequent tellurium-zinc-cadmium crystals can show good crystal orientation inheritance, and the monocrystal yield and quality of the crystals can be improved.
(2) The growth crucible is provided with a slender seed crystal bag, the longer the seed crystal part is, the more favorable the control of partial seed crystal dissolution is, and the invention introduces a first tellurium-zinc-cadmium polycrystal with the same diameter as that of the tellurium-zinc-cadmium single crystal seed crystal as a false seed crystal, and is arranged below the tellurium-zinc-cadmium single crystal seed crystal to jointly form a seed crystal system, thereby shortening the length requirement on the tellurium-zinc-cadmium single crystal seed crystal, improving the height of the tellurium-zinc-cadmium single crystal seed crystal, being favorable for the temperature monitoring of the tellurium-zinc-cadmium single crystal seed crystal and also being favorable for controlling the partial dissolution of the tellurium-zinc-cadmium single crystal seed crystal.
(3) According to the invention, through the heat dissipation design (namely the heat insulation bracket and the SiC heat conduction rod) of the device, the heat insulation bracket has the function of keeping the transverse temperature gradient stable, inhibiting transverse convection and facilitating crystal growth. The SiC heat conducting rod has the functions of increasing radial thermal gradient, being beneficial to release of latent heat of crystallization, improving a growth interface when the tellurium-zinc-cadmium single crystal seed crystal is connected in a dissolved mode, enabling a solid-liquid interface of tellurium-zinc-cadmium crystal growth to be changed into a flatter interface or even a convex interface, and being beneficial to improving the quality of tellurium-zinc-cadmium crystal.
(4) According to the invention, the thermocouples are respectively arranged at the upper end and the lower end of the tellurium-zinc-cadmium single crystal seed crystal and are used for monitoring the temperature between the tellurium-zinc-cadmium single crystal seed crystal and the first tellurium-zinc-cadmium polycrystal in real time, and the ratio of the dissolution quantity and the solubility of the tellurium-zinc-cadmium single crystal seed crystal at the temperature within the temperature range is strictly controlled to be less than 1 according to the CdTe T-X phase diagram, namely, the dissolution of only about 50% of the tellurium-zinc-cadmium single crystal seed crystal is controlled, so that the seeding growth effect is achieved.
Drawings
FIG. 1 is a schematic diagram of the structure of the device for growing tellurium-zinc-cadmium crystals based on THM.
FIG. 2 is a schematic charge diagram of a seed grafting method of growing cadmium zinc telluride crystals based on THM in accordance with the present invention.
FIG. 3 is a pictorial representation of a single crystal seed of tellurium-zinc-cadmium and a pseudo seed employed in the present invention.
FIG. 4 is a cross section of a cadmium zinc telluride single crystal ingot prepared according to the present invention.
The figures are identified as follows:
1, growing a crucible; 2 is a heat insulation bracket; 3 is a supporting rod; 4 is a thermocouple; 1a is a third tellurium-zinc-cadmium polycrystalline region; 1b is a tellurium-rich solvent zone; 1c is a tellurium-zinc-cadmium monocrystal seed crystal region; 1d is a first tellurium-zinc-cadmium polycrystalline region, and 5a is the upper end of a tellurium-zinc-cadmium single crystal seed crystal; and 5b is the lower end of the tellurium-zinc-cadmium single crystal seed crystal.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
In the following examples, unless otherwise specified, functional elements or structures are indicated as conventional elements or conventional structures employed in the art to accomplish the corresponding functions, and unless otherwise specified, raw materials or processing techniques are indicated as conventional commercially available raw material products or conventional processing techniques in the art.
Example 1:
as shown in fig. 1, the device for growing tellurium-zinc-cadmium crystals based on THM comprises a quartz growth crucible 1, a quartz heat insulation bracket 2, a SiC heat conduction rod 4, a support rod 3 and a thermocouple 5. The growth crucible 1 is in a cone structure with wide upper part and narrow lower part, and sequentially comprises a seed crystal seeding part, a growth shouldering part and an equal-diameter growth part from bottom to top, wherein the thickness of each part of the growth crucible 1 is consistent and equal-diameter. The heat insulation bracket 2 is a high-purity mullite cylindrical block, and is provided with a matched drilling design according to the bottom of the growth crucible 1 and the supporting rod 3. The support rod 3 is a SiC rod 4 with corundum on the outside and high thermal conductivity in the center. The growth crucible 1 is directly placed on the heat-insulating bracket 2 after vacuum tube sealing, and the growth crucible 1 and the heat-insulating bracket 2 are combined and placed on the support rod 3. The thermocouple 5 passes through the heat insulation bracket 2 through the reserved small holes, and monitors the upper end 5a (the junction of the tellurium-zinc-cadmium single crystal seed crystal and the taper angle of the growth crucible) and the lower end 5b (the junction of the tellurium-zinc-cadmium single crystal seed crystal and the first tellurium-zinc-cadmium polycrystalline false seed crystal) of the tellurium-zinc-cadmium single crystal seed crystal placed in the growth crucible 1. The growth crucible 1 is also subjected to carbon plating treatment to prevent side nucleation during the growth of tellurium-zinc-cadmium crystals.
Based on the device, the seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on the mobile heating method comprises the following steps:
(1) Selecting a piece of tellurium-zinc-cadmium crystal grown based on vertical Bridgman method for directional cutting
Figure BDA0004130655660000041
(±5)mm single crystal seed is used as tellurium zinc cadmium single crystal seed and soaked in HNO 3 Determining that tellurium zinc cadmium single crystal seed crystal has polar growth surface in etching solution prepared by the volume ratio of HF to HF of 2:1, grinding and polishing, etching with 2% bromomethanol (Br-MeOH) for 4min to remove mechanical damage and dirt on the surface, ultrasonic cleaning with absolute ethyl alcohol for 5min, ultrasonic cleaning with N 2 And (5) drying by air.
(2) Selecting any piece of tellurium-zinc-cadmium crystal grown by vertical Bridgman method to cut
Figure BDA0004130655660000051
Figure BDA0004130655660000052
As a first tellurium-zinc-cadmium polycrystal 'false seed crystal', is soaked in HNO 3 In an etching solution prepared by the volume ratio of HF to HF of 2:1, grinding and polishing, etching with 2% bromomethanol (Br-MeOH) for 4min to remove mechanical damage and dirt on the surface, ultrasonically cleaning with absolute ethanol for 5min, and ultrasonically cleaning with N 2 And (5) drying by air.
(3) Synthesizing pure tellurium and second tellurium-zinc-cadmium polycrystal into tellurium-rich solvent area material in a swing furnace according to the required solvent area proportion, wherein the material mixing temperature is 1000-1200 ℃, the material mixing temperature is 800 ℃, and the molar ratio of Te to Cd is 0.8:0.2 according to a CdTe T-X phase diagram.
(4) Sequentially loading the prepared first tellurium-zinc-cadmium polycrystal, tellurium-zinc-cadmium single crystal seed crystal, tellurium-rich solvent zone material and third tellurium-zinc-cadmium polycrystal into a growth crucible 1 with an elongated seed crystal bag according to a loading schematic diagram shown in figure 2, namely a first tellurium-zinc-cadmium polycrystal zone 1d (4.5 cm high), a tellurium-zinc-cadmium single crystal seed crystal zone 1c (3 cm high), a tellurium-zinc-rich solvent zone 1b (9 cm high) and a third tellurium-zinc-cadmium polycrystal zone 1a (6 cm high), and vacuumizing to ensure that the vacuum degree is superior to 10 -4 Pa。
(5) The growth crucible 1 was placed in a growth furnace, and the temperature was started to rise.
(6) Thermocouples 5 located at the upper end 5a and the lower end 5b of the tellurium-zinc-cadmium single crystal seed crystal monitor temperature in real time.
(7) Heating to the melting point (about 800 ℃) of the tellurium-rich solvent zone 1b, and preserving the heat until the material in the tellurium-rich solvent zone is melted and a small amount of third tellurium zinc cadmium polycrystal is dissolved, so that tellurium is saturated.
(8) The heater is lowered at the rate of 0.1mm/h, the temperature of the upper end 5a and the lower end 5b of the tellurium-zinc-cadmium single crystal seed crystal at the moment is monitored in real time through the thermocouple 5, the ratio of the dissolution amount to the solubility of the tellurium-zinc-cadmium single crystal seed crystal in the temperature range is strictly controlled to be less than 1, and the dissolution of the tellurium-zinc-cadmium single crystal seed crystal is not more than 50%.
(9) The heater is moved upward at the desired growth rate to initiate crystal growth. The growth speed is 0.1mm/h-0.2mm/h, and the growth gradient is 20 ℃/cm. The method comprises the following steps: the upward moving speed of the heater is 0.12mm/h in the seed crystal seeding stage and the growing shouldering stage; the upward moving speed of the heater is 0.2mm/h in the equal diameter growth stage of the tellurium-zinc-cadmium crystal.
(10) And slowly cooling after the growth is finished, and taking out the tellurium-zinc-cadmium single crystal ingot, wherein the single crystal ingot is shown in a cross section circling shown in fig. 4, and the single crystal rate is more than 60%.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.

Claims (10)

1. The seed crystal dissolving method for growing tellurium-zinc-cadmium crystals based on THM is characterized by comprising the following steps:
s1, preprocessing tellurium-zinc-cadmium single crystal seed crystal and first tellurium-zinc-cadmium polycrystal, sequentially placing the first tellurium-zinc-cadmium polycrystal, the tellurium-zinc-cadmium single crystal seed crystal, the tellurium-rich solvent zone material and the third tellurium-zinc-cadmium polycrystal from bottom to top, vacuumizing, heating, and preserving heat;
s2, downwards moving a heater to heat and dissolve part of components of the tellurium-zinc-cadmium monocrystal seed crystal;
s3, moving the heater upwards to enable tellurium-zinc-cadmium crystals to start to continuously grow.
2. The method for seed crystal grafting for growing tellurium-zinc-cadmium crystals based on THM as set forth in claim 1, wherein in step S1, the pretreatment of the tellurium-zinc-cadmium single crystal seed crystal and the first tellurium-zinc-cadmium polycrystal is to cut and soak the tellurium-zinc-cadmium single crystal seed crystal and the first tellurium-zinc-cadmium polycrystal, respectively, at first, in the HNO process 3 Adding the mixture into an etching solution prepared by the volume ratio of the mixture to HF of 2:1, taking out, grinding and polishing, etching for 4min by using 2% bromomethanol by mass fraction, ultrasonically cleaning for 5min by using absolute ethyl alcohol, and finally using N 2 And (5) drying by air.
3. The seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on THM of claim 1, wherein in step S1, the tellurium-rich solvent zone material comprises pure tellurium and a second tellurium-zinc-cadmium polycrystal, the quality of the pure tellurium and the second tellurium-zinc-cadmium polycrystal being determined in terms of mole percent with respect to Te-Cd on a CdTe T-X phase diagram.
4. The seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on THM according to claim 1, wherein in step S1, the temperature is maintained when the temperature is raised and the heating is continued until the melting point of the tellurium-rich solvent zone material, at which time the tellurium-rich solvent zone material starts to melt.
5. The seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on THM according to claim 1, wherein in step S1, the heat preservation is continued until the tellurium-rich solvent zone material is completely melted and the third tellurium-zinc-cadmium polycrystal thereabove is dissolved so that tellurium is saturated, and the heat preservation is ended.
6. The seed crystal grafting method for growing cadmium zinc telluride crystals based on THM according to claim 1, wherein in step S2, the downward moving speed of the heater is 0.1mm/h.
7. The seed crystal grafting method for growing tellurium-zinc-cadmium crystals based on THM according to claim 1, wherein in the S3 step, the upward moving speed of the heater is 0.12mm/h in both the seed crystal seeding stage and the growing shoulder stage of the tellurium-zinc-cadmium crystals; and in the equal diameter growth stage of the tellurium-zinc-cadmium crystal, the upward moving speed of the heater is 0.2mm/h, and the growth gradient is 20 ℃/cm.
8. An apparatus for growing cadmium zinc telluride crystals based on THM, for carrying out the seed crystal grafting method according to any one of claims 1-7, comprising a growth crucible (1) for the reaction, characterized in that it further comprises an adiabatic carrier (2) for placing said growth crucible (1), a SiC thermally conductive rod (4) placed at the bottom of said growth crucible (1) and for releasing its bottom temperature, and a thermocouple (5) provided on said growth crucible (1) and for monitoring the temperature of the single crystal seed crystals of zinc telluride.
9. The device for growing cadmium zinc telluride crystals based on THM according to claim 8, characterized in that said thermocouple (5) is provided in two, respectively placed in the upper end (5 a) and in the lower end (5 b) of said growth crucible (1) where the single crystal seed crystals of cadmium zinc telluride are placed.
10. The device for growing tellurium-zinc-cadmium crystals based on THM according to claim 8, wherein the SiC heat conducting rod (4) is further provided with a supporting rod (3).
CN202310259350.9A 2023-03-16 2023-03-16 Seed crystal dissolving method and device for growing tellurium-zinc-cadmium crystals based on THM Pending CN116334759A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116536768A (en) * 2023-06-29 2023-08-04 浙江珏芯微电子有限公司 Crucible for growth of tellurium-zinc-cadmium monocrystal and growth method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116536768A (en) * 2023-06-29 2023-08-04 浙江珏芯微电子有限公司 Crucible for growth of tellurium-zinc-cadmium monocrystal and growth method
CN116536768B (en) * 2023-06-29 2023-09-29 浙江珏芯微电子有限公司 Crucible for growth of tellurium-zinc-cadmium monocrystal and growth method

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