CN116163021A - Growth device and growth method of tellurium-zinc-cadmium crystal - Google Patents

Growth device and growth method of tellurium-zinc-cadmium crystal Download PDF

Info

Publication number
CN116163021A
CN116163021A CN202310174154.1A CN202310174154A CN116163021A CN 116163021 A CN116163021 A CN 116163021A CN 202310174154 A CN202310174154 A CN 202310174154A CN 116163021 A CN116163021 A CN 116163021A
Authority
CN
China
Prior art keywords
cadmium
zinc
tellurium
growth
crucible
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202310174154.1A
Other languages
Chinese (zh)
Inventor
黄晟
黄立
严冰
刘伟华
余志杰
喻畅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Gaoxin Technology Co Ltd
Original Assignee
Wuhan Gaoxin Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan Gaoxin Technology Co Ltd filed Critical Wuhan Gaoxin Technology Co Ltd
Priority to CN202310174154.1A priority Critical patent/CN116163021A/en
Publication of CN116163021A publication Critical patent/CN116163021A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention belongs to the technical field of crystal growth, and particularly relates to a growth device and a growth method for improving the single crystal rate and quality of tellurium-zinc-cadmium crystals. The invention provides a growth device and a growth method of tellurium-zinc-cadmium crystals, which effectively reduce adverse effects of crucible periphery unevenness caused by air flow in a furnace by vacuumizing and sealing a tube with double crucibles. And a graphite ring is arranged on the periphery of the tellurium-zinc-cadmium crystal, and surrounds the equal-diameter area of the crystal material, so that the tellurium-zinc-cadmium crystal material is uniformly heated and radiated, the uniformity in the crystal growth process is further improved, in addition, the solid-liquid shape of the tellurium-zinc-cadmium crystal growth can be flattened, and the growth of a large single crystal is facilitated.

Description

Growth device and growth method of tellurium-zinc-cadmium crystal
Technical Field
The invention relates to the technical field of crystal growth, in particular to a growth device and a growth method for improving the single crystal rate and quality of tellurium-zinc-cadmium crystals.
Background
Cadmium Zinc Telluride (CZT) substrate materials are the most ideal substrate materials for mercury cadmium telluride epitaxy. The development of high-performance tellurium-cadmium-mercury infrared focal plane devices, long-wave infrared focal plane devices, novel tellurium-cadmium-mercury avalanche type infrared focal plane technologies and high-temperature working infrared focal plane technologies depends on tellurium-zinc-cadmium substrate materials.
However, compared with crystal growth of semiconductor materials such as Si and GaAs, the physical properties of CZT are relatively special and belong to ternary alloys, and these physical properties determine that growing such single crystals has great difficulty: the low thermal conductivity ensures that the heat released in the crystallization process is not easy to be dispersed, and the solid-liquid interface shape of a flat or slightly convex melt is difficult to form; the stacking fault energy is low, twins and faults are easy to generate in the crystal growth process due to the non-uniformity of the temperature field, and a large number of dislocations are easy to generate.
The melt method is the main stream mode for growing tellurium-zinc-cadmium crystal at present, and the principle is that high-purity raw materials or polycrystal materials are melted at high temperature, and then the melt is slowly crystallized from the head part to the tail part of a crucible through various growth technologies, so that a monocrystal is obtained. The conventional technology mainly comprises a Bridgman method, a vertical gradient solidification method and a moving heater method.
In the growth device and the growth method for preparing tellurium-zinc-cadmium crystals in the prior art, the temperature field of a furnace body is uniformly limited by equipment manufacture, and convection in the furnace body is influenced. Points with uneven temperature often exist, heterogeneous nucleation points are easy to occur in the whole growth process, and various defects are generated in the growth process. Meanwhile, because the tellurium-zinc-cadmium thermal conductivity is low, a flat and slightly convex solid-liquid interface is difficult to form, so that the single crystal rate is low.
Thus, there is a need for a solution to the technical problems of the prior art.
Disclosure of Invention
The invention provides a growth device and a growth method of tellurium-zinc-cadmium crystals, which at least can solve part of problems in the prior art.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
the device for growing the tellurium-zinc-cadmium crystal comprises a first quartz crucible and a second quartz crucible, wherein the first quartz crucible is arranged in the second quartz crucible, and a PBN crucible is arranged in the first quartz crucible.
As a preferable scheme of the growth device of tellurium-zinc-cadmium crystals, the invention comprises the following steps: the growth device of the tellurium-zinc-cadmium crystal further comprises a graphite ring, and the graphite ring is positioned between the first quartz crucible and the second quartz crucible.
As a preferable scheme of the growth device of tellurium-zinc-cadmium crystals, the invention comprises the following steps: the graphite ring surrounds the isodiametric region of the tellurium-zinc-cadmium crystal material in the PBN crucible.
As a preferable scheme of the growth device of tellurium-zinc-cadmium crystals, the invention comprises the following steps: the growth device of the tellurium-zinc-cadmium crystal further comprises a crucible supporting quartz positioned in the second quartz crucible, and the crucible supporting quartz supports the first quartz crucible.
As a preferable scheme of the growth device of tellurium-zinc-cadmium crystals, the invention comprises the following steps: the growth device of the tellurium-zinc-cadmium crystal further comprises graphite ring supporting quartz which is positioned in the second quartz crucible, and the graphite ring supporting quartz supports the graphite ring.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
a method for growing tellurium-zinc-cadmium crystals, wherein: the growth method of the tellurium-zinc-cadmium crystal comprises the following steps:
s1: putting tellurium-zinc-cadmium materials into a PBN crucible positioned in a first quartz crucible, and vacuumizing and sealing the first quartz crucible;
s2: loading the first quartz crucible into the second quartz crucible;
s3: and (5) vacuumizing and sealing the second quartz crucible, and loading the second quartz crucible into a single crystal furnace to grow tellurium-zinc-cadmium crystals.
As a preferable scheme of the growth method of tellurium-zinc-cadmium crystal, the invention comprises the following steps: the step S2 further includes: and loading a graphite ring into the second quartz crucible, wherein the graphite ring is positioned between the first quartz crucible and the second quartz crucible.
As a preferable scheme of the growth method of tellurium-zinc-cadmium crystal, the invention comprises the following steps: the step S2 further includes: and loading crucible supporting quartz and graphite ring supporting quartz into a second quartz crucible for supporting the first quartz crucible and the graphite ring respectively.
As a preferable scheme of the growth method of tellurium-zinc-cadmium crystal, the invention comprises the following steps: the vacuum degree in the step S1 is 10 -5 -10 -4 Pa。
As a preferable scheme of the growth method of tellurium-zinc-cadmium crystal, the invention comprises the following steps: the vacuum degree in the step S3 is 0.1-10Pa.
As a preferable scheme of the growth device of tellurium-zinc-cadmium crystals, the invention comprises the following steps: in the step S3, the vertical Bridgman method or the vertical gradient solidification method is adopted for single crystal growth, the growth speed is 0.5-1.0mm/h, and the growth temperature gradient is 3-12 ℃/mm.
The beneficial effects of the invention are as follows:
1. the tellurium-zinc-cadmium crystal growth device adopts a double-crucible structure, and the convection of the gas at the periphery of the grown crystal is reduced to the greatest extent by vacuumizing and sealing the double-crucible, so that the adverse effect of the non-uniformity at the periphery of the crucible caused by the air flow in the furnace is effectively reduced.
2. According to the invention, the graphite ring is also arranged on the periphery of the tellurium-zinc-cadmium crystal, and can uniformly heat and radiate the tellurium-zinc-cadmium crystal material, so that the uniformity in the crystal growth process is further improved.
3. The graphite ring only wraps the isodiametric part of the tellurium-zinc-cadmium, so that the temperature of the outer wall of the crystal is higher, the temperature of the inner part of the crystal is lower, heat is guaranteed to be led out from the head part of the center of the crystal, the solid-liquid shape of the tellurium-zinc-cadmium crystal growth is flattened, and the growth of a large single crystal is facilitated.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a first growth crucible for producing cadmium zinc telluride crystals according to the present invention;
FIG. 2 is a schematic diagram of the structure of a double-layer crucible for tellurium-zinc-cadmium crystal growth.
Reference numerals illustrate:
1-first quartz crucible, 2-PBN crucible, 3-second quartz crucible, 4-crucible supporting quartz, 5-graphite ring, 6-graphite ring supporting quartz.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications (such as up, down, left, right, front, and rear … …) are included in the embodiments of the present invention, the directional indications are merely used to explain the relative positional relationship, movement conditions, etc. between the components in a specific posture (as shown in the drawings), and if the specific posture is changed, the directional indications are correspondingly changed.
In addition, if there is a description of "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The invention provides a growth device and a growth method of tellurium-zinc-cadmium crystals, which effectively reduce adverse effects of crucible periphery unevenness caused by air flow in a furnace by vacuumizing and sealing a tube with double crucibles. The periphery of the tellurium-zinc-cadmium crystal is also provided with a graphite ring, the graphite ring surrounds a main growth area of the crystal material, and the tellurium-zinc-cadmium crystal material is uniformly heated and radiated, so that the uniformity in the crystal growth process is further improved, meanwhile, the growth side wall is kept at a higher temperature, the solid-liquid shape of the tellurium-zinc-cadmium crystal growth is beneficial to planarization, and the growth of large single crystals is more beneficial to.
Example 1
The growth method of tellurium-zinc-cadmium crystal adopts a tellurium-zinc-cadmium crystal growth device to grow the crystal, as shown in figures 1-2, the tellurium-zinc-cadmium crystal growth device comprises a first quartz crucible 1 and a second quartz crucible 3, the first quartz crucible 1 is arranged in the second quartz crucible 3, a PBN (pyrolytic boron nitride) crucible 2 is arranged in the first quartz crucible 1, and the PBN crucible 2 is used for loading tellurium-zinc-cadmium crystal materials. The inner and outer double-crucible structures of the first quartz crucible 1 and the second quartz crucible 3 can provide a vacuum environment for tellurium-zinc-cadmium crystal growth, and the disturbance influence of the peripheral air flow of the crystal in the tellurium-zinc-cadmium crystal growth process is reduced to the greatest extent.
The second quartz crucible 3 is internally provided with a crucible supporting quartz 4 for supporting the first quartz crucible 1, so that the stability of the first quartz crucible 1 and the stable growth of tellurium-zinc-cadmium crystals are ensured.
A graphite ring 5 is arranged between the first quartz crucible 1 and the second quartz crucible 3, and the graphite ring 5 wraps the equal diameter area of the tellurium-zinc-cadmium crystal material. The shape of the crystal in the growth process of the tellurium-zinc-cadmium crystal is determined by the shape of the PBN crucible, and a necking growth area, a shouldering growth area and an equal diameter area are sequentially formed in the crystal growth process, wherein the equal diameter area is a part with the same fixed upper and lower diameters in the crystal rod.
And a graphite ring supporting quartz 6 is arranged in the second quartz crucible 3 and is used for supporting the graphite ring 5, so that the heating stability of the graphite ring is ensured.
The preparation method of the tellurium-zinc-cadmium crystal by adopting the crystal growth device comprises the following steps:
cadmium zinc telluride material is filled into a PBN crucible 2 positioned in a first quartz crucible 1, the first quartz crucible 1 is vacuumized and sealed, and the vacuum degree is set to be 10 -5 Pa；
Loading a crucible supporting quartz 4 and a graphite ring supporting quartz 6 into the second quartz crucible 3 for supporting the first quartz crucible 1 and the graphite ring 5 respectively;
a graphite ring 5 is placed on a graphite supporting quartz 6 in a second quartz crucible 3, and a first quartz crucible 1 is loaded into the second quartz crucible 3 and placed on a crucible supporting quartz 4. And (3) vacuumizing and sealing the tube of the second quartz crucible 3, setting the vacuum degree to be 10Pa, then loading the tube into a single crystal furnace, and adopting a vertical Bridgman method to grow tellurium-zinc-cadmium crystals, wherein the growth speed is 0.5mm/h, the growth temperature gradient is 3.0 ℃/mm, and the crystallization rate is 75%.
Example 2
The growth method of tellurium-zinc-cadmium crystal adopts the growth device of the embodiment 1 to prepare the tellurium-zinc-cadmium crystal, and specifically comprises the following steps:
cadmium zinc telluride material is filled into a PBN crucible 2 positioned in a first quartz crucible 1, the first quartz crucible 1 is vacuumized and sealed, and the vacuum degree is set to be 10 -5 Pa；
Loading a crucible supporting quartz 4 and a graphite ring supporting quartz 6 into the second quartz crucible 3 for supporting the first quartz crucible 1 and the graphite ring 5 respectively;
a graphite ring 5 is placed on a graphite supporting quartz 6 in a second quartz crucible 3, and a first quartz crucible 1 is loaded into the second quartz crucible 3 and placed on a crucible supporting quartz 4. And (3) vacuumizing and sealing the tube of the second quartz crucible 3, setting the vacuum degree to be 0.1Pa, then loading the tube into a single crystal furnace, and adopting a vertical Bridgman method to grow tellurium-zinc-cadmium crystals, wherein the growth speed is 1.0mm/h, the growth temperature gradient is 10.0 ℃/mm, and the crystallization rate is 70%.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.

Claims (10)

1. The growth device of the tellurium-zinc-cadmium crystal is characterized by comprising a first quartz crucible (1) and a second quartz crucible (3), wherein the first quartz crucible (1) is arranged in the second quartz crucible (3), and a PBN crucible (2) is arranged in the first quartz crucible (1).
2. A device for growing cadmium zinc telluride crystals as claimed in claim 1, characterized in that it further comprises a graphite ring (5), said graphite ring (5) being located between said first quartz crucible (1) and said second quartz crucible (3).
3. A growth device for cadmium zinc telluride crystals as claimed in claim 2, characterised in that the graphite ring (5) encloses the isodiametric region of the cadmium zinc telluride crystal material within the PBN crucible (2).
4. A growth device for cadmium zinc telluride crystals as claimed in claim 1, further comprising a crucible supporting quartz (4) located in the second quartz crucible (3), the crucible supporting quartz (4) supporting the first quartz crucible (1).
5. A growth device for cadmium zinc telluride crystals as claimed in claim 2, further comprising a graphite ring supporting quartz (6) located in the second quartz crucible (3), the graphite ring supporting quartz (6) supporting the graphite ring (5).
6. A growth method of tellurium-zinc-cadmium crystal is characterized in that: the growth method of the tellurium-zinc-cadmium crystal comprises the following steps:
s1: putting a tellurium-zinc-cadmium material into a PBN crucible (2) positioned in a first quartz crucible (1), and vacuumizing and sealing the first quartz crucible (1);
s2: loading a first quartz crucible (1) into a second quartz crucible (3);
s3: and (3) vacuumizing and sealing the second quartz crucible (3), and loading the second quartz crucible into a single crystal furnace to grow tellurium-zinc-cadmium crystals.
7. The method for growing cadmium zinc telluride crystals according to claim 6 wherein said step S2 further comprises: a graphite ring (5) is arranged in the second quartz crucible (3), and the graphite ring (5) is positioned between the first quartz crucible (1) and the second quartz crucible (3).
8. The method for growing cadmium zinc telluride crystals according to claim 7 wherein said step S2 further comprises: a crucible supporting quartz (4) and a graphite ring supporting quartz (6) are filled into a second quartz crucible (3) and are respectively used for supporting the first quartz crucible (1) and the graphite ring (5).
9. The method for growing tellurium-zinc-cadmium crystals according to claim 6, wherein: the vacuum degree in the step S1 is 10 -5 -10 -4 Pa, wherein the vacuum degree in the step S3 is 0.1-10Pa.
10. The method for growing tellurium-zinc-cadmium crystals according to claim 6, wherein: in the step S3, the vertical Bridgman method or the vertical gradient solidification method is adopted for single crystal growth, the growth speed is 0.5-1.0mm/h, and the growth temperature gradient is 3-12 ℃/mm.
CN202310174154.1A 2023-02-28 2023-02-28 Growth device and growth method of tellurium-zinc-cadmium crystal Pending CN116163021A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310174154.1A CN116163021A (en) 2023-02-28 2023-02-28 Growth device and growth method of tellurium-zinc-cadmium crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310174154.1A CN116163021A (en) 2023-02-28 2023-02-28 Growth device and growth method of tellurium-zinc-cadmium crystal

Publications (1)

Publication Number Publication Date
CN116163021A true CN116163021A (en) 2023-05-26

Family

ID=86418073

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310174154.1A Pending CN116163021A (en) 2023-02-28 2023-02-28 Growth device and growth method of tellurium-zinc-cadmium crystal

Country Status (1)

Country Link
CN (1) CN116163021A (en)

Similar Documents

Publication Publication Date Title
CN110983429A (en) Single crystal furnace and monocrystalline silicon preparation method
JP4083449B2 (en) CdTe single crystal manufacturing method
CN111020689A (en) Crystal growth apparatus and method
CN114481289A (en) Growth method and device for increasing tellurium-zinc-cadmium single crystal rate
JP5671057B2 (en) Method for producing germanium ingot with low micropit density (MPD) and apparatus for growing germanium crystals
CN103469304B (en) Branched shaping sapphire crystallization device and long crystal method thereof
CN116516463A (en) Thermal field structure and method for growing silicon carbide single crystal by solution method
CN116163021A (en) Growth device and growth method of tellurium-zinc-cadmium crystal
KR101530349B1 (en) The insulation structure for a sapphire single crystal growth
TWI760030B (en) A thermal barrier device for insulating heat and a smelting furnace
JP2704032B2 (en) Method for manufacturing compound semiconductor single crystal
CN114808106B (en) GaAs single crystal growth process
CN214193528U (en) Crucible support for crystal growth
JP2004099390A (en) Method of manufacturing compound semiconductor single crystal and compound semiconductor single crystal
JP2001080987A (en) Device for producing compound semiconductor crystal and production process using the same
CN117026360A (en) Device and method for growing large-size low dislocation density GaSb monocrystal
JPH11274537A (en) Manufacture of polycrystalline silicon of large grain size
JPH04198084A (en) Jig for preventing bottom adhesion in pull-up of semiconductor single crystal
CN117071053A (en) Method for preparing compound crystal by VGF in LEC growth system
JPH03193689A (en) Production of compound semiconductor crystal
JP2004026577A (en) Apparatus for growing compound semiconductor single crystal and method of growing compound semiconductor single crystal
JPH10212192A (en) Method for growing bulk crystal
JPH04187585A (en) Device of growing crystal
JP4155085B2 (en) Method for producing compound semiconductor single crystal
CN117071076A (en) Indium arsenide crystal synthesis growth device and method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination