CN106435738B - A kind of cadmium-zinc-teiluride polycrystalline preparation method - Google Patents
A kind of cadmium-zinc-teiluride polycrystalline preparation method Download PDFInfo
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- CN106435738B CN106435738B CN201610836469.8A CN201610836469A CN106435738B CN 106435738 B CN106435738 B CN 106435738B CN 201610836469 A CN201610836469 A CN 201610836469A CN 106435738 B CN106435738 B CN 106435738B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
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Abstract
The present invention provides a kind of cadmium-zinc-teiluride polycrystalline preparation methods, comprising: A) cadmium telluride powder is uniformly mixed with zinc telluridse powder, obtain mixed powder；B) under vacuum conditions, the mixed powder is warming up to 600~750 DEG C, kept the temperature, pressurization obtains the first sintered body；C) once cooled down to first sintered body, release, then be cooled down twice, obtain cadmium-zinc-teiluride polycrystalline.Using method of the invention, cadmium-zinc-teiluride polycrystalline can be prepared at a lower temperature, safety is easily-controllable, saves energy consumption, advantageously reduces cost, and obtained cadmium-zinc-teiluride polycrystalline quality is high, segregation-free, is conducive to be produced in enormous quantities using the present processes.
Description
Technical field
The present invention relates to technical field of semiconductors more particularly to a kind of cadmium-zinc-teiluride polycrystalline preparation methods.
Background technique
Tellurium-zincium-cadmium crystal (English name is cadmium zinc telluride, is abbreviated as CZT) is by the IIth A of B~IV
The wide bandgap compound semiconductor of race's element composition, has zincblende lattce structure, with the variation of Zn constituent content, growth temperature
Change between 1092~1295 DEG C, be a kind of infrared crystal material haveing excellent performance, is widely used in the outer of infrared detector
Prolong substrate and indoor temperature nucleus radiation detector etc..Tellurium-zincium-cadmium crystal is also with its excellent photoelectric properties and in nuclear industry, military affairs, doctor
, environment, photovoltaic power generation, astrophysics etc. have important application prospect, become a kind of great engineering significance and strategy
The functional material of meaning.Therefore, the preparation of tellurium-zincium-cadmium crystal material just has a very important significance.
And to grow difficulty big for tellurium-zincium-cadmium crystal itself, leads to prepare tellurium-zincium-cadmium crystal as a high-leveled and difficult technology, currently, system
The method that standby cadmium-zinc-teiluride polycrystalline mainly uses is to mix tellurium, zinc, cadmium simple substance, carries out synthetic reaction, and synthetic reaction needs
(usually 1092~1295 DEG C) carry out the demand for being just able to satisfy crystal growth under hot conditions, and this synthetic method is be easy to cause
Raw material utensil is burst, both dangerous, is also wasted raw material, higher cost, meanwhile, this high―temperature nuclei method stability is poor, is not easy
Control is easy to influence the growth quality of crystal, the segregation of zinc is be easy to cause in obtained cadmium-zinc-teiluride polycrystalline, it is difficult to it is raw to carry out high-volume
It produces.
Summary of the invention
The present invention provides a kind of cadmium-zinc-teiluride polycrystalline preparation methods, according to the preparation method of the application, in lower temperature
Can be prepared by cadmium-zinc-teiluride polycrystalline under degree, safety is easily-controllable, convenient for producing in batches, and segregation-free in obtained cadmium-zinc-teiluride polycrystalline.
The present invention provides a kind of cadmium-zinc-teiluride polycrystalline preparation methods, comprising the following steps:
A cadmium telluride powder is uniformly mixed with zinc telluridse powder), obtains mixed powder；
B) under vacuum conditions, the mixed powder is warming up to 600~750 DEG C, kept the temperature, pressurization obtains the first sintering
Body；
C) once cooled down to first sintered body, release, then be cooled down twice, obtain cadmium-zinc-teiluride polycrystalline.
Preferably, the mass ratio of the cadmium telluride powder and the zinc telluridse powder is 5:(0.03~0.8).
Preferably, the granularity of the cadmium telluride powder is less than 100 mesh；The granularity of the zinc telluridse powder is less than 100 mesh.
Preferably, the step B) in, the vacuum degree of the vacuum is less than 5Pa, and the rate of the heating is 3~5 DEG C/
Min, the time of the heat preservation are 1~2h.
Preferably, the step B) in, it pressurizes after starting 10~30min of heat preservation；The pressure of the pressurization is 10
~20MPa, time are 10~30min；Heat preservation decompression is carried out after the pressurization.
Preferably, the step C) in, the primary cooling is to be cooled to 530~560 DEG C.
Preferably, the step C) it specifically includes:
C1) once cooled down to first sintered body, release, then be cooled down twice, obtain Cdl-x_Znx_Te；
C2) under vacuum conditions, the Cdl-x_Znx_Te is warming up to 600~750 DEG C, kept the temperature, pressurization obtains the second burning
Knot body；
C3) once cooled down to second sintered body, release, then be cooled down twice, obtain cadmium-zinc-teiluride polycrystalline.
Preferably, the step C2) in, the vacuum degree of the vacuum is less than 5Pa, and the rate of the heating is 5~12 DEG C/
Min, the time of the heat preservation are 3~5h.
Preferably, the step C2) in, it pressurizes after starting 10~30min of heat preservation；The pressure of the pressurization is 25
~35MPa, time are 30~50min；Heat preservation decompression is carried out after the pressurization.
Preferably, the step C3) in, the primary cooling is to be cooled to 530~560 DEG C.
Compared with prior art, the present invention provides a kind of cadmium-zinc-teiluride polycrystalline preparation methods, comprising: A) by Cadmium Telluride powder
Body is uniformly mixed with zinc telluridse powder, obtains mixed powder；B) under vacuum conditions, the mixed powder is warming up to 600~
It 750 DEG C, keeps the temperature, pressurization obtains the first sintered body；C) once cooled down to first sintered body, release, then carry out secondary
Cooling, obtains cadmium-zinc-teiluride polycrystalline.Using method of the invention, cadmium-zinc-teiluride polycrystalline can be prepared at a lower temperature, pacify
It is complete easily-controllable, energy consumption is saved, cost is advantageously reduced, and obtained cadmium-zinc-teiluride polycrystalline quality is high, segregation-free, using the side of the application
Method is conducive to be produced in enormous quantities.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of cadmium-zinc-teiluride polycrystalline preparation methods, comprising the following steps:
A cadmium telluride powder is uniformly mixed with zinc telluridse powder), obtains mixed powder；
B) under vacuum conditions, the mixed powder is warming up to 600~750 DEG C, kept the temperature, pressurization obtains the first sintering
Body；
C) once cooled down to first sintered body, release, then be cooled down twice, obtain cadmium-zinc-teiluride polycrystalline.
According to the present invention, cadmium telluride powder is uniformly mixed with zinc telluridse powder first, obtains mixed powder.
In the present invention, the source of the cadmium telluride powder and zinc telluridse powder is general commercially available without specifically limited.Institute
The granularity for stating cadmium telluride powder is preferably smaller than 100 mesh；The granularity of the zinc telluridse powder is preferably smaller than 100 mesh.The cadmium telluride
The mass ratio of powder and zinc telluridse powder is preferably 5:(0.03~0.8), in certain embodiments of the present invention, the mass ratio
It can be 5:0.03,5:0.05 or 5:0.8 etc..In the present invention, the mode that cadmium telluride powder is mixed with zinc telluridse powder is not had
It is specifically limited, powder material can be uniformly mixed, such as can be mixed by mechanical stirring mode come mixed raw material
Close powder.
According to invention, after obtaining mixed powder, under vacuum conditions, the mixed powder is warming up to 600~750
DEG C, it keeps the temperature, pressurization obtains the first sintered body.
In the present invention, after obtaining mixed powder, preferably it is evacuated to less than 5Pa, under the vacuum condition, to mixed powder
Body heating, the rate of the heating is preferably 3~5 DEG C/min, and in certain embodiments of the present invention, the rate of the heating can
Think 3 DEG C/min, 4 DEG C/min or 5 DEG C/min etc..
The present invention is preferably warming up to 600~750 DEG C, more preferably 680~750 DEG C, in certain embodiments of the present invention,
680 DEG C, 700 DEG C or 750 DEG C etc. can be warming up to.
In the present invention, after being warming up to set temperature, held for some time, the time of the heat preservation is preferably 1~2h, more excellent
It is selected as 1.5~2h, in certain embodiments of the present invention, the time of the heat preservation can be 1.5h or 2h etc..
In the present invention, preferably after starting 10~30min of heat preservation, pressurize；The pressure dwell, temperature are kept not
Become；The pressure of the pressurization is preferably 10~20MPa, more preferably 15~17MPa；After being forced into setting value, preferably pressure maintaining one
Section the time, the present invention in, preferably remain 10~30min, more preferably holding 15~20min.In the present invention, heat-insulation pressure keeping it
It afterwards, further include that heat preservation decompression obtains the first sintered body after heat preservation decompression.
According to the present invention, after obtaining the first sintered body, once cooled down to first sintered body, release, then into
Row reducing temperature twice obtains cadmium-zinc-teiluride polycrystalline.
In the present invention, the primary cooling is preferably cooled to 530~560 DEG C, in certain embodiments of the present invention, can drop
Temperature is to 550 DEG C；After being cooled to set temperature, release is carried out, preferably laying down residual compression is zero；After release, secondary drop is carried out
Temperature, the reducing temperature twice are preferably cooled to room temperature, can such as be cooled to 35 DEG C hereinafter, being more preferably down to 25~35 DEG C；Carry out
After reducing temperature twice, cadmium-zinc-teiluride polycrystalline is obtained.
According to the present invention, preferably after above-mentioned reducing temperature twice, Cdl-x_Znx_Te is obtained；After obtaining Cdl-x_Znx_Te,
It is preferred that under vacuum conditions, the Cdl-x_Znx_Te being warming up to 600~750 DEG C, is kept the temperature, pressurization obtains the second sintered body.
For the present invention after obtaining Cdl-x_Znx_Te, it is also preferable to include the Cdl-x_Znx_Te is crushed to granularity less than 100
Mesh obtains cadmium-zinc-teiluride powder.
In the present invention, after obtaining cadmium-zinc-teiluride powder, preferably it is evacuated to less than 5Pa, under the vacuum condition, after progress
Continuous step；In the present invention, under the vacuum condition, the cadmium-zinc-teiluride powder is preferably warming up to 600~750 DEG C, more preferably
It is 680~750 DEG C；The rate of the heating is preferably 5~12 DEG C/min, in certain embodiments of the present invention, the heating
Rate can be 10 DEG C/min.
In the present invention, after being warming up to the set temperature, held for some time；The time of the heat preservation is preferably 3~5h.
In the present invention, preferably after starting 10~30min of heat preservation, pressurize；The pressure dwell, temperature are kept not
Become；The pressure of the pressurization is preferably 25~35MPa, more preferably 25~30MPa；After being forced into setting value, preferably pressure maintaining one
Section the time, the present invention in, preferably remain 30~50min, more preferably holding 40~50min.In the present invention, heat-insulation pressure keeping it
It afterwards, further include that heat preservation decompression obtains the second sintered body after heat preservation decompression.
In the present invention, after obtaining the second sintered body, once cooled down to second sintered body, release, then carry out
Reducing temperature twice obtains cadmium-zinc-teiluride polycrystalline.
In the present invention, the primary cooling is preferably dropped to 530~560 DEG C, in certain embodiments of the present invention, can drop
Temperature is to 550 DEG C；After being cooled to set temperature, release is carried out, preferably laying down residual compression is zero；After release, secondary drop is carried out
Temperature, the reducing temperature twice are preferably cooled to room temperature, can such as be cooled to 35 DEG C hereinafter, being more preferably down to 25~35 DEG C；Carry out
After reducing temperature twice, cadmium-zinc-teiluride polycrystalline is obtained.Using method of the invention, double sintering is carried out, is conducive to preferably promote tellurium zinc
Cadmium crystal growth, the uniform segregation-free of cadmium-zinc-teiluride polycrystalline made, quality are higher.
In the present invention, after obtaining cadmium-zinc-teiluride polycrystalline, the cadmium-zinc-teiluride polycrystalline can be surface-treated, it such as can be by right
Cadmium-zinc-teiluride polycrystalline surface carries out the mode of polishing etc., to purify the cadmium-zinc-teiluride polycrystalline.It, can be according to need after surface treatment
It asks and the cadmium-zinc-teiluride polycrystalline is crushed to different size of cadmium-zinc-teiluride multiple grain or cadmium-zinc-teiluride polycrystal powder etc..
In the present invention, mixed powder raw material is preferably subjected to above-mentioned sintering loaded on being placed in agglomerating plant in material container
Process；In certain embodiments of the present invention, the material container can be hot pressing graphite grinding tool；The agglomerating plant can be
Hot pressing furnace.
The present invention provides a kind of cadmium-zinc-teiluride polycrystalline preparation methods, comprising the following steps: A) by cadmium telluride powder and tellurium
Change zinc powder body to be uniformly mixed, obtains mixed powder；B) under vacuum conditions, the mixed powder is warming up to 600~750 DEG C,
Heat preservation, pressurization, obtains the first sintered body；C) once cooled down to first sintered body, release, then be cooled down twice,
Obtain cadmium-zinc-teiluride polycrystalline.Using ad hoc approach of the invention, cadmium-zinc-teiluride polycrystalline can be prepared at a lower temperature, safety
It is easily-controllable, energy consumption is saved, cost is advantageously reduced, and obtained cadmium-zinc-teiluride polycrystalline quality is high, segregation-free, using the present processes
Be conducive to carry out high-volume industrial production.
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1
Zinc telluridse powder of the cadmium telluride powder with 0.03Kg granularity less than 100 mesh by 5kg granularity less than 100 mesh mixes
It is even, obtain mixed powder；The mixed powder is fitted into hot pressing graphite jig and is placed in hot pressing furnace；Hot pressing furnace is evacuated to
Less than 5Pa, hot pressing furnace is warming up to 680 DEG C with the heating rate of 3 DEG C/min, keeps the temperature 1.5h；Start 10min in above-mentioned heat preservation
Afterwards, it pressurizes, adds to 17MPa, after keeping 20min, start heat preservation decompression and start to cool down, drop to after keeping the temperature up to 1.5h
At 550 DEG C, it is zero that residual compression, which is laid down, is cooled to 25~35 DEG C later, takes out hot pressing graphite jig and demoulds, obtains tellurium zinc
Cadmium material.Gained Cdl-x_Znx_Te is crushed to granularity less than 100 mesh, is fitted into hot pressing graphite jig and is placed in hot pressing furnace；
Hot pressing furnace is evacuated to less than 5Pa, hot pressing furnace is warming up to 680 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 3h；Above-mentioned
It after heat preservation starts 10min, pressurizes, adds to 30MPa, after keeping 40min, start heat preservation decompression, reach 3h in heat preservation total duration
Afterwards, start to cool down, when dropping to 550 DEG C, it is zero that residual compression, which is laid down, is cooled to 25~35 DEG C later, takes out hot pressing graphite mo(u)ld
Have and demould, obtains cadmium-zinc-teiluride polycrystalline.
Segregation detection is carried out to gained cadmium-zinc-teiluride polycrystalline using ICP method, that is, utilizes the analysis method point of statistical distribution in situ
Whether the constituent content for analysing different location point in polycrystal is uniform；The point of 4 or more different locations is taken to gained cadmium-zinc-teiluride polycrystalline,
It analyzes the mass ratio of position Zn element and compares, the results show that the Zn constituent content of different location point is very close, respectively
The mass deviation of location point Zn element is lower than 0.25%, i.e. gained cadmium-zinc-teiluride polycrystalline is visibly homogeneous, segregation-free.
Embodiment 2
Zinc telluridse powder of the cadmium telluride powder with 0.8Kg granularity less than 100 mesh by 5kg granularity less than 100 mesh mixes
It is even, obtain mixed powder；The mixed powder is fitted into hot pressing graphite jig and is placed in hot pressing furnace；Hot pressing furnace is evacuated to
Less than 5Pa, hot pressing furnace is warming up to 750 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 2h；After above-mentioned heat preservation starts 10min,
It pressurizes, adds to 15MPa, after keeping 20min, start heat preservation decompression and start to cool down, drop to 550 DEG C after keeping the temperature up to 2h
When, it is zero that residual compression, which is laid down, is cooled to 25~35 DEG C later, takes out hot pressing graphite jig and demoulds, obtains cadmium-zinc-teiluride material
Material.Gained Cdl-x_Znx_Te is crushed to granularity less than 100 mesh, is fitted into hot pressing graphite jig and is placed in hot pressing furnace；It will be hot
Stove evacuation to less than 5Pa are pressed, hot pressing furnace is warming up to 750 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 5h；In above-mentioned heat preservation
It after beginning 10min, pressurizes, adds to 28MPa, after keeping 50min, start heat preservation decompression, after heat preservation total duration reaches 5h, open
Begin to cool down, when dropping to 550 DEG C, it is zero that residual compression, which is laid down, is cooled to 25~35 DEG C later, takes out hot pressing graphite jig and simultaneously takes off
Mould obtains cadmium-zinc-teiluride polycrystalline.
Segregation detection is carried out to gained cadmium-zinc-teiluride polycrystalline according to the method for embodiment 1, the results show that the Zn of different location point
Constituent content is very close, and the mass deviation of each position point Zn element is lower than 0.04%, i.e. gained cadmium-zinc-teiluride polycrystalline is visibly homogeneous,
Segregation-free.
Embodiment 3
Zinc telluridse powder of the cadmium telluride powder with 0.05Kg granularity less than 100 mesh by 5kg granularity less than 100 mesh mixes
It is even, obtain mixed powder；The mixed powder is fitted into hot pressing graphite jig and is placed in hot pressing furnace；Hot pressing furnace is evacuated to
Less than 5Pa, hot pressing furnace is warming up to 700 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 1.5h；Start 10min in above-mentioned heat preservation
Afterwards, it pressurizes, adds to 15MPa, after keeping 15min, start heat preservation decompression and start to cool down, drop to after keeping the temperature up to 1.5h
At 550 DEG C, it is zero that residual compression, which is laid down, is cooled to 25~35 DEG C later, takes out hot pressing graphite jig and demoulds, obtains tellurium zinc
Cadmium material.Gained Cdl-x_Znx_Te is crushed to granularity less than 100 mesh, is fitted into hot pressing graphite jig and is placed in hot pressing furnace；
Hot pressing furnace is evacuated to less than 5Pa, hot pressing furnace is warming up to 700 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 4h；Above-mentioned
It after heat preservation starts 10min, pressurizes, adds to 25MPa, after keeping 40min, start heat preservation decompression, reach 4h in heat preservation total duration
Afterwards, start to cool down, when dropping to 550 DEG C, it is zero that residual compression, which is laid down, is cooled to 25~35 DEG C later, takes out hot pressing graphite mo(u)ld
Have and demould, obtains cadmium-zinc-teiluride polycrystalline.
Segregation detection is carried out to gained cadmium-zinc-teiluride polycrystalline according to the method for embodiment 1, the results show that the Zn of different location point
Constituent content is very close, and the mass deviation of each position point Zn element is lower than 0.29%, i.e. gained cadmium-zinc-teiluride polycrystalline is visibly homogeneous,
Segregation-free.
Preparing the method that cadmium-zinc-teiluride polycrystalline mainly uses in the prior art is to mix tellurium, zinc, cadmium simple substance, synthesize anti-
It answers, and synthetic reaction needs carry out the need for being just able to satisfy crystal growth under the high temperature conditions (usually 1092~1295 DEG C)
It asks, this synthetic method be easy to cause raw material utensil to burst, and it is both dangerous, it also wastes raw material, higher cost, single can only carry out
A small amount of synthesis, it is difficult to the preparation of kilogram magnitude is carried out, meanwhile, this high―temperature nuclei method stability is not poor, easily-controllable, is easy shadow
The growth quality of crystal is rung, be easy to cause segregation in obtained cadmium-zinc-teiluride polycrystalline, it is difficult to be produced in enormous quantities.Compared to existing
Cadmium-zinc-teiluride polycrystalline can be prepared in technology, the method according to the invention at a lower temperature, and safety is easily-controllable, save energy consumption,
Cost is advantageously reduced, and obtained cadmium-zinc-teiluride polycrystalline quality is high, segregation-free, and single may be implemented and largely synthesize, and uses
The present processes are conducive to carry out high-volume industrial production.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.To these embodiments
A variety of modifications will be readily apparent to those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to widest model consistent with the principles and novel features disclosed in this article
It encloses.
Claims (9)
1. a kind of cadmium-zinc-teiluride polycrystalline preparation method, which comprises the following steps:
A cadmium telluride powder is uniformly mixed with zinc telluridse powder), obtains mixed powder；
B) under vacuum conditions, the mixed powder is warming up to 600~750 DEG C, kept the temperature, pressurization obtains the first sintered body；
The time of the heat preservation is 1~2h；
C) once cooled down to first sintered body, release, then be cooled down twice, obtain cadmium-zinc-teiluride polycrystalline；
The temperature once to cool down is 530~560 DEG C.
2. preparation method according to claim 1, which is characterized in that the cadmium telluride powder and the zinc telluridse powder
Mass ratio is 5:(0.03~0.8).
3. preparation method according to claim 1, which is characterized in that the granularity of the cadmium telluride powder is less than 100 mesh；Institute
The granularity of zinc telluridse powder is stated less than 100 mesh.
4. preparation method according to claim 1, which is characterized in that the step B) in, the vacuum degree of the vacuum is small
In 5Pa, the rate of the heating is 3~5 DEG C/min.
5. preparation method according to claim 1, which is characterized in that the step B) in, starting 10~30min of heat preservation
After pressurize；The pressure of the pressurization is 10~20MPa, and the time is 10~30min；Heat preservation drop is carried out after the pressurization
Pressure.
6. preparation method according to claim 1, which is characterized in that the step C) it specifically includes:
C1) once cooled down to first sintered body, release, then be cooled down twice, obtain Cdl-x_Znx_Te；
C2) under vacuum conditions, the Cdl-x_Znx_Te is warming up to 600~750 DEG C, kept the temperature, pressurization obtains the second sintering
Body；
C3) once cooled down to second sintered body, release, then be cooled down twice, obtain cadmium-zinc-teiluride polycrystalline.
7. preparation method according to claim 6, which is characterized in that the step C2) in, the vacuum degree of the vacuum is small
In 5Pa, the rate of the heating is 5~12 DEG C/min, and the time of the heat preservation is 3~5h.
8. preparation method according to claim 6, which is characterized in that the step C2) in, start heat preservation 10~
It pressurizes after 30min；The pressure of the pressurization is 25~35MPa, and the time is 30~50min；It is protected after the pressurization
Temperature drop pressure.
9. preparation method according to claim 6, which is characterized in that the step C3) in, the primary cooling is cooling
To 530~560 DEG C.
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| CN113818086B (en) * | 2021-09-23 | 2022-07-08 | 安徽光智科技有限公司 | Growth method of cadmium zinc telluride crystal |
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