CN106435738A - Preparation method of cadmium zinc telluride polycrystals - Google Patents

Preparation method of cadmium zinc telluride polycrystals Download PDF

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Publication number
CN106435738A
CN106435738A CN201610836469.8A CN201610836469A CN106435738A CN 106435738 A CN106435738 A CN 106435738A CN 201610836469 A CN201610836469 A CN 201610836469A CN 106435738 A CN106435738 A CN 106435738A
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cadmium
preparation
zinc
temperature
teiluride
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CN106435738B (en
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文崇斌
朱刘
胡智向
何志达
李琴香
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Qingyuan Xiandao Materials Co Ltd
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Vital Materials Co Ltd
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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
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/02Production of homogeneous polycrystalline material with defined structure directly from the solid state

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

Abstract

The invention provides a preparation method of cadmium zinc telluride polycrystals. The preparation method comprises the following steps of A, uniformly mixing cadmium telluride powder and zinc telluride power to obtain mixed powder; B, under the vacuum condition, raising the temperature of the mixed powder to 600 to 750 DEG C; performing heat insulation and pressurization to obtain a first sintering body; C, performing primary temperature reduction on the first sintering body; relieving the pressure; then, performing secondary temperature reduction to obtain the cadmium zinc telluride polycrystals. By using the method, the cadmium zinc telluride polycrystals can be obtained through preparation at low temperature; safety is realized; the control is easy; the energy consumption is reduced; the cost is favorably reduced; in addition, the obtained cadmium zinc telluride polycrystals have high quality and no segregation. By using the method provided by the invention, the mass production can be favorably performed.

Description

A kind of preparation method of cadmium-zinc-teiluride polycrystalline
Technical field
The present invention relates to technical field of semiconductors, more particularly, to a kind of preparation method of cadmium-zinc-teiluride polycrystalline.
Background technology
Tellurium-zincium-cadmium crystal (English name is cadmium zinc telluride, is abbreviated as CZT) is by the IIth B~IV A The elementary composition wide bandgap compound semiconductor of race, has zincblende lattce structure, with the change of Zn constituent content, its growth temperature Change between 1092~1295 DEG C, be a kind of infrared crystal material of excellent performance, be widely used in the outer of Infrared Detectorss Prolong substrate and indoor temperature nucleus radiation detector etc..Tellurium-zincium-cadmium crystal is also with its excellent photoelectric properties in nuclear industry, military affairs, doctor The aspects such as, environment, photovoltaic generation, astrophysics 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 and is of great significance.
And tellurium-zincium-cadmium crystal growth difficulty itself is big, leading to prepare tellurium-zincium-cadmium crystal becomes a high-leveled and difficult technology, at present, system The method that standby cadmium-zinc-teiluride polycrystalline mainly adopts is by tellurium, zinc, the mixing of cadmium simple substance, carries out synthetic reaction, and synthetic reaction needs Under hot conditionss, (usually 1092~1295 DEG C) carry out meeting the demand of crystal growth, and this synthetic method easily causes Raw material utensil bursts, both dangerous, also wastes raw material, relatively costly, and meanwhile, this high-temperature nuclei method stability is poor, be difficult Control, easily affects the growth quality of crystal, easily causes the segregation of zinc it is difficult to carry out high-volume life in the cadmium-zinc-teiluride polycrystalline obtaining Produce.
Content of the invention
The invention provides a kind of preparation method of cadmium-zinc-teiluride polycrystalline, according to the preparation method of the application, in relatively low temperature Can be prepared by cadmium-zinc-teiluride polycrystalline under degree, safety is easily-controllable, be easy to produce in batches, and segregation-free in the cadmium-zinc-teiluride polycrystalline obtaining.
The invention provides a kind of preparation method of cadmium-zinc-teiluride polycrystalline, comprise the following steps:
A) cadmium telluride powder body is mixed homogeneously with zinc telluridse powder body, obtain mixed powder;
B) under vacuum, described mixed powder is warming up to 600~750 DEG C, insulation, pressurization, obtain the first sintering Body;
C) described first sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.
Preferably, described cadmium telluride powder body and the mass ratio of described zinc telluridse powder body are 5:(0.03~0.8).
Preferably, the granularity of described cadmium telluride powder body is less than 100 mesh;The granularity of described zinc telluridse powder body is less than 100 mesh.
Preferably, described step B) in, the vacuum of described vacuum is less than 5Pa, and the speed of described intensification is 3~5 DEG C/ Min, the time of described insulation is 1~2h.
Preferably, described step B) in, pressurizeed after starting to be incubated 10~30min;The pressure of described pressurization is 10 ~20MPa, the time is 10~30min;Carry out being incubated blood pressure lowering after described pressurization.
Preferably, described step C) in, described once lower the temperature as being cooled to 530~560 DEG C.
Preferably, described step C) specifically include:
C1) described first sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain Cdl-x_Znx_Te;
C2) under vacuum, described Cdl-x_Znx_Te is warming up to 600~750 DEG C, insulation, pressurization, obtain the second burning Knot body;
C3) described second sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.
Preferably, described step C2) in, the vacuum of described vacuum is less than 5Pa, and the speed of described intensification is 5~12 DEG C/ Min, the time of described insulation is 3~5h.
Preferably, described step C2) in, pressurizeed after starting to be incubated 10~30min;The pressure of described pressurization is 25 ~35MPa, the time is 30~50min;Carry out being incubated blood pressure lowering after described pressurization.
Preferably, described step C3) in, described once lower the temperature as being cooled to 530~560 DEG C.
Compared with prior art, the invention provides a kind of preparation method of cadmium-zinc-teiluride polycrystalline, including:A) by Cadmium Telluride powder Body is mixed homogeneously with zinc telluridse powder body, obtains mixed powder;B) under vacuum, described mixed powder is warming up to 600~ 750 DEG C, insulation, pressurization, obtain the first sintered body;C) described first sintered body is once lowered the temperature, release, then carry out secondary Cooling, obtains cadmium-zinc-teiluride polycrystalline.Using the method for the present invention, cadmium-zinc-teiluride polycrystalline can be prepared at a lower temperature, peace Entirely easily-controllable, save energy consumption, advantageously reduce cost, and the cadmium-zinc-teiluride polycrystalline quality obtaining is high, segregation-free, using the side of the application Method is conducive to being produced in enormous quantities.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme is clearly and completely described it is clear that institute The embodiment of description is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, The every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, broadly falls into this The scope of bright protection.
The invention provides a kind of preparation method of cadmium-zinc-teiluride polycrystalline, comprise the following steps:
A) cadmium telluride powder body is mixed homogeneously with zinc telluridse powder body, obtain mixed powder;
B) under vacuum, described mixed powder is warming up to 600~750 DEG C, insulation, pressurization, obtain the first sintering Body;
C) described first sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.
According to the present invention, first cadmium telluride powder body is mixed homogeneously with zinc telluridse powder body, obtain mixed powder.
In the present invention, the source no particular restriction of described cadmium telluride powder body and zinc telluridse powder body, for typically commercially available.Institute The granularity stating cadmium telluride powder body is preferably smaller than 100 mesh;The granularity of described zinc telluridse powder body is preferably smaller than 100 mesh.Described cadmium telluride Powder body is preferably 5 with the mass ratio of zinc telluridse powder body:(0.03~0.8), in certain embodiments of the present invention, described mass ratio Can be 5:0.03、5:0.05 or 5:0.8 etc..In the present invention, the mode that cadmium telluride powder body is mixed with zinc telluridse powder body does not have Powder material mix homogeneously can such as can be mixed by particular restriction by modes such as mechanical agitation come mixed material Close powder body.
According to invention, after obtaining mixed powder, under vacuum, described mixed powder is warming up to 600~750 DEG C, insulation, pressurization, obtain the first sintered body.
In the present invention, after obtaining mixed powder, preferably it is evacuated to less than 5Pa, under this vacuum condition, to mixed powder Body heats up, and the speed of described intensification is preferably 3~5 DEG C/min, and in certain embodiments of the present invention, the speed of described intensification 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 design temperature, held for some time, the time of described insulation is preferably 1~2h, more excellent Elect 1.5~2h as, in certain embodiments of the present invention, the time of described insulation can be 1.5h or 2h etc..
In the present invention, preferably after starting to be incubated 10~30min, pressurizeed;Described pressure dwell, temperature keeps not Become;The pressure of described pressurization is preferably 10~20MPa, more preferably 15~17MPa;After being forced into setting value, preferably pressurize one The section time, in the present invention, preferably keep 10~30min, more preferably keep 15~20min.In the present invention, heat-insulation pressure keeping it Afterwards, also include being incubated blood pressure lowering, after described insulation blood pressure lowering, obtain the first sintered body.
According to the present invention, after obtaining the first sintered body, described first sintered body is once lowered the temperature, release, then enter Row reducing temperature twice, obtains cadmium-zinc-teiluride polycrystalline.
In the present invention, described once 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 design temperature, carry out release, preferably laying down residual compression is zero;After release, carry out secondary fall Temperature, described reducing temperature twice is preferably cooled to room temperature, such as can be cooled to less than 35 DEG C, more preferably be down to 25~35 DEG C;Carry out After reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.
According to the present invention, preferably after above-mentioned reducing temperature twice, obtain Cdl-x_Znx_Te;After obtaining Cdl-x_Znx_Te, Preferably under vacuum, described Cdl-x_Znx_Te is warming up to 600~750 DEG C, insulation, pressurization, obtain the second sintered body.
The present invention, after obtaining Cdl-x_Znx_Te, preferably also includes for described Cdl-x_Znx_Te being crushed to granularity less than 100 Mesh, obtains cadmium-zinc-teiluride powder body.
In the present invention, after obtaining cadmium-zinc-teiluride powder body, preferably it is evacuated to less than 5Pa, under this vacuum condition, after carrying out Continuous step;In the present invention, under described vacuum condition, preferably described cadmium-zinc-teiluride powder body is warming up to 600~750 DEG C, more preferably For 680~750 DEG C;The speed of described intensification is preferably 5~12 DEG C/min, in certain embodiments of the present invention, described intensification Speed can be 10 DEG C/min.
In the present invention, after being warming up to described design temperature, held for some time;The time of described insulation is preferably 3~5h.
In the present invention, preferably after starting to be incubated 10~30min, pressurizeed;Described pressure dwell, temperature keeps not Become;The pressure of described pressurization is preferably 25~35MPa, more preferably 25~30MPa;After being forced into setting value, preferably pressurize one The section time, in the present invention, preferably keep 30~50min, more preferably keep 40~50min.In the present invention, heat-insulation pressure keeping it Afterwards, also include being incubated blood pressure lowering, after described insulation blood pressure lowering, obtain the second sintered body.
In the present invention, after obtaining the second sintered body, described second sintered body is once lowered the temperature, release, then carry out Reducing temperature twice, obtains cadmium-zinc-teiluride polycrystalline.
In the present invention, described once 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 design temperature, carry out release, preferably laying down residual compression is zero;After release, carry out secondary fall Temperature, described reducing temperature twice is preferably cooled to room temperature, such as can be cooled to less than 35 DEG C, more preferably be down to 25~35 DEG C;Carry out After reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.Using the method for the present invention, carry out double sintering, be conducive to preferably promoting tellurium zinc Cadmium crystal growth so as to get the uniform segregation-free of cadmium-zinc-teiluride polycrystalline, quality is higher.
In the present invention, after obtaining cadmium-zinc-teiluride polycrystalline, described cadmium-zinc-teiluride polycrystalline can be surface-treated, it is right such as can to pass through The surface of described cadmium-zinc-teiluride polycrystalline carries out the mode of polishing etc., to purify described cadmium-zinc-teiluride polycrystalline.After surface treatment, can be according to need Ask and described 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, preferably mixed powder raw material is loaded in material container and is placed in agglomerating plant carrying out above-mentioned sintering Process;In certain embodiments of the present invention, described material container can be hot pressing graphite grinding tool;Described agglomerating plant can be Hot pressing furnace.
The invention provides a kind of preparation method of cadmium-zinc-teiluride polycrystalline, comprise the following steps:A) by cadmium telluride powder body and tellurium Change zinc powder body mix homogeneously, obtain mixed powder;B) under vacuum, described mixed powder is warming up to 600~750 DEG C, Insulation, pressurization, obtain the first sintered body;C) described first sintered body is once lowered the temperature, release, then carry out reducing temperature twice, Obtain cadmium-zinc-teiluride polycrystalline.Using the ad hoc approach of the present invention, cadmium-zinc-teiluride polycrystalline, safety can be prepared at a lower temperature Easily-controllable, save energy consumption, advantageously reduce cost, and the cadmium-zinc-teiluride polycrystalline quality obtaining is high, segregation-free, using the present processes Be conducive to carrying out high-volume commercial production.
For a further understanding of the present invention, with reference to embodiment, the preferred embodiment of the invention is described, but It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention Limit.
Embodiment 1
The zinc telluridse powder body that the cadmium telluride powder body that 5kg granularity is less than 100 mesh is less than 100 mesh with 0.03Kg granularity mixes all Even, obtain mixed powder;This mixed powder is loaded in hot pressing graphite jig and is placed in hot pressing furnace;Hot pressing furnace is evacuated to Less than 5Pa, with the heating rate of 3 DEG C/min, hot pressing furnace is warming up to 680 DEG C, is incubated 1.5h;Start 10min in above-mentioned insulation Afterwards, pressurizeed, added to 17MPa, after keeping 20min, start to be incubated blood pressure lowering, after insulation reaches 1.5h, start to lower the temperature, drop to When 550 DEG C, it is zero that residual compression is laid down, and is cooled to 25~35 DEG C afterwards, takes out hot pressing graphite jig the demoulding, obtains tellurium zinc Cadmium material.Gained Cdl-x_Znx_Te is crushed to granularity and is less than 100 mesh, load in hot pressing graphite jig and be placed in hot pressing furnace; Hot pressing furnace is evacuated to less than 5Pa, with the heating rate of 10 DEG C/min, hot pressing furnace is warming up to 680 DEG C, be incubated 3h;Above-mentioned After insulation starts 10min, pressurizeed, added to 30MPa, after keeping 40min, start to be incubated blood pressure lowering, reach 3h in insulation total duration Afterwards, start to lower the temperature, when dropping to 550 DEG C, it is zero that residual compression is laid down, and is cooled to 25~35 DEG C afterwards, takes out hot pressing graphite mo(u)ld Tool the demoulding, obtain cadmium-zinc-teiluride polycrystalline.
Using ICP method, segregation detection is carried out to gained cadmium-zinc-teiluride polycrystalline, divided using the analysis method of original position statistical distribution In analysis polycrystal, whether the constituent content of diverse location point is uniform;Gained cadmium-zinc-teiluride polycrystalline is taken with the point of more than 4 diverse locations, The mass ratio of analysis position Zn element simultaneously compares, and result shows, the Zn constituent content of diverse location point is very close, respectively The mass deviation of location point Zn element is less than 0.25%, and that is, gained cadmium-zinc-teiluride polycrystalline is visibly homogeneous, segregation-free.
Embodiment 2
The zinc telluridse powder body that the cadmium telluride powder body that 5kg granularity is less than 100 mesh is less than 100 mesh with 0.8Kg granularity mixes all Even, obtain mixed powder;This mixed powder is loaded in hot pressing graphite jig and is placed in hot pressing furnace;Hot pressing furnace is evacuated to Less than 5Pa, with the heating rate of 5 DEG C/min, hot pressing furnace is warming up to 750 DEG C, is incubated 2h;After above-mentioned insulation starts 10min, Pressurizeed, added to 15MPa, after keeping 20min, start to be incubated blood pressure lowering, after insulation reaches 2h, start to lower the temperature, drop to 550 DEG C When, it is zero that residual compression is laid down, and is cooled to 25~35 DEG C afterwards, takes out hot pressing graphite jig the demoulding, obtains cadmium-zinc-teiluride material Material.Gained Cdl-x_Znx_Te is crushed to granularity and is less than 100 mesh, load in hot pressing graphite jig and be placed in hot pressing furnace;By heat Hot pressing furnace, to less than 5Pa, is warming up to 750 DEG C with the heating rate of 10 DEG C/min by pressure stove evacuation, is incubated 5h;In above-mentioned insulation After starting 10min, pressurizeed, added to 28MPa, after keeping 50min, start to be incubated blood pressure lowering, after insulation total duration reaches 5h, opened Begin to lower the temperature, when dropping to 550 DEG C, it is zero that residual compression is laid down, and is cooled to 25~35 DEG C afterwards, take out hot pressing graphite jig and simultaneously take off Mould, obtains cadmium-zinc-teiluride polycrystalline.
Method according to embodiment 1 carries out segregation detection to gained cadmium-zinc-teiluride polycrystalline, and result shows, the Zn of diverse location point Constituent content is very close, and the mass deviation of each position point Zn element is less than 0.04%, and that is, gained cadmium-zinc-teiluride polycrystalline is visibly homogeneous, Segregation-free.
Embodiment 3
The zinc telluridse powder body that the cadmium telluride powder body that 5kg granularity is less than 100 mesh is less than 100 mesh with 0.05Kg granularity mixes all Even, obtain mixed powder;This mixed powder is loaded in hot pressing graphite jig and is placed in hot pressing furnace;Hot pressing furnace is evacuated to Less than 5Pa, with the heating rate of 5 DEG C/min, hot pressing furnace is warming up to 700 DEG C, is incubated 1.5h;Start 10min in above-mentioned insulation Afterwards, pressurizeed, added to 15MPa, after keeping 15min, start to be incubated blood pressure lowering, after insulation reaches 1.5h, start to lower the temperature, drop to When 550 DEG C, it is zero that residual compression is laid down, and is cooled to 25~35 DEG C afterwards, takes out hot pressing graphite jig the demoulding, obtains tellurium zinc Cadmium material.Gained Cdl-x_Znx_Te is crushed to granularity and is less than 100 mesh, load in hot pressing graphite jig and be placed in hot pressing furnace; Hot pressing furnace is evacuated to less than 5Pa, with the heating rate of 10 DEG C/min, hot pressing furnace is warming up to 700 DEG C, be incubated 4h;Above-mentioned After insulation starts 10min, pressurizeed, added to 25MPa, after keeping 40min, start to be incubated blood pressure lowering, reach 4h in insulation total duration Afterwards, start to lower the temperature, when dropping to 550 DEG C, it is zero that residual compression is laid down, and is cooled to 25~35 DEG C afterwards, takes out hot pressing graphite mo(u)ld Tool the demoulding, obtain cadmium-zinc-teiluride polycrystalline.
Method according to embodiment 1 carries out segregation detection to gained cadmium-zinc-teiluride polycrystalline, and result shows, the Zn of diverse location point Constituent content is very close, and the mass deviation of each position point Zn element is less than 0.29%, and that is, gained cadmium-zinc-teiluride polycrystalline is visibly homogeneous, Segregation-free.
The method that in prior art, preparation cadmium-zinc-teiluride polycrystalline mainly adopts is by tellurium, zinc, the mixing of cadmium simple substance, carries out synthesis anti- Should, and this synthetic reaction needs (usually 1092~1295 DEG C) under the high temperature conditions to carry out meeting the need of crystal growth Ask, this synthetic method easily causes raw material utensil and bursts, both dangerous, also wastes raw material, relatively costly, single can only be carried out It is difficult to carry out the preparation of kilogram magnitude, meanwhile, this high-temperature nuclei method stability is poor, not easily-controllable, easy shadow for a small amount of synthesis Ring the growth quality of crystal, in the cadmium-zinc-teiluride polycrystalline obtaining, easily cause segregation it is difficult to be produced in enormous quantities.Compared to existing Technology, according to the method for the present invention, can prepare cadmium-zinc-teiluride polycrystalline, safety is easily-controllable, saves energy consumption at a lower temperature, Advantageously reduce cost, and the cadmium-zinc-teiluride polycrystalline quality obtaining is high, segregation-free, and single can be realized and synthesize in a large number, adopt The present processes are conducive to carrying out high-volume commercial production.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.To these embodiments Multiple modifications will be apparent from for those skilled in the art, generic principles defined herein is permissible Without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will not be limited In the embodiments shown herein, and it is to fit to the wide model consistent with principles disclosed herein and features of novelty Enclose.

Claims (10)

1. a kind of preparation method of cadmium-zinc-teiluride polycrystalline is it is characterised in that comprise the following steps:
A) cadmium telluride powder body is mixed homogeneously with zinc telluridse powder body, obtain mixed powder;
B) under vacuum, described mixed powder is warming up to 600~750 DEG C, insulation, pressurization, obtain the first sintered body;
C) described first sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.
2. preparation method according to claim 1 is it is characterised in that described cadmium telluride powder body and described zinc telluridse powder body Mass ratio is 5:(0.03~0.8).
3. preparation method according to claim 1 is it is characterised in that the granularity of described cadmium telluride powder body is less than 100 mesh;Institute The granularity stating zinc telluridse powder body is less than 100 mesh.
4. preparation method according to claim 1 is it is characterised in that described step B) in, the vacuum of described vacuum is little In 5Pa, the speed of described intensification is 3~5 DEG C/min, and the time of described insulation is 1~2h.
5. preparation method according to claim 1 is it is characterised in that described step B) in, starting to be incubated 10~30min After pressurizeed;The pressure of described pressurization is 10~20MPa, and the time is 10~30min;Carry out insulation fall after described pressurization Pressure.
6. preparation method according to claim 1 is it is characterised in that described step C) in, described once lower the temperature as cooling To 530~560 DEG C.
7. preparation method according to claim 1 is it is characterised in that described step C) specifically include:
C1) described first sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain Cdl-x_Znx_Te;
C2) under vacuum, described Cdl-x_Znx_Te is warming up to 600~750 DEG C, insulation, pressurization, obtain the second sintering Body;
C3) described second sintered body is once lowered the temperature, release, then carry out reducing temperature twice, obtain cadmium-zinc-teiluride polycrystalline.
8. preparation method according to claim 7 is it is characterised in that described step C2) in, the vacuum of described vacuum is little In 5Pa, the speed of described intensification is 5~12 DEG C/min, and the time of described insulation is 3~5h.
9. preparation method according to claim 7 is it is characterised in that described step C2) in, starting to be incubated 10~ Pressurizeed after 30min;The pressure of described pressurization is 25~35MPa, and the time is 30~50min;Protected after described pressurization Temperature drop pressure.
10. preparation method according to claim 7 is it is characterised in that described step C3) in, described once lower the temperature as fall Temperature is to 530~560 DEG C.
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CN113023688A (en) * 2021-04-23 2021-06-25 先导薄膜材料(广东)有限公司 Preparation method of arsenic-doped cadmium telluride
CN113818086A (en) * 2021-09-23 2021-12-21 安徽光智科技有限公司 Growth method of cadmium zinc telluride crystal
CN115726031A (en) * 2022-09-26 2023-03-03 湖南大合新材料有限公司 Method and equipment for synthesizing tellurium-zinc-cadmium polycrystal

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