CN106380198B - Cadmium-zinc-teiluride target, preparation method and application - Google Patents

Cadmium-zinc-teiluride target, preparation method and application Download PDF

Info

Publication number
CN106380198B
CN106380198B CN201610836897.0A CN201610836897A CN106380198B CN 106380198 B CN106380198 B CN 106380198B CN 201610836897 A CN201610836897 A CN 201610836897A CN 106380198 B CN106380198 B CN 106380198B
Authority
CN
China
Prior art keywords
cadmium
zinc
target
powder
teiluride
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.)
Active
Application number
CN201610836897.0A
Other languages
Chinese (zh)
Other versions
CN106380198A (en
Inventor
文崇斌
朱刘
胡智向
曾成亮
余明
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.)
Vital Thin Film Materials Guangdong Co Ltd
Original Assignee
Guangdong Pioneer Precious Metals Material 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 Guangdong Pioneer Precious Metals Material Co Ltd filed Critical Guangdong Pioneer Precious Metals Material Co Ltd
Priority to CN201610836897.0A priority Critical patent/CN106380198B/en
Publication of CN106380198A publication Critical patent/CN106380198A/en
Application granted granted Critical
Publication of CN106380198B publication Critical patent/CN106380198B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/547Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/645Pressure sintering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/446Sulfides, tellurides or selenides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Photovoltaic Devices (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The present invention provides a kind of preparation methods of cadmium-zinc-teiluride target, comprising the following steps: A) cadmium telluride powder, zinc telluridse powder and cuprous telluride powder are uniformly mixed, obtain mixed powder;B the mixed powder) is subjected to vacuum heating-press sintering, obtains cadmium-zinc-teiluride target.Raw material of the present invention using cadmium telluride powder, zinc telluridse powder and cuprous telluride powder as preparation cadmium-zinc-teiluride target, cadmium-zinc-teiluride target is made by vacuum hot-pressing, preparation method is simple, it is easy to industrialization production, the cadmium-zinc-teiluride target consistency as made from this method is higher, better mechanical property.In addition, cadmium-zinc-teiluride target produced by the present invention can be applied in solar film battery.The experimental results showed that the density of cadmium-zinc-teiluride target prepared by the present invention has been more than the 99% of theoretical density, consistency is higher;Meanwhile bending strength is in 12MPa or more.

Description

Cadmium-zinc-teiluride target, preparation method and application
Technical field
The present invention relates to sputtering target material more particularly to a kind of cadmium-zinc-teiluride targets, preparation method and application.
Background technique
With the rapid development of electronics and information industry, membrane science is using increasingly extensive, using film preparation solar-electricity The industry in pond is also more and more prosperous.Sputtering method is to prepare one of major technique of thin-film material, and the source material of sputter-deposited thin films Material is target.
Specifically, target is by magnetron sputtering, multi-arc ion coating or other kinds of coating system in work appropriate The sputtering source that various function films are formed on substrate is sputtered under the conditions of skill.It is found in the developmental research of target, target is different (such as aluminium target, copper target, stainless steel target, titanium target, nickel target), obtained membrane system (such as superhard, wear-resisting, corrosion-resistant alloy film etc.) also if Difference, final solar film battery obtained also will be provided with different characteristics.
Target huge number disclosed in the prior art can be divided into metal targets, alloy target material and ceramics according to composition Compound target.However, the particularity of solar battery makes and not all target is suitable for preparing solar energy film Battery.In disclosed ceramic compound target, suitable for solar film battery and the target of industrialization production may be implemented Material type is simultaneously few, meanwhile, rarely have document to refer to the preparation method of corresponding target, thus, still need continual exploitation have compared with The target and its preparation process of high-compactness and preferable mechanical performance, to expand the industrialization production of target.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of cadmium-zinc-teiluride target, preparation method and answering With cadmium-zinc-teiluride target consistency disclosed by the invention is higher, and better mechanical property can be applied in solar film battery.
The present invention provides a kind of cadmium-zinc-teiluride targets, comprising: cadmium telluride, zinc telluridse and cuprous telluride.
Preferably, the molar ratio of the cadmium telluride and the zinc telluridse is 0.9~1.2:0.8~1.1;
Content of the cuprous telluride in the cadmium-zinc-teiluride target is 250mg/kg~330mg/kg.
The present invention provides a kind of preparation methods of cadmium-zinc-teiluride target, comprising the following steps:
A) cadmium telluride powder, zinc telluridse powder and cuprous telluride powder are uniformly mixed, obtain mixed powder;
B the mixed powder) is subjected to vacuum heating-press sintering, obtains cadmium-zinc-teiluride target.
Preferably, the granularity of the cadmium telluride powder is less than 100 mesh, and the granularity of the zinc telluridse powder is less than 100 mesh, institute The granularity of cuprous telluride powder is stated less than 325 mesh.
Preferably, the molar ratio of the cadmium telluride powder and the zinc telluridse powder is 0.9~1.2:0.8~1.1;It is described Content of the cuprous telluride powder in mixed powder is 250mg/kg~330mg/kg.
Preferably, step B) in, the vacuum heating-press sintering specifically:
It heats under conditions of vacuum, when temperature reaches 500 DEG C~900 DEG C, is kept the temperature.
Preferably, described keep the temperature includes:
After keeping the temperature 10~50min, start heat-insulating pressurizing, then heat preservation decompression.
Preferably, the pressure of the heat-insulating pressurizing is 10MPa~40MPa, time of the heat-insulating pressurizing be 20min~ 40min。
Preferably, after the heat preservation, further includes:
Cooling, decompression, then cools down.
The cadmium-zinc-teiluride target prepared the present invention also provides above-mentioned cadmium-zinc-teiluride target or above-mentioned preparation method is thin in solar energy The application in film battery field.
The present invention provides a kind of cadmium-zinc-teiluride targets, comprising: cadmium telluride, zinc telluridse and cuprous telluride.This target is fine and close Degree is higher, and better mechanical property can be applied in solar film battery.
The present invention also provides a kind of preparation methods of cadmium-zinc-teiluride target, comprising the following steps: A) by cadmium telluride powder, tellurium Change zinc powder body and cuprous telluride powder is uniformly mixed, obtains mixed powder;B the mixed powder) is subjected to vacuum heating-press sintering, Obtain cadmium-zinc-teiluride target.The present invention is using cadmium telluride powder, zinc telluridse powder and cuprous telluride powder as preparation cadmium-zinc-teiluride target Cadmium-zinc-teiluride target is made by vacuum hot-pressing in the raw material of material, and preparation method is simple, is easy to industrialization production, by this Cadmium-zinc-teiluride target consistency made from method is higher, better mechanical property.In addition, cadmium-zinc-teiluride target produced by the present invention can answer For in solar film battery.The experimental results showed that the density of cadmium-zinc-teiluride target prepared by the present invention has been more than theoretical close The 99% of degree, consistency is higher;Meanwhile bending strength is in 12MPa or more.
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 targets, comprising: cadmium telluride, zinc telluridse and cuprous telluride.Include these three groups The target consistency divided is higher, better mechanical property, meanwhile, also there is preferably electric conductivity, can be applied to solar energy film In battery.
In above-mentioned cadmium-zinc-teiluride target, the molar ratio of the cadmium telluride and the zinc telluridse be preferably 0.9~1.2:0.8~ 1.1;More preferably 0.9~1.1:0.8~1.1.Content of the cuprous telluride in the cadmium-zinc-teiluride target be preferably 250mg/kg~330mg/kg;More preferably 270mg/kg~310mg/kg.
The present invention also provides a kind of preparation methods of cadmium-zinc-teiluride target, comprising the following steps:
A) cadmium telluride powder, zinc telluridse powder and cuprous telluride powder are uniformly mixed, obtain mixed powder;
B the mixed powder) is subjected to vacuum heating-press sintering, obtains cadmium-zinc-teiluride target.
Cadmium telluride powder, zinc telluridse powder and cuprous telluride powder are first uniformly mixed by the present invention, obtain mixed powder.This Invention has no special limitation, Ke Yiwei to the source of used cadmium telluride powder, zinc telluridse powder and cuprous telluride powder It is general commercially available.In the present invention, the granularity of the cadmium telluride powder is preferably smaller than 100 mesh;The granularity of the zinc telluridse powder is excellent Choosing is less than 100 mesh;The granularity of the cuprous telluride powder is preferably smaller than 325 mesh.
In the present invention, the molar ratio of the cadmium telluride powder and the zinc telluridse powder be preferably 0.9~1.2:0.8~ 1.1;More preferably 0.9~1.1:0.8~1.1;In certain embodiments of the present invention, the cadmium telluride powder and the telluride The molar ratio of zinc powder body is 1:1,0.9:1.1 or 1.2:0.8.Content of the cuprous telluride powder in the mixed powder is excellent It is selected as 250mg/kg~330mg/kg;More preferably 270mg/kg~310mg/kg;In certain embodiments of the present invention, described Content of the cuprous telluride powder in the mixed powder is 280mg/kg, 290mg/kg or 300mg/kg.
After obtaining mixed powder, the mixed powder is carried out vacuum heating-press sintering by the present invention, obtains cadmium-zinc-teiluride target.It is excellent Choosing, specifically: the mixed powder is packed into mold, vacuum heating-press sintering is carried out, cadmium-zinc-teiluride target is obtained after demoulding.
In the present invention, the mold is preferably graphite jig;The equipment of the vacuum heating-press sintering is preferably Vacuum Heat Press furnace.
The vacuum heating-press sintering is preferred are as follows:
It heats under conditions of vacuum, when temperature reaches 500 DEG C~900 DEG C, is kept the temperature.
The present invention has no special limitation to the vacuum degree of the vacuum, under vacuum condition, the present invention preferably≤ 5Pa.The present invention has no special limitation to the mode of the heating, is using heating method well known to those skilled in the art It can.Present invention preferably employs graphite rod heating.The heating rate of the heating is preferably 2~10 DEG C/min, in certain of the invention In a little embodiments, the heating rate of the heating is 2 DEG C/min, 3 DEG C/min, 5 DEG C/min, 8 DEG C/min, 10 DEG C/min.This hair It is bright that the uniformity of crystal grain in target is improved by the control rate of heat addition, it has been avoided as much as occurring inside target layering now As being more advantageous to the mechanical performance for improving target.
When the temperature of heating reaches sintering temperature, kept the temperature.The sintering temperature is 500 DEG C~900 DEG C, in this hair In bright some embodiments, the sintering temperature is 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C.The present invention is burnt by control Junction temperature is more advantageous to the consistency for improving target, while being avoided as much as possible the case where target fragmentation occurs and falls side, improves The mechanical performance of target.The total time of the heat preservation is preferably 1~3h, in certain embodiments of the present invention, the heat preservation Total time be 1.2h, 1.5h, 1.9h or 2h.
Preferably, the heat preservation specifically: after 10~50min of heat preservation, start heat-insulating pressurizing, then heat preservation decompression.It is more excellent It is selected as: after 20~30min of heat preservation, starting heat-insulating pressurizing, then heat preservation decompression.
The pressure of the heat-insulating pressurizing is preferably 10MPa~40MPa, more preferably 25MPa~35MPa;The heat preservation adds The time of pressure is preferably 20min~40min, more preferably 35min~40min.
After the heat-insulating pressurizing, heat preservation decompression is carried out.Preferably, specifically: after the heat-insulating pressurizing, lay down the heat preservation The pressure of pressurization carries out nature decompression under conditions of heat preservation.
After above-mentioned heat preservation, it is also preferable to include following steps:
Cooling, decompression, then cools down.
The cooling preferably cools down under conditions of being depressured naturally.The present invention to the rate of temperature fall of the cooling simultaneously Without special limitation, the preferred natural cooling of the present invention.The temperature of the cooling is preferably dropped to 400 DEG C~600 DEG C, is more preferably down to 500 DEG C~600 DEG C, in certain embodiments of the present invention, the temperature of the cooling is down to 400 DEG C, 500 DEG C, 550 DEG C or 600 ℃。
After the cooling, depressurized.Pressure after the decompression is preferably 3MPa~15MPa, and more preferably 12MPa~ 15MPa。
After the decompression, cooled down.After the cooling, it is also preferable to include demouldings, and then obtain cadmium-zinc-teiluride target.This hair The bright mode to the cooling has no special limitation, and the present invention is preferably natural cooling.The temperature of the cooling is preferably 35 DEG C hereinafter, more preferably 25~35 DEG C.
The present invention provides a kind of preparation methods of cadmium-zinc-teiluride target, comprising the following steps: A) by cadmium telluride powder, telluride Zinc powder body and cuprous telluride powder are uniformly mixed, and obtain mixed powder;B the mixed powder) is subjected to vacuum heating-press sintering, is obtained To cadmium-zinc-teiluride target.The present invention is using cadmium telluride powder, zinc telluridse powder and cuprous telluride powder as preparation cadmium-zinc-teiluride target Raw material, cadmium-zinc-teiluride target is made by vacuum hot-pressing, preparation method is simple, is easy to industrialization production, by this side Cadmium-zinc-teiluride target consistency made from method is higher, better mechanical property.The present invention passes through the processing step to vacuum heating-press sintering And Parameter Conditions further limit, and are more advantageous to cadmium-zinc-teiluride target obtained and obtain higher consistency and preferably mechanicalness Energy.Meanwhile processing step disclosed by the invention is simple, and process conditions more mitigate, and it is lower to equipment requirement, it is more advantageous to industry Metaplasia produces.The experimental results showed that the density of cadmium-zinc-teiluride target prepared by the present invention has been more than the 99% of theoretical density, consistency It is higher;Meanwhile bending strength is in 12MPa or more.
The cadmium-zinc-teiluride target prepared the present invention also provides above-mentioned cadmium-zinc-teiluride target or above-mentioned preparation method is thin in solar energy The application in film battery field.The applicant can apply the study found that cadmium-zinc-teiluride target electric conductivity prepared by the present invention is preferable In solar film battery, and higher transfer efficiency can be obtained.Thus, above-mentioned cadmium-zinc-teiluride target or above-mentioned preparation is claimed Application of the cadmium-zinc-teiluride target of method preparation in solar film battery field.
In order to further illustrate the present invention, with reference to embodiments to a kind of cadmium-zinc-teiluride target provided by the invention, its system Preparation Method and application are described in detail, but cannot be understood as limiting the scope of the present invention.
Embodiment 1
By granularity less than the cadmium telluride powders of 100 mesh, granularity less than 100 mesh zinc telluridse powder and granularity less than 325 Purpose cuprous telluride powder is uniformly mixed, and obtains mixed powder.The molar ratio of the cadmium telluride powder and the zinc telluridse powder For 1:1, content of the cuprous telluride powder in the mixed powder is 300mg/kg.
Mixed powder is packed into graphite jig, is placed in vacuum hotpressing stove.Vacuum hotpressing stove is vacuumized, vacuum is worked as It when degree reaches 5Pa, begins to warm up, the rate of the heating is that 5 DEG C/min is kept the temperature when temperature reaches 700 DEG C.It is described The total time of heat preservation is 1.5h.The specific steps of the heat preservation are as follows: after heat preservation 20min, start heat-insulating pressurizing, then heat preservation drop Pressure;The pressure of the heat-insulating pressurizing is 30MPa, and the time of the heat-insulating pressurizing is 40min;After the heat-insulating pressurizing, institute is laid down The pressure for stating heat-insulating pressurizing carries out nature decompression under conditions of heat preservation.Then, cool down under conditions of being depressured naturally, After temperature is down to 600 DEG C, start to depressurize, after pressure is down to 12MPa, naturally cools to 25~35 DEG C.Open fire door, demoulding Afterwards, cadmium-zinc-teiluride target is obtained.
The detection that obtained cadmium-zinc-teiluride target is carried out to consistency, specifically, the cadmium-zinc-teiluride target measured using drainage The density of material, the experimental results showed that, the density for the cadmium-zinc-teiluride target that the present embodiment obtains is the 99.1% of theoretical density, consistency It is higher.
According to GB/T 14452-93 " metal bending mechanical test method " standard, to the cadmium-zinc-teiluride target of above-mentioned acquisition The detection of material progress bending strength.Wherein, specimen size b*h*L (mm)=10*20*100, the experimental results showed that, the present embodiment The bending strength of obtained cadmium-zinc-teiluride target is 12.5MPa.
Embodiment 2
By granularity less than the cadmium telluride powders of 100 mesh, granularity less than 100 mesh zinc telluridse powder and granularity less than 325 Purpose cuprous telluride powder is uniformly mixed, and obtains mixed powder.The molar ratio of the cadmium telluride powder and the zinc telluridse powder For 1:1, content of the cuprous telluride powder in the mixed powder is 300mg/kg.
Mixed powder is packed into graphite jig, is placed in vacuum hotpressing stove.Vacuum hotpressing stove is vacuumized, vacuum is worked as It when degree reaches 5Pa, begins to warm up, the rate of the heating is that 10 DEG C/min is kept the temperature when temperature reaches 800 DEG C.It is described The total time of heat preservation is 2h.The specific steps of the heat preservation are as follows: after heat preservation 25min, start heat-insulating pressurizing, then heat preservation decompression; The pressure of the heat-insulating pressurizing is 25MPa, and the time of the heat-insulating pressurizing is 40min;After the heat-insulating pressurizing, the guarantor is laid down The pressure of temperature pressurization carries out nature decompression under conditions of heat preservation.Then, cool down under conditions of being depressured naturally, work as temperature After degree is down to 500 DEG C, starts to depressurize, after pressure is down to 12MPa, naturally cool to 25~35 DEG C.Fire door is opened, after demoulding, is obtained To cadmium-zinc-teiluride target.
The detection that obtained cadmium-zinc-teiluride target is carried out to consistency, specifically, the cadmium-zinc-teiluride target measured using drainage The density of material, the experimental results showed that, the density for the cadmium-zinc-teiluride target that the present embodiment obtains is the 99.3% of theoretical density, consistency It is higher.
According to GB/T 14452-93 " metal bending mechanical test method " standard, to the cadmium-zinc-teiluride target of above-mentioned acquisition The detection of material progress bending strength.Wherein, specimen size b*h*L (mm)=10*20*100, the experimental results showed that, the present embodiment The bending strength of obtained cadmium-zinc-teiluride target is 12.3MPa.
Embodiment 3
By granularity less than the cadmium telluride powders of 100 mesh, granularity less than 100 mesh zinc telluridse powder and granularity less than 325 Purpose cuprous telluride powder is uniformly mixed, and obtains mixed powder.The molar ratio of the cadmium telluride powder and the zinc telluridse powder For 1:1, content of the cuprous telluride powder in the mixed powder is 300mg/kg.
Mixed powder is packed into graphite jig, is placed in vacuum hotpressing stove.Vacuum hotpressing stove is vacuumized, vacuum is worked as It when degree reaches 5Pa, begins to warm up, the rate of the heating is that 8 DEG C/min is kept the temperature when temperature reaches 900 DEG C.It is described The total time of heat preservation is 1.2h.The specific steps of the heat preservation are as follows: after heat preservation 30min, start heat-insulating pressurizing, then heat preservation drop Pressure;The pressure of the heat-insulating pressurizing is 35MPa, and the time of the heat-insulating pressurizing is 35min;After the heat-insulating pressurizing, institute is laid down The pressure for stating heat-insulating pressurizing carries out nature decompression under conditions of heat preservation.Then, cool down under conditions of being depressured naturally, After temperature is down to 600 DEG C, start to depressurize, after pressure is down to 15MPa, naturally cools to 25~35 DEG C.Open fire door, demoulding Afterwards, cadmium-zinc-teiluride target is obtained.
The detection that obtained cadmium-zinc-teiluride target is carried out to consistency, specifically, the cadmium-zinc-teiluride target measured using drainage The density of material, the experimental results showed that, the density for the cadmium-zinc-teiluride target that the present embodiment obtains is the 99.2% of theoretical density, consistency It is higher.
According to GB/T 14452-93 " metal bending mechanical test method " standard, to the cadmium-zinc-teiluride target of above-mentioned acquisition The detection of material progress bending strength.Wherein, specimen size b*h*L (mm)=10*20*100, the experimental results showed that, the present embodiment The bending strength of obtained cadmium-zinc-teiluride target is 12.2MPa.
Embodiment 4
By granularity less than the cadmium telluride powders of 100 mesh, granularity less than 100 mesh zinc telluridse powder and granularity less than 325 Purpose cuprous telluride powder is uniformly mixed, and obtains mixed powder.The molar ratio of the cadmium telluride powder and the zinc telluridse powder For 0.9:1.1, content of the cuprous telluride powder in the mixed powder is 280mg/kg.
Mixed powder is packed into graphite jig, is placed in vacuum hotpressing stove.Vacuum hotpressing stove is vacuumized, vacuum is worked as It when degree reaches 4Pa, begins to warm up, the rate of the heating is that 2 DEG C/min is kept the temperature when temperature reaches 600 DEG C.It is described The total time of heat preservation is 1.9h.The specific steps of the heat preservation are as follows: after heat preservation 30min, start heat-insulating pressurizing, then heat preservation drop Pressure;The pressure of the heat-insulating pressurizing is 30MPa, and the time of the heat-insulating pressurizing is 35min;After the heat-insulating pressurizing, institute is laid down The pressure for stating heat-insulating pressurizing carries out nature decompression under conditions of heat preservation.Then, cool down under conditions of being depressured naturally, After temperature is down to 550 DEG C, start to depressurize, after pressure is down to 12MPa, naturally cools to 25~35 DEG C.Open fire door, demoulding Afterwards, cadmium-zinc-teiluride target is obtained.
The detection that obtained cadmium-zinc-teiluride target is carried out to consistency, specifically, the cadmium-zinc-teiluride target measured using drainage The density of material, the experimental results showed that, the density for the cadmium-zinc-teiluride target that the present embodiment obtains is the 99.3% of theoretical density, consistency It is higher.
According to GB/T 14452-93 " metal bending mechanical test method " standard, to the cadmium-zinc-teiluride target of above-mentioned acquisition The detection of material progress bending strength.Wherein, specimen size b*h*L (mm)=10*20*100, the experimental results showed that, the present embodiment The bending strength of obtained cadmium-zinc-teiluride target is 12.3MPa.
Embodiment 5
By granularity less than the cadmium telluride powders of 100 mesh, granularity less than 100 mesh zinc telluridse powder and granularity less than 325 Purpose cuprous telluride powder is uniformly mixed, and obtains mixed powder.The molar ratio of the cadmium telluride powder and the zinc telluridse powder For 1.2:0.8, content of the cuprous telluride powder in the mixed powder is 290mg/kg.
Mixed powder is packed into graphite jig, is placed in vacuum hotpressing stove.Vacuum hotpressing stove is vacuumized, vacuum is worked as It when degree reaches 3Pa, begins to warm up, the rate of the heating is that 3 DEG C/min is kept the temperature when temperature reaches 500 DEG C.It is described The total time of heat preservation is 2h.The specific steps of the heat preservation are as follows: after heat preservation 25min, start heat-insulating pressurizing, then heat preservation decompression; The pressure of the heat-insulating pressurizing is 35MPa, and the time of the heat-insulating pressurizing is 25min;After the heat-insulating pressurizing, the guarantor is laid down The pressure of temperature pressurization carries out nature decompression under conditions of heat preservation.Then, cool down under conditions of being depressured naturally, work as temperature After degree is down to 400 DEG C, starts to depressurize, after pressure is down to 12MPa, naturally cool to 25~35 DEG C.Fire door is opened, after demoulding, is obtained To cadmium-zinc-teiluride target.
The detection that obtained cadmium-zinc-teiluride target is carried out to consistency, specifically, the cadmium-zinc-teiluride target measured using drainage The density of material, the experimental results showed that, the density for the cadmium-zinc-teiluride target that the present embodiment obtains is the 99.1% of theoretical density, consistency It is higher.
According to GB/T 14452-93 " metal bending mechanical test method " standard, to the cadmium-zinc-teiluride target of above-mentioned acquisition The detection of material progress bending strength.Wherein, specimen size b*h*L (mm)=10*20*100, the experimental results showed that, the present embodiment The bending strength of obtained cadmium-zinc-teiluride target is 12.1MPa.
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 (6)

1. a kind of cadmium-zinc-teiluride target, which is characterized in that be made of cadmium telluride, zinc telluridse and cuprous telluride;
The cadmium-zinc-teiluride target is prepared in accordance with the following methods:
A) cadmium telluride powder, zinc telluridse powder and cuprous telluride powder are uniformly mixed, obtain mixed powder;
B the mixed powder) is subjected to vacuum heating-press sintering, obtains cadmium-zinc-teiluride target;
The vacuum heating-press sintering specifically:
It heats under conditions of vacuum, when temperature reaches 500 DEG C~900 DEG C, is kept the temperature;The total time of the heat preservation be 1~ 3h;
The heating rate of the heating is 2~10 DEG C/min;
The heat preservation includes:
After keeping the temperature 10~50min, starts heat-insulating pressurizing, then lay down the pressure of the heat-insulating pressurizing, under conditions of heat preservation, into Row is depressured naturally;
The pressure of the heat-insulating pressurizing is 10MPa~40MPa, and the time of the heat-insulating pressurizing is 20min~40min;
After the heat preservation, further includes:
400 DEG C~600 DEG C are cooled under conditions of being depressured naturally, then is decompressed to 3MPa~15MPa, is then cooled down.
2. cadmium-zinc-teiluride target according to claim 1, which is characterized in that
The molar ratio of the cadmium telluride and the zinc telluridse is 0.9~1.2:0.8~1.1;
Content of the cuprous telluride in the cadmium-zinc-teiluride target is 250mg/kg~330mg/kg.
3. a kind of preparation method of cadmium-zinc-teiluride target, which comprises the following steps:
A) cadmium telluride powder, zinc telluridse powder and cuprous telluride powder are uniformly mixed, obtain mixed powder;
B the mixed powder) is subjected to vacuum heating-press sintering, obtains cadmium-zinc-teiluride target;
The vacuum heating-press sintering specifically:
It heats under conditions of vacuum, when temperature reaches 500 DEG C~900 DEG C, is kept the temperature;The total time of the heat preservation be 1~ 3h;
The heating rate of the heating is 2~10 DEG C/min;
The heat preservation includes:
After keeping the temperature 10~50min, starts heat-insulating pressurizing, then lay down the pressure of the heat-insulating pressurizing, under conditions of heat preservation, into Row is depressured naturally;
The pressure of the heat-insulating pressurizing is 10MPa~40MPa, and the time of the heat-insulating pressurizing is 20min~40min;
After the heat preservation, further includes:
400 DEG C~600 DEG C are cooled under conditions of being depressured naturally, then is decompressed to 3MPa~15MPa, is then cooled down.
4. preparation method according to claim 3, 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, the granularity of the cuprous telluride powder is less than 325 mesh.
5. preparation method according to claim 3, which is characterized in that
The molar ratio of the cadmium telluride powder and the zinc telluridse powder is 0.9~1.2:0.8~1.1;
Content of the cuprous telluride powder in mixed powder is 250mg/kg~330mg/kg.
6. preparation side described in cadmium-zinc-teiluride target or claim 3~5 any one described in claim 1~2 any one Application of the cadmium-zinc-teiluride target of method preparation in solar film battery field.
CN201610836897.0A 2016-09-20 2016-09-20 Cadmium-zinc-teiluride target, preparation method and application Active CN106380198B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610836897.0A CN106380198B (en) 2016-09-20 2016-09-20 Cadmium-zinc-teiluride target, preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610836897.0A CN106380198B (en) 2016-09-20 2016-09-20 Cadmium-zinc-teiluride target, preparation method and application

Publications (2)

Publication Number Publication Date
CN106380198A CN106380198A (en) 2017-02-08
CN106380198B true CN106380198B (en) 2019-01-29

Family

ID=57936671

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610836897.0A Active CN106380198B (en) 2016-09-20 2016-09-20 Cadmium-zinc-teiluride target, preparation method and application

Country Status (1)

Country Link
CN (1) CN106380198B (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108179387A (en) * 2017-12-28 2018-06-19 清远先导材料有限公司 A kind of preparation method of copper indium gallium selenide base system row target
CN109704766A (en) * 2019-01-21 2019-05-03 江西科泰新材料有限公司 Zinc telluridse mixes the production technology of cuprous telluride target
CN111647857A (en) * 2020-05-27 2020-09-11 先导薄膜材料(广东)有限公司 Method for recycling residual target of cadmium telluride thin film battery
CN113121232A (en) * 2021-04-23 2021-07-16 先导薄膜材料(广东)有限公司 Preparation method of conductive zinc telluride target
CN113233870B (en) * 2021-04-25 2023-01-13 先导薄膜材料(广东)有限公司 Cadmium oxide-doped target material and preparation method and application thereof
CN113372117B (en) * 2021-06-11 2023-03-10 先导薄膜材料有限公司 Preparation method of zinc telluride copper-doped target material
CN113336549B (en) * 2021-06-15 2023-10-10 先导薄膜材料(广东)有限公司 Tellurium-selenium-cadmium target material and preparation method thereof
CN113526955A (en) * 2021-07-30 2021-10-22 广东先导稀材股份有限公司 Preparation method of cadmium zinc telluride target

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201780976U (en) * 2010-07-29 2011-03-30 比亚迪股份有限公司 CdTe (cadmium telluride) solar cell
CN102492927A (en) * 2011-12-08 2012-06-13 上海太阳能电池研究与发展中心 Method for preparing tellurium-zinc-cadmium film material with adjustable forbidden bandwidth
CN103911666A (en) * 2013-01-08 2014-07-09 广东先导稀材股份有限公司 Tellurium zinc cadmium polycrystal synthesis tool and tellurium zinc cadmium polycrystal synthesis method
CN104357902A (en) * 2014-10-16 2015-02-18 中国科学院上海技术物理研究所 Synthesizing device and method for synthesizing Cd(1-x)ZnxTe polycrystal by utilizing temperature gradient
CN104694889A (en) * 2013-12-10 2015-06-10 北京有色金属研究总院 Preparation method of CdTe sputtering target material

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090053453A1 (en) * 2005-12-21 2009-02-26 Durham Scientific Crystals Limited Semiconductor device and method of manufacture thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201780976U (en) * 2010-07-29 2011-03-30 比亚迪股份有限公司 CdTe (cadmium telluride) solar cell
CN102492927A (en) * 2011-12-08 2012-06-13 上海太阳能电池研究与发展中心 Method for preparing tellurium-zinc-cadmium film material with adjustable forbidden bandwidth
CN103911666A (en) * 2013-01-08 2014-07-09 广东先导稀材股份有限公司 Tellurium zinc cadmium polycrystal synthesis tool and tellurium zinc cadmium polycrystal synthesis method
CN104694889A (en) * 2013-12-10 2015-06-10 北京有色金属研究总院 Preparation method of CdTe sputtering target material
CN104357902A (en) * 2014-10-16 2015-02-18 中国科学院上海技术物理研究所 Synthesizing device and method for synthesizing Cd(1-x)ZnxTe polycrystal by utilizing temperature gradient

Also Published As

Publication number Publication date
CN106380198A (en) 2017-02-08

Similar Documents

Publication Publication Date Title
CN106380198B (en) Cadmium-zinc-teiluride target, preparation method and application
CN110698205B (en) Preparation method of graphene-toughened silicon carbide ceramic
CN107620049B (en) A kind of preparation method of soap-free emulsion polymeization phase pure WC target
CN109180187B (en) Preparation method of highly oriented nanometer MAX phase ceramic and MAX phase in-situ authigenic oxide nanometer complex phase ceramic
CN110127633A (en) A kind of cadmium telluride target and preparation method thereof
CN105562694A (en) Hot isostatic pressing three-control method suitable for additive manufacturing parts
CN104894516A (en) Method for efficiently preparing ternary laminar MAX phase ceramic coating layer at low temperature
CN110128143A (en) A kind of cadmium selenide target and preparation method thereof
CN107603571B (en) Preparation of shaped expanded graphite-based erythritol intermediate-temperature composite phase-change heat storage material
CN103264542A (en) Titanium aluminum-ceramic layered material and preparation method thereof
CN107586987B (en) Titanium carbide-titanium diboride two-phase enhancing Cu-base composites and preparation method thereof
CN102424918A (en) Method for preparing MoCu gradient material by combining molybdenum powder grading and infiltration
CN102699325A (en) Preparing method for Ti-Si alloy target materials
CN109824382A (en) A kind of heat management SiC/ graphite film laminar composite and preparation method thereof
CN111393170A (en) Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic
CN106587940A (en) High-purity compact magnesium oxide target material and preparation method thereof
CN106521631A (en) Preparation method of polycrystal zinc sulfide
CN109234691A (en) A kind of high thermal conductivity graphite film-metallic composite and preparation method thereof
CN102485378B (en) Preparation method of ruthenium metal sputtering target material
CN110791693B (en) High-entropy alloy with low Al content, high strength and toughness and acid corrosion resistance and preparation method thereof
CN107746280A (en) A kind of high-compactness TiB2The preparation method of ceramic target
CN104003728B (en) A kind of pressureless sintering prepares Ti2The method of SC ceramics
CN106278264A (en) A kind of high density chromic lanthanum ceramics heater manufacture method
CN107445625B (en) High-density ZrB2Method for producing ceramic
CN109503169A (en) A kind of special graphite and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information

Inventor after: Wen Chongbin

Inventor after: Zhu Liu

Inventor after: Hu Zhixiang

Inventor after: Zeng Chengliang

Inventor after: Yu Ming

Inventor before: Wen Chongbin

Inventor before: Zhu Liu

Inventor before: Hu Zhixiang

Inventor before: Zeng Chengliang

Inventor before: Yu Ming

Inventor before: Li Qinxiang

CB03 Change of inventor or designer information
TA01 Transfer of patent application right

Effective date of registration: 20181122

Address after: 511500 Tellurium Chemical Workshop of Guangdong Pioneer Rare Materials Co., Ltd., Heyun Town, Qingxin District, Qingyuan City, Guangdong Province

Applicant after: Guangdong Pioneer Precious Metals Material Co., Ltd.

Address before: 511500 Industrial Zone, wo Yun town, Qingxin County, Qingyuan, Guangdong (beside the fish dam road)

Applicant before: Guangdong Vital Rare Material Co., Ltd.

TA01 Transfer of patent application right
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20210610

Address after: 511500 area a, no.27-9 Baijia Industrial Park, high tech Zone, Qingyuan City, Guangdong Province

Patentee after: Leading film materials (Guangdong) Co.,Ltd.

Address before: 511500 Tellurium Chemical Workshop of Guangdong Pioneer Rare Materials Co., Ltd., Heyun Town, Qingxin District, Qingyuan City, Guangdong Province

Patentee before: Guangdong Pioneer Precious Metals Material Co.,Ltd.

TR01 Transfer of patent right