CN104388901B - Cobalt-antimonide-base thermoelectric film and preparation method thereof - Google Patents

Cobalt-antimonide-base thermoelectric film and preparation method thereof Download PDF

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Publication number
CN104388901B
CN104388901B CN201410626851.7A CN201410626851A CN104388901B CN 104388901 B CN104388901 B CN 104388901B CN 201410626851 A CN201410626851 A CN 201410626851A CN 104388901 B CN104388901 B CN 104388901B
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preparation
thermal electric
antimony cobalt
sputtering
doping
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CN104388901A (en
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范平
郑壮豪
梁广兴
张银
范卫芳
罗景庭
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Shenzhen University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

Abstract

The invention discloses a cobalt-antimonide-base thermoelectric film and a preparation method thereof. The preparation method comprises the following steps: by using a cobalt antimonide target as a sputtering target, and separately making a material to be doped into a doping target; fixing the sputtering target and doping target to a rotating target rack of a multi-station sputtering system for later sputtering; and plating a cobalt antimonide film on an insulating substrate by sputtering deposition while sputtering the doping material on the antimonide cobalt film by many times to obtain a laminated-structure film, and finally, carrying out in-situ heat treatment to obtain the cobalt-antimonide-base thermoelectric film. The method has high controllability, and is beneficial to generation of the film structure; the film has favorable adhesiveness and repetitiveness, can satisfy the demands for large-scale production, and can accurately control the sputtering power, time and other parameters as well as the doping amount of the doping material; and by adopting the lamination mode, multiple elements can be simultaneously doped conveniently, and the complex techniques for preparing the multi-doping-element target are reduced.

Description

A kind of antimony cobalt base thermal electric film and preparation method thereof
Technical field
The present invention relates to thermoelectricity field of functional materials, more particularly to a kind of achievable independent element doping or multi-element doping High performance antimony cobalt base thermal electric film and preparation method thereof.
Background technology
Thermoelectric material be it is a kind of can realize the environmental type functional material that heat energy and electric energy are directly mutually changed, with heat The thermoelectric device that electric material makes, size is little, light weight, without any mechanical rotation part, work noiseless, service life It is long, without liquid or gaseous medium, not there is a problem of polluting environment, can be widely applied to thermoelectric generator, TEC with And the field such as sensor.Therefore high performance thermoelectric material is prepared, finally realizes the solar energy optical-thermal and industrial exhaust heat of environment-friendly type Waste-heat power generation, and replace the compressor cooling with freon as working medium of high pollution to realize free of contamination semiconductor thermoelectric refrigeration Technology, not only conforms to environmental protection and the requirement of low-carbon economy, while with important scientific meaning and being widely applied prospect.
Currently, due to being limited by pyroelectric material performance, the application of thermo-electric device is also far from reaching using waste heat used heat The stage of mechanical refrigerator is generated electricity and replaces, this has become the bottleneck of thermo-electric device large-scale application, therefore high-performance thermoelectricity Material is one of hot subject of current international material research field.
What the performance of thermoelectric material was mainly characterized by dimensionless figure factor Z T value, ZT=T σ S2/ κ, wherein T are definitely temperature Degree；σ is the electrical conductivity of material；S is Seebeck coefficients；κ is thermal conductivity.Wherein σ S in ZT values2Sometimes and individually it is defined as Power factor（PF=σS2）.
Antimony cobalt（CoSb3）Thermoelectric material is a kind of one of thermoelectric material for being applied to middle warm area with application prospect, The optimization of its thermoelectricity capability and the advanced subject that raising is world thermoelectric material science at present.Recent study discovery, thermoelectricity material Material filming is conducive to improving the pyroelecthc properties of thermoelectric material, main reason is that：First, boundary can be formed by the reduction of dimension Area scattering effect increases the thermoelectric figure of merit of material so as to reduce the thermal conductivity of material, can also when film thickness is in nanometer scale Produce the power factor that quantum confinement effect improves material；2nd, filming can improve its response speed, energy density and small-sized quiet The ability of state localization.In addition, the thermoelectric material of filming is in terms of transformation efficiency and in terms of cost, there is very big excellent Gesture.Therefore for CoSb3The research of base thermal electric film has great importance.
At present for CoSb3The preparation research of thermal electric film only has a small amount of report, and effect is also not satisfactory, mainly mesh Front simple technology of preparing can not prepare many doping, high performance CoSb3Base thermoelectric film material, although complicated technique The higher CoSb of the figure of merit can be prepared3Base thermal electric film, but its preparation cost height, complex process cannot all meet its industrialization Demand.And for CoSb3For base thermal electric film, it will be used for a long time under high temperature degree environment, and the high warm of film is steady The physical characteristics such as qualitative, oxidation-adsorption are most important for film.In addition, CoSb3Need mixing for associated materials It is miscellaneous, the larger raising of thermoelectricity capability can be realized.At present the most frequently used doping way be first by the material of required doping with CoSb3Same target is prepared by mixing into, then is plated and is made film, this mode high cost, tedious process, the time is long, while target With the chemical composition of film and do not correspond, poor controllability.Therefore how CoSb is simplified3The synthesis and preparation process of base thermal electric film, it is real Existing CoSb3The optimum doping of base thermal electric film, obtains Stability Analysis of Structures, the CoSb of superior performance3The key technology of base thermal electric film, It is current research emphasis.
As can be seen here, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of antimony cobalt base thermal electric film and its system Preparation Method, it is intended to solve the problems, such as that existing antimony cobalt base thermal electric film preparation method technique is loaded down with trivial details, efficiency is low, poor controllability.
Technical scheme is as follows：
A kind of preparation method of antimony cobalt base thermal electric film, wherein, including step：
Using antimony cobalt target as sputtering target material, and by the separately made doping target of the material that need to be adulterated；
Turn to be sputtered on target holder by what sputtering target material and doping target were fixed on multistation sputtering system；
Antimony cobalt film layer is coated with an insulating substrate using sputter deposition, while in sputter procedure, will adulterate Material be splashed to antimony cobalt film layer several times so as to prepare the film with laminated construction；
Antimony cobalt base thermal electric film is obtained finally by situ heat treatment.
The preparation method of described antimony cobalt base thermal electric film, wherein,
Sputter procedure is carried out under the conditions of inert gas atmosphere, and by high-temp in-situ heat treatment the antimony cobalt is prepared Base thermal electric film.
The preparation method of described antimony cobalt base thermal electric film, wherein, the material of doping is splashed to into several times antimony cobalt Film layer.
The preparation method of described antimony cobalt base thermal electric film, wherein, after the completion of sputtering, close sputtering source and air inlet Valve, by pressure in vacuum tank below 0.1MPa is evacuated to, then is passed through inert gas in a vacuum chamber, while increasing the antimony cobalt being coated with Film layer temperature.
The preparation method of described antimony cobalt base thermal electric film, wherein, the inert gas is nitrogen or argon gas.
The preparation method of described antimony cobalt base thermal electric film, wherein, the material of the doping includes simple substance and compound One or more.
The preparation method of described antimony cobalt base thermal electric film, wherein, the simple substance is In, Ti, Se, Mo, Zn, Bi, Cu And one or more of Yb etc..
The preparation method of described antimony cobalt base thermal electric film, wherein, the compound is ZnO, AZO, Bi2Te3Deng a kind of Or it is several.
A kind of antimony cobalt base thermal electric film, wherein, made using preparation method as above.
Beneficial effect：, by preparing antimony cobalt base thermal electric film using sputter-deposition technology, controllability is strong, favorably for the present invention In the generation of membrane structure, film has good tack and repeatability, can meet large-scale production needs, and can be accurate Control sputtering power, the parameter such as time and dopant material doping, by the way of many laminations, be easy to multiple element same When be doped, decrease the loaded down with trivial details technique for preparing many doped chemical targets, simplify preparation technology.
Description of the drawings
Fig. 1 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 1.
Fig. 2 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 2.
Fig. 3 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 3.
Fig. 4 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 4.
Fig. 5 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 5.
Fig. 6 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 6.
Fig. 7 is antimony cobalt base thermal electric film preparation flow figure in the embodiment of the present invention 7.
Fig. 8 a to Fig. 8 c are antimony cobalt base thermal electric film spectral measurement result of the present invention.
Fig. 9 provides antimony cobalt base thermal electric film and surveys with the thermoelectricity capability of undoped p thermal electric film by the embodiment of the present invention 1 Amount comparative result figure.
Specific embodiment
The present invention provides a kind of antimony cobalt base thermal electric film and preparation method thereof, to make the purpose of the present invention, technical scheme And effect is clearer, clear and definite, below the present invention is described in more detail.It should be appreciated that described herein be embodied as Example is not intended to limit the present invention only to explain the present invention.
A kind of preparation method of antimony cobalt base thermal electric film provided by the present invention, it includes step：
Using antimony cobalt target as sputtering target material, and by the separately made doping target of the material that need to be adulterated；
Turn to be sputtered on target holder by what sputtering target material and doping target were fixed on multistation sputtering system；
Antimony cobalt film layer is coated with an insulating substrate using sputter deposition, while in sputter procedure, will adulterate Material be splashed to antimony cobalt film layer several times so as to prepare the film with laminated construction；
Antimony cobalt base thermal electric film is obtained finally by situ heat treatment.
The present invention is using sputter deposition during antimony cobalt base thermal electric film is prepared, by multistep cosputtering Method prepares lamination alloy firm, and the mode of this lamination is easy to multiple element to adulterate simultaneously, simplifies technique, improves efficiency, Manufacturing cost is lower.And can accurately control the doping of the parameters such as sputtering power, time and dopant material, moreover it is possible to ensure Material doped uniformity.The method controllability is strong, and beneficial to the generation of membrane structure, the film of generation has good tack And repeatability, large-scale production needs can be met.
Specifically, the sputter procedure is carried out under the conditions of inert gas atmosphere, is made by high-temp in-situ heat treatment It is standby to obtain the antimony cobalt base thermal electric film.
Specifically the material of doping can be several times splashed to antimony cobalt film layer.It is thin that antimony cobalt is coated with an insulating substrate During film layer, when first antimony cobalt being sputtered onto into different time, the sputtering source of dopant material is opened, beginning is carried out altogether together with antimony cobalt Sputtering, many lamination antimony cobalt base thermal electric films with periodic structure are prepared by this multistep processes.
For example, when 1/4,1/2,3/4 of total sputtering time needed for antimony cobalt is sputtered onto, the material of doping needed for opening （Represented with A）Sputtering source, beginning carries out cosputtering together with antimony cobalt, time of each cosputtering doping time for needed for 1/3, i.e., the time of each cosputtering is identical.So can be had " CoSb by above-mentioned three-step approach3+CoSb3/A+CoSb3” Many lamination antimony cobalt base alloy films of periodic structure.
In addition, after the completion of sputtering, sputtering source and intake valve are closed, pressure in vacuum tank is evacuated to into below 0.1MPa, then Inert gas is passed through in vacuum chamber, while increase the antimony cobalt film layer temperature that has been coated with, by situ heat treatment being obtained most Whole antimony cobalt base thermal electric film.
By the method for the present invention, different doping contents, the antimony cobalt base thermal electric film of different doping types can be prepared. Also, its controllability is strong, repeatability is high, and preparation process is simple, is capable of achieving independent element doping or multi-element doping.
The inert gas in the present invention is nitrogen or argon gas.
The material for wherein adulterating includes simple substance and/or compound.For simple substance, its can be In, Ti, Se, Mo, Zn, Bi, One or more in Cu and Yb etc..For compound, it can be ZnOAZO and Bi2Te3Deng one or more.
Based on said method, the present invention also provides a kind of antimony cobalt base thermal electric film, and it adopts preparation side as above Method is made.The antimony cobalt base thermal electric film can be actually used on thin-film power generating device.
Embodiment
Using In as dopant material（A）, first, by CoSb3Sputter is separately fixed at In targets（Multistation is sputtered System）Two station target framves on it is to be sputtered；With polyimides（PI）As substrate（Dielectric substrate）, substrate is placed on into appearance In device, ultrasonic wave cleaning is carried out successively using acetone, alcohol and deionized water；Sputtering system base vacuum is evacuated to 6.0 × 10- 4Pa, is passed through flow for 40 sccmAr gas（It is high-purity）, operating pressure control is 3.0 × 10-1 Pa；It is less than using ion gun energy The ion beam of 1KeV is bombarded substrate surface, and impurity molecule of the absorption in substrate surface is further removed；
As Fig. 1 shows, in the 1st embodiment, CoSb is coated with substrate initially with sputtering method3Thermal electric film, always Sputtering time be 60 min, work as CoSb3When being sputtered onto 15 min, In sputtering sources are opened, allow In（Doped chemical）With CoSb3Together Shi Jinhang is sputtered, and the cosputtering time is 30 s；After the completion of, In sputtering sources are closed, continue to sputter CoSb3;Work as CoSb3It is sputtered onto 30 During min, continue and the s of In cosputterings 30；Work as CoSb3When being sputtered onto 45 min, continue and the s of In cosputterings 30；Last CoSb3After It is continuous to be sputtered onto 60 min.After the completion of sputtering, after plated film terminates, sputtering source and intake valve are closed, pressure in vacuum tank is evacuated to Below 0.1Pa, then Ar gas is passed through in a vacuum chamber, pressure in vacuum tank is higher than 100 Pa, while increasing at the film layer being coated with Temperature to 350 DEG C, synthesis obtain CoSb3Base thermal electric film.
Fig. 2 is the CoSb of the present invention3The preparation flow figure of the embodiment of base thermal electric film preparation method the 2nd, with embodiment 1 not Same is not to be divided into three steps, can be divided into N steps（I.e. N number of cycle）Cosputtering doping is carried out, N is the integer more than or equal to 1.
Fig. 3 is the CoSb of the present invention3The preparation flow figure of the embodiment of base thermal electric film preparation method the 3rd, with embodiment 1 not With, the cosputtering doping of two and the above can be carried out, will doped chemical A and dopant material B together with CoSb3Carry out altogether Sputtering.
Fig. 4 is the CoSb of the present invention3The preparation flow figure of the embodiment of base thermal electric film preparation method the 4th, with embodiment 3 not Same is not to be divided into three steps, and can be divided into N steps carries out cosputtering doping, and N is the integer more than or equal to 1.
Fig. 5 is the CoSb of the present invention3The preparation flow figure of the embodiment of base thermal electric film preparation method the 5th, with embodiment 3 not With, when multi-element doping is carried out, doped chemical does not carry out cosputtering simultaneously, but respectively with CoSb3Splashed altogether Penetrate, i.e. A and CoSb3Doping, B and CoSb3Doping.
Fig. 6 is the CoSb of the present invention3The preparation flow figure of the embodiment of base thermal electric film preparation method the 6th, with embodiment 5 not Same is not to be divided into three steps, and can be divided into N steps carries out cosputtering doping, and N is the integer more than or equal to 1.
Fig. 7 is the CoSb of the present invention3The preparation flow figure of the embodiment of base thermal electric film preparation method the 7th, with embodiment 1 not Be the element of cosputtering doping each time can be identical A or B, alternatively different A or B.
Fig. 8 a to Fig. 8 c are CoSb3In base thermal electric film different elements surface distribution map, as can be seen from the figure respectively Element is planted in CoSb3Distribution is all visibly homogeneous, it can be seen that the present invention can coat the CoSb of Uniform Doped3Base thermal electric film.
Fig. 9 is the CoSb that the embodiment of the present invention one is provided3The thermoelectricity capability measurement result of base thermal electric film（In adulterate with In undoped ps）, can be learnt by figure：Film performance after doping is more excellent.
In sum, by preparing antimony cobalt base thermal electric film using sputter-deposition technology, controllability is strong, favorably for the present invention In the generation of membrane structure, film has good tack and repeatability, can meet large-scale production needs, and can be accurate Control sputtering power, the parameter such as time and dopant material doping, by the way of many laminations, be easy to multiple element same When be doped, decrease the loaded down with trivial details technique for preparing many doped chemical targets, simplify preparation technology.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, and for those of ordinary skills, can To be improved according to the above description or be converted, all these modifications and variations should all belong to the guarantor of claims of the present invention Shield scope.

Claims (8)

1. a kind of preparation method of antimony cobalt base thermal electric film, it is characterised in that including step：
Using antimony cobalt target as sputtering target material, and by the separately made doping target of the material that need to be adulterated；
Turn to be sputtered on target holder by what sputtering target material and doping target were fixed on multistation sputtering system；
Antimony cobalt film layer is coated with an insulating substrate using sputter deposition, when antimony cobalt is sputtered onto different time, is beaten The sputtering source of dopant material is opened, beginning carries out cosputtering together with antimony cobalt, and the time of each cosputtering is identical, prepares tool There is the film of laminated construction；
After the completion of sputtering, sputtering source and intake valve are closed, pressure in vacuum tank is evacuated to into below 0.1MPa, then led in a vacuum chamber Enter inert gas, while increase the antimony cobalt film layer temperature that has been coated with, by situ heat treatment so that final antimony cobalt is obtained Base thermal electric film.
2. the preparation method of antimony cobalt base thermal electric film according to claim 1, it is characterised in that sputter procedure is in inertia Carry out under gas atmosphere, the antimony cobalt base thermal electric film is prepared by high-temp in-situ heat treatment.
3. the preparation method of antimony cobalt base thermal electric film according to claim 1, it is characterised in that by the material point of doping Repeatedly it is splashed to antimony cobalt film layer.
4. the preparation method of antimony cobalt base thermal electric film according to claim 1, it is characterised in that the inert gas is Nitrogen or argon gas.
5. the preparation method of antimony cobalt base thermal electric film according to claim 1, it is characterised in that the material of the doping One or more including simple substance and compound.
6. the preparation method of antimony cobalt base thermal electric film according to claim 5, it is characterised in that the simple substance be In, One or more in Ti, Se, Mo, Zn, Bi, Cu and Yb.
7. the preparation method of antimony cobalt base thermal electric film according to claim 5, it is characterised in that the compound is ZnO, AZO and Bi2Te3In one or more.
8. a kind of antimony cobalt base thermal electric film, it is characterised in that using the preparation method system as described in claim 1 to 7 is arbitrary Into.
CN201410626851.7A 2014-11-10 2014-11-10 Cobalt-antimonide-base thermoelectric film and preparation method thereof Active CN104388901B (en)

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CN107460443A (en) * 2017-08-01 2017-12-12 深圳大学 A kind of Ti adulterates CoSb3Thermal electric film and preparation method thereof
CN107385403A (en) * 2017-08-01 2017-11-24 深圳大学 A kind of ZnSb bases thermal electric film and preparation method thereof
CN107299326A (en) * 2017-08-16 2017-10-27 信利光电股份有限公司 A kind of vacuum coating doping target and preparation method thereof and vacuum coating method

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CN101969095B (en) * 2010-08-26 2012-08-29 中山大学 Quasi one-dimensional nano structural thermoelectric material, device and preparation method thereof

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