CN107460443A - A kind of Ti adulterates CoSb3Thermal electric film and preparation method thereof - Google Patents
A kind of Ti adulterates CoSb3Thermal electric film and preparation method thereof Download PDFInfo
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- CN107460443A CN107460443A CN201710646626.3A CN201710646626A CN107460443A CN 107460443 A CN107460443 A CN 107460443A CN 201710646626 A CN201710646626 A CN 201710646626A CN 107460443 A CN107460443 A CN 107460443A
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- cosb
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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
- C23C14/3464—Sputtering using more than one target
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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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
- C23C14/06—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
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
- C23C14/06—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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
Abstract
The present invention discloses a kind of Ti doping CoSb3Thermal electric film and preparation method thereof, method include step：Select purity for 99.99% Ti targets and purity be 99.99% CoSb3Target is as raw material, by Ti targets and CoSb3Target is respectively placed on the station target frame of sputtering system；Sputtering system background vacuum is evacuated to 8.0 × 10‑4Pa, inert gas is passed through, by the control of the pressure of the sputtering system in 0.4Pa and following；Using sputter deposition first on substrate depositing Ti film, then deposit CoSb on Ti films3Film；The good film of above-mentioned deposition is heat-treated, obtains Ti doping CoSb3Thermal electric film.The present invention by way of controlling Ti film thicknesses, can realize effective control of Ti doping；By controlling Fabrication parameters, regulate and control the nanostructured yardstick of film, realize increasing substantially for thin film thermoelectric performance.
Description
Technical field
The present invention relates to field of thin film material preparation, more particularly to a kind of Ti doping CoSb3Thermal electric film and its preparation side
Method.
Background technology
The current whole world routinizes a large amount of using having resulted in the energy crisis to grow in intensity and climate warming problem of the energy,
There is an urgent need to actively push forward and advocate using clean regenerative resource.Thermoelectric cell is the very wide environmental type of the scope of application
The energy, heat energy and electric energy are directly intercoupled, mutually changed by it using the pyroelectric effect of thermoelectric material, are realized and are generated electricity, have
The series of advantages such as noiseless, unharmful substance discharge, reliability height, long lifespan, it is scattered in waste heat waste-heat power generation and movement
Formula thermal source, which utilizes etc., to be played the role of to be difficult to substitute, but the characteristic based on thermoelectric material in itself, and its manufacturing cost is high, conversion
Efficiency is low, limits the large-scale use of thermo-electric generation unit.
The performance of thermoelectric material is mainly characterized by a dimensionless constant ZT, wherein ZT=S2× σ × T ÷ k, wherein S are
Seebeck coefficient, σ are electrical conductivity, and T is absolute temperature（Temperature i.e. residing for material, S under condition of different temperatures, σ, K values not phases
Together）, k is thermal conductivity.
CoSb3It is one of skutterudite material, there is higher electrical conductivity and relatively low thermal conductivity, because its thermoelectricity capability is high
Semi-conductor thermoelectric material in putting goods on the market at present, and there is optimal performance when temperature is higher, therefore in medium temperature thermoelectricity
Had broad application prospects in terms of generating, it is considered to be one of most promising thermoelectric material.Study both at home and abroad at present
Emphasis is mainly to improve the thermoelectricity capability of material using the doping filling of different elements and low-dimensional, obtain it is certain into
Effect.Wherein, it is one way in which by thermoelectric film, and the thin-film material of two dimension, it can be separately made as needed
Thermo-electric device, and be more easy to realize Miniaturized Thermoelectric device, there is the advantage that body material can not compare.
Therefore, for CoSb3The research of thermoelectric film material becomes one of important research direction of temperature difference devices field.
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 Ti to adulterate CoSb3Thermal electric film and
Its preparation method.
Technical scheme is as follows：
A kind of Ti adulterates CoSb3The preparation method of thermal electric film, wherein, including step：
A, select purity for 99.99% Ti targets and purity be 99.99% CoSb3Target as raw material, by Ti targets and
CoSb3Target is respectively placed on the station target frame of sputtering system；
B, sputtering system background vacuum is evacuated to 8.0 × 10-4Pa, inert gas is passed through, by the pressure of the sputtering system
Control is in 0.4Pa and following；
C, using sputter deposition first on substrate depositing Ti film, then deposit CoSb on Ti films3Film；
D, the good film of above-mentioned deposition is heat-treated, the temperature of the heat treatment is 200 DEG C ~ 500 DEG C, obtains Ti doping
CoSb3Thermal electric film.
Described Ti doping CoSb3The preparation method of thermal electric film, wherein, in step B, be passed through flow for 40 sccm with
Under Ar gas.
Described Ti doping CoSb3The preparation method of thermal electric film, wherein, in step C, the substrate is glass substrate.
Described Ti doping CoSb3The preparation method of thermal electric film, wherein, in step C, the speed of deposition film is 0.1
Å/s~10 Å/s。
Described Ti doping CoSb3The preparation method of thermal electric film, wherein, in step C, the thickness of the Ti films for 1 ~
100nm。
Described Ti doping CoSb3The preparation method of thermal electric film, wherein, in step C, the CoSb3The thickness of film is
100~1000nm。
Described Ti doping CoSb3The preparation method of thermal electric film, wherein, in step D, the temperature of the heat treatment is
300 DEG C or 463 DEG C.
A kind of Ti adulterates CoSb3Thermal electric film, wherein, as above any described Ti adulterates CoSb for use3The system of thermal electric film
Preparation Method is prepared.
A kind of Ti adulterates CoSb3The preparation method of thermal electric film, wherein, including step：
The CoSb that A1, selection purity are 99.99 % for 99.99 % Ti targets and purity3Target is as raw material, then by Ti targets
Material and CoSb3Target is respectively placed on the station target frame of sputtering system；
B1, sputtering system background vacuum is evacuated to 8.0 × 10-4Pa, it is 40 sccm Ar gas to be passed through flow, by the sputtering
The pressure of system is controlled in 0.4Pa；
C1, film deposition rate is controlled to be 5/s, using sputter deposition depositing Ti film on the glass substrate first, institute
The thickness for stating Ti films is 10nm, then deposits CoSb on Ti films3Film, the CoSb3The thickness of film is 500nm；
D1, the good film of above-mentioned deposition is heat-treated, the temperature of the heat treatment is 300 DEG C, obtains Ti doping CoSb3Heat
Conductive film.
Beneficial effect：The preparation method is that the Ti that nanostructured is grown using nano thickness preformed layer mode is adulterated
CoSb3Thermal electric film, by the regulation and control of preparation parameter, the content of Ti in film can not only be adjusted, can more prepare has
Completely, fine and close nano structure membrane.Compared with prior art, the inventive method can not only pass through thin film composition and nano junction
The regulation of structure, realize the significantly lifting of thin film thermoelectric performance；A nanometer Ti doping CoSb can also be reduced3The manufacturing process of film
Complexity and manufacturing cost.
Brief description of the drawings
Fig. 1 is the structural representation that one layer of Ti film is deposited on substrate.
Fig. 2 is to deposit CoSb on Ti films in Fig. 13The structural representation of film.
Fig. 3 is that the Ti that the film in Fig. 2 is formed after high-temperature heat treatment adulterates CoSb3The structural representation of thermal electric film.
Fig. 4 is the scanning electron microscope (SEM) photograph of the thermal electric film prepared by embodiment 1.
Embodiment
The present invention provides a kind of Ti doping CoSb3Thermal electric film and preparation method thereof, to make the purpose of the present invention, technical side
Case and effect are clearer, clear and definite, and the present invention is described in more detail below.It is it should be appreciated that described herein specific real
Example is applied only to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of Ti doping CoSb3The preparation method preferred embodiment of thermal electric film, wherein, including step：
A, select purity for 99.99% Ti targets and purity be 99.99% CoSb3Target as raw material, by Ti targets and
CoSb3Target is respectively placed on the station target frame of sputtering system；
B, sputtering system background vacuum is evacuated to 8.0 × 10-4Pa, inert gas is passed through, by the pressure of the sputtering system
Control is in 0.4Pa and following；
Preferably, it is passed through the Ar gas that flow is 40 below sccm.
C, using sputter deposition first on substrate depositing Ti film, then deposit CoSb on Ti films3Film；
Preferably, the speed of deposition film is 0.1/s ~ 10/s.
Preferably, the substrate is glass substrate.
Preferably, the thickness of the Ti films is 1 ~ 100nm, the CoSb3The thickness of film is 100 ~ 1000nm.
D, the good film of above-mentioned deposition is heat-treated, the temperature of the heat treatment is 200 DEG C ~ 500 DEG C, obtains Ti
Adulterate CoSb3Thermal electric film.
With reference to shown in Fig. 1 ~ Fig. 3, the present invention selects high-purity Ti pure metals and CoSb3As raw material, first with
Ti pure metals, one layer of Ti film 2 is deposited on substrate 1, sees Fig. 1；Then use CoSb3As raw material, in above-mentioned Ti
CoSb is deposited on film 23Film 3, is shown in Fig. 2；Finally, the film of above-mentioned deposition is carried out to 200 degree ~ 500 degree of high-temperature heat treatment,
Ultimately form Ti doping CoSb3Thermal electric film 4, is shown in Fig. 3.
Compared with prior art, preparation method of the present invention has the following advantages that：Can be by controlling the side of Ti preformed layer thickness
Formula, realize effective control of Ti doping；The film prepared has complete, fine and close nanostructured；It can be made by controlling
Standby parameter, regulate and control the nanostructured yardstick of film, realize increasing substantially for thin film thermoelectric performance, and this method has flexibly
Property, stronger controllability and Process simplicity.
The present invention also provides a kind of Ti doping CoSb3Thermal electric film, wherein, as above any described Ti adulterates CoSb for use3
The preparation method of thermal electric film is prepared.Ti of the present invention adulterates CoSb3Thermal electric film has complete, fine and close nano junction
Structure, increase substantially the thermoelectricity capability of thermal electric film.
Below by embodiment, the present invention is described in detail.
Embodiment 1
Using magnetron sputtering coater, by the Ti and CoSb that purity is 99.99 %3Target is placed in the sputtering target position of coating machine
On, substrate is used as using simple glass；Sputtering system base vacuum is evacuated to 8.0 × 10-4Pa, it is 40sccm high-purity Ars to be passed through flow
Gas, operating pressure are controlled in 0.4Pa；Ti thin film depositions are carried out first, and film deposition rate is 5/s, and thin film deposition thickness is
10nm；Then in Ti film layers, CoSb is carried out3Thin film deposition, deposit thickness 500nm；Finally by good thin of above-mentioned deposition
Film carries out high-temperature heat treatment, and heat treatment temperature is 300 DEG C.
Fig. 4 is the surface topography using the film prepared by the method, as shown in Figure 4, by thin prepared by this method
Film, its surface have fine and close, uniform nanostructured.
Table 1 is the thermoelectricity capability of prepared film, and it in measurement temperature is 300K that the thermoelectricity capability data in table, which are respectively,
Obtained with test under 463K.As shown in Table 1, by the film prepared by this method, there is preferably thermoelectricity capability.
Table 1
In summary, a kind of Ti doping CoSb provided by the invention3Thermal electric film and preparation method thereof.The present invention is from high-purity
Ti pure metals and CoSb3As raw material, first with Ti pure metals, one layer of Ti film is prepared on insulated substrate, with
CoSb is used afterwards3As raw material, CoSb is deposited on above-mentioned Ti films3Film.Finally, then 200 degree ~ 500 degree of height is carried out
Warm processing, ultimately form a nanometer Ti doping CoSb3Thermal electric film.Compared with prior art, preparation method of the present invention has such as
Lower advantage：By way of controlling Ti preformed layer thickness, the effective control of Ti doping can be realized；The film prepared has
Completely, fine and close nanostructured；It can regulate and control the nanostructured yardstick of film by controlling Fabrication parameters, realize thin film thermoelectric
Energy increases substantially, and this method has flexibility, stronger controllability and Process simplicity.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved or converted according to the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect scope.
Claims (9)
1. a kind of Ti adulterates CoSb3The preparation method of thermal electric film, it is characterised in that including step：
A, select purity for 99.99% Ti targets and purity be 99.99% CoSb3Target as raw material, by Ti targets and
CoSb3Target is respectively placed on the station target frame of sputtering system；
B, sputtering system background vacuum is evacuated to 8.0 × 10-4Pa, inert gas is passed through, by the pressure control of the sputtering system
System is in 0.4Pa and following；
C, using sputter deposition first on substrate depositing Ti film, then deposit CoSb on Ti films3Film；
D, the good film of above-mentioned deposition is heat-treated, the temperature of the heat treatment is 200 DEG C ~ 500 DEG C, obtains Ti doping
CoSb3Thermal electric film.
2. Ti according to claim 1 adulterates CoSb3The preparation method of thermal electric film, it is characterised in that in step B, be passed through
Flow is 40 below sccm Ar gas.
3. Ti according to claim 1 adulterates CoSb3The preparation method of thermal electric film, it is characterised in that described in step C
Substrate is glass substrate.
4. Ti according to claim 1 adulterates CoSb3The preparation method of thermal electric film, it is characterised in that in step C, deposition
The speed of film is 0.1 ~ 10.
5. Ti according to claim 1 adulterates CoSb3The preparation method of thermal electric film, it is characterised in that described in step C
The thickness of Ti films is 1 ~ 100nm.
6. Ti according to claim 1 adulterates CoSb3The preparation method of thermal electric film, it is characterised in that described in step C
CoSb3The thickness of film is 100 ~ 1000nm.
7. Ti according to claim 1 adulterates CoSb3The preparation method of thermal electric film, it is characterised in that described in step D
The temperature of heat treatment is 300 DEG C or 463 DEG C.
8. a kind of Ti adulterates CoSb3Thermal electric film, it is characterised in that using the Ti doping as described in claim 1-7 is any
CoSb3The preparation method of thermal electric film is prepared.
9. a kind of Ti adulterates CoSb3The preparation method of thermal electric film, it is characterised in that including step：
The CoSb that A1, selection purity are 99.99 % for 99.99 % Ti targets and purity3Target is as raw material, then by Ti targets
Material and CoSb3Target is respectively placed on the station target frame of sputtering system；
B1, sputtering system background vacuum is evacuated to 8.0 × 10-4Pa, it is 40 sccm Ar gas to be passed through flow, is by the sputtering
The pressure of system is controlled in 0.4Pa；
C1, film deposition rate is controlled to be 5/s, it is described using sputter deposition depositing Ti film on the glass substrate first
The thickness of Ti films is 10nm, then deposits CoSb on Ti films3Film, the CoSb3The thickness of film is 500nm；
D1, the good film of above-mentioned deposition is heat-treated, the temperature of the heat treatment is 300 DEG C, obtains Ti doping CoSb3Heat
Conductive film.
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| CN201710646626.3A CN107460443A (en) | 2017-08-01 | 2017-08-01 | A kind of Ti adulterates CoSb3Thermal electric film and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585145A (en) * | 2004-05-28 | 2005-02-23 | 中国科学院上海硅酸盐研究所 | Electrode material of cobalt base antimonide pyroelectric material and preparing process thereof |
| KR101375620B1 (en) * | 2012-11-08 | 2014-04-01 | 한국세라믹기술원 | Thermoelectric device having high interface matching and manufacturing method of the same |
| CN104388901A (en) * | 2014-11-10 | 2015-03-04 | 深圳大学 | Cobalt-antimonide-base thermoelectric film and preparation method thereof |
| CN105932150A (en) * | 2016-05-18 | 2016-09-07 | 深圳大学 | Sb-base flexible film thermoelectric cell and manufacturing method therefor |
-
2017
- 2017-08-01 CN CN201710646626.3A patent/CN107460443A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585145A (en) * | 2004-05-28 | 2005-02-23 | 中国科学院上海硅酸盐研究所 | Electrode material of cobalt base antimonide pyroelectric material and preparing process thereof |
| KR101375620B1 (en) * | 2012-11-08 | 2014-04-01 | 한국세라믹기술원 | Thermoelectric device having high interface matching and manufacturing method of the same |
| CN104388901A (en) * | 2014-11-10 | 2015-03-04 | 深圳大学 | Cobalt-antimonide-base thermoelectric film and preparation method thereof |
| CN105932150A (en) * | 2016-05-18 | 2016-09-07 | 深圳大学 | Sb-base flexible film thermoelectric cell and manufacturing method therefor |
Non-Patent Citations (1)
| Title |
|---|
| 范卫芳: "锑基热电薄膜及薄膜温差电池的制备", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
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Application publication date: 20171212 |