CN108218425A - A kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials and preparation method thereof - Google Patents

A kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials and preparation method thereof Download PDF

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CN108218425A
CN108218425A CN201810070316.6A CN201810070316A CN108218425A CN 108218425 A CN108218425 A CN 108218425A CN 201810070316 A CN201810070316 A CN 201810070316A CN 108218425 A CN108218425 A CN 108218425A
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cubic phase
base thermoelectricity
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CN108218425B (en
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温翠莲
张炜坚
谢秋罕
杨洪雷
张致远
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Fuzhou University
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Abstract

The invention discloses a kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials and preparation method thereof are to weigh Ca powder, Ge powder and Sb powder respectively in proportion, then place it in and supersonic oscillations are carried out in organic solvent, be allowed to be sufficiently mixed；Then after organic solvent completely volatilization, block is made through dry-press process；It places it in again in alumina crucible and uses Ca powder packings, be put into microwave vacuum high-temperature heater, in high-purity argon gas atmosphere, the cubic phase Ca that Sb adulterates is obtained through pyroreaction2Ge base thermoelectricity materials.The present invention is by microwave heating, and the phenomenon that avoiding abnormal grain growth during conventional sintering, final obtain has ultra-fine grain structural material, and realize the reduction of materials synthesis temperature, has preferable application prospect.

Description

A kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials and preparation method thereof
Technical field
The invention belongs to thermoelectricity field of functional materials, and in particular to a kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials And preparation method thereof.
Background technology
Since the last century nineties, material worker is dedicated to the research of energy conversion material so that thermoelectricity material Material becomes a research hotspot of material science.Thermoelectric material is called temperature difference material, is that one kind has fuel factor and electrical effect The new function material mutually converted.Thermoelectric material is not needed to using transmission parts in use, noiseless, nothing during work Dump object, have and solar energy, wind energy, water can etc. the comparable advantage of secondary energy sources, there are no pollution to the environment, and thermoelectric material Dependable performance, service life is long, is a kind of environmentally friendly material with wide application prospect.
In recent years, since intermetallic compound has the performances such as excellent thermoelectricity and mechanics, investigation of materials worker is to this Class novel alloy gives great concern, Ca2Ge is exactly one of them.It is not only because Ca2Ge has good pyroelectricity Can, and the raw material resources of alloying element Ca, Ge are enriched, stratum reserves are big, cheap so that and it becomes a kind of potential Can extensive utilization new structural material, therefore Ca2The research of Ge just seems significant.
Sb doping is to reduce thermal conductivity, optimize electrical property, further improve conducting material thermoelectricity performance and improve mechanical property Important channel.The cubic phase Ca of Sb doping2Ge can be realized due to being made of three kinds of service life extremely long element sb, Ca and Ge Recycle, and to environment a series of substantially pollution-free etc. features and receive much attention.At present from the point of view of domestic and international research situation, nothing By be theoretical research or experimental study all only to block Ca2The report of Ge researchs, and to Sb doping cubic phase Ca2Ge materials Preparation research have not been reported.
Invention content
The purpose of the present invention is to provide a kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials and preparation method thereof, Adulterate to reduce thermal conductivity, optimization electrical property, the thermoelectricity capability and mechanical property for improving material by Sb, obtain purity it is high, Composition determines the Sb doping cubic phase Ca of ratio2Ge base thermoelectricity materials.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of cubic phase Ca of Sb doping2Ge base thermoelectricity materials, preparation method include the following steps：
（1）In molar ratio 70:33:(0.3 ~ 2) weighs Ca powder, Ge powder and Sb powder respectively, is then poured into organic solvent, surpasses 20 ~ 60 min of sonication is allowed to be sufficiently mixed；
（2）Treat step（1）Gained mixed liquor is under 25 ~ 60 DEG C of environment after complete volatile organic solvent, using dry-press process work It is pressed into the cylindrical idiosome of 10 ~ 60 mm of Φ by skill under 20 ~ 60 Mpa pressure；
（3）Gained idiosome is placed in alumina crucible, and with Ca powder packings, is then placed into microwave vacuum high-temperature heater It is interior, high-purity argon gas is passed through, 400 ~ 700 DEG C are warming up under the conditions of 2.45 GHz of microwave frequency, 1.5 ~ 3.5 kW of microwave power；
（4）After temperature reaches, 0.5 ~ 6 h of isothermal holding, then cools to material with the furnace room under 1.5 ~ 2.5 kW power Temperature obtains the cubic phase Ca of Sb doping2Ge base thermoelectricity materials.
Step（1）In organic solvent used be ethyl alcohol.
Step（3）Deionized water, alcohol, acetone progress ultrasonic wave should be used clear before alumina crucible use used successively It washes, ultrasonic cleaning total time is 15 ~ 50 min.The purity of argon gas used is 99% ~ 99.99%.
Compared with the prior art, the present invention has the following advantages:
1）The present invention is by microwave heating, the phenomenon that avoiding abnormal grain growth during conventional sintering, is finally had The material of ultra-fine grain structure, and realize the reduction of materials synthesis temperature；
2）The method of the present invention heating temperature is low, can be to avoid the high temperature evaporation loss problem of Ca, and control composition is fixed well compares, weight Renaturation is preferable；
3）The present invention prepared under vacuum, can effectively prevent impurity be mixed into and problem of oxidation, to finally obtain height Pure product.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of thermoelectric material prepared by embodiment 1；
Fig. 2 is embodiment 1 and Seebeck coefficient-temperature curve of thermoelectric material prepared by reference examples；
Fig. 3 is embodiment 1 and the conductivity versus temperature curve of thermoelectric material prepared by reference examples；
Fig. 4 is embodiment 1 and power factor-temperature curve of thermoelectric material prepared by reference examples.
Specific embodiment
In order to which content of the present invention is made to easily facilitate understanding, With reference to embodiment to of the present invention Technical solution is described further, but the present invention is not limited only to this.
The purity that the purity of Ca powder used is more than 99%, Ge powder is more than the purity of 99%, Sb powder more than 99%.Argon gas used Purity is more than 99%.
Deionized water, alcohol, acetone should be used to carry out ultrasonic cleaning, ultrasonic cleaning before alumina crucible use successively Total time is 15 ~ 50 min.
Embodiment 1
（1）In molar ratio 70:33:0.5 weighs Ca powder, Ge powder and Sb powder respectively, is then poured into ethyl alcohol, supersonic oscillations 30 min are allowed to be sufficiently mixed；
（2）Treat step（1）Gained mixed liquor volatilizees under 30 DEG C of environment completely after ethyl alcohol, using dry process for forming, by its The cylindrical idiosome of 15 mm of Φ is pressed under 25 Mpa pressure；
（3）Gained idiosome is placed in alumina crucible, and with Ca powder packings, is then placed into microwave vacuum high-temperature heater It is interior, high-purity argon gas is passed through, 500 DEG C are warming up under the conditions of 2.45 GHz of microwave frequency, 1.5 kW of microwave power；
（4）After temperature reaches, 1 h of isothermal holding, then cools to material with the furnace room temperature, obtains Sb under 1.5 kW power The cubic phase Ca of doping2Ge base thermoelectricity materials.
The cubic phase Ca of 1 Sb manufactured in the present embodiment of table doping2The constituent analysis of Ge
Fig. 1 is the scanning electron microscope (SEM) photograph of thermoelectric material prepared by the present embodiment.As seen from Figure 1, gained final product crystallite dimension is thin It is small, uniform.
Embodiment 2
（1）In molar ratio 70:33:1 weighs Ca powder, Ge powder and Sb powder respectively, is then poured into ethyl alcohol, supersonic oscillations 50 Min is allowed to be sufficiently mixed；
（2）Treat step（1）Gained mixed liquor volatilizees under 20 DEG C of environment completely after ethyl alcohol, using dry process for forming, by its The cylindrical idiosome of 30 mm of Φ is pressed under 40 Mpa pressure；
（3）Gained idiosome is placed in alumina crucible, and with Ca powder packings, is then placed into microwave vacuum high-temperature heater It is interior, high-purity argon gas is passed through, 400 DEG C are warming up under the conditions of 2.45 GHz of microwave frequency, 3 kW of microwave power；
（4）After temperature reaches, 4 h of isothermal holding, then cools to material with the furnace room temperature under 2 kW power, obtains Sb and mixes Miscellaneous cubic phase Ca2Ge base thermoelectricity materials.
Embodiment 3
（1）In molar ratio 70:33:1.8 weigh Ca powder, Ge powder and Sb powder respectively, are then poured into ethyl alcohol, supersonic oscillations 40 min are allowed to be sufficiently mixed；
（2）Treat step（1）Gained mixed liquor volatilizees under 60 DEG C of environment completely after ethyl alcohol, using dry process for forming, by its The cylindrical idiosome of 60 mm of Φ is pressed under 50 Mpa pressure；
（3）Gained idiosome is placed in alumina crucible, and with Ca powder packings, is then placed into microwave vacuum high-temperature heater It is interior, high-purity argon gas is passed through, 600 DEG C are warming up under the conditions of 2.45 GHz of microwave frequency, 3.5 kW of microwave power；
（4）After temperature reaches, 5 h of isothermal holding, then cools to material with the furnace room temperature, obtains Sb under 2.5 kW power The cubic phase Ca of doping2Ge base thermoelectricity materials.
Reference examples
（1）In molar ratio 2.2:1 weighs Ca powder and Ge powder respectively, is then poured into ethyl alcohol, 25 min of supersonic oscillations makes Be sufficiently mixed；
（2）Treat step（1）Gained mixed liquor volatilizees under 50 DEG C of environment completely after ethyl alcohol, using dry process for forming, by its The cylindrical idiosome of 20 mm of Φ is pressed under 60 Mpa pressure；
（3）Gained idiosome is placed in alumina crucible, and with Ca powder packings, is then placed into microwave vacuum high-temperature heater It is interior, high-purity argon gas is passed through, 600 DEG C are warming up under the conditions of 2.45 GHz of microwave frequency, 3 kW of microwave power；
（4）After temperature reaches, 1 h of isothermal holding, then cools to material with the furnace room temperature under 2 kW power, obtains cube Phase Ca2Ge base thermoelectricity materials.
The room temperature electrical property comparison of the different embodiment samples of table 1
The foregoing is merely presently preferred embodiments of the present invention, and all equivalent changes done according to scope of the present invention patent are with repairing Decorations should all belong to the covering scope of the present invention.

Claims (5)

1. a kind of cubic phase Ca of Sb doping2The preparation method of Ge base thermoelectricity materials, it is characterised in that：Include the following steps：
（1）In molar ratio 70:33:(0.3 ~ 2) weighs Ca powder, Ge powder and Sb powder respectively, is then poured into organic solvent, surpasses 20 ~ 60 min of sonication is allowed to be sufficiently mixed；
（2）Treat step（1）After organic solvent volatilization completely in gained mixed liquor, using dry process for forming by it in a level pressure Idiosome is pressed under power；
（3）Gained idiosome is placed in alumina crucible, and with Ca powder packings, is then placed into microwave vacuum high-temperature heater It is interior, high-purity argon gas is passed through, 400 ~ 700 DEG C are warming up under the conditions of 2.45 GHz of microwave frequency, 1.5 ~ 3.5 kW of microwave power；
（4）After temperature reaches, 0.5 ~ 6 h of isothermal holding, then cools to material with the furnace room under 1.5 ~ 2.5 kW power Temperature obtains the cubic phase Ca of the Sb doping2Ge base thermoelectricity materials.
2. the cubic phase Ca of Sb doping according to claim 12The preparation method of Ge base thermoelectricity materials, it is characterised in that：Step Suddenly（1）In organic solvent used be ethyl alcohol.
3. the cubic phase Ca of Sb doping according to claim 12The preparation method of Ge base thermoelectricity materials, it is characterised in that： Step（2）In be that volatile organic solvent to after dry, is pressed under 20 ~ 60 Mpa pressure under 25 ~ 60 DEG C of environment by mixed liquor The cylindrical idiosome of 10 ~ 60 mm of Φ.
4. the cubic phase Ca of Sb doping according to claim 12The preparation method of Ge base thermoelectricity materials, it is characterised in that：Step Suddenly（3）The purity of middle argon gas is 99% ~ 99.99%.
5. the cubic phase Ca that Sb made from a kind of method as described in claim 1 is adulterated2Ge base thermoelectricity materials.
CN201810070316.6A 2018-01-24 2018-01-24 Sb-doped cubic phase Ca2Ge-based thermoelectric material and preparation method thereof Expired - Fee Related CN108218425B (en)

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CN106116587A (en) * 2016-06-22 2016-11-16 福州大学 A kind of Emission in Cubic Ca2si thermoelectric material and preparation method thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
JPS5879220A (en) * 1981-11-05 1983-05-13 Nec Corp Liquid crystal light valve
CN104591299A (en) * 2015-01-16 2015-05-06 郑州大学 Microwave sintering synthesis method of oxide thermoelectric material Ca3-xKxCo4O9
CN106116587A (en) * 2016-06-22 2016-11-16 福州大学 A kind of Emission in Cubic Ca2si thermoelectric material and preparation method thereof

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Title
JUN-ICHI TANI等: "Investigation of structural,elastic,and lattic-dynamical properties of Ca2Si，Ca2Ge,and Ca2Sn based on first-principles density functional theory", 《COMPUTATIONAL MATERIALS SCIENCE》 *
RAFAEL SANTOS等: "Effect of the Fabrication Technique on the Thermoelectric Performance of Mg-Based Compounds-A Case Study of n-Type Mg2Ge", 《ACS OMEGA》 *
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