CN104446575B - A kind of activeness and quietness thermoelectric composite material and preparation method thereof - Google Patents
A kind of activeness and quietness thermoelectric composite material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of activeness and quietness thermoelectric composite material and preparation method thereof, the composite is made up of thermoelectric material matrix and the activeness and quietness material being dispersed in the thermoelectric material matrix, wherein described activeness and quietness material is fiber and/or whisker, and volume fraction is 0.1%~30%.The present invention improves the mechanical property of thermoelectric material using fiber or crystal whisker reinforced and toughened method.Not only its mechanical property has obtained significant raising to the fiber or crystal whisker reinforced and toughened thermoelectric composite material that the present invention is obtained, and the introducing of fiber or whisker also improves the thermoelectricity capability of composite in right amount.
Description
Technical field
The present invention relates to a kind of method of activeness and quietness thermoelectric material mechanical property and its thermoelectric composite material, belong to thermoelectricity
Material Field.
Background technology
Bismuth telluride based alloys have been always the optimal heat to electricity conversion of near room temperature performance since the fifties is found from last century
Material, this material is widely used in thermoelectric cooling field, such as automobile air-conditioning seat and environment-friendly type refrigerator.In recent years,
Along with the development of nanometer technology and material preparation technology etc., researcher bismuth telluride-base material electrical transmission performance optimization and
Substantial amounts of research has all been carried out in terms of the reduction of heat conveyance performance.It is reported that passing through doping, low-dimensional and the means such as nano combined
The thermoelectricity capability of p-type and n-type bismuth telluride-base material is set to be obtained for very big raising, the thermoelectric figure of merit of p-type material is even
Reach 1.4（B.Poudel,Q.Hao,Y.Ma,Y.C.Lan,A.Minnich,B.Yu,X.Yan,D.Z.Wang,A.Muto,
D.Vashaee,X.Y.Chen,J.M.Liu,M.S.Dresselhaus,G.Chen,Z.F.Ren,High-Thermoelectric
Performance of Nanostructured Bismuth Antimony Telluride Bulk Alloys,
Science320,634-638(2008)；X.F.Tang,W.J.Xie,H.Li,W.Y.Zhao,Q.J.zhang,M.Niino,
Preparation and thermoelectric transport properties of high-performance p-
type Bi2Te3with layered nanostructure,Appl.Phys.Lett.90012102(2007)；F.Li,
X.Y.Huang,Z.L.Sun,J.Ding,J.Jiang,W.Jiang,L.D.Chen,Enhanced thermoelectric
properties of n-type Bi2Te3-based nanocomposite fabricated by spark plasma
sintering,J Alloys Compd.509,4769-4773(2011)）.The material used in bismuth telluride-based thermoelectric device leads to
It is often using bismuth telluride-base crystal bar material made from zone-melting process or Bridgman method.This material is due between Te (1)-Te (1)
Combined with weaker Van der Waals force and easily occur cleavage along perpendicular to the adjacent Te atomic layers in (00l) face especially two of C axles, from
And make its mechanical strength very low（Fig. 1）.The low mechanical property of bismuth telluride-base material necessarily affects the machinability and member of material
The use reliability of device, reduction bismuth telluride-based thermoelectric device and the competitiveness of tradition machinery Refrigeration Technique, will also limit it
As the application of Thermoelectric Generator, especially as the core of the tail gas of the car generation device used in vibration environment
Part.
In recent years, SiC fibers are all used as activeness and quietness material in many research and are introduced into different materials system.
The introducing of SiC fibers can many carbon interfaces formed in situ, this will be greatly enhanced the fracture toughness of composite.Typically recognize
For the toughening mechanisms of fiber have following three kinds：The bridging toughness reinforcing of the extraction toughness reinforcing of fiber, fibre debonding toughness reinforcing and fiber.To mesh
Before untill, it is fiber reinforced to be widely used in multiple material system, such as structural ceramics, plastics and concrete
In.Heat treated SiC fibers are introduced into sialon by Adem etc., obtained composite bending strength and disconnected
Splitting toughness has significant raising (D.Adem, P.Derek, High performance SiC-fiber reinforced
CMCS prepared from heat treated nicalon fibers,Journal of the European
Ceramic Society,21(2001)639-647)；Yang etc. is prepared for the short fibres of SiC using the method for traditional hot pressed sintering
Tie up the ZrB of activeness and quietness2- SiC ceramic matrix composite material, have studied after fiber is introduced to material microstructure, mechanical property and anti-oxidant
The influence of property, obtained fracture of composite materials toughness improve about 50% (F.Y.Yang, X.H.Zhang,
Characterization of hot-pressed short carbon fiber reinforced ZrB2–SiC ultra-
high temperature ceramic composites,Journal of alloys and compounds,472(2009)
395-399).Up to the present, the research and development of thermoelectric material are still wholly constrained to thermoelectricity capability sheet, to the work of thermoelectric material
Material strength problem that can be potentially encountered in journeyization application etc. lacks targetedly system research.Although passing through device
Design and integrated technology improvement can partly make up because thermoelectric material mechanical strength it is too low caused by device reliability not
Foot, but certainly, the use of the thermoelectric material of strong mechanical performance will significantly improve the use reliability of device.And by SiC
The activeness and quietness material such as fiber is introduced into thermoelectric material to be still rarely reported so far with improving its mechanical property.
The content of the invention
The purpose of the present invention be for the low deficiency of existing high performance thermoelectric material mechanical property, using plus fiber or
The method of person's crystal whisker excess weld metal and toughness reinforcing, optimizes the thermoelectricity capability of material while thermoelectricity matrix material mechanical property is improved.With
Exemplified by bismuth telluride material, the present inventor it has been investigated that, the bismuth telluride-base that uses in prepared by bismuth telluride-based thermoelectric device
Material mechanical performance is poor, by introducing the activeness and quietness materials such as SiC fibers in bismuth telluride-base thermoelectric material, and combines electric discharge
The hot-pressing technique of plasma sintering etc., can prepare the fine and close bismuth telluride-base composite block material of high-performance.
Herein, on the one hand, the present invention provides a kind of thermoelectric composite material, and the composite is by thermoelectric material matrix and
It is even be scattered in the thermoelectric material matrix activeness and quietness material composition, wherein the activeness and quietness material be fiber and/or
Whisker, volume fraction is 0.1%~30%.
The present invention improves the mechanical property of thermoelectric material using fiber or crystal whisker reinforced and toughened method.Of the invention
To fiber or crystal whisker reinforced and toughened thermoelectric composite material not only its mechanical property has obtained significant raising, it is and appropriate fine
The introducing of dimension or whisker also improves the thermoelectricity capability of composite.
Preferably, the volume fraction of the activeness and quietness material is 0.3%~5%.
It is preferred that the thermoelectric material can be BiTe sills, filling or doping CoSb3Sill, PbTe base materials
Material, ZrNiSn base half-Heusler materials, SiGe solid solution, CaMnO3Solid solution and Ca3Co4O9It is any one in solid solution
Kind.
It is preferred that the activeness and quietness material can be SiC fibers, fiber C, alumina fibre, Zirconium oxide fibre, Mo Lai
At least one of mineral wool, SiC whiskers, alumina whisker, zirconium oxide whisker and mullite crystal whisker.
Mechanical property such as hardness, Young's modulus, mechanical strength and the fracture toughness of the thermoelectric composite material of the present invention are complete
Portion or most of thermoelectric material matrix for being higher than the thermoelectric composite material.
The ratio between the Vickers hardness of heretofore described composite and Vickers hardness of the thermoelectric material can be（1.0~
1.15）：1.
The ratio between the Young's modulus of heretofore described composite and Young's modulus of the thermoelectric material can be（1.0~
2.15）：1.
The ratio between the fracture toughness of heretofore described composite and fracture toughness of the thermoelectric material can be（1.0~
1.15）：1.
The thermoelectricity capability of the thermoelectric composite material of the present invention is higher than the thermoelectric material matrix of the thermoelectric composite material.
The maximum thermoelectricity of the maximum thermoelectric figure of merit and the thermoelectric material of the synthermal lower composite is excellent in the present invention
The ratio between value can be（0.5~1.2）：1.
On the other hand, the present invention also provides a kind of preparation method of the thermoelectric composite material, including：By the thermoelectricity material
Material matrix powder is well mixed by the volume fraction with the activeness and quietness material and composite granule is made；Using plasma discharging
Sintering or hot pressed sintering the composite granule are made the block materials of densification；And carry out the block materials at annealing
Manage to eliminate thermal stress.
The preparation method technique of the present invention is simple, is suitable for large-scale production.
It is preferred that the sintering temperature of the discharge plasma sintering can be 653~713K, sintering pressure can for 30~
100MPa, sintering time can be 3~10 minutes.
It is preferred that the sintering temperature of the hot pressed sintering can be 613~873K, sintering pressure can for 20~
100MPa, sintering time can be 3~100 minutes.
It is preferred that the annealing can be handled 1~72 hour in 500~800K.
Brief description of the drawings
Fig. 1 is bismuth telluride-base thermoelectric material structure chart；
Fig. 2 is Bi2Se0.3Te2.7+ 1vol%SiC composite sections SEM（ESEM）Figure；
Fig. 3 is Bi2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) composite Vickers hardness variation diagram；
Fig. 4 is Bi2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) composite Young's modulus variation diagram；
Fig. 5 is Bi2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) fracture of composite materials change in toughness figure；
Fig. 6 is Bi2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) composite thermoelectric figure of merit varies with temperature relation
Figure.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiments, it should be appreciated that following drawings and embodiments
The present invention is merely to illustrate, is not intended to limit the present invention.
The present invention provides a kind of thermoelectric composite material, and its composition formula may be defined as TE/z vol.%M, wherein, TE is thermoelectricity
Material, M is activeness and quietness material, and z vol.% are the volume fractions that the activeness and quietness material M accounts for thermoelectric material TE, wherein,
0.1≤z≤30, preferably 0.3≤z≤5.
Thermoelectricity matrix material used in the present invention, can be BiTe sills, filling or doping CoSb3Sill,
PbTe sills, ZrNiSn base half-Heusler materials, SiGe solid solution, CaMnO3Solid solution and Ca3Co4O9Solid solution etc.
In one kind.
The introduced fiber or crystal whisker reinforced and toughened material of the present invention, can be SiC fibers, fiber C, alumina fibre,
It is a kind of or many in Zirconium oxide fibre, mullite fiber, SiC whiskers, alumina whisker, zirconium oxide whisker and mullite crystal whisker etc.
Kind.
Mechanical property such as hardness, Young's modulus, mechanical strength and the fracture toughness of the thermoelectric composite material of the present invention are complete
Portion or most of matrix for being higher than the thermoelectric composite material.
In an example embodiment, the ratio between the Vickers hardness of the composite and Vickers hardness of its matrix can be
（1.0~1.15）：1.
In another example embodiment, the ratio between the Young's modulus of the composite and Young's modulus of its matrix can be
（1.0~2.15）：1.
In another example embodiment, the fracture toughness of the composite and the fracture toughness of its matrix are than being
（1.0~1.15）：1.
The thermoelectricity capability of the thermoelectric composite material of the present invention is higher than the matrix material of the thermoelectric composite material.
In an example embodiment, the maximum heat of the maximum thermoelectric figure of merit of the synthermal lower composite and its matrix
The ratio between electric figure of merit can be（0.5~1.2）：1.
The present invention also provides a kind of preparation method of the thermoelectric composite material, including：By the thermoelectric material matrix powder
Body is well mixed by the volume fraction with the activeness and quietness material and composite granule is made；Using discharge plasma sintering or
Hot pressed sintering the composite granule is made the block materials of densification；And made annealing treatment the block materials to eliminate
Thermal stress.
Specifically, the present invention may comprise steps of：
A, the thermoelectric material powder for weighing appropriate quality first；
B, the proportion according to activeness and quietness material, weigh the activeness and quietness fiber or whisker of appropriate quality, so that enhancing
The volume fraction that toughening material accounts for thermoelectric material is 0.1%~30%；
C, fiber or whisker be well mixed with thermoelectric material powder；
D, the block materials that homogeneous mixture is made to using discharge plasma sintering or hot pressed sintering densification；
E, the block materials being made are made annealing treatment to eliminate thermal stress.
In step a, the thermoelectric material can be prepared by method commonly used in the art.For example, in an example reality
Apply in example, bismuth telluride-base crystal bar material can be prepared by the method for growing by zone melting crystal., can in another example embodiment
To prepare Ce by melting annealing process0.9Fe4Sb12Skutterudite-base thermoelectrical material.Also, the thermoelectric material for example can be led to
Cross and pulverize and sieve obtained powder.
In step c, mixed method is not limited, and the mode such as can use mechanical mixture is well mixed.
In step d, the sintering temperature of the discharge plasma sintering can be 653~713K, sintering pressure can for 30~
100MPa, sintering time can be 3~10 minutes.The sintering temperature of the hot pressed sintering can be 613~873K, and sintering pressure can be
20~100MPa, sintering time can be 3~100 minutes.
In step e, the annealing can be handled 1~72 hour in 500~800K.
Strengthen the method and its corresponding thermoelectric composite material of thermoelectric material mechanical property the invention provides a kind of, it is most
Big the characteristics of, is the mechanical property that thermoelectric material is improved using fiber or crystal whisker reinforced and toughened method.The present invention is obtained
Fiber or crystal whisker reinforced and toughened thermoelectric composite material not only its mechanical property has obtained significant raising, and appropriate fiber
Or the introducing of whisker also improves the thermoelectricity capability of composite.
Illustrate the substantive distinguishing features of the present invention and significant progress with reference to specific embodiment.It should be understood that these realities
Example is applied to be served only for that the present invention is further described, and it is not intended that limiting the scope of the invention, this area
Some nonessential modifications and adaptations that technical staff makes according to the above of the present invention belong to the protection model of the present invention
Enclose.The experimental method of unreceipted actual conditions in the following example, generally according to normal condition, the bar e.g. in workshop manual
Part, or according to the condition proposed by manufacturer.
Embodiment 1
The method melted first with area prepares n-type Bi2Se0.3Te2.7Bismuth telluride-base crystal bar material, by crystal bar material disintegrating
Sieving obtains bismuth telluride-base powder, and powder and commercially available SiC fibre machineries uniformly are being obtained into composite granule, in conjunction with putting
The method of electro-plasma sintering sinters the block materials for obtaining densification in a vacuum, and sintering temperature is 713K, and pressure is
60MPa, is incubated 10 minutes, that is, has obtained fibre-reinforced bismuth telluride-based thermoelectric composite.
Fig. 2 is Bi manufactured in the present embodiment2Se0.3Te2.7The stereoscan photograph of+1vol%SiC composite sections
(SEM), it can be found that fracture shows as obvious spike protein gene mechanism from section picture, illustrates that the introducing of fiber is served and carry
The effect of strong mechanical performance.
Fig. 3 is Bi manufactured in the present embodiment2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) composite Vickers hardness with
The graph of a relation of fiber introduction volume change.When it is 1% to introduce SiC fiber volume fractions, the hardness of composite has reached maximum
Value, improves 15% compared with matrix material.
Fig. 4 is Bi manufactured in the present embodiment2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) composite Young's modulus with
The graph of a relation of fiber introduction volume change.When it is 1% to introduce SiC fiber volume fractions, the Young's modulus of composite reaches
Maximum.Compared with matrix material, there is significant raising.
Fig. 5 is Bi manufactured in the present embodiment2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) fracture of composite materials toughness with
The graph of a relation of fiber introduction volume change.When it is 1% to introduce SiC fiber volume fractions, the fracture toughness of composite reaches
Maximum.Compared with matrix material, fracture toughness has significant raising.
Fig. 6 is Bi manufactured in the present embodiment2Se0.3Te2.7+ x vol%SiC (x=0,1,3,5) composite thermoelectric figure of merit ZT
Vary with temperature graph of a relation.When it is 1% to introduce SiC fiber volume fractions, the thermoelectricity capability of composite has been obtained to a certain degree
Raising, in 400K, Bi2Se0.3Te2.7+ 1vol%SiC composites maximum ZT is 1.07, with synthermal lower substrate material
Maximum ZT is compared and is improved about 20%.
Embodiment 2
Ce is made first with traditional melting annealing process0.9Fe4Sb12Skutterudite-base thermoelectrical material, by skutterudite original washing powder
Body and commercially available fiber C machinery are uniformly mixed so as to obtain composite granule, in conjunction with hot pressed sintering method in 873K temperature, 60MPa
Insulation prepares the fibre-reinforced skutterudite-base thermoelectrical composite material of densification for 5 minutes under pressure.
When it is 1% to introduce fiber C volume fraction, Vickers hardness, Young's modulus and the fracture toughness of composite are obtained
Significant raising, compared with matrix material, Vickers hardness improves about 10%, and Young's modulus improves 15%, and fracture toughness is carried
It is high by 15%.And the Ce in 773K0.9Fe4Sb12It is 0.9 that+1vol%C composites, which have obtained maximum ZT, with synthermal lower substrate
The maximum ZT of material is compared and is improved about 10%.
Industrial applicability：The invention provides a kind of method of activeness and quietness thermoelectric material mechanical property and its thermoelectricity are compound
Material, fiber or whisker reinforcement thermoelectric composite material produced by the present invention, not only its mechanical property obtained significant raising,
And the introducing of appropriate fiber also improves the thermoelectricity capability of composite, can apply to thermo-electric device field.
Claims (11)
1. a kind of thermoelectric composite material, it is characterised in that the composite is by thermoelectric material matrix and is dispersed in described
Activeness and quietness material composition in thermoelectric material matrix, wherein the activeness and quietness material is fiber and/or whisker, volume fraction
For 0.1%~5%, the preparation method of the thermoelectric composite material includes：The thermoelectric material matrix powder is increased with the enhancing
Tough material is by the well mixed obtained composite granule of the volume fraction；Will be described using discharge plasma sintering or hot pressed sintering
The block materials of densification are made in composite granule；And made annealing treatment the block materials to eliminate thermal stress.
2. thermoelectric composite material according to claim 1, it is characterised in that the volume fraction of the activeness and quietness material is
0.3%~5%.
3. thermoelectric composite material according to claim 1, it is characterised in that the thermoelectric material is BiTe sills, filled out
Fill or the CoSb that adulterates3Sill, PbTe sills, ZrNiSn base half-Heusler materials, SiGe solid solution, CaMnO3Gu
Solution and Ca3Co4O9Any one in solid solution.
4. thermoelectric composite material according to claim 1, it is characterised in that the activeness and quietness material is SiC fibers, C
Fiber, alumina fibre, Zirconium oxide fibre, mullite fiber, SiC whiskers, alumina whisker, zirconium oxide whisker and mullite are brilliant
At least one of must.
5. thermoelectric composite material according to claim 1, it is characterised in that the Vickers hardness of the composite with it is described
The ratio between Vickers hardness of thermoelectric material is（1.0~1.15）：1.
6. thermoelectric composite material according to claim 1, it is characterised in that the Young's modulus of the composite with it is described
The ratio between Young's modulus of thermoelectric material is（1.0~2.15）：1.
7. thermoelectric composite material according to claim 1, it is characterised in that the fracture toughness of the composite with it is described
The ratio between fracture toughness of thermoelectric material is（1.0~1.15）：1.
8. thermoelectric composite material according to claim 1, it is characterised in that the maximum heat of the synthermal lower composite
The ratio between the electric figure of merit and maximum thermoelectric figure of merit of the thermoelectric material are（0.5~1.2）：1.
9. thermoelectric composite material according to claim 1, it is characterised in that the sintering temperature of the discharge plasma sintering
For 653~713K, sintering pressure is 30~100MPa, and sintering time is 3~10 minutes.
10. thermoelectric composite material according to claim 1, it is characterised in that the sintering temperature of the hot pressed sintering is 613
~873K, sintering pressure is 20~100MPa, and sintering time is 3~100 minutes.
11. thermoelectric composite material according to claim 1, it is characterised in that the annealing is at 500~800K
Reason 1~72 hour.
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