CN105895796A - Preparation method of CuGaX2/ multilayer nano graphene sheet composite material - Google Patents
Preparation method of CuGaX2/ multilayer nano graphene sheet composite material Download PDFInfo
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
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- H—ELECTRICITY
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- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
Abstract
The invention provides a preparation method of a CuGaX2/ multilayer nano graphene sheet composite material. The method comprises the following steps: grinding a pure-phase copper-based compound CuGaX2 into powder, wherein CuGaX2 is CuGaSySezTe2-y-z, y is more than or equal to 0 and less than or equal to 2, z is more than or equal to 0 and less than or equal to 2, and y+z is is more than or equal to 0 and less than or equal to 2; preparing 0.01-0.5g/L organic solvent suspension from multilayer nano graphene sheets; weighing a predetermined amount of CuGaX2 powder, adding the powder into the suspension, and heating the suspension at 50-80 DEG C while stirring for vaporizing; and performing hot pressing and sintering molding on the composite powder heated and dried by vaporization at 300-500 DEG C and under the pressure of 100-500MPa. The preparation method reduces the band gap width of the composite material, improves the efficiency of carrier transport, and improves the electrical conductivity, particularly thermal conductivity nearby room temperature, so that the thermoelectric potential of the composite material is improved within the temperature interval of room temperature to 600 DEG C, and the thermoelectric performance of the composite material is finally improved. The reaction condition in the preparation method is mild, the temperature is easy to control, the physical phase of the composite material is uniform, and the preparation method is easy to implement and facilitates large-scale production.
Description
Technical field
The present invention relates to thermoelectric composite material, especially relate to a kind of CuGaX2The preparation method of/multi-layer nano graphite flake composite.
Background technology
Thermoelectric material is a kind of functional material directly heat energy and electric energy mutually converted, heat energy is converted into electric energy by the Seebeck effect of its utilization itself, have noiseless, volume is little, reliability is high and without advantages such as drive disk assemblies, except applying in addition to space industry, space power system, generate electricity at waste heat, vehicle exhaust, the field such as underground heat also has the biggest potentiality, in the modern society of energy growing tension, the exploitation of thermoelectric material is increasingly given sufficient attention.
The conversion efficiency of thermoelectric of thermoelectric material is characterized by a dimensionless group ZT, and wherein T is temperature, and Z is referred to as thermoelectric figure of merit or quality factor (figure of merit), and it with the physical function parameter relation of material is:
ZT=S2QT/K
In formula, S is thermoelectric power (Seebeck coefficient), and Q is electrical conductivity, and T is absolute temperature, K=Kc+KL(KcFor the thermal conductance of carrier contribution, KLLattice or phonon thermal conductivity) it is material total heat conductance.From the expression formula of Z, the conversion efficiency of thermoelectric of thermoelectric material to be improved, high S, σ value should be selected, the material of low k, but these three physical quantity is mutually restriction, because being to be determined by the scattering of the inherent carrier concentration of material, electronic band structure and electronics or hole in these three quality entity.At present, thermoelectric figure of merit is higher and applies wide thermoelectric material mainly to have materials such as Tellurobismuthite., lead telluride, filled-type skutterudite and cage compound, but these materials contain heavy metal or relatively costly mostly, and large-scale production difficulty is bigger.
Research shows to add up compound CuGaX2It is the arrowband based semiconductor material with yellow copper structure, there is higher Seebeck coefficient.Yellow copper structure has three metaclass zincblende lattce structures it is considered to be the superlattice structure of sphalerite.Arrowband system energy gap makes electronics (hole) be easier to be energized into the energy of valence band (conduction band) from conduction band (valence band), has higher electrical conductivity.Owing to X atom is in by the tetrahedron space of Cu, Ga atomic building, tetrahedral structure makes it show big carrier mobility, and due to tetrahedron Atom spacing and electronegativity difference, this tetrahedral structure has certain distortion, contribute to heat-carrying phon scattering so that it is there is the most relatively low thermal conductivity.In recent years, yellow copper structure compound receives more and more attention because it has relatively high thermoelectricity capability.But it is up to the present little for promoting the research report of CuGaX2 thermoelectricity capability.
Summary of the invention
In view of this, it is provided that a kind of CuGaX2The preparation method of/multi-layer nano graphite flake composite, this preparation method technique is simple, and reaction condition gentleness is easily controllable, and compound phase is uniformly dispersed, and the thermoelectricity capability of material is good.
A kind of CuGaX2/ multi-layer nano graphite flake composite material and preparation method thereof, it uses solvent-thermal process method and hot-pressing sintering method to make, comprises the following steps:
(1) by the copper-based compound CuGaX of pure phase2Grind into powder；
(2) multi-layer nano graphite flake is configured to the outstanding mixed liquid of organic solvent, and its concentration is 0.01-0.5g/L；
(3) by step (1) the gained CuGaX of scheduled volume2Powder joins in the outstanding mixed liquid of step (2) gained, stirs and heats and is evaporated into powder；Wherein CuGaX2The scheduled volume of powder is 2-20g, and heating-up temperature is 50-80 DEG C, it is thus achieved that CuGaX2/ x wt. %G composite, wherein, G represents multi-layer nano graphite flake, and x represents multi-layer nano graphite flake weight/mass percentage composition in the composite, 0 ＜ x≤0.56；
(4) step (3) is evaporated after gained composite powder grinds hot-forming in loading hot pressing die；Wherein hot pressing temperature is 300-500 DEG C, and pressure is 100-500MPa.
Preferably, described copper-based compound CuGaX2For CuGaSySezTe2-y-z, wherein, 0≤y≤2,0≤z≤2,0≤y+z≤2.
Preferably, described copper-based compound CuGaX2For CuGaTe2。
Preferably, described CuGaX2The architectural feature of/multi-layer nano graphite flake composite is:
1) in this composite, compound phase is multi-layer nano graphite flake, and percentage is 0.14-0.56wt. %, and matrix is CuGaX2/ multi-layer nano graphite flake composite；
2) described CuGaX2The particle size of/multi-layer nano graphite flake composite is between 10 nanometers to 10 micron.
Preferably, in described composite, the addition of multi-layer nano graphite flake is CuGaX2The 0.42wt. % of/multi-layer nano graphite flake composite.
Preferably, described multi-layer nano graphite flake thickness be 2-20 nanometer, length or width be 10-50 micron, its number of plies is 2-30 layer.
Preferably, the one during described organic solvent is ethanol or acetone.
Preferably, the mode that is evaporated described in is the one in water-bath or oil bath.
Preferably, in described composite, the content of multi-layer nano graphite flake is CuGaX2The 0.42-0.56wt. % of/x wt. %G composite.
Preferably, described hot pressing die is sintered-carbide die.
Above-mentioned CuGaX2The preparation method of/multi-layer nano graphite flake composite includes the steps such as preparation of raw material, solvent-thermal process method and hot-pressing sintering method, utilizes the outstanding mixed liquid of the organic solvent being configured to use solution thermal synthesis method to prepare CuGaX as raw material2/ multi-layer nano graphite flake composite material powder, multi-layer nano graphite flake evenly spreads in matrices of composite material material, gives full play to nano-scale effect and the excellent heat electrical property of multi-layer nano graphite flake, and recycling hot pressing and sintering technique is by CuGaX2/ x wt. %G powder body is hot-forming, so that the thermoelectricity capability of composite gets a promotion, hot pressing temperature controls at 300-500 DEG C, and reaction condition gentleness is easily controllable, beneficially large-scale production and the realization of processing.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, the accompanying drawing used required in embodiment will be briefly described below, it is to be understood that, the following drawings illustrate only certain embodiments of the present invention, therefore the restriction to scope it is not construed as, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain other relevant accompanying drawings according to these accompanying drawings.
Fig. 1 is CuGaX2Pure phase powder and CuGaTe2 / x wt.
The thermal conductivity variation with temperature curve chart of %G (wherein x=0.14,0.28,0.42,0.56, G is multi-layer nano graphite flake).
Fig. 2 is CuGaX2Pure phase powder and CuGaTe2 / x wt.
The thermoelectrical potential variation with temperature curve chart of %G (wherein x=0.14,0.28,0.42,0.56, G is multi-layer nano graphite flake).
Fig. 3 is CuGaX2Pure phase powder and CuGaTe2 / x wt.
The thermoelectric figure of merit ZT variation with temperature curve chart of %G (wherein x=0.14,0.28,0.42,0.56, G is multi-layer nano graphite flake) composite.
Fig. 4 is CuGaX2Pure phase powder and CuGaX2/ x wt. %G(x=0.42, G are multi-layer nano graphite flake) composite XRD figure spectrum.
Fig. 5 is CuGaX2/ x wt. %G(x=0.56, G are multi-layer nano graphite flake) transmission electron microscope picture of composite.
Fig. 6 is CuGaX2/x wt. %
G(x=0.56, G are multi-layer nano graphite flake) scanning electron microscope diagram of composite.
Detailed description of the invention
Below by way of instantiation and accompanying drawing, the present invention is described.
A kind of CuGaX2/ multi-layer nano graphite flake composite material and preparation method thereof, it uses solvent-thermal process method and hot-pressing sintering method to make, comprises the following steps:
(1) by the copper-based compound CuGaX of pure phase2Grind into powder；
(2) it is the outstanding mixed liquid of 0.01-0.5g/L organic solvent that multi-layer nano graphite flake is configured to concentration；
(3) by step (1) gained CuGaX that scheduled volume is 2-20g2Powder joins in the outstanding mixed liquid of step (2) gained, and stirs in the heating-up temperature of 50-80 DEG C and heat and be evaporated into powder；
(4) step (3) being evaporated after gained powder mull and load in hot pressing die, be 300-500 DEG C in hot pressing temperature, pressure is hot-forming under the conditions of 100-500MPa.
In step (1), described copper-based compound CuGaX2For CuGaSySezTe2-y-z(wherein 0≤y≤2,0≤z≤2,0≤y+z≤2).
Described CuGaX2/ multi-layer nano graphite flake composite, its architectural feature is:
1) chemical general formula is CuGaX2/ x G, wherein compound phase is multi-layer nano graphite flake, and percentage is 0.14,0.28,0.42,0.56wt. %, and matrix is CuGaX2/ multi-layer nano graphite flake composite, G is multi-layer nano graphite flake；
2) described CuGaX2/ multi-layer nano graphite flake composite, multi-layer nano graphite flake is homogeneously dispersed in CuGaX2In/multi-layer nano graphite flake composite；
3) described CuGaX2The particle size of/multi-layer nano graphite flake composite is between tens nanometers and several microns.
Wherein the addition of multi-layer nano graphite flake preferably accounts for CuGaX2During the 0.42wt. % of/multi-layer nano graphite flake composite, gained CuGaX2The thermoelectricity capability of/multi-layer nano graphite flake composite is optimal, such as, and CuGaTe2The thermoelectric figure of merit of/multi-layer nano graphite flake composite is compared to pure phase CuGaTe2 ZT value lifting 21%.
It is 10-50 micron that described multi-layer nano graphite flake thickness is preferably 2-20 nanometer, length or width, and its number of plies is 2-30 layer.Described organic solvent is the one in ethanol or acetone.The described mode that is evaporated is the one in water-bath or oil bath.Described hot pressing die is sintered-carbide die.
In view of S, Se, Te belong to congeners, and they constitute CuGaX2The chemical constitution of type is mutually the most similar with performance, describes the idiographic flow of the preparation method of the thermoelectric composite material of the present invention below as a example by Te in detail, and the aspect such as the performance describing thermoelectric material prepared by the method, containing CuGaS2、CuGaSe2Or CuGaX2Doping S, the preparation method of the thermoelectric composite material of Se, Te element compound, with reference to specific examples below, does not repeats them here.
Fig. 1 is pure phase CuGaTe2Powder and CuGaX2/ x wt. %G(x=0.14,0.28,0.42,0.56) thermoelectrical potential of composite.Seebeck coefficient be on the occasion of, illustrate that this material is P-type semiconductor.Additionally, the CuGaTe of pure phase2Rise linearly along with the rising of temperature in the range of 300K to 750K, increase slowly along with the continuation of temperature rises thermoelectrical potential value.It addition, the thermoelectrical potential S value that with the addition of the composite of multi-layer nano graphite flake is all higher than the CuGaTe of pure phase2S value.The S value of the multi-layer nano graphite flake composite of Different adding amount is because impedance behavior difference is less.
Fig. 2 is pure phase CuGaTe2Powder and CuGaX2/ x wt. %G(x=0.14,0.28,0.42,0.56) thermal conductivity.In whole temperature range, K value declines along with the rising of temperature.
Fig. 3 is pure phase CuGaTe2Powder and CuGaX2/ x wt. %G(x=0.14,0.28,0.42,0.56) thermoelectric figure of merit Z.Along with the rising of temperature, the ZT value of composite rises along with the rising of temperature, and higher than the ZT value of pure phase.When the content of the multi-layer nano graphite flake added is CuGaTe20.42wt. % time, when 873K, Z value reaches peak 0.93, compared to pure phase CuGaTe2 ZT value lifting 21%.
Embodiment 1
By the copper-based compound CuGaTe of pure phase2Grind into powder is standby.Thickness is 10 nanometers, and width is 10 microns, and the number of plies is that to be configured to concentration be that the outstanding mixed liquid of 0.01g/L organic solvent is standby for the multi-layer nano graphite flake of 10 layers, and described organic solvent is preferably ethanol.Weigh the standby CuGaTe of 2g2Powder joins in the standby outstanding mixed liquid of 32.5mL, is sufficiently stirred for and heats being evaporated, and the mode of being evaporated is water-bath, and heating-up temperature is 60 DEG C.To be evaporated loading hot pressing die after gained powder is fully ground, hot pressing condition is 350 DEG C, and 300MPa is hot pressed into block.Hot pressing gained block is cut into by demand the sample being available for thermoelectricity capability test.
Embodiment 2
By the copper-based compound CuGaTe of pure phase2Grind into powder is standby.Thickness is 10 nanometers, and width is 10 microns, and the number of plies is that to be configured to concentration be that the outstanding mixed liquid of 0.2g/L organic solvent is standby for the multi-layer nano graphite flake of 10 layers, and described organic solvent is preferably ethanol.Weigh the standby CuGaTe of 8g2Powder joins in the standby outstanding mixed liquid of 15.5mL, is sufficiently stirred for and heats being evaporated, and the mode of being evaporated is water-bath, and heating-up temperature is 60 DEG C.To be evaporated loading hot pressing die after gained powder is fully ground, hot pressing condition is 350 DEG C, and 300MPa is hot pressed into block.Hot pressing gained block is cut into by demand the sample being available for thermoelectricity capability test.
Embodiment 3
By the copper-based compound CuGaTe of pure phase2Grind into powder is standby.Thickness is 10 nanometers, and width is 10 microns, and the number of plies is that to be configured to concentration be that the outstanding mixed liquid of 0.4g/L organic solvent is standby for the multi-layer nano graphite flake of 10 layers, and described organic solvent is preferably ethanol.Weigh the standby CuGaTe of 14g2Powder joins in the standby outstanding mixed liquid of 25.3mL, is sufficiently stirred for and heats being evaporated, and the mode of being evaporated is water-bath, and heating-up temperature is 60 DEG C.To be evaporated loading hot pressing die after gained powder is fully ground, hot pressing condition is 350 DEG C, and 300MPa is hot pressed into block.Hot pressing gained block is cut into by demand the sample being available for thermoelectricity capability test.
Fig. 4 is the copper-based compound CuGaTe of pure phase2Pure phase powder and CuGaX2/ x wt. %G(x=0.42) the XRD diffracting spectrum of composite.The all CuGaTe of diffraction maximum2Diffraction maximum, owing to multi-layer nano graphite flake amount is relatively fewer, XRD collection of illustrative plates does not finds its diffraction maximum, without other impurity diffraction maximum yet.
Embodiment 4
By the copper-based compound CuGaTe of pure phase2Grind into powder is standby.Thickness is 10 nanometers, and width is 10 microns, and the number of plies is that to be configured to concentration be that the outstanding mixed liquid of 0.5g/L organic solvent is standby for the multi-layer nano graphite flake of 10 layers, and described organic solvent is preferably ethanol.Weigh the standby CuGaTe of 20g2Powder joins in the standby outstanding mixed liquid of 50.9mL, is sufficiently stirred for and heats being evaporated, and the mode of being evaporated is water-bath, and heating-up temperature is 60 DEG C.To be evaporated loading hot pressing die after gained powder is fully ground, hot pressing condition is 350 DEG C, and 300MPa is hot pressed into block.Hot pressing gained block is cut into by demand the sample being available for thermoelectricity capability test.
Fig. 5 is CuGaTe2Pure phase powder and CuGaX2/ x wt. %G(x=0.56) the transmission picture of composite, the size of crystal grain is between nanometer and several microns, and the interpolation of multi-layer nano graphite flake adds the interface scattering of phonon, reduces the thermal conductivity of material.
Fig. 6 is CuGaTe2Pure phase powder and CuGaX2/ x wt. %G(x=0.56) the sem observation picture of composite, during multi-layer nano graphite flake evenly spreads to the matrix material of yellow copper structure as can be seen from Fig..
The above; being only a kind of detailed description of the invention of invention, but protection scope of the present invention is not limited thereto, any those familiar with the art is in the technical scope that the invention discloses; change can be readily occurred in or replace, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with described scope of the claims.
Claims (10)
1. a CuGaX2/ multi-layer nano graphite flake composite material and preparation method thereof, it uses solvent-thermal process method and hot-pressing sintering method to make, comprises the following steps:
(1) by the copper-based compound CuGaX of pure phase2Grind into powder；
(2) multi-layer nano graphite flake is configured to the outstanding mixed liquid of organic solvent, and its concentration is 0.01-0.5g/L；
(3) by step (1) the gained CuGaX of scheduled volume2Powder joins in the outstanding mixed liquid of step (2) gained, stirs and heats and is evaporated into powder；Wherein CuGaX2The scheduled volume of powder is 2-20g, and heating-up temperature is 50-80 DEG C, it is thus achieved that CuGaX2/ x wt. %G composite, wherein, G represents multi-layer nano graphite flake, and x represents multi-layer nano graphite flake weight/mass percentage composition in the composite, 0 ＜ x≤0.56；
(4) step (3) is evaporated after gained composite powder grinds hot-forming in loading hot pressing die；Wherein hot pressing temperature is 300-500 DEG C, and pressure is 100-500MPa.
2. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described copper-based compound CuGaX2For CuGaSySezTe2-y-z, wherein, 0≤y≤2,0≤z≤2,0≤y+z≤2.
3. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described copper-based compound CuGaX2For CuGaTe2。
4. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described CuGaX2The architectural feature of/multi-layer nano graphite flake composite is:
In this composite, compound phase is multi-layer nano graphite flake, and percentage is 0.14-0.56 wt. %, and matrix is CuGaX2/ multi-layer nano graphite flake composite；
Described CuGaX2The particle size of/multi-layer nano graphite flake composite is between 10 nanometers to 10 micron.
5. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that in described composite, the addition of multi-layer nano graphite flake is CuGaX20.42 wt.% of/multi-layer nano graphite flake composite.
6. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described multi-layer nano graphite flake thickness be 2-20 nanometer, length or width be 10-50 micron, its number of plies is 2-30 layer.
7. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described organic solvent is the one in ethanol or acetone.
8. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described in be evaporated mode be the one in water-bath or oil bath.
9. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that in described composite, the content of multi-layer nano graphite flake is CuGaX2The 0.42-0.56wt. % of/multi-layer nano graphite flake composite.
10. according to the CuGaX described in claim 12/ multi-layer nano graphite flake composite material and preparation method thereof, it is characterised in that described hot pressing die is sintered-carbide die.
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Application publication date: 20160824 |