CN104671222B - A kind of Sb2te3the Self-propagating Sintering Synthetic method of base thermoelectricity material and combustion adjuvant thereof - Google Patents
A kind of Sb2te3the Self-propagating Sintering Synthetic method of base thermoelectricity material and combustion adjuvant thereof Download PDFInfo
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Abstract
The invention discloses a kind of Sb2Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material and combustion adjuvant thereof, it is with Sb, Te simple substance as raw material, uses In simple substance to promote Self-propagating Sintering Synthetic reaction as combustion adjuvant, prepares Sb2Te3Base thermoelectricity material powder.Present invention firstly discloses a kind of Self-propagating Sintering Synthetic Sb2Te3The combustion adjuvant In simple substance of base thermoelectricity material, promotes that raw material Sb, Te simple substance can occur Self-propagating Sintering Synthetic reaction to generate Sb2Te3Base thermoelectricity material, and combine discharge plasma sintering, prepare the Sb of densification2Te3Base block thermoelectric material, is improving while thermoelectricity capability, also has that preparation time is ultrashort, technique is simple, low for equipment requirements, energy-conserving and environment-protective, is suitable for the advantages such as large-scale production, for Sb2Te3The scale preparation of base thermoelectricity material and large-scale application are had laid a good foundation.
Description
Technical field
The invention belongs to technical field of new energy material preparation, be specifically related to Self-propagating Sintering Synthetic method and the combustion adjuvant thereof of a kind of Sb2Te3 base thermoelectricity material.
Background technology
Increasingly serious due to energy shortage and environmental pollution, studies and taps a new source of energy material and new forms of energy transformation technology becomes the focus of extensive concern the most in the world.Thermoelectric material is a kind of eco-friendly new energy materials, has commercial applications prospect widely in thermoelectric power generation and thermoelectric cooling technology.The conversion efficiency of thermoelectric material is by dimensionless thermoelectric figure of merit ZT (ZT=α2σ T/ κ wherein α be Seebeck coefficient, σ be electrical conductivity, κ be thermal conductivity, T be absolute temperature) determine, ZT is the biggest, and the conversion efficiency of thermoelectric of material is the highest.
Sb2Te3Based compound has the room temperature thermoelectricity capability of excellence, and at room temperature thermoelectric figure of merit is up to 1, is one of a kind of generally acknowledged and commercial applications room temperature thermoelectric material, is currently mainly applied to thermoelectric cooling.
At present, preparation Sb2Te3The method of base thermoelectricity material mainly uses powder metallurgic method and chemical method, gets rid of method, mechanical alloying method and wet chemical method etc. including fusion method, zone-melting process, melt rotation.But these methods easily cause component segregation, it is difficult to be precisely controlled to point, manufacturing cycle is longer simultaneously; and temperature required higher, time consumption and energy consumption is higher to equipment requirement and degree of dependence is high; scale preparation cost is high, greatly limits field and the scope of its scale application.Therefore, developing the supper-fast technology of preparing of new low cost is Sb2Te3The major subjects that base thermoelectricity material commercial applications faces,
Self-propagating Sintering Synthetic is the new technology utilizing the reaction synthetically prepared material of self-heat generation, and it has, and reaction speed is fast, technique is simple, low for equipment requirements, energy consumption is low, effective regulation material microstructure and accurately control the advantages such as product composition.Therefore, Self-propagating Sintering Synthetic has caused extensive concern in field of material preparation.A.G.Merzhanov et al. proposes T according to experiment experiencead≥1800K(TadFor adiabatic combustion temperature) conbustion synthesis criterion, i.e. as the T of systemad≥1800K(TadFor adiabatic combustion temperature) time, spontaneous could carry out Self-propagating Sintering Synthetic reaction, but Self-propagating Sintering Synthetic experiment shows, even if the adiabatic combustion temperature of a large amount of compound is less than 1800K, also can pass through Self-propagating Sintering Synthetic；In the recent period, Tang Xinfeng et al. is by substantial amounts of experimental study, it is proposed that the spontaneous new criterion carried out of SHS process, it is believed that Tad/Tm,L>=1, i.e. the adiabatic combustion temperature of system should be not less than the minimum fusing point of component.
For Sb2Te3Compound, because it is binary compound, preparation generally uses simple substance element.It is prepared according to simple substance powder, the adiabatic combustion temperature T of theoretical counting systemad=702K, the fusing point of low melting point Te is 723K, its Tad/Tm,L＜ 1, cannot occur SHS process to react in theory；Meanwhile, experiment shows Sb2Te3The Self-propagating Sintering Synthetic reaction that simple substance powder can not be used at room temperature to be lighted a fire by one end is prepared.This is owing to only preparing Sb from simple substance powder2Te3Chemical reaction liberated heat be not enough to promote combustion wave propagate and spread, even if combustion reaction has caused, combustion wave also can propagate during extinguish and cannot by self-propagating combustion reaction obtain Sb2Te3。
Summary of the invention
The technical problem to be solved is the deficiency existed for above-mentioned prior art and provides a kind of Sb2Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material and combustion adjuvant thereof, technique is simple, and preparation process is supper-fast, low for equipment requirements, suitable for scale production.
The present invention solves that the technical scheme that problem set forth above is used is:
A kind of Self-propagating Sintering Synthetic Sb2Te3The combustion adjuvant of base thermoelectricity material, this combustion adjuvant is In simple substance.
A kind of Sb2Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material, it is with Sb, Te simple substance as raw material, uses In simple substance to promote Self-propagating Sintering Synthetic reaction as combustion adjuvant, prepares Sb2Te3Base thermoelectricity material powder.
By such scheme, the ratio of the amount of described material between simple substance Sb, Te, In is 2 (1-x): 3:2x, and wherein x is 0.01-0.07.
By such scheme, the method for described Self-propagating Sintering Synthetic reaction is: mix as reactant using Sb, Te, In simple substance, in a vacuum or inert atmosphere, uses one end igniting to cause Self-propagating Sintering Synthetic reaction, obtains Sb2Te3Base thermoelectricity material powder.
By such scheme, described reactant is powder or is pressed into block.
Sb described above2Te3Base thermoelectricity material powder, can prepare Sb by discharge plasma sintering2Te3Base thermoelectricity material block.It is to say, invention also provides a kind of Sb2Te3The supper-fast synthetic method of base block thermoelectric material, with Sb, Te simple substance as raw material, uses In simple substance to promote Self-propagating Sintering Synthetic reaction as combustion adjuvant, prepares Sb2Te3Base thermoelectricity material powder, then prepare Sb by discharge plasma sintering2Te3Base block thermoelectric material.
By such scheme, the condition of described discharge plasma sintering is: sintering temperature is 400-500 DEG C, and sintering pressure is 30-50MPa, and temperature retention time is 2-5min.
By such scheme, the heating rate of described discharge plasma sintering is 50-100 DEG C.Preferably, the heating rate of described discharge plasma sintering is first to be raised to 400 DEG C with the speed of 100 DEG C/min, then be raised to 450 DEG C with the speed of 50 DEG C/min.
The Sb that said method prepares2Te3Base thermoelectricity material, wherein the introducing form of element In is to replace Sb2Te3In Sb position, its chemical composition can be expressed as chemical formula Sb2(1-x)In2xTe3。
The Sb that said method prepares2Te3Base thermoelectricity material, thermoelectricity capability is excellent, when x is 0.07, the ZT of 250 DEG Cmax0.71 can be reached.
Based on foregoing, on the premise of without departing from basic fundamental thought of the present invention, according to ordinary technical knowledge and the means of this area, its content can also be had the amendment of various ways, replace or change.
Compared with prior art, the invention has the beneficial effects as follows:
First, present invention firstly discloses a kind of Self-propagating Sintering Synthetic Sb2Te3The combustion adjuvant of base thermoelectricity material, this combustion adjuvant is In simple substance, and under the effect with In simple substance, raw material Sb, Te simple substance can occur Self-propagating Sintering Synthetic reaction to generate Sb2Te3Base thermoelectricity material；
Second, in the present invention, simple substance In is not only combustion adjuvant, is effective adulterant simultaneously, and the simple substance In of trace and raw material Sb, Te simple substance are collectively as reactant, by mixing a small amount of In on Sb position, can promote Self-propagating Sintering Synthetic reaction completely, obtain single-phase Sb2(1-x)In2xTe3Compound (Sb2Te3Base thermoelectricity material)；Combine discharge plasma sintering afterwards, prepare the Sb of densification2Te3Base block thermoelectric material; while improving thermoelectricity capability; also have that preparation time ultrashort (manufacturing cycle was shortened in 10min by the tens of the past hours), technique is simple, low for equipment requirements, energy-conserving and environment-protective, be suitable for the advantages such as large-scale production, for Sb2Te3The scale preparation of base thermoelectricity material and large-scale application are had laid a good foundation.
Accompanying drawing explanation
Fig. 1 is comparative example step 2) the XRD spectrum of lower end base and top product in quartz glass tube afterwards.
Fig. 2 is embodiment step 2) XRD of product spectrum.
Fig. 3 is the product X RD collection of illustrative plates of discharge plasma sintering in embodiment.
Fig. 4 is that in embodiment, the thermal conductivity of the product of discharge plasma sintering varies with temperature graph of relation.
Fig. 5 is that in embodiment, the electrical conductivity of the product of discharge plasma sintering varies with temperature graph of relation.
Fig. 6 is that in embodiment, the Seebeck coefficient of the product of discharge plasma sintering varies with temperature graph of relation.
Fig. 7 is that in embodiment, the power factor of the product of discharge plasma sintering varies with temperature graph of relation.
During in Fig. 8, solid line is embodiment, the dimensionless thermoelectric figure of merit of the product of discharge plasma sintering varies with temperature graph of relation (value of x is respectively 0.01,0.03,0.05,0.07)；Dotted line is the pure Sb prepared with fusion method2Te3The dimensionless thermoelectric figure of merit of sample varies with temperature graph of relation (i.e. the value of x is 0).
Fig. 9 is embodiment step 3) the FESEM collection of illustrative plates of product, x=0.07.
Detailed description of the invention
In order to be better understood from the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but present disclosure is not limited solely to the following examples.
Comparative example
With Sb, Te simple substance as raw material in this comparative example, do not use In simple substance as combustion adjuvant, attempt Self-propagating Sintering Synthetic reaction preparation Sb2Te3Base thermoelectricity material powder, specifically comprises the following steps that
1) Sb is pressed2Te3The stoichiometric proportion of middle element sb and Te weighs Sb powder and Te powder is 2:3 as raw material, the i.e. mol ratio of Sb powder and Te powder, then they is mixed, and in 4MPa pressurize 10min, is pressed into the cylindrical block of diameter 12mm；
2) under room temperature, by step 1) gained block sealed under vacuum in quartz glass tube, quartz glass tube bottom is shifted to coal gas flame heating igniting, do not observe spreading of combustion wave, Self-propagating Sintering Synthetic i.e. can not be caused to react.
To comparative example step 2) afterwards the product at quartz glass tube inner bottom part and top carry out material phase analysis respectively, as shown in Figure 1, be positioned at the product bottom quartz glass tube and be essentially single-phase Sb2Te3Compound, and be positioned in the product at quartz glass tube top and be still mainly Sb and Te simple substance, thus can prove that at room temperature, only using Sb, Te simple substance as reactant, can not Self-propagating Sintering Synthetic Sb by the way of lighting a fire in one end2Te3Thermoelectric material, although combustion reaction can cause, but combustion wave extinguishes during propagating and cannot complete self-propagating combustion reaction and prepare Sb2Te3Thermoelectric material.
Embodiment
A kind of Self-propagating Sintering Synthetic Sb2Te3The combustion adjuvant of base thermoelectricity material, this combustion adjuvant is In simple substance.
A kind of Sb2Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material, it is with Sb, Te simple substance as raw material, uses In simple substance to promote Self-propagating Sintering Synthetic reaction as combustion adjuvant, prepares Sb2Te3Base thermoelectricity material powder, wherein the ratio of the amount of the material between simple substance Sb, Te, In is 2 (1-x): 3:2x, and wherein x is 0.01-0.07, and in the present embodiment, the value of x is respectively 0.01,0.03,0.05,0.07, and concrete preparation process is as follows:
1) stoichiometrically 2 (1-x): 2x:3 weigh Sb powder, In powder, Te powder is 5g as raw material, raw material total amount, mixes in agate mortar, and the mixed powder obtained is as reactant；Reactant is put in steel grinding tool, tablet press machine uses pressure the pressurize 5min of 4MPa, prepare into diameter 12mm ingot body；
2) by step 1) gained ingot body is vacuum-sealed in quartz glass tube, quartz glass tube bottom is shifted to the heating igniting of coal gas flame, it was observed that combustion wave spreads to whole ingot body, has the most successfully caused Self-propagating Sintering Synthetic reaction, naturally cooling after having reacted, products therefrom is Sb2Te3Base thermoelectricity material powder.
By the present embodiment step 2) products therefrom all carries out phase composition analysis, result as in figure 2 it is shown, as seen from the figure, after mixing trace combustion adjuvant In simple substance (in terms of x, x is 0.01-0.07 to incorporation), obtained product is pure Sb2Te3Single-phase, it was demonstrated that to add trace combustion adjuvant In simple substance and can promote that what this Self-propagating Sintering Synthetic react is smoothed out, and react complete.
Sb prepared by the present embodiment2Te3Base thermoelectricity material powder prepares block thermoelectric material by follow-up discharge plasma sintering (SPS), specifically comprises the following steps that
By step 2) products therefrom grind into powder, powder is loaded in diameter 15mm graphite jig and be compacted, then be 40MPa in vacuum less than 10Pa, sintering pressure, sintering temperature carry out discharge plasma sintering (SPS) under conditions of being 450 DEG C, first it is raised to 400 DEG C with the speed of 100 DEG C/min, it is raised to sintering temperature 450 DEG C again with the speed of 50 DEG C/min, insulation 2min, i.e. obtains the Sb of densification2Te3Base thermoelectricity material block.
It can be seen in figure 3 that sample still keeps good Sb after discharge plasma sintering2Te3Single-phase.Curve is varied with temperature it can be seen that along with the increase of In volume, thermal conductivity declines from the thermal conductivity of Fig. 4, this is because Sb2Te3After single-phase middle trace In replaces Sb, due to both quality and radius difference, cause strong quality fluctuation scattering and stress field fluctuation scattering, strongly scatter phonon, reduce lattice thermal conductivity；Varying with temperature curve from Fig. 5 electrical conductivity it can be seen that along with the increase of In volume, electrical conductivity declines, this is owing to carrier concentration declines caused；This varies with temperature curvilinear trend with Seebeck coefficient in Fig. 6 is consistent, and along with the increase of In volume, Seebeck coefficient increases；Power factor varies with temperature curve as it is shown in fig. 7, along with the increase of In volume, power factor is declined slightly.
The above-mentioned Sb prepared2Te3Base thermoelectricity material block, wherein introduces element In, and the introducing form of In is to replace Sb2Te3In Sb position, its chemical composition can be expressed as chemical formula Sb2(1-x)In2xTe3, as shown in Figure 8, Sb2Te3The incorporation of single-phase middle trace In, thermoelectricity capability is compared and is not incorporated into the sample of element In and is greatly improved, when x is 0.07, the ZT of 250 DEG Cmax0.71 can be reached.
The above is only the preferred embodiment of the present invention, it is noted that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, it is also possible to make some modifications and variations, and these broadly fall into protection scope of the present invention.
Claims (8)
1.In simple substance as combustion adjuvant at Self-propagating Sintering Synthetic Sb2Te3Application in base thermoelectricity material.
2. a Sb2Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material, it is characterised in that it is with Sb, Te simple substance as raw material, uses In simple substance to react as combustion adjuvant generation Self-propagating Sintering Synthetic, prepares Sb2Te3Base thermoelectricity material powder；The ratio of the amount of described material between simple substance Sb, Te, In is 2 (1-x): 3:2x, and wherein x is 0.01-0.07.
A kind of Sb the most according to claim 22Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material, it is characterized in that the method that described Self-propagating Sintering Synthetic reacts is: mix as reactant using Sb, Te, In simple substance, in a vacuum or inert atmosphere, use one end igniting to cause Self-propagating Sintering Synthetic reaction, obtain Sb2Te3Base thermoelectricity material powder.
A kind of Sb the most according to claim 32Te3The Self-propagating Sintering Synthetic method of base thermoelectricity material, it is characterised in that described reactant is powder or is pressed into block.
5. a Sb2Te3The supper-fast synthetic method of base block thermoelectric material, it is characterised in that it is with Sb, Te simple substance as raw material, uses In simple substance to react as combustion adjuvant generation Self-propagating Sintering Synthetic, prepares Sb2Te3Base thermoelectricity material powder；Described Sb2Te3Base thermoelectricity material powder prepares Sb by discharge plasma sintering2Te3Base block thermoelectric material；The ratio of the amount of described material between simple substance Sb, Te, In is 2 (1-x): 3:2x, and wherein x is 0.01-0.07.
A kind of Sb the most according to claim 52Te3The supper-fast synthetic method of base block thermoelectric material, it is characterised in that the condition of described discharge plasma sintering is: sintering temperature is 400-500 DEG C, sintering pressure is 30-50 MPa, and temperature retention time is 2-5 min.
A kind of Sb the most according to claim 52Te3The supper-fast synthetic method of base block thermoelectric material, it is characterised in that the heating rate of described discharge plasma sintering is 50-100 DEG C/min.
8. the Sb prepared according to the supper-fast synthetic method one of claim 5-7 Suo Shu2Te3Base thermoelectricity material.
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