CN106952999B - A kind of multiple level doping PbTe base thermoelectricity materials and preparation method thereof - Google Patents
A kind of multiple level doping PbTe base thermoelectricity materials and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/854—Thermoelectric active materials comprising inorganic compositions comprising only metals
Abstract
The present invention provides a kind of multiple level to adulterate PbTe base thermoelectricity materials and preparation method thereof, and the molecular formula of the multiple level doping PbTe base thermoelectricity materials is In x Pb1‑x Te1‑y A y ；Wherein, A Cl, Br, I, Ga, Al；0<x≤ 0.02,0<y≤0.03.Technical scheme of the present invention is adulterated simultaneously using depth energy level, carrier concentration when improving lower temperature is adulterated using shallow energy level, carrier concentration when improving higher temperature is adulterated using deep energy level, and bipolar diffusion temperature is improved, it is final to obtain the thermoelectric material with high thermoelectric figure of merit in wide temperature range, improve the thermoelectrical efficiency of material.
Description
Technical field
The invention belongs to field of thermoelectric material technique more particularly to a kind of multiple level doping PbTe base thermoelectricity materials and its systems
Preparation Method.
Background technology
The material of thermoelectric generator or thermoelectric cooling module is known as thermoelectric material, be it is a kind of can realize electric energy interacted with thermal energy turn
The material of change.The thermo-electric generation and refrigeration device made by thermoelectric material has pollution-free, noiseless, easy to maintain, safety can
By the advantages that.The earliest Soviet Union is powered in outlying district for household radio electricity receiver using kerosene lamp or timber as heat source.With
It the increase of space exploration interest and in the increasingly increased resource survey of the earth and Exploratory behavior, needs exploitation one kind can
Itself energy supply and the power-supply system without looking after, thermoelectric power generation are particularly suitable these applications.For remote space probe
For, the thermoelectric generator of radioactive isotope heat supply is unique power supply system.It is successfully applied to NASA
On more than 20 a spacecrafts such as Apollo, Pioneer, Voyager and the Ulysses of NASA transmittings.In Russia, there are more than 1000
Similar radiosotope thermoelectric generator device for the ocean lighthouse near the Arctic Circle there is non-maintaining 20 years of operation to set
Count the service life.Can be outlying district, the small army of field operation in addition, using the small-sized electric generating apparatus of the fuel heats such as fuel oil or timber
Deng offer small-power power；Using crops, rubbish even human body thermal energy, can be established in house, farm etc. one small
Type electricity generation system meets the needs of people are for low-power energy.U.S. Department of Energy disclosed one on November 12nd, 2003
" the advanced thermoelectric material of industrial waste heat thermo-electric generation " project, using the waste-heat power generation of the industrial high temperatures stove such as metallurgical furnace to reduce energy
Consumption, issued again in March, 2004 carry out automobile engine residual heat thermo-electric generation research, Europe 20 Yu Ge research institutions combine into
The research gone in terms of automobile engine residual heat power generation, and organized " nanowatt to megawatt thermal electric energy conversion " large size scientific research item
Mesh, u s company are mounted with 1000W grades of cogeneration systems on Large freight truck, and accessory power supply etc. is provided for automobile,
Japan establishes " 7500W grades of garbage fuel cogeneration demonstration systems ", achieves good actual effect.The nearly more than ten years, I
State has also carried out a large amount of research on using the nature temperature difference and industrial waste heat thermoelectric power generation, and makes great progress,
With good comprehensive social benefit.Thermoelectric cooler has the advantages that mechanical compression refrigeration machine is difficult to match in excellence or beauty：Size is small, quality
Gently, the problem of without any mechanical rotation part, work noiseless, no liquid or gaseous medium, therefore there is no pollution environment, can
Realization accurate temperature controlling, fast response time, device service life are long.Low temperature environment can also be provided for the use of superconductor.In addition
The micro element prepared using thermoelectric material is used to prepare cooling micro power, microcell, optical communication laser diode and infrared ray
The thermoregulating system of sensor has expanded the application field of thermoelectric material significantly.In the heat dissipation of electronic product, biomedicine operation
Temperature control aspect all have good application prospect.It should say, thermoelectric material is a kind of material of extensive application foreground
Material, in today of environmental pollution and energy crisis getting worse, there is very strong reality to anticipate for the research for carrying out new thermoelectric materials
Justice.
Thermoelectric generation technology may be implemented thermal energy and electric energy and directly mutually convert, and be the key issues of current new energy research
One of.Greatly develop application of the thermoelectric power generation technology in solar thermal energy power generation (increasing income) and waste heat waste-heat power generation (throttling) etc. fields
The current energy shortages in China and problem of environmental pollution can be effectively relieved, there is important strategic importance.The performance of thermoelectric material
By dimensionless figure of merit ZT=[S2σ/(κe+κL)] T characterizations, conductivityσ and Seebeck coefficient S are improved, while reducing thermal conductivity κ (κ
It is carrier thermal conductivity κeWith phonon thermal conductivity κLThe sum of) it is the key that optimization of material, but three physical quantitys are interrelated, make
The optimization of performance is obtained by actual limitation.In recent years, not turning off by using energy band engineering, nanometer engineering and new material
Hair, a large amount of progress are achieved in terms of improving peak value thermoelectric figure of merit.But thermoelectrical efficiency is dependent on material within the scope of total temperature
Average thermoelectric figure of merit, ηmax=[(TH-TC)/TH][(1+ZTIt is average)1/2-1]/[(1+ZTIt is average)1/2+TC/TH], TH：Hot-side temperature, TC：
Cold junction temperature.It is difficult to obtain higher conversion efficiency of thermoelectric to have larger peak value thermoelectric figure of merit merely, will such as have different heat
The material of electric peak temperature links together, it can be expected that generating higher efficiency, but can face many engineering problems, as interface connects
It connects, the matching problem of interface diffusion and coefficient of thermal expansion, these all can be in the final efficiency for influencing device in various degree.Therefore
Best bet is the thermoelectric material that optimization has wide temperature range better performances.
Thermoelectric material is typically semiconductor, can adjust its carrier concentration by adulterating so that electronics or hole
Referred to as mostly sub based on middle one kind, when temperature reaches intrinsic excitation temperature, few son is excited, and is simultaneously participated in by two kinds of carriers defeated
Fortune, will produce thermoelectricity capability certain influence, referred to as dipolar effect.When dipolar effect occurs, contrary sign carrier can be offset
The Seebeck coefficients of material, although conductivity increased at this time, total electric property (power factor S2It σ) or can be big
Width reduces；Meanwhile carrier thermal conductivity κc=κe+κh+κbiBy electron thermal conductivity κe, hole thermal conductivity κhAnd bipolar diffusion thermal conductivity
Rate κbiComposition, when intrinsic excitation occurs, thermal conductivity be can not ignore caused by few son and bipolar diffusion so that total thermal conductivity is aobvious
It writes and increases, so the optimization of usually thermoelectricity capability is all bound in bipolar diffusion temperature or less.Thermoelectric figure of merit is generally with temperature liter
It is high and increases, therefore as can bipolar diffusion temperature is improved, the high thermoelectric figure of merit in wide temperature range will be obtained, realized efficiently
The exploitation of rate thermoelectric material.
More common method is the energy gap that doping increases majority carrier density and alloying increases material.It is also possible to use
Passing through for the selective few son of obstruction of potential barrier of heterogenous junction is added.Have recently scientist borrow permanent magnetism nano-particle from ferromagnet to
The property of paramagnet transformation, makes it capture electronics when less than Curie temperature, and release capture when higher than Curie temperature
Electronics can also solve the problems, such as thermoelectric material in intrinsic excitation area performance degradation as " electronic repository ".
The study found that can effectively inhibit bipolar diffusion using deep energy level doping, the thermoelectricity capability of material is improved, temperature is worked as
When higher, deep energy level doping will produce more majority carriers compared with shallow energy level doping, and then inhibit the excitation of few son, slow down double
Bipolar diffusion temperature can be improved, is finally reached in larger temperature range by the negative effect of pole diffusion, the deep-level impurity state
It is that pyroelectric material performance improves and provides a kind of new method inside all to keep higher ZT values, the research, has important section
Learn meaning.
Analyze the studies above, at present there are still the problem of it is as follows：
(1) in theory, the reduction of minority carrier density will be corresponded to by increasing the majority carrier density of material, bipolar to reduce
Effect, however from the angle of optimization ZT, each material has optimal carrier concentration, and it is anti-to increase carrier concentration simply
And the thermoelectric figure of merit of material can be reduced；
(2) alloying process will bring lattice defect to cause declining to a great extent for mobility；
(3) it is one and its difficult thing for the selection of potential barrier of heterogenous junction, is also theoretical prediction at present, not
Experimental result；
(4) deep energy level, which is adulterated, can effectively improve bipolar diffusion temperature, but the more difficult ionization of deep energy level doping itself, only
Least a portion of impurity contributes carrier concentration, although can obtain more carrier at high temperature, is carried in low temperature
It is very low to flow sub- concentration.
Invention content
For the above technical problem, the invention discloses a kind of multiple level doping PbTe base thermoelectricity materials and its preparation sides
Method, multiple level doping PbTe base thermoelectricity materials effectively increase the bipolar diffusion temperature of material, improve wide temperature range
Interior thermoelectric figure of merit improves the thermoelectrical efficiency of material.
In this regard, the technical scheme is that：
A kind of multiple level doping PbTe base thermoelectricity materials, molecular formula InxPb1-xTe1-yAy, wherein A Cl, Br, I,
Ga, Al；0<X≤0.02,0<Y≤0.03.Preferably, the A is I.
As a further improvement on the present invention, 0<X≤0.01,0<Y≤0.002.
As a further improvement on the present invention, 0.0010≤X≤0.01,0.0010<Y≤0.02.
As a further improvement on the present invention, the multiple level doping PbTe base thermoelectricity materials are prepared into using following steps
It arrives：
Step S1：By In, Pb, Te, A according to proportioning vacuum seal in quartz ampoule, with the heating rate of 180~220 DEG C/h
900~1100 DEG C are warming up to, soaking time is 4~8h；Wherein, it is according to according to proportioning by In, Pb, Te, AxPb1-xTe1-yA
The element ratio of molecular formula；Wherein, Cl uses compound PbCl2, Br is using compound PbBr2, I is using compound PbI2, other
Element selects simple substance；
Step S2：Then 500~700 DEG C are dropped to the cooling rate of 180~220 DEG C/h, at such a temperature anneal 40~
60h finally drops to room temperature with the cooling rate of 180~220 DEG C/h, obtains ingot casting；
Step S3：Obtained ingot casting is cleaned to milling in glove box, by powder with direct current hot press 550~650 DEG C,
Hot pressing 1~3 minute under 70~90MPa.
As a further improvement on the present invention, in step S1,1000 DEG C are warming up to the heating rate of 200 DEG C/h, heat preservation
Time is 6h.
As a further improvement on the present invention, in step S2,600 DEG C are dropped to the cooling rate of 200 DEG C/h, in the temperature
Lower annealing 50h, finally drops to room temperature with the cooling rate of 200 DEG C/h.
As a further improvement on the present invention, in step S3, by powder direct current hot press hot pressing at 600 DEG C, 80MPa
2 minutes.
The present invention also provides the preparation sides that the multiple level described in a kind of any one as above adulterates PbTe base thermoelectricity materials
Method, which is characterized in that it includes the following steps：
Step S1：By In, Pb, Te, A according to proportioning vacuum seal in quartz ampoule, with the heating rate of 180~220 DEG C/h
900~1100 DEG C are warming up to, soaking time is 4~8h；Wherein, wherein Cl uses compound PbCl2, Br is using compound
PbBr2, I is using compound PbI2, other elements selection simple substance；
Step S2：Then 500~700 DEG C are dropped to the cooling rate of 180~220 DEG C/h, at such a temperature anneal 40~
60h finally drops to room temperature with the cooling rate of 180~220 DEG C/h；
Step S3：Obtained ingot casting is cleaned to milling in glove box, by powder with direct current hot press 550~650 DEG C,
Hot pressing 1~3 minute under 70~90MPa.
As a further improvement on the present invention, in step S1,1000 DEG C are warming up to the heating rate of 200 DEG C/h, heat preservation
Time is 6h.
As a further improvement on the present invention, in step S2,600 DEG C are dropped to the cooling rate of 200 DEG C/h, in the temperature
Lower annealing 50h, finally drops to room temperature with the cooling rate of 200 DEG C/h.
As a further improvement on the present invention, in step S3, by powder direct current hot press hot pressing at 600 DEG C, 80MPa
2 minutes.
Compared with prior art, beneficial effects of the present invention are：
Technical scheme of the present invention is adulterated simultaneously using depth energy level, and load when improving lower temperature is adulterated using shallow energy level
Sub- concentration is flowed, carrier concentration when improving higher temperature is adulterated using deep energy level, and bipolar diffusion temperature is improved, finally obtains
The thermoelectric material with high thermoelectric figure of merit in wide temperature range is obtained, the thermoelectrical efficiency of material is improved.
Description of the drawings
Fig. 1 is the multiple level doping In of the present inventionxPb1-xTe0.996I0.004(x=0,0.00125,0.0025,0.0035 and
0.005) conductivity (a), Seebeck coefficient (b), power factor (c), thermal diffusion coefficient (d), specific heat (e), total thermal conductivity and
The comparison diagram of lattice thermal conductivity (f)；In figure, (a), (b), (c), (d), (e), (f) ordinate correspond to conductivity, Sai Bei respectively
Gram coefficient, power factor, thermal diffusion coefficient, specific heat, total thermal conductivity and lattice thermal conductivity.
Fig. 2 is the multiple level doping In of the present inventionxPb1-xTe0.996I0.004(x=0,0.00125,0.0025,0.0035 and
0.005), shallow energy level adulterates PbTe1-yIyIn is adulterated with deep energy level0.02Pb0.98Te1-ySyThe relationship of carrier concentration and mobility
Figure.
Fig. 3 is the multiple level doping In of the present inventionxPb1-xTe0.996I0.004(x=0,0.00125,0.0025,0.0035 and
0.005) ZT values adulterate PbTe with shallow energy level1-yIyZT values (i.e. dimensionless thermoelectric figure of merit) compare figure.
Fig. 4 multiple level adulterates In0.0035Pb0.9965Te0.996I0.004, shallow energy level doping PbTe1-yIyIt is adulterated with deep energy level
In0.02Pb0.98Te1-ySyThermoelectrical efficiency compares figure.
Specific implementation mode
The preferably embodiment of the present invention is described in further detail below.
The thermal conductivity κ of material is according to the thermal diffusion system measured using Netzsch LFA-457 type laser pulse thermal analyzers
The density of number, the specific heat measured using Netzsch DSC-404 type difference specific heat instrument and material is calculated.The conductance of material
Rate σ and Seebeck coefficient S tests to obtain using ZEM-3 conductivity with Seebeck coefficient tester.The thermoelectric figure of merit Z and nothing of material
Dimension thermoelectric figure of merit ZT is calculated according to above-mentioned measured value.
Embodiment 1
A kind of multiple level doping PbTe base thermoelectricity materials, molecular formula InxPb1-xTe0.996I0.004, wherein 0<X≤
0.01.X=0.00125,0.0025,0.0035 is selected separately below, and 0.005 is prepared thermoelectric material according to the following steps
In0.00125Pb0.99875Te0.996I0.004,In0.0025Pb0.9975Te0.996I0.004,In0.0035Pb0.9965Te0.996I0.004With
In0.005Pb0.995Te0.996I0.004。
Step S1：In, Pb, Te, I are warming up in quartz ampoule with the heating rate of 200 DEG C/h according to proportioning vacuum seal
1000 DEG C, soaking time 6h.
Step S2：Then 600 DEG C are dropped to the cooling rate of 200 DEG C/h, anneal 50h at such a temperature, finally with 200
DEG C/cooling rate of h drops to room temperature.
Step S3：Obtained ingot casting is cleaned to milling in glove box, by powder with direct current hot press in 600 DEG C, 80MPa
Lower hot pressing 2 minutes.
Then analysis is detected to the above-mentioned material being prepared.Fig. 1 is that multiple level adulterates InxPb1-xTe0.996I0.004
(x=0,0.00125,0.0025,0.0035 and conductivity (a) 0.005), Seebeck coefficients (b), power factor (c), heat
The comparison figure of diffusion coefficient (d), specific heat (e), total thermal conductivity and lattice thermal conductivity (f) is adulterated using multiple level as seen from Figure 1
Thermoelectric material obtains wide temperature range high power factor and low thermal conductivity.
Fig. 2 is that multiple level adulterates InxPb1-xTe0.996I0.004(x=0,0.00125,0.0025,0.0035 and 0.005) with
Shallow energy level adulterates PbTe1-yIyIn is adulterated with deep energy level0.02Pb0.98Te1-ySyThe comparison figure of carrier concentration and mobility.Pass through
PbTe is adulterated with shallow energy level1-yIyIn is adulterated with deep energy level0.02Pb0.98Te1-ySyThe comparison of progress carrier concentration and mobility
It arrives, alloy scattering is overcome using multiple level doped thermoelectric material, the mobility of carrier is adulterated compared with deep energy level
In0.02Pb0.98Te1-ySyIt increases.
Fig. 3 is multiple level doping InxPb1-xTe0.996I0.004(x=0,0.00125,0.0025,0.0035's and 0.005)
ZT values adulterate PbTe with shallow energy level1-yIyZT values compare.It is found by comparing, multiple level doped thermoelectric material has wider
The high thermoelectric figure of merit of temperature range.
Fig. 4 is multiple level doping In0.0035Pb0.9965Te0.996I0.004, shallow energy level doping PbTe1-yIyIt is adulterated with deep energy level
In0.02Pb0.98Te1-ySyThermoelectrical efficiency compares.As it can be seen that opposite with for shallow energy level doping and deep energy level doping, multiple level is adulterated
With higher thermoelectrical efficiency.
The present invention is put forward for the first time using the bipolar diffusion temperature for improving material as breach using multiple level doped thermoelectric material
Obtain the high-efficiency thermal electric material of the high figure of merit of wide temperature range.It is dense that carrier when improving lower temperature is adulterated using shallow energy level
Degree adulterates carrier concentration when improving higher temperature using deep energy level, and bipolar diffusion temperature is improved, it is final obtain compared with
The thermoelectric material with high thermoelectric figure of merit, improves the thermoelectrical efficiency of material in wide temperature range.
Embodiment 2
Multiple level doping PbTe base thermoelectricity materials In is carried out using different element AsxPb1-xTe1-yAy, wherein A Cl, Br,
I, Ga, Al；0<X≤0.02,0<Y≤0.03, the preparation method is the same as that of Example 1, and performance evaluation has been carried out to it.
Table 1 gives embodiment and corresponding comparative example using deep-level impurity In and different shallow level impurity A 500
DEG C when thermoelectric figure of merit Z and thermoelectrical efficiency (50 DEG C of low-temperature end) data.
Table 1
By the data in table 1 as it can be seen that the thermoelectricity obtained using deep-level impurity In and different shallow level impurity A co-dopeds
Material is compared with comparative example, is all had high thermoelectric figure of merit, is improved the thermoelectrical efficiency of material.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
The specific implementation of the present invention is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the present invention's
Protection domain.
Claims (7)
1. a kind of multiple level adulterates PbTe base thermoelectricity materials, it is characterised in that：Its molecular formula is In x Pb1-x Te1-y A y , wherein A is
Cl, Br, Ga, Al；0<X≤0.02,0<Y≤0.03；The multiple level doping PbTe base thermoelectricity materials are prepared using following steps
It obtains：
Step S1：In, Pb, Te, A are warming up in quartz ampoule with the heating rate of 180 ~ 220 DEG C/h according to proportioning vacuum seal
900 ~ 1100 DEG C, soaking time is 4 ~ 8 h；
Step S2：Then 500 ~ 700 DEG C are dropped to the cooling rate of 180 ~ 220 DEG C/h, anneal 40 ~ 60 h at such a temperature, most
Room temperature is dropped to the cooling rate of 180 ~ 220 DEG C/h afterwards, obtains ingot casting；
Step S3：The ingot casting that step S2 is obtained cleans milling in glove box, by powder with direct current hot press 550 ~ 650
DEG C, hot pressing 1 ~ 3 minute under 70 ~ 90MPa.
2. multiple level according to claim 1 adulterates PbTe base thermoelectricity materials, it is characterised in that：0<X≤0.01,0<Y≤
0.02。
3. multiple level according to claim 2 adulterates PbTe base thermoelectricity materials, it is characterised in that：0.0010≤X≤0.01,
0.0010<Y≤0.02。
4. the preparation method of the multiple level doping PbTe base thermoelectricity materials described in claim 1 ~ 3 any one, which is characterized in that
It includes the following steps：
Step S1：In, Pb, Te, A are warming up in quartz ampoule with the heating rate of 180 ~ 220 DEG C/h according to proportioning vacuum seal
900 ~ 1100 DEG C, soaking time is 4 ~ 8 h；
Step S2：Then 500 ~ 700 DEG C are dropped to the cooling rate of 180 ~ 220 DEG C/h, anneal 40 ~ 60 h at such a temperature, most
Room temperature is dropped to the cooling rate of 180 ~ 220 DEG C/h afterwards, obtains ingot casting；
Step S3：The ingot casting that step S2 is obtained cleans milling in glove box, by powder with direct current hot press 550 ~ 650
DEG C, hot pressing 1 ~ 3 minute under 70 ~ 90MPa.
5. the preparation method of multiple level doping PbTe base thermoelectricity materials according to claim 4, it is characterised in that：Step S1
In, 1000 DEG C are warming up to the heating rate of 200 DEG C/h, soaking time is 6 h.
6. the preparation method of multiple level doping PbTe base thermoelectricity materials according to claim 4, it is characterised in that：Step S2
In, 600 DEG C are dropped to the cooling rate of 200 DEG C/h, anneal 50 h at such a temperature, is finally dropped with the cooling rate of 200 DEG C/h
To room temperature.
7. the preparation method of multiple level doping PbTe base thermoelectricity materials according to claim 4, it is characterised in that：Step S3
In, by powder with direct current hot press hot pressing 2 minutes at 600 DEG C, 80 MPa.
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| CN111628071B (en) * | 2020-05-26 | 2022-01-25 | 电子科技大学 | Medium-temperature-range thermoelectric material and preparation method thereof |
| CN114477107B (en) * | 2022-01-19 | 2023-06-20 | 深圳热电新能源科技有限公司 | N-type PbTe-based thermoelectric material without nano precipitated phase and preparation method thereof |
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| CN104064666A (en) * | 2014-05-28 | 2014-09-24 | 南方科技大学 | High-effect potassium-doped lead telluride-lead sulfide alloy thermoelectric material and preparation method thereof |
| CN105140383A (en) * | 2015-07-08 | 2015-12-09 | 上海大学 | Composite PbSe-based thermoelectric material doped with Sr and Na and preparation method thereof |
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| CN104064666A (en) * | 2014-05-28 | 2014-09-24 | 南方科技大学 | High-effect potassium-doped lead telluride-lead sulfide alloy thermoelectric material and preparation method thereof |
| CN105140383A (en) * | 2015-07-08 | 2015-12-09 | 上海大学 | Composite PbSe-based thermoelectric material doped with Sr and Na and preparation method thereof |
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