CN104591103A - Bi2Te3-xSx thermoelectric material and preparation method thereof - Google Patents
Bi2Te3-xSx thermoelectric material and preparation method thereof Download PDFInfo
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- CN104591103A CN104591103A CN201410844212.8A CN201410844212A CN104591103A CN 104591103 A CN104591103 A CN 104591103A CN 201410844212 A CN201410844212 A CN 201410844212A CN 104591103 A CN104591103 A CN 104591103A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
Abstract
The invention provides a Bi2Te3-xSx thermoelectric material and a preparation method thereof, belongs to a thermoelectric material and a preparation method therefore and aims at improving the related thermoelectric properties of a Bi2Te3-xSx-based thermoelectric material applied to a low temperature region in a medium temperature region, and meanwhile, solving the problem of the adverse effect of the existing medium-temperature thermoelectric material on the environment. The preparation method comprises the following steps: weighing and mixing the prepared high-purity bismuth powder (Bi), tellurium powder (Te) and sulfur powder (S) according to a predetermined atomic ratio respectively, putting the mixture into a ball milling jar, performing mechanical alloying treatment in an argon protection atmosphere, and then putting the obtained powder into a graphite die for discharge plasma sintering, thereby obtaining the Bi2Te3-xSx block material. According to the preparation method of the Bi2Te3-xSx thermoelectric material, the process is simple, the preparation period is short, the material consumption in the preparation process is low, the cost is low, and the operability is high; due to the introduction of the element S into the material, the related thermoelectric properties of the Bi2Te3-xSx-based thermoelectric material applied to the low temperature region in the medium temperature region are improved; in addition, the material is environmentally friendly, and the problem of the adverse effect of the existing medium-temperature thermoelectric material on the environment is solved.
Description
Technical field
The invention belongs to thermoelectric material and preparation method thereof, be specifically related to a kind of Bi
2te
3-xs
xthermoelectric material and preparation method thereof.
Technical background
Thermoelectricity originates from three basic effects relevant with thermo-electric conversion: Seebeck effect (Seebeckeffect), paltie effect (Peltier effect) and Thomson effect (Thomson effect), based on these three effects, the thermo-electric device that can realize heat energy and electric energy and mutually change just can be produced.Due to the utility value that pyroelectricity show in low grade heat energy, and it is reliable and stable, free of contamination operating characteristics, and present thermoelectric material obtains large-scale utilization in thermoelectric power generation and thermoelectric refrigeration two.
Most thermoelectric materials has an identical character, is exactly that thermoelectricity capability is very large by the impact of temperature, uses the difference of temperature, be usually divided into room temperature thermoelectric material (with Bi according to different thermoelectric material
2te
3base alloy is representative), warm thermoelectric material (400-700K, with PbTe alloy for representative), high-temperature thermoelectric material (800-1000K, with SiGe alloy for representative) three kinds.As having most the thermoelectric material using potentiality under room temperature, Bi
2te
3base thermoelectricity material has higher electroconductibility and lower thermal conductivity, is the emphasis that people study always, is widely used in the various fields such as waste heat recovery, thermo-electric generation, refrigeration and medical treatment.Because the disadvantageous effect that temperature raises for thermoelectricity capability is mainly reflected in the reduction of electric property, work as Bi
2te
3when base thermoelectricity material is used for middle temperature, electric property reduces; And contain the reasons such as heavy metal with the existing warm thermoelectric material that PbTe alloy is representative, in the preparation of thermoelectric material and the use procedure of thermo-electric device, all can cause some adverse influences to environment.
Summary of the invention
The invention provides a kind of Bi
2te
3-xs
xthermoelectric material, provides its preparation method simultaneously, and object is to improve originally for the Bi of cold zone
2te
3the associated hot electrical property of base thermoelectricity material in middle warm area, solves existing warm thermoelectric material causes disadvantageous effect problem to environment simultaneously.
A kind of Bi provided by the present invention
2te
3-xs
xthermoelectric material, comprises bismuth, tellurium element, it is characterized in that:
It is according to Bi
2te
3-xs
xthe atomic ratio determined of stoichiometric equation bismuth meal, tellurium powder, sulphur powder to be weighed mixing, through mechanical alloying process and sintering obtained, 0 < X < 3.
Described Bi
2te
3-xs
xthermoelectric material, it is further characterized in that:
Before mechanical alloying process, in raw material, add the copper powder of 0.5at.% ~ 1at.%, to obtain better repeatability.
Described Bi
2te
3-xs
xthermoelectric material preparation method, is characterized in that, comprises the following step:
(1) with bismuth meal (Bi), tellurium powder (Te), sulphur powder (S) for raw material, according to synthesized Bi
2te
3-xs
xthe atomic ratio determined of stoichiometric equation raw material to be weighed mixing, need for subsequent operations, 0 < X < 3;
(2) step (1) mixed raw material is positioned in ball grinder, under argon shield atmosphere, carries out mechanical alloying process, the diameter 5mm ~ 10mm of abrading-ball in ball grinder;
(3) loaded in graphite jig by the powder of step (2) mechanical alloy process gained, sinter in plasma agglomeration stove, sintering environment is vacuum, obtains block materials.
Described in described step (1), the quality purity of each raw material is all greater than 99.99%, crosses 100 ~ 200 mesh sieves respectively before using to tellurium powder (Te), bismuth meal (Bi);
In described step (2), the ball material mass ratio in ball grinder is 15:1 ~ 20:1, and rotating speed is 350 ~ 500rpm, and Ball-milling Time is 12 ~ 20h.
In described step (3), sintering temperature 320 DEG C ~ 450 DEG C, intensification duration 40min ~ 60min, insulation duration 10min ~ 15min, sintering pressure 35MPa ~ 50MPa.
In above-mentioned preparation method, in described step (1), can add the copper powder of 0.5at.% ~ 1at.% in raw material, to obtain better repeatability, the quality purity of described copper powder is greater than 99.99%.
The present invention introduces S element in the material, the synthesis of compound powder is carried out by mechanical alloying, shaping preparation is carried out by discharge plasma sintering, the block materials cutting machine obtained after sintering is cut out and meets the sample of testing tool to dimensional requirement, testing tool is put into after sand papering surface, carry out the test of resistivity (ρ) and Seebeck coefficient (α), with power factor PF=α
2/ ρ evaluates its electric property; Result shows, the Bi prepared by method of the present invention
2te
3-xs
xthermoelectric material has higher power factor at middle warm area, such as, in embodiment 1 Bi
2te
2.5s
0.5150 DEG C time, power factor still can reach 2981 μ Wm
-1k
-2though, decline to some extent when 250 DEG C and also can reach 1550 μ Wm
-1k
-2, electric property is good; And the existing traditional warm thermoelectric material being representative with PbTe alloy is because containing reasons such as heavy metal elements, in the preparation of thermoelectric material and the use procedure of thermo-electric device, all bad impact can be caused on environment; Integrate and see, Bi
2te
3-xs
xthermoelectric material has good applying value relative to warm area thermoelectric material in other.
Compared with other existing preparation methods, it is simple that the present invention has technique, and preparation cycle is short, and preparation process consumptive material is few, and material use efficiency is high, and cost is low, workable, and preparation process is easy to the clear superiorities such as control.
Accompanying drawing explanation
Fig. 1 is the Changing Pattern schematic diagram of resistivity (ρ) along with temperature of the embodiment of the present invention;
Fig. 2 is the Changing Pattern schematic diagram of Seebeck coefficient (α) along with temperature of the embodiment of the present invention;
Fig. 3 is that the embodiment of the present invention is by PF=α
2the power factor that/ρ calculates is along with the Changing Pattern schematic diagram of temperature.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.These embodiments are only not used in restriction application claims protection domain for illustration of the present invention should be understood.
Embodiment 1: a kind of Bi
2te
2.5s
0.5the preparation method of thermoelectric material, comprises the steps:
(1) with the bismuth meal (Bi of 4N level, 200 orders), tellurium powder (Te, 100 orders), sulphur powder (S) is raw material, according to bismuth meal: tellurium powder: raw material is weighed mixing by the atomic ratio of sulphur powder=2:2.5:0.5, the total amount of three kinds of powder stocks is 15g, add the copper powder of 0.5at.% in raw material, to obtain better repeatability, the quality purity of described copper powder is greater than 99.99%;
(2) be positioned in ball grinder by step (1) mixed raw material, under argon shield atmosphere, carry out mechanical alloying process, in ball grinder, diameter is the mass ratio of the abrading-ball of 5mm, 8mm, 10mm is 1:1:8; Ball material mass ratio in ball grinder is 20:1, and drum's speed of rotation is 500rpm, and Ball-milling Time is 12h;
(3) powder of step (2) mechanical alloy process gained is loaded in graphite jig, vacuum sintering is carried out in plasma agglomeration stove, sintering temperature 450 DEG C, intensification duration 60min, insulation duration 15min, sintering pressure 50MPa, the internal diameter of described graphite jig is Φ 23mm, obtains block materials.
Being undertaken cutting, polishing by sintering the block materials obtained, obtaining the sample of 3 × 3 × 15mm, test sample associated electrical performance; The test result of sample resistivity (ρ) and Seebeck coefficient (α) respectively as shown in Figure 1, Figure 2 shown in, calculate the power factor at each measuring tempeature point place according to ρ and α, as shown in Figure 3.As can see from Figure 3, due to adding of S element, Bi
2te
2.5s
0.5electric property in 150 DEG C, there is optimum value, reach 2981 μ W*m
-1k
-2, afterwards along with the power factor that increases again of temperature starts to reduce, to being reduced to 1550 μ Wm when 250 DEG C
-1k
-2.
Embodiment 2: a kind of Bi
2te
2the preparation method of S thermoelectric material, comprises the steps:
(1) with the bismuth meal (Bi of 4N level, 200 orders), tellurium powder (Te, 100 orders), sulphur powder (S) is raw material, according to bismuth meal: tellurium powder: raw material is weighed mixing by the atomic ratio of sulphur powder=2:2:1, the total amount of three kinds of powder stocks is 15g, add the copper powder of 0.5at.% in raw material, to obtain better repeatability, the quality purity of described copper powder is greater than 99.99%;
(2) be positioned in ball grinder by step (1) mixed raw material, under argon shield atmosphere, carry out mechanical alloying process, in ball grinder, diameter is the mass ratio of the abrading-ball of 5mm, 8mm, 10mm is 1:1:8; Ball material mass ratio in ball grinder is 15:1, and rotating speed is 350rpm, and Ball-milling Time is 20h;
(3) powder of step (2) mechanical alloy process gained is loaded in graphite jig, vacuum sintering is carried out in plasma agglomeration stove, sintering temperature 380 DEG C, intensification duration 50min, insulation duration 15min, sintering pressure 40Mpa, the internal diameter of described graphite jig is Φ 23mm, obtains block materials.
Being undertaken cutting, polishing by sintering the block materials obtained, obtaining the sample of 3 × 3 × 15mm, test sample associated electrical performance; The test result of sample resistivity (ρ) and Seebeck coefficient (α) is distinguished as shown in Figure 1 and Figure 2, the power factor at each measuring tempeature point place is calculated according to ρ and α, as shown in Figure 3.As can see from Figure 3, Bi
2te
2the power factor of S constantly increases in Range of measuring temp, has reached 1358 μ Wm 250 DEG C time
-1k
-2.
Embodiment 3: a kind of Bi
2te
1.5s
1.5the preparation method of thermoelectric material, comprises the steps:
(1) with the bismuth meal (Bi of 4N level, 200 orders), tellurium powder (Te, 100 orders), sulphur powder (S) is raw material, according to bismuth meal: tellurium powder: raw material is weighed mixing by the atomic ratio of sulphur powder=2:1.5:1.5, the total amount of three kinds of powder stocks is 15g, add the copper powder of 1at.% in raw material, to obtain better repeatability, the quality purity of described copper powder is greater than 99.99%;
(2) be positioned in ball grinder by step (1) mixed raw material, under argon shield atmosphere, carry out mechanical alloying process, in ball grinder, diameter is the mass ratio of the abrading-ball of 5mm, 8mm, 10mm is 1:1:8; Ball material mass ratio in ball grinder is 20:1, and drum's speed of rotation is 420rpm, and Ball-milling Time is 14h;
(3) powder of step (2) mechanical alloy process gained is loaded in graphite jig, vacuum sintering is carried out in plasma agglomeration stove, sintering temperature 340 DEG C, intensification duration 40min, insulation duration 10min, sintering pressure 40Mpa, the internal diameter of described graphite jig is Φ 23mm, obtains block materials.
Being undertaken cutting, polishing by sintering the block materials obtained, obtaining the sample of 3 × 3 × 15mm, test sample associated electrical performance; The test result of sample resistivity (ρ) and Seebeck coefficient (α) is distinguished as shown in Figure 1 and Figure 2, the power factor at each measuring tempeature point place is calculated according to ρ and α, as shown in Figure 3.As can see from Figure 3, Bi
2te
1.5s
1.5power factor constantly increase in experiment test temperature range, maximumly 250 DEG C time reach 587 μ Wm
-1k
-2.
Embodiment four: a kind of Bi
2teS
2the preparation method of thermoelectric material, comprises the steps:
(1) with the bismuth meal (Bi of 4N level, 200 orders), tellurium powder (Te, 100 orders), sulphur powder (S) is raw material, according to bismuth meal: tellurium powder: raw material is weighed mixing by the atomic ratio of sulphur powder=2:1:2, the total amount of three kinds of powder stocks is 15g, add the copper powder of 1at.% in raw material, to obtain better repeatability, the quality purity of described copper powder is greater than 99.99%;
(2) be positioned in ball grinder by step (1) mixed raw material, under argon shield atmosphere, carry out mechanical alloying process, in ball grinder, diameter is the mass ratio of the abrading-ball of 5mm, 8mm, 10mm is 1:1:8; Ball material mass ratio in ball grinder is 20:1, and drum's speed of rotation is 420rpm, Ball-milling Time 14h;
(3) powder of step (2) mechanical alloy process gained is loaded in graphite jig, vacuum sintering is carried out in plasma agglomeration stove, sintering temperature 320 DEG C, intensification duration 40min, insulation duration 10min, sintering pressure 35MPa, the internal diameter of described graphite jig is Φ 23mm, obtains block materials.
Being undertaken cutting, polishing by sintering the block materials obtained, obtaining the sample of 3 × 3 × 15mm, test sample associated electrical performance; The test result of sample resistivity (ρ) and Seebeck coefficient (α) is distinguished as shown in Figure 1 and Figure 2, calculate the power factor at each measuring tempeature point place according to ρ and α, as shown in Figure 3.As can see from Figure 3, Bi
2teS
2power factor constantly increase in Range of measuring temp, 360 μ Wm can be reached when probe temperature 250 DEG C
-1k
-2.
Claims (7)
1. a Bi
2te
3-xs
xthermoelectric material, comprises bismuth, tellurium element, it is characterized in that:
It is according to Bi
2te
3-xs
xthe atomic ratio determined of stoichiometric equation bismuth meal, tellurium powder, sulphur powder to be weighed mixing, through mechanical alloying process and sintering obtained, 0 < X < 3.
2. Bi as claimed in claim 1
2te
3-xs
xthermoelectric material, is characterized in that:
Before mechanical alloying process, in raw material, add the copper powder of 0.5at.% ~ 1at.%, to obtain better repeatability.
3. Bi described in claim 1
2te
3-xs
xthe preparation method of thermoelectric material, is characterized in that, comprises following step:
(1) with bismuth meal, tellurium powder, sulphur powder for raw material, according to synthesized Bi
2te
3-xs
xthe atomic ratio determined of stoichiometric equation raw material to be weighed mixing, need for subsequent operations, 0 < X < 3;
(2) step (1) mixed raw material is positioned in ball grinder, under argon shield atmosphere, carries out mechanical alloying process, the diameter 5mm ~ 10mm of abrading-ball in ball grinder;
(3) loaded in graphite jig by the powder of step (2) mechanical alloy process gained, sinter in plasma agglomeration stove, sintering environment is vacuum, obtains block materials.
4. preparation method as claimed in claim 3, is characterized in that:
Described in described step (1), the quality purity of each raw material is all greater than 99.99%, crosses 100 ~ 200 mesh sieves respectively before using to tellurium powder, bismuth meal.
5. preparation method as claimed in claim 3, is characterized in that:
In described step (2), the ball material mass ratio in ball grinder is 15:1 ~ 20:1, and rotating speed is 350 ~ 500rpm, and Ball-milling Time is 12 ~ 20h.
6. preparation method as claimed in claim 3, is characterized in that:
In described step (3), sintering temperature 320 DEG C ~ 450 DEG C, intensification duration 40min ~ 60min, insulation duration 10min ~ 15min, sintering pressure 35MPa ~ 50MPa.
7. the preparation method as described in claim 4,5 or 6, is characterized in that:
In described step (1), add the copper powder of 0.5at.% ~ 1at.% in raw material, to obtain better repeatability, the quality purity of described copper powder is greater than 99.99%.
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| CN112939078A (en) * | 2021-01-26 | 2021-06-11 | 昆明理工大学 | Method for improving performance of bismuth sulfide-based thermoelectric material |
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