CN101613814A - A kind of quick preparation n type Bi 2(Se xTe 1-x) 3The method of thermoelectric material - Google Patents
A kind of quick preparation n type Bi 2(Se xTe 1-x) 3The method of thermoelectric material Download PDFInfo
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Abstract
The present invention relates to a kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material.A kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material is characterized in that it comprises the steps: 1) be 2 according to the mol ratio of Bi powder, Te powder, Se powder: 3x: (3-3x), take by weighing Bi powder, Te powder and Se powder, wherein x is 0.08～0.12; Bi powder, Te powder and Se powder are mixed the back on tabletting machine, be pressed into block materials; 2) block materials that suppresses is obtained uniform Tellurobismuthite melt by the high-frequency induction heating fusion, then by single roller quench, the rotating speed of control whiff pressure and copper roller obtains thin band material; 3) thin band material is pulverized, dress adopts the discharge plasma sintering technology, by control sintering temperature, time, pressure, obtains n type Bi
2(Se
xTe
1-x)
3Thermoelectric material.This method has the advantages that technology is simple, preparation time is short.
Description
Technical field
The invention belongs to the new energy materials field, be specifically related to a kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material.
Background technology
Thermoelectric generation technology is to utilize the Sai Beike of semiconductor material (Seebeck) effect and Pa Er card (Peltier) effect to carry out the directly technology of conversion of energy, and efficiency of conversion depends primarily on zero dimension performance index ZT value (the ZT=α of material
2σ T/ κ, wherein α is the Seebeck coefficient; σ is a specific conductivity; T is an absolute temperature; κ is a thermal conductivity).Owing to do not contain the needed huge transmission rig of conventional energy transformation technology, thereby have that volume is little, reliability is high, manufacturing and characteristics such as running cost is low, the life-span long, manufacturing process is simple, application surface is very wide, thereby, be expected wide model and be applied to a large amount of and disperse the thermoelectric power generation of the low density heat energy (as solar heat, refuse burner waste heat, factory's heat extraction and vehicle exhaust heat extraction etc.) that exists as a kind of novel, the environmental harmony type clear energy sources switch technology of 21st century.In addition, at aerospace, ocean exploitation, fields such as military particular power source also have broad application prospects.
The Tellurobismuthite compound is to study the earliest, also is to develop one of the most sophisticated thermoelectric material at present, is widely used in the generating of refrigeration device and cold zone.The prepared n type Tellurobismuthite compound maximum heat electrical property figure of merit ZT of traditional technology (zone melting method) is 0.7～0.9, and needs long preparation time, be 3～5 days, and energy-output ratio is bigger.Therefore the research emphasis for bismuth telluride thermoelectric material is to seek novel preparation process, to obtain the block materials of thermoelectricity capability excellence.
Summary of the invention
The object of the present invention is to provide a kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material, this method have the advantages that technology is simple, preparation time is short.
To achieve these goals, technical scheme of the present invention is: a kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material is characterized in that it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 3x: (3-3x), taking by weighing Bi powder, Te powder and Se powder { is raw material with Bi powder, Te powder and Se powder promptly, according to Bi
2(Se
xTe
1-x)
3The stoichiometric ratio batching }, wherein x is 0.08～0.12; Bi powder, Te powder and Se powder are mixed the back on tabletting machine, be pressed into block materials; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses is put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, be 2～11A at electric current, voltage be under 100～500V with block materials heating and melting (be 15～30 seconds heat-up time), obtain uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is greater than 0.01MPa when getting rid of band, and the speed of rotation of copper roller is that (with different speed of cooling melt is thrown away, the speed of cooling of liquid phase quench is controlled at 10 to 500～5000r/min
5～10
6℃/sec between, the speed of rotation of speed of cooling by the copper roller regulated, corresponding copper roller rotating speed is 500～5000r/min), obtains thin band material and { promptly obtains having the Bi of nanometer laminated structure
2(Se
xTe
1-x)
3(0.08≤x≤0.12) thin band material, strip width are that 1～3mm, thickness are 5～60 μ m; The contact copper roll surface of strip is no crystalloid, and strip free surface (not contacting the copper roll surface) is dendritic };
3). thin band material is pulverized, and compacting in the graphite jig of packing into is put into discharge plasma sintering (SPS) equipment (or claiming stove) together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 40～100 ℃/min, and sintering temperature is 350～500 ℃, and pressure is 20～200MPa, and the sintering densification time is 4～6min; Sintering finishes postcooling to room temperature and takes out, and obtains n type Bi
2(Se
xTe
1-x)
3Thermoelectric material (being the layered nano-structure block sample of homogeneous grain size).
Heating mode is self-regulating temperature programming in the SPS sintering process, and pressuring method comprises the preceding plus-pressure of intensification and heated up the back before being sintered the material densification.
When the speed of rotation of copper roller was 1000～5000rpm, the SPS sintering temperature was 450 ℃, the Bi that sintering time obtains during for 5min
2(Se
xTe
1-x)
3The thermoelectricity capability figure of merit ZT of thermoelectric material reaches more than 0.7 at 300～460K, and to reach maximum value near 420K be 0.76.
So-called single roller quench, be initial feed to be heated into uniform melt by the ratio-frequency heating mode, melt is blown from the aperture of quartz glass tube bottom under certain argon gas spraying pressure, be ejected on the copper roller rotating at full speed and be thrown out of, change the speed of cooling of melt by the speed of rotation of regulating argon gas spraying pressure and copper roller, thereby obtain the thin ribbon shaped sample of different size.This preparation technology's distinguishing feature is that the fast and resulting sample crystal grain of speed is tiny.
Described single roller fast cooling device adopts day VF-RQT50 type atmosphere liquisol quenching device of reality wall company production.
So-called discharge plasma sintering (Spark Plasma Sintering, be called for short SPS), be by graphite pressure head up and down under vacuum condition, utilizing pulsed current direct heating and surface active in the sintered compact pressurization, the quick densifying of realization material under relatively low temperature and very short time.Compare with traditional sintering method, can save energy, improve equipment efficient, reduce cost and prepared block materials uniform crystal particles, density height.
The invention has the beneficial effects as follows:
1), preparation technology is simple, preparation time is short, processing parameter is controlled easily; The whole process of preparation of material only needs about 30min from the former block sample of expecting densification, and its preparation time melts legal system less than the tradition district and is equipped with block n type Bi
2Te
3One of percentage of material has been saved a large amount of time and the energy.
2), the present invention adopts discharge plasma agglomerating temperature low, the time is short, the energy-and time-economizing.
3), the resulting n type of the present invention Bi
2(Se
xTe
1-x)
3The thermoelectricity capability of thermoelectric material can compare favourably with the performance of the molten sample in commercialization district, and the space of further raising performance is arranged.Thermoelectricity capability figure of merit ZT of the present invention reaches more than 0.7 at 300～460K, and to reach maximum value near 420K be 0.76.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the molten sample of strip sample and district of embodiment 1, embodiment 2 and embodiment 3;
Fig. 2 a is field emission scanning electron microscope (FESEM) photo of the strip sample contact surface of embodiment 2;
Fig. 2 b is field emission scanning electron microscope (FESEM) photo on the strip sample free surface of embodiment 2;
Fig. 2 c is low power field emission scanning electron microscope (FESEM) photo of block sample behind the sintering of embodiment 2;
Fig. 2 d is high power field emission scanning electron microscope (FESEM) photo of block sample behind the sintering of embodiment 2;
Fig. 3 a is that the Seebeck coefficient of sample and the relation of temperature are melted in embodiment 1, embodiment 2 and embodiment 3 prepared material and districts;
Fig. 3 b is that the specific conductivity of sample and the relation of temperature are melted in embodiment 1, embodiment 2 and embodiment 3 prepared material and districts;
Fig. 3 c is that the thermal conductivity of sample and the relation of temperature are melted in embodiment 1, embodiment 2 and embodiment 3 prepared material and districts;
Fig. 3 d is that the zero dimension thermoelectric figure of merit ZT of sample and the relation of temperature are melted in embodiment 1, embodiment 2 and embodiment 3 prepared material and districts.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with example, but content of the present invention not only is confined to the following examples.
Embodiment 1:
A kind of quick preparation Bi
2(Se
0.08Te
0.92)
3The method of thermoelectric material, it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 0.24: 2.76, and taking by weighing Bi powder, Te powder and Se powder { is raw material with Bi powder, Te powder and Se powder promptly, according to Bi
2(Se
0.08Te
0.92)
3Stoichiometric ratio batching }; Bi powder, Te powder and Se powder total amount take by weighing 5g; The steel die of putting into 10mm after Bi powder, Te powder and the mixing of Se powder is pressed into block materials on tabletting machine; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses is put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, be that 2～11A, voltage are to heat under 100～500V 15～30 seconds at electric current, with the block materials heating and melting, obtain uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is 0.02MPa when getting rid of band, and the speed of rotation of copper roller is 4000r/min, and { the strip width is that 1～2mm, thickness are 15～20 μ m to obtain thin band material; The contact copper roll surface of strip is no crystalloid, and strip free surface (not contacting the copper roll surface) is dendritic }; Shown in Fig. 1 (embodiment 1), strip is monophasic Bi
2Te
3Structure.
3). thin band material is pulverized, and compacting in the graphite jig of the 12.7mm that packs into is put into discharge plasma sintering (SPS) equipment (or claiming stove) together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 100 ℃/min, and sintering temperature is 450 ℃, and pressure is 25MPa, and sintering time is 5min; Cool to room temperature after sintering finishes with the furnace and take out, obtain Bi
2(Se
0.08Te
0.92)
3Thermoelectric material (being the layered nano-structure block sample of homogeneous grain size).
With Bi
2(Se
0.08Te
0.92)
3Rectangular parallelepiped and thickness that thermoelectric material (being the block sample) cuts into 2mm * 2mm * 8.0mm are the disk of 1.5mm, are used to measure Sai Beike (Seebeck) coefficient, specific conductivity and thermal conductivity.Thin band material and block sample are carried out the thing identification of phases and microstructure analysis, and the block sample is carried out the thermoelectricity capability test.Prepared Bi
2(Se
0.08Te
0.92)
3The thermoelectricity capability of the molten sample of thermoelectric material and district and the relation of temperature are seen Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d.
Fig. 1 has illustrated that prepared sample is single-phase Bi
2Te
3, no dephasign exists; Fig. 3 a-Fig. 3 d has provided Seebeck coefficient, specific conductivity, thermal conductivity and the zero dimension thermoelectric figure of merit ZT of prepared embodiment one sample respectively.Resulting Bi has been described
2(Se
0.1Te
0.9)
3The ZT value of thermoelectric material sample reaches more than 0.5 at 400～480K, and thermoelectricity capability ZT reaches 0.53 when 460K.
Embodiment 2:
A kind of quick preparation Bi
2(Se
0.1Te
0.9)
3The method of thermoelectric material, it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 0.3: 2.70, and taking by weighing Bi powder, Te powder and Se powder { is raw material with Bi powder, Te powder and Se powder promptly, according to Bi
2(Se
0.1Te
0.9)
3Stoichiometric ratio batching }; Bi powder, Te powder and Se powder total amount take by weighing 5g; The steel die of putting into 10mm after Bi powder, Te powder and the mixing of Se powder is pressed into block materials on tabletting machine; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses is put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, be that 2～11A, voltage are to heat under 100～500V 15～30 seconds at electric current, with the block materials heating and melting, obtain uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is 0.02MPa when getting rid of band, and the speed of rotation of copper roller is 4000r/min, and { the strip width is that 1～2mm, thickness are 15～20 μ m to obtain thin band material; The contact copper roll surface of strip is no crystalloid, and strip free surface (not contacting the copper roll surface) is dendritic }; Shown in Fig. 1 (embodiment 2), strip is monophasic Bi
2Te
3Structure.
3). thin band material is pulverized, and compacting in the graphite jig of the 12.7mm that packs into is put into discharge plasma sintering (SPS) equipment (or claiming stove) together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 100 ℃/min, and sintering temperature is 450 ℃, and pressure is 25MPa, and sintering time is 5min; Cool to room temperature after sintering finishes with the furnace and take out, obtain Bi
2(Se
0.1Te
0.9)
3Thermoelectric material (being the layered nano-structure block sample of homogeneous grain size).
With Bi
2(Se
0.1Te
0.9)
3Rectangular parallelepiped and thickness that thermoelectric material (being the block sample) cuts into 2mm * 2mm * 8.0mm are the disk of 1.5mm, are used to measure Sai Beike (Seebeck) coefficient, specific conductivity and thermal conductivity.Thin band material and block sample are carried out the thing identification of phases and microstructure analysis, and the block sample is carried out the thermoelectricity capability test.Prepared Bi
2(Se
0.1Te
0.9)
3The thermoelectricity capability of the molten sample of thermoelectric material and district and the relation of temperature are seen Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d.
Fig. 1 has illustrated that prepared sample is single-phase Bi
2Te
3, no dephasign exists; Fig. 3 a-Fig. 3 d has provided Seebeck coefficient, specific conductivity, thermal conductivity and the zero dimension thermoelectric figure of merit ZT of prepared embodiment one sample respectively.Resulting Bi has been described
2(Se
0.1Te
0.9)
3The ZT value of thermoelectric material sample reaches more than 0.7 at 300～460K, and thermoelectricity capability ZT reaches 0.76 when 420K.
Embodiment 3:
A kind of quick preparation Bi
2(Se
0.12Te
0.88)
3The method of thermoelectric material, it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 0.36: 2.64, and taking by weighing Bi powder, Te powder and Se powder { is raw material with Bi powder, Te powder and Se powder promptly, according to Bi
2(Se
0.12Te
0.88)
3Stoichiometric ratio batching }; Bi powder, Te powder and Se powder total amount take by weighing 5g; The steel die of putting into 10mm after Bi powder, Te powder and the mixing of Se powder is pressed into block materials on tabletting machine; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses is put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, be that 2～11A, voltage are to heat under 100～500V 15～30 seconds at electric current, with the block materials heating and melting, obtain uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is 0.02MPa when getting rid of band, and the speed of rotation of copper roller is 4000r/min, and { the strip width is that 1～2mm, thickness are 15～20 μ m to obtain thin band material; The contact copper roll surface of strip is no crystalloid, and strip free surface (not contacting the copper roll surface) is dendritic }; Shown in Fig. 1 (embodiment 3), strip is monophasic Bi
2Te
3Structure.
3). thin band material is pulverized, and compacting in the graphite jig of the φ 12.7mm that packs into is put into discharge plasma sintering (SPS) equipment (or claiming stove) together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 100 ℃/min, and sintering temperature is 450 ℃, and pressure is 25MPa, and sintering time is 5min; Cool to room temperature after sintering finishes with the furnace and take out, obtain Bi
2(Se
0.12Te
0.88)
3Thermoelectric material (being the layered nano-structure block sample of homogeneous grain size).
With Bi
2(Se
0.12Te
0.88)
3Rectangular parallelepiped and thickness that thermoelectric material (being the block sample) cuts into 2mm * 2mm * 8.0mm are the disk of 1.5mm, are used to measure Sai Beike (Seebeck) coefficient, specific conductivity and thermal conductivity.Thin band material and block sample are carried out the thing identification of phases and microstructure analysis, and the block sample is carried out the thermoelectricity capability test.Prepared Bi
2(Se
0.12Te
0.88)
3The thermoelectricity capability of the molten sample of thermoelectric material and district and the relation of temperature are seen Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d.
Fig. 1 has illustrated that prepared sample is single-phase Bi
2Te
3, no dephasign exists; Fig. 3 a-Fig. 3 d has provided Seebeck coefficient, specific conductivity, thermal conductivity and the zero dimension thermoelectric figure of merit ZT of prepared embodiment one sample respectively.Resulting Bi has been described
2(Se
0.12Te
0.88)
3The ZT value of thermoelectric material sample reaches more than 0.65 at 400～500K, and thermoelectricity capability ZT reaches 0.72 when 440K.
Embodiment 4:
A kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material, it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 3x: (3-3x), taking by weighing Bi powder, Te powder and Se powder { is raw material with Bi powder, Te powder and Se powder promptly, according to Bi
2(Se
xTe
1-x)
3The stoichiometric ratio batching }, wherein x is 0.08; Bi powder, Te powder and Se powder are mixed the back on tabletting machine, be pressed into block materials; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses being put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, is that 2A, voltage are to heat under the 100V 15～30 seconds at electric current, with the block materials heating and melting, obtains uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is 0.011MPa when getting rid of band, and the speed of rotation of copper roller is 500r/min, obtains thin band material;
3). thin band material is pulverized, and compacting in the graphite jig of packing into is put into the discharge plasma agglomerating plant together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 40 ℃/min, and sintering temperature is 350 ℃, and pressure is 20MPa, and sintering time is 4min; Cool to room temperature after sintering finishes with the furnace and take out, obtain n type Bi
2(Se
xTe
1-x)
3Thermoelectric material (x is 0.08).
Embodiment 5:
A kind of quick preparation n type Bi
2(Se
xTe
1-x)
3The method of thermoelectric material, it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 3x: (3-3x), taking by weighing Bi powder, Te powder and Se powder { is raw material with Bi powder, Te powder and Se powder promptly, according to Bi
2(Se
xTe
1-x)
3The stoichiometric ratio batching }, wherein x is 0.12; Bi powder, Te powder and Se powder are mixed the back on tabletting machine, be pressed into block materials; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses being put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, is that 11A, voltage are to heat under the 500V 15～30 seconds at electric current, with the block materials heating and melting, obtains uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is 0.2MPa when getting rid of band, and the speed of rotation of copper roller is 5000r/min, obtains thin band material;
3). thin band material is pulverized, and compacting in the graphite jig of packing into is put into discharge plasma agglomerating plant (or claiming stove) together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 100 ℃/min, and sintering temperature is 500 ℃, and pressure is 200MPa, and sintering time is 6min; Cool to room temperature after sintering finishes with the furnace and take out, obtain n type Bi
2(Se
xTe
1-x)
3Thermoelectric material (x is 0.12).
The bound value and the interval value of each raw material of the present invention can both be realized the present invention, and the bound value of each processing parameter of the present invention and interval value can both realize the present invention, just do not enumerate embodiment one by one at this.
Claims (1)
1. one kind prepares n type Bi fast
2(Se
xTe
1-x)
3The method of thermoelectric material is characterized in that it comprises the steps:
1). the mol ratio according to Bi powder, Te powder, Se powder is 2: 3x: (3-3x), take by weighing Bi powder, Te powder and Se powder, wherein x is 0.08～0.12; Bi powder, Te powder and Se powder are mixed the back on tabletting machine, be pressed into block materials; Wherein the purity of Bi powder, Te powder, Se powder all 〉=99.99% (quality);
2). the block materials that suppresses being put into the silica tube of single roller fast cooling device, under the argon gas atmosphere protection, utilize the high-frequency induction heating mode, is 2～11A at electric current, voltage be under 100～500V with the block materials heating and melting, obtain uniform melt; Then melt is got rid of tape handling, the whiff pressure of argon gas is greater than 0.01MPa when getting rid of band, and the speed of rotation of copper roller is 500～5000r/min, obtains thin band material;
3). thin band material is pulverized, and compacting in the graphite jig of packing into is put into the discharge plasma agglomerating plant together with mould then, carries out sintering under less than the 10Pa vacuum condition; Temperature rise rate is 40～100 ℃/min, and sintering temperature is 350～500 ℃, and pressure is 20～200MPa, and sintering time is 4～6min; Sintering finishes postcooling to room temperature and takes out, and obtains n type Bi
2(Se
xTe
1-x)
3Thermoelectric material.
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| US10100437B2 (en) | 2013-06-25 | 2018-10-16 | Zhiming Chen | Method for manufacturing N-type semiconductor element for cooling or heating device |
| EP3016155A4 (en) * | 2013-06-25 | 2016-11-30 | Zhiming Chen | Method for manufacturing n-type semiconductor element for refrigeration or heating device |
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