CN101602494B - Sonochemistry method for preparing AgSbTe2 thermoelectric compound powder - Google Patents

Sonochemistry method for preparing AgSbTe2 thermoelectric compound powder Download PDF

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CN101602494B
CN101602494B CN2009100631934A CN200910063193A CN101602494B CN 101602494 B CN101602494 B CN 101602494B CN 2009100631934 A CN2009100631934 A CN 2009100631934A CN 200910063193 A CN200910063193 A CN 200910063193A CN 101602494 B CN101602494 B CN 101602494B
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thermoelectric compound
agsbte
compound powder
agsbte2
deionized water
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CN101602494A (en
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唐新峰
徐静静
杜保立
张文浩
张清杰
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a method for preparing AgSbTe2 thermoelectric compound powder, in particular to a sonochemistry method for preparing the AgSbTe2 thermoelectric compound powder. The method is characterized by including the following steps: 1) deionized water is used as solvent, and analytically pure AgNO3, C4H4KO7Sb-1/2H2O and TeO2 are added to and stirred and mixed with the solvent, thereby obtaining mixed liquid A; 2) ammonia is poured into the mixed liquid A, and the mixture obtained is processed by ultrasound for 30 minutes, thereby obtaining mixed liquid B; 3) reducing agent NaBH4 is added to and thoroughly reacts with the mixed liquid B under ultrasound for 2 to 6 hours, thereby obtaining a product C; 4) the product C obtained in the step 3) is centrifuged and is dried in a vacuum drying oven to obtain a precursor of the AgSbTe2 thermoelectric compound; and 5) the precursor obtained in the step 4) is processed by reduction in hydrogen at 450 to 500 DEG C for 1 to 4 hours, thereby obtaining the AgSbTe2 thermoelectric compound powder. The method has the advantages of low-cost and easily accessed raw materials, simple and easily controlled technology, short reaction time, low energy consumption, high safety, favorable repeatability and no pollution, and can be used for large-scale preparation.

Description

AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder
Technical field
The invention belongs to the new energy materials field, be specifically related to a kind of AgSbTe 2The preparation method of thermoelectric compound powder.
Background technology
Thermoelectric generation technology is to utilize the Seebeck effect of semi-conductor thermoelectric material heat energy to be directly changed into the technology of electric energy.Because it does not contain the needed huge transmission rig of other generation technology, have that volume is little, the life-span is long, reliability is high, manufacturing process is simple, manufacturing and characteristics such as running cost is low, wide application and be subjected to scientific worker's attention, at numerous areas vast potential for future development is arranged.
AgSbTe 2Compound is research a kind of p type thermoelectric material early, has low-down lattice thermal conductivity under the normal temperature and makes this material have the ZT value high than other traditional materials.Because this material at low temperature is down unstable, often has heterogeneous structure, the performance of its stability there is certain influence.Therefore need the synthetic single AgSbTe of phase composite 2Polycrystalline compounds improves its thermoelectricity capability.At present, for AgSbTe 2The preparation method of polycrystalline compounds has solid reaction process (Solid state reaction, SSR), scorification (Melt reaction, MR), mechanical alloying (Mechanicai alloying, MA), but aforesaid method needs high temperature or reaction time longer, energy consumption is bigger, and the AgSbTe that obtains of different preparation methods 2Thing phase, microstructure and the performance of polycrystalline material are different, are difficult to obtain the single compound of phase composite.
Summary of the invention
The object of the present invention is to provide a kind of AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder, this method raw material is cheap and easy to get, technology is simple and easy to control, the reaction times is short.
To achieve these goals, technical scheme of the present invention is: AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder is characterized in that it comprises the steps:
1) presses deionized water: AgNO 3In Ag +: C 4H 4KO 7Sb1/2H 2Sb among the O 3+: TeO 2In Te 4+Proportioning be 1L: 0.0166～0.02mol: 0.02～0.0212mol: 0.04mol, choose deionized water, AgNO 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, standby;
Deionized water as solvent, is added analytically pure AgNO then 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, and mix, obtain mixed solution A and (form Ag in the mixed solution A +, Sb 3+, Te 4+Three metal ion species concentration are respectively 0.0166～0.02mol/L, 0.02～0.0212mol/L, 0.04mol/L);
2) be to measure ammoniacal liquor at 8: 100 by the volume ratio of ammoniacal liquor and mixed solution A, ammoniacal liquor poured in the mixed solution A that ultrasonic 30min obtains mixing solutions B;
3) press mixing solutions B and reductive agent NaBH 4Proportioning be 1L: 0.08mol, choose reductive agent NaBH 4In mixing solutions B, add reductive agent NaBH 4(concentration is 0.08mol/L), ultrasonic abundant reaction 2～6 hours obtains product C;
4) product C that step 3) is obtained is carried out centrifugal (time is 3min, and rotating speed is 8000rpm), centrifugal obtain be deposited in the vacuum drying oven dry (temperature is 60 ℃, and the time is 6h), obtain AgSbTe 2The presoma of thermoelectric compound;
5) presoma that step 4) is obtained in 1～4 hour (placing atmosphere furnace) of 450～500 ℃ of reduction, obtains AgSbTe under hydrogen atmosphere 2Thermoelectric compound powder.
The AgSbTe that the present invention obtains 2Thermoelectric compound powder can be applied to prepare AgSbTe 2Block thermoelectric material.
Described ultransonic frequency is that 42KHz, power are 100-400W.
The invention has the beneficial effects as follows: the ultrasonic method of employing makes carries out reduction heat behind forerunner's powder and handles and obtain required thing phase, and forerunner's powder activity is bigger, and reduction heat is handled and is easy to obtain AgSbTe 2Powder need not long-time solid state reaction or ball milling.This method raw material is cheap and easy to get, and technology is simple and easy to control, and the reaction times is short, and energy consumption is low, safety non-pollution, and good reproducibility, and can be used for mass preparation.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the AgSbTe of the embodiment of the invention 1 preparation 2The XRD figure spectrum of thermoelectric compound precursor.
Fig. 3 is the AgSbTe of the embodiment of the invention 1 preparation 2The SEM shape appearance figure of thermoelectric compound precursor.
Fig. 4 is the AgSbTe of the embodiment of the invention 1 preparation 2The XRD figure spectrum of thermoelectric compound.
Fig. 5 is the AgSbTe of the embodiment of the invention 1 preparation 2The SEM shape appearance figure of thermoelectric compound.
Fig. 6 is the AgSbTe of the embodiment of the invention 1 preparation 2The EDS collection of illustrative plates of thermoelectric compound.
Fig. 7 is the AgSbTe of the embodiment of the invention 2 preparations 2The XRD figure spectrum of thermoelectric compound.
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:
As shown in Figure 1, AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder, it comprises the steps:
1) presses deionized water: AgNO 3In Ag +: C 4H 4KO 7Sb1/2H 2Sb among the O 3+: TeO 2In Te 4+Proportioning be 1L: 0.0166mol: 0.0212mol: 0.04mol, choose deionized water, AgNO 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, standby;
Deionized water as solvent, is added analytically pure AgNO then 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, and mix, obtain mixed solution A;
2) be to measure ammoniacal liquor at 8: 100 by the volume ratio of ammoniacal liquor and mixed solution A, ammoniacal liquor poured in the mixed solution A that ultrasonic 30min obtains mixing solutions B;
3) press mixing solutions B: reductive agent NaBH 4Proportioning be 1L: 0.08mol, choose reductive agent NaBH 4In mixing solutions B, add reductive agent NaBH 4(concentration is 0.08mol/L), ultrasonic abundant reaction 6 hours obtains product C;
4) product C that step 3) is obtained is carried out centrifugal (time is 3min, and rotating speed is 8000rpm), centrifugal obtain be deposited in the vacuum drying oven dry (temperature is 60 ℃, and the time is 6h), obtain AgSbTe 2The presoma of thermoelectric compound;
5) presoma that step 4) is obtained in 500 ℃ of reductase 12s hour (placing atmosphere furnace), obtains AgSbTe under hydrogen atmosphere 2Thermoelectric compound powder (final product).
Described ultransonic frequency is that 42KHz, power are 100-400W.
Fig. 2 illustrates that resulting precursor is not for single-phase; Fig. 3 illustrates below the gained precursor particle size 50nm.Fig. 4 illustrates that the gained final product is single-phase AgSbTe 2Thermoelectric compound; Fig. 5 illustrates gained AgSbTe 2Thermoelectric compound is blocky-shaped particle size～10 μ m.Fig. 6 illustrates gained AgSbTe 2Thermoelectric compound meets its stoichiometric ratio substantially.
Embodiment 2:
As shown in Figure 1, AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder, it comprises the steps:
1) presses deionized water: AgNO 3In Ag +: C 4H 4KO 7Sb1/2H 2Sb among the O 3+: TeO 2In Te 4+Proportioning be 1L: 0.02mol: 0.02mol: 0.04mol, choose deionized water, AgNO 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, standby;
Deionized water as solvent, is added analytically pure AgNO then 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, and mix, obtain mixed solution A and (form Ag in the mixed solution A +, Sb 3+, Te 4+Three metal ion species concentration are respectively 0.0166mol/L, 0.02mol/L, 0.04mol/L);
2) be to measure ammoniacal liquor at 8: 100 by the volume ratio of ammoniacal liquor and mixed solution A, ammoniacal liquor poured in the mixed solution A that ultrasonic 30min obtains mixing solutions B;
3) press mixing solutions B: reductive agent NaBH 4Proportioning be 1L: 0.08mol, choose reductive agent NaBH 4In mixing solutions B, add reductive agent NaBH 4(concentration is 0.08mol/L), ultrasonic abundant reaction 2 hours obtains product C;
4) product C that step 3) is obtained is carried out centrifugal (time is 3min, and rotating speed is 8000rpm), centrifugal obtain be deposited in the vacuum drying oven dry (temperature is 60 ℃, and the time is 6h), obtain AgSbTe 2The presoma of thermoelectric compound;
5) presoma that step 4) is obtained in 4 hours (placing atmosphere furnace) of 450 ℃ of reduction, obtains AgSbTe under hydrogen atmosphere 2Thermoelectric compound powder (final product).
Fig. 7 illustrates that resulting final product is single-phase AgSbTe 2Thermoelectric compound.
Embodiment 3:
As shown in Figure 1, AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder, it comprises the steps:
1) presses deionized water: AgNO 3In Ag +: C 4H 4KO 7Sb1/2H 2Sb among the O 3+: TeO 2In Te 4+Proportioning be 1L: 0.0176mol: 0.0204mol: 0.04mol, choose deionized water, AgNO 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, standby;
Deionized water as solvent, is added analytically pure AgNO then 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, and mix, obtain mixed solution A and (form Ag in the mixed solution A +, Sb 3+, Te 4+Three metal ion species concentration are respectively 0.02mol/L, 0.0212mol/L, 0.04mol/L);
2) be to measure ammoniacal liquor at 8: 100 by the volume ratio of ammoniacal liquor and mixed solution A, ammoniacal liquor poured in the mixed solution A that ultrasonic 30min obtains mixing solutions B;
3) press mixing solutions B: reductive agent NaBH 4Proportioning be 1L: 0.08mol, choose reductive agent NaBH 4In mixing solutions B, add reductive agent NaBH 4(concentration is 0.08mol/L), ultrasonic abundant reaction 6 hours obtains product C;
4) product C that step 3) is obtained is carried out centrifugal (time is 3min, and rotating speed is 8000rpm), centrifugal obtain be deposited in the vacuum drying oven dry (temperature is 60 ℃, and the time is 6h), obtain AgSbTe 2The presoma of thermoelectric compound;
5) presoma that step 4) is obtained in 1 hour (placing atmosphere furnace) of 500 ℃ of reduction, obtains AgSbTe under hydrogen atmosphere 2Thermoelectric compound powder.
The bound value and the interval value of each raw material of the present invention can both be realized the present invention, just do not enumerate embodiment one by one at this.

Claims (1)

1.AgSbTe 2The sonochemistry preparation method of thermoelectric compound powder is characterized in that it comprises the steps:
1) presses deionized water: AgNO 3In Ag +: C 4H 4KO 7Sb1/2H 2Sb among the O 3+: TeO 2In Te 4+Proportioning be 1L: 0.0166～0.02mol: 0.02～0.0212mol: 0.04mol, choose deionized water, AgNO 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, standby;
Deionized water as solvent, is added analytically pure AgNO then 3, C 4H 4KO 7Sb1/2H 2O and TeO 2, and mix, obtain mixed solution A;
2) be to measure ammoniacal liquor at 8: 100 by the volume ratio of ammoniacal liquor and mixed solution A, ammoniacal liquor poured in the mixed solution A that ultrasonic 30min obtains mixing solutions B;
3) press mixing solutions B and reductive agent NaBH 4Proportioning be 1L: 0.08mol, choose reductive agent NaBH 4In mixing solutions B, add reductive agent NaBH 4, ultrasonic abundant reaction 2～6 hours obtains product C;
4) product C that step 3) is obtained carry out centrifugal, centrifugal obtain be deposited in the vacuum drying oven dryly, obtain AgSbTe 2The presoma of thermoelectric compound;
The centrifugal time is 3min, centrifugal rotation speed 8000rpm; Drying temperature is 60 ℃, and the time is 6h;
5) presoma that step 4) is obtained in 450～500 ℃ of reduction 1～4 hour, obtains AgSbTe under hydrogen atmosphere 2Thermoelectric compound powder.
CN2009100631934A 2009-07-17 2009-07-17 Sonochemistry method for preparing AgSbTe2 thermoelectric compound powder Expired - Fee Related CN101602494B (en)

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