CN102583274B - Method for preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis method - Google Patents
Method for preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis method Download PDFInfo
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- CN102583274B CN102583274B CN201210090379.0A CN201210090379A CN102583274B CN 102583274 B CN102583274 B CN 102583274B CN 201210090379 A CN201210090379 A CN 201210090379A CN 102583274 B CN102583274 B CN 102583274B
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- thermoelectric material
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Abstract
The invention discloses a method for preparing a silver telluride thermoelectric material by using an ordinary pressure microwave synthesis method and relates to a thermoelectric material and a preparation method thereof. The invention aims to solve the problems that process is complicated and reaction time is long in the process of preparing an alloy thermoelectric material with the existing method. The preparation method disclosed by the invention comprises the following steps of: 1, respectively dissolving Na2TeO3 and AgNO3 into a glycol solvent; 2, adding NaOH into the glycol solution of Na2TeO3 and then placing into an ordinary pressure microwave synthesis instrument, and reacting at a certain temperature until the solution is blue; 3, temporarily stopping the microwave synthesis instrument, pouring the glycol solution of AgNO3 prepared in advance into the blue solution, and then further reacting for a plurality of minutes; and 4, washing the obtained product with deionized water, and drying to obtain the silver telluride thermoelectric material. The method disclosed by the invention is low in reaction temperature, short in reaction time, simple in process and energy-saving, and is operated at ordinary pressure. The prepared material is uniform in powder particle, good in crystallization degree and high in yield. The method disclosed by the invention can be applied to the field of alloy thermoelectric materials.
Description
Technical field
The present invention relates to a kind of thermoelectric material and preparation method, belong to the alloy thermoelectric material field in functional materials; Be specifically related to a kind of Ag
2te thermoelectric material and preparation method thereof.
Background technology
Thermoelectric power generation and thermoelectric refrigeration are as a class solid state energy conversion regime, compare with other energy transformation mode, there is movement-less part, noiseless, easy microminiaturized, safe and reliable, the feature such as can work under severe environment, but because its transformation efficiency is on the low side, so thermoelectric conversion device only for reliability and accessibility than the prior limited occasion of economy, be difficult to Industry Promotion and form huge market.The key that improves thermoelectric conversion device efficiency is to prepare high performance thermoelectric material, and in recent years, Nanoalloy thermoelectric material is the focus of various countries scientist research.In numerous Nanoalloy thermoelectric materials, Ag
2te, because the ZT value having compared with high receives much attention, is a kind of good middle low-temperature thermoelectric material.
At present existing multiple preparation nanometer Ag
2the method of Te thermoelectric material, but the most of complex process of these methods, power consumption, consuming time, by comparison, normal pressure microwave is synthetic has that rate of heating is fast, heat utilization rate is high, energy-conserving and environment-protective, be quick on the draw, high quality, in nano material is synthetic, obtained many application, and relevant Ag
2the synthetic report that has no up to now of normal pressure microwave method of Te nano wire.
Summary of the invention
The object of the invention is preparing alloy thermoelectric material pattern heterogeneity in order to solve existing method, the problem that thermoelectricity capability is poor, and a kind of method of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis is provided.
The method of a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis of the present invention is to realize according to the following steps: one, by Na
2teO
3with the ethylene glycol solvent ratio that is 0.4～0.5g:35mL in mass volume ratio at ambient temperature, with the speed of 500～600 revs/min, stir 1～3min, obtain solution A; Separately by AgNO
3with the ethylene glycol solvent ratio that is 0.6～0.7g:10mL in mass volume ratio at ambient temperature, with the speed of 500～600 revs/min, stir 1～3min, obtain solution B; Two, after the ratio that solution A NaOH being obtained with step 1 is 0.2g:30～40mL in mass volume ratio mixes, put into normal pressure microwave synthesizer, at power, be 200～400W, temperature is to react 2～3min under the condition of 170 ℃～180 ℃, obtains solution C; Three, the solution C that solution B step 1 being obtained obtains with step 2 is by volume for the ratio of 10:30～40 mixes, put into normal pressure microwave synthesizer, at power, be 200～400W, temperature is to react 12～15min under the condition of 170 ℃～180 ℃, obtains head product; Four, head product step 3 being obtained deionized water wash 4～6 times after dry 20～30min, obtain silver telluride thermoelectric material at the temperature of 50 ℃～70 ℃.
Beneficial effect of the present invention is:
The present invention adopts Na
2teO
3and AgNO
3as the raw material of microwave building-up reactions, and take ethylene glycol as solvent, by NaOH regulator solution pH value, the Ag making
2the crooked nano wire pattern of Te homogeneous, narrow particle size distribution; Adopt normal pressure microwave synthesis method to prepare Ag
2short 13～the 18min of generated time of Te, and existing hydrothermal method is prepared Ag
2the time of Te is 12h, and sample purity is 99%, energy consumption is little, normal-temperature operation, technique are simple, safe.From prepared Ag
2the electric property of Te thermoelectric material varies with temperature curve can be found out, Ag of the present invention
2the power factor of Te thermoelectric material in the time of 180 ℃ reaches 13.5 * 10
-4wm
-1k
-2, show good electric property.
Accompanying drawing explanation
Fig. 1 is test 1 Ag making
2the XRD figure spectrum of Te powder;
Fig. 2 is test 1 Ag making
2the SEM collection of illustrative plates of Te powder;
Fig. 3 is test 1 Ag making
2the specific conductivity collection of illustrative plates of Te powder;
Fig. 4 is test 1 Ag making
2the Seebeck coefficient collection of illustrative plates of Te powder;
Fig. 5 is test 1 Ag making
2the power factor collection of illustrative plates of Te powder.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination of other embodiment.
Embodiment one: the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis of present embodiment is to realize according to the following steps: one, by Na
2teO
3with the ethylene glycol solvent ratio that is 0.4～0.5g:35mL in mass volume ratio at ambient temperature, with the speed of 500～600 revs/min, stir 1～3min, obtain solution A; Separately by AgNO
3with the ethylene glycol solvent ratio that is 0.6～0.7g:10mL in mass volume ratio at ambient temperature, with the speed of 500～600 revs/min, stir 1～3min, obtain solution B; Two, after the ratio that solution A NaOH being obtained with step 1 is 0.2g:30～40mL in mass volume ratio mixes, put into normal pressure microwave synthesizer, at power, be 200～400W, temperature is to react 2～3min under the condition of 170 ℃～180 ℃, obtains solution C; Three, the solution C that solution B step 1 being obtained obtains with step 2 is by volume for the ratio of 10:30～40 mixes, put into normal pressure microwave synthesizer, at power, be 200～400W, temperature is to react 12～15min under the condition of 170 ℃～180 ℃, obtains head product; Four, head product step 3 being obtained deionized water wash 4～6 times after dry 20～30min, obtain silver telluride thermoelectric material at the temperature of 50 ℃～70 ℃.
Present embodiment adopts Na
2teO
3and AgNO
3as the raw material of microwave building-up reactions, and take ethylene glycol as solvent, by NaOH regulator solution pH value, the Ag making
2the crooked nano wire pattern of Te homogeneous, narrow particle size distribution; Adopt normal pressure microwave synthesis method to prepare Ag
2short 13～the 18min of generated time of Te, and existing hydrothermal method is prepared Ag
2the time of Te is 12h, and sample purity is 99%, energy consumption is little, normal-temperature operation, technique are simple, safe.From prepared Ag
2the electric property of Te thermoelectric material varies with temperature curve can be found out, the Ag of present embodiment
2the power factor of Te thermoelectric material in the time of 180 ℃ reaches 13.5 * 10
-4wm
-1k
-2, show good electric property.
Embodiment two: present embodiment is from specifically embodiment one is different: the Na described in step 1
2teO
3with ethylene glycol solvent by mass volume ratio, be 0.422g:35mL.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is from specifically embodiment one to two is different: the AgNO described in step 1
3with ethylene glycol solvent by mass volume ratio, be 0.68g:10mL.Other step and parameter are identical with embodiment one to two.
Embodiment four: present embodiment is from specifically one of embodiment one to three is different: the solution A that the NaOH described in step 2 and step 1 obtain is 0.2g:35mL by mass volume ratio.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is from specifically one of embodiment one to four is different: the temperature described in step 2 and step 3 is 175 ℃.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is from specifically one of embodiment one to five is different: the reaction times described in step 2 is 2.5min.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is from specifically one of embodiment one to six is different: the solution C that the solution B that the step 1 described in step 3 obtains and step 2 obtain is 10:35 by volume.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is from specifically one of embodiment one to seven is different: the reaction times described in step 3 is 14min.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is from specifically one of embodiment one to eight is different: the temperature described in step 4 is 60 ℃.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: present embodiment is from specifically one of embodiment one to nine is different: be 25min the time of drying described in step 4.Other step and parameter are identical with one of embodiment one to nine.
By following verification experimental verification effect of the present invention:
The method of a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis of this test is to realize according to the following steps: the Na that, gets 2mmol
2teO
3be dissolved in the ethylene glycol solvent of 35mL, at room temperature, with the speed of 600 revs/min, stir 2min, obtain solution A; Get the AgNO of 4mmol
3be dissolved in the ethylene glycol solvent of 10mL, at room temperature, with the speed of 600 revs/min, stir 2min, obtain solution B; Two, solution A step 1 being obtained is poured in 50mL glass there-necked flask, after adding the NaOH of 0.2g to mix, puts into normal pressure microwave synthesizer, at power, is 300W, and temperature is that under the condition of 180 ℃, reaction 3min, obtains solution C; Three, the 10mL solution B solution C of step 2 35mL being obtained with step 1 mixes, and puts into normal pressure microwave synthesizer, at power, is 300W, and temperature is under the condition of 180 ℃, and reaction 15min, obtains head product; Four, head product step 3 being obtained deionized water wash 5 times after dry dry 25min, obtain Ag at the temperature of 60 ℃
2te powder.
The normal pressure microwave synthesizer using in this test is MAS-II type, buys from Xinyi Microwave Chemistry Tech Co., Ltd..
The raw material using in this test is commercially available analytical pure raw material.
The Ag that this test is obtained
2te powder carries out XRD detection, result as shown in Figure 1, as shown in Figure 1, in figure all diffraction peak all with monoclinic phase Ag
2te(standard card JCPDS34-0142) diffraction peak is coincide, and does not find the diffraction peak of other impurity, illustrates that prepared sample is Ag
2te pure phase.
Ag to this test
2te powder carries out SEM detection, result as shown in Figure 2, as shown in Figure 2, the Ag of this test
2te morphology microstructure is crooked nano wire, and the diameter of nano wire is 100～200nm, and length is 5～10 μ m.
Under normal temperature 16Mpa, the Ag that this test is obtained
2te powder is pressed into long strip shape block, respectively it is carried out the test of specific conductivity and Seebeck coefficient, and calculates its power factor.Ag
2the specific conductivity of Te block varies with temperature graphic representation as shown in Figure 3, as can be seen from Figure 3, and Ag
2the specific conductivity of Te, with the first slow decreasing of temperature, then sharply reduces between 400K-500K, according to bibliographical information, and Ag
2can there is crystal transition in 410K left and right in Te, by low temperature monoclinic phase (β-Ag
2te) change high temperature center of area Emission in Cubic (α-Ag into
2te), low temperature monoclinic phase belongs to narrow gap semiconductor, have good electroconductibility, and high temperature center of area Emission in Cubic is with unordered Ag
+be main ionophore, Ag
+concentration differs several orders of magnitude before and after changing, and larger reduction has just occurred electronic conductance like this.From Fig. 3, it can also be seen that, along with the continuation rising of temperature, there is flex point in 550K left and right in specific conductivity, and this may be that oxidation has occurred sample because the resistance to air loss of test later stage body of heater is bad, thereby causes specific conductivity to reduce.
Ag
2the Seebeck coefficient of Te block varies with temperature graphic representation as shown in Figure 4, and as can be seen from Figure 4, prepared material is p-type thermoelectric material, curve first rises and declines afterwards, in 400K left and right, also occurred flex point, this is consistent with the flex point that specific conductivity curve occurs, Ag is described
2te in about 400K, occurred crystal transition
In conjunction with specific conductivity and Seebeck coefficient test result, we have carried out power factor calculating to sample, result as shown in Figure 5, as can be seen from Figure 5, Ag
2with the rising first increases and then decreases of temperature, there is maximum value in 450K left and right in the power factor of Te, maximum value reaches 13.5 * 10
-4wm
-1k
-2, Ag prepared by this test is described
2te powder has better electric property.
Claims (10)
1. a method for preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis, is characterized in that the method for preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis is carried out according to the following steps: one, by Na
2teO
3with the ethylene glycol solvent ratio that is 0.4～0.5g:35mL in mass volume ratio at ambient temperature, with the speed of 500～600 revs/min, stir 1～3min, obtain solution A; Separately by AgNO
3with the ethylene glycol solvent ratio that is 0.6～0.7g:10mL in mass volume ratio at ambient temperature, with the speed of 500～600 revs/min, stir 1～3min, obtain solution B; Two, after the ratio that solution A NaOH being obtained with step 1 is 0.2g:30～40mL in mass volume ratio mixes, put into normal pressure microwave synthesizer, at power, be 200～400W, temperature is to react 2～3min under the condition of 170 ℃～180 ℃, obtains solution C; Three, the solution C that solution B step 1 being obtained obtains with step 2 is by volume for the ratio of 10:30～40 mixes, put into normal pressure microwave synthesizer, at power, be 200～400W, temperature is to react 12～15min under the condition of 170 ℃～180 ℃, obtains head product; Four, head product step 3 being obtained deionized water wash 4～6 times after dry 20～30min, obtain silver telluride thermoelectric material at the temperature of 50 ℃～70 ℃.
2. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the Na described in step 1
2teO
3with ethylene glycol solvent by mass volume ratio, be 0.422g:35mL.
3. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the AgNO described in step 1
3with ethylene glycol solvent by mass volume ratio, be 0.68g:10mL.
4. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the solution A that NaOH described in step 2 and step 1 obtain is 0.2g:35mL by mass volume ratio.
5. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the temperature described in step 2 and step 3 is 175 ℃.
6. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the reaction times described in step 2 is 2.5min.
7. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the solution C that solution B that the step 1 described in step 3 obtains and step 2 obtain is 10:35 by volume.
8. the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis according to claim 1, is characterized in that the reaction times described in step 3 is 14min.
9. according to the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis claimed in claim 1, it is characterized in that the temperature described in step 4 is 60 ℃.
10. according to the method for a kind of preparing silver telluride thermoelectric material by using ordinary pressure microwave synthesis claimed in claim 1, it is characterized in that be 25min the time of drying described in step 4.
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| CN113443609B (en) * | 2021-07-02 | 2022-03-08 | 之江实验室 | Novel-phase two-dimensional galena silver telluride synthesized based on two-dimensional tellurium template method and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654747A (en) * | 2009-08-14 | 2010-02-24 | 哈尔滨工业大学 | Preparation method of AgPb10SbTe12 thermoelectric material |
| CN101711970A (en) * | 2009-12-18 | 2010-05-26 | 南京航空航天大学 | Multifunctional ultrasonic microwave collaborative chemical reactor and method for preparing nano semiconductor chalcogenide by using same |
| CN101906665A (en) * | 2010-09-09 | 2010-12-08 | 哈尔滨工业大学 | Method for preparing silver-lead-lanthanum-tellurium thermoelectric material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654747A (en) * | 2009-08-14 | 2010-02-24 | 哈尔滨工业大学 | Preparation method of AgPb10SbTe12 thermoelectric material |
| CN101711970A (en) * | 2009-12-18 | 2010-05-26 | 南京航空航天大学 | Multifunctional ultrasonic microwave collaborative chemical reactor and method for preparing nano semiconductor chalcogenide by using same |
| CN101906665A (en) * | 2010-09-09 | 2010-12-08 | 哈尔滨工业大学 | Method for preparing silver-lead-lanthanum-tellurium thermoelectric material |
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