CN109728156A - A kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material - Google Patents
A kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 45
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910002688 Ag2Te Inorganic materials 0.000 claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910004273 TeO3 Inorganic materials 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 229910001215 Te alloy Inorganic materials 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 230000005619 thermoelectricity Effects 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000012512 characterization method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
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- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
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Abstract
The present invention relates to field of thermoelectric material technique, specifically disclose a kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material, comprising the following steps: step (1) powder preparation: by Na2TeO3Powder and AgNO3Powder dissolves makes the molar ratio of Ag and Te in solution not less than 2:1 in a solvent, and reducing agent is added afterwards, obtains mixed solution, by mixed solution in 100~140 DEG C of heat preservation 6-24h, carries out hydro-thermal reaction, cleans and be dried to obtain afterwards Ag-Ag2Te alloy powder；Step (2) block preparation: by Ag-Ag obtained in step (1)2Te alloy powder is sintered using plasma discharging technique, by Ag-Ag2Te alloy powder pours into graphite jig, is 400-500 DEG C in temperature, under conditions of pressure is 10-50MPa, sintering time 5-30min obtains the Ag of Ag auto-dope2Te material.The Ag of Ag auto-dope has been prepared using the technical solution of this patent2Te thermoelectric material, thermoelectric figure of merit are higher than pure Ag2Te material.
Description
Technical field
The present invention relates to field of thermoelectric material technique, in particular to a kind of Ag of Ag auto-dope2The preparation of Te thermoelectric material
Method.
Background technique
The performance of thermoelectric material is characterized by dimensionless thermoelectric figure of merit ZT, ZT=σ S2T/ κ, σ, κ, S and T distinguish among these
Indicate conductivity, thermal conductivity, Seebeck coefficient and absolute temperature.T value takes the average value of hot end and cold junction temperature.ZT value more it is high just
Show that the thermoelectricity capability of the material is better, and high ZT value needs to exist simultaneously big Seebeck coefficient, big conductance in material
Rate and low thermal conductivity, but due to the relationship between these parameters there is coupling promote ZT value within a very long time all
It is a kind of challenge.
Ag2A kind of semiconductor material (at room temperature Eg~0.09eV) of the Te as narrowband possesses many special performances,
Become the low-temperature thermoelectric material haveing excellent performance: (1) Ag2The higher mobility of Ag atom and irregular structure are led in Te lattice
The lower thermal conductivity of cause.(2) high conductivity caused by high electron mobility.It (3) can be by preparing non-stoichiometric
Ag2Donor and acceptor's energy level that Te is created respectively adjusts carrier concentration.(4) occur near 418K temperature by monoclinic phase
To the phase transition process of cubic phase transition.
Currently, powder Ag2The preparation method of Te is very more, and common method mainly has hydrothermal synthesis and ball-milling method, due to
Ag2Te is using in hydro-thermal method synthesis process, and Te element can be entered in solution in the form of ion, so that Te element is losing
While can also introduce the second phase of Ag, since in thermoelectric material industry, everybody usually thinks that two different materials are not sent out
It is biochemical reaction and only physical mixed when, the thermoelectricity capability of the material is poor, therefore everybody will be considered that Ag2Te material
The introducing of the second phase of Ag in material, thermoelectricity capability will appear decline certainly and obtain phenomenon.
Therefore it is based on this understanding, the technical staff in industry would generally consider how to avoid in Ag2It is introduced in Te material
The second phase of Ag, and everybody widespread practice are as follows: one, by adjusting the proportion of Ag and Te, to obtain pure Ag2Te, inventor
It was found that single-phase Ag can be obtained by hydrothermal synthesis when the proportion of Ag and Te is adjusted to 2:1.052Te cable architecture；Two, lead to
Cross ball milling legal system Ag2Nanocrystalline loss introducing the second phase of Ag to avoid Te element of Te.
Summary of the invention
The present invention provides a kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material has obtained thermoelectric figure of merit and has been higher than
Pure Ag2The Ag of the Ag auto-dope of Te2Te thermoelectric material, thermoelectricity capability are obviously improved.
In order to achieve the above object, base case of the invention are as follows:
A kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material, comprising the following steps:
The preparation of step (1) powder: the molar ratio of Ag and Te is not less than to the Na of 2:12TeO3Powder and AgNO3Powder dissolution
In a solvent, reducing agent 0.4-1.2ml is added afterwards, obtains mixed solution, by mixed solution in 100~140 DEG C of heat preservation 6-24h,
Hydro-thermal reaction is carried out, by cleaning and be dried to obtain Ag-Ag2Te alloy powder；
Step (2) block preparation: by Ag-Ag obtained in step (1)2Te alloy powder using plasma discharging technique into
Row sintering, sintering temperature are 400-500 DEG C, and sintering pressure is 10-50MPa, and sintering time 5-30min obtains Ag auto-dope
Ag2Te material.
The technical principle and effect of this base case are:
1, inventor is preparing pure Ag2When Te material, in order to set off pure Ag2Te conducting material thermoelectricity performance is better than introducing
The Ag of the second phase of Ag2The thermoelectricity capability of Te material, therefore to the Ag for introducing the second phase of Ag2Te using discharge plasma sintering technique into
Row sintering, and find during the sintering process, Ag2The second phase of Ag has been added to Ag again while the grain growth of Te2In Te phase,
Realize the auto-dope of the second phase of Ag.
Since the auto-dope of Ag simple substance helps to improve the concentration of carrier, and inventor by creating donor level
The Ag of Ag auto-dope has been obtained according to experiment detection2Thermoelectric figure of merit is greater than single-phase Ag to Te material at the same temperature2Te material,
And then demonstrate the thermoelectricity capability that the technique in the technical program effectively raises Ag2Te thermoelectric material.
2, due to the Ag of hydrothermal synthesis2Te monocrystalline is in nanowire structure, and is closely arranged between nano wire, therefore introduce
Ag second meets irregular distribution in Ag2Between Te nanowire structure, in this way in sintering, on the one hand, due to the second phase of Ag
Meeting is randomly distributed so that the second phase of Ag is dissolving in Ag again2When in Te, Ag atom it is mixed and disorderly be distributed in Ag2In Te phase；Another party
Face, due to the discharge plasma sintering process that the sintering of the technique uses, the sintering time of the technique is short, does not mention to Ag atom
For enough diffusion times, i.e. Ag atom in a short time will not be in Ag2Uniform diffusion is generated in Te phase；And for thermoelectricity material
For material, dopant profiles must be more uniform, and thermoelectricity capability will be lower, therefore Ag the second phase auto-dope for using this method to obtain
Ag2Te thermoelectricity capability is improved.
3, inventor, which has broken, thinks that there are the Ag of the second phase of Ag in industry2The thermoelectricity capability of Te material will be lower than pure
Ag2The technology prejudice of Te material, to the Ag for introducing the second phase of Ag2After Te material is sintered, a kind of thermoelectricity capability is obtained and has wanted excellent
In pure Ag2The Ag auto-dope Ag of Te2Te material.
Further, the Na in the step (1)2TeO3The purity of powder is greater than 99.9%, AgNO3The purity of powder is greater than
99.8%.
The utility model has the advantages that reducing the introducing of impurity using the higher precursor powder of purity, and then the introducing of impurity is avoided to reduce
The thermoelectricity capability of material.
Further, the reducing agent in the step (1) is hydrazine hydrate, is added in the backward mixed solution of hydrazine hydrate and matter is added
Measure the ammonium hydroxide 0.4-1.2ml that score is 25-28%.
The utility model has the advantages that since hydrazine hydrate is in reduction Ag2TeO3When, ammonium hydroxide can be also generated while producing Ag, by the way that matter is added
The ammonium hydroxide that amount score is 25-28% can inhibit to a certain extent the reaction, that is, slow down hydrazine hydrate reduction Ag2TeO3
Reaction, so that the second phase of Ag be avoided largely to generate.
Further, the cleaning in the step (1) is using deionized water and washes of absolute alcohol.
The utility model has the advantages that using deionized water and washes of absolute alcohol, to remove Ag-Ag2The solution of Te powder surface remnants
And ion.
Further, sintering time is 5min in the step (2).
The utility model has the advantages that the Ag for the Ag auto-dope that inventor by multiple authentication has found that this programme is selected to obtain2Te material
Thermoelectricity capability is preferable.
Further, sintering pressure is 50MPa in the step (2).
The utility model has the advantages that the Ag for the Ag auto-dope that inventor by multiple authentication has found that this programme is selected to obtain2Te material
Thermoelectricity capability is preferable.
Further, sintering temperature is 450 DEG C in the step (2).
The utility model has the advantages that the Ag for the Ag auto-dope that inventor by multiple authentication has found that this programme is selected to obtain2Te material
Thermoelectricity capability is preferable.
Further, hydrazine hydrate 0.4ml is added in step (1) the powder preparation.
The utility model has the advantages that the Ag for the Ag auto-dope that inventor by multiple authentication has found that this programme is selected to obtain2Te material
Thermoelectricity capability is preferable.
Further, in step (1) powder preparation hydro-thermal reaction soaking time 12h.
The utility model has the advantages that the Ag for the Ag auto-dope that inventor by multiple authentication has found that this programme is selected to obtain2Te material
Thermoelectricity capability is preferable.
Further, hydrothermal temperature is 100 DEG C in step (1) the powder preparation.
The utility model has the advantages that inventor proves by repetition test, the Ag auto-dope Ag obtained using the parameter of this programme2Te exists
When temperature is 623K, the ZT value that measures is 1.1, much larger than pure Ag under synthermal2The ZT value of Te.
Detailed description of the invention
Fig. 1 is the XRD comparison diagram of powder before the embodiment of the present invention 1 and 1 discharge plasma sintering of comparative example；
Fig. 2 is the XRD comparison diagram of block after the embodiment of the present invention 1 and 1 discharge plasma sintering of comparative example；
Fig. 3 is the Ag auto-dope Ag that the embodiment of the present invention 1 obtains2The pure Ag that Te and comparative example 1 obtain2The ZT value of Te is with temperature
Spend the relational graph of variation.
Specific embodiment
It is further described below by specific embodiment:
A kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material the following steps are included:
The preparation of step (1) powder:
Weigh the Na that purity is greater than 99.9%2TeO3Powder 0.11g, purity are greater than 99.8% AgNO3Powder 0.17-
0.21g is as precursor powder, by Na2TeO3Powder and AgNO3Powder is dissolved in 15ml solvent, makes rubbing for Ag and Te in solution
You stir 5min, reducing agent 0.4-1.2ml and buffer 0.4-1.2ml are added afterwards, obtains mixed solution than being not less than 2:1；Its
Middle solvent uses deionized water, and reducing agent uses hydrazine hydrate, and buffer uses ammonium hydroxide, and wherein the concentration of hydrazine hydrate is greater than 80%,
The concentration of ammonium hydroxide is 25-28%.
Mixed solution is put into water heating kettle, under conditions of temperature is 100~140 DEG C, keeps the temperature 6-24h, mixed solution
Hydro-thermal reaction is carried out, after reaction, cooled to room temperature is rear dry with deionized water and washes of absolute alcohol multipass, obtains
To Ag-Ag2Te alloy powder, i.e. Ag2Te cable architecture and it is distributed in Ag2The second phase of Ag between Te cable architecture.
Include following 6 reaction equations in step (1) hydrothermal reaction process, is respectively as follows:
2AgNO3+Na2TeO3=Ag2TeO3↓+NaNO3 (1)
Ag2TeO3+N2H4+2H2O=2Ag ↓+2NH3OH++TeO3 2- (2)
2NH3OH++N2H4=2NH4 ++N2↑+2H2O (3)
2TeO3 2-+3N2H4→2TeX 2-+3N2↑+6H2O (4)
TeX 2-→(X-1)Te+Te2- (5)
2Ag+Te=Ag2Te/2Ag++Te2-=Ag2Te (6)
The preparation of step (2) block:
By Ag-Ag obtained in step (1)2Te alloy powder is sintered using plasma discharging technique, the present embodiment
Middle agglomerating plant is that Japanese fuji electric wave company produces, model: FDC SPS6321X, Japan, by Ag-Ag2Te alloy powder falls
Enter in the graphite jig that diameter is 15mm, is 400-500 DEG C in sintering temperature, under conditions of sintering pressure is 10-50MPa, burns
Tie 5-30min, Ag in sintering process2The crystal grain of Te cable architecture is gradually grown up, and the second phase of Ag is gradually dissolved in Ag2In Te crystal grain, obtain
The Ag of Ag auto-dope is arrived2Te material.
The following table 1 is a kind of Ag of Ag auto-dope2The parameter list of the preparation method embodiment 1-5 of Te thermoelectric material:
Comparative example 1: the Na that purity is greater than 99.9% is weighed2TeO3Powder 0.2g, purity are greater than 99.8% AgNO3Powder
Pure Ag is made in 0.105g2(i.e. the material only exists single-phase Ag to Te thermoelectric material2Te)。
Above-described embodiment 1-5 is detected with comparative example 1 using following experiment:
The element of powder and block in step (2) characterizes in 1 step (1):
1.1 XRD (X-ray diffraction) characterization:
The powder and step (2) that the step (1) in embodiment 1 and comparative example 1 is obtained respectively using X-ray diffractometer
Obtained in block detected, the result of detection is as depicted in figs. 1 and 2: (Fig. 1 be embodiment 1 and 1 powder of comparative example XRD
Comparison diagram, Fig. 2 are the XRD comparison diagram of embodiment 1 and 1 block of comparative example)
Powder obtained in the step of embodiment 1 (1) as the result is shown, in addition to Ag2Outside Te main phase, there is also the second phase of Ag,
And block obtained in step (2), in addition to Ag2Outside Te main phase, there is not the second phase of Ag, shows in the sintered of step (2)
The auto-dope of Ag is completed in journey.And Ag is only existed always in comparative example 12Mono- phase of Te.
1.2 EDS (energy spectrum analysis) characterization:
Block obtained in the step of using energy disperse spectroscopy to embodiment 1-5 (2) detects respectively, and the result of detection is as follows
Shown in table 2:
By the way that in the block of embodiment 1-5 preparation, the content of Ag element and the content ratio of Te element are big known to table two
In 2:1, i.e., Ag is not only formd in sintering step2Te main phase, also completes the auto-dope of Ag, and the Ag element in comparative example 1
Content and Te element content be equal to 2:1, illustrate to be pure Ag in comparative example 12Te。
It is able to demonstrate that by XRD characterization and EDS characterization, the Ag of Ag auto-dope has been made using the above method2Te thermoelectricity
The block of material.
2 thermoelectric property characterizations
2.1 power factor
The performance of thermoelectric material is characterized by dimensionless thermoelectric figure of merit ZT, and formula is ZT=σ S2T/ κ, wherein σ S2Indicate function
The rate factor, T are absolute temperature, and κ is thermal conductivity.
The block cutting that step (2) obtains in embodiment 1-5 is used to detect power factor at the strip of 12 × 3 × 3mm,
It is tested using resistivity Seebeck coefficient tester, test result is as follows shown in table 3:
2.2 ZT values
The block that step (2) obtains in embodiment 1-5 is polishing toCircle sheet for testing thermal conductivity κ,
It is tested using laser conductometer, and passes through above-mentioned formula ZT=σ S2T/ κ, in 623K temperature, test result is as follows table 4
It is shown:
Pure Ag made from comparative example 12Te detects its ZT value, as shown in figure 3, pure Ag2The ZT value of Te will be lower than real
Apply Ag auto-dope Ag obtained in example 12The ZT value of Te material detects pure Ag when temperature is 623K2The ZT value of Te is 0.8,
The Ag of Ag auto-dope made from respectively less than embodiment 1-52The ZT value of Te material.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (10)
1. a kind of Ag of Ag auto-dope2The preparation method of Te thermoelectric material, it is characterised in that: the following steps are included:
The preparation of step (1) powder: the molar ratio of Ag and Te is not less than to the Na of 2:12TeO3Powder and AgNO3Powder is dissolved in molten
It is rear that reducing agent 0.4-1.2ml is added in agent, mixed solution is obtained, by mixed solution in 100~140 DEG C of heat preservation 6-24h, is carried out
Hydro-thermal reaction, by cleaning and be dried to obtain Ag-Ag2Te alloy powder；
Step (2) block preparation: by Ag-Ag obtained in step (1)2Te alloy powder is burnt using plasma discharging technique
Knot, sintering temperature are 400-500 DEG C, and sintering pressure is 10-50MPa, and sintering time 5-30min obtains Ag auto-dope
Ag2Te material.
2. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
Na in step (1)2TeO3The purity of powder is greater than 99.9%, AgNO3The purity of powder is greater than 99.8%.
3. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
Reducing agent in step (1) is hydrazine hydrate, and the ammonia for being added that mass fraction is 25-28% is added in the backward mixed solution of hydrazine hydrate
Water 0.4-1.2ml.
4. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
Cleaning in step (1) is using deionized water and washes of absolute alcohol.
5. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
Sintering time is 5min in step (2).
6. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
Sintering pressure is 50MPa in step (2).
7. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
Sintering temperature is 450 DEG C in step (2).
8. a kind of Ag of Ag auto-dope according to claim 32The preparation method of Te thermoelectric material, it is characterised in that: described
Hydrazine hydrate 0.4ml is added in the preparation of step (1) powder, ammonium hydroxide 0.4ml is added.
9. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: described
The soaking time 12h of hydro-thermal reaction in the preparation of step (1) powder.
10. a kind of Ag of Ag auto-dope according to claim 12The preparation method of Te thermoelectric material, it is characterised in that: institute
Stating hydrothermal temperature in the preparation of step (1) powder is 100 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420529A (en) * | 2015-11-04 | 2016-03-23 | 武汉理工大学 | Ultrafast synthetic method of Ag2X block thermoelectric material |
| CN107792838A (en) * | 2016-09-07 | 2018-03-13 | 武汉理工大学 | A kind of supper-fast preparation Ag2The method of X block thermoelectric materials |
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- 2018-12-29 CN CN201811640664.9A patent/CN109728156B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420529A (en) * | 2015-11-04 | 2016-03-23 | 武汉理工大学 | Ultrafast synthetic method of Ag2X block thermoelectric material |
| CN107792838A (en) * | 2016-09-07 | 2018-03-13 | 武汉理工大学 | A kind of supper-fast preparation Ag2The method of X block thermoelectric materials |
Non-Patent Citations (2)
| Title |
|---|
| FENG XIAO等: "Simple synthesis of ultra-long Ag2Te nanowires through solvothermal co-reduction method", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
| HAORAN YANG等: "Composition Modulation of Ag2Te Nanowires for Tunable Electrical and Thermal Properties", 《NANO LETT.》 * |
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