CN112310268A - Preparation method of novel medium-temperature thermoelectric material - Google Patents
Preparation method of novel medium-temperature thermoelectric material Download PDFInfo
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- CN112310268A CN112310268A CN202011192316.7A CN202011192316A CN112310268A CN 112310268 A CN112310268 A CN 112310268A CN 202011192316 A CN202011192316 A CN 202011192316A CN 112310268 A CN112310268 A CN 112310268A
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- 239000000463 material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000007731 hot pressing Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 241001062472 Stokellia anisodon Species 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 229910005900 GeTe Inorganic materials 0.000 claims description 7
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 17
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000005485 electric heating Methods 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 18
- 229910045601 alloy Inorganic materials 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 4
- 229910052732 germanium Inorganic materials 0.000 description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 229910052714 tellurium Inorganic materials 0.000 description 4
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910002665 PbTe Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/007—Preparing arsenides or antimonides, especially of the III-VI-compound type, e.g. aluminium or gallium arsenide
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/01—Manufacture or treatment
Abstract
The invention provides a preparation method of a novel medium-temperature thermoelectric material, which comprises the following steps: s1: crushing the raw materials into small blocks with the diameter not more than 30mm, and placing the small blocks on filter paper; s2: weighing the small blocks according to a certain stoichiometric ratio, adding the small blocks into a crucible, and then starting to smelt to obtain an ingot; s3: grinding the cast ingot, and sieving the powder obtained after grinding by using a sieve; s4: putting the sieved powder into a mold for hot-pressing sintering to obtain a sintered material; s5: and putting the sintered material into an annealing furnace for annealing treatment to obtain the novel intermediate-temperature thermoelectric material. The invention has the beneficial effects of effectively solving the problems that the TAGS system material is seriously volatilized in the working temperature range, the electric heating performance and the mechanical performance of the TAGS system material are influenced, and the long-term working stability is influenced, and laying a good foundation for preparing the thermoelectric generator with high thermoelectric conversion efficiency for deep space exploration in the future.
Description
Technical Field
The invention belongs to the technical field of thermoelectric materials, and particularly relates to a preparation method of a novel medium-temperature thermoelectric material.
Background
Thermoelectric materials (thermoelectric materials) are functional materials that utilize the interaction between carriers and lattice vibrations in the materials to achieve direct interconversion of thermal energy and electrical energy. The thermoelectric generator made of the thermoelectric material has the characteristics of compact structure, high reliability, strong capability of resisting severe environment, no need of maintenance, no influence of environment and the like, and is widely applied to the fields of aerospace, military, oceans, medicine and the like. The improvement of the thermoelectric conversion efficiency of the thermoelectric generator can reduce the dosage of a radioisotope heat source and reduce the cost, and numerous researchers have been making continuous efforts and researches in this respect for many years. The main way to improve the thermoelectric conversion efficiency of the thermoelectric generator is to improve the thermoelectric performance of the thermoelectric material.
(GeTe)x(AgSbTe2)100-xThe solid solution is also called as a TAGS system material, and is a middle-temperature p-type thermoelectric material with higher efficiency. The thermoelectric figure of merit of the material reaches 1.4-1.7, but the material can reliably work only at the temperature of not more than 500 ℃, even if the temperature of not more than 500 ℃, the material is seriously volatilized in the working temperature range, the sublimation rate is about 50 times of that of a PbTe material, the electrothermal property and the mechanical property of the material are influenced, and the stability of long-term work is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a novel intermediate-temperature thermoelectric material, effectively solves the problems that the TAGS system material is seriously volatilized in a working temperature range, the electric heating performance and the mechanical performance of the TAGS system material are influenced, and the long-term working stability is influenced, and lays a good foundation for preparing a thermoelectric generator with high thermoelectric conversion efficiency for deep space exploration in the future.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a novel medium-temperature thermoelectric material comprises the following steps: s1: crushing the raw materials into small blocks with the diameter not more than 30mm, and placing the small blocks on filter paper; s2: weighing the small blocks according to a certain stoichiometric ratio, adding the small blocks into a crucible, and then starting to smelt to obtain an ingot; s3: grinding the cast ingot, and sieving the powder obtained after grinding by using a sieve; s4: putting the sieved powder into a mold for hot-pressing sintering to obtain a sintered material; s5: and putting the sintered material into an annealing furnace for annealing treatment to obtain the novel intermediate-temperature thermoelectric material.
Preferably, the raw material is a combination of simple substances of Ge, Te, Ag and Sb.
Preferably, in the step S2, the stoichiometric ratio is (GeTe)x(AgSbTe2)100-x(x＝60～90)。
Preferably, in the step S2, the melting temperature is 700-900 ℃, and the melting time is 0.5-2 h.
Preferably, in step S3, the grinding manner is ball milling, and the ingot is put into a ball mill, and ball milling is performed after a protective atmosphere is introduced.
Preferably, the protective atmosphere is one or more of helium, argon, nitrogen and hydrogen-argon mixed gas.
Preferably, the ball milling time is 2-24 h.
Preferably, in the step S3, the mesh size is 170-300 mesh.
Preferably, in the step S4, the hot pressing temperature of the powder in the hot pressing sintering is 300-600 ℃, the hot pressing pressure is 40-80MPa, and the heat preservation time is 0.5-2 h.
Preferably, in the step S5, the annealing temperature of the sintered material during annealing treatment is 300-1000 ℃, and the heat preservation time is 4-48 h.
The raw materials are mixed according to a certain stoichiometric proportion, ground, sieved and hot-pressed, sintered and molded, so that the problems that the TAGS system material is seriously volatilized within the working temperature range, the electric heating performance and the mechanical performance of the TAGS system material are influenced, and the stability of long-term working is influenced can be effectively solved, the mechanical performance and the electric heating performance of the TAGS system material are optimized, the volatility is reduced, and a good foundation is laid for preparing a thermoelectric generator with high thermoelectric conversion efficiency for deep space exploration in the future.
Drawings
FIG. 1 is a schematic view of the compressive strength of the TAGS material in the preparation method of the novel intermediate temperature thermoelectric material of the embodiment of the present invention
FIG. 2 is a schematic diagram of the change curve of thermoelectric figure of merit of the TAGS material with temperature according to the preparation method of the novel intermediate temperature thermoelectric material of the embodiment of the present invention
Detailed Description
The invention is further illustrated below with reference to examples and figures:
example 1
S1: crushing raw materials: respectively placing vacuum-packed tellurium ingots, antimony ingots and germanium ingots on filter paper, and smashing the materials into small pieces through packing by a wood hammer. Opening the packaging bag, clamping small pieces with diameter not more than 30mm with tweezers, and placing on clean filter paper. The raw materials are crushed and selected to be raw material blocks with the size of 30mm, so that the raw materials can be better smelted when smelting is carried out in the step S2, and the phenomenon that large raw materials are agglomerated and cannot be completely smelted is avoided.
S2: alloy smelting: according to (GeTe)85(AgSbTe2)15The raw materials obtained in the step S1 and the silver powder are weighed according to the stoichiometric ratio, the raw materials are added into a graphite crucible and then melted, the melting temperature is 900 ℃, and the melting time is 2 hours. The stoichiometric ratio can enable the thermoelectric material to have better electrothermal performance and mechanical performance.
S3: ball milling and sieving: and (5) putting the alloy smelted in the step S2 into a ball milling tank, introducing nitrogen, carrying out ball milling for 8 hours, and sieving the alloy powder obtained after ball milling by using a 200-mesh sieve. The alloy powder after ball milling is finer and more uniform than the powder after common crushing, the alloy powder is not wasted, and the production cost is reduced.
S4: hot-pressing and sintering: and (3) loading the alloy powder sieved in the step (3) into a graphite die, carrying out vacuum hot-pressing sintering at 500 ℃ and 50MPa, and keeping the temperature and the pressure for 1 hour. The product obtained by hot-pressing sintering is obtained by carrying out solid solution alloying on the raw materials, enhancing the scattering of the material on phonons, and enabling the thermoelectric material to have better electric heating performance and mechanical performance and reduce the high-temperature volatility of the material.
S5: annealing treatment: and (4) putting the sintered material obtained in the step (S4) into an annealing furnace for annealing treatment, wherein the annealing temperature is 400 ℃, and the heat preservation time is 24 hours.
Example 2
S1: crushing raw materials: respectively placing vacuum-packed tellurium ingots, antimony ingots and germanium ingots on filter paper, and smashing the materials into small pieces through packing by a wood hammer. Opening the packaging bag, clamping small pieces with diameter not more than 30mm with tweezers, and placing on clean filter paper.
S2: alloy smelting: according to (GeTe)60(AgSbTe2)40The raw materials obtained in the step S1 and the silver powder are weighed according to the stoichiometric ratio, the raw materials are added into a graphite crucible and then melted, the melting temperature is 700 ℃, and the melting time is 2 hours.
S3: ball milling and sieving: and (5) putting the alloy smelted in the step S2 into a ball milling tank, introducing argon gas, carrying out ball milling for 24 hours, and sieving the alloy powder obtained after ball milling by using a 300-mesh sieve.
S4: hot-pressing and sintering: and (3) loading the alloy powder sieved in the step (3) into a graphite die, carrying out vacuum hot-pressing sintering at 600 ℃ and 80MPa, and keeping the temperature and the pressure for 2 hours.
S5: annealing treatment: and (5) putting the sintered material obtained in the step (S4) into an annealing furnace for annealing treatment, wherein the annealing temperature is 1000 ℃, and the heat preservation time is 48 hours.
Example 3
S1: crushing raw materials: respectively placing vacuum-packed tellurium ingots, antimony ingots and germanium ingots on filter paper, and smashing the materials into small pieces through packing by a wood hammer. Opening the packaging bag, clamping small pieces with diameter not more than 30mm with tweezers, and placing on clean filter paper.
S2: alloy smelting: according to (GeTe)90(AgSbTe2)10The raw material obtained in the step S1 and silver powder were weighed according to the stoichiometric ratio, and the raw material was added to a graphite crucible and then melted at a temperature of 700 ℃ for 1.5 hours.
S3: ball milling and sieving: and (5) putting the alloy smelted in the step S2 into a ball milling tank, introducing nitrogen, carrying out ball milling for 8 hours, and sieving the alloy powder obtained after ball milling by using a 250-mesh sieve.
S4: hot-pressing and sintering: and (3) loading the alloy powder sieved in the step (3) into a graphite die, carrying out vacuum hot-pressing sintering at 300 ℃ and 40MPa, and keeping the temperature and the pressure for 1 hour.
S5: annealing treatment: and (4) putting the sintered material obtained in the step (S4) into an annealing furnace for annealing treatment, wherein the annealing temperature is 300 ℃, and the heat preservation time is 4 hours.
Example 4
S1: crushing raw materials: respectively placing vacuum-packed tellurium ingots, antimony ingots and germanium ingots on filter paper, and smashing the materials into small pieces through packing by a wood hammer. Opening the packaging bag, clamping small pieces with diameter not more than 30mm with tweezers, and placing on clean filter paper.
S2: alloy smelting: according to (GeTe)70(AgSbTe2)30The raw materials obtained in the step S1 and the silver powder are weighed according to the stoichiometric ratio, the raw materials are added into a graphite crucible and then melted, the melting temperature is 900 ℃, and the melting time is 0.5 hour.
S3: ball milling and sieving: and (5) putting the alloy smelted in the step (S2) into a ball milling tank, introducing nitrogen, carrying out ball milling for 8 hours, and sieving the alloy powder obtained after ball milling by using a 170-mesh sieve.
S4: hot-pressing and sintering: and (3) loading the alloy powder sieved in the step (3) into a graphite die, carrying out vacuum hot-pressing sintering at 400 ℃ and 60MPa, and keeping the temperature and the pressure for 1.5 hours.
S5: annealing treatment: and (5) putting the sintered material obtained in the step (S4) into an annealing furnace for annealing treatment, wherein the annealing temperature is 900 ℃, and the heat preservation time is 20 hours.
As shown in a schematic diagram of the compressive strength of the TAGS material in the preparation method of the novel medium-temperature thermoelectric material in FIG. 1, the compressive strength of the TAGS material can reach 210MPa at most, the mechanical strength of the thermoelectric material is improved, and the use duration can be prolonged when the TAGS material is later applied to a deep space exploration spacecraft. The successful preparation of the material can improve the thermoelectric conversion efficiency of the isotope thermoelectric battery for deep space exploration, reduce the dosage of a radioactive isotope heat source and reduce the cost of a generator.
As shown in fig. 2, a schematic diagram of a curve showing the change of the thermoelectric figure of the TAGS material along with the temperature in the preparation method of the novel intermediate-temperature thermoelectric material, the thermoelectric figure of merit of the TAGS material can reach 1.8 at 500 ℃, so that the volatility of the thermoelectric material is reduced, the thermoelectric performance is greatly improved, the production cost can be greatly reduced, and the service life is prolonged.
Although the embodiments of the present invention have been described in detail, the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. A preparation method of a novel medium-temperature thermoelectric material comprises the following steps:
s1: crushing the raw materials into small blocks with the diameter not more than 30mm, and placing the small blocks on filter paper;
s2: weighing the small blocks according to a certain stoichiometric ratio, adding the small blocks into a crucible, and then starting to smelt to obtain an ingot;
s3: grinding the cast ingot, and sieving the powder obtained after grinding by using a sieve;
s4: putting the sieved powder into a mold for hot-pressing sintering to obtain a sintered material;
s5: and putting the sintered material into an annealing furnace for annealing treatment to obtain the novel intermediate-temperature thermoelectric material.
2. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: the raw materials are the combination of Ge, Te, Ag and Sb simple substances.
3. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: in the step S2, the stoichiometric ratio is (GeTe)x(AgSbTe2)100-x(x＝60～90)。
4. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: in the step S2, the melting temperature is 700-900 ℃, and the melting time is 0.5-2 h.
5. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: in the step S3, the grinding method is ball milling, and the ingot is put into a ball mill and ball milled after introducing a protective atmosphere.
6. The method for preparing a novel intermediate temperature thermoelectric material according to claim 5, wherein: the protective atmosphere is one or a combination of helium, argon, nitrogen and hydrogen-argon mixed gas.
7. The method for preparing a novel intermediate temperature thermoelectric material according to claim 5, wherein: the ball milling time is 2-24 h.
8. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: in the step S3, the mesh size is 170-300 mesh.
9. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: in the step S4, the hot pressing temperature of the powder in the hot pressing sintering is 300-600 ℃, the hot pressing pressure is 40-80MPa, and the heat preservation time is 0.5-2 h.
10. The method for preparing a novel intermediate-temperature thermoelectric material according to claim 1, wherein the method comprises the following steps: in the step S5, the annealing temperature of the sintered material is 300-1000 ℃ and the heat preservation time is 4-48 h.
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Application publication date: 20210202 |