CN116022743A - Antimony ditelluride and preparation method thereof - Google Patents
Antimony ditelluride and preparation method thereof Download PDFInfo
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 58
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 54
- JPIIVHIVGGOMMV-UHFFFAOYSA-N ditellurium Chemical compound [Te]=[Te] JPIIVHIVGGOMMV-UHFFFAOYSA-N 0.000 title claims description 6
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 92
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 17
- 230000001603 reducing effect Effects 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 27
- 239000001257 hydrogen Substances 0.000 claims description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 21
- 239000001301 oxygen Substances 0.000 abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 abstract description 21
- 238000012824 chemical production Methods 0.000 abstract description 2
- 229910052714 tellurium Inorganic materials 0.000 description 18
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000000630 rising effect Effects 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 238000010248 power generation Methods 0.000 description 4
- MRPWWVMHWSDJEH-UHFFFAOYSA-N antimony telluride Chemical compound [SbH3+3].[SbH3+3].[TeH2-2].[TeH2-2].[TeH2-2] MRPWWVMHWSDJEH-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 229910000410 antimony oxide Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000026058 directional locomotion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000678 plasma activation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The application relates to the technical field of chemical production, and discloses a preparation method of antimony tri-telluride, which comprises the following steps: step 1: mixing Te powder and Sb powder to obtain a mixed material; step 2: placing the mixed material in an inert gas environment; step 3: heating the mixed materials in sections; step 4: cooling the mixed material to obtain a finished antimony tri-telluride product; in the step 3, the sectional heating comprises primary heating and secondary heating, wherein the primary heating specifically comprises the following steps: heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 30-45 min to obtain a primary heating product; the secondary heating specifically comprises the following steps: heating the primary heating product to 500-580 ℃, and preserving heat for 60-90 min to obtain a secondary heating product; and continuously introducing reducing gas in the heating process. Through the design, the oxygen content of the prepared antimony tritelluride is greatly reduced, the purity of the antimony tritelluride is improved, and in addition, the application also discloses the antimony tritelluride.
Description
Technical Field
The application relates to the technical field of chemical production, in particular to antimony ditelluride and a preparation method thereof.
Background
With the increasing prominence of problems such as energy crisis and environmental pollution, thermoelectric technology, which is one of clean energy technologies, is rapidly receiving attention in the fields of waste heat power generation and refrigeration. The direct interconversion between heat energy and electric energy is realized by utilizing the directional motion principle of the semiconductor internal carriers in a temperature field and an electric field, namely the so-called semiconductor thermoelectric generation and refrigeration technology. Compared with the traditional power generation and refrigeration equipment, the thermoelectric related equipment has the advantages of modularized structure, stable performance, long service life, safety, no noise, no pollutant emission and the like during operation. The modularized structural characteristics of the thermoelectric device enable the thermoelectric device to be easily utilized for some energy sources (such as solar energy, nuclear energy and waste heat discharged by industry or vehicles) to form corresponding power generation equipment or be combined into a combined power generation system, so that the thermoelectric technology has wide application space in many fields, can play a certain role in improving the comprehensive utilization efficiency of the energy sources in the whole social system, and tellurium-antimony compounds are paid attention to in recent years as important thermoelectric materials.
Chinese patent 201510143622.4 discloses a method for rapidly preparing an antimony telluride thermoelectric material, which mainly comprises the following steps:
1) According to Sb 2 Te 3 The stoichiometric ratio of each element of the mixture is that Sb powder and Te powder are weighed and then are ground and mixed uniformly to obtain a mixed material;
2) Performing spark plasma activation sintering on the mixed material obtained in the step 1), and naturally cooling to obtain the antimony telluride thermoelectric material; the discharge plasma activated sintering process comprises the following steps: firstly, heating to 380-410 ℃ at a heating rate of 60-80 ℃/min under the conditions that the vacuum degree is less than 10Pa and the sintering pressure is not added, preserving heat for 10-15 min, then pressurizing to 30-40 MPa, and continuing preserving heat and sintering for 5-10 min.
According to the scheme, the mixed material is heated to the vicinity of the tellurium melting point at a heating rate of 60-80 ℃/min, is kept for 10-15 min, is pressurized to 30-40 MPa, is continuously kept for 5-10 min for sintering, and finally the antimony telluride thermoelectric material is obtained.
Problems to be solved by the present application: how to develop a preparation method of antimony tritelluride with the advantages of large-scale production and high purity.
Disclosure of Invention
The preparation method reduces the occurrence of free tellurium in the reaction process by heating twice, simultaneously uses excessive tellurium to react, prevents incomplete antimony reaction in the reaction process, reduces the heating rate in the heating process, cooperates with the hydrogen environment, reduces the oxygen content in the product, further improves the purity of the product antimony tritelluride, and has the advantages of simple operation steps, lower energy consumption, good repeatability and suitability for large-scale production.
A method for preparing antimony tri-telluride, comprising the following steps:
step 1: mixing Te powder and Sb powder to obtain a mixed material;
step 2: placing the mixed material in an inert gas environment;
step 3: heating the mixed materials in sections;
step 4: cooling the mixed material to obtain a finished antimony tri-telluride product;
in the step 3, the sectional heating comprises primary heating and secondary heating, wherein the primary heating specifically comprises the following steps: heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 30-45 min to obtain a primary heating product;
the secondary heating specifically comprises the following steps: heating the primary heating product to 500-580 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 60-90 min to obtain a secondary heating product;
and continuously introducing reducibility in the heating process of the step 3, wherein the flow rate of the reducibility is 4-10L/min.
Preferably, the reducing gas includes, but is not limited to, hydrogen, carbon monoxide, hydrogen sulfide, methane, sulfur monoxide.
Preferably, the step 1 specifically comprises: the mole ratio of Te to Sb is 3.05-3.10: and 2, weighing Te powder and Sb powder, and uniformly mixing in an inert gas atmosphere to obtain a mixed material.
More preferably, the molar ratio of Te to Sb includes, but is not limited to, 3.05: 2. 3.06: 2. 3.07: 2. 3.08:2. 3.09: 2. 3.10:2.
preferably, step 2 specifically comprises: and (2) placing the mixed material prepared in the step (1) into a graphite boat, placing the graphite boat into a tubular atmosphere furnace, opening an air inlet end and an air outlet end of the tubular atmosphere furnace, and continuously introducing inert gas, wherein the volume of the introduced inert gas is 2-3 times of that of the tubular atmosphere furnace.
It should be noted and understood that in step 2, the purpose of introducing the inert gas into the tubular atmosphere furnace is to exhaust the air in the tubular atmosphere furnace, so that those skilled in the art can choose the volume of introducing the inert gas according to the actual situation, the volume of introducing the inert gas into the tubular atmosphere furnace is not excessively limited in the present application, but in the purpose of being able to realize the exhaust of the air, the present application suggests that the volume of introducing the inert gas is 2 to 3 times the volume of the tubular atmosphere furnace in view of energy saving.
Preferably, the step 3 specifically comprises: starting a heating mode of the tubular atmosphere furnace, heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 30-45 min, heating to 500-580 ℃ and preserving heat for 60-90 min;
continuously introducing reducing gas in the heating process of the step 3, wherein the flow rate of the reducing gas is 4-6L/min;
in consideration of safety in the use process, more recommended use of nontoxic hydrogen gas to reduce oxygen content is adopted, so that more preferable, in the step 3, the temperature is raised to 360-390 ℃ at a temperature raising rate of 6-9 ℃/min, the temperature is kept for 30-45 min, then the temperature is raised to 520-570 ℃, the temperature is kept for 60-90 min, and hydrogen gas is continuously introduced in the temperature raising process of the step 3, wherein the flow rate of the hydrogen gas is 4-6L/min;
more preferably, in step 3, the text forming rate includes, but is not limited to, 6 ℃, 6.5 ℃, 7 ℃, 7.5 ℃, 8 ℃, 8.5 ℃, 9 ℃;
it should be noted and understood that in step 2, the purpose of introducing hydrogen into the tubular atmosphere furnace is to reduce the oxidized tellurium powder and antimony powder, so as to reduce the oxygen content of the tellurium powder and antimony powder and improve the purity of the tellurium powder and antimony powder, so that those skilled in the art can choose the flow rate of introducing hydrogen according to practical situations, the flow rate of introducing hydrogen into the tubular atmosphere furnace is not excessively limited, but in the case of being able to achieve the above purpose, the flow rate of introducing hydrogen is recommended to be 4-6L/min in view of energy conservation.
Preferably, the step 4 specifically comprises: introducing inert gas into the tubular atmosphere furnace, discharging reducing gas in the tubular atmosphere furnace, cooling to room temperature, and taking out the material to obtain the antimony ditelluride.
Preferably, in step 1, the molar ratio of Te to Sb is 3.06-3.08: 2.
in addition, the application also discloses antimony tritelluride prepared by the preparation method of the antimony tritelluride.
The beneficial effects of this application are:
the preparation method reduces the occurrence of free tellurium in the reaction process by heating twice, simultaneously uses excessive tellurium to react, prevents incomplete antimony reaction in the reaction process, reduces the heating rate in the heating process, cooperates with the hydrogen environment, reduces the oxygen content in reactants, further improves the purity of the product antimony tritelluride, and has the advantages of simple operation steps, lower energy consumption, good repeatability and suitability for large-scale production.
Detailed Description
The present application will be described more fully hereinafter with reference to the accompanying examples, in which specific conditions are not identified, and are indicated by conventional or manufacturer-suggested conditions. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Step 1: the mole ratio of Te to Sb is 3.05: and 2, weighing Te powder and Sb powder, and uniformly mixing in an argon atmosphere to obtain a mixed material.
Step 2: and (3) placing the mixed powder in a graphite boat, placing the graphite boat in a tubular atmosphere furnace, wherein an air inlet end and an air outlet end of the tubular atmosphere furnace are in an open state, and introducing argon into the tubular atmosphere furnace, wherein the volume of the introduced argon is 3 times that of the tubular atmosphere furnace.
Step 3: and starting a heating mode of the tubular atmosphere furnace, heating to 350 ℃ at a heating rate of 8 ℃/min, preserving heat for 45min, heating to 550 ℃ at a heating rate of 8 ℃/min, preserving heat for 80min, and introducing hydrogen into the tubular atmosphere furnace only during heating, wherein the hydrogen flow is 8L/min.
Step 4: and then stopping heating, and simultaneously introducing argon into the tubular atmosphere furnace, cooling to room temperature, and taking out the materials to obtain the antimony trioxide finished product.
Example 2
Step 1: the mole ratio of Te to Sb is 3.1: and 2, weighing Te powder and Sb powder, and uniformly mixing in a helium atmosphere to obtain a mixed material.
Step 2: and (3) loading the mixed powder into a graphite boat, and putting the graphite boat into a tubular atmosphere furnace, wherein an air inlet end and an air outlet end of the tubular atmosphere furnace are in an open state, and helium is introduced into the tubular atmosphere furnace, and the volume of the introduced helium is 2 times of the volume of the tubular atmosphere furnace.
Step 3: and starting a heating mode of the tubular atmosphere furnace, heating to 400 ℃ at a heating rate of 8 ℃/min, preserving heat for 40min, heating to 580 ℃ at a heating rate of 8 ℃/min, preserving heat for 60min, and introducing hydrogen into the tubular atmosphere furnace only during heating, wherein the hydrogen flow is 6L/min.
Step 4: and then stopping heating, and simultaneously introducing helium into the tubular atmosphere furnace, cooling to room temperature, and taking out the materials to obtain the antimony trioxide finished product.
Example 3
Step 1: the mole ratio of Te to Sb is 3.08: and 2, weighing Te powder and Sb powder, and uniformly mixing in a xenon atmosphere to obtain a mixed material.
Step 2: and (3) loading the mixed powder into a graphite boat, and putting the graphite boat into a tubular atmosphere furnace, wherein the air inlet end and the air outlet end of the tubular atmosphere furnace are in an open state, and xenon is introduced into the tubular atmosphere furnace, and the volume of the introduced xenon is 2 times of that of the tubular atmosphere furnace.
Step 3: and starting a heating mode of the tubular atmosphere furnace, heating to 380 ℃ at a heating rate of 8 ℃/min, preserving heat for 30min, heating to 550 ℃ at a heating rate of 8 ℃/min, preserving heat for 90min, and introducing hydrogen into the tubular atmosphere furnace only during heating, wherein the hydrogen flow is 5L/min.
Step 4: and then stopping heating, and simultaneously introducing xenon into the tubular atmosphere furnace, cooling to room temperature, and taking out the materials to obtain the antimony trioxide finished product.
Example 4
Substantially the same as in example 1, except that in step 3, the temperature rise rates of the primary heating and the secondary heating were 10℃per minute.
Example 5
Substantially the same as in example 1, except that the temperature rise rates of the primary heating and the secondary heating were 5℃per minute.
Example 6
Substantially the same as in example 1, except that carbon monoxide was introduced in place of hydrogen during the temperature raising in step 3.
Comparative example 1
Substantially the same as in example 1, except that xenon was introduced in place of hydrogen during the temperature raising in step 3.
Comparative example 2
Substantially the same as in example 1, except that in step 3, the temperature was once raised to 550℃at a temperature raising rate of 10℃per minute.
Comparative example 3
Substantially the same as in example 1, except that in step 3, the temperature rise rates of the primary heating and the secondary heating were 60℃per minute.
Comparative example 4
Substantially the same as in example 1, except that in step 1, the molar ratio of Te and Sb was 3.05: and 2, weighing Te powder and Sb powder, uniformly mixing in an inert gas atmosphere, and compacting the mixed Te and Sb mixture to obtain a mixed material.
Comparative example 5
Substantially the same as in example 1, except that the molar ratio of Te and Sb in step 1 was 3.5:2.
comparative example 6
Substantially the same as in example 1, except that the molar ratio of Te and Sb in step 1 was 3:2.
the testing method comprises the following steps:
testing oxygen content using an energy spectrometer (EDS, energy Dispersive Spectrometer)
Table 1: performance test results table
Analysis of results:
1. as can be seen from examples 1-3, when the flow rate of hydrogen gas is gradually reduced, the oxygen content of antimony tritelluride is gradually increased, and the purity is gradually reduced, it is not difficult to see that the flow rate of hydrogen gas and the oxygen content of antimony tritelluride are in inverse proportion, and it is speculated that the contact amount of antimony tritelluride and hydrogen gas is increased in unit time due to the increase of the flow rate of hydrogen gas, so that tellurium oxide and antimony oxide impurities in antimony tritelluride are reduced, and the oxygen content in raw materials is reduced, and the oxygen content of antimony tritelluride is reduced, but from the practical production point of view, although the oxygen content between examples 1-3 has a certain difference, the purity of antimony tritelluride of examples 1-3 is in an acceptable range, and from the practical production cost point of view, it is more recommended that the flow rate of hydrogen gas is 4-6L/min.
2. It can be seen from examples 1 and 4-5 that as the temperature rising rates of the primary heating and the secondary heating decrease, the oxygen content of antimony tristelluride gradually decreases, probably due to the decrease in the temperature rising rate, resulting in an elongation of the temperature rising process, and thus, a prolonged contact time of hydrogen with antimony tristelluride and a decrease in the oxygen content of antimony tristelluride. However, from the practical production point of view, the difference in oxygen content between examples 4 and 5 is not large, and the temperature rising rate of example 4 is lower, which results in the production cost of example 4 being higher than that of example 5, so that it is more recommended to control the temperature rising rate between 6 and 9 ℃/min in view of the production cost.
3. It can be seen from examples 1 and 6 that the same reduction effect on the oxygen content of antimony tri-telluride is achieved by using carbon monoxide instead of hydrogen, but due to the toxicity of carbon monoxide itself, we propose more selection of hydrogen to suppress the oxygen content.
4. It can be seen from example 1 and comparative example 1 that the oxygen content of antimony tristelluride could not be reduced by using an inert gas having no reducing properties instead of hydrogen.
5. As is evident from example 1 and comparative example 2, in step 3, the antimony content in antimony tritelluride was too high by using one heating instead of multiple heating, and it is presumed that the reason for this is that the oxygen content is mainly derived from tellurium oxide and antimony oxide after oxidative deterioration, and oxygen is removed as much as possible before they reach the reaction temperature, and once the compound is synthesized, the internal oxygen is not good.
6. As can be seen from example 1 and comparative example 3, in step 3, when the temperature rising rate is 60 ℃/min, the temperature rising process is too short, the temperature rising is faster, the reaction between tellurium and antimony is not complete, and at high temperature, tellurium volatilizes due to vapor pressure, so that the antimony content in antimony tritelluride is too high.
7. As can be seen from examples 1 and 4, the antimony content of the antimony tritelluride prepared using the compacted tellurium and antimony powders was too high, presumably because the reaction was severe after compaction, and a large amount of heat was generated to volatilize tellurium.
8. As can be seen from example 1 and comparative examples 5 and 6, when the tellurium content is increased, antimony tristelluride having a lower oxygen content is obtained, but the free tellurium in the product is too much, so that on one hand, the impurity content in the antimony tristelluride is too high, and on the other hand, the tellurium powder is too wasted, and the production cost is too high;
and when 3:2, the antimony content in the obtained ditelluride is too high, presumably due to the fact that part of tellurium does not react, resulting in too high antimony content.
Claims (9)
1. A method for preparing antimony tri-telluride, which is characterized by comprising the following steps:
step 1: mixing Te powder and Sb powder to obtain a mixed material;
step 2: placing the mixed material in an inert gas environment;
step 3: heating the mixed materials in sections;
step 4: cooling the mixed material to obtain a finished antimony tri-telluride product;
in the step 3, the sectional heating comprises primary heating and secondary heating, wherein the primary heating specifically comprises the following steps: heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 30-45 min to obtain a primary heating product;
the secondary heating specifically comprises the following steps: heating the primary heating product to 500-580 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 60-90 min to obtain a secondary heating product;
and continuously introducing reducing gas in the heating process of the step 3, wherein the flow rate of the reducing gas is 4-10L/min.
2. The method for producing antimony trioxide according to claim 1, characterized in that the reducing gas is selected from any one of hydrogen, carbon monoxide, hydrogen sulfide, methane, and sulfur monoxide.
3. The method for preparing antimony tri-telluride according to claim 1, wherein step 1 specifically comprises: the mole ratio of Te to Sb is 3.05-3.10: and 2, weighing Te powder and Sb powder, and uniformly mixing in an inert gas atmosphere to obtain a mixed material.
4. The method for preparing antimony tri-telluride according to claim 1, wherein step 2 specifically comprises: and (2) placing the mixed material prepared in the step (1) into a graphite boat, placing the graphite boat into a tubular atmosphere furnace, opening an air inlet end and an air outlet end of the tubular atmosphere furnace, and continuously introducing inert gas, wherein the volume of the introduced inert gas is 2-3 times of that of the tubular atmosphere furnace.
5. The method for preparing antimony tri-telluride according to claim 1, wherein step 3 specifically comprises: starting a heating mode of the tubular atmosphere furnace, heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 30-45 min, heating to 500-580 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 60-90 min;
and continuously introducing reducing gas in the heating process of the step 3, wherein the flow rate of the reducing gas is 4-6L/min.
6. The method for preparing antimony tritelluride according to claim 5, wherein in step 3, the temperature is raised to 360-390 ℃ at a temperature raising rate of 6-9 ℃/min, the temperature is kept for 30-45 min, then the temperature is raised to 520-570 ℃ at a temperature raising rate of 6-9 ℃/min, the temperature is kept for 60-90 min, and hydrogen is continuously introduced during the temperature raising process of step 3, wherein the flow rate of the hydrogen is 4-6L/min.
7. The method for preparing antimony tri-telluride according to claim 1, wherein step 4 specifically comprises: introducing inert gas into the tubular atmosphere furnace, discharging reducing gas in the tubular atmosphere furnace, cooling to room temperature, and taking out the material to obtain the antimony ditelluride.
8. The method for producing antimony tritelluride according to claim 2, wherein in step 1, the molar ratio of Te to Sb is 3.06-3.08: 2.
9. antimony tritelluride prepared by the process of any one of claims 1-8.
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| CN108069456A (en) * | 2017-12-28 | 2018-05-25 | 成都中建材光电材料有限公司 | A kind of preparation method of cadmium telluride |
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