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SnI2 doped CsGeI3 perovskite type thermoelectric material and preparation method thereof

A thermoelectric material and perovskite-type technology, which is applied in the field of rapid sintering to prepare SnI2-doped CsGeI3 perovskite-type thermoelectric materials, can solve the problem that it is difficult to obtain single-phase dense bulk materials, and inorganic perovskite materials are unstable and unfavorable. Large-scale production and other issues, to achieve the effect of high block density, short cycle, and small environmental hazards

Inactive Publication Date: 2020-04-21
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For SnI 2 doped bulk CsGeI 3 The preparation method of the material is mainly the vacuum sealing method. If the dense block obtained by this method takes a long time and a high temperature, and the prepared block has orientation, it is not conducive to large-scale production; Generally, inorganic perovskite materials are unstable, and are prone to oxidation, decomposition and phase transition during sintering, and it is difficult to obtain single-phase dense bulk materials. Therefore, it is difficult for those skilled in the art to think of using SPS sintering method to prepare polycrystalline perovskite structures. Bulk materials, so far not reported

Method used

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  • SnI2 doped CsGeI3 perovskite type thermoelectric material and preparation method thereof
  • SnI2 doped CsGeI3 perovskite type thermoelectric material and preparation method thereof
  • SnI2 doped CsGeI3 perovskite type thermoelectric material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0023] A Perovskite Thermoelectric Material 10%SnI 2 doped CsGeI 3 The preparation method specifically comprises the following steps:

[0024] (1) Powder preparation: CsI, SnI 2 and GeI 2 Weigh 1.5588g, 0.2235g and 1.7627g respectively according to the ratio of 1:0.1:0.9 and put them into the quartz tube, then vacuumize, the vacuum degree is 10 -5 Pa, put the quartz tube containing the raw material into the sintering furnace, heat it up to 490°C at a rate of 3°C / min and keep it for 24h, then cool it down to 320°C at a rate of 3°C / min; take out the obtained block in the glove box Grinding for 15 minutes, you can get 10% SnI 2 doped CsGeI 3 of powder.

[0025] (2) Block preparation: the powder obtained in step (1) is sintered by a spark plasma process, and 10% SnI 2 doped CsGeI 3 Pour 2g of the powder into a graphite mold, under the conditions of a temperature of 290°C and a pressure of 10MPa, and a sintering time of 5min, a 10% SnI 2 doped CsGeI 3 bulk material.

Embodiment 2

[0027] A perovskite-type thermoelectric material 20%SnI 2 doped CsGeI3 The preparation method specifically comprises the following steps:

[0028] (1) Powder preparation: CsI, SnI 2 and GeI 2 Weigh 1.5588g, 0.447g and 1.5668g respectively according to the ratio of 1:0.2:0.8 and put them into the quartz tube, then vacuumize, the vacuum degree is 10 -3 Pa; Put the quartz tube containing the raw material into the sintering furnace, heat it up to 490°C at a rate of 3°C / min and keep it for 24 hours, and then cool it down to 320°C at a rate of 3°C / min; take out the obtained block in the glove box Grinding for 15 minutes, you can get 20% SnI 2 doped CsGeI 3 of powder.

[0029] (2) Block preparation: the powder obtained in step (1) is sintered by a spark plasma process, and 20% SnI 2 doped CsGeI 3 Pour 2g of the powder into a graphite mold, under the conditions of a temperature of 290°C and a pressure of 10MPa, and a sintering time of 5min, a 20% SnI 2 doped CsGeI 3 bulk mate...

Embodiment 3

[0031] A perovskite-type thermoelectric material 30%SnI 2 doped CsGeI 3 The preparation method specifically comprises the following steps:

[0032] (1) Powder preparation: CsI, SnI 2 and GeI 2 Weigh 1.5588g, 0.6705g and 1.3710g respectively according to the ratio of 1:0.3:0.7 and put them into the quartz tube. After vacuuming, fill the tube with high-purity argon to seal the tube tightly. The pressure of the inert gas in the quartz tube is -1bar; Put the quartz tube containing the raw material into the sintering furnace, raise the temperature to 450°C at a rate of 2°C / min and keep it warm for 18h, then cool down to 200°C at a rate of 2°C / min; take out the obtained block and grind it in the glove box for 15min , you can get 30% SnI 2 doped CsGeI 3 of powder.

[0033] (2) Block preparation: The powder obtained in step (1) is sintered by a spark plasma process, and 30% SnI 2 doped CsGeI 3 Pour 2g of the powder into a graphite mold, under the conditions of temperature 200°...

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Abstract

The invention discloses a SnI2 doped CsGeI3 perovskite type thermoelectric material and a preparation method thereof and belongs to the technical field of new energy material preparation. The preparation method comprises the steps of powder preparation and block preparation. According to the powder preparation, CsI, SnI2 and GeI2 are added into a quartz tube proportionally, after the quartz tube is vacuumized, the quartz tube is filled with high-purity argon, and the tube is sealed; the quartz tube containing the raw materials is arranged in a sintering furnace, the quartz tube is heated to 450-550 DEG C at a speed of 2-5 DEG C / min, is subjected to heat preservation for 12-24 hours, and then is cooled to 200-350 DEG C at a speed of 2-5 DEG C / min; and an obtained block is taken out and ground in a glove box for 10-15 min, so that SnI2 doped CsGeI3 powder can be obtained. According to the block preparation, the SnI2 doped CsGeI3 powder is sintered through a spark plasma technology; the powder is poured into a graphite mold; and the powder is sintered for 5-30 min under temperature of 200-400 DEG C and pressure intensity of 5-40 MPa, and a block material is obtained. With the method adopted, the perovskite type thermoelectric material SnI2 doped CsGeI3 block can be prepared; and the obtained block is high in density. The method has the advantages of low preparation temperature andshort preparation time.

Description

technical field [0001] The invention belongs to the technical field of thermoelectric material preparation, and in particular provides a method for preparing SnI by rapid sintering. 2 doped CsGeI 3 The method of the perovskite type thermoelectric material involves a vacuum sealing method and a spark plasma sintering (Spark PlasmaSintering, SPS) process. Background technique [0002] Thermoelectric materials (also known as thermoelectric materials) can efficiently convert thermal energy into electrical energy by utilizing the transport and interaction of carriers and phonons inside solids. At present, the energy utilization rate of human beings is low, and more than 55% of the energy is released into the environment in the form of waste heat. Therefore, thermoelectric materials can improve energy utilization rate and receive more and more attention. In terms of electric temperature difference, it is mainly used in electronic component refrigeration and daily small-scale ref...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L35/34H01L35/14H10N10/01H10N10/851
CPCH10N10/855H10N10/01
Inventor 冯晶钱峰葛振华胡明钰
Owner KUNMING UNIV OF SCI & TECH
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