Preparation method of Ca3Co2O6 based oxide thermoelectric material

A technology of thermoelectric materials and oxides, applied in chemical instruments and methods, cobalt compounds, calcium/strontium/barium compounds, etc., can solve the problems of high reaction temperature, long reaction time, difficult grain size, etc., and achieve chemical stability. High, short reaction time, fast sintering effect

Inactive Publication Date: 2005-06-01
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] But, when adopting solid-phase reaction method, in order to obtain uniform single-phase product, generally need to repeatedly grind and roast for a long time, thereby usually cause process period long (Physical Review B, Vol.61, No.19 (2000) pp.R12551 -12554), the product is impure, and the grain size is difficult to control, etc.
Moreover, the ball milling process is easy to introduce impurities, and it is difficult to accurately control the quality of the product.
[0008] In short, the traditional solid-phase synthesis method has a series of problems such as high reaction temperature, relatively long reaction time, poor chemical uniformity, high energy consumption, and difficulty in obtaining thermoelectric compounds with fine grain size.

Method used

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  • Preparation method of Ca3Co2O6 based oxide thermoelectric material
  • Preparation method of Ca3Co2O6 based oxide thermoelectric material
  • Preparation method of Ca3Co2O6 based oxide thermoelectric material

Examples

Experimental program
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Effect test

Embodiment 1

[0047] [Example 1] Ca 3 co 2 o 6 Compound preparation

[0048] Accurately weigh 1.18 grams of Ca(NO 3 ) 2 4H 2 O, 0.97 g Co(NO3)2 6H 2 O, 0.5 mL CH 3 CH 2 OH and 1.75 g C 6 h 8 o 7 ·H 2 O, placed in a reaction vessel, add 49.5 milliliters of deionized water therein, after the above-mentioned raw materials are fully dissolved, slowly add ammoniacal liquor prepared dropwise under constant stirring (water: strong ammoniacal liquor volume ratio is 1: 2), when the solution When the pH value reaches 1.2, stop adding ammonia water dropwise, and continue stirring for 1 hour to obtain a light purple-red clear colloid. The obtained colloid is further stirred and concentrated to obtain xerogel. Grind the xerogel into powder, put it into a muffle furnace for pretreatment at 400°C for 2 hours, then heat it to 950°C and keep it warm for 2 hours to obtain the desired Ca 3 co 2 o 6 powder. Finally, the powder product is ground, put into a mold, placed in a spark plasma sinter...

Embodiment 2

[0049] [Example 2] Ca 3 co 2 o 6 Compound preparation

[0050] Accurately weigh 1.18 grams of Ca(NO 3 ) 2 4H 2 O, 0.97 g Co(NO 3 ) 2 ·6H 2 O, 0.5 mL CH 3 CH 2 OH and 3.5 g C 6 h 8 o 7 ·H 2 0, be placed in a beaker, add 49.0 milliliters of deionized water therein, after the above-mentioned raw materials are fully dissolved, slowly add ammoniacal liquor prepared dropwise under constant stirring (water: concentrated ammoniacal liquor volume ratio is 1: 2), when the solution ph When the value reaches 2.7, stop dripping ammoniacal liquor, continue to stir to obtain dark red transparent colloid. Concentrate the obtained colloid to obtain xerogel. Grind the xerogel into powder, put it into a muffle furnace for pretreatment at 500°C for 2 hours, then heat it to 900°C and keep it for 4 hours to obtain the desired Ca 3 co 2 o 6 powder. Finally, the powder product is ground, put into a mold, placed in a spark plasma sintering (SPS) furnace, heated to 900°C at a heating...

Embodiment 3

[0051] [Example 3] Ca 3 co 2 o 6 Compound preparation

[0052] Accurately weigh 1.18 grams of Ca(NO 3 ) 2 4H 2 O, 0.97 g Co(NO 3 ) 2 ·6H 2 O, 1.0 ml C 64H124O26 and 0.875 g C 6 h 8 o 7 ·H 2 0, be placed in a beaker, add 49.0 milliliters of deionized water therein, after the above-mentioned raw materials are fully dissolved, slowly add ammoniacal liquor prepared dropwise under constant stirring (water: concentrated ammoniacal liquor volume ratio is 1: 2), when the solution ph When the value reaches 3.5, stop dripping ammoniacal liquor, continue to stir to obtain light red clear colloid. Concentrate the obtained colloid to obtain xerogel. Grind the xerogel into powder, put it into a muffle furnace for pretreatment at 600°C for 2 hours, then heat it to 900°C and keep it for 8 hours to obtain the desired Ca 3 co 2 o 6 powder. Finally, the powder product is ground, put into a mold, placed in a spark plasma sintering (SPS) furnace, heated to 950°C at a heating rate o...

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Abstract

The present invention is the preparation process of Ca3Co2O6-base thermoelectric oxide material. The preparation process includes dissolving the material in the ratio of Can ion to Co ion of 3/2, complexing agent citric acid or tartaric acid and surface dispersant hexadiol or Tween and regulating pH value to 1.2-3.5; concentration to form gel; grinding, pre-treatment at 400-600 deg.c to eliminate organic matter and nitrate, and calcining at 900-950 deg.c to obtain Ca3Co2O6 oxide powder; and densifying the oxide powder in some mold, plasma discharge to sinter at temperature raising speed of 130-150 deg.c/min and temperature 850-900 deg.c for 3-10 min. The present invention has relatively low reaction temperature and relatively short reaction time, and the synthesized Ca3Co2O6-base thermoelectric oxide material has high chemical homogeneity and crystal grain homogeneity.

Description

technical field [0001] The present invention relates to a Ca 3 co 2 o 6 Preparation method of based oxide thermoelectric materials, including Ca 3 co 2 o 6 and doped with Ca 3 co 2 o 6 The invention discloses a method for synthesizing an oxide-based thermoelectric material, belonging to the technical field of oxide thermoelectric material preparation. Background technique [0002] The discovery of the thermoelectric effect in 1823 opened a chapter on the application of thermoelectric materials. After the 1950s, thermoelectric materials have been widely used in various technical fields, such as thermoelectric power generation of automobile exhaust and other industrial waste heat, as well as in electronic technology, industry and vacuum technology, agriculture and biology, medical, commercial, national defense and other fields Thermoelectric cooling in . The thermoelectric performance of a material is usually expressed by the thermoelectric figure of merit Z: [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/00C01G51/00C04B35/01C04B35/624
Inventor 张久兴路清梅刘科高张隆刘燕琴周美玲
Owner BEIJING UNIV OF TECH
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