CN113004039B - Tungsten bronze type high-temperature thermistor material and preparation method thereof - Google Patents

Tungsten bronze type high-temperature thermistor material and preparation method thereof Download PDF

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CN113004039B
CN113004039B CN202110452865.1A CN202110452865A CN113004039B CN 113004039 B CN113004039 B CN 113004039B CN 202110452865 A CN202110452865 A CN 202110452865A CN 113004039 B CN113004039 B CN 113004039B
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张博
武锐锋
常爱民
林元伟
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a tungsten bronze high-temperature thermistor material and a preparation method thereof, the material takes barium carbonate, samarium oxide and titanium dioxide as raw materials, and the material is subjected to mixing grinding, calcination, cold isostatic pressing forming, high-temperature sintering and electrode coating and sintering to obtain the material with the constant ofB 400℃/850℃ =15300K-16400K, resistivity at 400 ℃ of 4.8 × 10 7 Ωcm‑1.43×10 8 The omega cm tungsten bronze type high-temperature thermistor material has stable performance, good consistency, obvious negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, and is suitable for manufacturing high-temperature thermistors.

Description

Tungsten bronze type high-temperature thermistor material and preparation method thereof
Technical Field
The invention relates to a tungsten bronze high-temperature thermistor material and a preparation method thereof, the thermistor material has good negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, and is a novel thermistor material suitable for manufacturing a high-temperature thermistor.
Background
The rapid development of modern science and information technology is not independent of the development and application of new materials. Negative temperature coefficient thermistors (NTCR) play an important role in temperature detection, control, compensation, and the like. Since the rapid development of electronic information technology, research on novel NTC materials has been a research direction of researchers. The NTCR is widely applied to the fields of household appliances, medical instruments, aerospace, automobile manufacturing and the like. However, the spinel thermistor material has unstable structure and deteriorated thermal sensitivity at high temperature, and is mainly used at temperatures below 300 ℃. Therefore, the development of the research on the high-temperature thermistor material with a novel structure has important significance for enriching thermistor material systems.
BaSm 2 Ti 4 O 12 The material is a material having an orthorhombic tungsten bronze type structure, the atoms of which are closely arranged, which has a high bulk density, and which has a high thermal stability. At high temperatures, baSm 2 Ti 4 O 12 Oxygen will escape from the material, creating oxygen vacancies. In general, the generation of oxygen vacancies is accompanied by the formation of free electrons, and therefore, baSm 2 Ti 4 O 12 The material is expected to be used as a negative temperature coefficient thermistor material.
The invention adopts the traditional solid-phase sintering method to prepare the BaSm 2 Ti 4 O 12 The negative temperature coefficient thermistor adopts different sintering conditions to prepare the tungsten bronze high-temperature thermistor material with the temperature zone of 350-1100 ℃.
Disclosure of Invention
The invention aims to provide a tungsten bronze type high-temperature thermistor material and a preparation method thereof 400℃/850℃ =15300K-16400K, resistivity at 400 ℃ of 4.8 × 10 7 Ωcm-1.43×10 8 Omega cm tungsten bronze high-temperature thermistor material. The thermistor material has stable performance and good consistency, has obvious negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, and is suitable for manufacturing high-temperature thermistors.
The invention relates to a tungsten bronze high-temperature thermistor material which takes barium carbonate, samarium sesquioxide and titanium dioxide as raw materials and has the chemical composition of BaSm 2 Ti 4 O 12 It is an oblique square tungsten bronze structure. The specific operation is carried out according to the following steps:
a. according to BaSm 2 Ti 4 O 12 Weighing barium carbonate, samarium oxide and titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 6-10 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1000-1200 ℃ for 4-8 hours, and grinding for 5-8 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 10-20Kg/cm 2 Is pressed into blocks for molding for a long timePerforming cold isostatic pressing on the formed block material for 0.5-1.5min, maintaining the pressure at 250-350MPa for 1-3min, and sintering at 1300-1400 ℃ for 4-8 h to obtain a high-temperature thermosensitive ceramic material;
d. coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, wherein the material constant is B 400℃/850℃ =15300K-16400K, resistivity at 400 ℃ of 4.8 × 10 7 Ωcm-1.43×10 8 Omega cm tungsten bronze high-temperature thermistor material.
A preparation method of a tungsten bronze high-temperature thermistor material comprises the following steps:
a. according to BaSm 2 Ti 4 O 12 Weighing barium carbonate, samarium oxide and titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 6-10 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1000-1200 ℃ for 4-8 hours, and grinding for 5-8 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 10-20Kg/cm 2 The pressure of the raw material is pressed into blocks for molding for 0.5 to 1.5 minutes, the molded block material is subjected to cold isostatic pressing, pressure is maintained for 1 to 3 minutes under the pressure of 250 to 350MPa, and then the block material is sintered for 4 to 8 hours at the temperature of 1300 to 1400 ℃ to prepare the high-temperature thermal sensitive ceramic material;
d. coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, wherein the material constant is B 400℃/850℃ =15300K-16400K, and resistivity of 4.8 × 10 at 400 ℃ 7 Ωcm-1.43×10 8 Omega cm tungsten bronze high temperature thermistor material.
The invention relates to a tungsten bronze type high-temperature thermistor material and a preparation method thereof, wherein oxides of barium, samarium and titanium are mixed and ground, calcined, mixed and ground again by adopting a solid phase method to obtain a negative electrodeThe powder material of the thermistor with temperature coefficient is formed by sheet type cold isostatic pressing, platinum slurry electrodes are coated and sintered on the front and back surfaces after high-temperature sintering to obtain a thermistor ceramic sheet, and the thermistor of the ceramic sheet is an orthorhombic tungsten bronze BaSm 2 Ti 4 O 12 Of a ceramic material having a material constant B 400℃/850℃ =15300K-16400K, resistivity at 400 ℃ of 4.8 × 10 7 Ωcm-1.43×10 8 Omega cm. The rhombic tungsten bronze type high-temperature thermistor material prepared by the method has stable performance and good consistency, has obvious negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, and is suitable for manufacturing high-temperature thermistors.
Drawings
FIG. 1 is an XRD spectrum of a heat-sensitive ceramic material sintered at 1375 ℃ in accordance with the present invention.
FIG. 2 is a graph showing the temperature resistance of a heat-sensitive ceramic material sintered at 1375 ℃ in accordance with the present invention.
Detailed Description
Example 1
a. Firstly, press BaSm 2 Ti 4 O 12 Weighing 6.8642g of analytically pure barium carbonate, 12.0204g of samarium sesquioxide and 11.1154g of titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 6 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1000 ℃ for 4 hours, and grinding for 5 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. b, mixing the powder material obtained in the step b at a ratio of 10Kg/cm 2 Pressing the block material under the pressure of the pressure sensor for 0.5 minute, performing cold isostatic pressing on the formed block material, maintaining the pressure at 250MPa for 1 minute, and sintering the block material at 1300 ℃ for 4 hours to obtain a high-temperature thermosensitive ceramic material;
d. coating platinum slurry electrodes on the front and back surfaces of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 400-1100 ℃, wherein the material constant is B 400℃/850℃ =16400K, resistivity at 400 ℃ of 1.43X 10 8 Omega cm tungsten bronze high-temperature thermistor material.
Example 2
a. According to BaSm 2 Ti 4 O 12 Weighing 6.8642g of barium carbonate, 12.0204g of samarium trioxide and 11.1154g of titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 7 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1125 ℃ for 5 hours, and grinding for 6 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 15Kg/cm 2 The pressure of the raw material is pressed into a block for 1 minute, the formed block material is subjected to cold isostatic pressing, the pressure is maintained for 2 minutes under the pressure of 300MPa, and then the block material is sintered for 5 hours at the temperature of 1325 ℃ to prepare the high-temperature thermal sensitive ceramic material;
d. coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 400-1100 ℃, wherein the material constant is B 400℃/850℃ 16200K, a temperature of 400 deg.C and a resistivity of 1.14 × 10 8 Omega cm tungsten bronze high-temperature thermistor material.
Example 3
a. According to BaSm 2 Ti 4 O 12 Weighing 6.8642g of barium carbonate, 12.0204g of samarium sesquioxide and 11.1154g of titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 8 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1150 ℃ for 6 hours, and grinding for 7 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 15Kg/cm 2 The pressure of the high-temperature heat-sensitive ceramic material is pressed into a block for molding for 1 minute, the molded block material is subjected to cold isostatic pressing, pressure is maintained for 3 minutes under the pressure of 300MPa, and then the block material is sintered for 6 hours at the temperature of 1350 ℃ to prepare a high-temperature heat-sensitive ceramic material;
d. c, sintering the ceramic material obtained in the step cCoating platinum slurry electrodes on the reverse two sides, and annealing at 900 ℃ for 30 minutes to obtain the alloy with negative temperature coefficient characteristic in the temperature range of 350-1100 ℃ and material constant of B 400℃/850℃ =15800K, resistivity at 400 ℃ of 6.7X 10 7 Omega cm tungsten bronze high-temperature thermistor material.
Example 4
a. According to BaSm 2 Ti 4 O 12 Weighing 6.8642g of barium carbonate, 12.0204g of samarium trioxide and 11.1154g of titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 9 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1175 ℃ for 7 hours, and grinding for 8 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 15Kg/cm 2 The pressure of the pressure is used for briquetting and forming for 1 minute, the formed block material is subjected to cold isostatic pressing, the pressure is maintained for 3 minutes under the pressure of 300MPa, and then the block material is sintered for 7 hours at the temperature of 1375 ℃ to prepare the high-temperature thermal sensitive ceramic material;
d. coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, wherein the material constant is B 400℃/850℃ =15300K, resistivity at 400 ℃ of 5.37 × 10 7 Omega cm tungsten bronze high-temperature thermistor material.
Example 5
a. According to BaSm 2 Ti 4 O 12 Weighing 6.8642g of barium carbonate, 12.0204g of samarium trioxide and 11.1154g of titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 10 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1200 ℃ for 8 hours, and grinding for 8 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 20Kg/cm 2 Is pressed into blocks for 1.5 minutesCarrying out cold isostatic pressing on the formed block material, keeping the pressure for 3 minutes under the pressure of 350MPa, and then sintering for 8 hours at the temperature of 1400 ℃ to prepare a high-temperature thermal sensitive ceramic material;
d. coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, wherein the material constant is B 400℃/850℃ =15800K, resistivity at 400 ℃ of 4.8X 10 7 Omega cm tungsten bronze high-temperature thermistor material.

Claims (1)

1. The application of tungsten bronze structure material in high-temperature thermistor material is characterized in that the thermistor material takes barium carbonate, samarium trioxide and titanium dioxide as raw materials, and the chemical composition of the thermistor material is BaSm 2 Ti 4 O 12 The method is an oblique square tungsten bronze structure, and the specific operation is carried out according to the following steps:
a. according to BaSm 2 Ti 4 O 12 Weighing barium carbonate, samarium oxide and titanium dioxide respectively, mixing, and grinding the mixed raw materials in an agate mortar for 6-10 hours to obtain powder;
b. calcining the powder ground in the step a at the temperature of 1000-1200 ℃ for 4-8 hours, and grinding for 5-8 hours to obtain BaSm 2 Ti 4 O 12 Powder;
c. c, mixing the powder material obtained in the step b at a ratio of 10-20Kg/cm 2 The pressure is pressed into blocks for 0.5-1.5min, the formed block material is subjected to cold isostatic pressing, the pressure is maintained at 250-350MPa for 1-3min, and then the block material is sintered for 4-8 hours at 1300-1400 ℃ to prepare the high-temperature thermal sensitive ceramic material;
d. coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 900 ℃ for 30 minutes to obtain the ceramic material with the negative temperature coefficient characteristic in the temperature range of 350-1100 ℃, wherein the material constant isB 400℃/850℃ =15300K-16400K, resistivity at 400 ℃ of 4.8 × 10 7 Ω·cm-1.43×10 8 Omega cm tungsten bronze high-temperature thermistor material.
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