CN110550947A - yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material and preparation method thereof - Google Patents

yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material and preparation method thereof Download PDF

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CN110550947A
CN110550947A CN201910981746.8A CN201910981746A CN110550947A CN 110550947 A CN110550947 A CN 110550947A CN 201910981746 A CN201910981746 A CN 201910981746A CN 110550947 A CN110550947 A CN 110550947A
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张博
陈星宇
常爱民
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

the invention relates to a yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material and a preparation method thereof, the material takes analytically pure calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide as raw materials, and Ca 1- x Y x Cu 3 Ti 4- y Zr y O 12 (0 is equal to or more than x and equal to or less than 0.15; 0 is equal to or more than y and equal to or less than 0.15) thermal sensitive ceramic materials with perovskite-like structures can be obtained through mixed grinding, calcining, cold isostatic pressing, high-temperature sintering and electrode coating firing, the material constant is B 25℃/300℃ =4390K-6880K, the temperature 25 ℃ resistivity is 2.41 multiplied by 10 6 omega cm-3.76 multiplied by 10 8 omega cm., the thermal sensitive resistor material prepared by the invention has stable performance and good consistency, the thermal sensitive resistor material has obvious negative temperature coefficient characteristics in the temperature range of 25 ℃ -900 ℃, the material system is stable in electrical performance and good in consistency, and is suitable for manufacturing wide-high-temperature thermistors.

Description

Yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material and preparation method thereof
Technical Field
The invention relates to an yttrium and zirconium co-doped wide-temperature-range high-temperature thermistor material and a preparation method thereof, wherein the thermistor material has obvious negative temperature coefficient characteristic in the temperature range of 25-900 ℃, and is a novel thermistor material suitable for manufacturing wide-temperature-range high-temperature thermistors.
background
Generally, the thermistor with the use temperature region reaching 250 ℃ and the maximum use temperature higher than 300 ℃ is considered to be a wide-temperature-region high-temperature thermistor. The wide-temperature-zone high-temperature thermistor is an ideal product for replacing industrial metal sensors, has wide prospect and becomes one of four main subjects attacked in the field of thermistors. Wide temperature zone high temperature thermistors are commonly used in conjunction with digital instruments. The technical key to obtain the wide-temperature-zone high-temperature element is to develop a thermosensitive material with low B (material constant) value, high resistance value and good stability. The transition metal oxide multi-element ceramics which have been researched and applied in a great deal are negative temperature coefficient heat-sensitive materials with stable performance, but almost all research results show that the low B high resistance characteristic is difficult to obtain for the materials, because the main crystal phase of the materials is generally in a spinel structure, when the resistivity of the materials is large, the B value is also large, and conversely, the B value of the materials with small resistivity is also small. The method also promotes the research of the wide-temperature-zone high-temperature thermal resistance material, and provides a new challenging subject for the development of a novel wide-temperature-zone high-temperature thermistor material.
The electrical properties of the CaCu 3 Ti 4 O 12 thermistor material prepared by an oxide solid phase method are preliminarily researched, the material constant is 6362K, and the material is expected to be used for manufacturing wide-temperature-zone high-temperature thermistors, considering the high-temperature resistance of Y 2 O 3 and ZrO 2, Y 3+ and Ca 2+ as well as Zr 4+ and Ti 4+ have similar ionic radii, Y 3+ replaces Ca 2+, and Zr 4+ replaces Ti 4+ to adjust the electrical properties of the CaCu 3 Ti 4 O 12 thermistor material, so that wide-temperature-zone high-temperature thermistors with different electrical property parameters are manufactured.
Based on the semiconductor characteristics of CaCu 3 Ti 4 O 12, the perovskite-like Ca 1-x Y x Cu 3 Ti 4-y Zr y O 12 (x is more than or equal to 0 and less than or equal to 0.15, and Y is more than or equal to 0 and less than or equal to 0.15) high-temperature thermistor material with a wide temperature range (25 ℃ -900 ℃) is synthesized through the co-doping design of Y 2 O 3 and ZrO 2.
disclosure of Invention
the invention aims to provide a yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material and a preparation method thereof, the material takes calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide as raw materials, and the perovskite-like wide-temperature-zone thermistor material can be obtained by mixing, grinding, calcining, cold isostatic pressing, high-temperature sintering and electrode coating, wherein the material constant is B 25℃/300℃ -4390K-6880K, the resistivity at the temperature of 25 ℃ is 2.41 x 10 6 omega cm-3.76 x 10 8 omega cm..
The yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material takes calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide as raw materials, has a chemical formula of Ca 1-x Y x Cu 3 Ti 4-y Zr y O 12, and has a body-centered cubic perovskite-like structure, wherein x is more than or equal to 0 and less than or equal to 0.15, and Y is more than or equal to 0 and less than or equal to 0.15.
The preparation method of the yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material comprises the following steps:
a. Respectively weighing calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide according to the composition of Ca 1-x Y x Cu 3 Ti 4-y Zr y O 12, 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 800-1000 ℃ for 5-8 hours, and grinding for 6-9 hours to obtain Ca 1-x Y x Cu 3 Ti 4-y Zr y O 12 powder;
c. Pressing the powder material obtained in the step b into a block under the pressure of 15-30Kg/cm 2 for 0.5-2 minutes, carrying out cold isostatic pressing on the formed block material, maintaining the pressure at 200-300MPa for 1-3 minutes, and then sintering at the temperature of 1000-1200 ℃ for 6-14 hours to obtain the wide-temperature-zone negative temperature coefficient thermal sensitive ceramic material;
d. and (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ -4390K-6880K, the temperature of 25 ℃ and the resistivity of 2.41 multiplied by 10 6 omega cm-3.76 multiplied by 10 8 omega cm.
the invention relates to a yttrium and zirconium codoped wide-temperature-zone high-temperature thermistor material and a preparation method thereof, wherein oxides of calcium, yttrium, copper, titanium and zirconium are mixed and ground, calcined, mixed and ground again by adopting a solid phase method to obtain a negative temperature coefficient thermistor powder material, then the powder material is subjected to sheet cold isostatic pressing forming, platinum slurry electrodes are coated and sintered on the front and back surfaces of the powder material after high-temperature sintering to obtain a thermistor wafer, the wafer thermistor is a ceramic material of Ca 1-x Y x Cu 3 Ti 4-y Zr y O 12 with a calcium-titanium-like structure, the material constant is B 25℃/300℃ -4390K-6880K, the resistivity at 25 ℃ is 2.41 x 10 6 omega cm-76 x 10 8 omega cm., the perovskite-like temperature-zone high-temperature thermistor material prepared by adopting the method has stable performance and good consistency, has obvious negative temperature coefficient characteristics in the temperature range of 25 ℃ -900 ℃, and is suitable for manufacturing wide-temperature thermistor, and the performance parameters are shown in temperature zone table 1 and table 2:
TABLE 1 Material constant B 25℃/300℃ (Unit: K) of thermistor Material
TABLE 2 thermistor material resistivity at 25 deg.C (unit: omega cm)
drawings
FIG. 1 is an X-ray diffraction pattern of a heat-sensitive ceramic material of the present invention.
Detailed Description
Example 1
a. firstly, according to the composition of CaCu 3 Ti 4 O 12, analytically pure calcium carbonate, copper oxide and titanium dioxide are respectively weighed and mixed, and the mixed raw materials are placed in an agate mortar to be ground for 6 hours to obtain powder;
b. Calcining the powder ground in the step a at the temperature of 800 ℃ for 5 hours, and grinding for 6 hours to obtain CaCu 3 Ti 4 O 12 powder;
c. B, briquetting the powder material obtained in the step b under the pressure of 30Kg/cm 2 for 0.5 minute, carrying out cold isostatic pressing on the formed block material, keeping the pressure at 200MPa for 3 minutes, and then sintering at the temperature of 1000 ℃ for 14 hours to obtain a thermal sensitive ceramic material;
d. and (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ -6360K, and the resistivity of 2.41 multiplied by 10 6 omega cm at the temperature of 25 ℃.
Example 2
a. Respectively weighing analytically pure calcium carbonate, yttrium oxide, copper oxide and titanium dioxide according to the composition of Ca 0.85 Y 0.15 Cu 3 Ti 4 O 12, 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 900 ℃ for 6 hours, and grinding for 7 hours to obtain Ca 0.85 Y 0.15 Cu 3 Ti 4 O 12 powder;
c. b, briquetting and molding the powder material obtained in the step b under the pressure of 15Kg/cm 2 for 2 minutes, carrying out cold isostatic pressing on the molded block material, keeping the pressure at 300MPa for 1 minute, and then sintering at 1200 ℃ for 6 hours to obtain a thermal sensitive ceramic material;
d. And (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ -6450K, and the resistivity of 1.80 multiplied by 10 7 omega cm at the temperature of 25 ℃.
example 3
a. weighing analytically pure calcium carbonate, copper oxide, titanium dioxide and zirconium dioxide respectively according to the composition of CaCu 3 Ti 3.85 Zr 0.15 O 12, mixing, placing the mixed raw materials in an agate mortar, and grinding for 8 hours to obtain powder;
b. Calcining the powder ground in the step a at the temperature of 1000 ℃ for 7 hours, and grinding for 8 hours to obtain CaCu 3 Ti 3.85 Zr 0.15 O 12 powder;
c. B, briquetting and molding the powder material obtained in the step b under the pressure of 20Kg/cm 2 for 1 minute, carrying out cold isostatic pressing on the molded block material, keeping the pressure at 250MPa for 2 minutes, and then sintering at 1200 ℃ for 8 hours to obtain a thermal sensitive ceramic material;
d. And (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ -4390K, and the resistivity of 2.69 multiplied by 10 7 omega cm at the temperature of 25 ℃.
Example 4
a. respectively weighing analytically pure calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide according to the composition of Ca 0.85 Y 0.15 Cu 3 Ti 3.85 Zr 0.15 O 12, 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 1000 ℃ for 8 hours, and grinding for 9 hours to obtain Ca 0.85 Y 0.15 Cu 3 Ti 3.85 Zr 0.15 O 12 powder;
c. B, briquetting and molding the powder material obtained in the step b under the pressure of 20Kg/cm 2 for 1 minute, carrying out cold isostatic pressing on the molded block material, keeping the pressure at 250MPa for 2 minutes, and then sintering at 1100 ℃ for 10 hours to obtain a thermal sensitive ceramic material;
d. and (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ -5100K, and the resistivity of 1.89 x 10 7 omega cm at the temperature of 25 ℃.
example 5
a. firstly, according to the composition of Ca 0.95 Y 0.05 Cu 3 Ti 4 O 12, respectively weighing analytically pure calcium carbonate, yttrium oxide, copper oxide and titanium dioxide, 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 800 ℃ for 8 hours, and grinding for 9 hours to obtain Ca 0.95 Y 0.05 Cu 3 Ti 4 O 12 powder;
c. B, briquetting the powder material obtained in the step b under the pressure of 30Kg/cm 2 for 0.5 minute, carrying out cold isostatic pressing on the formed block material, keeping the pressure at 200MPa for 3 minutes, and then sintering at the temperature of 1000 ℃ for 10 hours to obtain a thermal sensitive ceramic material;
d. And (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ being 6880K, and the resistivity of 25 ℃ being 2.99 multiplied by 10 8 omega cm.
Example 6
a. Respectively weighing analytically pure calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide according to the composition of Ca 0.95 Y 0.05 Cu 3 Ti 3.9 Zr 0.1 O 12, 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 900 ℃ for 7 hours, and grinding for 8 hours to obtain Ca 0.95 Y 0.05 Cu 3 Ti 3.9 Zr 0.1 O 12 powder;
c. B, briquetting and molding the powder material obtained in the step b under the pressure of 15Kg/cm 2 for 2 minutes, carrying out cold isostatic pressing on the molded block material, keeping the pressure at 300MPa for 1 minute, and then sintering at 1100 ℃ for 12 hours to obtain a thermal sensitive ceramic material;
d. And (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step (c), and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ -5970K, and the resistivity of 3.76 x 10 8 omega cm at the temperature of 25 ℃.

Claims (2)

1. The yttrium and zirconium co-doped wide-temperature-region high-temperature thermistor material is characterized in that calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide are used as raw materials, the chemical formula of the material is Ca 1- x Y x Cu 3 Ti 4- y Zr y O 12, the material is a body-centered cubic perovskite-like structure, wherein x is more than or equal to 0 and less than or equal to 0.15, and y is more than or equal to 0 and less than or equal to 0.15.
2. The preparation method of the yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material according to claim 1, characterized by comprising the following steps:
a. respectively weighing calcium carbonate, yttrium oxide, copper oxide, titanium dioxide and zirconium dioxide according to the composition of Ca 1- x Y x Cu 3 Ti 4- y Zr y O 12, 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 800-1000 ℃ for 5-8 hours, and grinding for 6-9 hours to obtain Ca 1- x Y x Cu 3 Ti 4- y Zr y O 12 powder;
c. pressing the powder material obtained in the step b into a block under the pressure of 15-30Kg/cm 2 for 0.5-2 minutes, carrying out cold isostatic pressing on the formed block material, maintaining the pressure at 200-300MPa for 1-3 minutes, and then sintering at the temperature of 1000-1200 ℃ for 6-14 hours to obtain the wide-temperature-zone negative temperature coefficient thermal sensitive ceramic material;
d. And (c) coating platinum slurry electrodes on the front surface and the back surface of the ceramic material sintered in the step c, and annealing at 850 ℃ for 30 minutes to obtain the wide-temperature-zone high-temperature thermistor material with the temperature range of 25-900 ℃, the material constant of B 25℃/300℃ =4390K-6880K, the temperature of 25 ℃ and the resistivity of 2.41 × 10 6 Ω cm-3.76 × 10 8 Ω cm.
CN201910981746.8A 2019-10-16 2019-10-16 yttrium and zirconium co-doped wide-temperature-zone high-temperature thermistor material and preparation method thereof Pending CN110550947A (en)

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CN113004039A (en) * 2021-04-26 2021-06-22 中国科学院新疆理化技术研究所 Tungsten bronze type high-temperature thermistor material and preparation method thereof
CN114388204A (en) * 2021-12-20 2022-04-22 中科立民新材料（扬州）有限公司 Fe3+Ion-doped perovskite-like high-temperature thermistor material and preparation method thereof
CN114956789A (en) * 2022-06-07 2022-08-30 中国科学院新疆理化技术研究所 Linear wide-temperature-zone high-temperature thermistor material and preparation method thereof
CN115433007A (en) * 2022-09-22 2022-12-06 江苏开放大学（江苏城市职业学院） Solar spectrum wide-frequency absorption material and preparation method thereof
CN115849898A (en) * 2021-09-24 2023-03-28 华为技术有限公司 Thermal sensitive ceramic material, preparation method thereof and thermistor

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Application publication date: 20191210