CN111548159A - Zirconate system negative temperature coefficient thermistor material and preparation method thereof - Google Patents
Zirconate system negative temperature coefficient thermistor material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a novel zirconate system negative temperature coefficient thermistor material, which takes zirconium dioxide, samarium trioxide, ytterbium trioxide, neodymium trioxide and gadolinium trioxide as raw materials, the zirconium dioxide is respectively mixed with the samarium trioxide, the ytterbium trioxide, the neodymium trioxide or the gadolinium trioxide, and the zirconate system material is obtained through ball milling, cold isostatic pressing and high-temperature sintering, wherein the electrical property parameters of the system material are as follows: b is400℃/1000℃=9812‑14060K，ρ1000℃=1.513‑5.289×103Omega cm. The zirconate system negative temperature coefficient thermistor material prepared by the invention has a temperature range of 400-1000 DEG CThe material has obvious negative temperature coefficient characteristics, stable electrical property, good consistency, stable aging performance and insensitivity to oxygen partial pressure, and is a novel thermistor material suitable for manufacturing environments with high temperature and different oxygen partial pressures.
Description
Technical Field
The invention relates to a novel zirconate system negative temperature coefficient thermistor material and a preparation method thereof, the system thermistor material has obvious negative temperature coefficient characteristics and insensitive oxygen partial pressure characteristics within the range of 400-1000 ℃, and belongs to the field of semiconductor sensors.
Background
The sensitive element and the sensor are one of three major pillars in the electronic information industry, are considered to be electronic technical products with the greatest development prospect at present, and the development of the sensitive element plays a very important role in improving the international position of the electronic industry in China. At present, with the vigorous development of automobile electronics, military and aerospace industries, the monitoring requirements of people on a high-precision and severe environment resistant sensing system are higher and higher, and negative temperature coefficient thermistors (NTCs) are more and more emphasized by people. The traditional spinel structure NTCC ceramic material is based on transition metal oxides of Mn, Co, Ni, Fe, Cu, Zn and the like, the material cannot be used at the temperature of more than 300 ℃, and has certain limitation, and the polynary ceramic material composed of the spinel structure is unstable at high temperature, and the sintered material is in a non-equilibrium state, so that the electrical characteristics of the material are changed, and the development of the material is limited. Therefore, it is imperative to develop a new high temperature NTC thermistor material suitable for high temperature regions.
A key challenge in developing high temperature NTC thermistor materials is that such materials must have a high degree of chemical and thermal stability; capable of withstanding high pressures and severe oxidative or corrosive harsh environments that may be caused by high temperatures. Several materials such as perovskite, perovskite-based composite materials, spinel-based composite materials, and high-temperature polymer-derived ceramics have been used as high-temperature NTC thermistor materials so far. Although great progress has been made, the maximum temperature upper limit for most reported materials is only 800 ℃ and a few materials can reach 1000 ℃. Meanwhile, the resistance is only tens of ohms when the temperature rises to the upper limit of the temperature, which limits the practical application of the materials in high-temperature environment, and the materials also have poor aging characteristics and the electrical properties are easily affected by oxygen environment. Therefore, the invention discloses a novel zirconate system negative temperature coefficient thermistor material, which has the advantages of obvious negative temperature coefficient characteristic within 400-1000 ℃, stable electrical property, good consistency, stable aging performance and insensitivity to oxygen partial pressure, and is a novel thermistor material suitable for manufacturing thermistors in high-temperature environments.
Disclosure of Invention
The invention aims to provide a zirconate system negative temperature coefficient thermistor material and a preparation method thereof, wherein the thermistor material takes zirconium dioxide, samarium trioxide, ytterbium trioxide, neodymium trioxide and gadolinium trioxide as raw materials, the zirconium dioxide is respectively mixed with the samarium trioxide, the ytterbium trioxide, the neodymium trioxide or the gadolinium trioxide, and the zirconate system material can be obtained through ball milling, cold isostatic pressing and high-temperature sintering, wherein the electrical performance parameters of the system material are as follows: b is400℃/1000℃＝9812-14060K，ρ1000℃＝1.513-5.289×103Omega cm. The zirconate system negative temperature coefficient thermistor material has obvious negative temperature coefficient characteristics within a temperature range of 400-1000 ℃, has stable electrical property, good consistency, stable aging performance and insensitivity to oxygen partial pressure, and is a novel thermistor material suitable for manufacturing thermistors in high-temperature environments.
The invention relates to a zirconate system negative temperature coefficient thermistor material, which is characterized in that the chemical general formula of the thermistor material is as follows: a. the2Zr2O7Wherein A is Nd, Sm, Gd or Yb, and is prepared by mixing and firing zirconium dioxide as raw material with samarium sesquioxide, ytterbium sesquioxide, neodymium sesquioxide or gadolinium sesquioxide respectively.
The preparation method of the zirconate system negative temperature coefficient thermistor material comprises the following steps:
a. according to A2Zr2O7Weighing zirconium dioxide, mixing with samarium oxide, ytterbium oxide, neodymium oxide or gadolinium oxide, placing in an agate ball milling tank, wet milling for 6-8h with analytically pure absolute ethyl alcohol as a dispersion medium, and subjecting the slurry after wet milling to temperatureDrying at 150 ℃, taking out and grinding for 1h to obtain powder;
b. b, mixing the powder obtained in the step a at a ratio of 15-25kg/cm2The pressure is pressed and molded for 1-2min, the molded block is subjected to cold isostatic pressing, the pressure is maintained at 250-300MPa for 1-3min, and then the block is sintered for 10h at the temperature of 1650 ℃ to obtain the zirconate system negative temperature coefficient thermistor material;
c. coating platinum slurry electrodes on the front and back surfaces of the zirconate system negative temperature coefficient thermistor material obtained in the step b, and then annealing at the temperature of 900 ℃ for 1-2h to obtain the material with the electrical performance parameters as follows: b is400℃/1000℃＝9812-14060K,ρ1000℃＝1.513-5.289×103Omega cm zirconate system negative temperature coefficient thermistor material.
The invention relates to a zirconate system negative temperature coefficient thermistor material and a preparation method thereof, analytically pure zirconium dioxide is respectively mixed with analytically pure samarium sesquioxide, analytically pure ytterbium sesquioxide, analytically pure neodymium sesquioxide or analytically pure gadolinium sesquioxide by a ball milling method, ball milling, drying and grinding are carried out, then the powder is formed by cold isostatic pressing in a chip type, platinum slurry electrodes are coated on the front side and the back side after high-temperature sintering to obtain the thermistor, and the system thermistor material is A2Zr2O7The electrical performance parameters of the system are as follows: b is400℃/1000℃＝9812-14060K，ρ1000℃＝1.513-5.289×103Omega cm. Can obtain a series of novel A by changing A-site cation2Zr2O7The innovation points of the high-temperature negative temperature coefficient thermistor material mainly comprise:
(1)A2Zr2O7the ceramic material has typical NTC characteristics in a higher temperature range (400-1000 ℃) and is stable in high-temperature environment.
(2) The resistivity of the material is almost irrelevant to the change of oxygen partial pressure, and can keep higher resistivity in a high-temperature environment, still reaches the kilohm level, and is beneficial to the practical application in the high-temperature environment.
The material has obvious negative temperature coefficient characteristic, and the system material has stable electrical property, good consistency, stable aging performance and insensitivity to oxygen partial pressure, and is a novel thermistor material suitable for manufacturing environments with high temperature and different oxygen partial pressures.
Drawings
FIG. 1 shows the present invention A2Zr2O7The resistivity of (A ═ Nd, Sm, Gd, Yb) materials is plotted against temperature.
FIG. 2 shows the present invention A2Zr2O7Graph of resistivity versus partial pressure of oxygen for (a ═ Nd, Sm, Gd, Yb) materials.
Detailed Description
Example 1
a. According to Nd2Zr2O7Weighing zirconium dioxide and neodymium oxide, mixing, placing in an agate ball milling tank, wet milling for 8h by using analytically pure absolute ethyl alcohol as a dispersion medium, drying slurry after wet milling at the temperature of 150 ℃, taking out and grinding for 1h to obtain powder;
b. b, mixing the powder obtained in the step a at a ratio of 25kg/cm2The pressure of the zirconium oxide is pressed into blocks for molding for 2min, the molded blocks are subjected to cold isostatic pressing, the pressure is maintained at 300MPa for 3min, and then the blocks are sintered for 10h at the temperature of 1650 ℃ to obtain the zirconate system negative temperature coefficient thermistor material;
c. coating platinum slurry electrodes on the front and back surfaces of the zirconate system negative temperature coefficient thermistor material obtained in the step B, and then annealing at the temperature of 900 ℃ for 2 hours to obtain the material with the electrical property parameter B400/1000＝9812K，ρ1000℃1513 Ω · cm, a new zirconate system negative temperature coefficient thermistor material.
Example 2
a. According to Sm2Zr2O7Weighing zirconium dioxide and samarium sesquioxide, mixing, placing in an agate ball milling tank, wet milling for 7h by using analytically pure absolute ethyl alcohol as a dispersion medium, drying slurry after the wet milling at the temperature of 150 ℃, taking out and grinding for 1h to obtain powder;
b. b, mixing the powder obtained in the step a at a ratio of 20kg/cm2Pressing into blocks for 2min to obtain the final productCarrying out cold isostatic pressing on the block, maintaining the pressure at 300MPa for 3min, and then sintering the block at 1650 ℃ for 10h to obtain the zirconate system negative temperature coefficient thermistor material;
c. coating platinum slurry electrodes on the front and back surfaces of the zirconate system negative temperature coefficient thermistor material obtained in the step B, and then annealing at the temperature of 900 ℃ for 2 hours to obtain the material with the electrical property parameter B400/1000＝10781K，ρ1000℃2095 Ω · cm, and a new zirconate system negative temperature coefficient thermistor material.
Example 3
a. According to Gd2Zr2O7Weighing zirconium dioxide and gadolinium oxide, mixing, placing in an agate ball milling tank, wet milling for 6h by using analytically pure absolute ethyl alcohol as a dispersion medium, drying slurry after wet milling at the temperature of 150 ℃, taking out and grinding for 1h to obtain powder;
b. b, mixing the powder obtained in the step a at a ratio of 15kg/cm2The pressure of the raw materials is pressed into a block for 1min, the formed block is subjected to cold isostatic pressing, the pressure is maintained at 250MPa for 1min, and then the block is sintered at the temperature of 1650 ℃ for 10h to obtain the zirconate system negative temperature coefficient thermistor material;
c. coating platinum slurry electrodes on the front and back surfaces of the zirconate system negative temperature coefficient thermistor material obtained in the step B, and then annealing for 1 hour at the temperature of 900 ℃ to obtain the material with the electrical property parameter B400/1000＝12117K，ρ1000℃2810 Ω · cm, and a new zirconate system negative temperature coefficient thermistor material.
Example 4
a. According to Yb2Zr2O7Weighing zirconium dioxide and ytterbium trioxide, mixing, placing in an agate ball milling tank, wet milling for 6 hours by using analytically pure absolute ethyl alcohol as a dispersion medium, drying slurry after the wet milling at the temperature of 150 ℃, taking out and grinding for 1 hour to obtain powder;
b. b, mixing the powder obtained in the step a at a ratio of 15kg/cm2Pressing the block for 1min, cold isostatic pressing the block at 250MPa for 1min, and maintaining the pressureSintering the block at 1650 ℃ for 10h to obtain the zirconate system negative temperature coefficient thermistor material;
c. coating platinum slurry electrodes on the front and back surfaces of the zirconate system negative temperature coefficient thermistor material obtained in the step B, and then annealing for 1 hour at the temperature of 900 ℃ to obtain the material with the electrical property parameter B400/1000＝14060K，ρ1000℃A novel zirconate-based negative temperature coefficient thermistor material of 5289 Ω · cm.
Example 5
Any one of the zirconate system negative temperature coefficient thermistor materials obtained in the examples 1 to 4 is subjected to cation change at the A position, so that a novel pyrochlore structure high-temperature negative temperature coefficient thermistor material is obtained. The material has the advantages of simple preparation process, good consistency, stable aging performance and insensitivity to oxygen partial pressure, and is a novel thermistor material suitable for manufacturing environments with high temperature and different oxygen partial pressures.
Claims (2)
1. A zirconate system negative temperature coefficient thermistor material is characterized in that the chemical general formula of the thermistor material is as follows: a. the2Zr2O7Wherein A = Nd, Sm, Gd or Yb, is prepared by mixing and firing zirconium dioxide as a raw material with samarium sesquioxide, ytterbium sesquioxide, neodymium sesquioxide or gadolinium sesquioxide respectively.
2. The method of making a zirconate system ntc thermistor according to claim 1, comprising the steps of:
a. according to A2Zr2O7Weighing zirconium dioxide, mixing the zirconium dioxide with samarium sesquioxide, ytterbium sesquioxide, neodymium sesquioxide or gadolinium sesquioxide respectively, placing the mixture into an agate ball milling tank, wet-milling the mixture for 6 to 8 hours by using analytically pure absolute ethyl alcohol as a dispersion medium, drying the slurry after the wet milling at the temperature of 150 ℃, taking out and milling the slurry for 1 hour to obtain powder;
b. b, mixing the powder obtained in the step a at a ratio of 15-25kg/cm2Pressing into blocks for 1-2min, and coolingIsostatic pressing, maintaining the pressure at 250-300MPa for 1-3min, and sintering the block at 1650 ℃ for 10h to obtain the zirconate system negative temperature coefficient thermistor material;
c. coating platinum slurry electrodes on the front and back surfaces of the zirconate system negative temperature coefficient thermistor material obtained in the step b, and then annealing at the temperature of 900 ℃ for 1-2h to obtain the material with the electrical performance parameters as follows: b is400℃/1000℃=9812-14060K, ρ1000℃=1.513-5.289×103Omega cm zirconate system negative temperature coefficient thermistor material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112759391A (en) * | 2020-12-31 | 2021-05-07 | 中科立民新材料（扬州）有限公司 | Ytterbium-doped NTC (negative temperature coefficient) type high-temperature thermistor ceramic material as well as preparation method and application thereof |
| CN112876238A (en) * | 2021-02-25 | 2021-06-01 | 中国科学院新疆理化技术研究所 | Stannate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112939602A (en) * | 2021-02-25 | 2021-06-11 | 中国科学院新疆理化技术研究所 | Titanate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112960979A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Zirconate system high-temperature negative temperature coefficient thermistor material and preparation method thereof |
| CN115894029A (en) * | 2023-01-03 | 2023-04-04 | 中国科学院新疆理化技术研究所 | Oxygen-insensitive negative temperature coefficient thermosensitive material based on high-entropy rare earth zirconate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112759391A (en) * | 2020-12-31 | 2021-05-07 | 中科立民新材料（扬州）有限公司 | Ytterbium-doped NTC (negative temperature coefficient) type high-temperature thermistor ceramic material as well as preparation method and application thereof |
| CN112876238A (en) * | 2021-02-25 | 2021-06-01 | 中国科学院新疆理化技术研究所 | Stannate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112939602A (en) * | 2021-02-25 | 2021-06-11 | 中国科学院新疆理化技术研究所 | Titanate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112960979A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Zirconate system high-temperature negative temperature coefficient thermistor material and preparation method thereof |
| CN112939602B (en) * | 2021-02-25 | 2023-04-18 | 中国科学院新疆理化技术研究所 | Titanate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112876238B (en) * | 2021-02-25 | 2023-04-18 | 中国科学院新疆理化技术研究所 | Stannate system negative temperature coefficient thermistor material and preparation method thereof |
| CN115894029A (en) * | 2023-01-03 | 2023-04-04 | 中国科学院新疆理化技术研究所 | Oxygen-insensitive negative temperature coefficient thermosensitive material based on high-entropy rare earth zirconate |
| CN115894029B (en) * | 2023-01-03 | 2023-09-01 | 中国科学院新疆理化技术研究所 | Oxygen-insensitive negative temperature coefficient thermosensitive material based on high-entropy rare earth zirconate |
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