CN105967674A - Chromium-doped magnesium aluminate high temperature thermistor material and preparation method thereof - Google Patents

Chromium-doped magnesium aluminate high temperature thermistor material and preparation method thereof Download PDF

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CN105967674A
CN105967674A CN201610297600.8A CN201610297600A CN105967674A CN 105967674 A CN105967674 A CN 105967674A CN 201610297600 A CN201610297600 A CN 201610297600A CN 105967674 A CN105967674 A CN 105967674A
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temperature
chromium
thermistor material
magnesium aluminate
high temperature
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张博
杨田
赵青
常爱民
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a chromium-doped magnesium aluminate high temperature thermistor material and a preparation method thereof. The Mg(Al1-xCrx)2O4 (wherein x is greater than or equal to 0 and less than or equal to 0.5) thermistor material is prepared from aluminum oxide, magnesium oxide and chromic oxide by mixing and grinding, calcination, grinding, molding, cold isostatic pressing molding and high temperature sintering. The high temperature thermistor material has a constant of B500 DEG C/800 DEG C=(6800-12000)*(1+/-2%)K, electrical resistivity of (2.7*10<3>-3.8*10<7>)*(1+/-5%) omega cm at a temperature of 500 DEG C and has a resistance change rate within +/-10% after 500 DEG C high temperature aging for 300h. The chromium-doped magnesium aluminate high temperature thermistor material has a negative temperature coefficient, stable electrical properties, good uniformity and table aging performances and is suitable for manufacture of a novel thermistor material of a thermistor in a high temperature environment.

Description

A kind of chromium doping magnesium aluminate high-temperature thermistor material and preparation method thereof
Technical field
The present invention relates to a kind of chromium doping magnesium aluminate high-temperature thermistor material and preparation method thereof, this thermistor material There is in the range of temperature 500-1000 DEG C obvious negative temperature coefficient feature, be that one is applicable to manufacture high-temperature thermistor Novel thermosensitive ceramic material, belong to semiconductor transducer field.
Background technology
Sensing element and sensor are one of three big pillars of the electronics and information industry that country determines, have been considered as Having the electronic technology product of development prospect, development Sensitive Apparatus has act foot light to promoting China's electronics industry status in the world The effect of weight.Critesistor has highly sensitive, good reliability, lower-price characteristic, has been widely used in daily life Electrical appliance and the temperature sensing of industrial equipment and control.The main application of NTC thermistor includes: temperature-compensating, suppression surge Electric current, therm-param method.For meeting the high temperature application demand of auto industry and aircraft industry, high-temperature thermistor material is Become the new development trend in NTC thermistor field and study hotspot.
MgAl2O4There is the highest fusing point (2130 DEG C), and it is excellent to have excellent mechanical behavior under high temperature and resistance to chemical attack etc. Point, has been widely used as the fields such as refractory material, moisture sensor, and crystalline ceramics.Adulterated by Cr, MgAl can be made2O4Tool There are semiconduction, high-melting-point and a characteristic such as high-temperature stability, high intensity, and then become and prepare high-temperature thermistor ideal material.
The present invention passes through Cr doped spinel type MgAl2O4Material prepares new type high temperature thermistor material.This material Having obvious negative temperature coefficient feature, material system electric performance stablity, concordance is preferable, and ageing properties is stable, is suitable for manufacturing Thermal resistor in hot environment.
Summary of the invention
It is an object of the invention to, it is provided that a kind of chromium doping magnesium aluminate high-temperature thermistor material and preparation method thereof, should Material with aluminium sesquioxide, magnesium oxide and chromic oxide as raw material, blended grinding, calcine, grind, molding, isostatic cool pressing Molding, high temperature sintering, i.e. can get Mg (Al1-xCrx)2O4(0≤x≤0.5) high-temperature thermistor material, its material constant is B500℃/800℃=(6800-12000) × (1 ± 2%) K, 500 DEG C of resistivity of temperature are (2.7 × 103–3.8×107)×(1± 5%) Ω cm, 500 DEG C of high temperature ageings of temperature after 300 hours resistance varying-ratio within ± 10%.Use chromium prepared by the present invention Doping magnesium aluminate thermistor material has negative temperature coefficient feature, material system electric performance stablity, and concordance is preferable, aging Can be stable, it is suitable for manufacturing the thermal resistor in hot environment.
A kind of chromium doping magnesium aluminate high-temperature thermistor material of the present invention, the structural formula of this thermistor material is Mg(Al1-xCrx)2O4, wherein 0≤x≤0.5, it is made up of raw material aluminium sesquioxide, magnesium oxide and chromic oxide.
The preparation method of described chromium doping magnesium aluminate high-temperature thermistor material, follows these steps to carry out:
A, by raw material aluminium sesquioxide, magnesium oxide and chromic oxide by molecular formula Mg (Al1-xCrx)2O4Wherein 0≤x≤ The composition of 0.5, calculates the quality of needed raw material, and uniformly mixes, be placed in agate mortar and be ground, time Between 5-8 hour, obtain powder body；
B, the powder body that obtains in step a is calcined 5-8 hour in temperature 1100-1300 DEG C, then after grinding 6-10 hour i.e. Obtain critesistor powder body；
C, powder body step b obtained are with 30-60Kg/cm2Pressure carry out compound stalk forming, the time is 1-3 minute, will become The block materials of type carries out isostatic cool pressing, and pressurize 1-4 minute under pressure is 200-400MPa, then by block in temperature At 1500-1800 DEG C sinter 4-7 hour, chromium doping magnesium aluminate thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then at temperature 1200 DEG C, annealing 2 is little Time, i.e. obtain chromium doping magnesium aluminate high-temperature thermistor material.
Chromium of the present invention doping magnesium aluminate high-temperature thermistor material, uses solid phase method that analytical pure three is aoxidized two Aluminum, analytical pure chromic oxide and analytical pure magnesium oxide carry out mixing and grind, calcining, grind and i.e. obtain negative temperature coefficient thermistor power again Resistance powder body material, then by this powder body material chip cold isostatic compaction, after high temperature sintering, tow sides blackening platinum slurry electrode obtains Critesistor disk, this thermo-sensitive material is single spinel structure, and material constant of thermistor is B500℃/800℃=(6800- 12000) × (1 ± 2%) K, 500 DEG C of resistivity of temperature are (2.7 × 103–3.8×107) × (1 ± 5%) Ω cm, 500 DEG C of high temperature After aging 300 hours, resistance varying-ratio is within ± 10%
The present invention utilizes chromium doping MgAl2O4Spinel is prepared for chromium doping magnesium aluminate high-temperature thermistor material, its Innovative point mainly has following two aspect.
(1)MgAl2O4Material is materials with high melting point, stable performance in hot environment, and it is special to have certain negative temperature Property, as matrix material.Doping variable valency Cr element after have the most simultaneously semiconduction, high-melting-point and high-temperature stability, The characteristics such as high intensity so that it becomes the ideal material preparing high-temperature thermistor.
(2) chromium doping MgAl2O4Material, wherein Cr3+Replace part Al3+Ion, forms solid solution, it is achieved that MgAl2O4Material The regulation of material electrical property.
This material has obvious negative temperature coefficient feature, material system electric performance stablity, and concordance is preferable, ageing properties Stable, it is suitable for manufacturing the thermal resistor in hot environment.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the present invention, wherein ◆ for MgAl2O4；
Fig. 2 is the scanning electron microscope (SEM) photograph of the present invention.
Detailed description of the invention
Embodiment 1
A, by MgAl2O4Composition, weigh analytical pure aluminium sesquioxide 57.3373g and analytical pure magnesium oxide respectively 22.6627g mixes, and is placed in agate mortar and is ground, and 5 hours time, obtains powder body；
B, powder body ground in step a is calcined 5 hours temperature 1100 DEG C, more i.e. obtain MgAl after grinding 6 hours2O4 Powder body；
C, powder body step b obtained weigh 0.3g, with 30Kg/cm2Pressure carry out compound stalk forming, the dwell time is 1 Minute, the block materials of molding is carried out isostatic cool pressing, pressurize 1 minute under pressure 200MPa, then in temperature 1500 DEG C burning Tie 4 hours, prepare thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then at temperature 1200 DEG C, annealing 2 is little Time, i.e. obtain a size of Φ 8.15mm × 1.9mm chromium doping magnesium aluminate high-temperature thermistor disk.
The thermistor material obtained by the method is 3.8 × 10 in 500 DEG C of resistivity of temperature7× (1 ± 5%) Ω Cm, material constant is B500℃/800℃=12000 × (1 ± 2%) K, 500 DEG C of high temperature ageings of temperature resistance varying-ratio after 300 hours For ± 10%.
Embodiment 2
A, by Mg (Al1.9Cr0.1)2O4Composition, weigh analytical pure aluminium sesquioxide 49.7990g, analytical pure three oxygen respectively Change two chromium 8.3308g and analytical pure magnesium oxide 21.8702g, and mix, be placed in agate mortar and be ground, time Between 6 hours, obtain powder body；
B, the powder body that obtains in step a is calcined 6 hours temperature 1200 DEG C, after grinding 7 hours, i.e. obtain Mg (Al1.9Cr0.1)2O4Powder body；
C, powder body material step b obtained weigh 0.3g, with 40Kg/cm2Pressure carry out compound stalk forming, the time is 2 Minute, the block materials of molding is carried out isostatic cool pressing, pressurize 2 minutes under pressure 300MPa, then in temperature 1600 DEG C burning Tie 3 hours, prepare thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then at temperature 1200 DEG C, annealing 2 is little Time, i.e. obtain a size of Φ 8.5mm × 2.0mm chromium doping magnesium aluminate high-temperature thermistor disk.
The thermistor material resistivity at temperature is 500 DEG C obtained by the method is 5.4 × 106× (1 ± 5%) Ω cm, material constant is B500℃/800℃=10800 × (1 ± 2%) K, 100 DEG C of high temperature ageings of temperature change in resistance after 300 hours Rate is ± 10%.
Embodiment 3
A, by Mg (Al1.9Cr0.1)2O4Composition, weigh analytical pure aluminium sesquioxide 49.7990g, analytical pure three oxygen respectively Change two chromium 8.3308g and analytical pure magnesium oxide 21.8702g, and mix, be placed in agate mortar and be ground, time Between 7 hours, obtain powder body；
B, by powder body ground in step a temperature 1200 DEG C calcine 6 hours, i.e. obtain Mg after grinding 7 hours (Al1.9Cr0.1)2O4Powder body；
C, powder body material step b obtained weigh 0.3g, with 40Kg/cm2Pressure carry out compound stalk forming, the time is 2 Minute, the block materials of molding is carried out isostatic cool pressing, pressurize 2 minutes under pressure 300MPa, then in temperature 1700 DEG C burning Tie 3 hours, prepare thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then at temperature 1200 DEG C, annealing 2 is little Time, i.e. obtain a size of Φ 8.3mm × 2.0mm chromium doping aluminic acid high-temperature thermistor disk.
The thermistor material resistivity at temperature is 500 DEG C obtained by the method is 5.1 × 106× (1 ± 5%) Ω cm, material constant is B500℃/800℃=10500 × (1 ± 2%) K, 500 DEG C of high temperature ageings of temperature change in resistance after 300 hours Rate is ± 8%.
Embodiment 4
A, by Mg (Al1.7Cr0.3)2O4Composition, weigh analytical pure aluminium sesquioxide 36.2007g, analytical pure three oxygen respectively Change two chromium 23.3586g and analytical pure magnesium oxide 20.4406g, and mix, be placed in agate mortar and be ground, time Between 6 hours, obtain powder body；
B, by powder body ground in step a temperature 1300 DEG C calcine 6 hours, i.e. obtain Mg after grinding 7 hours (Al1.7Cr0.3)2O4Powder body；
C, powder body material step b obtained weigh 0.3g, with 50Kg/cm2Pressure carry out compound stalk forming, the time is 2 Minute, the block materials of molding is carried out isostatic cool pressing, pressurize 3 minutes under pressure 300MPa, then in temperature 1800 DEG C burning Tie 7 hours, prepare thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then at temperature 1200 DEG C, annealing 2 is little Time, i.e. obtain a size of Φ 8.1mm × 1.8mm chromium doping magnesium aluminate high-temperature thermistor disk.
The thermistor material resistivity at temperature is 500 DEG C obtained by the method is 2.6 × 104× (1 ± 5%) Ω cm, material constant is B500℃/800℃=10300 × (1 ± 2%) K, 500 DEG C of high temperature ageings of temperature change in resistance after 300 hours Rate is ± 7%.
Embodiment 5
A, by Mg (Al1.5Cr0.5)2O4Composition, weigh analytical pure aluminium sesquioxide 24.2711g, analytical pure three oxygen respectively Change two chromium 36.5424g and analytical pure magnesium oxide 19.1865g, and mix, be placed in agate mortar and be ground, time Between 8 hours, obtain powder body；
B, by powder body ground in step a temperature 1300 DEG C calcine 8 hours, i.e. obtain Mg after grinding 10 hours (Al1.5Cr0.5)2O4Powder body；
C, powder body material step b obtained, weigh 0.3g, with 60Kg/cm2Pressure carry out compound stalk forming, the time is 3 Minute, the block materials of molding is carried out isostatic cool pressing, pressurize 4 minutes under pressure 400MPa, then in temperature 1800 DEG C burning Tie 7 hours, prepare thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then at temperature 1200 DEG C, annealing 2 is little Time, i.e. obtain a size of Φ 8.1mm × 1.7mm chromium doping magnesium aluminate high-temperature thermistor disk.
The thermistor material resistivity at temperature is 500 DEG C obtained by the method is 2.7 × 103× (1 ± 5%) Ω cm, material constant is B500℃/800℃=6800 × (1 ± 2%) K, 500 DEG C of high temperature ageings of temperature resistance varying-ratio after 300 hours For ± 10%.

Claims (2)

1. a chromium doping magnesium aluminate high-temperature thermistor material, it is characterised in that the structural formula of this thermistor material is Mg (Al1-xCrx)2O4, wherein 0≤x≤ 0.5, it is made up of raw material aluminium sesquioxide, magnesium oxide and chromic oxide.
The preparation method of chromium the most according to claim 1 doping magnesium aluminate thermistor material, it is characterised in that by following Step is carried out:
A, by raw material aluminium sesquioxide, magnesium oxide and chromic oxide by molecular formula Mg (Al1-xCrx)2O4, wherein 0≤x≤0.5 Composition, calculate the quality of needed raw material, and uniformly mix, be placed in agate mortar and be ground, the time 5-8 hour, obtain powder body；
B, the powder body that obtains in step a is calcined 5-8 hour in temperature 1100-1300 DEG C, more i.e. obtain after grinding 6-10 hour hot Quick resistance powder body；
C, powder body step b obtained are with 30-60Kg/cm2Pressure carry out compound stalk forming, the time is 1-3 minute, by molding Block materials carries out isostatic cool pressing, and pressurize 1-4 minute under pressure is 200-400MPa, then by block in temperature 1500- At 1800 DEG C sinter 4-7 hour, chromium doping magnesium aluminate thermal sensitive ceramic material；
D, ceramic material tow sides step c obtained coating platinum slurry electrode, then anneals 2 hours at temperature 1200 DEG C, I.e. obtain chromium doping magnesium aluminate high-temperature thermistor material.
CN201610297600.8A 2016-05-06 2016-05-06 Chromium-doped magnesium aluminate high temperature thermistor material and preparation method thereof Pending CN105967674A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN107056273A (en) * 2017-05-25 2017-08-18 中国科学院新疆理化技术研究所 A kind of double-deck negative tempperature coefficient thermistor and preparation method thereof
CN107324799A (en) * 2017-08-07 2017-11-07 中国科学院新疆理化技术研究所 A kind of perovskite-like type high-temperature thermistor material and preparation method thereof
CN108640671A (en) * 2018-05-17 2018-10-12 赵娟 The preparation method of NTC sensitive ceramic resistor materials
CN109550492A (en) * 2018-12-12 2019-04-02 余嘉琪 A kind of preparation method of high thermal conductivity high-specific surface area magnesium aluminate spinel
CN112624740A (en) * 2020-12-26 2021-04-09 重庆材料研究院有限公司 High-entropy NTC thermistor ceramic material and preparation method thereof
CN113603475A (en) * 2021-07-27 2021-11-05 西南科技大学 Preparation method of trivalent chromium ion doped magnesium aluminate spinel transparent ceramic
CN114195505A (en) * 2021-11-25 2022-03-18 天津津航技术物理研究所 Ceramic with red fluorescence property and preparation method thereof

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JPS5123691A (en) * 1974-08-20 1976-02-25 Matsushita Electric Ind Co Ltd KOONDOYOSAAMISUTA
EP1179825A2 (en) * 2000-08-10 2002-02-13 Denso Corporation Reduction resistant thermistor method of production thereof, and temperature sensor
US20110042627A1 (en) * 2008-04-14 2011-02-24 Katsunori Yamada Thermistor material for use in reducing atmosphere

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Publication number Priority date Publication date Assignee Title
JPS5123691A (en) * 1974-08-20 1976-02-25 Matsushita Electric Ind Co Ltd KOONDOYOSAAMISUTA
EP1179825A2 (en) * 2000-08-10 2002-02-13 Denso Corporation Reduction resistant thermistor method of production thereof, and temperature sensor
US20110042627A1 (en) * 2008-04-14 2011-02-24 Katsunori Yamada Thermistor material for use in reducing atmosphere

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107056273A (en) * 2017-05-25 2017-08-18 中国科学院新疆理化技术研究所 A kind of double-deck negative tempperature coefficient thermistor and preparation method thereof
CN107324799A (en) * 2017-08-07 2017-11-07 中国科学院新疆理化技术研究所 A kind of perovskite-like type high-temperature thermistor material and preparation method thereof
CN107324799B (en) * 2017-08-07 2020-11-06 中国科学院新疆理化技术研究所 Perovskite-like high-temperature thermistor material and preparation method thereof
CN108640671A (en) * 2018-05-17 2018-10-12 赵娟 The preparation method of NTC sensitive ceramic resistor materials
CN109550492A (en) * 2018-12-12 2019-04-02 余嘉琪 A kind of preparation method of high thermal conductivity high-specific surface area magnesium aluminate spinel
CN109550492B (en) * 2018-12-12 2022-06-28 余嘉琪 Preparation method of high-thermal-conductivity high-specific-surface-area magnesium aluminate spinel
CN112624740A (en) * 2020-12-26 2021-04-09 重庆材料研究院有限公司 High-entropy NTC thermistor ceramic material and preparation method thereof
CN112624740B (en) * 2020-12-26 2022-08-02 重庆材料研究院有限公司 High-entropy NTC thermistor ceramic material and preparation method thereof
CN113603475A (en) * 2021-07-27 2021-11-05 西南科技大学 Preparation method of trivalent chromium ion doped magnesium aluminate spinel transparent ceramic
CN114195505A (en) * 2021-11-25 2022-03-18 天津津航技术物理研究所 Ceramic with red fluorescence property and preparation method thereof

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