CN107056273A - A kind of double-deck negative tempperature coefficient thermistor and preparation method thereof - Google Patents

A kind of double-deck negative tempperature coefficient thermistor and preparation method thereof Download PDF

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CN107056273A
CN107056273A CN201710379104.1A CN201710379104A CN107056273A CN 107056273 A CN107056273 A CN 107056273A CN 201710379104 A CN201710379104 A CN 201710379104A CN 107056273 A CN107056273 A CN 107056273A
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赵青
印杏莲
张博
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 present invention relates to a kind of double-deck negative tempperature coefficient thermistor and preparation method thereof.The resistance is by A layers of MgAl2O4With B layers of LaCrO3 Constitute double-decker, or A layers of MgAl2O4Dopant Mg1−xMxAl2O4With B layers of LaCrO3Constitute double-decker, or A layers of MgAl2O4With B layers of LaCrO3Dopant La1‑xMxCrO3Constitute double-decker, or A layers of MgAl2O4Dopant Mg1−xMxAl2O4With B layers of LaCrO3Dopant La1‑xMxCrO3Double-decker is constituted, after tested：The electrical resistivity range of double-deck negative tempperature coefficient thermistor of the present invention is 342-5.5 × 108The ratio between cm, A layers of Ω and B layers molal quantity are：A / B=0.28‑2.33.Compared with prior art, the double-deck NTC thermistors working range that prepared by the present invention is wide, is applicable to room temperature to 1000 DEG C, electric performance stablity under high temperature, preparation flow is simply efficient.

Description

A kind of double-deck negative tempperature coefficient thermistor and preparation method thereof
Technical field
The present invention relates to negative temperature coefficient (NTC) thermistor technology field, and in particular to one kind can be in room temperature to 1000 Double-deck negative tempperature coefficient thermistor in DEG C working range and preparation method thereof.
Background technology
Research to negative temperature coefficient (NTC) thermistor is divided into low temperature (≤- 60 DEG C)；Middle temperature (- 60 DEG C -300 DEG C) and High temperature (>=300 DEG C).High-temperature NTC heat-sensitive resistance exists：Cosmic space, the measurement of automobile effluent air temp, the temperature of industrial equipment There is the application that it can not be substituted in the field such as degree measurement and control.But the NTC thermistor under high-temperature work environment easily occurs Electrical property is unstable, i.e., resistance fluctuating is excessive, application of the influence NTC thermistor in practical study and production.Therefore obtain Obtain functional at high temperature and stable NTC material is critically important.
Application of the double-decker in NTC thermistor field is broadly divided into two kinds：It is NTC sensitive layers, B layers that one kind, which is A layers, For high conductance supporting layer, resistance is reduced to reduce the thickness of sensitive layer, at the same B value changes less so that obtain high B values, it is low Negative temperature coefficient of resistance (NTC) material；Another to be A layers, B layers be negative temperature coefficient (NTC) sensitive layer, negative by two layers Effect between temperature coefficient (NTC) thermo-sensitive material adjusts the electrical property of negative temperature coefficient (NTC) material.
Disclosed through retrieving the A of Chinese patent CN 104124014, use one kind with AxMn3-xO4(A is in Zn, Ni, Co, Fe It is one or more) and LaSryBO3Double-deck negative temperature coefficient (NTC) heat of (B is the one or more in Fe, Co, Ni, Mn) composition Quick resistance, electrical resistivity range is 10-104Ω cm, resistivity is too small, may be only available for the environment below 300 DEG C of temperature, and its Double-decker is the bilayer film prepared by way of curtain coating, and the limitation to raw material is more, and not every material can be compared with Slurry is prepared into well, then obtains bilayer film.
The content of the invention
It is an object of the present invention to overcome the unstable defect of negative temperature coefficient under high temperature (NTC) material electrical property there is provided One kind can apply to room temperature to 1000 DEG C, and the double-deck negative tempperature coefficient thermistor of energy steady operation and preparation method thereof.Should Resistance is by A layers of MgAl2O4With B layers of LaCrO3Constitute double-decker, or A layers of MgAl2O4Dopant Mg1-xMxAl2O4With B layers LaCrO3Constitute double-decker, or A layers of MgAl2O4With B layers of LaCrO3Dopant La1-xMxCrO3Constitute double-decker, or A layers MgAl2O4Dopant Mg1-xMxAl2O4With B layers of LaCrO3Dopant La1-xMxCrO3Double-decker is constituted, after tested：Institute of the present invention The electrical resistivity range for the double-deck negative tempperature coefficient thermistor stated is 342-5.5 × 108Cm, the A layers of molal quantitys with B layers of Ω The ratio between be：A/B=0.28-2.33.Compared with prior art, the double-deck NTC thermistor working range that prepared by the present invention is wide, can Suitable for room temperature to 1000 DEG C, electric performance stablity under high temperature, preparation flow is simply efficient.
A kind of double-deck negative tempperature coefficient thermistor of the present invention, the resistance is by A layers of MgAl2O40.1-0.8g and B layers of LaCrO30.3-1.6g constitutes double-decker, or A layers of Mg1-xCaxAl2O4, 0.01≤x≤0.5 and B layers of LaCrO3Composition is double Rotating fields, wherein A layer are 0.2-0.8536g, and B layers are 0.3-1.6g；Or A layers of MgAl2O4With B layers of La1-xCaxCrO3, 0.01≤x ≤ 0.38 composition double-decker, wherein A layers is 0.1-0.8g, and B layers are 0.2389-1.4336g；Or A layers of Mg1-xCaxAl2O4, 0.01≤x≤0.5 and B layers of La1-xCaxCrO3, the composition double-decker of 0.01≤x≤0.38, wherein A layer is 0.2-0.8536g, B Layer is 0.2389-1.4336g, and the operating temperature range of the double-deck negative tempperature coefficient thermistor is from room temperature to 1000 DEG C, resistance Rate scope is 342-5.5 × 108The ratio between cm, A layers of Ω and B layers molal quantity are：A/B=0.28-2.33.
The preparation method of the double-deck negative tempperature coefficient thermistor, follows these steps to carry out：
a、MgAl2O4The preparation of powder：Pure Al will be analyzed respectively2O3Mixed with pure MgO is analyzed, be placed in agate mortar Middle grinding 6h-10h, obtains oxide powder, oxide powder is calcined into 1.5-4h at 1000-1300 DEG C of temperature, after calcining Powder grind MgAl is produced after 8h again2O4Powder；
b、LaCrO3The preparation of powder：Pure La will be analyzed respectively2O3With the pure Cr of analysis2O3Mixed, be placed in agate mortar Middle grinding 6-10h, obtains oxide powder, oxide powder is calcined into 1.5-4h at 1000-1300 DEG C of temperature, after calcining Powder grinds LaCrO is produced after 8h again3Powder；
C, double-deck NTC thermistor preparation：The MgAl that step a is obtained is weighed respectively2O40.1-0.8g powders, step b Obtained LaCrO30.3-1.6g powders, first by LaCrO3Powder pours into shaping Ф 10mm moulds, pours into MgAl after shaking up again2O4 Powder, with 30-60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 1-3min, the block materials of shaping is carried out cold Isostatic pressed, the pressurize 1min in the case where pressure is 180-400MPa, then in 1500-1800 DEG C of ordinary sinter temperature, vacuum-sintering temperature It is sintered at 1200-1500 DEG C of 1300-1600 DEG C of degree or hot pressed sintering temperature, sintering time is 1-6h, obtains A layers and B layers Double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 1.5-3h, produce double-deck negative tempperature coefficient thermistor.
Compared with prior art, the present invention has advantages below：(1) operating temperature range is wide (room temperature is to 1000 DEG C)：It is logical Overregulate bilayer (high-resistance MgAl2O4And its dopant and the LaCrO of high stability3And its dopant) between thickness ratio (mol ratio) or experiment condition and parameter, can obtain resistivity and be applied to room temperature to 1000 DEG C of negative temperature coefficient (NTC) thermistor.(2) high temperatures are good：By by high-resistance MgAl2O4And its dopant and high stability LaCrO3And its double-decker that dopant is built into, have high resistance, the big feature of high stability two concurrently, at high temperature can obtain Negative temperature coefficient (NTC) thermistor of steady operation.(3) experiment flow is simply efficient, reduces cost：For double-decker Realization only need to simple compressing, sintering, it is not necessary to such as curtain coating, sputtering complicated technology.
Brief description of the drawings
Fig. 1 is the SEM photograph of the embodiment of the present invention 1.
Embodiment
Embodiment given by the present invention, but it is not limited to following embodiments.
Embodiment 1
a、MgAl2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3Pure MgO is analyzed with 5.6661g to carry out Mixing, is placed in agate mortar and grinds 6h, obtain oxide powder, and oxide powder is calcined into 1.5h at 1100 DEG C of temperature, Powder after calcining is ground again produces MgAl after 8h2O4Powder；
b、LaCrO3The preparation of powder：20.3920g is weighed respectively analyzes pure La2O3Pure Cr is analyzed with 9.6080g2O3Carry out Mixing, is placed in agate mortar and grinds 6h, obtain oxide powder, oxide powder is calcined into 1.5h at 1000 DEG C, after calcining Powder grind LaCrO is produced after 8h again3Powder；
C, double-deck negative tempperature coefficient thermistor preparation：The 0.498gMgAl that step a is obtained is weighed respectively2O4Powder, step The 0.359gLaCrO that rapid b is obtained3Powder, first by LaCrO3Powder pours into Ф 10mm moulds, pours into MgAl after shaking up again2O4 Powder, with 30Kg/cm2Pressure carry out compound stalk forming, the dwell time is 1min, the block materials of shaping is carried out cold etc. quiet Then pressure, the pressurize 1min under pressure 200MPa obtains A layers and B layers bilayer using ordinary sinter in 1650 DEG C of sintering 6h of temperature Ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 1.5h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to resistance temperature test is carried out to obtained double-deck negative tempperature coefficient thermistor at 1000 DEG C, in temperature 500h burn-in test, resistance fluctuating=(R-R of thermistor are carried out at 800 DEG C of degree0)/R0* 100%, R0For without aging Thermistor in 800 DEG C of temperature, the resistance measured, R is the electricity measured through 800 DEG C of aging 500h of temperature after 800 DEG C of temperature Resistance, the resulting double-deck negative tempperature coefficient thermistor resistivity at 1000 DEG C of temperature is 2.47 × 106Ω cm, temperature Aging 500h resistance fluctuating is 7.59%, A layers and is with B layers of mole ratio at 800 DEG C：A/B=2.33.
Embodiment 2
a、MgAl2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3Pure MgO is analyzed with 5.6661g to carry out Mixing, is placed in agate mortar and grinds 8h, obtain oxide powder, and oxide powder is calcined into 2h at 1000 DEG C of temperature, forged Powder after burning is ground again produces MgAl after 8h2O4Powder；
b、LaCrO3The preparation of powder：20.3920g is weighed respectively analyzes pure La2O3Pure Cr is analyzed with 9.6080g2O3Carry out Mixing, is placed in agate mortar and grinds 8h, obtain oxide powder, by oxide powder in 1300 DEG C of calcining 4h of temperature, calcining Powder afterwards is ground again produces LaCrO after 8h3Powder；
C, double-deck NTC thermistor preparation：The 0.8gMgAl that step a is obtained is weighed respectively2O4Powder, step b is obtained 1.6gLaCrO3Powder, first by LaCrO3Powder pours into the supporting graphite jig of vacuum hotpressing stove, and MgAl is poured into after shaking up2O4Powder Body, to sinter 1h under conditions of 1500 DEG C of temperature, 1ton, obtains A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 2h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to resistance temperature test is carried out to obtained double-deck negative tempperature coefficient thermistor at 1000 DEG C, in temperature Carry out 500h burn-in test at 800 DEG C of degree, the resulting double-deck negative tempperature coefficient thermistor resistance at 1000 DEG C of temperature Rate is 2542 Ω cm, and resistivity is 2.47 × 10 at room temperature6Aging 500h resistance fluctuating at Ω cm, 800 DEG C of temperature It is with B layers of mole ratio for 7.59%, A layers：A/B=0.84.
Embodiment 3
a、MgAl2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3Pure MgO is analyzed with 5.6661g to carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 4h at 1300 DEG C, after calcining Powder grind MgAl is produced after 8h again2O4Powder；
b、LaCrO3The preparation of powder：20.3920g is weighed respectively analyzes pure La2O3Pure Cr is analyzed with 9.6080g2O3Carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 2h at 1300 DEG C, after calcining Powder grinds LaCrO is produced after 8h again3Powder；
C, double-deck NTC thermistor preparation：The 0.1gMgAl that step a is obtained is weighed respectively2O4Powder, step b is obtained 0.6gLaCrO3Powder, first by LaCrO3Powder pours into Ф 10mm moulds, pours into MgAl after shaking up again2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, the block materials of shaping is carried out into isostatic cool pressing, in pressure Pressurize 1min under 400MPa, then carries out vacuum-sintering, and temperature is 1500 DEG C, vacuum is to sinter 1 hour under -0.8bar, is obtained To A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 342 Ω cm at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor, at room temperature resistivity For 1.49 × 106Aging 500h resistance fluctuating is the mole ratio of 19.19%, A layers and B layers at Ω cm, 800 DEG C of temperature For：A/B=0.28.
Embodiment 4
a、Mg0.99Ca0.01Al2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3, 5.6044g analysis it is pure MgO and 0.079g analyzes pure CaO and mixed, and is placed in agate mortar and grinds 10h, obtain oxide powder, by oxidate powder Body calcines 4h at 1300 DEG C, and the powder after calcining is ground again produces Mg after 8h0.99Ca0.01Al2O4Powder；
b、LaCrO3The preparation of powder：20.3920g is weighed respectively analyzes pure La2O3Pure Cr is analyzed with 9.6080g2O3Carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 3h at 1300 DEG C, after calcining Powder grinds LaCrO is produced after 8h again3Powder；
C, double-deck NTC thermistor preparation：The 0.2gMg that step a is obtained is weighed respectively0.99Ca0.01Al2O4Powder, step The 0.4gLaCrO that rapid b is obtained3Powder, first by LaCrO3Powder pours into Ф 10mm moulds, is poured into again after shaking up Mg0.99Ca0.01Al2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, by the block material of shaping Material carries out isostatic cool pressing, and then the pressurize 1min under pressure 400MPa carries out vacuum-sintering, temperature is 1300 DEG C, vacuum for- Sintered 6 hours under 0.8bar, obtain A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 1 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor6Ω cm, 500 DEG C of temperature Lower resistivity is 5.5 × 108Aging 500h resistance fluctuating is 17.3%, A layers and rubbed with B layers at Ω cm, 800 DEG C of temperature You are at number ratio：A/B=0.842.
Embodiment 5
a、Mg0.5Ca0.5Al2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3, 2.8331g analyze pure MgO Pure CaO is analyzed with 3.9414g to be mixed, and is placed in agate mortar and is ground 8h, obtain oxide powder, oxide powder is existed 4h is calcined at 1200 DEG C, the powder after calcining is ground again produces Mg after 8h0.5Ca0.5Al2O4Powder；
b、LaCrO3The preparation of powder：20.3920g is weighed respectively analyzes pure La2O3Pure Cr is analyzed with 9.6080g2O3Carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 3h at 1300 DEG C, after calcining Powder grinds LaCrO is produced after 8h again3Powder；
C, double-deck NTC thermistor preparation：The 0.3gMg that step a is obtained is weighed respectively0.5Ca0.5Al2O4Powder, step b Obtained 0.4gLaCrO3Powder, first by LaCrO3Powder pours into Ф 10mm moulds, is poured into again after shaking up Mg0.5Ca0.5Al2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, by the block materials of shaping Isostatic cool pressing is carried out, then the pressurize 1min under pressure 400MPa carry out ordinary sinter, is sintered 6 hours at 1500 DEG C of temperature, Obtain A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 2h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 2.13 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor3Ω cm, at room temperature Resistivity is 4.22 × 106Aging 500h resistance fluctuating is mole of 9.7%, A layers and B layers at Ω cm, 800 DEG C of temperature Counting ratio is：A/B=1.1972.
Embodiment 6
a、Mg0.7Ca0.3Al2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3, 1.6998g analyze pure MgO Pure CaO is analyzed with 3.3783g to be mixed, and is placed in agate mortar and is ground 10h, obtain oxide powder, by oxide powder 4h is calcined at 1200 DEG C, the powder after calcining is ground again produces Mg after 8h0.7Ca0.3Al2O4Powder；
b、LaCrO3The preparation of powder：20.3920g is weighed respectively analyzes pure La2O3Pure Cr is analyzed with 9.6080g2O3Carry out Mixing, is placed in agate mortar and grinds 6h, obtain oxide powder, by oxide powder in 1300 DEG C of calcining 2h of temperature, calcining Powder afterwards is ground again produces LaCrO after 8h3Powder；
C, double-deck NTC thermistor preparation：The 0.2gMg that step a is obtained is weighed respectively0.7Ca0.3Al2O4Powder, step b Obtained 0.5gLaCrO3Powder, first by LaCrO3Powder pours into Ф 10mm moulds, is poured into again after shaking up Mg0.7Ca0.3Al2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, by the block materials of shaping Isostatic cool pressing is carried out, then the pressurize 1min under pressure 400MPa carry out ordinary sinter, is sintered 1 hour at 1800 DEG C of temperature, Obtain A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 2.13 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor3Ω cm, at room temperature Resistivity is 7.81 × 107Aging 500h resistance fluctuating is 12.1%, A layers and rubbed with B layers at Ω cm, 800 DEG C of temperature You are at number ratio：A/B=0.7981.
Embodiment 7
a、MgAl2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3Pure MgO is analyzed with 5.6661g to carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 4h at 1300 DEG C, after calcining Powder grind MgAl is produced after 8h again2O4Powder；
b、La0.99Ca0.01CrO3The preparation of powder：20.1881g is weighed respectively analyzes pure La2O3, 9.6080g analysis it is pure Cr2O3Pure CaO is analyzed with 0.0709g to be mixed, and is placed in agate mortar and is ground 10h, obtain oxide powder, by oxide Powder calcines 2h at 1300 DEG C, and the powder after calcining is ground again produces La after 8h0.99Ca0.01CrO3Powder；
C, double-deck NTC thermistor preparation：The 0.1778gMgAl that step a is obtained is weighed respectively2O4Powder, step b is obtained The 0.2986gLa arrived0.99Ca0.01CrO3Powder, first by La0.99Ca0.01CrO3Powder pours into Ф 10mm moulds, after shaking up again Pour into MgAl2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, and the block materials of shaping are entered Then row isostatic cool pressing, the pressurize 1min under pressure 400MPa carries out vacuum-sintering, temperature is 1600 DEG C, vacuum for- Sintered 2 hours under 0.8bar, obtain A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 8.03 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor3Ω cm, at room temperature Resistivity is 4.22 × 106Aging 500h resistance fluctuating is 18.4%, A layers and rubbed with B layers at Ω cm, 800 DEG C of temperature You are at number ratio：A/B=1.002.
Embodiment 8
a、MgAl2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3Pure MgO is analyzed with 5.6661g to carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 4h at 1300 DEG C, after calcining Powder grind MgAl is produced after 8h again2O4Powder；
b、La0.87Ca0.13CrO3The preparation of powder：17.7410g is weighed respectively analyzes pure La2O3, 9.6080g analysis it is pure Cr2O3Pure CaO is analyzed with 1.0488g to be mixed, and is placed in agate mortar and is ground 10h, obtain oxide powder, by oxide Powder calcines 2h at 1300 DEG C, and the powder after calcining is ground again produces La after 8h0.87Ca0.13CrO3Powder；
C, double-deck NTC thermistor preparation：The 0.5692gMgAl that step a is obtained is weighed respectively2O4Powder, step b is obtained The 1.4336gLa arrived0.87Ca0.13CrO3Powder, first by La0.87Ca0.13CrO3Powder pours into supporting graphite jig, after shaking up again Pour into MgAl2O4Powder, then carries out hot pressed sintering, and temperature is 1200 DEG C, pressure is to sinter 6 hours under 1ton, obtains A layers and B Layer double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 5.98 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor4Ω cm, at room temperature Resistivity is 8.12 × 105Aging 500h resistance fluctuating is 6.53%, A layers and rubbed with B layers at Ω cm, 800 DEG C of temperature You are at number ratio：A/B=0.667.
Embodiment 9
a、MgAl2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3Pure MgO is analyzed with 5.6661g to carry out Mixing, is placed in agate mortar and grinds 10h, obtain oxide powder, oxide powder is calcined into 4h at 1300 DEG C, after calcining Powder grind MgAl is produced after 8h again2O4Powder；
b、La0.62Ca0.38CrO3The preparation of powder：12.6430g is weighed respectively analyzes pure La2O3, 9.6080g analysis it is pure Cr2O3Pure CaO is analyzed with 4.3020g to be mixed, and is placed in agate mortar and is ground 10h, obtain oxide powder, by oxide Powder calcines 2h at 1300 DEG C, and the powder after calcining is ground again produces La after 8h0.62Ca0.38CrO3Powder；
C, double-deck NTC thermistor preparation：The 0.2134gMgAl that step a is obtained is weighed respectively2O4Powder, step b is obtained The 0.2389gLa arrived0.62Ca0.38CrO3Powder, first by La0.62Ca0.38CrO3Powder pours into Ф 10mm moulds, is poured into again after shaking up MgAl2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, the block materials of shaping is carried out cold Isostatic pressed, the pressurize 1min under pressure 400MPa, then carries out ordinary sinter, sinters 4.5 hours, obtains at 1600 DEG C of temperature A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 3.31 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor4Ω cm, at room temperature Resistivity is 4.81 × 106Aging 500h resistance fluctuating is 11.2%, A layers and rubbed with B layers at Ω cm, 800 DEG C of temperature You are at number ratio：A/B=1.314.
Embodiment 10
a、Mg0.89Ca0.11Al2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3, 5.0428g analysis it is pure MgO and 0.9742g analyzes pure CaO and mixed, and is placed in agate mortar and grinds 10h, obtain oxide powder, by oxidate powder Body calcines 4h at 1300 DEG C, and the powder after calcining is ground again produces Mg after 8h0.89Ca0.11Al2O4Powder；
b、La0.62Ca0.38CrO3The preparation of powder：12.6430g is weighed respectively analyzes pure La2O3, 9.6080g analysis it is pure Cr2O3Pure CaO is analyzed with 4.3020g to be mixed, and is placed in agate mortar and is ground 10h, obtain oxide powder, by oxide Powder calcines 2h at 1300 DEG C, and the powder after calcining is ground again produces La after 8h0.62Ca0.38CrO3Powder；
C, double-deck NTC thermistor preparation：The 0.2134gMg that step a is obtained is weighed respectively0.89Ca0.11Al2O4Powder, The 0.2389gLa that step b is obtained0.62Ca0.38CrO3Powder, first by La0.62Ca0.38CrO3Powder pours into Ф 10mm moulds, shakes up Pour into Mg again afterwards0.89Ca0.11Al2O4Powder, with 60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 3min, will be molded Block materials carry out isostatic cool pressing, then the pressurize 1min under pressure 400MPa carries out ordinary sinter, at 1600 DEG C of temperature Sintering 4.5 hours, obtains A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 1.21 × 10 at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor3Ω cm, at room temperature Resistivity is 3.81 × 105Aging 500h resistance fluctuating is 8.81%, A layers and rubbed with B layers at Ω cm, 800 DEG C of temperature You are at number ratio：A/B=1.437.
Embodiment 11
a、Mg0.89Ca0.11Al2O4The preparation of powder：14.3339g is weighed respectively analyzes pure Al2O3, 5.0428g analysis it is pure MgO and 0.9742g analyzes pure CaO and mixed, and is placed in agate mortar and grinds 10h, obtain oxide powder, by oxidate powder Body calcines 4h at 1300 DEG C, and the powder after calcining is ground again produces Mg after 8h0.89Ca0.11Al2O4Powder；
b、La0.87Ca0.13CrO3The preparation of powder：17.7410g is weighed respectively analyzes pure La2O3, 9.6080g analysis it is pure Cr2O3Pure CaO is analyzed with 1.0488g to be mixed, and is placed in agate mortar and is ground 10h, obtain oxide powder, by oxide Powder calcines 2h at 1300 DEG C, and the powder after calcining is ground again produces La after 8h0.87Ca0.13CrO3Powder；
C, double-deck NTC thermistor preparation：The 0.8536gMg that step a is obtained is weighed respectively0.89Ca0.11Al2O4Powder, The 0.9556gLa that step b is obtained0.87Ca0.13CrO3Powder, first by La0.87Ca0.13CrO3Powder pours into supporting graphite jig, shakes Mg is poured into after even again0.89Ca0.11Al2O4Powder, then carries out hot pressed sintering, sinters 2 hours, obtains under 1300 DEG C of temperature, 1ton To A layers and B layers of double-layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum slurry electrode, and burning infiltration electrode, temperature Spend for 1200 DEG C, the time is 3h, produce double-deck negative tempperature coefficient thermistor.
Test：In room temperature to carrying out hindering warm test to it at 1000 DEG C, the aging that 500h is carried out at 800 DEG C of temperature is surveyed Resistivity is 2374 Ω cm at examination, 1000 DEG C of the temperature of resulting double-deck negative tempperature coefficient thermistor, at room temperature resistance Rate is 4.39 × 105Aging 500h resistance fluctuating is the molal quantity of 5.54%, A layers and B layers at Ω cm, 800 DEG C of temperature Than for：A/B=1.402.

Claims (2)

1. a kind of double-deck negative tempperature coefficient thermistor, it is characterised in that the resistance is by A layers of MgAl2O40.1-0.8g and B layers LaCrO3 0.3-1.6g constitutes double-decker, or A layers of Mg1−xCaxAl2O4, 0.01≤x≤ 0.5 and B layers of LaCrO3The double-deck knot of composition Structure, wherein A layer are 0.2-0.8536g, and B layers are 0.3-1.6g；Or A layers of MgAl2O4With B layers of La1-xCaxCrO3, 0.01≤x≤ 0.38 composition double-decker, wherein A layers is 0.1-0.8g, and B layers are 0.2389-1.4336g；Or A layers of Mg1−xCaxAl2O4, 0.01 ≤x≤ 0.5 and B layers of La1-xCaxCrO3, 0.01≤x≤ 0.38 composition double-decker, wherein A layers is 0.2-0.8536g, and B layers are 0.2389-1.4336g, the operating temperature range of the double-deck negative tempperature coefficient thermistor is from room temperature to 1000 DEG C, resistivity model Enclose for 342-5.5 × 108The ratio between cm, A layers of Ω and B layers molal quantity are：A / B=0.28-2.33.
2. a kind of preparation method of double-deck negative tempperature coefficient thermistor as claimed in claim 1, it is characterised in that by following Step is carried out：
a、MgAl2O4The preparation of powder：Pure Al will be analyzed respectively2O3Mixed with pure MgO is analyzed, be placed in agate mortar and grind 6h-10h is ground, oxide powder is obtained, oxide powder 1.5-4h is calcined at 1000-1300 DEG C of temperature, the powder after calcining Body grinds MgAl is produced after 8h again2O4Powder；
b、LaCrO3The preparation of powder：Pure La will be analyzed respectively2O3With the pure Cr of analysis2O3Mixed, be placed in agate mortar and grind 6-10h is ground, oxide powder is obtained, oxide powder 1.5-4h is calcined at 1000-1300 DEG C of temperature, the powder after calcining Grind again and LaCrO is produced after 8h3Powder；
C, bilayer NTC thermistors preparation：The MgAl that step a is obtained is weighed respectively2O4 0.1-0.8g powders, step b is obtained The LaCrO arrived30.3-1.6g powders, first by LaCrO3Powder pours into shaping Ф 10mm moulds, pours into MgAl after shaking up again2O4Powder Body, with 30-60Kg/cm2Pressure carry out compound stalk forming, the dwell time is 1-3min, the block materials of shaping is carried out cold etc. Static pressure, the pressurize 1min in the case where pressure is 180-400MPa, then in 1500-1800 DEG C of ordinary sinter temperature, vacuum-sintering temperature It is sintered at 1300-1600 DEG C or 1200-1500 DEG C of hot pressed sintering temperature, sintering time is 1-6h, obtains A layers and B layer pairs Layer ceramic block；
D, the A layers that step c is obtained and B layers of double-layer ceramic block tow sides coating platinum starch electrodes, and burning infiltration electrode, and temperature is 1200 DEG C, the time is 1.5-3h, produces double-deck negative tempperature coefficient thermistor.
CN201710379104.1A 2017-05-25 2017-05-25 A kind of double-deck negative tempperature coefficient thermistor and preparation method thereof Pending CN107056273A (en)

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CN110054493A (en) * 2019-03-26 2019-07-26 济南大学 A kind of Lanthanum Chromite based perovskite phase and Spinel NTC thermal sensitive ceramic material and preparation method
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CN108640671A (en) * 2018-05-17 2018-10-12 赵娟 The preparation method of NTC sensitive ceramic resistor materials
CN109256246B (en) * 2018-11-28 2020-07-28 中国科学院新疆理化技术研究所 Calcium-containing quaternary system negative temperature coefficient thermistor material and preparation method thereof
CN109256246A (en) * 2018-11-28 2019-01-22 中国科学院新疆理化技术研究所 A kind of calcic quaternary system negative temperature coefficient thermistor material and preparation method thereof
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CN112876232A (en) * 2021-01-26 2021-06-01 南京理工大学 High-temperature NTC thermal sensitive ceramic material and discharge plasma sintering method thereof
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CN114134457B (en) * 2021-12-07 2023-11-24 中国科学院新疆理化技术研究所 Preparation method of grating-like structure composite NTC thermosensitive film
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