CN102311259A - Composite-phase negative temperature coefficient thermal-sensitive ceramic material - Google Patents
Composite-phase negative temperature coefficient thermal-sensitive ceramic material Download PDFInfo
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Abstract
The invention relates to a novel composite-phase negative temperature coefficient thermal-sensitive ceramic material, which is prepared from La2O3, TiO2, MnO2 and Ni2O3 by the following steps of: preparing perovskite-phase LaTiMnO and spinel-phase NiMnO powder by using an oxide solid-phase method; and sequentially carrying out wet grinding, drying, calcinating, biphase mixed grinding, pre-press molding, cold isostatic pressing and sintering processing on the powder. Through an electrical property test on the material, the electrical parameters of the material are as follows: B25/50= 1639-3997 K +/- 1%, and Rho 25 DEG C = 4-32951 ohm.cm +/- 2%, and the material provided by the invention has the advantages of strong parameter adjustability, good consistency, high stability and repeatability, therefore, the material is applicable for temperature measurement and control, line compensation and the like under various conditions.
Description
Technical field
The present invention relates to a kind of employing oxide compound solid phase method and prepare compound phase negative temperature coefficient thermosensitive ceramics material.
Background technology
NTC (NTC) thermistor; Because of advantages such as it have the temperature measurement accuracy height, interchangeability is good, safety is high, with low cost; Many-sides such as Long-distance Control at temperature survey, control, compensation and communication equipment have obtained using widely; Be considered to have the electronic devices and components of very big development potentiality, good application prospects is arranged.Common AB
2O
4The type spinel structure is the principal crystalline phase of NTC thermal sensitive ceramic material, and along with the development of science and technology and demand, the limitation of this type material also becomes increasingly conspicuous.Its B value is also high when the resistivity of material is higher; Vice versa, the less stable of the polynary system stupalith that the while spinel structure is formed, and the stupalith behind the sintering is in nonequilibrium situations; Cause the material electric property to change these 2 the wide application that restrict the NTC thermal sensing element.The key of head it off is to explore new NTC thermal sensitive ceramic material, through the spinel of high resistant mutually in compound a kind of low-resistance phase, preparation two-phase compound material.The research and development scope of material has been expanded in the appearance of compound NTC thermal sensitive ceramics greatly, utilizes and forms learning from other's strong points to offset one's weaknesses on the phase performance in the composite ceramic material, can design a series of New NTC thermo-sensitive materials with potential using value.Because multiplicity, the connection type of matrix material can be adjusted and change, reach the premium properties that single-material institute can not obtain, also can be owing to the product effect produces single-material and the technological brand-new characteristic that can't obtain.
The present invention changes (low B, high resistant) with the contrary gesture of needing badly at present of high precision, parameter and the strong components and parts of parameter adjustability are background; Demand according to contrary gesture is changed negative temperature coefficient thermosensitive ceramics material and safety is a foundation; Composition of raw materials, preparation method and sintering process have been carried out design and optimization; The present invention at first designs the prescription of material, makes the parameter of material that contrary gesture variation and in very large range adjustable take place; Again the calcined temperature of powder is regulated and control, and, made ginseng inverse of a number gesture variation tendency and adjustability strengthen, subdue other dephasigns except that spinel and two principal phases of uhligite the optimization of composite block material sintering temperature afterwards; Combine wet-milling in this external process of lapping, make that grinding is more abundant, grind size is more carefully more even, has also improved mill efficiency simultaneously, the compound phase negative temperature coefficient thermosensitive ceramics material that final obtained performance is stable, repeatability is high.
The object of the invention is, a kind of compound phase negative temperature coefficient thermosensitive ceramics material is provided, and this material is with La
2O
3, TiO
2, MnO
2And Ni
2O
3Be raw material, adopt the oxide compound solid phase method to prepare uhligite phase LaTiMnO and spinel NiMnO powder body material mutually, powder is processed through wet-milling, drying, calcining, bipolar mixed grinding, pre-molding, isostatic cool pressing, sintering.The electrical parameter of this material is: B
25/50=1639-3997K ± 1%, ρ
25 ℃=4-32951 Ω cm ± 2% has that the parameter adjustability is strong, high conformity, stability are high, advantage repeatably, is applicable to the measurement, control, line build-out of temperature under the multiple condition etc.
Compound phase negative temperature coefficient thermosensitive ceramics material of the present invention follows these steps to carry out:
A, with La
2O
3, TiO
2, MnO
2And Ni
2O
3Be raw material; By atomic percent among the uhligite phase LaTiMnO be La: Ti: Mn=45-55: 0-40: 5-55 with spinel phase NiMnO in atomic percent be Ni: Mn=30: 70 take by weighing respectively and place different agate jars; With the deionized water is dispersion medium, wet-milling 8h;
B, two kinds of slurries after the wet-milling among the step a are dry down 80 ℃ of temperature respectively, and grinding 1h obtains powder;
C, with two kinds of powders that obtain among the step b respectively at temperature 900-1100 ℃ of following pre-burning 2h, obtain uhligite phase LaTiMnO and the spinel powder of NiMnO mutually among the step a respectively;
D, with the uhligite phase LaTiMnO that obtains among the step c and spinel mutually the powder of NiMnO be LaTiMnO: NiMnO=0.5-2 by mass ratio: 1 mixed grinding 4h obtains mixed powder;
E, with the mixed powder that obtains in the steps d at 20Kg/cm
2Pressure under precompressed become the disk of Φ 20mm; Dwell time is 3min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 10min under the 350MPa at pressure; In 1200-1300 ℃ of high temperature sintering 2-4h, can obtain compound phase negative temperature coefficient thermosensitive ceramics material then.
Step a ball milling is for along counterclockwise hocketing, along 30min pitch time counterclockwise.
Each material mass ratio is in the step a control ball grinder: agate ball: material: deionized water=2.5: 1: 1.
Step c uhligite phase LaTiMnO powder granularity is 0.183-2.385 μ m, and spinel phase NiMnO powder granularity is 0.157-2.155 μ m.
The mixed powder granularity that steps d obtains is 0.044-1.857 μ m.
Compound phase negative temperature coefficient thermosensitive ceramics material electrical parameter is B
25/50=1639-3997K ± 1%, ρ
25 ℃=4-32951 Ω cm ± 2%.
Compound phase negative temperature coefficient thermosensitive ceramics material of the present invention; Fully controlling under the parameter and processing condition of solid state reaction; It is accurate to obtain stoichiometric ratio; The uniform negative temperature coefficient heat-sensitive powder of granularity and composition obtains the negative temperature coefficient thermosensitive ceramics material that the contrary gesture of parameter changes the strong compound phase of (low B, high resistant) and parameter adjustability again behind calcining, moulding, high temperature sintering, the characteristics of this material are:
(1) when powder preparing, the mode of abrasive material is to the granularity and the homogeneity important influence of powder.The present invention adopts the mode of wet-milling, is the Ball milling medium with the deionized water, ball milling under the atmosphere of liquid phase, because capillary effect, the ball milling that has improved powder is active; And in the process of ball milling, replace rule and carry out along ball milling counterclockwise, make ball milling more abundant, the powder granularity that obtains so evenly, good dispersivity; Particle size is little; The material that behind forming and sintering, obtains becomes porcelain property good, the thermal sensitive ceramic material high conformity, and stability is high.
(2) the present invention adopt uhligite phase LaTiMnO and spinel mutually the contrary gesture of NiMnO two mutually compound preparation parameters change (low B, high resistant) and the strong thermal sensitive ceramic material of parameter adjustability; Because multiplicity, the connection type of matrix material can be adjusted and change; Utilize and form learning from other's strong points to offset one's weaknesses on the phase performance in the composite ceramic material; Reach single phase material the premium properties that can not obtain, also can be owing to the product effect produces the brand-new characteristic that single phase material and technology can't obtain.
When (3) preparing composite ceramic material, directly mix La
2O
3, TiO
2, MnO
2, Ni
2O
3Possibly can't form strict the stoichiometric ratio LaTiMnO and spinel NiMnO mutually of uhligite phase accurately; So that can not reach two phase compound purposes; Produce monophasic LaTiMnO and NiMnO earlier so adopt; And then with two mutually compound, adjustment uhligite phase LaTiMnO and the different mass ratio of spinel phase NiMnO obtain that the contrary gesture of material parameter changes (low B, high resistant) and the parameter adjustability is strong, the compound negative temperature coefficient thermosensitive ceramics material of stability height, high conformity.This material is carried out electric performance test, its electrical parameter B
25/50=1639-3997K ± 1%, ρ
25 ℃=4-32951 Ω cm ± 2% has that the parameter adjustability is strong, high conformity, stability are high, advantage repeatably, is applicable to the measurement, control, line build-out of temperature under the multiple condition etc.
Embodiment
Embodiment 1
A, at first with La
2O
3, TiO
2, MnO
2, Ni
2O
3Be raw material; By atomic percent among the uhligite phase LaTiMnO is La: Ti: Mn=50: 30: 20 with spinel phase NiMnO in atomic percent be Ni: Mn=30: 70 take by weighing respectively and place different agate jars; Each material mass ratio is in the control ball grinder: agate ball: material: deionized water=2.5: 1: 1 is a dispersion medium with the deionized water, wet-milling 8h; Ball milling is for along counterclockwise hocketing, along 30min pitch time counterclockwise;
B, two kinds of slurries after the wet-milling among the step a are dry down 80 ℃ of temperature respectively, and grinding 1h obtains powder;
C, with two kinds of powders that obtain among the step b respectively at 900 ℃ of pre-burning 2h of temperature, obtain the uhligite phase LaTiMnO powder among the step a respectively, granularity is 0.183-2.074 μ m and the spinel powder of NiMnO mutually, granularity is 0.157-2.045 μ m;
D, with the uhligite phase LaTiMnO that obtains among the step c and spinel mutually the powder of NiMnO be LaTiMnO: NiMnO=0.5 by mass ratio: 1 mixed grinding 4h, the mixed powder that obtains, granularity is 0.044-1.574 μ m;
E, with the mixed powder that obtains in the steps d at 20Kg/cm
2Pressure under precompressed become the disk of Φ 20mm, the dwell time is 3min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 10min under the 350MPa at pressure, then in 1200 ℃ of high temperature sintering 2h, can obtain compound phase negative temperature coefficient thermosensitive ceramics material.
The compound phase negative temperature coefficient thermosensitive ceramics material that obtains is carried out electric performance test, and its electrical parameter is B
25/50=3997K ± 1%, ρ
25 ℃=32951 Ω cm ± 2%.This material has high B, high resistant, is applicable to measurement, control, the line build-out of high temperature service temperature such as auto exhaust, mover and drying oven, reactive tank, electric oven.
Embodiment 2
A, at first with La
2O
3, TiO
2, MnO
2And Ni
2O
3Be raw material; By atomic percent among the uhligite phase LaTiMnO is La: Ti: Mn=50: 35: 15 with spinel phase NiMnO in atomic percent be Ni: Mn=30: 70 take by weighing respectively and place different agate jars; Each material mass ratio is in the control ball grinder: agate ball: material: deionized water=2.5: 1: 1 is a dispersion medium with the deionized water, wet-milling 8h; Ball milling is for along counterclockwise hocketing, along 30min pitch time counterclockwise;
B, two kinds of slurries after the wet-milling among the step a are dry down 80 ℃ of temperature respectively, and grinding 1h obtains powder;
C, with two kinds of powders that obtain among the step b respectively at 1000 ℃ of pre-burning 2h of temperature, obtain the uhligite phase LaTiMnO powder among the step a respectively, granularity is 0.225-2.165 μ m and the spinel powder of NiMnO mutually, granularity is 0.346-2.038 μ m;
D, with the uhligite phase LaTiMnO that obtains among the step c and spinel mutually the powder of NiMnO be LaTiMnO: NiMnO=1 by mass ratio: 1 mixed grinding 4h, the mixed powder that obtains, granularity is 0.050-1.648 μ m;
E, with the mixed powder that obtains in the steps d at 20Kg/cm
2Pressure under precompressed become the disk of Φ 20mm, the dwell time is 3min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 10min under the 350MPa at pressure, then in 1250 ℃ of high temperature sintering 3h, can obtain compound phase negative temperature coefficient thermosensitive ceramics material.
The compound phase negative temperature coefficient thermosensitive ceramics material that obtains is carried out electric performance test, obtain electrical parameter B
25/50=2898K ± 1%, ρ
25 ℃=4633 Ω cm ± 2%, this material has low B, high resistant, is applicable to temperature survey, control, the line build-out of wide warm area.
Embodiment 3
A, at first with La
2O
3, TiO
2, MnO
2And Ni
2O
3Be raw material; By atomic percent among the uhligite phase LaTiMnO is La: Ti: Mn=50: 0: 50 with spinel phase NiMnO in atomic percent be Ni: Mn=30: 70 take by weighing respectively and place different agate jars; Each material mass ratio is in the control ball grinder: agate ball: material: deionized water=2.5: 1: 1 is a dispersion medium with the deionized water, wet-milling 8h; Ball milling is for along counterclockwise hocketing, along 30min pitch time counterclockwise;
B, two kinds of slurries after the wet-milling among the step a are dry down 80 ℃ of temperature respectively, and grinding 1h obtains powder;
C, with two kinds of powders that obtain among the step b respectively at 1100 ℃ of pre-burning 2h of temperature, obtain the uhligite phase LaTiMnO powder among the step a respectively, granularity is 0.245-2.385 μ m and the spinel powder of NiMnO mutually, granularity is 0.458-2.155 μ m;
D, with the uhligite phase LaTiMnO that obtains among the step c and spinel mutually the powder of NiMnO be LaTiMnO: NiMnO=2 by mass ratio: 1 mixed grinding 4h, the mixed powder granularity that obtains is 0.075-1.857 μ m;
E, with the mixed powder that obtains in the steps d at 20Kg/cm
2Pressure under precompressed become the disk of Φ 20mm, the dwell time is 3min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 10min under the 350MPa at pressure, then in 1300 ℃ of high temperature sintering 4h, can obtain compound phase negative temperature coefficient thermosensitive ceramics material.
The compound phase negative temperature coefficient thermosensitive ceramics material that obtains is carried out electric performance test, obtain electrical parameter B
25/50=1639K ± 1%, ρ
25 ℃=4 Ω cm ± 2%, this material has low B, low-resistance, is applicable to measurement, control, the line build-out of temperature under the low temperature.
Claims (5)
1. compound phase negative temperature coefficient thermosensitive ceramics material is characterized in that following these steps to carrying out:
A, with La
2O
3, TiO
2, MnO
2And Ni
2O
3Be raw material; By atomic percent among the uhligite phase LaTiMnO be La: Ti: Mn=45-55: 0-40: 5-55 with spinel phase NiMnO in atomic percent be Ni: Mn=30: 70 take by weighing respectively and place different agate jars; With the deionized water is dispersion medium, wet-milling 8h;
B, two kinds of slurries after the wet-milling among the step a are dry down 80 ℃ of temperature respectively, and grinding 1h obtains powder;
C, with two kinds of powders that obtain among the step b respectively at temperature 900-1100 ℃ of following pre-burning 2h, obtain uhligite phase LaTiMnO and the spinel powder of NiMnO mutually among the step a respectively;
D, with the uhligite phase LaTiMnO that obtains among the step c and spinel mutually the powder of NiMnO be LaTiMnO: NiMnO=0.5-2 by mass ratio: 1 mixed grinding 4h obtains mixed powder;
E, with the mixed powder that obtains in the steps d at 20Kg/cm
2Pressure under precompressed become the disk of Φ 20mm; Dwell time is 3min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 10min under the 350MPa at pressure; In 1200-1300 ℃ of high temperature sintering 2-4h, can obtain compound phase negative temperature coefficient thermosensitive ceramics material then.
2. method according to claim 1 is characterized in that step a ball milling for along counterclockwise hocketing, along 30min pitch time counterclockwise.
3. method according to claim 2 is characterized in that each material mass ratio is in the step a control ball grinder: agate ball: material: deionized water=2.5: 1: 1.
4. method according to claim 3 is characterized in that step c uhligite phase LaTiMnO powder granularity is 0.183-2.385 μ m, and spinel phase NiMnO powder granularity is 0.157-2.155 μ m.
5. method according to claim 4 is characterized in that the mixed powder granularity that steps d obtains is 0.044-1.857 μ m.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121837A (en) * | 2013-03-20 | 2013-05-29 | 中国科学院新疆理化技术研究所 | Aluminium-doped perovskite phase negative temperature coefficient thermal sensitive ceramic material |
| CN105753474A (en) * | 2016-03-31 | 2016-07-13 | 中国科学院新疆理化技术研究所 | Strontium-doped lanthanum chromite thermistor material |
| CN105777093A (en) * | 2016-01-30 | 2016-07-20 | 中国科学院新疆理化技术研究所 | High-B-value low-resistance thermometry composite thermistor material and preparing method thereof |
| CN106242533A (en) * | 2016-08-26 | 2016-12-21 | 中国振华集团云科电子有限公司 | A kind of high stable NTC thermal sensitive ceramic material and preparation method thereof |
| CN110423112A (en) * | 2019-08-08 | 2019-11-08 | 中国科学院新疆理化技术研究所 | A kind of warm area and the adjustable double-perovskite phase composite thermistor material of B value and preparation method thereof |
| CN113603484A (en) * | 2021-08-26 | 2021-11-05 | 陕西君普新航科技有限公司 | Preparation method of negative temperature coefficient thermistor manganese lanthanum titanate-lead niobate nickelate |
| CN114134457A (en) * | 2021-12-07 | 2022-03-04 | 中国科学院新疆理化技术研究所 | Preparation method of composite NTC thermosensitive film with grating-like structure |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103121837A (en) * | 2013-03-20 | 2013-05-29 | 中国科学院新疆理化技术研究所 | Aluminium-doped perovskite phase negative temperature coefficient thermal sensitive ceramic material |
| CN105777093A (en) * | 2016-01-30 | 2016-07-20 | 中国科学院新疆理化技术研究所 | High-B-value low-resistance thermometry composite thermistor material and preparing method thereof |
| CN105753474A (en) * | 2016-03-31 | 2016-07-13 | 中国科学院新疆理化技术研究所 | Strontium-doped lanthanum chromite thermistor material |
| CN106242533A (en) * | 2016-08-26 | 2016-12-21 | 中国振华集团云科电子有限公司 | A kind of high stable NTC thermal sensitive ceramic material and preparation method thereof |
| CN110423112A (en) * | 2019-08-08 | 2019-11-08 | 中国科学院新疆理化技术研究所 | A kind of warm area and the adjustable double-perovskite phase composite thermistor material of B value and preparation method thereof |
| CN110423112B (en) * | 2019-08-08 | 2022-01-18 | 中国科学院新疆理化技术研究所 | Double-perovskite phase composite thermistor material with adjustable temperature zone and B value and preparation method thereof |
| CN113603484A (en) * | 2021-08-26 | 2021-11-05 | 陕西君普新航科技有限公司 | Preparation method of negative temperature coefficient thermistor manganese lanthanum titanate-lead niobate nickelate |
| CN113603484B (en) * | 2021-08-26 | 2022-08-30 | 陕西君普新航科技有限公司 | Preparation method of negative temperature coefficient thermistor manganese lanthanum titanate-lead niobate nickelate |
| CN114134457A (en) * | 2021-12-07 | 2022-03-04 | 中国科学院新疆理化技术研究所 | Preparation method of composite NTC thermosensitive film with grating-like structure |
| 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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Application publication date: 20120111 |