CN109796203A - A kind of zno-based negative temperature coefficient heat-sensitive resistance material - Google Patents
A kind of zno-based negative temperature coefficient heat-sensitive resistance material Download PDFInfo
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- CN109796203A CN109796203A CN201910235582.4A CN201910235582A CN109796203A CN 109796203 A CN109796203 A CN 109796203A CN 201910235582 A CN201910235582 A CN 201910235582A CN 109796203 A CN109796203 A CN 109796203A
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Abstract
The present invention relates to one kind to meet the material that preparation has resistance negative temperature coefficient (NTC) thermistor.NTC thermistor material of the invention is formed by main component of zinc oxide, by changing the room temperature resistivity and material constant B value for achieving the purpose that adjusting thermistor element at the content for being grouped as middle each element, the adjusting of wide scope room temperature resistance value and material constant B value is realized.The NTC thermistor material that the present invention relates to has the characteristics that raw material sources are wide, cost of material is low, room temperature resistivity value and material constant are regulatable, is suitble to prepare sensitive ceramic resistor element, thick-film thermistor element, thin-film thermistor element.NTC thermistor of the invention is suitable for temperature measurement, temperature control, inhibits the application fields such as surge, line build-out and infrared acquisition.
Description
Technical field
The present invention relates to a kind of materials for preparing the thermistor element with resistance negative temperature coefficient (NTC) effect, fit
Wave for temperature measurement, temperature control, line build-out, infrared acquisition, flow velocity detector and electronic component and circuit
Gush protection application field.
Background technique
Thermistor (temperature) sensor be varied with temperature using thermistor as key element, using the resistivity of thermistor and
The excellent characteristics of variation and manufactured device.The feature varied with temperature by resistivity, thermistor element mainly include positive temperature
Spend coefficient (PTC) thermistor element and negative temperature coefficient (NTC) thermistor element, the resistivity of PTC thermistor element
It increases and increases with temperature, the resistivity of NTC thermistor element increases with temperature and reduced.NTC thermistor device is wide
The general correlation for being applied to thermometric, temperature control, temperature-compensating, the protection of circuit and electronic component and flow velocity, flow, radionetric survey
Instrument and application field are widely applied in fields such as daily life, national economy, military affairs and aerospaces.
By using temperature classifications, NTC thermistor element has low form, normal temperature type and three kinds of high temperature modification thermistor.Often
Warm type NTC thermistor element, currently spinelle made of the main oxide for using manganese, iron, cobalt, nickel, copper transition metal is brilliant
The NTC thermistor element of body structure.The NTC thermistor material of this spinel structure has obtained extensive research and has answered
With.Such as: the Mn-Ni-O ceramics system NTC thermo-sensitive material that Chinese invention patent CN102627446A is announced；Chinese invention patent
CN1332405C announce using manganese, nickel, magnesium, aluminium nitrate as raw material, using the NTC temperature-sensitive electricity of liquid-phase coprecipitation synthesis
Hinder material；The Fe-Ni-Mn-Cr-O system NTC thermal sensitive ceramic material that Chinese invention patent CN101585707 is announced；American invention is special
Manganese-nickel-cobalt-iron-copper system NTC thermistor material of sharp 6861622 publications description.These NTC thermistor materials
Denominator is the oxide containing at least two transition metal elements, and using spinel type crystal structure as principal crystalline phase.
In using multicomponent NTC thermistor material made of transition metal manganese, iron, cobalt, nickel, Cu oxide, due to
The volatilization temperature of these transition metal oxides is lower, and this kind of NTC thermistor element is be easy to cause in preparation sintering process
The volatilization of composition of raw material, so that the repeatability between the ultimate constituent of product, homogeneity of product and different production batch is difficult to
Control.Under normal circumstances, AB2O4The room temperature resistivity of the NTC thermistor of type spinel crystal structure relies primarily on lattice B
Ionic valence condition and concentration the ratio ([Mn in such as manganate spinel resistance material4+]/[Mn3+Mn4+]), concentration ratio is higher, resistance
Rate is smaller.Therefore, the room temperature resistivity of this kind of material is affected by techniques such as sintering temperature, sintering atmosphere, cooling velocities,
Lower homogeneity of product is easily led to, and resistivity value is not easy to.Meanwhile it is current widely applied with spinel structure
Transition metal oxide NTC thermistor element, be easy to produce cationic slowly redistribution in use and cause
Structural relaxation.This relaxation phenomena will cause the unstable of NTC ceramic material electric property, easily lead to the old of thermistor element
Change, influences the service performances such as the temperature measurement accuracy of thermistor (temperature) sensor.
In order to develop new oxide base NTC thermistor material, scientific worker has also carried out some new material systems
Exploration and research.Six side BaTiO3Good NTC performance (Chinese invention patent ZL 2009 is presented in system material
10043274.8；Chinese invention patent ZL 200910303525.1), rutile-type SnO2Ceramics have good NTC characteristic
(electronic component and material, 2009,6:56-59；Journal of Materials Science:Materials in
Electronics, 2015,26:6163-6169)；LaCoO3The NTC ceramic of based perovskite structure has been reported (Journal of
The European Ceramics Society, 2000,20:2367-2376).BaBiO3、BaSnO3、SrTiO3、YMnO3With
LaMnO3NTC thermistor (Journal of the American is successfully made by the means such as doping, compound in equal materials
Ceramics Society, 1997,80:2153-2156；Solid state Science, 2006,8:137-141).It grinds recently
Study carefully report, the CuO base ceramics of doping vario-property also have good NTC temperature-sensitive property (Journal of Materials
Science:Materials in Electronics, 2015,26:10151-10185；Chinese invention patent, number of patent application:
201510360036.5,201610298467.8)；NiO base NTC thermistor material, the Y of doping vario-property adulterate zinc-nickel oxide
System NTC thermistor material is also obtained (Chinese invention patent, number of patent application: 201610298726.7, in succession
201610298669.2,201610296987.5,201610306430.5)；Nickel zinc magnesium-based NTC thermistor material, Li-Fe mix
The nickel zinc oxide system of miscellaneous modification, the nickel zinc oxide system of Al-Li doping vario-property are also found to have room temperature resistance and material
Expect the regulatable NTC sensitive characteristic of constant (Chinese invention patent, number of patent application: 201711016767.3,
201710948170.6、201710505976.8)。
As the industries such as refrigerator, air-conditioning, microwave equipment, automobile, communication and aerospace are to the steady of NTC themistor
Qualitative requirement is higher and higher, and improving existing component system or exploitation novel components system just seems particularly significant.For the above shape
Condition, the present invention use zinc oxide for main component, carry out material modification by microelement doping and sinter additives, obtain
Thermistor material system with excellent NTC effect；In the system, the content and burning of change doped chemical can be passed through
The content of additive is tied to adjust the room temperature resistivity and material constant B value of thermistor element.
It is that main material prepares NTC thermistor material that the present invention, which selects zinc oxide, not no more than molar fraction by addition
Doped chemical greater than 2% and the sinter additives no more than 2% are to adjust the performance of material；NTC thermistor material composition
Simply, electric performance stablity, and electric property can be regulated and controled on a large scale；The selected prices of raw materials are cheap, and preparation flow is simple, temperature-sensitive
Resistance material preparation cost is low.
Summary of the invention
The object of the present invention is to provide one kind can manufacture the NTC thermistor material with resistance negative temperature coefficient effect
System.This thermistor material can be by changing the content of doped chemical and the content of sinter additives to adjust temperature-sensitive electricity
The room temperature resistivity of resistance element and the thermal constant of material.
The present invention form NTC thermistor material at being grouped as are as follows: Zn1-x-2yAlxCuyMoyO, wherein 0.001≤x≤
0.03,0 y≤0.01 <.
The crucial group that the present invention forms NTC material becomes Zn1-x-2yAlxCuyMoyO, in formula components containing zinc, aluminium, copper and
Molybdenum element, raw material can be the simple substance containing these elements, be also possible to oxide, inorganic salts or organic containing these elements
Salt compound.Wherein, semiconducting doped chemical aluminium is the room temperature resistivity in order to adjust resistive element, and copper molybdate is to adjust
The room temperature resistivity and material constant B value of thermistor element and the sintering character of ceramics.
The object phase composition of high-purity single-phase hexagonal crystal system can be obtained by preparation method described in the embodiment of the present invention, it is prepared
Performance stabilization, the high reliablity of NTC thermistor element.
The component prescription for focusing on thermistor material of the invention can according to need pairing in actual application
It is adjusted accordingly at method and production technology, flexibility is big.For example, the simple substance containing these elements, oxygen can be selected in raw material
The substances such as compound, inorganic salts or organic salt；It is heavy that wet chemistry method, coprecipitation, sol-gel method, gas phase can be used in synthetic method
Area method or the preparation method of other ceramic materials are realized.
The performance detection of NTC thermistor material of the invention is to be ground using coating silver electrode by the Central China University of Science and Technology
The room temperature resistance and resistance of the R-T resistance temperature test macro measurement resistive element of system are with the raised variation characteristic of temperature.It is practical
In production and application, other materials is can be selected such as in electrode: aluminium electrode, In-Ga alloy electrode, Ni-Cr alloy electrode or copper electricity
The instrument of other resistance and resistance-temperature characteristic test also can be selected in pole, performance test.
The characteristic and Heterosis of NTC thermistor material of the present invention exist: 1. material composition is simple, and raw material are rich
Richness, it is cheap, it is nontoxic and environmental-friendly；2. being suitble to the production of the NTC thermistors elements such as ceramics, film；3. by adjusting
The content of semiconducting doped chemical aluminium can adjust room temperature resistivity value, material constant and the temperature system of thermistor element on a large scale
Number；4. the material room temperature resistance of temperature-sensitive element can be adjusted to a wide range by the content for adjusting copper molybdate in preparation process
Rate and material constant and temperature coefficient.
The electrical property of NTC thermistor material of the present invention can realize following parameter request: room temperature resistivity 140k Ω cm
≤ρ25≤ 620k Ω cm, material constant 4200K≤B≤5300K.
The contents of the present invention are described further with the following Examples.Following embodiment only meets the technology of the present invention
Several examples of content do not illustrate that present invention is limited only to content described in following examples.Of the invention focuses on NTC temperature-sensitive
The component prescription of resistance material, the raw material, process and preparation with production stage can according to actual production conditions into
The corresponding adjustment of row, flexibility are big.
Detailed description of the invention
Fig. 1 is the spy that the resistivity log (ln ρ) of thermistor material in embodiment changes with inverse temperature (1000/T)
Linearity curve, the figure illustrate that typical NTC characteristic is presented in all embodiment materials.
Fig. 2 is room temperature resistivity logarithm (the ln ρ of thermistor material in embodiment25) and the data of NTC material constant it is bent
Line chart.NTC material constant calculates gained by the resistivity of 25 DEG C of -85 DEG C of temperature ranges of experiment measurement.The figure illustrates the present invention
NTC thermistor material system is able to achieve the adjusting of large-scale room temperature resistivity, and keeps higher NTC material constant B value.
Specific embodiment
Embodiment 1
The present embodiment presses chemical molecular formula Zn0.98828Al0.01Cu0.00086Mo0.00086O carries out ingredient, wherein x=0.01, y
=0.0008.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) initial feed is pressed into Zn0.98828Al0.01Cu0.00086Mo0.00086O is formulated ingredient, weighs ZnO with assay balance
161.152g、Al(NO3)3·9H2O 7.5027g、Cu(OH)2 7.0509g、H2MoO4 14.0584g。
(2) by the Cu (OH) in the upper weighed raw material of a processing step2Be dissolved in 100mL volume fraction be 30% it is dilute
In nitric acid solution, H2MoO4Dissolution of raw material is in 20mL ammonium hydroxide.Both solution are mixed, stirring stood 24 after 1 hour
Hour, by sediment with being dried in 80 DEG C of vacuum oven after deionized water filtration washing 2 times, by the CuMoO of drying4Powder
Last (CMO) is spare after 300 DEG C are calcined 2 hours and removed in conjunction with water.
(3) by raw material A l (NO weighed in processing step (1)3)3·9H2O and ZnO pours into poly- four equipped with zirconia ball
In vinyl fluoride ball grinder, it is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is dried in 100 DEG C of drying box
It is dry, it takes the powder of drying to be placed in crucible, is calcined 5 hours in 1000 DEG C of air atmospheres, obtain the ZnO powder of Al doping
(AZO)。
(4) it weighs CMO powder 0.4052g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(5) powder for obtaining a upper processing step, is binder with polyvinyl alcohol water solution well prepared in advance, is carried out
It is granulated, is then pressed into green body, blank diameter 15mm, thickness 2-3mm in the case where axial compressive force is 8MPa.
(6) green body made from a upper processing step be sintered in air environment, sintering schedule is 200 DEG C of heat preservations 0.5
Hour, 700 DEG C keep the temperature 0.5 hour, and 1100 DEG C keep the temperature 5 hours, and 1300 DEG C keep the temperature 1 hour, and heating rate of temperature fall is 5 DEG C/
Min obtains NTC ceramic piece with this.
(7) by potsherd made from a upper processing step, two disc surface layer of potsherd is ground off with sand paper, so that two discs are flat
It is whole smooth, it is coated with silver paste and makes electrode through 600 DEG C of solidifications, obtain NTC thermistor element.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 2
The present embodiment presses chemical molecular formula Zn0.98656Al0.01Cu0.00172Mo0.00172O carries out ingredient, wherein x=0.01, y
=0.00172.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 0.8103g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 3
The present embodiment presses chemical molecular formula Zn0.98484Al0.01Cu0.00258Mo0.00258O carries out ingredient, wherein x=0.01, y
=0.00258.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 1.2155g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 4
The present embodiment presses chemical molecular formula Zn0.98312Al0.01Cu0.00344Mo0.00344O carries out ingredient, wherein x=0.01, y
=0.00344.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 1.6207g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 5
The present embodiment presses chemical molecular formula Zn0.9814Al0.01Cu0.0043Mo0.0043O carries out ingredient, wherein x=0.01, y=
0.0043.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid H2MoO4。
Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 2.0258g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 6
The present embodiment presses chemical molecular formula Zn0.97968Al0.01Cu0.00516Mo0.00516O carries out ingredient, wherein x=0.01, y
=0.00516.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 2.4310g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 7
The present embodiment presses chemical molecular formula Zn0.97796Al0.01Cu0.00602Mo0.00602O carries out ingredient, wherein x=0.01, y
=0.00602.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 2.8362g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.
Prepared material property is as shown in table 1, Fig. 1 and Fig. 2.
Embodiment 8
The present embodiment presses chemical molecular formula Zn0.97624Al0.01Cu0.00688Mo0.00688O carries out ingredient, wherein x=0.01, y
=0.00688.Initial raw materials are selected from zinc oxide ZnO, aluminum nitrate Al (NO3)3·9H2O, Kocide SD Cu (OH)2, molybdic acid
H2MoO4.Material preparation is completed with test by the processing step of following experiment:
(1) preparation process is identical as processing step (1)-(3) in embodiment 1.
(2) it weighs CMO powder 3.2413g in processing step (1) and dress is added together with the AZO powder in processing step (3)
Have in the polytetrafluoroethylene (PTFE) ball grinder of zirconia ball, is added 50mL deionized water ball milling 2 hours.Slurry after ball milling is existed
It is dried in 100 DEG C of drying box.
(3) preparation process is identical as processing step (5)-(7) in embodiment 1.Prepared material property such as table
1, shown in Fig. 1 and Fig. 2.
The performance indicator of NTC thermistor element in 1 embodiment of table
| Serial number | Room temperature resistivity (k Ω cm) | Material constant (K) |
| Embodiment 1 | 142.19 | 4236 |
| Embodiment 2 | 249.23 | 4419 |
| Embodiment 3 | 541.44 | 4648 |
| Embodiment 4 | 589.76 | 4905 |
| Embodiment 5 | 618.70 | 5133 |
| Embodiment 6 | 597.57 | 5190 |
| Embodiment 7 | 329.48 | 5237 |
| Embodiment 8 | 286.98 | 5298 |
Claims (2)
1. a kind of negative temperature coefficient heat-sensitive resistance material, it is characterized in that the material at being grouped into Zn1-x-2yAlxCuyMoyO,
In 0.001≤x≤0.03,0 y≤0.01 <.
2. negative temperature coefficient heat-sensitive resistance material according to claim 1, it is characterised in that: prepare this negative temperature coefficient
The raw material of thermistor are containing zinc, aluminium, molybdenum, the simple substance of copper, oxide, hydroxide, inorganic acid salt, inorganic salts, have
Machine salt.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110304905A (en) * | 2019-06-15 | 2019-10-08 | 山东格仑特电动科技有限公司 | A kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110304905A (en) * | 2019-06-15 | 2019-10-08 | 山东格仑特电动科技有限公司 | A kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting |
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