CN107200563A - Al Li optimization Ni Zn oxide negative temperature coefficient heat-sensitive resistance materials - Google Patents
Al Li optimization Ni Zn oxide negative temperature coefficient heat-sensitive resistance materials Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
- H01C7/042—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient mainly consisting of inorganic non-metallic substances
- H01C7/043—Oxides or oxidic compounds
- H01C7/044—Zinc or cadmium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
- C04B2235/3203—Lithium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
Abstract
Meet the present invention relates to one kind and prepare the thermistor material with resistance negative temperature coefficient (NTC).The NTC thermistor material of the present invention is constituted by main component of zinc-nickel oxide, lithium and aluminium are submember component, is suitable for preparing sensitive ceramic resistor element, thin-film thermistor element.Material of the present invention can adjust the material constant B values and room temperature resistance value of thermistor element by changing the content of the composition component lithium and aluminium, and room temperature resistivity ρ can be achieved25In 5 Ω cm‑1~10M Ω cm‑1The regulation of scope and material constant B in 2500~6500K scopes.The thermistor material of the present invention has that stability is good, uniformity is good, it is reproducible the characteristics of; with the electrical characteristics such as resistance value, material constant, temperature-coefficient of electrical resistance it is controllable the characteristics of; suitable for temperature survey, temperature control and line build-out, and the protection of circuit and electronic component and flow, flow velocity, the instrument of radionetric survey and application field.
Description
Technical field
The present invention relates to the NTC temperature-sensitives that one kind prepares the thermistor element with resistance negative temperature coefficient (NTC) effect
Resistance material.Suitable for temperature survey, temperature control, line build-out, radionetric survey, flow velocity detector, and electronics member
The surge protection application field of part and circuit.
Background technology
Thermistor (temperature) sensor be varied with temperature using thermistor as key element, using the resistivity of thermistor and
The excellent specific property of change and the device being made.The feature varied with temperature by resistivity, thermistor element mainly includes resistance
The subzero temperature that positive temperature coefficient (PTC) thermistor element and resistivity that rate is raised and increased with temperature are raised and reduced with temperature
Spend two kinds of coefficient (NTC) thermistor element.NTC thermistor device is widely used to thermometric, temperature control, temperature-compensating, with
And the protection of circuit and electronic component and flow velocity, flow, the pertinent instruments and application field of radionetric survey.
Classify by temperature in use, NTC thermistor element has three kinds of low form, normal temperature type and high temperature modification thermistor.
In normal temperature type NTC thermistor element, the current main AB being made of transition metal manganese, iron, cobalt, nickel, the oxide of copper2O4
Spinel structure NTC thermistor element.The NTC thermistor material of this spinel structure has obtained extensive research with answering
With.Such as, the Mn-Ni-O ceramics system NTC thermo-sensitive materials that Chinese invention patent CN102627446A is announced；Chinese invention patent
The NTC temperature-sensitives electricity synthesized using the nitrate of manganese, nickel, magnesium, aluminium as raw material, using liquid-phase coprecipitation that CN1332405C is announced
Hinder material；The Fe-Ni-Mn-Cr-O systems NTC thermal sensitive ceramic materials that Chinese invention patent CN101585707A is announced；American invention
Manganese-nickel-cobalt-iron-copper system NTC thermo-sensitive materials of the publication of patent 6861622 description.These NTC thermistor materials are total to
Same is characterized in the oxide containing at least two transition metal, and using spinel-type cubic crystal structure as principal crystalline phase.
In the multicomponent NTC thermistor material being made of transition metal manganese, iron, cobalt, nickel, Cu oxide, due to
The volatilization temperature of these transition metal oxides is relatively low, is easily caused in the preparation sintering process of this kind of NTC thermistor element
The volatilization of composition of raw material so that the repeatability between the ultimate constituent, homogeneity of product and the production different batches of product is difficult to
Control.Generally, AB2O4The room temperature resistivity of the NTC thermistor of spinel structure relies primarily on the ion of lattice B
Valence state and concentration ratio (such as [Mn4+]/[Mn3++Mn4+]), concentration is higher, and resistivity is smaller.Therefore, the room temperature resistance of this kind of material
Rate is influenceed larger by techniques such as sintering temperature, sintering atmosphere, cooling velocities, and it is larger to be easily caused relatively low homogeneity of product, and
Resistance value is not easy to regulation and control.In AB2O4In the NTC thermistor material of spinel structure, temperature coefficient with room temperature resistivity drop
It is low and reduce, it is difficult to ensure to realize in similar temperature coefficient why a wide range of controllable adjustment of resistivity.Meanwhile, it is current extensive
The transistion metal compound NTC thermistor element with spinel structure of application, easily produces four sides in use
Body and octahedra cationic slowly redistribute and cause structure Relaxation.This Relaxation Phenomena causes NTC ceramic material electricity
The unstable of performance is learned, the aging of thermistor element is easily caused, the usability such as the temperature measurement accuracy of thermistor (temperature) sensor are influenceed
Energy.
In recent years, in order to develop new oxide base NTC thermistor material, scientific worker has also carried out some green woods
The exploration and research of material system.Six side BaTiO3Good NTC performances (Chinese invention patent ZL 2009 is presented in system
10043274.8；Chinese invention patent ZL 2,009 1 0303525.1), rutile-type SnO2Ceramics have good NTC characteristics
(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(14):2367-2376)。BaBiO3、BaSnO3、SrTiO3、
YMnO3And LaMnO3NTC thermistor (Journal of the are successfully made by the means such as doping, compound Deng material
American Ceramics Society,1997,80(8):2153-2156；Solid State Science,2006,8(2):
137-141).Research is reported recently, and the CuO bases ceramics of doping vario-property also have good NTC temperature-sensitives property (Journal of
Materials Science:Materials in Electronics,2015,26(12):10151-10158；Chinese invention is special
Profit, number of patent application：201510360036.5、201610298467.8)；The NiO NTC thermistors material of doping vario-property with
And Y doping zinc-nickel oxide system (Chinese invention patent, number of patent application：201610298726.7、201610298669.2、
201610296987.5、201610306430.5)。
As the industries such as refrigerator, air-conditioning, microwave equipment, automobile, communication and Aero-Space are to the steady of NTC themistor
Qualitative requirement more and more higher, improves existing component system or exploitation novel components system just seems particularly significant.For above shape
Condition, the present invention is used using zinc-nickel composite oxides as main component, by the material of micro- doping vario-property, is had
The thermistor material system of excellent NTC effects；In the system, temperature-sensitive can be adjusted by changing the content of doped chemical
The room temperature resistivity of resistive element and the NTC material constant B values of material.
The content of the invention
The NTC thermistor material with resistance negative temperature coefficient effect can be manufactured it is an object of the invention to provide a kind of
System.This thermistor material can adjust the room temperature resistivity of thermistor element by changing the content of doped chemical
With the thermal constant of material.
The NTC thermistor material of the present invention into being grouped into：(Ni1-xZnx)1-y-zLiyAlzO, wherein x=0.0001
~0.4, y=0.0001~0.1, z=0~0.1.
The crucial composition of present invention composition NTC material is (Ni1-xZnx)1-y-zLiyAlzIn O, formula components containing zinc, nickel,
Lithium and aluminum metal element, its raw material can be the simple substance containing these elements or oxide containing these elements, inorganic
The compound such as salt or organic salt.Wherein, semiconducting element lithium and aluminium be in order to adjust the room temperature resistivity of thermistor element and
NTC material constant B values.
The preparation method as described in the embodiment of the present invention can obtain the thing phase composition of high-purity single phase cubic crystallographic system, prepared
The performance of NTC thermistor element is stable, reliability is high.
The component prescription for focusing on thermistor material of the present invention, can pairing as needed in actual application
Adjusted accordingly into method and production technology, flexibility is big.For example, raw material can select the simple substance containing these elements, oxygen
The compounds such as compound, inorganic salts or organic salt；Synthetic method can use solid state reaction, coprecipitation, sol-gel process, gas
Phase sedimentation or the preparation method of other ceramic materials are realized.
The performance detection of the NTC thermistor material of the present invention is to use coating silver paste for electrode, big by Central China science and technology
The room temperature resistance and resistance for learning the R-T resistance-temperature characteristics test system measurement resistive element developed are special with the elevated change of temperature
Property.In actual production and application, electrode can select other materials such as aluminium electrode, In-Ga alloy electrodes or nickel electrode material, property
The tester that also can select other resistance and resistance-temperature characteristic can be tested.
The characteristic and Heterosis of NTC thermistor material of the present invention exist：1. material composition is simple, and raw material are rich
It is rich, nontoxic, it is environment-friendly；2. it is adapted to the production of the NTC thermistor elements such as ceramics, film；3. adulterated by adjusting semiconducting
The content of element lithium and iron can adjust the room temperature resistance value, material constant and temperature coefficient of thermistor element on a large scale；4. lead to
Nickel, zinc, the content of aluminium in composition composition are overregulated, room temperature resistance value, the material that temperature-sensitive element can be adjusted to a wide range are normal
Number and temperature coefficient.
The electrical property of NTC thermistor material of the present invention can realize following parameter request：Room temperature resistivity ρ25=5 Ω
cm-1~10M Ω cm-1, material constant B=2500~6500K.
Present disclosure is further described with the following Examples.Following examples are to meet the technology of the present invention
Several examples of content, do not illustrate that present invention is limited only to the content described in following examples.The composition that focuses on of the present invention is matched somebody with somebody
Side, the raw material, process and step can be adjusted correspondingly according to actual production conditions, and flexibility is big.
Brief description of the drawings
Fig. 1 is the characteristic curve that varies with temperature of resistivity of thermistor material in embodiment, and the figure illustrates all realities
Apply a material and typical NTC characteristics are presented.
Fig. 2 is room temperature resistivity logarithm (the ln ρ of thermistor material in each embodiment25) and NTC material constant block diagram.
NTC material constant calculates gained by 25 DEG C of -85 DEG C of temperature ranges of experiment measurement.The figure illustrates NTC thermistor material of the present invention
Material system can realize the regulation of large-scale room temperature resistivity, and keep higher NTC material constant B values.
Embodiment
Embodiment 1
The present embodiment presses chemical molecular formula (Ni1-xZnx)1-y-zLiyAlzO carries out dispensing, wherein x=0.3, y=0.0005, z
=0.0.Initial raw materials are selected from zinc oxide ZnO, basic nickel carbonate NiCO3·2Ni(OH)2·4H2O.Prepared by material presses following reality
The processing step tested：
(1) initial feed is pressed into (Ni0.7Zn0.3)0.9995Li0.0005O is formulated dispensing, and ZnO is weighed with assay balance
2.4422g、NiCO3·2Ni(OH)2·4H2O 8.7775g、Li2CO3 0.0018g。
(2) raw material for weighing a upper processing step are dissolved separately in 15% dust technology.
(3) three kinds of solution for preparing a upper processing step are mixed, and mixed using the stirring of magnetic agitation heater
Close uniform, heat drying.
(4) Precursor Powder made from a upper processing step is carried out calcining in air ambient, heating rate is 5 DEG C/min,
Calcining heat is 1000 DEG C, is incubated 3 hours.
(5) a upper processing step is calcined to the powder of synthesis, is binding agent with previously prepared polyvinyl alcohol water solution, enters
Row granulation, is then pressed into base substrate；Base substrate is wafer type, and a diameter of 15 millimeters of disk, thickness is 2.5~3.0 millimeters.
(6) base substrate for obtaining a upper processing step sintered in air ambient, and sintering temperature is 1320 DEG C, insulation 2
Hour, heating rate is 5 DEG C per minute.Thus obtain NTC thermal sensitive ceramics pieces.
(7) by potsherd made from a upper processing step, it is 1.5~2.0 millimeters that two sides top layer to thickness is ground off with sand paper,
And two sides is polished, it is coated with silver paste and makes electrode through 600 DEG C of solidifications.
(8) NTC thermistor element made from a upper processing step is subjected to resistance-temperature characteristics measurement.
Prepared material room temperature resistivity is 68.55 Ω cm-1With material constant B values be 4401K, such as table 1, Fig. 1 and
Shown in Fig. 2.
Embodiment 2
The present embodiment presses chemical molecular formula (Ni1-xZnx)1-y-zLiyAlzO carries out dispensing, wherein x=0.3, y=0.01, z=
0.Initial raw materials are selected from zinc oxide ZnO, basic nickel carbonate NiCO3·2Ni(OH)2·4H2O, without lithium carbonate Li2CO3.Material system
The standby processing step for pressing following experiment：
(1) initial feed is pressed into (Ni0.7Zn0.3)0.99Li0.01O is formulated dispensing, weighs ZnO 2.4178g, NiCO3·2Ni
(OH)2·4H2O 8.6898g、Li2CO3 0.0369g。
(2) preparation process is identical with processing step (2)~(8) in embodiment 1.
Prepared material room temperature resistivity is 36.10 Ω cm-1With material constant B values be 3850K, such as table 1, Fig. 1 and
Shown in Fig. 2.
Embodiment 3
The present embodiment presses chemical molecular formula (Ni1-xZnx)1-y-zLiyAlzO carries out dispensing, wherein x=0.2, y=0.02, z=
0.Initial raw materials are selected from zinc oxide ZnO, basic nickel carbonate NiCO3·2Ni(OH)2·4H2O, without lithium carbonate Li2CO3.Material system
The standby processing step for pressing following experiment：
(1) initial feed is pressed into (Ni0.8Zn0.2)0.98Li0.02O is formulated dispensing, weighs ZnO 1.5956g, NiCO3·2Ni
(OH)2·4H2O 9.8308g、Li2CO30.0739g；
(2) preparation process is identical with processing step (2)~(8) in embodiment 1.
Prepared material room temperature resistivity is 8.12 Ω cm-1It is 3059K, such as table 1, Fig. 1 and figure with material constant B values
Shown in 2.
Embodiment 4
The present embodiment presses chemical molecular formula (Ni1-xZnx)1-y-zLiyAlzO carries out dispensing, wherein x=0.3, y=0.03, z=
0.005.Initial raw materials are selected from zinc oxide ZnO, basic nickel carbonate NiCO3·2Ni(OH)2·4H2O, without lithium carbonate Li2CO3, nitre
Sour aluminium Al (NO3)3·9H2O.Material prepares the processing step by following experiment：
(1) initial feed is pressed into (Zn0.3Ni0.7)0.965Li0.03Al0.005O be formulated dispensing, weigh ZnO 2.34568g,
NiCO3.2Ni(OH)2.4H2O 8.4703g、Li2CO3 0.1108g、Al(NO3)3.9H2O 0.1876g。
(2) preparation process is identical with processing step (2)~(8) in embodiment 1.
Prepared material room temperature resistivity is 15.55 Ω cm-1With material constant B values be 3870K, such as table 1, Fig. 1 and
Shown in Fig. 2.
Embodiment 5
The present embodiment presses chemical molecular formula (Ni1-xZnx)1-y-zLiyAlzO carries out dispensing, wherein x=0.3, y=0.03, z=
0.015.Initial raw materials are selected from zinc oxide ZnO, basic nickel carbonate NiCO3·2Ni(OH)2·4H2O, without lithium carbonate Li2CO3, nitre
Sour aluminium Al (NO3)3·9H2O.Material prepares the processing step by following experiment：
(1) initial feed is pressed into (Zn0.3Ni0.7)0.955Li0.03Al0.015O be formulated dispensing, weigh ZnO 2.3323g,
NiCO3·2Ni(OH)2·4H2O 8.3825g、Li2CO3 0.1108g、Al(NO3)3·9H2O 0.5627g。
(2) preparation process is identical with processing step (2)~(8) in embodiment 1.
Prepared material room temperature resistivity is 284.40 Ω cm-1With material constant B values be 5018K, such as table 1, Fig. 1 and
Shown in Fig. 2.
Embodiment 6
The present embodiment presses chemical molecular formula (Ni1-xZnx)1-y-zLiyAlzO carries out dispensing, wherein x=0.1, y=0.03, z=
0.03.Initial raw materials are selected from zinc oxide ZnO, basic nickel carbonate NiCO3·2Ni(OH)2·4H2O, without lithium carbonate Li2CO3, nitre
Sour aluminium Al (NO3)3·9H2O.Material prepares the processing step by following experiment：
(1) initial feed is pressed into (Zn0.1Ni0.9)0.95Li0.03Al0.02O be formulated dispensing, weigh ZnO 0.7734g,
NiCO3·2Ni(OH)2·4H2O 10.7211g、Li2CO3 0.1108g、Al(NO3)3·9H2O 1.1254g。
(2) preparation process is identical with processing step (2)~(8) in embodiment 1.
Prepared material room temperature resistivity is 41520 Ω cm-1With material constant B values be 5821K, such as table 1, Fig. 1 and
Shown in Fig. 2.
The performance indications of the embodiment thermistor element of table 1
Claims (5)
1. a kind of negative temperature coefficient heat-sensitive resistance material, it is characterized in that the material into being grouped into (Ni1-xZnx)1-y- zLiyAlzO。
2. it is according to claim 1 into being grouped into (Ni1-xZnx)1-y-wLiyAlzO oxide negative temperature coefficient thermistor power
Material is hindered, it is characterized in that Zn content is in (Ni1-xZnx)1-y-wLiyAlzO compositions composition in for x span by 0.0001 to
0.4。
3. according to claim 1 and claim 2 into being grouped into (Ni1-xZnx)1-y-wLiyAlwO oxide subzero temperature
Coefficient heat-sensitive resistance material is spent, it is characterized in that adulterating elemental lithium to realize the room temperature resistivity and material constant of thermistor material
Regulation, lithium doping content is in (Ni1-xZnx)1-y-zLiyAlzO compositions composition in for y span by 0.0001 to 0.1.
4. the negative temperature coefficient heat-sensitive resistance material according to claim 1, claim 2 and claim 3, it is characterized in that
Aluminium element adulterate to realize the regulation of the room temperature resistivity and material constant of thermistor material, Fe2O3 doping content is in (Ni1- xZnx)1-y-zLiyAlzO compositions composition in for z span by 0 to 0.1.
5. the negative tempperature coefficient thermistor material according to claim 1, claim 2, claim 3 and claim 4
Material, the raw material for preparing this thermistor can be containing zinc, nickel, lithium, aluminium element simple substance, oxide, inorganic salts are organic
Salt.
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Cited By (2)
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| CN115536367A (en) * | 2022-09-29 | 2022-12-30 | 肇庆市金龙宝电子有限公司 | High-resistance low-B-value thermistor ceramic body, preparation method and thermistor |
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| CN108002746A (en) * | 2017-11-23 | 2018-05-08 | 苏州南尔材料科技有限公司 | A kind of preparation method of NTC thermistor material |
| CN115536367A (en) * | 2022-09-29 | 2022-12-30 | 肇庆市金龙宝电子有限公司 | High-resistance low-B-value thermistor ceramic body, preparation method and thermistor |
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Application publication date: 20170926 |