CN110304905A - A kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting - Google Patents
A kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting Download PDFInfo
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- CN110304905A CN110304905A CN201910518265.3A CN201910518265A CN110304905A CN 110304905 A CN110304905 A CN 110304905A CN 201910518265 A CN201910518265 A CN 201910518265A CN 110304905 A CN110304905 A CN 110304905A
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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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention discloses the NTC thermistor materials and preparation method thereof that a kind of copper samarium is semiconducting, belong to electronic information function material and device arts, the present invention is formed using the oxide of manganese nickel cobalt as main component, copper samarium is semiconducting doped chemical, it is prepared using solid reaction process, by ball milling, drying, pre-burning, the processes such as secondary ball milling, dries, pulverizes and sieves and prepare.It can be used for making NTC thermistor, film NTC thermistor, lamination NTC thermistor.Thermistor material of the invention has stability good, and sintering temperature is low, has the characteristics that the electrical characteristics such as resistance value, material constant, temperature-coefficient of electrical resistance are controllable.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to be a kind of there is height to cause at porcelain
Close property has spinel structure, the stable NTC thermistor material and preparation method thereof of resistivity, B value.
Background technique
NTC (Negative Temperature Coefficient), which refers to have exponent relation with temperature rising resistance, to be subtracted
Small thermistor phenomenon and material with negative temperature coefficient.The material is to utilize two kinds of manganese, copper, silicon, cobalt, iron, nickel, zinc etc.
Or two or more metal oxides such as is sufficiently mixed, is formed, is sintered at the semiconductive ceramic made of techniques, can be made into has
The thermistor of negative temperature coefficient (NTC).Its resistivity and material constant are with material composition ratio, sintering atmosphere, sintering temperature
It is different with configuration state and change.The non-oxidized substance system with silicon carbide, stannic selenide, tantalum nitride etc. for representative is had also appeared now
NTC thermistor material.
The development experience of NTC themistor very long stage.1834, it is negative that scientist has found that silver sulfide has for the first time
The characteristic of temperature coefficient.Nineteen thirty, scientist have found that cuprous oxide-copper oxide also has the performance of negative temperature coefficient, and by it
It is successfully used in the temperature-compensation circuit of aeronautical instrument.Subsequently, as the continuous development of transistor technology, thermal resistor
Research make substantial progress.Nineteen sixty has developed NTC themistor.NTC themistor is widely used in thermometric, control
Temperature, temperature-compensating etc..
Power-type NTC thermistor is chiefly used in power supply and inhibits surge.Inhibit surge NTC themistor, is a kind of big
The disk thermistor of power is usually used in the electronic circuit for having capacitor, heater and motor starting.
High times of the surge current when circuit power is connected moment, can be generated in circuit than working normally, and NTC
The initial resistance value of thermal resistor is larger, can be with electric current excessive in suppression circuit, to protect its power circuit and load.When
When circuit enters normal operating conditions, due to causing resistance body temperature to rise by electric current, resistance value drops to thermal resistor
Very little will not influence the normal work of circuit.
There is also stability, sintering temperature, resistance value, material constant, temperature-coefficient of electrical resistances to be not easy for current resistance material
The characteristics of control.To overcome disadvantages described above, present applicant has proposed a kind of copper samarium be semiconducting NTC thermistor material and its
Preparation method.
Summary of the invention
The object of the present invention is to provide a kind of low-resistivity, sintering temperature are low, it can be achieved that the NTC temperature-sensitive stably produced
Resistance material and preparation method thereof.
The present invention solve the technical problem the technical solution adopted is as follows:
A kind of copper samarium is the NTC thermistor material of semiconducting, by main crystal phase material and doping phase material through ball milling mixing, pre-
It burns, adulterate ball milling, filters pressing drying is made.Wherein: the main crystal phase material is Mn3O4Mass percent is 50~70%, NiO matter
Amount percentage is 20~30%, Co2O3Mass percent is 5~15%；The doping phase material CuO, mass percent 0.1
~2%, Sm2O3Mass percent is 0.1~2%.
Molar ratio in the main crystal phase material between Mn, Ni, Co is 1-x-y:x:y, x be 0.2~0.4, y be 0.1~
0.3。
The doping phase material is oxide, and CuO mass percent is 0.1~2%, Sm2O3Mass percent be 0.1~
2%.
A kind of copper samarium is the preparation method of the NTC thermistor material of semiconducting, includes the following steps: main crystal phase material system
It is standby, Mn is weighed in molar ratio3O4、NiO、Co2O3, in material: ball: the ratio 1:2:0.8 of water carries out ball milling, after filters pressing drying,
Pre-burning under the conditions of 900/6H；Main crystal phase material after pre-burning, in the ratio addition doping phase material CuO of 1:0.1~2% after crushing
And Sm2O3, secondary ball milling is carried out by the condition of step 1, then filters pressing drying pulverizes and sieves.
The crucial group that the present invention forms NTC material becomes Mn1-x-yNixCoy, in formula components containing manganese, nickel, cobalt and copper,
Samarium element, raw material Mn, Ni, Co, Cu, the Sm for preparing this thermistor are the oxides containing these elements.Wherein, semiconducting
Elemental copper, samarium are the room temperature resistivities in order to adjust thermistor element, and elemental copper is the room for adjusting thermistor element
Warm resistivity and the material constant and temperature coefficient for embodying sensitive characteristic, while the burning of thermistor also can be enhanced in the introducing of copper
Knot property.
Primary focus of the invention is the component prescription of thermistor material, can according to need in actual application
Synthetic method and production technology are adjusted accordingly, flexibility is big.Solid reaction process, sol-gel can be used in synthetic method
Method, coprecipitation, the synthetic method of vapour deposition process or other ceramic materials are realized.The present invention, which selects, is suitable for industrial mass production
Solid reaction process, be conducive to production cost reduce.
The detection of thermistor material characteristic of the invention is using coating silver paste, and high temperature burning infiltration is electrode, measuring cell
Room temperature resistance and resistance-temperature characteristics.
The characteristic and Heterosis of NTC thermistor material of the present invention exist: 1. material composition is simple, raw material ratio
It is relatively abundant, it is environmental-friendly；2. sintering temperature is lower in preparation process, it is suitble to the NTC thermistors such as ceramic component, film, chip
The production of element；3. material is using rare earth element bismuth, cerium as semiconducting doped chemical；4. by adjusting semiconducting doped chemical
Bismuth, cerium content can adjust the room temperature resistance value of thermistor element on a large scale；5. by the content of titanium in modifying ingredients composition,
The material constant and temperature coefficient of temperature-sensitive element can be adjusted to a wide range.
The electrical property of NTC thermistor material of the present invention can realize following parameter request: room temperature resistivity ρ25=3.8 ± 4%
Ω·mm-1, B value=3380 ± 1%.
The contents of the present invention are further described 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 contents described in following examples.The ingredient that focuses on of the invention is matched
Side, the raw material, process and step can be adjusted correspondingly according to actual production conditions, and flexibility is big.
Specific embodiment
The present invention uses the MnCO of purity assay3、NiO、Co2O3Principal crystalline phase is prepared for raw material, is analytically pure with purity
The Sm of CuO, 4N2O3It is doped, specific embodiment is as follows:
Ingredient is weighed by table 1, mixture is put into stirring-type ball grinder, by pellet water quality ratio 1:2:0.8, ball milling 2~6 is small
When, revolving speed is 260 revs/min.Granularity is controlled in D50Within=1.2 μm, by the material filters pressing that ball milling is mixed, it is put in 100 DEG C of baking ovens
Drying, smashes it through 40 meshes, and 900 DEG C/6H condition pre-burning is pressed in chamber type electric resistance furnace, it is spare to smash it through 40 meshes；By table
Ratio addition doping phase material CuO, Sm in 12O3Secondary ball milling, filters pressing, drying are carried out, 80 meshes is smashed it through, PVA is added to make
Grain forms Φ 12.2mm × 2mm disk with handpress 20MPa.Green compact sample is placed in sintering furnace, 1200 DEG C/4H condition
Under, sinter thermal sensitive ceramics sample into, Tu Yinhou burning infiltration under the conditions of 850 DEG C/10M passes through thermostatic oil bath, precision resistance instrument, thousand
Ruler etc. is divided to be tested for the property sample.
The specific embodiment of the invention is shown in Table 2 at porcelain density, resistivity, B value result in detail.
The percentage of raw material in each example of table 1.
The properties of sample of each example of table 2.
Claims (5)
1. the NTC thermistor material and preparation method thereof that a kind of copper samarium is semiconducting, it is characterised in that by main crystal phase material and
Doping phase material is made through ball milling mixing, pre-burning, doping ball milling, filters pressing drying；
Wherein: the main crystal phase material is Mn3O4Mass percent is that 50~70%, NiO mass percent is 20~30%,
Co2O3Mass percent is 5~15%；The doping phase material CuO, mass percent are 0.1~2%, Sm2O3Quality percentage
Than being 0.1~2%.
2. a kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting according to claim 1, special
Sign is, the molar ratio in the main crystal phase material between Mn, Ni, Co be 1-x-y: x: y, x be 0.2~0.4, y be 0.1~
0.3。
3. a kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting according to claim 1, special
Sign is that the doping phase material is oxide, and CuO mass percent is 0.1~2%, Sm2O3Mass percent be 0.1~
2%.
4. a kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting according to claim 1, special
Sign is the preparation method of resistance material of the present invention, includes the following steps: prepared by main crystal phase material, weighs Mn in molar ratio3O4、
NiO、Co2O3, in material: ball: the ratio 1: 2: 0.8 of water carries out ball milling, after filters pressing drying, pre-burning under the conditions of 900/6H；After pre-burning
Main crystal phase material, after crushing in 1: 0.1~2% ratio addition doping phase material CuO and Sm2O3, by step 1 condition into
Row secondary ball milling, filters pressing drying, then pulverizes and sieves.
5. a kind of copper samarium is the NTC thermistor material and preparation method thereof of semiconducting according to claim 1, special
Sign is that the crucial group of resistance material of the present invention becomes Mn1-x-yNixCoy, manganese, nickel, cobalt and copper, samarium member are contained in formula components
Element, raw material Mn, Ni, Co, Cu, the Sm for preparing this thermistor are the oxides containing these elements；Wherein, semiconducting element
Copper, samarium are the room temperature resistivities in order to adjust thermistor element, and elemental copper is the room temperature electricity for adjusting thermistor element
Resistance rate and the material constant and temperature coefficient for embodying sensitive characteristic, while the sintering of thermistor also can be enhanced in the introducing of copper
Property.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394819A (en) * | 2022-02-10 | 2022-04-26 | 广东风华高新科技股份有限公司 | High-reliability chip NTC thermistor material and preparation method and application thereof |
| CN114678158A (en) * | 2022-05-30 | 2022-06-28 | 西安宏星电子浆料科技股份有限公司 | Resistor slurry, resistor and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104987059A (en) * | 2015-06-26 | 2015-10-21 | 中南大学 | Novel NTC thermal resistance material based on copper oxide |
| CN109796203A (en) * | 2019-03-27 | 2019-05-24 | 中南大学 | A kind of zno-based negative temperature coefficient heat-sensitive resistance material |
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2019
- 2019-06-15 CN CN201910518265.3A patent/CN110304905A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104987059A (en) * | 2015-06-26 | 2015-10-21 | 中南大学 | Novel NTC thermal resistance material based on copper oxide |
| CN109796203A (en) * | 2019-03-27 | 2019-05-24 | 中南大学 | A kind of zno-based negative temperature coefficient heat-sensitive resistance material |
Non-Patent Citations (4)
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| M.N. MURALIDHARAN ET AL.: "《Effect of Cu and Fe addition on electrical properties of Ni–Mn–Co–O NTC thermistor compositions》", 《CERAMICS INTERNATIONAL》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394819A (en) * | 2022-02-10 | 2022-04-26 | 广东风华高新科技股份有限公司 | High-reliability chip NTC thermistor material and preparation method and application thereof |
| CN114394819B (en) * | 2022-02-10 | 2022-11-15 | 广东风华高新科技股份有限公司 | High-reliability chip NTC thermistor material and preparation method and application thereof |
| CN114678158A (en) * | 2022-05-30 | 2022-06-28 | 西安宏星电子浆料科技股份有限公司 | Resistor slurry, resistor and preparation method |
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