CN108002746A - A kind of preparation method of NTC thermistor material - Google Patents

A kind of preparation method of NTC thermistor material Download PDF

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Publication number
CN108002746A
CN108002746A CN201711186123.9A CN201711186123A CN108002746A CN 108002746 A CN108002746 A CN 108002746A CN 201711186123 A CN201711186123 A CN 201711186123A CN 108002746 A CN108002746 A CN 108002746A
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temperature
activated carbon
deionized water
dispensing
silicon nanowires
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不公告发明人
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Suzhou Nell Mstar Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/04Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/045Polyalkenes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/006Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/04Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/08Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing halogen
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-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
    • H01C7/04Non-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
    • H01C7/049Non-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 organic or organo-metal substances
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

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  • Thermistors And Varistors (AREA)
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Abstract

The invention discloses a kind of preparation method of NTC thermistor material, the performance of NTC thermistor element prepared by products obtained therefrom of the present invention stablizes high, reliability height, the thermistor has activated carbon supported silicon nano material prepared by special process as conductive filler, while the electric conductivity of thermistor is strengthened, there is stronger interaction also between high molecular polymer, non-conducting filler, the service life of thermistor is improved.

Description

A kind of preparation method of NTC thermistor material
Technical field
The present invention relates to resistance material manufacturing field, and in particular to a kind of preparation method of NTC thermistor material.
Background technology
Thermal resistor is a kind of sensitivity member that is temperature sensitive, showing different resistance values at different temperature Part, is divided into positive temperature coefficient thermistor (PTC) and negative temperature coefficient thermistor (NTC) according to temperature coefficient difference.
Wherein negative temperature coefficient thermistor (NTC) is the semiconductor material that a kind of resistance value increases and reduces with temperature Material, has the effects such as thermometric, temperature control, temperature-compensating, suppression surge.In room temperature NTC themistor, mainly using transition metal Manganese, nickel, cobalt, iron, copper oxide made of spinel structure NTC thermistor element, they obtained it is extensive research with Using.
Using spinel structure NTC thermistor material made of the oxide of transition metal manganese, nickel, cobalt, iron, copper In, because the volatilization temperature of these transition metal oxides is relatively low, hold in the preparation sintering process of this kind of NTC thermistor element It is also easy to produce the volatilization of composition of raw material so that the weight between the ultimate constituent of product, the uniformity of product and production different batches Renaturation is difficult to control.
The content of the invention
The present invention provides a kind of preparation method of NTC thermistor material, NTC temperature-sensitives electricity prepared by products obtained therefrom of the present invention The performance of resistance element stablizes high, reliability height, and the thermistor has activated carbon supported silicon nanometer material prepared by special process Material is used as conductive filler, while the electric conductivity of thermistor is strengthened, also between high molecular polymer, non-conducting filler There is stronger interaction, the service life of thermistor is improved.
To achieve these goals, the present invention provides a kind of preparation method of NTC thermistor material, this method to include Following steps:
(1)Prepare Ni-based resistance material
By molecular formula Ni1-xZnxO1-yClyCarry out dispensing, wherein x=0.01-0.03, y=0.005-0.01, initial raw materials choosing From basic nickel carbonate, ammonium chloride and zinc acetate;
Initial feed is pressed into Ni1-xZnxO1-yClyDispensing, weighs basic nickel carbonate, ammonium chloride and zinc acetate;
The raw material weighed by dissolve respectively, and basic nickel carbonate is dissolved in dust technology, and ammonium hydroxide is then added dropwise and adjusts pH value to 8-9; Ammonium chloride and zinc acetate are dissolved in deionized water respectively;
By dissolved three kinds of solution mix, and be uniformly mixed using magnetic agitation heater, heat drying;
Powder made from previous step is calcined, temperature is 880-950 DEG C, when insulation 4-5 is small, obtains Ni-based resistance material Material;
(2)Prepare activated carbon supported silicon nano material conductive filler
Small porcelain boat equipped with nanometer silicon monoxide powder is placed horizontally among alumina tube, the pipe is then placed on high temperature pipe In formula stove, vacuumize in 20-50Pa, then keep the temperature 900-1000 DEG C of temperature and respectively 60-80min, be warming up to 1300- afterwards 1400 DEG C of insulation 4-6h;500-600 DEG C is cooled to the speed of 10-15 DEG C/min and keep the temperature 30-40min afterwards, while with 60sccm blasts air to furnace chamber, and cooled to room temperature, obtains silicon nanowires, spare;
Silane coupling agent is added to deionized water, and with vinegar acid for adjusting pH to 3.5,30-50min is stirred at room temperature, afterwards The silicon nanowires is added, in 85-95 DEG C of back flow reaction 15-20h, filters, wash, is dry, the silicon nanowires after being coupled Compound;
Silicon nanowires compound, active carbon nanoparticles after obtained coupling are added to deionized water, with ultrasonic wave 45 DEG C, 30-50min is mixed under conditions of 150W, at room temperature static aging 30-40h, in being cleaned with deionized water and being in efflux repeatedly Property, 120-150 DEG C of drying 15-20h is to constant weight, cooling, dry then when 350-400 DEG C of roasting 3-5 is small, is made activated carbon supported Silicon nanowires, ball mill grinding obtain activated carbon supported silicon nano material conductive filler;
(3)According to following parts by weight dispensing:
42-51 parts of high molecular polymer
Above-mentioned 2-3.5 parts of activated carbon supported silicon nano material conductive filler
Above-mentioned Ni-based resistance material 22-27 parts;
(4)It is uniformly mixed by above-mentioned dispensing;Then extruding pelletization, obtains pellet;The pellet carries out to hot pressing is compound to obtain To NTC thermistor material.
Preferably, the high molecular polymer is high density polyethylene (HDPE), polypropylene(PP), Kynoar, poly- inclined chloroethene At least one of alkene.
Embodiment
Embodiment one
By molecular formula Ni0.99Zn0.01O0.995Cl0.005Dispensing is carried out, initial raw materials are selected from basic nickel carbonate, ammonium chloride and acetic acid Zinc.
The raw material weighed by dissolve respectively, and basic nickel carbonate is dissolved in dust technology, then be added dropwise ammonium hydroxide adjust pH value to 8-9;Ammonium chloride and zinc acetate are dissolved in deionized water respectively;By dissolved three kinds of solution mix, and utilize magnetic force Agitating and heating device is uniformly mixed, heat drying;Powder made from previous step is calcined, temperature is 880 DEG C, insulation 4 it is small when, obtain Ni-based resistance material.
Small porcelain boat equipped with nanometer silicon monoxide powder is placed horizontally among alumina tube, the pipe is then placed on height In warm tube furnace, vacuumize in 20Pa, then keep the temperature 900 DEG C of temperature and respectively 60min, be warming up to 1300 DEG C of insulations afterwards 4h;500 DEG C are cooled to the speed of 10 DEG C/min afterwards and keep the temperature 30min, while air is blasted to furnace chamber with 60sccm, it is natural It is cooled to room temperature, obtains silicon nanowires, it is spare.
Silane coupling agent is added to deionized water, and with vinegar acid for adjusting pH to 3.5,30min is stirred at room temperature, afterwards The silicon nanowires is added, in 85 DEG C of back flow reaction 15-20h, filters, wash, is dry, the silicon nanowires after being coupled is compound Thing.
Silicon nanowires compound, active carbon nanoparticles after obtained coupling are added to deionized water, with ultrasonic wave 45 DEG C, mix 30min under conditions of 150W, static aging 30h, is cleaned with deionized water and is repeatedly in neutrality to efflux at room temperature, 120 DEG C of drying 15h are to constant weight, cooling, dry then when 350 DEG C of roastings 3 are small, and activated carbon supported silicon nanowires, ball mill grinding is made Obtain activated carbon supported silicon nano material conductive filler.
According to following parts by weight dispensing:
42 parts of high molecular polymer
Above-mentioned 2 parts of activated carbon supported silicon nano material conductive filler
Above-mentioned 22 parts of Ni-based resistance material.
Preferably, the high molecular polymer is high density polyethylene (HDPE).
It is uniformly mixed by above-mentioned dispensing;Then extruding pelletization, obtains pellet;The pellet carries out to hot pressing is compound to obtain To NTC thermistor material.
Embodiment two
By molecular formula Ni0.97Zn0.03O0.99Cl0.01Dispensing is carried out, initial raw materials are selected from basic nickel carbonate, ammonium chloride and acetic acid Zinc;Initial feed is pressed into Ni0.97Zn0.03O0.99Cl0.01Dispensing.
The raw material weighed by dissolve respectively, and basic nickel carbonate is dissolved in dust technology, then be added dropwise ammonium hydroxide adjust pH value to 8-9;Ammonium chloride and zinc acetate are dissolved in deionized water respectively;By dissolved three kinds of solution mix, and utilize magnetic force Agitating and heating device is uniformly mixed, heat drying;Powder made from previous step is calcined, temperature is 950 DEG C, insulation 5 it is small when, obtain Ni-based resistance material.
Small porcelain boat equipped with nanometer silicon monoxide powder is placed horizontally among alumina tube, the pipe is then placed on height In warm tube furnace, vacuumize in 50Pa, then keep the temperature 1000 DEG C of temperature and respectively 80min, be warming up to 1400 DEG C of insulations afterwards 6h;600 DEG C are cooled to the speed of 15 DEG C/min afterwards and keep the temperature 40min, while air is blasted to furnace chamber with 60sccm, it is natural It is cooled to room temperature, obtains silicon nanowires, it is spare.
Silane coupling agent is added to deionized water, and with vinegar acid for adjusting pH to 3.5,50min is stirred at room temperature, afterwards The silicon nanowires is added, in 95 DEG C of back flow reaction 20h, filters, wash, is dry, the silicon nanowires compound after being coupled.
Silicon nanowires compound, active carbon nanoparticles after obtained coupling are added to deionized water, with ultrasonic wave 45 DEG C, mix 30-50min under conditions of 150W, static aging 40h at room temperature, in being cleaned with deionized water and being in efflux repeatedly Property, 150 DEG C of drying 20h are to constant weight, cooling, dry then when 400 DEG C of roastings 5 are small, and activated carbon supported silicon nanowires, ball milling is made Crushing obtains activated carbon supported silicon nano material conductive filler.
According to following parts by weight dispensing:
51 parts of high molecular polymer
Above-mentioned 3.5 parts of activated carbon supported silicon nano material conductive filler
Above-mentioned 27 parts of Ni-based resistance material.
Preferably, the high molecular polymer is Vingon.
It is uniformly mixed by above-mentioned dispensing;Then extruding pelletization, obtains pellet;The pellet carries out to hot pressing is compound to obtain To NTC thermistor material.

Claims (2)

1. a kind of preparation method of NTC thermistor material, this method comprises the following steps:
(1)Prepare Ni-based resistance material
By molecular formula Ni1-xZnxO1-yClyCarry out dispensing, wherein x=0.01-0.03, y=0.005-0.01, initial raw materials choosing From basic nickel carbonate, ammonium chloride and zinc acetate;
Initial feed is pressed into Ni1-xZnxO1-yClyDispensing, weighs basic nickel carbonate, ammonium chloride and zinc acetate;
The raw material weighed by dissolve respectively, and basic nickel carbonate is dissolved in dust technology, and ammonium hydroxide is then added dropwise and adjusts pH value to 8-9; Ammonium chloride and zinc acetate are dissolved in deionized water respectively;
By dissolved three kinds of solution mix, and be uniformly mixed using magnetic agitation heater, heat drying;
Powder made from previous step is calcined, temperature is 880-950 DEG C, when insulation 4-5 is small, obtains Ni-based resistance material Material;
(2)Prepare activated carbon supported silicon nano material conductive filler
Small porcelain boat equipped with nanometer silicon monoxide powder is placed horizontally among alumina tube, the pipe is then placed on high temperature pipe In formula stove, vacuumize in 20-50Pa, then keep the temperature 900-1000 DEG C of temperature and respectively 60-80min, be warming up to 1300- afterwards 1400 DEG C of insulation 4-6h;500-600 DEG C is cooled to the speed of 10-15 DEG C/min and keep the temperature 30-40min afterwards, while with 60sccm blasts air to furnace chamber, and cooled to room temperature, obtains silicon nanowires, spare;
Silane coupling agent is added to deionized water, and with vinegar acid for adjusting pH to 3.5,30-50min is stirred at room temperature, afterwards The silicon nanowires is added, in 85-95 DEG C of back flow reaction 15-20h, filters, wash, is dry, the silicon nanowires after being coupled Compound;
Silicon nanowires compound, active carbon nanoparticles after obtained coupling are added to deionized water, with ultrasonic wave 45 DEG C, 30-50min is mixed under conditions of 150W, at room temperature static aging 30-40h, in being cleaned with deionized water and being in efflux repeatedly Property, 120-150 DEG C of drying 15-20h is to constant weight, cooling, dry then when 350-400 DEG C of roasting 3-5 is small, is made activated carbon supported Silicon nanowires, ball mill grinding obtain activated carbon supported silicon nano material conductive filler;
(3)According to following parts by weight dispensing:
42-51 parts of high molecular polymer
Above-mentioned 2-3.5 parts of activated carbon supported silicon nano material conductive filler
Above-mentioned Ni-based resistance material 22-27 parts;
(4)It is uniformly mixed by above-mentioned dispensing;Then extruding pelletization, obtains pellet;The pellet carries out to hot pressing is compound to obtain To NTC thermistor material.
2. preparation method as claimed in claim 1, it is characterised in that the high molecular polymer is high density polyethylene (HDPE), gathers Propylene(PP), at least one of Kynoar, Vingon.
CN201711186123.9A 2017-11-23 2017-11-23 A kind of preparation method of NTC thermistor material Pending CN108002746A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863160A (en) * 2018-07-06 2018-11-23 句容市博远电子有限公司 A kind of preparation method of the Ni-based thermistor material of NTC
CN108899144A (en) * 2018-07-06 2018-11-27 句容市博远电子有限公司 A kind of preparation method of Ni-based thermistor material
CN108962519A (en) * 2018-07-06 2018-12-07 句容市博远电子有限公司 A kind of preparation method of high temperature thermistor material
WO2021068888A1 (en) * 2019-10-09 2021-04-15 湖北中烟工业有限责任公司 Ni-based composite material heating body and preparation method therefor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863160A (en) * 2018-07-06 2018-11-23 句容市博远电子有限公司 A kind of preparation method of the Ni-based thermistor material of NTC
CN108899144A (en) * 2018-07-06 2018-11-27 句容市博远电子有限公司 A kind of preparation method of Ni-based thermistor material
CN108962519A (en) * 2018-07-06 2018-12-07 句容市博远电子有限公司 A kind of preparation method of high temperature thermistor material
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WO2021068888A1 (en) * 2019-10-09 2021-04-15 湖北中烟工业有限责任公司 Ni-based composite material heating body and preparation method therefor

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Application publication date: 20180508