CN110317469A - A kind of positive temperature coefficient thermoplasticity thermistor composite material and preparation method thereof - Google Patents
A kind of positive temperature coefficient thermoplasticity thermistor composite material and preparation method thereof Download PDFInfo
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- CN110317469A CN110317469A CN201910559068.6A CN201910559068A CN110317469A CN 110317469 A CN110317469 A CN 110317469A CN 201910559068 A CN201910559068 A CN 201910559068A CN 110317469 A CN110317469 A CN 110317469A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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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
- H01C7/02—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 positive temperature coefficient
- H01C7/027—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 positive temperature coefficient consisting of conducting or semi-conducting material dispersed in a non-conductive organic material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/068—Ultra high molecular weight polyethylene
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention discloses a kind of positive temperature coefficient thermoplasticity thermistor composite materials and preparation method thereof, by weight percentage, including following components: thermoplastic macromolecule material 60wt%-90wt%, ultra-high molecular weight polyethylene 5wt%-30wt%, conductive filler 1wt%-30wt%, coupling agent 0.1wt%-2wt%, antioxidant 0.05wt%-1.5wt%, UV absorbers 0.05wt%-1.5wt%, naphthenic oil 0.01wt%-1.0wt%；Thermistor composite material resistivity of the present invention is low, positive temperature coefficient (PTC) intensity is high, without negative temperature coefficient (NTC) effect.
Description
Technical field
The present invention relates to thermistor field, in particular to a kind of positive temperature coefficient thermoplasticity thermistor composite material and
Preparation method.
Background technique
Posive temperature coefficient thermistor is a kind of phenomenon that its resistance value steeply rises as the temperature rises.Positive temperature system
Number thermistor is mainly using the polymer composite with positive temperature coefficient, and performance is mainly by with positive temperature system
The self-characteristic of several polymer composites limits.Thermistor can be divided into posive temperature coefficient thermistor and negative temperature coefficient
Thermistor, the latter are not allow to occur in the application of overcurrent protection.
As matrix, the posive temperature coefficient thermistor filling conductive filler and making has been widely applied macromolecule resin
In circuit fields such as overcurrent protection, overheat protectors.It adds the positive temperature that conductive filler can be shown in hemicrystalline resin
Coefficient effect is spent, referred to as PTC (positive temperature coefficient) effect, i.e., at a normal temperature, material show low resistance value state, and with
Temperature increase, when being raised near macromolecule resin fusing point, unexpected transition state is presented in resistance.Under usual state, electric current is smaller
When, the heat that the heat and external environment that thermistor generates distribute reaches balance, and resistance does not change significantly.When having
It when high current circulates, for example breaks down, circuit can generate a large amount of heat and can not distribute in time, and temperature is caused quickly to increase
Add, when near the fusing point for reaching matrix resin, the resistance value of circuit increases suddenly, the electric current of circulation is reduced, to protect
Circuit, is not burned out.After electric current restores normal, temperature decline, resistance value restores normal again.PTC intensity refers to room temperature
The difference of the logarithm of the maximum resistance generated after resistance and jumping, PTC intensity is bigger, can more protect circuit, it can be seen that room temperature
The resistance value the low more PTC intensity can be made to increase.Therefore the conductive filler for needing conductive effect excellent is as filler.Generally exist
After PTC effect occurs, with continuing growing for temperature, resistance can be there is a phenomenon where declining, this is known as negative temperature coefficient effect
It answers, referred to as NTC (negative temperature coefficient) effect, the effect can make circuit burnout, and for good PTC element material, NTC effect is
Do not allow to occur.
Currently, the most commonly used is graphite, carbon black, carbon fiber, carbon nanotube, metal powder etc., room temperature resistances for conductive filler
Rate is still higher, causes PTC intensity insufficient, buries security risk in industrial production and daily life.Such as carbon black
Patent CN01109754.X, CN201210510975.X of filling；The patent CN02149593.9 of metallic filling,
CN03136754.2,CN201010190326.7,CN201210013768.3；Carbon black/metal mixed filling patent
CN200810142631.1；The patent CN201610648447.9 of conductive fiber filling；The patent of nanocarbon/metal mixing filling
CN200810142631.1；Particle/fiber mixing filling patent CN200910100323.7；Carbon nano-tube filled patent
CN201510318361.5；The patent of Sectional packings: CN99111213.X, US5378407, there is different degrees of room in them
The defects of warm resistivity is higher, and PTC intensity is insufficient, and applicable surface is narrow.Method in order to reduce resistivity, by increasing filer content
So that the processing of compound becomes difficult, comprehensive performance decline is serious, such as tensile strength, bending strength；Using metallic
Method can obtain higher PTC intensity, but density increases, higher cost.
In addition, the current solution of NTC effect is radiation cross-linking process or addition crosslinking agent heat cross-linking method, these methods effect
Rate is low, complex procedures, at high cost, such as patent CN200510033327.X, CN200710301867.0,
CN200910109968.7、CN201510318361.5、CN201510318425.1、CN201710315891.3。
Therefore there are the resistivity of positive temperature coefficient (PTC) conducing composite material height, PTC intensity are lower, negative for the prior art
Temperature coefficient (NTC) effect eliminates the problems such as complex process.
Summary of the invention
In view of the problems of the existing technology, have that resistivity is low, positive temperature system the purpose of the present invention is to provide one kind
Number (PTC) intensity height and the thermoplasticity thermistor composite material and preparation method thereof without negative temperature coefficient (NTC) effect.
The invention adopts the following technical scheme:
A kind of positive temperature coefficient thermoplasticity thermistor composite material, by weight percentage, including following components:
Optionally, a kind of positive temperature coefficient thermoplasticity thermistor composite material, by weight percentage, including with the following group
Point:
Further, the conductive filler is the carbon fiber powder that surface grows carbon nanotube.
Further, the molecular weight ranges of the ultra-high molecular weight polyethylene are 2,000,000-300 ten thousand, and density is 0.1-1g/
cm3, such as 0.94g/cm3, fusing point is 100-200 DEG C, such as 140 DEG C, and viscosity is greater than 108Pas, it is total from Daqing petrochemical
Factory.
Further, the preparation method of the carbon fiber powder of the surface growth carbon nanotube, comprising the following steps:
(1) unidirectional carbon fiber is subjected to high temperature and pre-processes 4-6h, be subsequently placed in nickel nitrate solution and impregnate 1-5h, preferably
4h, volatilize moisture, can carry out moisture evaporation in air, obtain unidirectional carbon fiber precast body；The pretreated temperature of high temperature is
1500-3000 DEG C, such as 2000 DEG C；The concentration of nickel nitrate solution is 0.01-0.5%, it is therefore preferable to 0.1%；
(2) unidirectional carbon fiber precast body is put into tube furnace, in N2300-600 DEG C, preferably 450 are heated in atmosphere
DEG C, 0.5-3h, preferably 1.5h are optionally kept the temperature, NO is removed3, then it is warming up to 400-800 DEG C, preferably 550 DEG C, it is passed through H2It is gone back
Original obtains catalyst n i particle；
(3) it is continuously heating to 650-1000 DEG C, preferably 750 DEG C, stops logical N2, while being passed through CO and H2Mixed gas, protect
Warm 120-170min, preferably 150min, obtain in-situ growing carbon nano tube；
(4) after completion of the reaction, CO and H is closed2, then logical N2It is cooled to room temperature, obtains the carbon fiber of surface growth carbon nanotube
Powder.
Further, the performance parameter of the carbon fiber powder of the surface growth carbon nanotube are as follows: length of carbon nanotube 10-
30 microns, 10-200 nanometers of diameter, resistivity 1.3x10-4-3.4x10-4ohm·cm。
Raw material producer and model:
Further, the unidirectional carbon fiber be selected from Jilin Tan Su limited liability company, trade mark T300, filament diameter 7um,
Density 1.76g/cm3, volume resistivity 1.8x10-3ohm·cm。
Further, the nickel nitrate is selected from Hubei Ju Sheng Science and Technology Ltd., content 98%, and molecular weight 290.81 melts
56.7 DEG C of point.
Further, the conductive filler dosage is 1wt%-30wt%, optional 1wt%-25wt%, 1wt%-
20wt%, 1wt%-15wt%, 1wt%-10wt% or 1wt%-5wt%.
Further, remover of the ultra-high molecular weight polyethylene as negative temperature coefficient effect.
Further, the thermoplastic macromolecule material is the high molecular material with high crystalline, is optionally included: poly-
One of ethylene, polypropylene, polyvinylidene fluoride, polyamide, polyphenylene sulfide, thermoplastic polyester are a variety of.
Further, the coupling agent is silane coupling agent, specifically, the coupling agent include: KH-550, KH560,
One of KH570 or a variety of.
Further, the antioxidant includes: one of antioxidant 1010, irgasfos 168, antioxidant 264 or a variety of.
Further, the UV absorbers include: UV-P, UV-326, UV-531, UV-327, UV-770, UV-
328, one of UV-329, BP-21 or a variety of.
Further, the boiling point of the naphthenic oil is greater than 300 degrees Celsius, and the naphthenic oil can make ultra-high molecular weight polyethylene
Preferably dispersion is selected from hundred million petrochemical industry Co., Ltd of Hengshui Supreme Being.
Further, thermistor composite material of the present invention grows the carbon fiber powder of carbon nanotube using surface
(the carbon fiber scanning electron microscope diagram piece that Fig. 1 is surface growth carbon nanotube) as conductive filler, carbon fiber is in composite wood
Rod type conducting matrix grain is provided in material, and (Fig. 2 is rod type conduction bone of the carbon fiber of surface growth carbon nanotube in composite material
Frame figure), the carbon nanotube of carbon fiber surface growth is close to each other or contacts, this substantially reduces the conductive path between carbon fiber,
A plurality of new conductive network (Fig. 3 is that the carbon fiber surface conductive network of surface growth carbon nanotube forms schematic diagram) is formd,
This makes under less conductive filler amount, and conductive effect is significant, and resistivity is low.As the temperature rises, the resistance of composite material
Rate slowly increases, but near the fusing point of crystalline polymer material, and resistance occurs to increase suddenly, in the process, originally mutually
The carbon nanotube for the carbon fiber surface growth for being close or contacting, near macromolecule fusing point, distance is pulled open by macromolecular chain, is led
By considerable damage, (Fig. 4 is the carbon fiber signal that conductive network destroys in temperature-rise period of surface growth carbon nanotube to electric network
Figure), so that resistance mutation formula be made to increase, positive temperature coefficient (NTC) effect occurs, is finally obtained biggish positive temperature system
Number intensity.The thermistor composite material is after melting, and because of the addition of the ultra-high molecular weight polyethylene, composite material is viscous
(range of viscosities of composite material is 2.96x10 to degree6Pa·s-8.43x106Pas it) greatly increases, conductive network will not weigh automatically
It is new to be formed, so that resistivity will not occur to reduce brought negative temperature coefficient (NTC) effect.
Further, thermistor composite material resistivity of the present invention is low, positive temperature coefficient (PTC) intensity is high,
Without negative temperature coefficient (NTC) effect.
Further, the positive temperature coefficient thermoplasticity thermistor composite material is made by following steps and (weighs quality
Referring to proportion):
(1) conductive filler (carbon fiber powder of surface growth carbon nanotube) and coupling agent are mixed at 50 DEG C to 100 DEG C
It closes uniformly, it is dry, obtain mixture A；The drying temperature be 50-100 DEG C, more specifically 60-80 DEG C, for example, 60 DEG C, 70 DEG C,
80℃；The drying time is 10-60min, more specifically 15-30min, such as 15min, 20min, 30min；
(2) thermoplastic macromolecule material and ultra-high molecular weight polyethylene are mixed with mixture A room temperature mechanical stirring, is obtained
Mixture B；
(3) by mixture B and antioxidant, UV absorbers, naphthenic oil room temperature after mixing in double screw extruder
Interior extrusion, it is cooling, it dries and is granulated, obtain thermoplasticity thermistor composite material；The cooling can be water-bath cooling, cooling
Temperature is 5 DEG C to 30 DEG C, more specifically 20 DEG C to 30 DEG C, such as 20 DEG C, 25 DEG C, 30 DEG C；Drying temperature is 50-200 DEG C, such as
90℃。
Compared with the prior art, the beneficial effects of the present invention are:
(1) present invention uses the carbon fiber powder of surface growth carbon nanotube as conductive filler, in carbon fiber guiding power grid
While network formation, the conductive network of carbon nanotube further enhances the electric conductivity of thermistor composite material, and realization is led
Electric filler is few, resistivity is low；
(2) thermistor composite material of the invention produces big resistance jumping, forms higher near fusion point
Positive temperature coefficient intensity；
(3) thermistor composite material of the invention has used ultra-high molecular weight polyethylene, composite material after melting,
Due to ultra-high molecular weight polyethylene bring high viscosity effect, conductive network will not be re-formed, i.e., negative temperature system do not occur
Number effect；
(4) thermistor composite material production method of the invention it is simple, it is at low cost, can be mass.
Detailed description of the invention
Fig. 1 is the carbon fiber scanning electron microscope diagram piece of surface growth carbon nanotube；
Fig. 2 is rod type conducting matrix grain figure of the carbon fiber of surface growth carbon nanotube in composite material；
Fig. 3 is that the carbon fiber surface conductive network of surface growth carbon nanotube forms schematic diagram；
Fig. 4 is the carbon fiber schematic diagram that conductive network destroys in temperature-rise period of surface growth carbon nanotube.
Specific embodiment
In order to preferably explain the present invention, it is described further now in conjunction with following specific embodiments, but the present invention is unlimited
In specific embodiment.
Embodiment 1
A kind of positive temperature coefficient thermoplasticity thermistor composite material, by weight percentage, including following components:
A kind of positive temperature coefficient thermoplasticity thermistor composite material is made by following steps:
(1) carbon fiber powder of surface growth carbon nanotube is uniformly mixed with KH-550, it is dry, obtain mixture A；Institute
Stating drying temperature is 50 DEG C, drying time 60min；
(2) thermoplastic macromolecule material and ultra-high molecular weight polyethylene are mixed with mixture A room temperature mechanical stirring, is obtained
Mixture B；
(3) mixture B and antioxidant 1010, UV-P, naphthenic oil room temperature are squeezed in double screw extruder after mixing
Out, cooling, drying is granulated, and obtains thermoplasticity thermistor composite material；The cooling temperature is 30 DEG C.
Embodiment 2
A kind of positive temperature coefficient thermoplasticity thermistor composite material, by weight percentage, including following components:
A kind of positive temperature coefficient thermoplasticity thermistor composite material is made by following steps:
(1) carbon fiber powder of surface growth carbon nanotube is uniformly mixed with KH560, it is dry, obtain mixture A；Institute
Stating drying temperature is 100 DEG C, drying time 10min；
(2) thermoplastic macromolecule material and ultra-high molecular weight polyethylene are mixed with mixture A room temperature mechanical stirring, is obtained
Mixture B；
(3) mixture B and irgasfos 168, UV-326, naphthenic oil room temperature are squeezed in double screw extruder after mixing
Out, cooling, drying is granulated, and obtains thermoplasticity thermistor composite material；The cooling temperature is 5 DEG C.
Embodiment 3
A kind of positive temperature coefficient thermoplasticity thermistor composite material, by weight percentage, including following components:
A kind of positive temperature coefficient thermoplasticity thermistor composite material is made by following steps:
(1) carbon fiber powder of surface growth carbon nanotube is uniformly mixed with KH570, it is dry, obtain mixture A；Institute
Stating drying temperature is 90 DEG C, drying time 50min；
(2) thermoplastic macromolecule material and ultra-high molecular weight polyethylene are mixed with mixture A room temperature mechanical stirring, is obtained
Mixture B；
(3) mixture B and antioxidant 264, UV-531, naphthenic oil room temperature are squeezed in double screw extruder after mixing
Out, cooling, drying is granulated, and obtains thermoplasticity thermistor composite material；The cooling temperature is 20 DEG C.
Embodiment 4
A kind of positive temperature coefficient thermoplasticity thermistor composite material, by weight percentage, including following components:
A kind of positive temperature coefficient thermoplasticity thermistor composite material is made by following steps:
(1) carbon fiber powder of surface growth carbon nanotube is uniformly mixed with KH560, it is dry, obtain mixture A；Institute
Stating drying temperature is 60 DEG C, drying time 40min；
(2) thermoplastic macromolecule material and ultra-high molecular weight polyethylene are mixed with mixture A room temperature mechanical stirring, is obtained
Mixture B；
(3) mixture B and UV-327, irgasfos 168, naphthenic oil room temperature are squeezed in double screw extruder after mixing
Out, cooling, drying is granulated, and obtains thermoplasticity thermistor composite material；The cooling temperature is 15 DEG C.
Above is only a specific embodiment of the present invention, it is not intended to limit the scope of the invention, all utilizations
The equivalent transformation that the present invention makees, is applied directly or indirectly in other relevant technical fields, similarly includes of the invention
Among scope of patent protection.
Claims (10)
1. a kind of positive temperature coefficient thermoplasticity thermistor composite material, which is characterized in that by weight percentage, including it is following
Component:
2. composite material according to claim 1, which is characterized in that the conductive filler is that surface grows carbon nanotube
Carbon fiber powder.
3. composite material according to claim 2, which is characterized in that the carbon fiber powder of the surface growth carbon nanotube
Preparation method, comprising the following steps:
(1) unidirectional carbon fiber is subjected to high temperature pretreatment, is subsequently placed in nickel nitrate solution and impregnates 1-5h, volatilize moisture, obtains
Unidirectional carbon fiber precast body；
(2) unidirectional carbon fiber precast body is put into N2It is heated to 300-600 DEG C in atmosphere, removes NO3, then it is warming up to 400-800
DEG C, it is passed through H2It is restored, obtains catalyst n i particle；
(3) it is continuously heating to 650-1000 DEG C, stops logical N2, while being passed through CO and H2Mixed gas, heat preservation；
(4) after completion of the reaction, CO and H is closed2, then logical N2It is cooled to room temperature, obtains the carbon fiber powder of surface growth carbon nanotube
End.
4. composite material according to claim 2, which is characterized in that the carbon fiber powder of the surface growth carbon nanotube
Length of carbon nanotube be 10-30 micron, diameter be 10-200 nanometers, resistivity 1.3x10-4-3.4x10-4ohm·cm。
5. composite material according to claim 1, which is characterized in that the ultra-high molecular weight polyethylene is as negative temperature system
The remover of number effect, the thermoplastic macromolecule material includes polyethylene, polypropylene, polyvinylidene fluoride, polyamide, polyphenyl
One of thioether, thermoplastic polyester are a variety of.
6. composite material according to claim 1, which is characterized in that the coupling agent is silane coupling agent, the idol
It includes: one of KH-550, KH560, KH570 or a variety of for joining agent.
7. composite material according to claim 1, which is characterized in that the antioxidant includes: antioxidant 1010, antioxidant
168, one of antioxidant 264 or a variety of.
8. composite material according to claim 1, which is characterized in that the UV absorbers include: UV-P, UV-
326, one of UV-531, UV-327, UV-770, UV-328, UV-329, BP-21 or a variety of.
9. composite material according to claim 1, which is characterized in that the boiling point of the naphthenic oil is greater than 300 degrees Celsius.
10. a kind of preparation method of composite material of any of claims 1-9, which is characterized in that including following step
It is rapid:
(1) conductive filler is uniformly mixed at 50 DEG C to 100 DEG C, and dry 10-60min with coupling agent, obtains mixture A；
(2) thermoplastic macromolecule material and ultra-high molecular weight polyethylene are mixed with mixture A room temperature mechanical stirring, is mixed
Object B；
(3) mixture B and antioxidant, UV absorbers, naphthenic oil room temperature are squeezed in double screw extruder after mixing
Out, cooling, drying is granulated, and obtains thermoplasticity thermistor composite material；The cooling temperature is 5 DEG C to 30 DEG C.
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