CN102888126A - Thermal resistor composite material and preparation method thereof and thermal resistor containing thermal resistor composite material - Google Patents
Thermal resistor composite material and preparation method thereof and thermal resistor containing thermal resistor composite material Download PDFInfo
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- CN102888126A CN102888126A CN2011102035266A CN201110203526A CN102888126A CN 102888126 A CN102888126 A CN 102888126A CN 2011102035266 A CN2011102035266 A CN 2011102035266A CN 201110203526 A CN201110203526 A CN 201110203526A CN 102888126 A CN102888126 A CN 102888126A
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Abstract
The invention provides a thermal resistor composite material. The composite material comprises a high molecular polymer, a filling polymer and a conductive filler, wherein the filling polymer is a nonpolar polymer of which the degree of crystallinity is 90-100 percent, the melting point is 250-400 DEG C, and the average particle diameter is 1-5 mum. The invention further provides a preparation method of the composite material and a thermal resistor containing the composite material. The resistor prepared from the composite material has high voltage resistance and high current resistance.
Description
Technical field
[0001]The present invention relates to a kind of thermistor composite material and preparation method thereof and the thermistor that contains this matrix material, belong to technical field of polymer composite materials.
Background technology
Thermistor (PTC) matrix material with positive temperature coefficient effect, its resistivity is extremely responsive to temperature variation, and along with the rising of temperature, its volume specific resistance sharply rises, even is state of insulation surpassing under a certain switch temperature.This specific character is so that the components and parts of being made by this kind matrix material can play the effect of overcurrent, overheating protection in circuit.This overcurrent and overheating protection device is widely used in the fields such as Medical Instruments, computer, SPC telephone exchange, battery of mobile phone, auto parts machinery, household appliances, industrial instrument, launch vehicle, fire alarm.
The polymer matrix PTC components and parts that overcurrent protection is used require to have resistance low, have good stability, the intensity high.And the low-drag type conducing composite material that conducting metal or metallic compound are filled; this performance is more outstanding; its room temperature resistivity is lower than 0.1 Ω cm, and PTC intensity surpasses 8 orders of magnitude, and the corresponding overcurrent protective device that obtains has lower power consumption and sensitiveer protection feature in circuit.But research finds that the anti-current capability of proof voltage of such low-drag type thermistor composite material is relatively low, and in normally used thickness range, it pastes the electric current and voltage that can bear behind the electrode and is no more than 10V/5A/mm
2Application Areas and the scope of application of such thermal conducting matrix material overcurrent protective device have so greatly been limited.
For example Chinese patent CN1254932 discloses the core that a kind of thermistor is used, this core is mixed by high molecular polymer, conductive filler material, mineral filler and processing aid, its prescription following (weight percentage): high molecular polymer 34-60%, conductive filler material 34-60%, mineral filler 5-20%, processing aid 1-5%.
The anti-current capability of proof voltage of the used matrix material of above-mentioned core is relatively low, has limited Application Areas and the scope of application of such thermal conducting matrix material overcurrent protective device.
Summary of the invention
The technical problem to be solved in the present invention is the lower defective of the anti-current capability of matrix material proof voltage of thermistor of the prior art, thereby a kind of thermistor composite material and preparation method and the thermistor that contains this matrix material of high withstand voltage anti-fluidity energy are provided.
The invention provides a kind of thermistor composite material, this matrix material comprises high molecular polymer, filled polymer, conductive filler material; Described filled polymer is non-polar polymer, and its degree of crystallinity is 90-100%, and fusing point is 250-400 ℃, and median size is 1-5 μ m.
The present invention also provides this composite manufacture method, and the method comprises that the mixture with high molecular polymer, filled polymer and conductive filler material mixes, mixing, moulding, obtains matrix material.
The present invention also provides a kind of thermistor, this thermistor is made of the leading-out end of the sheet conducting polymer composite material of centre, the metal electrode paillon foil that is covered on the flaky composite material two sides, electrode and the insulation layer of outer end coating, and described conducting polymer composite material is matrix material of the present invention.
Filled polymer in the matrix material of the present invention can on the basis that does not affect original conducing composite material conductivity, electric performance stablity, improve the anti-current capability of its proof voltage and widen its Application Areas.The fusing point height can increase the heat-resisting breakdown performance of matrix material, and simultaneously the degree of crystallinity height has increased the intensity of matrix material, and median size to be 1-5 μ m can be easy to mix with other materials.
Embodiment
The invention provides a kind of thermistor composite material, this matrix material comprises high molecular polymer, filled polymer, conductive filler material; Described filled polymer is non-polar polymer, and its degree of crystallinity is 90-100%, and fusing point is 250-400 ℃, and median size is 1-5 μ m.
Filled polymer in the matrix material of the present invention, degree of crystallinity is 90-100%, has increased the intensity of matrix material, makes it reach various requirement; Fusing point is higher, has improved the resistance of matrix material and has worn performance; And median size is less, and itself and other material can better be mixed.
According to matrix material provided by the present invention, for the withstand voltage anti-fluidity that makes matrix material can be better, preferably, take the gross weight of described matrix material as benchmark, the content of described high molecular polymer is 10-40wt%, the content of described filled polymer is 5-10wt%, and the content of described conductive filler material is 50-75wt%.
According to matrix material provided by the present invention, can be better for the withstand voltage anti-fluidity that makes matrix material, preferably, described filled polymer is the fluorinated polymkeric substance.More preferably, described filled polymer is polytetrafluoroethylene polymer.
According to matrix material provided by the present invention, described high molecular polymer is various conductive polymers well known in the art, and preferably, described high molecular polymer is the multipolymer of a kind of polymkeric substance or two or more polymkeric substance.For example can be in polyethylene, polypropylene, polybutene, polyvinylidene difluoride (PVDF), the poly-trieline at least a.
According to matrix material provided by the present invention, in order further to improve the mechanical property of matrix material, preferably, the molecular weight of described high molecular polymer is more than 1,500,000.
According to matrix material provided by the present invention, described conductive filler material is various conductive filler material well known in the art, for example can be in carbon black, graphite, metal and the metal compound powders at least a.More preferably, described conductive filler material is at least a in nickel powder, bronze, iron powder, silver powder, titanium carbide and the titanium nitride.
According to matrix material provided by the present invention, in order further to improve the mechanical property of matrix material, preferably, described matrix material also contains auxiliary agent, and take the gross weight of described matrix material as benchmark, the content of described auxiliary agent is 0.5-5wt%.More preferably, described auxiliary agent is at least a in inorganic insulation filler, nucleator, oxidation inhibitor and the lubricant.Described inorganic insulation filler, nucleator, oxidation inhibitor, lubricant and expanding material all are technology well known in the art.For example, the inorganic insulation filler can be selected from silicate, carbonate, metal oxide; Nucleator can be selected from one or more in potassium stearate, phenylformic acid, Sodium Benzoate and the sorbyl alcohol; Oxidation inhibitor can be selected from hindered phenolic oxidation inhibitor or amine antioxidants; Lubricant can be selected from stearates, oleic acid salt, low-molecular-weight polyethylene wax and low-molecular-weight Poly Propylene Wax.
The present invention also provides a kind of composite manufacture method of the present invention, and the method comprises that the mixture with high molecular polymer, filled polymer and conductive filler material mixes, mixing, moulding, obtains matrix material.
According to preparation method provided by the present invention, preferably, before mixing, also comprise in mixture adding auxiliary agent.
According to preparation method provided by the present invention; because the particle diameter of general filled polymer is larger; in order to access the particle size range that needs; preferably; described method also comprises carries out pre-treatment with filled polymer, and described pretreated method is under vacuum or nitrogen protection condition, adopts gamma-ray irradiation to process; gamma-ray irradiation can interrupt the segment of this polymkeric substance, and what be convenient to pulverize further carries out.Then it is ground, at last screening obtains median size at the withstand voltage polymkeric substance of 1-5 μ m.
According to preparation method provided by the present invention, can be good at degraded in order to make filled polymer, preferably, the irradiation dose 50-100KGy of described gamma-ray irradiation.
According to preparation method provided by the present invention, described Ginding process is known in this field, for example can be in mechanical ball milling, comminution by gas stream and the ultrasonic grinding a kind of.
According to preparation method provided by the present invention, for better compatible with high molecular polymer, preferably, described conductive filler material is coupling agent modified conductive powder body.
The method of described coupling agent modified conductive filler material is known in this field, as, described coupling agent modified conductive powder body preparation process is as follows: a) conductive filler material is put in the vacuum drying oven and dries 180min under vacuum tightness 0.09MPa; B) with titanate coupling agent NDZ-201 isopropanol, add in the conductive filler material of a) middle oven dry, be 0.09MPa in vacuum tightness again after the stirring fully, in the vacuum drying oven that temperature is 90 ℃, oven dry 180min; It is 1.0% that coupling agent accounts for whole matrix material volume ratio.
The present invention also provides a kind of thermistor, this thermistor is made of the leading-out end of the sheet conducting polymer composite material of centre, the metal electrode paillon foil that is covered on the flaky composite material two sides, electrode and the insulation layer of outer end coating, and described conducting polymer composite material is matrix material of the present invention.
The preparation method of described thermistor is: two conducting base nickel plating Copper Foils are placed in the mould, and above-mentioned PTC material placed the nickel plating Copper Foil, on thermocompressor, 180 ℃ of lower preheatings 10 minutes, then hot-forming is three layers of composite core material, with the thermal treatment 16 hours in 80 ℃ vacuum chamber of gained core.Be main reaction in order to make the polymkeric substance body produce crosslinked, the system performance is more stable even be improved, and preferably, with gamma-rays these three layers of composite core materials is carried out radiation crosslinking, irradiation dose 150KGy.
With punch press these three layers of composite core materials are tailored into the small pieces that are of a size of 3 millimeters * 4 mm in sizes at last, and respectively at two conducting base welding conductive electrode nickel straps, then cover conductive electrode with adhesive tape, in epoxy resin solution, flooded 2 minutes at last, and lower dry 30 minutes at 100 ℃, form 25 microns Resins, epoxy rete on its surface, make posistor.
The below further describes in detail the present invention with embodiment.
Embodiment 1
Filled polymer is carried out pre-treatment: select polytetrafluoroethylene polymer (327 ℃ of fusing points), mean particle size is 100 μ m.Under vacuum condition, gamma-ray irradiation pre-treatment, irradiation dose 50KGy.Then, the mode by ultrasonic grinding grinds it, obtains median size at the polytetrafluoroethylene polymer powder of 3 μ m through screening again.
Coupling agent modified conductive powder body preparation process is as follows: a) the Ni powder is put in and dries 180min in the vacuum drying oven under vacuum tightness 0.09MPa; B) with titanate coupling agent NDZ-201 isopropanol, add in the conductive filler material of a) middle oven dry, be 0.09MPa in vacuum tightness again after the stirring fully, in the vacuum drying oven that temperature is 90 ℃, oven dry 180min; It is 1.0% that coupling agent accounts for whole matrix material volume ratio.
According to the proportioning of table 1, in high mixer, all raw materials at the lower abundant premix of room temperature (25 ℃), stirred 10 minutes under 800 rev/mins rotating speed first, and then stirring were obtained mixture in 3 minutes under 2000 rev/mins rotating speed.With mixture obtained above 200 ℃ of lower mixing 20min in Banbury mixer, then mixture obtained above is sent in the twin screw compounding forcing machine mixing evenly, obtain composite A 1.
Two conducting base nickel plating Copper Foils are placed in the mould, and above-mentioned PTC material placed the nickel plating Copper Foil, on thermocompressor, 180 ℃ of lower preheatings 10 minutes, then hot-forming is three layers of composite core material, with the thermal treatment 16 hours in 80 ℃ vacuum chamber of gained core, and with gamma-rays these three layers of composite core materials are carried out radiation crosslinking, irradiation dose 150KGy.
With punch press these three layers of composite core materials are tailored into the small pieces that are of a size of 3 millimeters * 4 mm in sizes at last, and respectively at two conducting base welding conductive electrode nickel straps, then cover conductive electrode with adhesive tape, in epoxy resin solution, flooded 2 minutes at last, and lower dry 30 minutes at 100 ℃, form 25 microns Resins, epoxy rete on its surface, make posistor B1.
Embodiment 2-5
Specific implementation method is with embodiment 1, and difference is: screening obtains the median size of polytetrafluoroethylene polymer powder at 1 μ m, 5 μ m, 4 μ m and 3 μ m.Wherein each material and its content such as table 1 obtain composite A 2-A5 and thermistor B2-B5.
Comparative Examples 1
Specific implementation method is with embodiment 1, and distinctive points is: the content of polyethylene (molecular weight 2,000,000) is 30%, and the content of nickel powder is 65%, lubricant 3%, and oxidation inhibitor 2% obtains matrix material DA1 and thermistor DB1.
Comparative Examples 2
Specific implementation method is with embodiment 1, and distinctive points is that described material and mass percent thereof are: high density polyethylene(HDPE) 47.7%, carbon black A17.9%, carbon black B23.9%, magnesium hydroxide 9.5%, oxidation inhibitor 0.2%, crosslinking accelerator 0.6% and coupling agent 0.2%.Obtain matrix material DA2 and thermistor DB2.
Table 1
Testing method
1, volume specific resistance
Adopt the room temperature internal resistance R of four-probe measurement thermistor B1-B5 and DB1, DB2
0, use battery Inner Resistance Tester in Virtual Instrument (BS-VR type, Guangzhou are held up the sky), precision 0.1m Ω.And calculate the volume specific resistance ρ of thermistor B1-B5 and DB1, DB2 according to following formula, the results are shown in Table 2.
ρ=?R
0*(S/L)
In the formula, S is the sample area; L is sample thickness.The test of S and L is used vernier callipers directly to measure and is got final product.
2, intensity
According to formula: PTC intensity=lg (R
Peak value/ R
0) calculate PTC intensity, the results are shown in Table 2.
In the formula: R
Peak valueBe the highest resistance of thermistor apparatus on the R-T curve; The R-T curved measurement is measured according to requiring among the standard JB/T 9474; R
0Be material resistance value at room temperature.
3, withstand voltage anti-flow valuve
According to formula: the withstand voltage of anti-stream=Imax/S calculates withstand voltage anti-flow valuve, the results are shown in Table 2.
In the formula: S is the sample area, uses vernier callipers directly to measure and gets final product;
The maximum withstand current value of Imax is the mode with stepping, namely at 0.1A in the striking current scope, every increases 0.1A keeps 10s, the maximum withstand current value Imax that the measurement thermistor can be under a certain voltage.
Table 2
As can be seen from Table 2, embodiment 1-5 is worth in the situation in low resistance with respect to Comparative Examples 1, and the withstand voltage anti-flow valuve of embodiment 1-5 is far above Comparative Examples 1.And with respect to Comparative Examples 2, the resistance value of embodiment 1-5 is far below Comparative Examples 2, and PTC intensity is higher than Comparative Examples 2, and its withstand voltage anti-flow valuve is also good than Comparative Examples 2.So the withstand voltage anti-flow valuve of the thermistor that matrix material of the present invention prepares is better than the withstand voltage anti-flow valuve of thermistor of the prior art.
Claims (16)
1. a thermistor composite material is characterized in that, this matrix material comprises high molecular polymer, filled polymer, conductive filler material; Described filled polymer is non-polar polymer, and its degree of crystallinity is 90-100%, and fusing point is 250-400 ℃, and median size is 1-5 μ m.
2. matrix material according to claim 1, it is characterized in that take the gross weight of described matrix material as benchmark, the content of described high molecular polymer is 10-40wt%, the content of described filled polymer is 5-10wt%, and the content of described conductive filler material is 50-75wt%.
3. matrix material according to claim 2 is characterized in that, described filled polymer is the fluorinated polymkeric substance.
4. matrix material according to claim 3 is characterized in that, described filled polymer is polytetrafluoroethylene polymer.
5. matrix material according to claim 1 is characterized in that, described high molecular polymer is at least a in polyethylene, polypropylene, polybutene, polyvinylidene difluoride (PVDF), the poly-trieline.
6. matrix material according to claim 1 is characterized in that, the molecular weight of described high molecular polymer is more than 1,500,000.
7. matrix material according to claim 1 is characterized in that, described conductive filler material is at least a in carbon black, graphite, metal and the metal compound powders.
8. matrix material according to claim 7 is characterized in that, described conductive filler material is at least a in nickel powder, bronze, iron powder, silver powder, titanium carbide and the titanium nitride.
9. matrix material according to claim 1 is characterized in that, described matrix material also contains auxiliary agent, and take the gross weight of described matrix material as benchmark, the content of described auxiliary agent is 0.5-5wt%.
10. matrix material according to claim 9 is characterized in that, described auxiliary agent is at least a in inorganic insulation filler, nucleator, oxidation inhibitor and the lubricant.
11. composite manufacture method claimed in claim 1 is characterized in that, with the mixture of high molecular polymer, filled polymer and conductive filler material mix, mixing, moulding, obtain matrix material.
12. preparation method according to claim 11 is characterized in that, also comprises in mixture adding auxiliary agent before mixing.
13. preparation method according to claim 12; it is characterized in that; described method also comprises carries out pre-treatment with filled polymer; described pretreated method is under vacuum or nitrogen protection condition; the employing gamma-ray irradiation is processed; then it is ground, at last screening obtains the withstand voltage polymkeric substance of median size below 5 μ m.
14. preparation method according to claim 13 is characterized in that, the irradiation dose 50-100KGy of described gamma-ray irradiation.
15. preparation method according to claim 13 is characterized in that, the described method that grinds is a kind of in mechanical ball milling, comminution by gas stream and the ultrasonic grinding.
16. thermistor, it is characterized in that, this thermistor is made of the leading-out end of the sheet conducting polymer composite material of centre, the metal electrode paillon foil that is covered on the flaky composite material two sides, electrode and the insulation layer of outer end coating, and described conducting polymer composite material is matrix material claimed in claim 1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015055012A1 (en) * | 2013-10-18 | 2015-04-23 | 纳米新能源（唐山）有限责任公司 | Friction generator and vibration sensor using dipolymer composite film and preparation method therefor |
| CN104720784A (en) * | 2013-12-20 | 2015-06-24 | 纳米新能源（唐山）有限责任公司 | Vibration sensor and production method thereof |
| CN106243586A (en) * | 2016-08-11 | 2016-12-21 | 苏州柯创电子材料有限公司 | High life electronic isolation compositions |
| CN106280444A (en) * | 2016-08-09 | 2017-01-04 | 安徽省宁国天成电工有限公司 | A kind of PTC themistor based on conducting polymer and application thereof |
| CN106893254A (en) * | 2016-11-23 | 2017-06-27 | 德阳九鼎智远知识产权运营有限公司 | A kind of new energy car battery positive temperature coefficient conductive composite material |
| CN107230511A (en) * | 2016-03-24 | 2017-10-03 | 瑞侃电子(上海)有限公司 | Conductive polymer compositions, electric device and preparation method thereof |
| CN107286443A (en) * | 2017-08-01 | 2017-10-24 | 合肥欧仕嘉机电设备有限公司 | A kind of preparation method of thermal resistance material |
| CN107556751A (en) * | 2017-09-19 | 2018-01-09 | 苏州南尔材料科技有限公司 | A kind of preparation method of carbon doping PPS thermistors |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015055012A1 (en) * | 2013-10-18 | 2015-04-23 | 纳米新能源（唐山）有限责任公司 | Friction generator and vibration sensor using dipolymer composite film and preparation method therefor |
| CN104720784A (en) * | 2013-12-20 | 2015-06-24 | 纳米新能源（唐山）有限责任公司 | Vibration sensor and production method thereof |
| CN107230511A (en) * | 2016-03-24 | 2017-10-03 | 瑞侃电子(上海)有限公司 | Conductive polymer compositions, electric device and preparation method thereof |
| CN107230511B (en) * | 2016-03-24 | 2019-09-03 | 上海利韬电子有限公司 | Conductive polymer compositions, electric device and preparation method thereof |
| CN106280444A (en) * | 2016-08-09 | 2017-01-04 | 安徽省宁国天成电工有限公司 | A kind of PTC themistor based on conducting polymer and application thereof |
| CN106243586A (en) * | 2016-08-11 | 2016-12-21 | 苏州柯创电子材料有限公司 | High life electronic isolation compositions |
| CN106893254A (en) * | 2016-11-23 | 2017-06-27 | 德阳九鼎智远知识产权运营有限公司 | A kind of new energy car battery positive temperature coefficient conductive composite material |
| CN107286443A (en) * | 2017-08-01 | 2017-10-24 | 合肥欧仕嘉机电设备有限公司 | A kind of preparation method of thermal resistance material |
| CN107556751A (en) * | 2017-09-19 | 2018-01-09 | 苏州南尔材料科技有限公司 | A kind of preparation method of carbon doping PPS thermistors |
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