CN101560325B - High-temperature resistant PTC electroconductive composition, high-temperature resistant PTC device containing composition and manufacturing method thereof - Google Patents
High-temperature resistant PTC electroconductive composition, high-temperature resistant PTC device containing composition and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature resistant PTC electroconductive composition, which comprises 20 to 70 percent of organic polymers, 25 to 75 percent of electroconductive filler, 1 to 30 percent of inorganic filler and 0.1 to 10 percent of additive, wherein the preferred melting point of the organic polymers is more than 150 DEG C; the organic polymers are one or more crystalline or semi-crystalline polymers and made of one or more of nylon 11, nylon 12, polyvinylidene fluoride, soluble poly(tetrafluoroethylene), ethylene-tetrafluoroethylene copolymers, perfluoroethylene-propylene, ethylene-chlorotrifluoroethylene and copolymers thereof. The invention also provides a high-temperature resistant PTC device containing the composition and a manufacturing method thereof. The high-temperature resistant PTC device containing the composition has low resistance, high PTC strength and superior resistance stability, so that the high-temperature resistant PTC device can be used for overcurrent protection of circuits in high-temperature environments such as automobile motors and the like. Moreover, the high-temperature resistant PTC device is simple and convenient to manufacture and has high efficiency.
Description
Technical field
The present invention relates to the electrically conductive composition technical field; Be particularly related to PTC (Positive temperature coefficient; PTC) electrically conductive composition technical field specifically is meant a kind of high-temperature resistant PTC electroconductive composition, comprises the high-temperature resistant PTC device and the method for manufacture thereof of said composition.
Background technology
PTC (Positive temperature coefficient) material is also referred to as PTC material, and its resistivity before critical transition temperature keeps constant basically, reach critical transition temperature after, resistivity increases suddenly, and the transformation of several magnitude takes place.Improve the ptc characteristics that rises because the resistance of this type material has with envrionment temperature, thereby can under comparatively high temps, reduce or cut off electric current, reach the purpose that temperature control was incubated or played overcurrent, overheated, overvoltage protection.
Mostly early stage ptc material is ceramic matrix, and the PTC of polymer composite (being called for short PPTC) phenomenon is to be found first to propose by Frydman in 1945, and begins suitability for industrialized production and application the sixties in 20th century.Because the high molecular PTC material has at adjustable in a big way conductivity, to be easy to moulding, flexible, cost low, has been widely used in making self controlled heating cable, over-current protecting element and temp-sensitive sensor etc.
At present; The high molecular PTC material is generally filled crystallization or hemicrystalline organic polymer by conductive filler material and is processed; Conductive filler material generally is carbon black, graphite, metal etc.; And organic polymer generally is based on the polymkeric substance of vinyl, comprises high density polyethylene(HDPE), new LDPE (film grade), linear low density polyethylene, ethylene, ethylene/ethyl acrylate multipolymer, ethylene/butylacrylate copolymer etc.Material bodies reveals lower resistivity when temperature is low, and when temperature is elevated near the fusing point, and during promptly so-called critical transition temperature, resistivity raises suddenly, the variation of generation several magnitude.But the fusing point of this base polymer is lower, and transition temperature is all below 125 ℃.For higher fields of operating ambient temperature such as automobile micromotors, use the thermistor of this type to carry out overcurrent protection, flase operation takes place easily and cisco unity malfunction.Therefore, can under hot environments such as automobile motor, carry out work in order to make thermistor, need to seek dystectic polymkeric substance, the polymkeric substance of promptly selecting those fusing points can be higher than 150 ℃ prepares thermistor.The fusing point of pvdf, soluble poly tetrafluoroethylene, ethylene-tetrafluoroethylene copolymer, perfluoroethylene-propylene (copolymer), ethylene-chlorinated all more than 150 ℃, can satisfy the requirement of hot environment.Yet, this series products ubiquity resistance power cycles poor stability, defective such as promptly repeatedly action back resistance significantly departs from initial value, and PTC intensity is lower during low initial resistance, this has limited its use.Therefore, the PTC thermistor of exploitation high PTC effect of tool and good resistance cyclical stability is still the focus and the difficult point of industry.
Summary of the invention
The objective of the invention is to have overcome above-mentioned shortcoming of the prior art; A kind of high-temperature resistant PTC electroconductive composition is provided, comprises the high-temperature resistant PTC device and the method for manufacture thereof of said composition; The high-temperature resistant PTC device that comprises said composition has low resistance, high PTC intensity and good resistance stability; Thereby can be used on the circuit over-current protection under the hot environment such as automobile motor, and make easyly, efficient is high.
To achieve these goals, in first aspect of the present invention, a kind of high-temperature resistant PTC electroconductive composition is provided; Be characterized in, by weight, comprise 20～70% organic polymer; 25～75% conductive filler material, 1～30% mineral filler and 0.1～10% additive.
Preferably, the fusing point of said organic polymer is higher than 150 ℃.
Preferably, said organic polymer is one or more crystallizations or semi-crystalline polymer.
Preferably, said organic polymer is selected from one or more in Ni Long11, nylon 12, pvdf, soluble poly tetrafluoroethylene, ethylene-tetrafluoroethylene copolymer, perfluoroethylene-propylene (copolymer), ethylene-chlorinated and their multipolymer.
Preferably, said conductive filler material is selected from one or more of carbon black, thomel, graphite, graphite fibre, metallic particles.
More preferably, said sooty dibutyl phthalate absorption (DBP value) is at 40cm
3/ 100g is to 200cm
3Between/the 100g, said sooty particle diameter at 20nm between the 150nm.More preferably the DBP value is greatly about 50cm
3/ 100g is to 140cm
3Between/the 100g, particle diameter at 50nm between the 120nm.Satisfactory carbon black has: Raven 410 (particle diameter 101nm, DBP value 65cm
3/ 100g, Columbian company), Raven 430 (particle diameter 82nm, DBP value 78cm
3/ 100g, Columbian company), Sterling N550 (particle diameter 41nm, DBP value 120cm
3/ 100g, Cabot company).
Except described polymeric constituent and conductive filler material, the PTC electrically conductive composition also comprises one or more inert inorganic fillers usually, to improve the resistance stability of thermistor.Preferably, said mineral filler is selected from one or more of quicklime, zinc oxide, Natural manganese dioxide, aluminum oxide, silicon-dioxide, lime carbonate, Marinco H, white lake.
Preferably; Said additive comprises one or more of dispersion agent, oxidation inhibitor, crosslinking accelerator and coupling agent; Wherein said dispersion agent is a high melting-point wax; Said oxidation inhibitor is phenols or aminated compounds, and said crosslinking accelerator is the polyfunctional group unsaturated compound, and said coupling agent is silane or titanate ester organic cpds.Wherein the dispersion agent effect is the dispersion effect that improves filler, improves processing characteristics.And oxidation inhibitor is in order to increase the thermostability of product.Crosslinking accelerator is not reduce degree of crosslinking simultaneously again in order to reduce radiation dose.
More preferably; Said high melting-point wax is polyethylene wax, Poly Propylene Wax or polyimide wax, and said phenols or aminated compounds are N, and N ' 1; 6-dihexyl two (3; 5 two (1,1-diformazan ethyl)-4-hydroxybenzenes) propionic acid amide, N-stearyl-4-amino-phenol or N-dodecanoyl-4-amino-phenol, said polyfunctional group unsaturated compound is triallyl isocyanurate (TAIC).
Preferably, said high-temperature resistant PTC electroconductive composition is through irradiation and crosslinked.In order to improve elctrical stability, described PTC electrically conductive composition can pass through radiation crosslinking, and radiation dose is 1 to 100Mrads, and preferred 5 arrive 30Mrads.
In second aspect of the present invention; A kind of high-temperature resistant PTC device is provided; Comprise PTC chip and two metal foil electrode layers; Two said metal foil electrode layers are attached to respectively on the two opposite surfaces of said PTC chip, are characterized in, said PTC chip is the thin layer through cross-linking radiation that above-mentioned high-temperature resistant PTC electroconductive composition forms.
Preferably, said PTC device is 100 Ω .cm or littler at 25 ℃ volume specific resistance, 10 the when resistivity of said PTC device is 25 ℃ at least when temperature is higher than 150 ℃
4Doubly.
Preferably, said high-temperature resistant PTC device also comprises two extraction electrodes, and two said extraction electrodes are connected on the outside surface of two said metal foil electrode layers.
In the third aspect of the invention, the method for manufacture of above-mentioned high-temperature resistant PTC device is provided, be characterized in, may further comprise the steps:
A. said organic polymer, said conductive filler material, said mineral filler and said additive are carried out melt blending more than the fusing point of said organic polymer; After cooling and dicing or the pulverizing; Through extrusion calendaring or mold pressing, perhaps carry out melt blending close after directly through extrusion calendaring, obtain sheet material;
B. two said metal foil electrode layers are attached to respectively on the two opposite surfaces of said sheet material, obtain PCT device bullion;
C. said PCT device bullion is heat-treated, condition be more than the fusing point of said organic polymer 30～80 ℃ placed cool to room temperature then 1 to 60 minute;
D. the said PCT device bullion after the thermal treatment carries out crosslinkedly through gamma-rays or electron beam irradiation, and irradiation dose is 1 to 100Mrads.Preferred 5 to 30Mrads.
Preferably, in step a, said melt blending adopts twin screw extruder, mill or Banbury mixer, and the temperature of said melt blending is higher than 20～60 ℃ of the fusing points of described organic polymer.
And the moulding of PTC electrically conductive composition sheet material can be adopted that single screw extrusion machine is extruded, two roll calender calendering formation or thermocompressor are hot-forming.
Preferably, in step b, when extrusion calendaring or mold pressing, two said metal foil electrode layers are compound on the two opposite surfaces of described sheet material.
More preferably, in step b, said being compounded on two roll calender or the thermocompressor carried out, and the temperature of said two roll calender or said thermocompressor is higher than 5～50 ℃ of the fusing points of described organic polymer.
Preferably, in step c, said cooling is slow cooling, and rate of cooling is lower than 40 ℃/min.
Can also be as required the said PCT device bullion behind the irradiation carry out according to certain size die-cut after, two surface-welding extraction electrodes down above that.
Beneficial effect of the present invention is: the PTC chip of high-temperature resistant PTC device of the present invention is the thin layer through cross-linking radiation that high-temperature resistant PTC electroconductive composition of the present invention forms; High-temperature resistant PTC electroconductive composition comprises 20～70% organic polymer; 25～75% conductive filler material; 1～30% mineral filler and 0.1～10% additive; High-temperature resistant PTC device by this high-temperature resistant PTC electroconductive composition preparation has low resistance, high PTC intensity and good resistance stability; Particularly this device has lower resistivity (below the 100 Ω .cm or littler, preferred 30 Ω .cm) and high PTC effect (10 when the peak resistance rate the during action of PTC device is 25 ℃ at least in the time of 25 ℃
4Doubly, preferred 10
5Doubly, more preferably 10
6Doubly, even bigger), thereby can be used on the circuit over-current protection under the hot environment such as automobile motor, and high-temperature resistant PTC device of the present invention makes easyly, efficient is high.
Embodiment
In order more to be expressly understood technology contents of the present invention, the special following examples of lifting specify.
Embodiment 1
With the nylon 12 (Aesno-TL, fusing point: 165～180 ℃, melt finger: 0.3g/10min, ElfAtochem company) of 45wt%, carbon black Raven 430 (particle diameter 82nm, the DBP value 78cm of 50wt%
3/ 100g; Columbian company), the Natural manganese dioxide of 4.5wt% (MgO) and 0.5wt% antioxidant 1010 (Irganox1010; Ciba Geigy company) join melt blending in the twin screw extruder after the pre-mixing, the mixture melt directly gets into single screw extrusion machine by head, is pressed into certain thickness 0.3mm through two roll calender then; Simultaneously paste the nickel-clad copper foil electrode, thereby obtain the PTC sheet material on two surfaces up and down of compsn.The PTC sheet material was placed 30 minutes in 200 ℃ baking oven, turned off the baking oven power supply then, slowly cool to room temperature.With gamma-rays the good sheet material of thermal treatment is carried out crosslinkedly, irradiation dose is 20Mrads.At last, sheet material good behind the irradiation is die-cut into the PTC chip of 8 * 12mm.Measure its resistance (R in the time of 25 ℃
0) and the R-T resistance-temperature curve, calculate PTC intensity (Rmax/R
0, wherein Rmax is the maximum resistance after the PTC device action).Measure PTC device resistance value R after power cycles under 16V, the 100A 1000 times
1000With the resistance value R after lasting the energising 24 hours under 16V, the 50A
24, changes in resistance before and after relatively switching on.The physical performance data of PTC device is listed in the table 2.
Embodiment 2
According to making the PTC device with identical mode described in the embodiment 1, but nylon 12 (Aesno-TL) content is become 41wt% by 45wt%, carbon black Raven 430 content become 54wt% by 50wt%.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Embodiment 3
According to making the PTC device with identical mode described in the embodiment 1, but nylon 12 (Aesno-TL) content is become 37wt% by 45wt%, carbon black Raven 430 content become 58wt% by 50wt%.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Embodiment 4
According to making the PTC device with identical mode described in the embodiment 1, but nylon 12 (Aesno-TL) content is become 20wt% by 45wt%, carbon black Raven 430 content become 75wt% by 50wt%.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Embodiment 5
According to making the PTC device with identical mode described in the embodiment 1, but nylon 12 (Aesno-TL) content is become 70wt% by 45wt%, carbon black Raven 430 content become 25wt% by 50wt%.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Embodiment 6
According to making the PTC device with identical mode described in the embodiment 1, but with carbon black Sterling N550 (particle diameter 41nm, the DBP value 120cm of 45wt%
3/ 100g, Cabot company) replace 50wt% among the embodiment 1 carbon black Raven 430 make conductive filler material, the mass percent of corresponding nylon 12 (Aesno-TL) becomes 50wt% by 45wt%.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Embodiment 7
According to making the PTC device with identical mode described in the embodiment 1, but with carbon black Asahi#15HS (particle diameter 120nm, the DBP value 84cm of 54wt%
3/ 100g, Asahi company) replace 50wt% among the embodiment 1 carbon black Raven 430 make conductive filler material, the mass percent of corresponding nylon 12 (Aesno-TL) becomes 41wt% by 46wt%.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Comparative example 1
According to making the PTC device, but replace the irradiation dose of the 20Mrads among the embodiment 2 to carry out crosslinked with the irradiation dose of 10Mrads with identical mode described in the embodiment 2.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Comparative example 2
According to making the PTC device, be quenched to room temperature but the slow cooling of the heat-treat condition among the embodiment 2 changed into to room temperature with identical mode described in the embodiment 2.According to the physicals of the PTC device of measuring with identical mode described in the embodiment 1, the result lists in the table 2.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative example 1 | Comparative example 2 | |
| Nylon 12 (Aesno-TL) | 45 | 41 | 37 | 20 | 70 | 50 | 41 | 41 | 41 |
| Raven?430 | 50 | 54 | 58 | 75 | 25 | 54 | 54 | ||
| Sterling?N550 | 45 | ||||||||
| Asahi#15HS | 54 | ||||||||
| MgO | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 |
| Antioxidant 1010 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Irradiation dose Mrads | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 10 | 20 |
| Heat-treat condition | Slow cooling | Slow cooling | Slow cooling | Slow cooling | Slow cooling | Slow cooling | Slow cooling | Slow cooling | Chilling |
Annotate: material is formed unit: mass percent wt%
Table 2
| Room temperature resistance R 0(mΩ) | Room temperature resistivity (Ω .cm) | PTC intensity Rmax/R 0 | 1000 circulation resistance change rates of anti-stream | Durable 24 hours resistance change rates | |
| Embodiment 1 | 58.7 | 2.935 | 4.2×10 7 | 36.2 | 75.8 |
| Embodiment 2 | 18.9 | 0.945 | 5.8×10 6 | 45.8 | 90.3 |
| Embodiment 3 | 7.5 | 0.375 | 1.3×10 4 | 57.7 | 115.4 |
| Embodiment 4 | 2.6 | 0.13 | 3.1×10 2 | 79.8 | 136.7 |
| Embodiment 5 | 783 | 39.15 | 6.7×10 10 | 25.2 | 50.6 |
| Embodiment 6 | 16.3 | 0.815 | 3.4×10 4 | 67.5 | 136.5 |
| Embodiment 7 | 24.2 | 1.21 | 7.6×10 6 | 33.9 | 95.6 |
| Comparative example 1 | 16.4 | 0.82 | 2.3×10 6 | 58.3 | 108.7 |
| Comparative example 2 | 30.5 | 1.525 | 7.4×10 5 | 53.6 | 100.4 |
Through table 1 and table 2; Can know; Adopt the high-temperature resistant PTC device of high-temperature resistant PTC electroconductive composition manufacturing of the present invention when room temperature, to have lower resistivity (below the 100 Ω .cm or littler, preferred 30 Ω .cm) and high PTC effect (10 when the peak resistance rate the during action of PTC device is 25 ℃ at least
4Doubly, preferred 10
5Doubly, more preferably 10
6Doubly, even bigger), through comparing embodiment 2 and Comparative Examples 1 and 2, can find that the present invention heat treated slow cooling step and big slightly irradiation dose when preparing high-temperature resistant PTC device help the high-temperature resistant PTC device optimization in Properties.
To sum up, the high-temperature resistant PTC device that comprises high-temperature resistant PTC electroconductive composition of the present invention has low resistance, high PTC intensity and good resistance stability, thereby can be used on the circuit over-current protection under the hot environment such as automobile motor, and makes easyly, and efficient is high.
In this specification sheets, the present invention is described with reference to its certain embodiments.But, still can make various modifications and conversion obviously and not deviate from the spirit and scope of the present invention.Therefore, specification sheets and accompanying drawing are regarded in an illustrative, rather than a restrictive.
Claims (10)
1. a high-temperature resistant PTC electroconductive composition is characterized in that, by weight, comprises the carbon black Raven430 of 41% nylon 12,54%, 4.5% Natural manganese dioxide and 0.5% antioxidant 1010.
2. high-temperature resistant PTC electroconductive composition according to claim 1 is characterized in that, said high-temperature resistant PTC electroconductive composition is through irradiation and crosslinked.
3. high-temperature resistant PTC device; Comprise PTC chip and two metal foil electrode layers; Two said metal foil electrode layers are attached to respectively on the two opposite surfaces of said PTC chip; It is characterized in that said PTC chip is the thin layer through cross-linking radiation that high-temperature resistant PTC electroconductive composition according to claim 1 forms.
4. high-temperature resistant PTC device according to claim 3 is characterized in that, said PTC device is 100 Ω .cm or littler at 25 ℃ volume specific resistance, 10 the when resistivity of said PTC device is 25 ℃ at least when temperature is higher than 150 ℃
4Doubly.
5. high-temperature resistant PTC device according to claim 3 is characterized in that said high-temperature resistant PTC device also comprises two extraction electrodes, and two said extraction electrodes are connected on the outside surface of two said metal foil electrode layers.
6. the method for manufacture of a high-temperature resistant PTC device according to claim 3 is characterized in that, may further comprise the steps:
A. said nylon 12, said carbon black Raven 430, said Natural manganese dioxide and said antioxidant 1010 are carried out melt blending more than the fusing point of said nylon 12; After cooling and dicing or the pulverizing; Through extrusion calendaring or mold pressing, perhaps carry out melt blending close after directly through extrusion calendaring, obtain sheet material;
B. two said metal foil electrode layers are attached to respectively on the two opposite surfaces of said sheet material, obtain PCT device bullion;
C. said PCT device bullion is heat-treated, condition be more than the fusing point of said nylon 12 30～80 ℃ placed cool to room temperature then 1 to 60 minute;
D. the said PCT device bullion after the thermal treatment carries out crosslinkedly through gamma-rays or electron beam irradiation, and irradiation dose is 1 to 100Mrads.
7. the method for manufacture of high-temperature resistant PTC device according to claim 6 is characterized in that, in step a, said melt blending adopts twin screw extruder, mill or Banbury mixer, and the temperature of said melt blending is higher than 20～60 ℃ of the fusing points of said nylon 12.
8. the method for manufacture of high-temperature resistant PTC device according to claim 6 is characterized in that, in step b, when extrusion calendaring or mold pressing, two said metal foil electrode layers is compound on the two opposite surfaces of described sheet material.
9. the method for manufacture of high-temperature resistant PTC device according to claim 8; It is characterized in that; In step b, said being compounded on two roll calender or the thermocompressor carried out, and the temperature of said two roll calender or said thermocompressor is higher than 5～50 ℃ of the fusing points of said nylon 12.
10. the method for manufacture of high-temperature resistant PTC device according to claim 6 is characterized in that, in step c, said cooling is slow cooling, and rate of cooling is lower than 40 ℃/min.
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2009
- 2009-05-26 CN CN2009100520927A patent/CN101560325B/en active Active
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| CN111319256A (en) * | 2020-04-07 | 2020-06-23 | 常州大学 | Method for directly manufacturing organic polymer PTC thermosensitive device through 3D printing |
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| CN101560325A (en) | 2009-10-21 |
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