CN1970612A - Preparation method of electrically conductive composite material with positive temperature coefficient effect - Google Patents
Preparation method of electrically conductive composite material with positive temperature coefficient effect Download PDFInfo
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- CN1970612A CN1970612A CN 200610117543 CN200610117543A CN1970612A CN 1970612 A CN1970612 A CN 1970612A CN 200610117543 CN200610117543 CN 200610117543 CN 200610117543 A CN200610117543 A CN 200610117543A CN 1970612 A CN1970612 A CN 1970612A
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Abstract
The invention discloses a making method of conductive composite material with positive-temperature coefficient effect, which comprises the following steps: (1) putting two blending polymers and conductive filler in the double-screw squeezing machine or sealed fusing machine to fuse 5-20 min with fusing temperature higher than fusing point of polymer by 10-50 deg.c; (2) moulding the blending material into film in the flat sulfurized machine.
Description
Technical field
The invention belongs to the materials processing field, particularly relate to a kind of preparation method with positive temperature coefficient effect conducing composite material.
Background technology
(positive temperature coefficient, PTC) the conducing composite material characteristic of effect is that the resistivity of material increases with the temperature rising to have positive temperature coefficient.Conductive polymer composite be conducting material add to compound in the high molecular polymer by disperseing, lamination is compound and form a kind of functional high molecule material that mode such as surface conduction film constitutes.When the adding conductive filler material prepares conducing composite material in polymeric matrix, the variation of the specific conductivity of matrix material in certain conductive filler material concentration range is discontinuous, increase along with filler content, resistivity slowly descends, when filler content reaches a certain threshold value, the volume specific resistance of compound system sharply reduces suddenly, the small increase of filler content will cause resistivity to be undergone mutation, be that conductive filler particles can be in contact with one another or enough approaching, form successive conductive path or conductive network by tunnel effect or transition of electron, this moment, the critical volume fraction of conductive filler material was called as percolation threshold.Under certain transition temperature, the resistivity of electro-conductive material can rapidly increase to a ultimate value near percolation threshold, produces the jump of several magnitude, and the phase co-conversion from (partly) conductor to isolator takes place, and presents significant PTC effect.This material is usually used in telecommunications engineering, Automatic Control Temperature Heater, current limiter, overload circuit protector etc.An important parameters that characterizes ptc material is a PTC intensity.PTC intensity is meant the ratio of the resistance value under temperature variant maximum resistance of matrix material and the room temperature.
Conducting material comprises steel fiber, carbon black, carbon nanotube etc.For example: application number is 200510055197.X, and the Chinese patent that name is called " conducing composite material " discloses by joining the method for preparing a kind of conducing composite material in a kind of thermoplastic resin as complex conductive fillers with a kind of steel fiber and another low-melting metal.This method weak point is as the metal of conductive filler material oxidized easily, can make the conductivity and the PTC intensity instability of electro-conductive material after after a while.The inorganic conductive carrier performance is comparatively stable, as carbon black and metal oxide etc.
For conducing composite material, percolation threshold is big, means to add more conductive filler material, and this may make the melt viscosity of increase system, and poor processability reduces the shock strength of material, and mechanical property is influenced.For example, the conducing composite material of high percolation threshold the NTC phenomenon can occur when using as ptc material, and the ptc material of high percolation threshold can cause considerable wear to machine when producing, thereby influences its processing characteristics.With the single polymers is the compound system of matrix, will fill the carbon black of 15%～20% mass fraction usually.For example: name is called " polyolefine/carbon black PTC conducing composite material and preparation method thereof ", and (application number: Chinese patent 03135951.5) discloses by prepare the method for conducing composite material by a certain percentage with a kind of polyolefine and carbon black; Name is called " preparation method of polyethylene PTC material ", and (application number: Chinese patent 95104914.3) discloses a kind of method for preparing ptc material with high density polyethylene(HDPE) and carbon black.These two kinds of method weak points are that the carbon black content that uses has all surpassed 20% massfraction, and the percolation threshold of its composite system is bigger, and the patent in front also needs composite system is carried out microwave radiation.Carbon black so high filling can bring some adverse influences, as increasing the melt viscosity of system, poor processability; Reduce the shock strength of material; Carbon black particle easily comes off, and causes the pollution of clean room etc.System is carried out microwave radiation, make preparation technology increase, the cost of material is increased.
The present invention utilizes the theory of " two conductivity percolation threshold ", the electroconductibility of CB filling blend polymeric matrix presents two diafiltration effects, conducting particles is not to be dispersed in the polymkeric substance fully uniformly, but by in a kind of therein polymkeric substance of most of conducting particles precedence partition or two kinds of polymkeric substance form conductive channel at the interface, thereby reduce the percolation threshold of matrix material.The electroconductibility that is matrix material depends on two factors: the one, and the concentration of CB in its enrichment mutually, the 2nd, the continuity of CB enrichment phase structure.In other words, more than percolation threshold, the CB enrichment is transformed into conductor mutually, and this conductive phase forms successive conductive network structure in multiphase polymer system, and this moment, whole matrix material just can be transformed into conductor.Because the inspissated of the non-enrichment phase of CB, make that the percolation threshold of such system CB is low when adopting single matrix.The content of carbon black will reduce like this, obviously, can utilize two diafiltration effects of CB filling blend polymkeric substance, makes more high performance ptc material with the conductive filler material of filling still less, has solved the high problem of filling the mechanical properties decrease of bringing of carbon black simultaneously again.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have positive temperature coefficient effect and seek the preparation method who replies condensation material by cable, this method technology is simple, with low cost, the conducing composite material good stability that makes.
One of a kind of preparation method with positive temperature coefficient effect conducing composite material of the present invention may further comprise the steps:
(1) two kinds of blend polymers were placed in twin screw extruder or the Banbury mixer melt blending 5～20 minutes with conductive filler material, melt temperature is higher 10～50 ℃ than the fusing point of the polymkeric substance that fusing point is the highest in the used polymeric matrix;
(2) blend mold pressing film forming in vulcanizing press.
Described polymkeric substance is for to differ bigger by melting index, or the blend of the bigger two kinds of polymkeric substance of polarity difference, these polymkeric substance comprise new LDPE (film grade), high density polyethylene(HDPE), polypropylene, polyvinyl chloride, nylon, urethane, polystyrene, the poly-methyl methacrylate polyester is to the third dioctyl phthalate second diester and poly-to the third dioctyl phthalate fourth diester;
Described polypropylene (PP) and new LDPE (film grade) (LDPE) mass ratio are 30-70: 70-30;
Described poly-methyl methacrylate polyester (PMMA) and polystyrene (PS) mass ratio are 30-70: 70-30;
Described conductive filler material is conductive carbon black, conductive tin oxide or conductive zinc oxide, conductive filler material particle size range 10-100nm, or carbon nano fiber, CNT (carbon nano-tube), diameter 1-50nm.Weight content in polymkeric substance is 2%～17%.
Described carbon black can cooperate the formation complex conductive fillers with carbon nanotube, carbon fiber etc., and when the carbon black mass content was 5-9%, black grain diameter was 29-90nm.
The blend order of described polymkeric substance and carbon black can change, to obtain the electro-conductive material of different types of different PTC intensity.
Beneficial effect
The invention has the advantages that: by the method that the present invention adopts, the low diafiltration threshold value conducing composite material that can make.In addition, present method technology is simple, and is with low cost, pollution-free, safety and environmental protection.The multiple platform material percolation threshold of the conduction that positive temperature coefficient effect is arranged that makes is low, processing characteristics and good mechanical properties, and PTC intensity can be used for telecommunications engineering, Automatic Control Temperature Heater, current limiter, overload circuit protector etc. preferably.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
When polypropylene and new LDPE (film grade) are 40/60 and carbon black mass content when being 7%, carbon black (particle diameter is 29nm) and new LDPE (film grade) and polypropylene were placed in the Banbury mixer melt blending 12～15 minutes together, melt temperature is 180 ℃, blend is the mold pressing film forming in vulcanizing press, thickness 150～300 μ m, the PTC intensity of the electro-conductive material of gained is 3.9 * 10
3
Embodiment 2
When polypropylene and new LDPE (film grade) are 70/30 and carbon black mass content when being 5%, carbon black (particle diameter is 29nm) and new LDPE (film grade) and polypropylene were placed in the Banbury mixer melt blending 12～15 minutes together, melt temperature is 180 ℃, blend is the mold pressing film forming in vulcanizing press, thickness 150～300 μ m, the PTC intensity of the electro-conductive material of gained is 2.3 * 10
4
Embodiment 3
When polypropylene and new LDPE (film grade) are 70/30 and carbon black mass content when being 5%, it earlier is the carbon black of 29nm melt blending 6～7 minutes in Banbury mixer with new LDPE (film grade) and particle diameter, added the polypropylene melt blending again 5～6 minutes, melt temperature is 180 ℃, blend is the mold pressing film forming in vulcanizing press, thickness 150～300 μ m, the PTC intensity of the electro-conductive material of gained is 1.6 * 10
4
Embodiment 4
When polypropylene and new LDPE (film grade) are 70/30 and carbon black mass content when being 5%, it earlier is the carbon black of 29nm melt blending 6～7 minutes in Banbury mixer with polypropylene and particle diameter, added the new LDPE (film grade) blend again 5～6 minutes, melt temperature is 180 ℃, blend is the mold pressing film forming in vulcanizing press, thickness 150-300 μ m.The PTC intensity of prepared electro-conductive material is 1.5 * 10
5
Embodiment 5-12
Implementation method is same as embodiment 1, and other condition is seen specific embodiment.
| The embodiment numbering | PP/LDPE (mass ratio) | Black grain diameter (nm) | Order of addition(of ingredients) | Carbon black content (massfraction) | Melt temperature (℃) | PTC intensity |
| 5 | 70/30 | 65 | PP+LDPE+CB | 6％ | 180 | 3.8×10 5 |
| 6 | 70/30 | 65 | (LDPE+CB)+PP | 6％ | 180 | 5.6×10 4 |
| 7 | 70/30 | 65 | (PP+CB)+LDPE | 6％ | 180 | 3.6×10 6 |
| 8 | 70/30 | 90 | PP+LDPE+CB | 6％ | 180 | 1.6×10 6 |
| 9 | 70/30 | 90 | (LDPE+CB)+PP | 6％ | 180 | 2.5×10 5 |
| 10 | 70/30 | 90 | (PP+CB)+LDPE | 6％ | 180 | 2.9×10 7 |
| 11 | 50/50 | 29 | PP+LDPE+CB | 7％ | 180 | 5.3×10 2 |
| 12 | 30/70 | 29 | PP+LDPE+CB | 7％ | 180 | 1.4×10 2 |
Embodiment 13
When polypropylene and new LDPE (film grade) are 70/30, with mass ratio is that the hybrid conductive filler of 1/4 carbon nanotube and carbon black (particle diameter is 29nm) replaces carbon black, the mass content of hybrid conductive filler is 5%, melt blending is 12～15 minutes in Banbury mixer, melt temperature is 180 ℃, blend is the mold pressing film forming in vulcanizing press, thickness 150～300 μ m, and the PTC intensity of the electro-conductive material of gained is 2.3 * 10
4
Embodiment 14-21
Implementation method is same as embodiment 13, and other condition is seen specific embodiment.
| The embodiment numbering | PS/PMMA (mass ratio) | Black grain diameter (nm) | Order of addition(of ingredients) | Carbon black content (massfraction) | Melt temperature (℃) | PTC intensity |
| 14 | 65/35 | 29 | PS+PMMA+CB | 9％ | 245 | 1.7×10 3 |
| 15 | 65/35 | 29 | (PMMA+CB)+PS | 9％ | 245 | 9.7×10 2 |
| 16 | 65/35 | 29 | (PS+CB)+PMMA | 9％ | 245 | 5.3×10 4 |
| 17 | 65/35 | 65 | PS+PMMA+CB | 8％ | 245 | 7.8×10 3 |
| 18 | 65/35 | 65 | (PMMA+CB)+PS | 8％ | 245 | 1.6×10 3 |
| 19 | 65/35 | 65 | (PS+CB)+PMMA | 8％ | 245 | 8.6×10 4 |
| 20 | 50/50 | 29 | PS+PMMA+CB | 8％ | 245 | 7.6×10 2 |
| 21 | 40/60 | 29 | PS+PMMA+CB | 9％ | 245 | 2.4×10 2 |
Embodiment 22
When poly-methyl methacrylate polyester and polystyrene are 70/30 and conductive tin oxide (particle diameter is 72nm) when mass content is 15%, poly-methyl methacrylate polyester and polystyrene and conductive tin oxide were placed in the Banbury mixer melt blending 12～15 minutes together, melt temperature is 245 ℃, blend is the mold pressing film forming in vulcanizing press, thickness 150～300 μ m, the PTC intensity of the electro-conductive material of gained is 5.1 * 10
4
Embodiment 23
Implementation method is with 22, and with conductive zinc oxide (particle diameter is 36nm) replacement conductive tin oxide, and the mass content of conductive zinc oxide is 13%, and the PTC intensity of the electro-conductive material of gained is 6.8 * 10
2
Claims (8)
1. preparation method with positive temperature coefficient effect conducing composite material is characterized in that may further comprise the steps:
(1) two kinds of blend polymers were placed in twin screw extruder or the Banbury mixer melt blending 5～20 minutes with conductive filler material, melt temperature is higher 10～50 ℃ than the fusing point of the polymkeric substance that fusing point is the highest in the used polymeric matrix;
(2) blend mold pressing film forming in vulcanizing press.
2. a kind of preparation method with positive temperature coefficient effect conducing composite material according to claim 1 is characterized in that: polymkeric substance is selected from new LDPE (film grade), high density polyethylene(HDPE), polypropylene, polyvinyl chloride, nylon, urethane, polystyrene, poly-methyl methacrylate polyester, to the third dioctyl phthalate second diester, poly-a kind of in the third dioctyl phthalate fourth diester.
3. a kind of preparation method with positive temperature coefficient effect conducing composite material according to claim 2 is characterized in that: described polypropylene and new LDPE (film grade) mass ratio are 30-70: 70-30.
4. a kind of preparation method with positive temperature coefficient effect conducing composite material according to claim 2 is characterized in that: described poly-methyl methacrylate polyester and polystyrene mass ratio are 30-70: 70-30;
5. a kind of preparation method according to claim 1 with positive temperature coefficient effect conducing composite material, it is characterized in that: described conductive filler material is conductive carbon black, conductive tin oxide or conductive zinc oxide, conductive filler material particle diameter model 10-100nm, the weight content in polymkeric substance is 2%～17%.
6. a kind of preparation method with positive temperature coefficient effect conducing composite material according to claim 1 is characterized in that: described conductive filler material is carbon nano fiber or CNT (carbon nano-tube), and diameter 1-50nm, the weight content in polymkeric substance are 2%～17%.
7. a kind of preparation method according to claim 5 with positive temperature coefficient effect conducing composite material, it is characterized in that: described carbon black can cooperate the formation complex conductive fillers with carbon nanotube, carbon fiber etc., when the carbon black mass content was 5-9%, black grain diameter was 29-90nm.
8. a kind of preparation method with positive temperature coefficient effect conducing composite material according to claim 1 is characterized in that: the blend order of described polymkeric substance and carbon black can change arbitrarily.
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| CN 200610117543 CN1970612A (en) | 2006-10-25 | 2006-10-25 | Preparation method of electrically conductive composite material with positive temperature coefficient effect |
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| CN 200610117543 CN1970612A (en) | 2006-10-25 | 2006-10-25 | Preparation method of electrically conductive composite material with positive temperature coefficient effect |
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| CN101597396B (en) * | 2009-07-02 | 2011-04-20 | 浙江华源电热有限公司 | Polymer-based positive temperature coefficient thermistor material |
| CN102101361A (en) * | 2009-12-17 | 2011-06-22 | 尤洛考普特德国有限公司 | A method of fabricating an improved mold core and a mold core obtained by said method |
| CN102167859A (en) * | 2011-01-20 | 2011-08-31 | 中国工程物理研究院化工材料研究所 | Low-resistivity polymer positive temperature coefficient material and preparation method thereof |
| CN102460447A (en) * | 2009-04-27 | 2012-05-16 | 应用纳米结构方案公司 | Cnt-based resistive heating for deicing composite structures |
| CN102757587A (en) * | 2012-06-12 | 2012-10-31 | 四川大学 | Linear high-density polyethylene composite material and preparation method thereof |
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| US9111658B2 (en) | 2009-04-24 | 2015-08-18 | Applied Nanostructured Solutions, Llc | CNS-shielded wires |
| US8664573B2 (en) | 2009-04-27 | 2014-03-04 | Applied Nanostructured Solutions, Llc | CNT-based resistive heating for deicing composite structures |
| CN102460447A (en) * | 2009-04-27 | 2012-05-16 | 应用纳米结构方案公司 | Cnt-based resistive heating for deicing composite structures |
| CN101597396B (en) * | 2009-07-02 | 2011-04-20 | 浙江华源电热有限公司 | Polymer-based positive temperature coefficient thermistor material |
| CN102101361B (en) * | 2009-12-17 | 2014-06-04 | 尤洛考普特德国有限公司 | A method of fabricating an improved mold core and a mold core obtained by said method |
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