CN102522173A - Conducting composite material with resistance positive-temperature effect and overcurrent-protecting element - Google Patents
Conducting composite material with resistance positive-temperature effect and overcurrent-protecting element Download PDFInfo
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Abstract
The invention relates to a conducting composite material with a resistance positive-temperature effect and an overcurrent-protecting element. The conducting composite material with the resistance positive-temperature effect comprises a polymeric base material and a conducting filler, wherein the polymeric base material counts for 20 to 75 percent of the volume fraction of the conducting composite material; and the conducting filler has a core-shell type granular structure which is formed by an inner core and an outer shell, the conducting filler counts for 25 to 80 percent of the volume fraction of the conducting composite material, the grain diameter is 0.1 to 20 mu m, the volume resistivity is not greater than 100mu omega. cm, and the conducting filler is dispersed in the polymeric base material. The conducting composite material with the resistance positive-temperature effect disclosed by the invention has low resistivity and excellent weather resistance, the overcurrent-protecting element prepared from the conducting composite material with the resistance positive-temperature effect has extremely-low room-temperature resistivity and simultaneously still has good weather-resisting performance and excellent resistance reproducibility and PTC (Positive Temperature Coefficient) strength.
Description
Technical field
The present invention relates to a kind of resistance positive temperature degree effect conducing composite material and over-current protecting element.
Background technology
Conducing composite material with resistance positive temperature degree effect can be kept extremely low resistance value under normal temperature; And have the sharp characteristic of variations in temperature reaction; Promptly when overcurrent taking place in the circuit or crosses high temperataure phenomena; Its resistance can be increased to a high value moment, makes circuit be in off state, to reach the purpose of protective circuit element.Therefore can be connected to conducing composite material in the circuit, as the material of current sensing with resistance positive temperature degree effect.This type of material has been widely used on the electronic circuit protection components and parts.
Conducing composite material with resistance positive temperature degree effect generally is composited by at least a polymer and conductive filler, is uniformly distributed in the said polymer on the conductive filler macroscopic view.Polymer is generally polyolefin and copolymer thereof, for example: and polyethylene or ethylene-vinyl acetate copolymer etc., and conductive filler is generally carbon black, metal powder or conductivity ceramics powder.For the conducing composite material of making conductive filler with carbon black with resistance positive temperature degree effect, because special aggregate structure and its surface of carbon black has polar group, make the tack of carbon black and polymer better, therefore have good resistance stability.But,, can't satisfy low-resistance requirement because the conductive capability of carbon black itself is limited.With the metal powder is the conducing composite material with resistance positive temperature degree effect of conductive filler; Has extremely low resistance; But, raise because of the metal powder resistance that oxidation causes in air with prevention because the easy oxidation of metal powder need be sealed conducing composite material; And the volume of the over-current protecting element that process is sealed can not effectively reduce, and is difficult to satisfy the requirement of electronic devices and components miniaturization.For obtaining lower resistance value; Overcome the drawback that metal powder is prone to oxidation simultaneously; Tend to gradually in the industry with metal carbides, metal nitride or metal boride ceramic powder (like titanium carbide) conductive filler, and this type of material has had significant progress as low resistance resistance positive temperature degree effect conducing composite material.But the dimensional thickness by the over-current protecting element of metal carbides, metal nitride or the preparation of metal boride ceramic powder be limited (like 1.0mm, 0.9mm, 0.8mm; 0.7mm), and area further dwindles (as 1210,1206; 0805; 0603 size) time, its conductivity just can't meet the demands, therefore exploitation have low-resistivity more and have a conductive filler of excellent antioxidant performance imperative.
Summary of the invention
The object of the invention is to provide a kind of resistance positive temperature degree effect conducing composite material.
A purpose more of the present invention is to provide a kind of over-current protecting element by above-mentioned conducing composite material preparation, and this over-current protecting element has low room temperature resistivity, good weather resistance, good resistance reproducibility and PTC intensity.
The present invention provides following technical proposals in order to achieve the above object: a kind of resistance positive temperature degree effect conducing composite material, comprise polymeric substrate and conductive filler, wherein:
(a) polymeric substrate account for said conducing composite material volume fraction 20%～75%; Be preferably between the 25%-70%; More excellent is between the 30%-65%; Said polymeric substrate is a kind of and composition thereof in epoxy resin, polyethylene, polypropylene, Kynoar, polyolefin elastomer, ethylene-vinyl acetate copolymer, polymethyl methacrylate, ethylene-acrylic acid copolymer, the ethylene-propylene acetoacetic ester; Wherein, polyethylene comprises: high density polyethylene (HDPE), low density polyethylene (LDPE), LLDPE, ultra-high molecular weight polyethylene etc.;
(b) described conductive filler has the core-shell type grain structure of being made up of kernel and shell, and account for said conducing composite material volume fraction 25%～80%, be preferably between the 30%-75%; More excellent is between the 35%-70%; Particle diameter is 0.01 μ m～100 μ m, is preferably 0.05 μ m～50 μ m, and more excellent is 0.1 μ m～20 μ m, 0.1 μ m～20 μ m; Specific insulation is less than 300 μ Ω .cm; More excellent is less than 200 μ Ω .cm, optimum for being not more than 100 μ Ω .cm, is scattered in the said polymeric substrate.
Above-mentioned conducing composite material can contain other components; (often be called irradiation promoter, crosslinking agent or crosslinking accelerator like antioxidant, radiation crosslinker; Cyanacrylate for example), coupling agent, dispersant, stabilizer, non-conductive filler (like magnesium hydroxide, calcium carbonate), fire retardant, arc light inhibitor or other components.These components account for 15% of conducing composite material cumulative volume, for example 10% percent by volume usually at the most.
On the such scheme basis, said kernel is by a kind of composition the among metal, metal boride, metal nitride, metal carbides or the metal silicide; Said shell is made up of the metal boride, metal nitride, metal carbides or the metal silicide that have a same metal element with kernel.
On the such scheme basis, said metal is a kind of among tantalum, vanadium, zirconium, titanium, niobium, molybdenum, hafnium, tungsten or the chromium.
Said metal boride is a kind of among tantalum boride, tantalum diboride, vanadium boride, vanadium diboride, zirconium diboride, titanium diboride, niobium (Nb) boride, niobium dioxide, boronation two molybdenums, five boronations, two molybdenums, hafnium boride, boronation two tungsten, tungsten boride, boronation two chromium, chromium boride, two chromium borides or three boronations, five chromium.
Said metal nitride is a kind of in tantalum nitride, vanadium nitride, zirconium nitride, titanium nitride, niobium nitride or the hafnium nitride.
Said metal carbides are a kind of among ramet, vanadium carbide, zirconium carbide, titanium carbide, niobium carbide, dimolybdenum carbide, hafnium carbide, tungsten carbide, ditungsten carbide or the Cr3C2.
Said metal silicide is a kind of among tantalum silicide, three silication, five tantalums, silication three vanadium, two vanadium silicides, zirconium disilicide, titanium disilicide, three silication, five titaniums, two niobium silicides, molybdenum disilicide, two hafnium suicide, two tungsten silicides, silication three chromium or two chromium silicides.
The metal boride of said composition outer core, metal nitride, metal carbides or metal silicide have different molecular structures with metal boride, metal nitride, metal carbides or the metal silicide of composition kernel, and the outer material of kernel and the internal layer material of shell interpenetrate.
The present invention provides a kind of over-current protecting element that utilizes above-mentioned resistance positive temperature degree effect conducing composite material preparation; It constitutes over-current protecting element by two metal electrode film clamping resistance positive temperature degree effect conducing composite material layers, and said metal electrode film and said conducing composite material with resistance positive temperature degree effect are combined closely.
The specific insulation of this over-current protecting element in the time of 25 ℃ be less than 0.02 Ω .cm, and have good weather resistance, good resistance reproducibility and PTC intensity.
The over-current protecting element that has the conducing composite material of resistance positive temperature degree effect and prepared by this conducing composite material of the present invention can prepare as follows:
At least one polymer and conductive filler are dropped into mixing apparatus, under the temperature that is higher than more than the crystalline polymer melt temperature, carry out melting mixing.Mixing apparatus can be banbury, mill, single screw extrusion machine or double screw extruder.Then that melting mixing is good polymer is processed into sheet material through extrusion molding, compression molding or calendering formation.In general, the thickness of polymer sheet is 0.01-3.0mm, is preferably 0.05-2.0mm, is 0.1-1.0mm for the convenience of processing is more excellent.
The forming method of composite article is the composition metal electrode slice on the two sides of polymer sheet, and the method for composition metal electrode slice comprises that mold pressing is compound or polymer sheet is directly compound with it with electrode slice through cylinder when extruding the back and also being in molten condition on the two sides of polymer sheet.Compound good sheet material can become the surface-adhered type over-current protecting element through a series of PCB processes such as etching, lamination, boring, heavy copper, zinc-plated and scribings, also can be divided into to connect other metal partss behind the discrete component and be processed into the strip over-current protecting element.The method that is divided into composite article discrete component comprises any method of isolating discrete component from composite article, for example die-cut, etching, scribing and laser cutting.Said discrete component has flat shape, promptly have with electric current to flow through two vertical surfaces of direction, and the distance between two surfaces is quite thin, i.e. and 3.0mm at the most, preferably 2.0mm at the most particularly preferably is maximum 1.0mm, for example 0.4mm.Said discrete component can be an Any shape, and is irregularly shaped like square, triangle, circle, rectangle, annular, polygon or other.Metal electrode film and said conducing composite material layer with resistance positive temperature degree effect are combined closely.The thickness of metal electrode film generally is at most 0.3mm, preferably is at most 0.2mm, 0.1mm at the most particularly, for example, 0.035mm.The material that is applicable to metal electrode film comprises nickel, copper, aluminium, zinc and compound thereof, for example Copper Foil, nickel foil, single face nickel plating Copper Foil, two-sided nickel plating Copper Foil etc.
Other metal partss can be connected on the metal electrode film through spot welding, Reflow Soldering or electroconductive binder, thereby over-current protecting element is connected in the circuit.Term " metal parts " comprise any can with the structure member of metal electrode film conducting, it can be an Any shape, for example, point-like, wire, band shape, sheet, column, other are irregularly shaped and their assembly.The base material of said " metal parts " can be any metal and alloy thereof that can conduct electricity, like nickel, copper, aluminium, zinc, tin and alloy thereof.
Usually can improve the stability of over-current protecting element performance by crosslinked and/or heat-treating methods.Crosslinked can be chemical crosslinking or cross-linking radiation, crosslinking accelerator for example capable of using, electron beam irradiation or Co
60Irradiation is realized.The required irradiation dose of over-current protecting element is generally less than 100Mrad, is preferably 1-50Mrad, and more excellent is 1-20Mrad.Heat treatment can be annealing, thermal cycle, high low temperature alternation, for example+85 ℃/and-40 ℃ high low temperature alternations.The temperature environment of said annealing can be any temperature below the polymeric substrate decomposition temperature, for example is higher than the high annealing and the process annealing that is lower than the polymeric substrate melt temperature of polymeric substrate melt temperature.
Over-current protecting element of the present invention, less than 0.2 Ω .cm, preferably less than 0.1 Ω .cm, optimum is less than 0.05 Ω .cm 25 ℃ resistivity for it, therefore over-current protecting element of the present invention is very low at 25 ℃ resistance, for example 1.0m Ω-20 m Ω.
Superiority of the present invention is: the conductive composite material resistance rate with resistance positive temperature degree effect is low; Weatherability is good; By this over-current protecting element of conducing composite material preparation with resistance positive temperature degree effect when having utmost point low room temperature resistivity; Still has good weather resistance, good resistance reproducibility and PTC intensity.
Description of drawings:
Fig. 1 is the sketch map of conduction composite sheet of the present invention;
Fig. 2 is an over-current protecting element structural representation of the present invention;
Fig. 3 is the resistance-temperature profile of the over-current protecting element of the embodiment of the invention 1;
The explanation of accompanying drawing code name:
11---conducing composite material layer 11;
12---metal electrode film 12;
13---metal pins 13.
Embodiment:
Below through concrete embodiment the present invention is done further detailed description.
Embodiment 1
The composition of the conducing composite material of preparation over-current protecting element is shown in table one.Wherein polymer is a high density polyethylene (HDPE), and its melt temperature is 134 ℃, and density is 0.953g/cm
3Conductive filler 1 is a titanium carbide, and its Fei Shi particle diameter is 2-4 μ m, and density is 4.93 g/cm
3Conductive filler 2 is the core-shell type structure, and shell is a titanium carbide, and kernel is a Titanium, and its Fei Shi particle diameter is less than 10 μ m.The preparation process of over-current protecting element is following: the banbury temperature is set in 180 ℃; Rotating speed is 30 rev/mins; Add earlier the polymer banburying after 3 minutes, add conductive filler then and continue banburying 15 minutes, obtain one have resistance positive temperature degree effect conducing composite material.The conducing composite material that melting mixing is good is through the mill calendering, and obtaining thickness is the conducing composite material layer 11 of 0.20-0.25mm.
Like Fig. 1 is the sketch map of conduction composite sheet of the present invention, and conducing composite material layer 11 is placed between laterally zygomorphic two metal electrode films 12, and metal electrode film 12 is combined closely with conducing composite material layer 11.Method through hot pressing is closely linked conducing composite material 11 and metal electrode film 12.The temperature of hot pressing is 180 ℃; Elder generation's preheating 5 minutes is then with the pressure hot pressing of 5MPa 3 minutes, again with the pressure hot pressing of 12MPa 10 minutes; On cold press, colded pressing then 8 minutes; With mould it is die-cut into the discrete component of 3*4mm, the method through Reflow Soldering is connected two metal electrode film 12 surfaces with two metal pins 13 at last, forms an over-current protecting element.
Fig. 3 is the resistance-temperature profile of the over-current protecting element of present embodiment 1.Over-current protecting element has very low resistance value in the time of 25 ℃, along with the increase of temperature, resistance slowly rises; When temperature is increased to 130 ℃ of left and right sides; The resistance of over-current protecting element is undergone mutation, and increases about 10 one magnitude, and this moment, over-current protecting element became insulator by conductor; Make circuit be in off state, to reach the purpose of protective circuit element.
Embodiment 2
The composition of the conducing composite material of preparation over-current protecting element is identical with embodiment 1; But preparation has the conducing composite material of resistance positive temperature degree effect and the step of over-current protecting element becomes: with mixing 30 minutes with conductive filler dry state in blender behind the polymer abrasive dust; Then compound is added in the double screw extruder; Extruding pelletization after melting mixing under 180 ℃-220 ℃ the temperature forms the conducing composite material with resistance positive temperature degree effect.The conducing composite material pellet that will have resistance positive temperature degree effect adds in another double screw extruder; Under 180 ℃-220 ℃ temperature, conducing composite material is extruded into the conducing composite material sheet material 11 of molten condition through the extruder die head; Conducing composite material sheet material 11 is closely linked through hot pressing roller traction hot pressing with laterally zygomorphic two metal electrode films 12; Then they are cut into the core of 110*200mm size; Through mould it is die-cut into the discrete component of 3*4mm, the method through Reflow Soldering is connected two metal electrode film 12 surfaces with two metal pins 13 at last, forms an over-current protecting element.The prescription of the conducing composite material of present embodiment and the electrical characteristic of over-current protecting element are shown in table one.
Embodiment 3
The step of conducing composite material and over-current protecting element that preparation has resistance positive temperature degree effect is identical with embodiment 1, but the volume fraction of polymer is become 46% by 40%, and the volume fraction of conductive filler 2 is become 54% by 60%.The prescription of the conducing composite material of present embodiment and the electrical characteristic of over-current protecting element are shown in table one.
Embodiment 4
The step of conducing composite material and over-current protecting element that preparation has resistance positive temperature degree effect is identical with embodiment 1, but the volume fraction of polymer 2 is become 52% by 40%, and the volume fraction of conductive filler 2 is become 48% by 60%.The prescription of the conducing composite material of present embodiment and the electrical characteristic of over-current protecting element are shown in table one.
Comparative example 1
The step of conducing composite material and over-current protecting element that preparation has resistance positive temperature degree effect is identical with embodiment 1, but changes conductive filler 2 into conductive filler 1.The prescription of the conducing composite material of present embodiment and the electrical characteristic of over-current protecting element are shown in table one.
Comparative example 2
The step of conducing composite material and over-current protecting element that preparation has resistance positive temperature degree effect is identical with embodiment 3, but changes conductive filler 2 into conductive filler 1.The prescription of the conducing composite material of present embodiment and the electrical characteristic of over-current protecting element are shown in table one.
Comparative example 3
The step of conducing composite material and over-current protecting element that preparation has resistance positive temperature degree effect is identical with embodiment 4, but changes conductive filler 2 into conductive filler 1.The prescription of the conducing composite material of present embodiment and the characteristic of over-current protecting element are shown in table one.Wherein the resistance value of over-current protecting element is to measure with four electrode method.
Table one
Table one for by the over-current protecting element of the conducing composite material preparation with resistance positive temperature degree effect of the present invention after triggering under the condition of 6V/50A, the resistance test data after placing 1 hour in 25 ℃ the temperature environment.R in the table one resistance before two metal pins 13 of representing to burn-on on two metal electrode film 12 surfaces of over-current protecting element; R
0Burn-on on two electrode slice 12 surfaces of expression over-current protecting element resistance after two metal pins 13; R
1The expression over-current protecting element continued energising (6V/50A) after 6 seconds, measured resistance value after placing 1 hour in 25 ℃ the temperature environment; R
100The expression over-current protecting element continued energising (6V/50A) after 6 seconds, cut off the power supply 60 seconds, so circulated 100 times, then measured resistance value after placing 1 hour in 25 ℃ the temperature environment.Thermal cycle (Heat cycle) R
100cyclesThe expression over-current protecting element was placed 30 minutes in+85 ℃ of environment, in-40 ℃ of environment, placed 30 minutes then, so circulated 100 times, then measured resistance value after placing 1 hour in 25 ℃ the temperature environment.Hot and humid (High temperature and humidity) R
1000hThe expression over-current protecting element was placed 1000 hours in the environment of 85%RH at 85 ℃, then measured resistance value after placing 1 hour in 25 ℃ the temperature environment.High humidity (High humidity) R
1000hThe expression over-current protecting element was placed 1000 hours in the environment of 95%RH at 60 ℃, then measured resistance value after placing 1 hour in 25 ℃ the temperature environment.
Can find out from table one: embodiment 1-2 and comparative example 1, embodiment 3 and comparative example 2, embodiment 4 and comparative example 3 have the conductive filler of equal volume mark respectively; But used conductive filler is the core-shell type grain structure among the embodiment 1-4, and the comparative example 1-3 that its finished product resistance value is made conductive filler than the titanium carbide that uses non-core-shell type grain structure is little.Over-current protecting element among the embodiment 1-4 through 6V/50A rush of current 100 times after, its resistance value is little through the resistance value behind the 6V/50A rush of current 100 times than comparative example 1-3, explains that its resistance reproducibility is better.Over-current protecting element among the embodiment 1-4 is after hot and humid and 1000 hours high humiditys were placed through 100 high low temperature circulations, 1000 hours, and its resistance change is very little, explains that it has excellent weather resistance.As can beappreciated from fig. 3, the over-current protecting element with the preparation of core-shell type grain structure conductive filler has excellent PTC intensity.
Over-current protecting element of the present invention is employed to have the conducing composite material of resistance positive temperature coefficient owing to comprise the low-down conductive filler with core-shell type grain structure of resistivity, has very low room temperature resistivity, good withstand voltage properties, excellent resistance reproducibility and PTC intensity.And employed conductive filler has the core-shell type grain structure; Be difficult for oxidized; Therefore need not to protect conducing composite material through the mode of sealing, can prepare thickness is 0.2mm-2.0mm, and the loaded current area is a undersized over-current protecting element such as 1210,1206,0805,0603.
Content of the present invention and characteristics disclose as above, yet the present invention of front narration only relates to specific part of the present invention briefly or only, characteristic of the present invention maybe than content disclosed herein relate to more.Therefore, protection scope of the present invention should be not limited to the content that embodiment discloses, and the combination of all the elements that should be included in the different piece to be embodied, and does not variously deviate from replacement of the present invention and modification, and is contained by claims of the present invention.
Claims (9)
1. a resistance positive temperature degree effect conducing composite material comprises polymeric substrate and conductive filler, it is characterized in that:
(a) polymeric substrate account for said conducing composite material volume fraction 20%～75%, said polymeric substrate is a kind of and composition thereof in epoxy resin, polyethylene, polypropylene, Kynoar, polyolefin elastomer, ethylene-vinyl acetate copolymer, polymethyl methacrylate, the ethylene-acrylic acid copolymer;
(b) described conductive filler has the core-shell type grain structure of being made up of kernel and shell; Constitute by kernel and shell; And outer material of kernel and shell internal layer material interpenetrate, combine closely, and account for said conducing composite material volume fraction 25%～80%, particle diameter is 0.1 μ m～20 μ m; Specific insulation is not more than 100 μ Ω .cm, is scattered in the said polymeric substrate.
2. the conducing composite material of resistance positive temperature degree effect according to claim 1 is characterized in that: said kernel is by a kind of composition the among metal, metal boride, metal nitride, metal carbides or the metal silicide; Said shell is made up of the metal boride, metal nitride, metal carbides or the metal silicide that have a same metal element with kernel.
3. the conducing composite material of resistance positive temperature degree effect according to claim 2 is characterized in that, said metal is a kind of among tantalum, vanadium, zirconium, titanium, niobium, molybdenum, hafnium, tungsten or the chromium.
4. the conducing composite material of resistance positive temperature degree effect according to claim 2; It is characterized in that said metal boride is a kind of among tantalum boride, tantalum diboride, vanadium boride, vanadium diboride, zirconium diboride, titanium diboride, niobium (Nb) boride, niobium dioxide, boronation two molybdenums, five boronations, two molybdenums, hafnium boride, boronation two tungsten, tungsten boride, boronation two chromium, chromium boride, two chromium borides or three boronations, five chromium.
5. the conducing composite material of resistance positive temperature degree effect according to claim 2 is characterized in that, said metal nitride is a kind of in tantalum nitride, vanadium nitride, zirconium nitride, titanium nitride, niobium nitride or the hafnium nitride.
6. the conducing composite material with resistance positive temperature degree effect according to claim 2; It is characterized in that said metal carbides are a kind of among ramet, vanadium carbide, zirconium carbide, titanium carbide, niobium carbide, dimolybdenum carbide, hafnium carbide, tungsten carbide, ditungsten carbide or the Cr3C2.
7. the conducing composite material of resistance positive temperature degree effect according to claim 2; It is characterized in that said metal silicide is a kind of among tantalum silicide, three silication, five tantalums, silication three vanadium, two vanadium silicides, zirconium disilicide, titanium disilicide, three silication, five titaniums, two niobium silicides, molybdenum disilicide, two hafnium suicide, two tungsten silicides, silication three chromium or two chromium silicides.
8. the conducing composite material of resistance positive temperature degree effect according to claim 2; It is characterized in that the metal boride of said composition outer core, metal nitride, metal carbides or metal silicide have different molecular structures with metal boride, metal nitride, metal carbides or the metal silicide of composition kernel.
9. according to the over-current protecting element of the conducing composite material of the described resistance positive temperature degree of one of claim 1 to 8 effect preparation; It is characterized in that; Constitute over-current protecting element by two metal electrode film clamping resistance positive temperature degree effect conducing composite material layers, said metal electrode film and said conducing composite material with resistance positive temperature degree effect are combined closely.
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| CN104817747A (en) * | 2015-02-04 | 2015-08-05 | 上海长园维安电子线路保护有限公司 | Polymer based conductive composite material and overcurrent protection element |
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| CN106898446A (en) * | 2017-04-18 | 2017-06-27 | 上海长园维安电子线路保护有限公司 | Over-current protecting element |
| CN107749319A (en) * | 2017-10-16 | 2018-03-02 | 北京国能电池科技有限公司 | A kind of electrically conductive composite and preparation method thereof and protection device and application |
| CN108134104A (en) * | 2017-12-26 | 2018-06-08 | 成都新柯力化工科技有限公司 | Composite catalyst carrier for fuel cell and preparation method and application thereof |
| CN108134104B (en) * | 2017-12-26 | 2020-05-12 | 成都新柯力化工科技有限公司 | Composite catalyst carrier for fuel cell and preparation method and application thereof |
| CN110157211A (en) * | 2019-06-05 | 2019-08-23 | 上海宇之赫新材料测试有限公司 | A kind of conducing composite material and preparation method thereof |
| CN116462899A (en) * | 2023-04-26 | 2023-07-21 | 芜湖佳宏新材料股份有限公司 | Low-resistance PPTC material and preparation method thereof |
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