CN102391647A - Manufacturing method of polyphenylene sulfide composite heat conduction material for light-emitting diode (LED) - Google Patents

Manufacturing method of polyphenylene sulfide composite heat conduction material for light-emitting diode (LED) Download PDF

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CN102391647A
CN102391647A CN2011102612719A CN201110261271A CN102391647A CN 102391647 A CN102391647 A CN 102391647A CN 2011102612719 A CN2011102612719 A CN 2011102612719A CN 201110261271 A CN201110261271 A CN 201110261271A CN 102391647 A CN102391647 A CN 102391647A
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polyphenylene sulfide
led
heat
heat conduction
whisker
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CN102391647B (en
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宋大余
宋小春
苏心桐
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SICHUAN S GRANT ELECTRONICS TECHNOLOGY Co Ltd
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SICHUAN S GRANT ELECTRONICS TECHNOLOGY Co Ltd
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Abstract

The invention discloses a manufacturing method of a polyphenylene sulfide composite heat conduction material for a light-emitting diode (LED), which adopts the following raw material formulation: 40-60% wt of polyphenylene sulfide resin, 1.5-0.5% wt of heat stabilizer trisnonyl phenyl phosphate, 8-6% wt of nanoscale heat conduction metal fiber materials, 12-7.5% wt of inorganic filling materials, 6-4% wt of heat conduction powder materials and 32.5-22% wt of 95% aluminium oxide ceramic fiber. The polyphenylene sulfide composite heat conduction material prepared by the method of the invention has a certain heat-conducting property and good mechanical strength, can be widely used for the fields such as electronic and electric products, war industry, space flight and aviation, electrocommunication and the like which need heat conduction or electronic shielding materials after being molded by injection, and is especially used as the heat conduction material for the LED, so that the heat dispersion performance of the LED in high temperature can be improved, and the service life of the LED can be prolonged.

Description

The method of manufacture of the polyphenylene sulfide composite heat conducting material of a kind of LED
Affiliated technical field
The invention belongs to the macromolecular material Application Areas.
Because the volume specific resistance that polyphenylene sulfide of the present invention (PPS) matrix material has the semi-conductor scope; All has excellent characteristic in thermotolerance, weathering resistance, flame retardant resistance, chemically-resistant materiality, physical strength, toughness, low temperature reelability aspect, therefore applicable to requiring in thermal conductivity, preventing the field widespread uses such as electrical equipment, electronic component, household electrical appliance, stereo set aspect charging property, hertzian wave stopping property, the low resistance.Simultaneously can also be used for fields such as chemical machinery, petroleum machinery, military project, space flight and aviation, electronic communication.
Background technology
Support, chip and heat sink material are the big main raw material(s)s of three in the great power LED cooling technology.The quality of the heat conductivility of great power LED has very important influence to the stable use of LED light fixture.
It is heat radiation that thermally conductive material mainly acts on, and particularly at high temperature must have certain mechanical mechanics property.There is the factor of two aspects to cause sealing the damage of LED lamp easily; The one, because existing technical limitation; The electric energy of led chip 80% converts heat energy to; It is very severe to cause great power LED in use to generate heat, and the light source use temperature is very high, and thermally conductive material requires at life-time service more than 100 ℃ and insulating property are not affected; The 2nd, instantaneous temperature is up to more than 260 ℃ when welding for high-power LED light source, and short-term high temperature can not produce thermally conductive material and destroy, and insulating property and physical strength can not have too big decay.
Traditional plastics of sealing are common nylon enhancing modified material; The modified composite material that with nylon is matrix is all undesirable relatively in high temperature resistant, ageing-resistant, shock resistance, insulating property; In the light fixture manufacturing processed or in the light source welding process, often be not easy to bear and reach 260 ℃ of short time high temperatures; And cause aging insulating property to lower, even light fixture lost efficacy.
High-performance polyphenylene sulfide (PPS) has the excellent thermostability that gets under chemical proofing and the high temperature, and has high flame retardant, radiation hardness and favorable mechanical performance and electric property.
Introduced a kind of polyphenylene sulfide (PPS) matrix material that adds conductive graphite among the Chinese patent CN:1244887, this material except volume specific resistance span of control when its injection forming good and elongation at break outside more than 10%, its range of application relative narrower.
Introduce polyphenyl thioether material of a kind of heat-conductivity conducting and preparation method thereof in the one Chinese patent application numbers 200710012359.8; The material that wherein adds is thomel, spun glass, metal-powder, carbon black powder and mineral filler etc.; Its heat-conductivity conducting material addition is 10-25%; Find in the practice, though good shock resistance of heat conductivility and technology toughness are undesirable.
Introduce a kind of highly heat conductive polyphenylene sulfide composite material and preparation method thereof in the one Chinese patent application numbers 200710076484.8; The material that wherein adds still is thomel, spun glass, metal-powder, carbon black powder and mineral filler etc.; Its heat conduction addition is 3-4%, finds also to exist the unfavorable situation of heat conduction in the practice.
Above shortcoming in view of prior art; The present invention is from new thinking; Discussion utilizes the consistency of polyphenylene sulfide and metal and ceramic fiber to produce a kind of stabile against thermal denaturation, draws the Shen rate excellent, and heat conductivility excellence, high flame retardant, good processability are as the method for manufacture of polyphenylene sulfide (PPS) composite heat conducting material of LED.
Summary of the invention
The method of manufacture of the polyphenylene sulfide composite heat conducting material of a kind of LED; With weight-average molecular weight is 3-5 ten thousand; Melting index is the linear polyphenylene sulfide resin 40-60%wt of 330-380g/10min; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.5-0.5%wt, nano level heat-conducting metal fiber 8-6%wt, inorganic filling material 12-7.5%wt, particle diameter are that carbon black powder 6-4%wt, the 95% ceramic alumina fiber 32.5-22%wt of 5-10nm makes the thermal conductivity polyphenyl thioether composite material, and its concrete technical process comprises following steps:
1), the polyphenylene sulfide resin fat raw material makes heat of oxidation crosslinking Treatment, treatment temp is 240-260 ℃; The crosslinked 2-4 of the heat of oxidation hour;
2) will pass through β-(3; The 4-epoxycyclohexyl) the ethyl trimethoxy silane surface treatment agent is handled in said inorganic filling material later and carbon black powder adding (1) gained polyphenylene sulfide; Add thermo-stabilizer phosphoric acid triphenylmethyl methacrylate in the ninth of the ten Heavenly Stems with, thorough mixing is even in impeller; Wherein inorganic filling material is calcium sulfate crystal whiskers, calcium carbonate crystal whisker and magnesium carbonate whisker one of them or its mixture of two or three, and whisker is long to be 25-50 μ m; The conductive powder powder material is that particle diameter is the carbon black powder of 5-10nm;
3) with Preblend of (2) gained polyphenylene sulfide and process β-(3; The 4-epoxycyclohexyl) the 95% ceramic alumina fiber nano level handled of ethyl trimethoxy silane surface treatment agent and heat-conducting metal filamentary material input twin screw extruder forms the polyphenylene sulfide composite heat conducting material as LED through the mixing extrusion molding of twin screw extruder, cooling, pelletizing.
Among the present invention in order to improve the thermal conductivity of LED thermally conductive material; Adopting nano level steel fiber on the one hand is strongthener, on the other hand, removes the spun glass that can be used as lagging material; The purpose that adopts 95% sapphire whisker simultaneously also is to improve the thermal conductivity of LED thermally conductive material; Further reduce the heating temp of led chip, thus the work-ing life of improving led chip, simultaneously; Metal carbonate or vitriol whisker that the inorganic fillings that adds also is to use have improved the thermal conductivity of LED thermally conductive material.
The conduction material that can also use among the present invention is conduction materials such as graphite, copper, tin, aluminium, zinc, silit, silicon nitride, thomel; But,, make its powder diameter become very inhomogeneous because these materials receive the influence of grinding technology; Make the polyphenyl thioether composite material that is used for the LED thermally conductive material like this; Further add man-hour, can make the surface of goods become coarse, will have influence on Product Application.
The particle diameter of the thermally conductive material that uses is below 10nm in the present invention, and purpose is to improve the thermotolerance of polyphenyl thioether composite material, improves its extensibility simultaneously; In order to achieve the above object, and other physical propertys that improve polyphenyl thioether composite material, crystal nucleating agent can also be added therein; Releasing agent, lubricant, ultraviolet protecting agent; Staining agent, even add auxiliary agents such as fire retardant or plastics toughening agent.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is an embodiment of the invention performance of products table.
Embodiment:
A kind of method of manufacture of the polyphenyl thioether composite material as the LED thermally conductive material; Weight-average molecular weight is 5-8 ten thousand; Melting index is after the linear polyphenylene sulfide resin of 330-380g/10min adds thermo-stabilizer, surface treated inorganic filling material, conductive powder powder material, in impeller, mixes 2-3h through the crosslinked back of the heat of oxidation; After nano level heat-conducting metal fiber or 95% ceramic alumina fiber are also passed through the processing of surface treatment agent; Extruding pelletizing, make the polyphenyl thioether composite material of LED thermally conductive material through sweet refining of twin screw extruder.
Product each item index and employed detection method are among the present invention:
Each item index among the present invention is all with reference to polyphenylene sulfide product performance index requirement in the world:
Wherein tensile strength and elongation are all carried out by GB/T1040-1992, and test speed is 10mm/min; Bent pleat intensity is pressed GB/T9341-1988 and is carried out, and resistance to impact shock is pressed GB/T1843-1996 and carried out, and volume specific resistance and surface resistivity are pressed GB/T1410-1989 and carried out.
It is 5-8 ten thousand that the present invention adopts weight-average molecular weight, and melting index is the linear polyphenylene sulfide resin of 330-380g/10min, and conventional heat cross-linking is handled.The present invention uses technical process shown in Figure 1, and practical implementation is accomplished:
It below is the pre-treatment of adding material among the present invention
1, the pre-treatment of nanosized copper, aluminium, 304 stainless steel heat-conducting metal filamentary materials
Under the airy condition; It is the solution of 3%wt that β-(3,4-Huan Yanghuanjiji)Yi Jisanjiayangjiguiwan (A-168) surface treatment agent is dissolved in raw spirit formation content, in airtight container; Nano level heat-conducting metal filamentary material is immersed in 10min in the raw spirit solution that contains the 3%wt surface treatment agent; Take out then and insert in the thermostatic drying chamber, and, be for use behind the dry 2h under 160 ℃ of conditions in temperature in draughty situation.
2, the pre-treatment of calcium sulfate, lime carbonate, magnesium carbonate whisker inorganic filling material
Under the airy condition; It is the solution of 4%wt that β-(3,4-Huan Yanghuanjiji)Yi Jisanjiayangjiguiwan (A-168) surface treatment agent is dissolved in raw spirit formation content, in airtight container; Inorganic filling material is immersed in 40min in the raw spirit solution that contains the 4%wt surface treatment agent; Take out then and insert in the thermostatic drying chamber, and, be for use behind the dry 2h under 155 ℃ of conditions in temperature in draughty situation.
3, the pre-treatment of carbon black powder material
Under the airy condition; It is the solution of 5%wt that β-(3,4-Huan Yanghuanjiji)Yi Jisanjiayangjiguiwan (A-168) surface treatment agent is dissolved in raw spirit formation content, in airtight container; Carbon black powder is immersed in 60min in the raw spirit solution that contains the 5%wt surface treatment agent; Take out then and insert in the thermostatic drying chamber, and, be for use behind the dry 3h under 150 ℃ of conditions in temperature in draughty situation.
4, the pre-treatment of the material of 95% ceramic alumina fiber
Under the airy condition; It is the solution of 3.5%wt that β-(3,4-Huan Yanghuanjiji)Yi Jisanjiayangjiguiwan (A-168) surface treatment agent is dissolved in raw spirit formation content, in airtight container; 95% ceramic alumina fiber material is immersed in 30min in the raw spirit solution that contains the 3.5%wt surface treatment agent; Take out then and insert in the thermostatic drying chamber, and, be for use behind the dry 2h under 160 ℃ of conditions in temperature in draughty situation.
Embodiment 1:
Weight-average molecular weight is 30,000, and melting index is that the linear polyphenylene sulfide resin of 380g/10min is being 240 ℃; After crosslinked 4 hours of the heat of oxidation; Polyphenylene sulfide 40kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.5kg, calcium sulfate crystal whiskers 12kg, whisker length that pre-treatment is good are 50 μ m; The particle diameter that the 6%w pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 6kg of 10nm stirred after 3 hours; Then that pre-treatment is good nanosized copper heat-conducting metal filamentary material 8kg, Fibre diameter are the macrofiber of 1nm, and 95% ceramic alumina fiber 32.5kg, the Fibre diameter that pre-treatment is good is the macrofiber input twin screw extruder of 25 μ m, extrudes through parallel dual-screw extruding machine is mixing at last; Cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 2
Weight-average molecular weight is 50,000; Melting index be 330g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 60kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 0.5kg, calcium carbonate crystal whisker 7.5kg, whisker length that pre-treatment is good are 25 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 4kg of 5nm stirred after 2.5 hours, and then that pre-treatment is good nanometer aluminum heat-conducting metal filamentary material 6kg, Fibre diameter are the macrofiber of 5nm; 95% ceramic alumina fiber 22kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 10 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 3
Weight-average molecular weight is 40,000; Melting index be 337g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 50kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.0kg, magnesium carbonate whisker 10kg, whisker length that pre-treatment is good are 30 μ m, and the particle diameter that pre-treatment is good is that prescription 5kg, the adding stirrer high speed of the carbon black powder of 6nm stirred after 3 hours, and then that pre-treatment is good nano level 304 stainless steel heat-conducting metal filamentary material 7kg, Fibre diameter are the macrofiber of 4nm; 95% ceramic alumina fiber 27kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 20 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 4
Weight-average molecular weight is 50,000; Melting index be 330g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 55kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 0.75kg, calcium sulfate crystal whiskers 8.75kg, whisker length that pre-treatment is good are 35 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 4.5kg of 8nm stirred after 2 hours, and then that pre-treatment is good nanosized copper heat-conducting metal filamentary material 6.5kg, Fibre diameter are the macrofiber of 3nm; 95% ceramic alumina fiber 24.5kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 20 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
The comparative example 1
Weight-average molecular weight is 3.8 ten thousand; Melting index be 390g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 50kg, thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.0kg, calcium sulfate crystal whiskers 9kg, whisker length that pre-treatment is good are 50 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 5kg of 10nm stirred after 2.5 hours; Then that pre-treatment is good spun glass, Fibre diameter are the macrofiber input twin screw extruder of 1-5nm; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 5
Weight-average molecular weight is 4.5 ten thousand; Melting index be 375g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 47kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.3kg, magnesium carbonate whisker 9.7kg, whisker length that pre-treatment is good are 30 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 6kg of 9nm stirred after 3 hours, and then that pre-treatment is good nanometer aluminum heat-conducting metal filamentary material 8kg, Fibre diameter are the macrofiber of 4nm; 95% ceramic alumina fiber 28kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 22 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 6
Weight-average molecular weight is 4.2 ten thousand; Melting index be 374g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 48kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.5kg, calcium carbonate crystal whisker 11.5kg, whisker length that pre-treatment is good are 45 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 5kg of 5-10nm stirred after 2.5 hours, and then that pre-treatment is good nano level 304 stainless steel heat-conducting metal filamentary material 6kg, Fibre diameter are the macrofiber of 5nm; 95% ceramic alumina fiber 28kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 15 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 7
Weight-average molecular weight is 40,000; Melting index be 361g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 44kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.5kg, calcium sulfate crystal whiskers 12kg, whisker length that pre-treatment is good are 50 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 6kg of 10nm stirred after 3 hours, and then that pre-treatment is good nanosized copper heat-conducting metal filamentary material, Fibre diameter are the macrofiber of 2nm; 95% ceramic alumina fiber 28.5kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 15 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 8
Weight-average molecular weight is 4.6 ten thousand; Melting index be 345g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 47kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.0kg, calcium carbonate crystal whisker 11kg, whisker length that pre-treatment is good are 30 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder of 9nm stirred after 2 hours, and then that pre-treatment is good nanometer aluminum heat-conducting metal filamentary material, Fibre diameter are the macrofiber of 2nm; 95% ceramic alumina fiber 29kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 25 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
Embodiment 9
Weight-average molecular weight is 50,000; Melting index be 330g/10min the linear polyphenylene sulfide resin through the heat of oxidation crosslinked after; Adopt polyphenylene sulfide 53kg; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.0kg, magnesium carbonate whisker, whisker length that pre-treatment is good are 50 μ m, and the particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder of 10nm stirred after 3 hours, and then that pre-treatment is good nano level 304 stainless steel heat-conducting metal filamentary materials, Fibre diameter are the macrofiber of 1nm; 95% ceramic alumina fiber 27kg, the Fibre diameter that pre-treatment is good is the macrofiber twin screw extruder of 25 μ m; Extrude through parallel dual-screw extruding machine is mixing at last, cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
The comparative example 2
Weight-average molecular weight is 4.3 ten thousand; Melting index be the linear polyphenylene sulfide resin of 371g/10min through the heat of oxidation crosslinked after, adopt polyphenylene sulfide 56kg, thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 0.5kg, magnesium carbonate whisker 8.5kg, whisker length that pre-treatment is good are 45 μ m; The particle diameter that pre-treatment is good is that prescription, the adding stirrer high speed of the carbon black powder 5.5kg of 5-10nm stirred after 3 hours; Then that the 29.5kg pre-treatment is good basalt fibre, Fibre diameter are the macrofiber twin screw extruder of 25 μ m, extrude through parallel dual-screw extruding machine is mixing at last; Cooling, pelletizing, packing just make a kind of polyphenyl thioether composite material as the LED thermally conductive material
More than each embodiment to obtain performance of products as shown in Figure 2.
In experiment, can verify, when adding different strongtheners, though resistance to impact shock increase relatively,, toughness but reduces much.Polyphenyl thioether composite material of the present invention; Have certain heat conductivility and excellent mechanical intensity; Need favorable mechanical performance and flame retardant properties through being widely used in electronic apparatus, military project, space flight and aviation, electronic communication etc. behind the injection forming; And to the thermal conductivity use field that has certain requirements, for example in the screening of nucleus material and the heat sink material field of extreme working conditions.

Claims (4)

1. the method for manufacture of the polyphenylene sulfide composite heat conducting material of a LED; With weight-average molecular weight is 3-5 ten thousand; Melting index is the linear polyphenylene sulfide resin 40-60%wt of 330-380g/10min; Thermo-stabilizer phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems 1.5-0.5%wt, nano level heat-conducting metal fiber 8-6%wt, inorganic filling material 12-7.5%wt, particle diameter are that carbon black powder 6-4%wt, the 95% ceramic alumina fiber 32.5-22%wt of 5-10nm makes the thermal conductivity polyphenyl thioether composite material, and its concrete technical process comprises following steps:
1), the polyphenylene sulfide resin fat raw material makes heat of oxidation crosslinking Treatment, treatment temp is 240-260 ℃; The crosslinked 2-4 of the heat of oxidation hour;
2) will pass through β-(3; The 4-epoxycyclohexyl) the ethyl trimethoxy silane surface treatment agent is handled in said inorganic filling material later and carbon black powder adding (1) gained polyphenylene sulfide; Add thermo-stabilizer phosphoric acid triphenylmethyl methacrylate in the ninth of the ten Heavenly Stems with, thorough mixing is even in impeller; Wherein inorganic filling material is calcium sulfate crystal whiskers, calcium carbonate crystal whisker and magnesium carbonate whisker one of them or its mixture of two or three, and whisker is long to be 25-50 μ m; The conductive powder powder material is that particle diameter is the carbon black powder of 5-10nm;
3) with Preblend of (2) gained polyphenylene sulfide and process β-(3; The 4-epoxycyclohexyl) the 95% ceramic alumina fiber nano level handled of ethyl trimethoxy silane surface treatment agent and heat-conducting metal filamentary material input twin screw extruder forms the polyphenylene sulfide composite heat conducting material as LED through the mixing extrusion molding of twin screw extruder, cooling, pelletizing.
2. according to the method for manufacture of the polyphenylene sulfide composite heat conducting material of the said a kind of LED of claim 1; It is characterized in that said inorganic filling material is calcium sulfate crystal whiskers, calcium carbonate crystal whisker and magnesium carbonate whisker one of them or its mixture of two or three, whisker is long to be 25-50 μ m.
3. according to the method for manufacture of the polyphenylene sulfide composite heat conducting material of the said a kind of LED of claim 1; Pre-treatment is carried out on the surface that it is characterized in that said ceramic alumina fiber, inorganic filling material, conductive powder powder material, nano level heat-conducting metal filamentary material; Its processing technological flow and condition are: under the airy condition; It is the solution of 3-5%wt that the β-(3,4-Huan Yanghuanjiji)Yi Jisanjiayangjiguiwan surface treatment agent is dissolved in raw spirit formation content, in airtight container; These materials are immersed in 10-60min in the raw spirit solution of said surface treatment agent; Take out then and insert in the thermostatic drying chamber, and, be for use behind the dry 2-3h under the 150-160 ℃ of condition in temperature in draughty situation.
4. according to the method for manufacture of the polyphenylene sulfide composite heat conducting material of the said a kind of LED of claim 1; It is characterized in that; The nano level heat-conducting metal of the non-twist shape that uses is copper fiber, aluminum fiber and 304 Stainless Steel Fibres, and Fibre diameter is that macrofiber, the 95% ceramic alumina fiber diameter of 1-5nm is the macrofiber of 10-25 μ m.
CN 201110261271 2011-09-06 2011-09-06 Manufacturing method of polyphenylene sulfide composite heat conduction material for light-emitting diode (LED) Expired - Fee Related CN102391647B (en)

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Cited By (9)

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CN102408717A (en) * 2011-09-06 2012-04-11 四川瑞安特电子技术有限公司 Manufacturing method for polyphenylene sulfide composite heat conduction material for LED
CN103144362A (en) * 2013-02-26 2013-06-12 常州丰盛光电科技股份有限公司 Electrically-conductive and/or thermally-conductive composite material with three-dimensional structure and production method thereof
CN104292817A (en) * 2014-01-08 2015-01-21 上海智高贸易有限公司 Continuous fiber composite high thermal conductive material and processing technology thereof
CN104552970A (en) * 2013-10-25 2015-04-29 中国石油化工股份有限公司 Polymer composite fiber containing superfine metal fibers and preparation method of polymer composite fiber
CN107099139A (en) * 2017-06-29 2017-08-29 安特普工程塑料(苏州)有限公司 A kind of glass fibre, anhydrous calcium sulfate whisker strengthen plain polyphenyl thioether material of low chlorine and preparation method thereof
CN107177203A (en) * 2017-05-19 2017-09-19 合肥市惠科精密模具有限公司 A kind of AMOLED screens composite heat dissipation material
CN110343385A (en) * 2019-07-10 2019-10-18 厦门芒娅贸易有限公司 A kind of heat-conductive composite material of poly- diphenyl disulfide-ceramic fibre of high impact
JPWO2021246268A1 (en) * 2020-06-02 2021-12-09
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