CN102391647B - 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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CN102391647B
CN102391647B CN 201110261271 CN201110261271A CN102391647B CN 102391647 B CN102391647 B CN 102391647B CN 201110261271 CN201110261271 CN 201110261271 CN 201110261271 A CN201110261271 A CN 201110261271A CN 102391647 B CN102391647 B CN 102391647B
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polyphenylene sulfide
led
heat conduction
heat
treatment
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CN102391647A (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 manufacture method of the polyphenylene sulfide composite heat conduction 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 the 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 large main raw material(s)s of three in the great power LED cooling technique.The quality of the heat conductivility of great power LED has very important impact to the stable use of LED light fixture.
The thermally conductive material Main Function is heat radiation, particularly at high temperature must have certain mechanical mechanics property.There is the factor of two aspects easily to cause sealing the damage of LED lamp, the one, because existing technical limitation, the electric energy energy transform into heat energy of led chip 80%, cause great power LED in use to generate heat very severe, 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 large decay.
Traditional plastics of sealing are common nylon enhancing modified material, modified composite material take nylon as matrix is all relatively undesirable 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 good mechanical property and electric property.
Introduced a kind of polyphenylene sulfide (PPS) matrix material that adds conductive graphite among the China Patent No. CN:1244887, this material is good except volume specific resistance span of control when its injection forming, with elongation at break 10% with upper outside, its range of application relative narrower.
Introduce polyphenyl thioether material of a kind of heat-conductivity conducting and preparation method thereof in the Chinese patent application numbers 200710012359.8, the material that wherein adds is carbon fiber, glass fibre, metal-powder, carbon black powder and mineral filler etc., its heat-conductivity conducting Material Addition amount is 10-25%, find in the practice, although the good shock resistance of heat conductivility and technique toughness are undesirable.
Introduce a kind of highly heat conductive polyphenylene sulfide composite material and preparation method thereof in the Chinese patent application numbers 200710076484.8, material or carbon fiber, glass fibre, metal-powder, carbon black powder and the mineral filler etc. wherein added, its heat conduction addition is 3-4%, finds also to exist the undesirable 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 manufacture method of polyphenylene sulfide (PPS) composite heat conducting material of LED.
Summary of the invention
The manufacture method of the polyphenylene sulfide composite heat conduction material of a kind of LED, be 3-5 ten thousand with weight-average molecular weight, 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 technology flow 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 be through β-(3, the 4-epoxycyclohexyl) the ethyl trimethoxy silane surface treatment agent is processed in described 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 and, in homogenizer, fully mix; 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 the Preblend of (2) gained polyphenylene sulfide and process β-(3, the 4-epoxycyclohexyl) the 95% ceramic alumina fiber nano level processed of ethyl trimethoxy silane surface treatment agent and heat-conducting metal filamentary material input twin screw extruder forms the polyphenylene sulfide composite heat conduction material as LED through the shaping of twin screw extruder mixing extrusion, 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, remove the glass fibre that can be used as lagging material, the purpose that adopts simultaneously 95% sapphire whisker also is to improve the thermal conductivity of LED thermally conductive material, further reduce the heating temp of led chip, thereby improve the work-ing life of led chip, simultaneously, the inorganic fillings that adds also is metal carbonate or the vitriol whisker that uses, and has improved the thermal conductivity of LED thermally conductive material.
The conduction material that can also use among the present invention is the conduction materials such as graphite, copper, tin, aluminium, zinc, silicon carbide, silicon nitride, carbon fiber, but, because these materials are subjected to the impact of grinding technology, make its powder diameter become very inhomogeneous, make like this polyphenyl thioether composite material that is used for the LED thermally conductive material, further add man-hour, can make the surface of goods become coarse, will have influence on the application of goods.
The particle diameter of the thermally conductive material that uses is below 10nm in the present invention, purpose is to improve the thermotolerance of polyphenyl thioether composite material, improve simultaneously its extensibility, in order to achieve the above object, and other physical propertys that improve polyphenyl thioether composite material, can also add therein crystal nucleating agent, releasing agent, lubricant, ultraviolet protecting agent, staining agent, even add the auxiliary agents such as fire retardant or plastics toughening agent.
Description of drawings:
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the performance table of embodiment of the invention product.
Embodiment:
A kind of manufacture method 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 after crosslinked, mixes 2-3h in homogenizer through 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 through sweet refining of twin screw extruder, make the polyphenyl thioether composite material of LED thermally conductive material.
Product indices and employed detection method are among the present invention:
Indices among the present invention is all with reference in the world polyphenylene sulfide product performance index requirement:
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 processed.The present invention's technical process shown in Figure 1, implementation is finished:
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 condition of ventilating, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane (A-168) surface treatment agent is dissolved in raw spirit to form content is the solution of 3%wt, 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, then take out and insert in the thermostatic drying chamber, and in draughty situation, be stand-by behind the dry 2h under 160 ℃ of conditions in temperature.
2, the pre-treatment of calcium sulfate, calcium carbonate, magnesium carbonate whisker inorganic filling material
Under the condition of ventilating, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane (A-168) surface treatment agent is dissolved in raw spirit to form content is the solution of 4%wt, in airtight container, inorganic filling material is immersed in 40min in the raw spirit solution that contains the 4%wt surface treatment agent, then take out and insert in the thermostatic drying chamber, and in draughty situation, be stand-by behind the dry 2h under 155 ℃ of conditions in temperature.
3, the pre-treatment of carbon black powder material
Under the condition of ventilating, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane (A-168) surface treatment agent is dissolved in raw spirit to form content is the solution of 5%wt, in airtight container, carbon black powder is immersed in 60min in the raw spirit solution that contains the 5%wt surface treatment agent, then take out and insert in the thermostatic drying chamber, and in draughty situation, be stand-by behind the dry 3h under 150 ℃ of conditions in temperature.
4, the pre-treatment of the material of 95% ceramic alumina fiber
Under the condition of ventilating, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane (A-168) surface treatment agent is dissolved in raw spirit to form content is the solution of 3.5%wt, 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, then take out and insert in the thermostatic drying chamber, and in draughty situation, be stand-by behind the dry 2h under 160 ℃ of conditions in temperature.
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, the calcium sulfate crystal whiskers 12kg that pre-treatment is good, whisker length is 50 μ m, the particle diameter that the 6%w pre-treatment is good is the prescription of the carbon black powder 6kg of 10nm, adding the stirrer high speed stirred after 3 hours, then the nanosized copper heat-conducting metal filamentary material 8kg that pre-treatment is good, Fibre diameter is the macrofiber of 1nm, the 95% ceramic alumina fiber 32.5kg that pre-treatment is good, Fibre diameter is the macrofiber input twin screw extruder of 25 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the calcium carbonate crystal whisker 7.5kg that pre-treatment is good, whisker length is 25 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 4kg of 5nm, adding the stirrer high speed stirred after 2.5 hours, then the nanometer aluminum heat-conducting metal filamentary material 6kg that pre-treatment is good, Fibre diameter is the macrofiber of 5nm, the 95% ceramic alumina fiber 22kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 10 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the magnesium carbonate whisker 10kg that pre-treatment is good, whisker length is 30 μ m, the particle diameter that pre-treatment is good is the prescription 5kg of the carbon black powder of 6nm, adding the stirrer high speed stirred after 3 hours, then nano level 304 stainless steel heat-conducting metal filamentary material 7kg that pre-treatment is good, Fibre diameter is the macrofiber of 4nm, the 95% ceramic alumina fiber 27kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 20 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the calcium sulfate crystal whiskers 8.75kg that pre-treatment is good, whisker length is 35 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 4.5kg of 8nm, adding the stirrer high speed stirred after 2 hours, then the nanosized copper heat-conducting metal filamentary material 6.5kg that pre-treatment is good, Fibre diameter is the macrofiber of 3nm, the 95% ceramic alumina fiber 24.5kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 20 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the calcium sulfate crystal whiskers 9kg that pre-treatment is good, whisker length is 50 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 5kg of 10nm, adding the stirrer high speed stirred after 2.5 hours, then the glass fibre that pre-treatment is good, Fibre diameter is the macrofiber input twin screw extruder of 1-5nm, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the magnesium carbonate whisker 9.7kg that pre-treatment is good, whisker length is 30 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 6kg of 9nm, adding the stirrer high speed stirred after 3 hours, then the nanometer aluminum heat-conducting metal filamentary material 8kg that pre-treatment is good, Fibre diameter is the macrofiber of 4nm, the 95% ceramic alumina fiber 28kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 22 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the calcium carbonate crystal whisker 11.5kg that pre-treatment is good, whisker length is 45 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 5kg of 5-10nm, adding the stirrer high speed stirred after 2.5 hours, then nano level 304 stainless steel heat-conducting metal filamentary material 6kg that pre-treatment is good, Fibre diameter is the macrofiber of 5nm, the 95% ceramic alumina fiber 28kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 15 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the calcium sulfate crystal whiskers 12kg that pre-treatment is good, whisker length is 50 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 6kg of 10nm, adding the stirrer high speed stirred after 3 hours, then the nanosized copper heat-conducting metal filamentary material that pre-treatment is good, Fibre diameter is the macrofiber of 2nm, the 95% ceramic alumina fiber 28.5kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 15 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the calcium carbonate crystal whisker 11kg that pre-treatment is good, whisker length is 30 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder of 9nm, adding the stirrer high speed stirred after 2 hours, then the nanometer aluminum heat-conducting metal filamentary material that pre-treatment is good, Fibre diameter is the macrofiber of 2nm, the 95% ceramic alumina fiber 29kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 25 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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, the magnesium carbonate whisker that pre-treatment is good, whisker length is 50 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder of 10nm, adding the stirrer high speed stirred after 3 hours, then nano level 304 stainless steel heat-conducting metal filamentary materials that pre-treatment is good, Fibre diameter is the macrofiber of 1nm, the 95% ceramic alumina fiber 27kg that pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 25 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes 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 371g/10min the linear polyphenylene sulfide resin 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, the magnesium carbonate whisker 8.5kg that pre-treatment is good, whisker length is 45 μ m, the particle diameter that pre-treatment is good is the prescription of the carbon black powder 5.5kg of 5-10nm, adding the stirrer high speed stirred after 3 hours, then the basalt fibre that the 29.5kg pre-treatment is good, Fibre diameter is the macrofiber twin screw extruder of 25 μ m, finally by crossing the parallel dual-screw extruding machine mixing extrusion, cooling, pelletizing, packing just makes a kind of polyphenyl thioether composite material as the LED thermally conductive material
The performance that above each embodiment obtains product as shown in Figure 2.
In experiment, can verify, when adding different strongtheners, although resistance to impact shock relatively increase,, toughness but reduces much.Polyphenyl thioether composite material of the present invention, have certain heat conductivility and good physical strength, need good mechanical property 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 screening of nucleus material and the heat sink material field of extreme working conditions.

Claims (3)

1. the manufacture method of the polyphenylene sulfide composite heat conduction material of a LED, be 3-5 ten thousand with weight-average molecular weight, 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 technology flow 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 be through β-(3, the 4-epoxycyclohexyl) the ethyl trimethoxy silane surface treatment agent is processed in described 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, in homogenizer, fully mix; 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 the Preblend of (2) gained polyphenylene sulfide and process β-(3, the 4-epoxycyclohexyl) 95% ceramic alumina fiber processed of ethyl trimethoxy silane surface treatment agent and nano level heat-conducting metal filamentary material input twin screw extruder forms the polyphenylene sulfide composite heat conduction material as LED through the shaping of twin screw extruder mixing extrusion, cooling, pelletizing.
2. the manufacture method of the polyphenylene sulfide composite heat conduction material of described a kind of LED according to claim 1, it is characterized in that described ceramic alumina fiber, inorganic filling material, the conductive powder powder material, pre-treatment is carried out on the surface of nano level heat-conducting metal filamentary material, its processing technological flow and condition are: under the condition of ventilating, β-(3, the 4-epoxycyclohexyl) the ethyl trimethoxy silane surface treatment agent is dissolved in raw spirit to form content is the solution of 3-5%wt, in airtight container, these materials are immersed in 10-60min in the raw spirit solution of described surface treatment agent, then take out and insert in the thermostatic drying chamber, and in draughty situation, be stand-by behind the dry 2-3h under the 150-160 ℃ of condition in temperature.
3. the manufacture method of the polyphenylene sulfide composite heat conduction material of described a kind of LED according to claim 1, it is characterized in that, described nano level heat-conducting metal is that non-twist shape, Fibre diameter are the macrofiber of 1-5nm, and steel fiber wherein is copper fiber, aluminum fiber and 304 Stainless Steel Fibres; Described 95% ceramic alumina fiber diameter 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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Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN103144362B (en) * 2013-02-26 2015-11-18 常州丰盛光电科技股份有限公司 There is the conduction of stereochemical structure and/or heat-conductive composite material and production method thereof
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Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0953606A4 (en) * 1996-11-27 2000-11-08 Kureha Chemical Ind Co Ltd Polyarylene sulfide resin composition
JP4855030B2 (en) * 2004-12-21 2012-01-18 旭化成ケミカルズ株式会社 Polyphenylene sulfide resin composition
CN101113240A (en) * 2007-08-23 2008-01-30 深圳市科聚新材料有限公司 Highly heat conductive polyphenylene sulfide composite material and method for making same
CN101465403B (en) * 2008-12-31 2011-03-23 四川瑞安特电子技术有限公司 Technique for producing encapsulating material for high-power LED support frame
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

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