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CN104788951A - LED (light-emitting diode) high-thermal-conductivity composite material and preparation method thereof - Google Patents

LED (light-emitting diode) high-thermal-conductivity composite material and preparation method thereof Download PDF

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Publication number
CN104788951A
CN104788951A CN201510220412.0A CN201510220412A CN104788951A CN 104788951 A CN104788951 A CN 104788951A CN 201510220412 A CN201510220412 A CN 201510220412A CN 104788951 A CN104788951 A CN 104788951A
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Prior art keywords
inorganic filler
thermal conductivity
coupling agent
high thermal
matrix material
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CN201510220412.0A
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Chinese (zh)
Inventor
陈继兵
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Wuhan Polytechnic University
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Wuhan Polytechnic University
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Priority to CN201510220412.0A priority Critical patent/CN104788951A/en
Publication of CN104788951A publication Critical patent/CN104788951A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06Polyamides derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/22Halogen free composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to an LED (light-emitting diode) high-thermal-conductivity composite material and a preparation method thereof. The LED high-thermal-conductivity composite material is prepared by mixing 60-90 wt.% of nylon resin as a base material, 5-30 wt.% of flaky inorganic filler and powdery inorganic filler subjected to surface treatment by a coupling agent, 2-10 wt.% of flame retardant and 0.5-2 wt.% of compatilizer. Compared with the prior art, the method enhances the thermal conductivity of the material; the method can prevent the hazard of product combustion and ignition caused by overhigh heat, thereby greatly enhancing the safety performance; the molecule-atom combination reaction rate is greatly enhanced, so that the base material and filler can be combined together more quickly and compactly, thereby enhancing the thermal conductivity of the material; the composite material has the advantages of simple preparation technique and low cost, and can save abundant resources; and the method is suitable for mass production.

Description

A kind of LED high thermal conductivity matrix material and preparation method
Technical field
The present invention relates to polymer/inorganic composite materials technical field, specifically relate to a kind of LED high thermal conductivity matrix material and preparation method.
Background technology
Current LED illumination heat-dissipating casing is mainly based on metals such as Al and Alalloy, and it not only consumes a large amount of Mineral resources and the energy, environmental disruption and seriously polluted, and there is machine-shaping complexity, quality weight, the problem that cost is high, is not suitable for the popularization and application of daily life.Therefore in order to make LED illumination product come into huge numbers of families quickly, the present invention puts forth effort to solve the problem, research and development can carry out scale operation manufacture, and recyclablely to recycle, and it is light to have quality, the high thermal conductivity heat conduction functional materials of the advantages such as price is low is as heat-dissipating casing, LED heat-sinking capability can be improved, simplify the processing and forming technology of heat-dissipating casing, when substituting the metal shell of the LED of current use, will can greatly reduce LED illumination products production cost.Therefore the heat conduction functional materials developing semiconductor lighting high thermal conductivity promotes traditional lighting industry for country, drive the vital measure of related industries development, also be the important channel realizing energy-saving and emission-reduction, to promote domestic demands, expand and increase, the mode of accelerating development changes, and advances strategic restructuring of the economy, cultivates and has the new industry of international competitiveness to be significant.
Use the research of the heat-conducting plastic of high thermal conductivity less in addition for LED illumination heat-dissipating casing, in order to manufacture the thermally conductive material with excellent comprehensive performance, general is all select the metal of granular high thermal conductivity or mineral filler to fill macromolecular material, because under specific filler ratio, granular have good workability.Cheap, the easy machine-shaping of the thermally conductive material obtained like this, can be applied to the heat conduction requirement of some special dimension through suitable art breading or formula adjustment.
Summary of the invention
Technical problem to be solved by this invention proposes a kind of LED high thermal conductivity matrix material and preparation method for above-mentioned prior art, to replace the product adopting metallic substance as heat-dissipating casing, as various indoor and outdoors LED, overcome high, the unmanageable problem of metallic substance price, also solve shaping efficiency low, quality weight, not environmentally, uneasy congruent problem.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of LED high thermal conductivity matrix material, it is for following each component is through mixing, the nylon resin of 60-90wt.% is body material, the flaky inorganic filler of 5-30wt.% after coupling agent surface treatment and the mixing of powdered inorganic filler, the fire retardant of 2-10wt.% and the compatilizer of 0.5-2wt.%, described flaky inorganic filler is graphite, and described powdered inorganic filler is the mixing of one or more in silicon carbide, aluminium sesquioxide, magnesium oxide or aluminium nitride.
By such scheme, described nylon resin is granular PA66 or PA46, and its particle diameter is 1-5mm.
By such scheme, described graphite is sheet, and its diameter is 10-30 μm, and thickness is 1-5 μm.
By such scheme, described silicon carbide, aluminium sesquioxide, magnesium oxide or aluminium nitride are Powdered, and particle diameter is 10-100nm.
By such scheme, described coupling agent is silane coupling agent, aluminate coupling agent and titanate coupling agent.
By such scheme, described fire retardant is that high purity alumina-magnesia, Halogen or PA add fine type environmental protection fire retarding agent.
By such scheme, described compatilizer is the compatilizer of ring-type maleic anhydride or glycidyl methacrylate graft.
The preparation method of described LED high thermal conductivity matrix material, is characterized in that: comprise the following steps:
1) adopt coupling agent to carry out surface treatment to flaky inorganic filler, being add flaky inorganic filler in body material with nylon resin, being placed in ball mill and mixing;
2) powdered inorganic filler and fire retardant are added step 1) in gained mixture, be again placed in ball mill and mix;
3) by step 2) in gained mixture when being preheated to 60-80 DEG C, add compatilizer, be again placed in ball mill and mix;
4) by step 3) raw material that mixes puts into twin-screw extrusion machine and carries out granulation, is packaged into bag; Wherein each component concentration is: the nylon resin of 60-90wt.% is body material, the flaky inorganic filler of 5-30wt.% after coupling agent surface treatment and the mixing of powdered inorganic filler, the fire retardant of 2-10wt.% and the compatilizer of 0.5-2wt.%.
Flaky inorganic filler of the present invention and powdered inorganic filler mainly as filling body material, and play conductive force; Fire retardant plays fire-retardant and fireproofing function, prevents the overheated burning of material; Compatilizer mainly plays body material and filler generation block polymerization reaction, easily forms reticulated structure.
The present invention compared with prior art has following advantage:
(1) the present invention adopts sheet to mix mutually with body material with granular mineral filler, uses the various heat conductive fillers of different-grain diameter between filler, form maximum packing density, makes farthest on direction of heat flow, to form heat conduction network chain in system; Thus enhance the heat conductivility of material;
(2) the present invention adopts in the raw material mixed body material and mineral filler, then adds fire retardant, can prevent the too high product that causes of heat to burn danger on fire, greatly improve safety performance;
(3) after the present invention adopts and carries out preheating to body material and mineral filler at 60-80 DEG C, add compatilizer again, the consistency between each component in mixture can be improved, greatly improve molecule and interatomic association reaction speed, body material and filler are combined more fast and closely, thus the heat conductivility of strongthener;
(3) starting material of the present invention are easy to get, and composite material preparation process is simple, and cost is low, can save ample resources.
(4) the alternative metal heat-conducting goods of matrix material (radiator as LED) prepared of the present invention, are easy to injection moulding processing, are suitable for batch production.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of matrix material prepared by embodiment 1.
Embodiment
Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.Below in conjunction with accompanying drawing and example, the present invention is further illustrated.
A kind of LED high thermal conductivity matrix material, it is for following each component is through mixing, the nylon resin of 60-90wt.% is body material, the flaky inorganic filler of 5-30wt.% after coupling agent surface treatment and the mixing of powdered inorganic filler, the fire retardant of 2-10wt.% and the compatilizer of 0.5-2wt.%, described flaky inorganic filler is graphite, and described powdered inorganic filler is the mixing of one or more in silicon carbide, aluminium sesquioxide, magnesium oxide or aluminium nitride.
By such scheme, described nylon resin is granular PA66 or PA46, and its particle diameter is 1-5mm.
By such scheme, described graphite is sheet, and its diameter is 10-30 μm, and thickness is 1-5 μm.
By such scheme, described silicon carbide, aluminium sesquioxide, magnesium oxide or aluminium nitride are Powdered, and particle diameter is 10-100nm.
By such scheme, described coupling agent is silane coupling agent, aluminate coupling agent and titanate coupling agent.
By such scheme, described fire retardant is that high purity alumina-magnesia, Halogen or PA add fine type environmental protection fire retarding agent.
By such scheme, described compatilizer is the compatilizer of ring-type maleic anhydride (MAH) or glycidyl methacrylate (GMA) grafting.
The preparation method of described LED high thermal conductivity matrix material, is characterized in that: comprise the following steps:
1) adopt coupling agent to carry out surface treatment to flaky inorganic filler, being add flaky inorganic filler in body material with nylon resin, being placed in ball mill and mixing;
2) powdered inorganic filler and fire retardant are added step 1) in gained mixture, be again placed in ball mill and mix;
3) by step 2) in gained mixture when being preheated to 60-80 DEG C, add compatilizer, be again placed in ball mill and mix;
4) by step 3) raw material that mixes puts into twin-screw extrusion machine and carries out granulation, is packaged into bag; Wherein each component concentration is, the nylon resin of 60-90wt.% is body material, the flaky inorganic filler of 5-30wt.% after coupling agent treatment and the mixing of powdered inorganic filler, the fire retardant of 2-10wt.% and the compatilizer of 0.5-2wt.%.
Embodiment 1
Choose the granular nylon of 70% body material (PA46) and 20% flake graphite adopts silane coupling agent to carry out surface treatment 25 DEG C time, then insert in ball mill and carry out Homogeneous phase mixing; Then 5% heat conductive filler silicon carbide and 3% halogen-free flame retardants to be added in ball mill Homogeneous phase mixing again, test its flame retardant rating; Then after said mixture being heated to 70 DEG C, add 2% maleic anhydride (MAH) compatilizer, again mix in ball mill, test its heat conductivility and physical and mechanical properties, and its microtexture is analyzed (as shown in Figure 1); After 270 DEG C, carry out extruding pelletization finally by twin screw extruder, be cooled to normal temperature and pack, the concrete data of the physical function parameter of products obtained therefrom are as shown in table 1.
Table 1
Heat-conductive composite material performance index Parameter
Density (g/m 3) 1.35
Tensile strength (MaP) 90
Elongation at break (%) 2.8
Flexural strength (MaP) 160
Shock strength (GPa) 45
Thermal conductivity (W/m.K) 3.5
Heat-drawn wire (DEG C) 185
Resistivity (Ω .cm) 8.5×10 14
Flame retardant rating V0 level
Embodiment 2
Choose 75% body material nylon (PA66) and 15% flake graphite adopts titanate coupling agent to carry out surface treatment 25 DEG C time, then insert in ball mill and carry out Homogeneous phase mixing; Then 5% heat conductive filler silicon carbide and 2% high purity alumina-magnesia fire retardant to be added in ball mill Homogeneous phase mixing again, test its flame retardant rating; Then, after said mixture being heated to 80 DEG C, adding 3% glycidyl methacrylate (GMA) grafting compatilizer, again mix in ball mill, test its heat conductivility and physical and mechanical properties, and its microtexture is analyzed; After 275 DEG C, carry out extruding pelletization finally by twin screw extruder, be cooled to normal temperature and pack.
Embodiment 3
Choose 80% body material nylon (PA46) and 10% flake graphite adopts aluminate coupling agent to carry out surface treatment 25 DEG C time, then insert in ball mill and carry out Homogeneous phase mixing; Then 5% heat conductive filler silicon carbide and 4% high purity alumina-magnesia fire retardant to be added in ball mill Homogeneous phase mixing again, test its flame retardant rating; Then, after said mixture being heated to 80 DEG C, adding 1% maleic anhydride (MAH) compatilizer, again mix in ball mill, test its heat conductivility and physical and mechanical properties, and its microtexture is analyzed; After 280 DEG C, carry out extruding pelletization finally by twin screw extruder, be cooled to normal temperature and pack.
Embodiment 4
Choose 82% body material nylon (PA66) and 8% flake graphite adopts titanate coupling agent to carry out surface treatment 25 DEG C time, then insert in ball mill and carry out Homogeneous phase mixing; Then 5% heat conductive filler silicon carbide and 2% to be added in ball mill Homogeneous phase mixing again without halogenated flame retardant, test its flame retardant rating; Then, after said mixture being heated to 80 DEG C, adding 3% glycidyl methacrylate (GMA) grafting compatilizer, again mix in ball mill, test its heat conductivility and physical and mechanical properties, and its microtexture is analyzed; After 285 DEG C, carry out extruding pelletization finally by twin screw extruder, be cooled to normal temperature and pack.

Claims (8)

1. a LED high thermal conductivity matrix material, it is for following each component is through mixing, the nylon resin of 60-90wt.% is body material, the flaky inorganic filler of 5-30wt.% after coupling agent surface treatment and the mixing of powdered inorganic filler, the fire retardant of 2-10wt.% and the compatilizer of 0.5-2wt.%, described flaky inorganic filler is graphite, and described powdered inorganic filler is the mixing of one or more in silicon carbide, aluminium sesquioxide, magnesium oxide or aluminium nitride.
2. LED high thermal conductivity matrix material according to claim 1, it is characterized in that: described nylon resin is granular PA66 or PA46, its particle diameter is 1-5mm.
3. LED high thermal conductivity matrix material according to claim 1, it is characterized in that: described graphite is sheet, its diameter is 10-30 μm, and thickness is 1-5 μm.
4. LED high thermal conductivity matrix material according to claim 1, it is characterized in that: described silicon carbide, aluminium sesquioxide, magnesium oxide or aluminium nitride are Powdered, particle diameter is 10-100nm.
5. LED high thermal conductivity matrix material according to claim 1, is characterized in that: described coupling agent is silane coupling agent, aluminate coupling agent and titanate coupling agent.
6. LED high thermal conductivity matrix material according to claim 1, is characterized in that: described fire retardant is that high purity alumina-magnesia, Halogen or PA add fine type environmental protection fire retarding agent.
7. LED high thermal conductivity matrix material according to claim 1, is characterized in that: described compatilizer is the compatilizer of ring-type maleic anhydride or glycidyl methacrylate graft.
8. the preparation method of the LED high thermal conductivity matrix material described in any one of claim 1-7, is characterized in that: comprise the following steps:
1) adopt coupling agent and surface treatment agent to carry out surface treatment to flaky inorganic filler, being add flaky inorganic filler in body material with nylon resin, being placed in ball mill and mixing;
2) powdered inorganic filler and fire retardant are added step 1) in gained mixture, be again placed in ball mill and mix;
3) by step 2) in gained mixture when being preheated to 60-80 DEG C, add compatilizer, be again placed in ball mill and mix;
4) by step 3) raw material that mixes puts into twin-screw extrusion machine and carries out granulation, is packaged into bag; Wherein each component concentration is: the nylon resin of 60-90wt.% is body material, the flaky inorganic filler of 5-30wt.% after coupling agent surface treatment and the mixing of powdered inorganic filler, the fire retardant of 2-10wt.% and the compatilizer of 0.5-2wt.%.
CN201510220412.0A 2015-05-04 2015-05-04 LED (light-emitting diode) high-thermal-conductivity composite material and preparation method thereof Pending CN104788951A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295360A (en) * 2015-10-10 2016-02-03 惠州市沃特新材料有限公司 High thermal conductivity flame-retardant nylon composite material and preparation method thereof
CN106046779A (en) * 2016-07-05 2016-10-26 河南神马华威塑胶股份有限公司 Flame-retardant nylon composite material with good abrasion resistance and high heat conductivity coefficient and method for preparing flame-retardant nylon composite material
CN106800775A (en) * 2016-12-21 2017-06-06 马鞍山瑞美塑业有限公司 A kind of dehumidifier steeps the preparation method of cabinet with insulated water proof
CN109280378A (en) * 2018-10-17 2019-01-29 横店集团得邦工程塑料有限公司 A kind of heat conductive insulating type fiberglass reinforced fire retardant PA66 and preparation method thereof
CN109438984A (en) * 2018-11-08 2019-03-08 武汉轻工大学 A kind of heat-conductive composite material and preparation method thereof
CN109553963A (en) * 2018-10-30 2019-04-02 广东格瑞新材料股份有限公司 A kind of heat sink material and preparation method thereof
CN112352997A (en) * 2020-12-03 2021-02-12 湖北中烟工业有限责任公司 Preparation method for heating non-burning tobacco products by optimized rolling method

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US20110281051A1 (en) * 2008-11-27 2011-11-17 Arkema France Use of an expanded graphite in a polymer material
CN102719099A (en) * 2012-06-08 2012-10-10 金发科技股份有限公司 Thermal conductive molding compound and preparation method thereof
CN102786800A (en) * 2012-08-01 2012-11-21 张建滨 Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material
CN103044904A (en) * 2012-12-27 2013-04-17 安徽科聚新材料有限公司 Special heat-conducting and insulating material for LED (light-emitting diode) lamp holder and preparation method thereof
CN103602060A (en) * 2013-11-06 2014-02-26 上海大学 Heat-conducting, wear-resistant and insulated nylon 6 composite material and preparation method thereof
CN104371318A (en) * 2014-11-19 2015-02-25 上海大学 Polyamide composite material with high thermal conductivity and high heat resistance and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110281051A1 (en) * 2008-11-27 2011-11-17 Arkema France Use of an expanded graphite in a polymer material
CN102719099A (en) * 2012-06-08 2012-10-10 金发科技股份有限公司 Thermal conductive molding compound and preparation method thereof
CN102786800A (en) * 2012-08-01 2012-11-21 张建滨 Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material
CN103044904A (en) * 2012-12-27 2013-04-17 安徽科聚新材料有限公司 Special heat-conducting and insulating material for LED (light-emitting diode) lamp holder and preparation method thereof
CN103602060A (en) * 2013-11-06 2014-02-26 上海大学 Heat-conducting, wear-resistant and insulated nylon 6 composite material and preparation method thereof
CN104371318A (en) * 2014-11-19 2015-02-25 上海大学 Polyamide composite material with high thermal conductivity and high heat resistance and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295360A (en) * 2015-10-10 2016-02-03 惠州市沃特新材料有限公司 High thermal conductivity flame-retardant nylon composite material and preparation method thereof
CN105295360B (en) * 2015-10-10 2018-06-29 惠州市沃特新材料有限公司 High heat conduction fire-retardant nylon composite material and preparation method thereof
CN106046779A (en) * 2016-07-05 2016-10-26 河南神马华威塑胶股份有限公司 Flame-retardant nylon composite material with good abrasion resistance and high heat conductivity coefficient and method for preparing flame-retardant nylon composite material
CN106800775A (en) * 2016-12-21 2017-06-06 马鞍山瑞美塑业有限公司 A kind of dehumidifier steeps the preparation method of cabinet with insulated water proof
CN109280378A (en) * 2018-10-17 2019-01-29 横店集团得邦工程塑料有限公司 A kind of heat conductive insulating type fiberglass reinforced fire retardant PA66 and preparation method thereof
CN109553963A (en) * 2018-10-30 2019-04-02 广东格瑞新材料股份有限公司 A kind of heat sink material and preparation method thereof
CN109553963B (en) * 2018-10-30 2021-03-05 广东格瑞新材料股份有限公司 Heat dissipation material and preparation method thereof
CN109438984A (en) * 2018-11-08 2019-03-08 武汉轻工大学 A kind of heat-conductive composite material and preparation method thereof
CN112352997A (en) * 2020-12-03 2021-02-12 湖北中烟工业有限责任公司 Preparation method for heating non-burning tobacco products by optimized rolling method

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Application publication date: 20150722