CN102796372B - Laser-direct-structuring high-thermal-conductivity insulated polyamide 66 composition used for LED (Light Emitting Diode) light source substrate and preparation method of composition - Google Patents
Laser-direct-structuring high-thermal-conductivity insulated polyamide 66 composition used for LED (Light Emitting Diode) light source substrate and preparation method of composition Download PDFInfo
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Abstract
The invention discloses a laser-direct-structuring high-thermal-conductivity insulated polyamide 66 composition used for an LED (Light Emitting Diode) light source substrate and a preparation method of the composition, and the polyamide 66 composition has the advantages of high thermal conductivity, laser direct structuring, excellent insulating property, chemical resistance, corrosion and the like. The composition disclosed by the invention is prepared from the following raw materials according to parts by weight: 40-70 parts of polyamide 66, 5-35 parts of heat conducting agent, 5-8 parts of inorganic pigment, 0.15 part of antioxidant A, 0.15 part of antioxidant B, 0.5 part of lubricating agent and 0.3 part of coupling agent. The polyamide 66 composition provided by the invention has the advantages of light weight, easy forming, flexible circuit design, simple technology and the like, and has excellent high-temperature electrical insulating property.
Description
Technical field
The present invention relates to a kind of high heat conduction polyamide 66 composition for LED lamp plate, more specifically, relate to a kind ofly for LED lamp plate, having can laser direct forming, the polyamide 66 composition of excellent heat conductivity, high-insulativity.
Background technology
Anxious scarce in global energy, under the background of resource anxiety, this situation will be effectively alleviated in the appearance of LED light source, LED light source, as light source of new generation, with respect to existing light source, has energy-saving and environmental protection, the features such as the life-span is longer, be acknowledged as lighting engineering of future generation, popularization is all being done one's utmost by national governments, and it replaces existing various light sources (comprising electricity-saving lamp) is trend of the times.For LED light source, no matter be substrate or shell, it is crucial solving heat dissipation problem, and the substrate of LED light source mainly contains aluminium base and the large class of ceramic substrate two at present, and aluminium base is made up of circuit layer (copper foil layer), heat conductive insulating layer and metal-based layer.
High heat conductive insulating layer is the technology of aluminium base core.Determine whole aluminium base heat conductivility.It is generally that the special polymkeric substance of being filled by special cermacis forms, and aluminium base exists that cost is high, complex process, electrical insulation capability are poor;
Ceramic substrate refers to that Copper Foil is at high temperature bonded directly to aluminum oxide (Al
2o
3) or aluminium nitride (AlN) ceramic substrate surface (single or double) on special process plate.Ceramic substrate exists and wants that high temperature sintering moulding, quality are large, complex process, expensive, bad mechanical property, the shortcoming such as frangible, therefore adopt injection moldable and polyamide 66 (PA66) composition that can laser direct forming substitute a kind of new solution to LED light source substrate be provided.The advantage of this novel heat sink material is: the advantage such as light weight, easy-formation, electrical insulation capability, chemicals-resistant and corrosion that circuit layout is flexible, high.
Summary of the invention
The present invention be directed to the deficiencies in the prior art, object is to provide a kind of substrate for LED light source, have excellent heat conducting rate, can laser direct forming, polyamide 66 (PA66) composition and method of making the same of high-insulativity.Compare thermally conductive polyamides 66(PA66 that can laser direct forming with ceramic substrate composition with common aluminium base of the prior art) composition advantage is: the advantage such as light weight, easy-formation, electrical insulation capability, chemicals-resistant and corrosion that circuit layout is flexible, high.
For achieving the above object, the present invention adopts following scheme:
For LED light source substrate can laser direct forming a high heat conductive insulating polyamide 66 composition, said composition is prepared from by the raw material of following weight part:
In some embodiment, described thermal conducting agent is boron nitride powder (BET), at least 10m of its specific surface area therein
2/ g, preferred specific surface area is 13m
2/ g to 15m
2/ g, described BET specific surface area is measured according to ASTMD3037.
In some embodiment, described thermal conducting agent is boron nitride powder therein, at least 150um of its particle diameter, and preferred particle diameter is 170um to 190um, the particle size distribution being characterized by D (v, 0.9).
In some embodiment, the particle size distribution of described boron nitride powder has following feature therein: volume median diameter D (v, 0.5) is 45um at least, and volume median diameter D (v, 0.5) is preferably at least 50um to 55um.
Therein in some embodiment, the particle size distribution of described boron nitride powder also has following characteristics: D (v, 0.1) for 3um at least, is preferably at least 4um to 7um; Boron nitride powder has following particle size distribution, this particle size distribution with the D of 7um (v, 0.1) at least, at least the volume median diameter D of 55um (v, 0.5) and at least the D of 190um (v, 0.9) for feature.Particle size is not entangled in the specific upper limit, but it is subject to the long-pending restriction of required minimum specific surface in practice.Minimum specific surface is long-pending larger, and particle is conventionally less, and the overall dimension of particle is also less.
D (v, 0.1), D (v, 0.5), D (v, 0.9) adopt Malvern Mastersizer to pass through determination of laser diffraction.
In some embodiment, described thermal conducting agent boron nitride powder density is at 2.0～2.5g/cm therein
3between, preferably at 2.1～2.4g/cm
3between and 2.20～2.28g/cm
3between.
The feature of the present invention's boron nitride powder used has singularity, in the time being used as heat conductive filler, and common boron nitride powder relatively at present, in the time reaching equal thermal conductivity, usage quantity is lower.Such as: for obtaining the composition that is applicable to parallel conductive heating rate numerical value (5～15W/mk) in the face of LED light source heat abstractor, to the 25～35wt% that adds the gross weight based on composition in composition; The boron nitride powder using in the present invention just can reach, but need to use in order to obtain equal thermal conductivity the common boron nitride filler that exceedes 50wt%.Because amount of filler is lower, composition of the present invention has better mechanical property.
The present invention's boron nitride powder used has good high-temperature electric insulativity, and surface resistivity is 10 at 25 DEG C
14Ω cm, 2000 DEG C just reach 10
3Ω cm, is high-temperature electric insulating material best in pottery, and voltage breakdown 3kv/mm is 2.5 × 10 when low-dielectric loss 108Hz
-4, specific inductivity is 4.Therefore thermally conductive composition of the present invention has good high-temperature electric insulativity.
In some embodiment, described mineral dye is LDS additive therein.Make polyamide 66 (PA66) composition can be used in laser direct forming.In laser direct forming technique, described mineral dye, with after laser radiation, can discharge metal simple-substance, the reductive agent during as electroless copper, the deposition of catalytic copper metal.
In some embodiment, described mineral dye is metal oxide hybrid pigment therein, has spinel structure or structure relevant to spinel as cupric and chromic oxide spinel; Generated through high temperature solid state reaction by Multimetal oxide, the metallic element in metal oxide is one or more in Cu, Cr, Ag, Au, Ni, Ti, Cr, Co, Mn, Ce, Nb, Fe.Described metal oxide mixes the powder density of face at 4.5～5.8g/cm
3between, preferably at 4.8～5.6g/cm
3between, further preferably at 4.9～5.4g/cm
3between.The particle diameter of described metal oxide hybrid pigment is 0.1～30 μ m, is preferably 1～8 μ m; Described metal oxide hybrid pigment oil number is 5～40g/100g, is preferably 10～30g/100g.
In some embodiment, described coupling agent is silane coupling agent, titanate coupling agent or aluminate coupling agent, is preferably silane coupling agent therein, uses β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane.
In some embodiment, described lubricant is ethylene bis-fatty acid amides therein.
In some embodiment, described oxidation inhibitor A is Hinered phenols antioxidant, is specially therein: β-(4-hydroxy phenyl-3,5-di-t-butyl) propionic acid octadecyl ester.
In some embodiment, described oxidation inhibitor B is phosphite ester kind antioxidant, is specially therein: three (2,4-di-tert-butyl-phenyl) phosphorous acid ester.
In order to realize object of the present invention, the invention provides a kind of substrate for LED light source can laser direct forming the preparation method of high heat conduction polyamide 66 composition, comprise the following steps:
1) by the polyamide 66 of above-mentioned weight part (PA66) raw material at 110～130 DEG C, through 3～5 hours drying treatment;
2) in the first mixing machine, add mineral dye, lubricant, oxidation inhibitor A, the oxidation inhibitor B of dried polyamide 66 (PA66) and above-mentioned weight part, high-speed mixing 5～20 minutes, obtains premix;
3) in the second mixing machine, add the thermal conducting agent boron nitride powder of above-mentioned weight part, then limit adds the silane coupling agent limit stirring at low speed 1～10 minute of above-mentioned weight part, allows silane coupling agent fully wrap boron nitride, obtains mixture;
4) described premix step (2) being mixed adds in parallel double-screw extruder through feeder, and add the mixed described mixture of step (3) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 160～200rpm, another tetra-district He six district's dress venting ports;
Technique is as follows: 260～270 DEG C of parallel double-screw extruder one district's temperature, two 270～280 DEG C of district's temperature, three 270～280 DEG C of district's temperature, four 270～280 DEG C of district's temperature, five 270～280 DEG C of district's temperature, six 270～280 DEG C of district's temperature, seven 270～280 DEG C of district's temperature, eight 270～280 DEG C of district's temperature, nine 270～280 DEG C of district's temperature, 270～280 DEG C of die head temperatures, screw speed is 200～300rpm, material residence time in extruder barrel is controlled at 1～3 minute;
5) material that step (4) obtained is through tie rod, cooling, pelletizing, drying treatment.
In some embodiment, the screw rod of described parallel double-screw extruder has more than one gear block district therein, and the screw rod of parallel double-screw extruder has more than one left-hand thread district.
In some embodiment, the screw rod of described parallel double-screw extruder is shaped as single thread therein, and the ratio L/D of spiro rod length L and diameter D is 20～60.
Provided by the present invention for LED light source substrate can laser direct forming high heat conduction polyamide 66 composition have the following advantages:
The advantages such as 1, polyamide 66 composition of the present invention has light weight, easy-formation, circuit layout is flexible, technique is simple.
2, the present invention's boron nitride powder used has just been given the thermal conductivity that thermoplastic compounds is relatively high in the time being used as heat conductive filler under relatively low filler weight percentage.Because amount of filler is lower, so heat conductivity composition of the present invention has better mechanical property and mechanical property compared with modal heat conductivity composition (needing mass filler in order to obtain rational conductivity values).
3, polyamide 66 composition of the present invention provides a kind of novel heat sink material to LED light source substrate, also can be used for laser direct structuring technique, the bonding force good with having of metal plating simultaneously.
4, the green polyamide 66 composition of heat conduction of the present invention has good high-temperature electric insulativity.
Embodiment
For further understanding feature of the present invention, technique means and the specific purposes that reach, function, resolve the advantages and spirit of the present invention, by following embodiment, detailed description of the present invention is further understood.
The raw material that the embodiment of the present invention is used is as follows:
Polyamide 66 (PA66) is purchased from the first promise of the U.S.; The trade mark is 50BWFS;
Mineral dye is metal oxide hybrid pigment, and purchased from Hunan Ke Le pigment company limited, its density is 4.9～5.4g/cm
3, particle diameter is 1～8 μ m, oil number is 10～30g/100g;
Boron nitride powder BN100 has following particle size distribution, and this particle size distribution is with the D of 7um (v, 0.1) at least, at least volume median diameter D of 55um (v, 0.5), and at least the D of 190um (v, 0.9) is feature; Purchased from the brilliant hundred million ceramics company limiteds in Zibo;
Lubricant is purchased from photochemistry auxiliary agent company limited of Suzhou Xingtai state, and the trade mark is TAF;
β-(4-hydroxy phenyl-3,5-di-t-butyl) propionic acid octadecyl ester adopts Switzerland vapour bar IRGANOX 1076;
Three (2,4-di-tert-butyl-phenyl) phosphorous acid ester adopts Switzerland vapour bar IRGANOX 168;
β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane adopts the U.S. to step figure A-186.
The present invention is further elaborated by the following examples.
Embodiment 1:
1) prepare raw material by the formula of following weight part: 66.9 parts of polyamide 66s (PA66), 25 parts of boron nitride powder BN100,7 parts of mineral dyes, 0.15 part of oxidation inhibitor A, 0.15 part of oxidation inhibitor B, 0.5 part of lubricant, 0.3 part of coupling agent;
2) by polyamide 66 (PA66) raw material through 120 DEG C, 3 hours drying treatment;
3) in mixing machine 1, add dried polyamide 66 (PA66), mineral dye, oxidation inhibitor A, oxidation inhibitor B, high-speed mixing 10 minutes;
4) in mixing machine 2, add boron nitride BN100, then limit adds coupling agent limit stirring at low speed 4 minutes, allows coupling agent fully wrap boron nitride BN100;
5) premix step (3) being mixed adds in parallel double-screw extruder through feeder, and add the mixed mixture of step (4) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 180rpm, another tetra-district He six district's dress venting ports.Complete processing is as follows: 260 DEG C of parallel double-screw extruder one district's temperature, two 270 DEG C of district's temperature, three 270 DEG C of district's temperature, four 270 DEG C of district's temperature, five 270 DEG C of district's temperature, six 270 DEG C of district's temperature, seven 270 DEG C of district's temperature, eight 280 DEG C of district's temperature, nine 280 DEG C of district's temperature, 280 DEG C of die head temperatures, screw speed is 250rpm, material residence time in extruder barrel is controlled at 2 minutes.
6) material that step (5) obtained is through tie rod, cooling, pelletizing, drying treatment.
Embodiment 2:
1) prepare raw material by the formula of following weight part: 61.9 parts of polyamide 66s (PA66), 30 parts of boron nitride powder BN100,7 parts of mineral dyes, 0.15 part of oxidation inhibitor A, 0.15 part of oxidation inhibitor B, 0.5 part of lubricant, 0.3 part of coupling agent;
2) by polyamide 66 (PA66) raw material through 120 DEG C, 3 hours drying treatment;
3) in mixing machine 1, add dried polyamide 66 (PA66), mineral dye, oxidation inhibitor A, oxidation inhibitor B, high-speed mixing 10 minutes;
4) in mixing machine 2, add boron nitride BN100, then limit adds coupling agent limit stirring at low speed 4 minutes, allows coupling agent fully wrap boron nitride BN100;
5) premix step (3) being mixed adds in parallel double-screw extruder through feeder, and add the mixed mixture of step (4) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 180rpm, another tetra-district He six district's dress venting ports.Complete processing is as follows: 260 DEG C of parallel double-screw extruder one district's temperature, two 270 DEG C of district's temperature, three 270 DEG C of district's temperature, four 270 DEG C of district's temperature, five 270 DEG C of district's temperature, six 270 DEG C of district's temperature, seven 270 DEG C of district's temperature, eight 280 DEG C of district's temperature, nine 280 DEG C of district's temperature, 280 DEG C of die head temperatures, screw speed is 250rpm, material residence time in extruder barrel is controlled at 2 minutes;
6) material that step (5) obtained is through tie rod, cooling, pelletizing, drying treatment.
Embodiment 3:
1) prepare raw material by the formula of following weight part: 56.9 parts of polyamide 66s (PA66), 35 parts of boron nitride powder BN100,7 parts of mineral dyes, 0.15 part of oxidation inhibitor A, 0.15 part of oxidation inhibitor B, 0.5 part of lubricant, 0.3 part of coupling agent;
2) by polyamide 66 (PA66) raw material through 120 DEG C, 3 hours drying treatment;
3) in mixing machine 1, add dried polyamide 66 (PA66), mineral dye, oxidation inhibitor A, oxidation inhibitor B, high-speed mixing 10 minutes;
4) in mixing machine 2, add boron nitride BN100, then limit adds coupling agent limit stirring at low speed 4 minutes, allows coupling agent fully wrap boron nitride BN100;
5) premix step (3) being mixed adds in parallel double-screw extruder through feeder, and add the mixed mixture of step (4) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 180rpm, another tetra-district He six district's dress venting ports.Complete processing is as follows: 260 DEG C of parallel double-screw extruder one district's temperature, two 270 DEG C of district's temperature, three 270 DEG C of district's temperature, four 270 DEG C of district's temperature, five 270 DEG C of district's temperature, six 270 DEG C of district's temperature, seven 270 DEG C of district's temperature, eight 280 DEG C of district's temperature, nine 280 DEG C of district's temperature, 280 DEG C of die head temperatures, screw speed is 250rpm, material residence time in extruder barrel is controlled at 2 minutes;
6) material that step (5) obtained is through tie rod, cooling, pelletizing, drying treatment.
Embodiment 4:
1) prepare raw material by the formula of following weight part: 58.9 parts of polyamide 66s (PA66), 35 parts of boron nitride powder BN100,5 parts of mineral dyes, 0.15 part of oxidation inhibitor A, 0.15 part of oxidation inhibitor B, 0.5 part of lubricant, 0.3 part of coupling agent;
2) by polyamide 66 (PA66) raw material through 120 DEG C, 3 hours drying treatment;
3) in mixing machine 1, add dried polyamide 66 (PA66), mineral dye, oxidation inhibitor A, oxidation inhibitor B, high-speed mixing 10 minutes;
4) in mixing machine 2, add boron nitride BN100, then limit adds coupling agent limit stirring at low speed 4 minutes, allows coupling agent fully wrap boron nitride BN100;
5) premix step (3) being mixed adds in parallel double-screw extruder through feeder, and add the mixed mixture of step (4) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 180rpm, another tetra-district He six district's dress venting ports.Complete processing is as follows: 260 DEG C of parallel double-screw extruder one district's temperature, two 270 DEG C of district's temperature, three 270 DEG C of district's temperature, four 270 DEG C of district's temperature, five 270 DEG C of district's temperature, six 270 DEG C of district's temperature, seven 270 DEG C of district's temperature, eight 280 DEG C of district's temperature, nine 280 DEG C of district's temperature, 280 DEG C of die head temperatures, screw speed is 250rpm, material residence time in extruder barrel is controlled at 2 minutes;
6) material that step (5) obtained is through tie rod, cooling, pelletizing, drying treatment.
Embodiment 5:
1) prepare raw material by the formula of following weight part: 55.9 parts of polyamide 66s (PA66), 35 parts of boron nitride powder BN100,8 parts of mineral dyes, 0.15 part of oxidation inhibitor A, 0.15 part of oxidation inhibitor B, 0.5 part of lubricant, 0.3 part of coupling agent;
2) by polyamide 66 (PA66) raw material through 120 DEG C, 3 hours drying treatment;
3) in mixing machine 1, add dried polyamide 66 (PA66), mineral dye, oxidation inhibitor A, oxidation inhibitor B, high-speed mixing 10 minutes;
4) in mixing machine 2, add boron nitride BN100, then limit adds coupling agent limit stirring at low speed 4 minutes, allows coupling agent fully wrap boron nitride BN100;
5) premix step (3) being mixed adds in parallel double-screw extruder through feeder, and add the mixed mixture of step (4) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 180rpm, another tetra-district He six district's dress venting ports.Complete processing is as follows: 260 DEG C of parallel double-screw extruder one district's temperature, two 270 DEG C of district's temperature, three 270 DEG C of district's temperature, four 270 DEG C of district's temperature, five 270 DEG C of district's temperature, six 270 DEG C of district's temperature, seven 270 DEG C of district's temperature, eight 280 DEG C of district's temperature, nine 280 DEG C of district's temperature, 280 DEG C of die head temperatures, screw speed is 250rpm, material residence time in extruder barrel is controlled at 2 minutes;
6) material that step (5) obtained is through tie rod, cooling, pelletizing, drying treatment.
Comparative example 1:
1) prepare raw material by the formula of following weight part: 68.9 parts of polyamide 66s (PA66), 30 parts of boron nitride powder BN100,0.15 part of oxidation inhibitor A, 0.15 part of oxidation inhibitor B, 0.5 part of lubricant, 0.3 part of coupling agent;
2) by polyamide 66 (PA66) raw material through 120 DEG C, 3 hours drying treatment;
3) in mixing machine 1, add dried polyamide 66 (PA66), mineral dye, oxidation inhibitor A, oxidation inhibitor B, high-speed mixing 10 minutes;
4) in mixing machine 2, add boron nitride BN100, then limit adds coupling agent limit stirring at low speed 4 minutes, allows coupling agent fully wrap boron nitride BN100;
5) premix step (3) being mixed adds in parallel double-screw extruder through feeder, and add the mixed mixture of step (4) in the side direction (Si district) in parallel double-screw extruder (Gong Jiu district), above-mentioned feeder rotating speed is 180rpm, another tetra-district He six district's dress venting ports.Complete processing is as follows: 260 DEG C of parallel double-screw extruder one district's temperature, two 270 DEG C of district's temperature, three 270 DEG C of district's temperature, four 270 DEG C of district's temperature, five 270 DEG C of district's temperature, six 270 DEG C of district's temperature, seven 270 DEG C of district's temperature, eight 280 DEG C of district's temperature, nine 280 DEG C of district's temperature, 280 DEG C of die head temperatures, screw speed is 250rpm, material residence time in extruder barrel is controlled at 2 minutes;
6) material that step (5) obtained is through tie rod, cooling, pelletizing, drying treatment.
The plastic component that polyamide 66 (PA66) the composition injection molding that the various embodiments described above and comparative example are obtained is definite shape.Use according to conventional methods wavelength 900～1080nm, energy 150～300mJ/cm
2laser carries out laser ablation to the prospective region of above-mentioned plastic component according to setting shape under the scanning speed of 0.1～1mm/s, carries out electroless plating through the plastic component of laser ablation, forms metal plating in the laser ablation district of described plastic component.
Made above-mentioned each example plastic component sample is carried out to following performance test (result is as shown in table 1):
Tensile property: press ASTM-D638 standard testing, rate of extension 50mm/min;
Impact property: press ASTM-D256 standard testing, batten thickness is 3.2mm;
Bending property: press ASTM-D790 standard testing, bending speed 10mm/min;
Plastic component surface metal plating layer sticking power test (hundred lattice tests): press ASTM D3359 standard testing.
23 ± 2 DEG C of room temperatures, under the condition of relative humidity 50 ± 5%, draw 10 × 10 little grids of 1mm × 1mm with sharp cutter (knife edge angle is 15 °～30 °) in test sample surface, each is rule deeply and coating bottom; Hairbrush cleans down test zone; Firmly cling tested little grid with 3M600 adhesive tape, and with the eraser wiping adhesive tape of exerting oneself, to strengthen contact area and the dynamics in adhesive tape and tested region; Catch adhesive tape one end with hand, shut down rapidly gummed paper in the vertical direction with 60 ° of angles, same position carries out same test 2 times.
Result is judged: while requiring sticking power >=4B as qualified.
5B-scribing edge is smooth, line edge and point of crossing place all without peeling paint;
4B-has the peeling paint of small pieces at the point of crossing place of line, and the total area that comes off is less than 5%;
3B-has the peeling paint of small pieces at edge and the point of crossing place of line, and comes off the total area between 5%～15%;
2B-has peeling paint in blocks at edge and the point of crossing place of line, and comes off the total area between 15%～35%;
1B-has peeling paint in blocks at edge and the point of crossing place of line, and comes off the total area between 35%～65%;
0B-has peeling paint in blocks at edge and the point of crossing place of line, and the total area that comes off is greater than 65%.
Table 1: embodiment 1～5 and comparative example the performance test results
As seen from the above table, high heat conduction polyamide 66 (PA66) composition (embodiment 1, embodiment 2 and embodiment 3) that can laser direct forming of the present invention has the mechanical property that high conduction values is become reconciled in the time of relatively low amount of filler, and thermal conductive polymer composite of the present invention also has good high-temperature electric insulativity simultaneously.Therefore thermal conductive polymer composite of the present invention has high thermal conductivity, excellent high-temperature insulating quality and good mechanical property.
As seen from the above table, high heat conduction polyamide 66 (PA66) composition (embodiment 3,4,5 and comparative example 1) that can laser direct forming of the present invention is adding after mineral dye, there is fine sticking power with metal plating, in embodiment 3, sticking power can reach 5B, simultaneously of the present invention can laser direct forming composition also there is good thermotolerance and good mechanical property.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (6)
- For LED light source substrate can laser direct forming a high heat conductive insulating polyamide 66 composition, it is characterized in that, said composition is prepared from by the raw material of following weight part:40～70 parts of polyamide 66s;25～35 parts of boron nitride;5～8 parts, cupric and chromic oxide spinel;0.15 part of oxidation inhibitor A;0.15 part of oxidation inhibitor B;0.5 part of lubricant;0.3 part of coupling agent;The particle size distribution of described boron nitride powder has following feature: volume median diameter D (v, 0.5) is 45um at least; At least 3um of D (v, 0.1); At least 150um of D (v, 0.9);Described oxidation inhibitor A is Hinered phenols antioxidant;Described oxidation inhibitor B is phosphite ester kind antioxidant;Described coupling agent is silane coupling agent, titanate coupling agent or aluminate coupling agent;Described lubricant is ethylene bis-fatty acid amides.
- According to claim 1 for LED light source substrate can laser direct forming high heat conductive insulating polyamide 66 composition, it is characterized in that, described Hinered phenols antioxidant is β-(4-hydroxy phenyl-3,5-di-t-butyl) propionic acid octadecyl ester; Described phosphite ester kind antioxidant is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester.
- According to claim 1 for LED light source substrate can laser direct forming high heat conductive insulating polyamide 66 composition, it is characterized in that, described coupling agent is β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane.
- 4. prepare described in claim 1～3 any one for LED light source substrate can laser direct forming the method for high heat conductive insulating polyamide 66 composition, it is characterized in that, comprise the following steps:1., by the polyamide 66 raw material of described weight part at 110～130 DEG C, through 3～5 hours drying treatment;2., in the first mixing machine, add cupric and chromic oxide spinel, lubricant, oxidation inhibitor A, the oxidation inhibitor B of dried polyamide 66 and described weight part, high-speed mixing 5～20 minutes, obtains premix;3., in the second mixing machine, add the thermal conducting agent boron nitride powder of described weight part, then limit adds the silane coupling agent of described weight part, stirring at low speed 1～10 minute for limit, allows silane coupling agent fully wrap boron nitride, obtains mixture;4. the described premix, 2. step being mixed adds in parallel double-screw extruder through feeder, and parallel double-screw extruder tetra-district's side direction in Gong 9th district add 3. mixed described mixture of step, above-mentioned feeder rotating speed is 160～200rpm, another tetra-district He six district's dress venting ports;Described parallel double-screw extruder complete processing is as follows:Described parallel double-screw extruder is provided with nine temperature controlled region, wherein, and 260～270 DEG C of district's temperature, two 270～280 DEG C of district's temperature, three 270～280 DEG C of district's temperature, four 270～280 DEG C of district's temperature, five 270～280 DEG C of district's temperature, six 270～280 DEG C of district's temperature, seven 270～280 DEG C of district's temperature, eight 270～280 DEG C of district's temperature, nine 270～280 DEG C of district's temperature, 270～280 DEG C of die head temperatures, screw speed is 200～300rpm, material residence time in extruder barrel is controlled at 1～3 minute;5., material that 4. step is obtained is through tie rod, cooling, pelletizing, drying treatment, to obtain final product.
- 5. preparation method according to claim 4, is characterized in that, the screw rod of described parallel double-screw extruder has more than one gear block district, and the screw rod of described parallel double-screw extruder has more than one left-hand thread district.
- 6. preparation method according to claim 4, is characterized in that, the screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 20～60.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210273668.4A CN102796372B (en) | 2012-08-01 | 2012-08-01 | Laser-direct-structuring high-thermal-conductivity insulated polyamide 66 composition used for LED (Light Emitting Diode) light source substrate and preparation method of composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210273668.4A CN102796372B (en) | 2012-08-01 | 2012-08-01 | Laser-direct-structuring high-thermal-conductivity insulated polyamide 66 composition used for LED (Light Emitting Diode) light source substrate and preparation method of composition |
Publications (2)
| Publication Number | Publication Date |
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| CN102796372A CN102796372A (en) | 2012-11-28 |
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| WO2016057418A1 (en) * | 2014-10-07 | 2016-04-14 | Polyone Corporation | Thermally conductive polymer articles for electronic circuitry |
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