CN102719099A - Thermal conductive molding compound and preparation method thereof - Google Patents
Thermal conductive molding compound and preparation method thereof Download PDFInfo
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- CN102719099A CN102719099A CN2012101879553A CN201210187955A CN102719099A CN 102719099 A CN102719099 A CN 102719099A CN 2012101879553 A CN2012101879553 A CN 2012101879553A CN 201210187955 A CN201210187955 A CN 201210187955A CN 102719099 A CN102719099 A CN 102719099A
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Abstract
The invention discloses a thermal conductive molding compound and a preparation method thereof. The thermal conductive molding compound consists of the following components by weight percent: 15-40% of thermal conductive filler A, 10-30% of thermal conductive filler B, 1-5% of thermal conductive filler C, 5-15% of reinforcing component, 0.05-0.5% of surface modifier and 0-2% of other additives. The preparation method comprises the following steps: adding the thermal conductive filler B in a mixer, adding the surface modifier for mixing, and then adding the thermal conductive filler C for further mixing to obtain a mixture I; adding the thermal conductive filler A in a high-speed mixer, and adding the surface modifier for mixing to obtain a mixture II; after uniformly mixing a plastic matrix with other additives, adding the mixture of the plastic matrix and other additives from the main feeding port of a twin-screw extruder; adding the mixture I and the mixture II from the main feeding port or a feeding port on one side downstream of the extruder; independently adding the reinforcing component from a feeding port on the other side downstream of the extruder; and obtaining the thermal conductive molding compound from the twin-screw extruder. The thermal conductive molding compound has excellent thermal conductivity and good mechanical property.
Description
Technical field
The present invention relates to the functional high molecule material technical field, specifically, relate to a kind of heat conduction moulding compound and preparation method thereof.
Background technology
Along with microelectronics integrated technology and package technique high speed development, packing density improves rapidly, electronic component; Thousands of times of ground of logical circuit volume dwindle; The frivolous day by day miniaturized of electronic machine, and operating frequency sharply increases, the semiconductor heat environment changes rapidly to the high temperature direction.Heat run-up that electronics produced this moment, under the environment for use temperature, to make electronic devices and components still can high reliability works better expeditiously, in time heat-sinking capability becomes the critical limitation in its work-ing life factor that influences.Though traditional pottery or heat dissipation metal material have better heat radiating effect, several big defectives of its inherent have seriously limited their development, comprise that mainly density is big, difficult forming, and structure design is limited etc.The heat-conducting polymer matrix material of the excellent combination property of high reliability high-cooling property has well remedied the defective of traditional heat-dissipating material, as hot interface and packaged material, is substituting pottery and metal gradually, becomes the first-selection in heat radiation field.
In the prior art, the thinking major part of preparation polymer-based carbon thermally conductive material is the method for adding the high-content heat conductive filler that in polymeric matrix, adopts.Though this method can obtain the pretty good material of heat conductivility, high filler loading capacity often brings some serious problems, obviously descends like the mechanical property of material, especially toughness; Density of material is too big, influences its application; The product surface ratio is more coarse, and is not attractive in appearance; High in addition infill system is for the reinforced of processing units and disperse requirement also than higher, and processing is difficulty relatively.
Described in patent CN1318508C, in 100 parts of PPS, add 400 part of 20 μ m Natural manganese dioxide and 300 part of 5 μ m aluminum oxide prepares heat conduction PPS; The heat conductive filler loading level of material is up to 87.5wt%; The material thermal conductivity also has only 1.967W/mK, and notched Izod impact strength has only 3.3KJ/m
2, non-notched Izod impact strength also has only 5.9 KJ/m
2
Described in the patent CN 101568599B, the graphite that in PPS, adds 50wt%-70wt% prepares heat conduction PPS material.Heat conductive filler content is also up to 50wt%～70wt%, and the heat conductivility that has just indicated material in the patent does not still have for equally very important performance index such as toughness etc. to relate at 5W/mK～25W/mK.
Described in the patent CN102079864A, adding heat conductive insulating filler and heat conduction whisker prepare heat conductive insulating PA66 in PA66, and the heat conductive filler total content is up to 55wt%～85wt%.The shock strength of gained material is at 25J/m～30J/m, and toughness of material is poor.
Described in the patent CN101568577A; Adding graphite and SP 1 prepare the heat conduction alloy material in the PP/PA matrix; The total mass mark of graphite and SP 1 is up to 71wt%; The thermal conductivity of material has only been paid close attention to flowability at 2.2W/mK～4.0W/mK in the patent, mention for toughness of material.
The present invention has made mechanical property excellence and the good thermally conductive material of heat conductivility through specific heat conductive filler compounded combination and specific preparation method on the prior art basis.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, heat conduction moulding compound of a kind of heat conductivility excellence and good mechanical performance and preparation method thereof is provided, the heat-conducting plastic of this method preparation has excellent heat conductivility and good mechanical performance.
For realizing above purpose, the present invention adopts following technical scheme:
A kind of heat conduction moulding compound, form by the component of following weight percentage:
Plastic substrate 20～60%
Heat conductive filler A 15～40%
Heat conductive filler B 10～30%
Heat conductive filler C 1～5%
Enhancement component 5～15%
Surface-modifying agent 0.05～0.5%
Other additives 0～2 %.
Described plastic substrate is one or more the mixture in polyphenylene sulfide (PPS), liquid crystalline polymers (LCP), polymeric amide (like PA10T, PA6T/66, PA6T/6I, PA9T, PA46, PA6, PA66, PA6/66, PA12, PA6/12), polyester (like PBT, PET, PC), styrenic polymer (like ABS, PS) and the polyolefine (like PP, PE), but is not limited only to these plastic substrates;
Described heat conductive filler A is the microcosmic sheet structure, comprises graphite, the aluminum oxide (Al of sheet structure
2O
3), in Natural manganese dioxide (MgO), zinc oxide (ZnO), aluminium nitride AlN (AlN), SP 1 (BN), silit (SiC) etc. one or more, but be not limited only to these heat conductive fillers.Median size is at 10 μ m～200 μ m, preferred 15 μ m～150 μ m, more preferably 20 μ m～100 μ m.Radius-thickness ratio is 10～100, preferred 10-80, more preferably 10-50.
Described heat conductive filler B is that microcosmic is spherical, ellipsoid shape structure, comprises aluminum oxide (Al
2O
3), a kind of in the spherical or ellipsoid shape filler such as Natural manganese dioxide (MgO), zinc oxide (ZnO), aluminium nitride AlN (AlN), SP 1 (BN); But be not limited only to these heat conductive fillers; Its median size is at 1 μ m～20 μ m, preferred 2 μ m～15 μ m, more preferably 3 μ m～10 μ m.
Described heat conductive filler C is that microcosmic is spherical, comprises aluminum oxide (Al
2O
3), a kind of in the Natural manganese dioxide (MgO), zinc oxide (ZnO), aluminium nitride AlN (AlN), SP 1 ball filler such as (BN); But be not limited only to these heat conductive fillers; Its median size is at 10nm～100nm, preferred 15nm～80nm, more preferably 20nm～50nm.
The weight ratio of described heat conductive filler A and heat conductive filler B is controlled in 5:1～1:1 scope, preferred 4:1～1:1.Heat conductive filler C content is the 1wt%～10wt% of heat conductive filler B content, preferred 1wt%～5wt%.
The sheet heat conductive filler A of big particle diameter is main in resin matrix to play heat conduction network skeleton function, because particle diameter and radius-thickness ratio are very big, its maximum volume in resin matrix adds mark (maximum volume fraction, Φ
Max) lower, therefore under less content, just can play basic network skeleton effect.Than the heat conductive filler B outside surface of small particle size owing to adhered to one deck Nano filling C; And the chemical coupling processing has been passed through on its surface; Surperficial coupling processing has also been passed through on the sheet structure surface of heat conductive filler A; Because the polar attraction effect of surface treatment agent; Heat conductive filler B than small particle size is inclined between the sheet structure that is distributed in heat conductive filler A in system, and the adherent Nano filling layer in the top layer of heat conductive filler B has bigger specific surface area, and its surface has comparison intensive chemical attraction effect through heat conductive filler A to the same sheet structure through coupling processing around it after coupling processing; Thereby reduced the space length between sheet heat conductive filler A and spherical or the ellipsoid shape heat conductive filler B, formed the heat conduction network chain of continuous densification.In addition; Because the surface chemistry effect, at the heat conductive filler A described in the resin matrix, heat conductive filler B and heat conductive filler C are distributed on the heat conduction network chain of continuous densification basically; Isolated be distributed in do not form the heat conduction network chain in the matrix heat conductive filler seldom; Therefore with respect to common equally distributed heat conduction system, in order to reach identical heat conductivility, the required heat conductive filler total content of this system obviously reduces.
Nano heat-conductive filler C is evenly distributed on micron outside surface of heat conductive filler B, not only can play good heat-conducting effect, and the toughening effect of nanoparticle also has positive effect to the toughness that improves whole system.In addition since the mechanical property that total filler content reduces whole system also be significantly improved with respect to traditional high infill system.
Described enhancement component is one or more in short glass fiber, thomel, wollastonite fibre, lime carbonate, talcum powder, silicon-dioxide, mica, the potassium titanate crystal whisker etc., but is not limited only to these reinforcing fillers.Preferred short glass fiber, thomel and wollastonite fibre, more preferably short glass fiber and thomel.
Described surface-modifying agent is one or more in aromatic sulphonate, aromatic sulfonamide, silane coupling agent, aluminate coupling agent, the titanate coupling agent etc., but is not limited only to these surface-modifying agents;
Described other additives comprise one or more in lubricant, the oxidation inhibitor etc.Described oxidation inhibitor comprises one or more in Hinered phenols antioxidant, suffocated amine antioxidant, phosphite ester kind antioxidant, thiodipropionate antioxidant or the thio-alcohol oxidation inhibitor, but is not limited only to these oxidation inhibitor.Described lubricant comprises one or more in lignite acid derivative, macromolecule wax class, low molecular weight liquid crystal polymkeric substance, metallic soap of stearic acid salt, stearic amide, the silicone compound, but is not limited only to these lubricants.
The preparation method of above-mentioned heat conduction moulding compound comprises the steps:
(1) heat conductive filler B is joined in the mixing machine, then adds surface-modifying agent and mix, and then add heat conductive filler C and continue to mix, make heat conductive filler C evenly adhere to the superficies of heat conductive filler B, the mixture I;
(2) said heat conductive filler A is joined in the high-speed mixer, then add surface-modifying agent and mix, get the mixture II;
(3) the main spout from twin screw extruder adds behind plastic substrate and other additive mixings, and the mixture I of gained and mixture II are fed a mouthful entering from main spout adding or from the downstream side of forcing machine in the above-mentioned steps;
(4) feed a mouthful adding separately with described enhancement component from the downstream opposite side of forcing machine;
(5) behind the twin screw extruder melt blending, extrude, pass through water-cooled, pelletizing, sieve, adorn the job contract preface, prepare the heat conduction moulding compound.
The present invention compared with prior art has following advantage:
The present invention is through the big particle diameter sheet of the micron order heat conductive filler of specified shape and particle diameter specification; Micron order small particle size spherical or ellipsoid shape heat conductive filler and the composite use of the spherical heat conductive filler three of nano level small particle size; Control the distribution of these heat conductive filler mixtures in resin matrix through special preparation method simultaneously; Thereby form heat conduction network efficiently, the heat conductivility of material is very excellent.In addition, it is surperficial that the nano heat-conductive uniform filling of adding is distributed in micron order small particle size outer thin layer spherical or ellipsoid shape heat conductive filler, not only can play good heat-conducting effect, and the toughening effect of nanoparticle also has positive effect to the toughness that improves whole system.In addition since the mechanical property that total filler content reduces whole system also be significantly improved with respect to traditional high infill system.
Embodiment
Below in conjunction with embodiment the present invention is described further.
The table 1.1 heat conduction polymeric amide PA10T composition of filling a prescription
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Polymeric amide PA10T | 60 | 40 | 20 |
| 150 μ m SP 1 | 15 | 30 | 40 |
| 20 μ m Natural manganese dioxide | 10 | 20 | 30 |
| 20 nano aluminium oxides | 1 | 2 | 4.6 |
| Short glass fiber | 13.6 | 7.6 | 5 |
| Oxidation inhibitor | 0.2 | 0.2 | 0.2 |
| Lubricant | 0.2 | 0.2 | 0.2 |
Table 1.2 heat conduction polymeric amide PA10T performance
Table 1.1 is formed for the prescription of embodiment 1～embodiment 3 of heat conduction polymeric amide PA10T.The heat-resistant polyamide resin that described polymeric amide PA10T is a viscosity 2.0; Described short glass fiber is that diameter is the chopped strand of 12 μ m; Said SP 1 is the microcosmic sheet, and median size is 150 μ m, and radius-thickness ratio is 20.Said Natural manganese dioxide is that microcosmic is spherical, median size 20 μ m.Said aluminum oxide is that microcosmic is spherical, median size 20nm.Said surface-modifying agent is an aluminate coupling agent.Said oxidation inhibitor is the efficient anti-xanthochromia agent of amine nylon; Described lubricant is the montanic acid sodium salt.
Said 20 μ m Natural manganese dioxide are joined in the high-speed mixer; Then add the said aluminate coupling agent of 0.5wt% (with respect to the weight of SP 1); Mix, and then add the 20nm aluminum oxide and continue to mix, make nano aluminium oxide evenly adhere to the superficies of SP 1.Get the mixture I.
Said 150 μ m SP 1 are joined in the high-speed mixer, then add the aluminate coupling agent of 0.5wt% (with respect to the weight of SP 1), mix, get the mixture II.
Polymeric amide PA10T is added from the main spout of twin screw extruder; The mixture I of gained adds from main spout and resin simultaneously in the above-mentioned steps; Short glass fiber is fed a mouthful entering from first side in forcing machine downstream, and the mixture II is fed mouth from second side in forcing machine downstream and got into.250 ℃～320 ℃ of extrusion temperatures, screw speed 400rpm, granulation and dry after the water cooling excessively.Test according to iso standard injection moulding batten.
Table 1.2 is the performance data of embodiment 1～embodiment 3 of heat conduction polymeric amide PA10T.Can be got by data in the table, the heat conduction polymeric amide PA10T that makes according to the present invention not only has excellent heat conductivility, and the mechanical property of material is also very good.
Table 2.1 heat-conducting polyphenyl thioether prescription is formed
| ? | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Polyphenylene sulfide | 60 | 40 | 20 |
| 100 μ m aluminium nitride AlN | 15 | 30 | 40 |
| 15 μ m zinc oxide | 10 | 20 | 30 |
| 30 nano magnesias | 1 | 3 | 5 |
| Short glass fiber | 14 | 7 | 5 |
Table 2.2 heat-conducting polyphenyl thioether performance
Table 2.1 is that the prescription of the embodiment 4～embodiment 6 of heat-conducting polyphenyl thioether is formed.Described short glass fiber is that diameter is the chopped strand of 11 μ m; Said aluminium nitride AlN is the microcosmic sheet, and median size is 100 μ m, and radius-thickness ratio is 25.Said zinc oxide is that microcosmic is spherical, median size 15 μ m.Said nano magnesia is that microcosmic is spherical, median size 30nm.Said surface-modifying agent is a silane coupling agent.
Said 15 μ m zinc oxide are joined in the high-speed mixer; Then add the said silane coupling agent of 0.8wt% (with respect to the weight of zinc oxide); Mix, and then add 30nm Natural manganese dioxide and continue to mix, make nano magnesia evenly adhere to the superficies of zinc oxide.Get the mixture I.
Said 100 μ m aluminium nitride AlN are joined in the high-speed mixer, then add the silane coupling agent of 0.8wt% (with respect to the weight of aluminium nitride AlN), mix, get the mixture II.
The main spout of polyphenylene sulfide from twin screw extruder added; The mixture II of gained adds from main spout and resin simultaneously in the above-mentioned steps; Short glass fiber is fed a mouthful entering from first side in forcing machine downstream, and the mixture I is fed mouth from second side in forcing machine downstream and got into.250 ℃～290 ℃ of extrusion temperatures, screw speed 350rpm, granulation and dry after the water cooling excessively.Test according to iso standard injection moulding batten.
Table 2.2 is the performance data of the embodiment 4～embodiment 6 of heat-conducting polyphenyl thioether.Can be got by data in the table, the heat-conducting polyphenyl thioether that makes according to the present invention not only has excellent heat conductivility, and the mechanical property of material is also very good.
Claims (9)
1. heat conduction moulding compound, its characteristic comprises the component of following weight percentage:
Plastic substrate 20～60%
Heat conductive filler A 15～40%
Heat conductive filler B 10～30%
Heat conductive filler C 1～5%
Enhancement component 5～15%
Heat conduction moulding compound according to claim 1 is characterized in that described plastic substrate is one or more the mixture in polyphenylene sulfide, liquid crystalline polymers, polymeric amide, polyester, styrenic polymer and the polyolefine.
2. heat conduction moulding compound according to claim 1 is characterized in that described heat conductive filler A is one or more in graphite, aluminum oxide, Natural manganese dioxide, zinc oxide, aluminium nitride AlN, SP 1, the silit; The median size of heat conductive filler A is at 10 μ m～200 μ m, and radius-thickness ratio is 10～100.
3. heat conduction moulding compound according to claim 1 is characterized in that described heat conductive filler B is a kind of in aluminum oxide, Natural manganese dioxide, zinc oxide, aluminium nitride AlN, the SP 1, and median size is at 1 μ m～20 μ m.
4. heat conduction moulding compound according to claim 1 is characterized in that described heat conductive filler C is a kind of in aluminum oxide, Natural manganese dioxide, zinc oxide, aluminium nitride AlN, the SP 1, and the median size of heat conductive filler C is at 10nm～100nm.
5. heat conduction moulding compound according to claim 1 is characterized in that described enhancement component is one or more in short glass fiber, thomel, wollastonite fibre, lime carbonate, talcum powder, silicon-dioxide, mica, the potassium titanate crystal whisker.
6. heat conduction moulding compound according to claim 1; Its characteristic also comprises 0.05～0.5% surface-modifying agent, and described surface-modifying agent is one or more in aromatic sulphonate, aromatic sulfonamide, silane coupling agent, aluminate coupling agent, the titanate coupling agent.
7. heat conduction moulding compound according to claim 1, its characteristic also comprise other additives 0～2 %.
8. described other additives are lubricant or oxidation inhibitor; Described oxidation inhibitor is one or more in Hinered phenols antioxidant, suffocated amine antioxidant, phosphite ester kind antioxidant, thiodipropionate antioxidant or the thio-alcohol oxidation inhibitor; Described lubricant is one or more in lignite acid derivative, macromolecule wax class, low molecular weight liquid crystal polymkeric substance, metallic soap of stearic acid salt, stearic amide, the silicone compound.
9. the preparation method of the said heat conduction moulding compound of claim 1 is characterized in that comprising the steps:
(1) heat conductive filler B is joined in the mixing machine, then adds surface-modifying agent and mix, and then add heat conductive filler C and continue to mix, make heat conductive filler C evenly adhere to the superficies of heat conductive filler B, the mixture I;
(2) said heat conductive filler A is joined in the high-speed mixer, then add surface-modifying agent and mix, get the mixture II;
(3) the main spout from twin screw extruder adds behind plastic substrate and other additive mixings, and the mixture I of gained and mixture II are fed a mouthful entering from main spout adding or from the downstream side of forcing machine in the above-mentioned steps;
(4) feed a mouthful adding separately with described enhancement component from the downstream opposite side of forcing machine;
(5) behind the twin screw extruder melt blending, extrude, pass through water-cooled, pelletizing, sieve, adorn the job contract preface, prepare the heat conduction moulding compound.
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