CN102719099B - Thermal conductive molding compound and preparation method thereof - Google Patents
Thermal conductive molding compound and preparation method thereof Download PDFInfo
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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 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 day by day frivolous miniaturization of electronic machine, and operating frequency sharply increases, semiconductor heat environment changes rapidly to high temperature direction.The heat run-up that now electronics produces will make electronic devices and components still can high reliability normally work expeditiously at environment for use temperature, and heat-sinking capability becomes the critical limitation in its work-ing life factor that affects in time.Although traditional pottery or heat dissipation metal material have good radiating effect, its intrinsic several large defect has seriously limited their development, mainly comprises that density is large, difficult forming, and structure design is limited etc.The heat-conductivity polymer composite of the excellent combination property of high reliability high-cooling property has well made up the defect of traditional heat-dissipating material, as hot interface and packaged material, is substituting gradually pottery and metal, becomes the first-selection of field of radiating.
In the prior art, the thinking major part of preparing polymer-based carbon thermally conductive material is the method for adding high-content heat conductive filler that adopts in polymeric matrix.Although this method can obtain the pretty good material of heat conductivility, high filler loading capacity is often with and is served serious problems, as the mechanical property of material obviously declines, and especially toughness; Density of material is too large, affects its application; Product surface ratio is more coarse, not attractive in appearance; High infill system is also higher for the reinforced and dispersion requirement of processing units in addition, and processing is difficulty relatively.
Described in patent CN1318508C, in 100 parts of PPS, add 400 part of 20 μ m magnesium oxide and 300 part of 5 μ m alumina preparation heat conduction PPS, the heat conductive filler loading level of material is up to 87.5wt%, material thermal conductivity also only has 1.967W/mK, and notched Izod impact strength only has 3.3KJ/m
2, non-notched Izod impact strength also only has 5.9 KJ/m
2.
Described in patent CN 101568599B, in PPS, add the graphite of 50wt%-70wt% to prepare heat conduction PPS material.Heat conductive filler content, also up to 50wt%～70wt%, has just indicated the heat conductivility of material at 5W/mK～25W/mK in patent, but relates to as toughness etc. does not have for equally very important performance index.
Described in patent CN102079864A, add heat-conductive insulation filling and heat conduction whisker to prepare heat conductive insulating PA66 in PA66, heat conductive filler total content is up to 55wt%～85wt%.The shock strength of resulting materials is at 25J/m～30J/m, and toughness of material is poor.
Described in patent CN101568577A, in PP/PA matrix, add graphite and boron nitride to prepare heat conduction alloy material, the total mass mark of graphite and boron nitride is up to 71wt%, the thermal conductivity of material is at 2.2W/mK～4.0W/mK, in patent, only pay close attention to mobility, mentioned for toughness of material.
The present invention, on prior art basis, has made mechanical property excellence and the good thermally conductive material of heat conductivility by specific heat conductive filler compounded combination and specific preparation method.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, heat conduction moulding compound of a kind of heat conductivility excellence and good mechanical performance and preparation method thereof is provided, heat-conducting plastic prepared by the method has excellent heat conductivility and good mechanical property.
For realizing above object, the present invention adopts following technical scheme:
A kind of heat conduction moulding compound, is made up of 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 (as PA10T, PA6T/66, PA6T/6I, PA9T, PA46, PA6, PA66, PA6/66, PA12, PA6/12), polyester (as PBT, PET, PC), styrenic polymer (as ABS, PS) and polyolefine (as PP, PE), but is not limited only to these plastic substrates;
Described heat conductive filler A is microcosmic sheet structure, comprises graphite, the aluminum oxide (Al of sheet structure
2o
3), one or more in magnesium oxide (MgO), zinc oxide (ZnO), aluminium nitride (AlN), boron nitride (BN), silicon carbide (SiC) etc., but be not limited only to these heat conductive fillers.Median size is at 10 μ m～200 μ m, preferably 15 μ m～150 μ m, more preferably 20 μ m～100 μ m.Radius-thickness ratio is 10～100, preferably 10-80, more preferably 10-50.
Described heat conductive filler B is spherical, the ellipse ball-like structure of microcosmic, comprises aluminum oxide (Al
2o
3), one in the spherical or ellipse ball filler such as magnesium oxide (MgO), zinc oxide (ZnO), aluminium nitride (AlN), boron nitride (BN), but be not limited only to these heat conductive fillers, its median size is at 1 μ m～20 μ m, preferably 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), one in the ball filler such as magnesium oxide (MgO), zinc oxide (ZnO), aluminium nitride (AlN), boron nitride (BN), but be not limited only to these heat conductive fillers, its median size is at 10nm～100nm, preferably 15nm～80nm, more preferably 20nm～50nm.
Described heat conductive filler A and the weight ratio of heat conductive filler B are controlled within the scope of 5:1～1:1, preferably 4:1～1:1.Heat conductive filler C content is the 1wt%～10wt% of heat conductive filler B content, preferably 1wt%～5wt%.
The sheet heat conductive filler A of large particle diameter is the main heat conduction network skeleton function that rises in resin matrix, due to particle diameter and radius-thickness ratio very large, 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.Compared with the heat conductive filler B outside surface of small particle size owing to having adhered to one deck Nano filling C, and 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, due to the polar attraction effect of surface treatment agent, in system, be inclined between the sheet structure that is distributed in heat conductive filler A compared with the heat conductive filler B of small particle size, and the Nano filling layer that the top layer of heat conductive filler B adheres to has larger specific surface area, its surface has stronger chemical attraction effect to the heat conductive filler A of its same sheet structure through coupling processing around after coupling processing, thereby reduce the space length between sheet heat conductive filler A and spherical or ellipsoid shape heat conductive filler B, form the heat conduction network chain of continuous densification.In addition, due to surface chemistry, at the heat conductive filler A described in resin matrix, heat conductive filler B and heat conductive filler C are distributed on the heat conduction network chain of continuous densification substantially, isolated be distributed in that in matrix, not form the heat conductive filler of heat conduction network chain little, 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 a 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.The mechanical property that reduces whole system due to total filler content in addition is also significantly improved with respect to traditional high infill system.
Described enhancement component is one or more in short glass fiber, carbon fiber, wollastonite fibre, calcium carbonate, talcum powder, silicon-dioxide, mica, potassium titanate crystal whisker etc., but is not limited only to these reinforcing fillers.Preferably short glass fiber, carbon fiber and wollastonite fibre, more preferably short glass fiber and carbon fiber.
Described surface-modifying agent is one or more in aromatic sulphonate, aromatic sulfonamide, silane coupling agent, aluminate coupling agent, titanate coupling agent etc., but is not limited only to these surface-modifying agents;
Other described additives comprise one or more in lubricant, oxidation inhibitor etc.Described oxidation inhibitor comprises one or more in Hinered phenols antioxidant, suffocated amine antioxidant, phosphite ester kind antioxidant, thiodipropionate antioxidant or 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, 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 mixing machine, then add surface-modifying agent to mix, and then add heat conductive filler C to continue to mix, make heat conductive filler C evenly adhere to the superficies of heat conductive filler B, obtain mixture I;
(2) described heat conductive filler A is joined in high-speed mixer, then add surface-modifying agent to mix, obtain mixture II;
(3) plastic substrate and other additives add from the main spout of twin screw extruder after mixing, and in above-mentioned steps, the mixture I of gained and mixture II add or enter from downstream side hello the mouth of forcing machine from main spout;
(4) feeding mouth by described enhancement component from the downstream opposite side of forcing machine adds separately;
(5) after twin screw extruder melt blending, extrude, pass through water-cooled, pelletizing, sieve, fill job contract order, prepare heat conduction moulding compound.
The present invention compared with prior art tool has the following advantages:
The present invention is by the large 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 by special preparation method simultaneously, thereby form efficient heat conduction network, the heat conductivility of material is very excellent.In addition, the nano heat-conductive uniform filling adding is distributed in the outer thin layer surface of the spherical or ellipsoid shape heat conductive filler of micron order small particle size, 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.The mechanical property that reduces whole system due to total filler content in addition is also significantly improved with respect to traditional high infill system.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
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 boron nitride | 15 | 30 | 40 |
| 20 μ m magnesium oxide | 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
The formula composition of embodiment 1～embodiment 3 that table 1.1 is heat conduction polymeric amide PA10T.Described polymeric amide PA10T is the heat-resistant polyamide resin of viscosity 2.0; Described short glass fiber is that diameter is the chopped strand of 12 μ m; Described boron nitride is microcosmic sheet, and median size is 150 μ m, and radius-thickness ratio is 20.Described magnesium oxide is that microcosmic is spherical, median size 20 μ m.Described aluminum oxide is that microcosmic is spherical, median size 20nm.Described surface-modifying agent is aluminate coupling agent.Described oxidation inhibitor is the efficient resistance to xanthochromia agent of amine nylon; Described lubricant is montanic acid sodium salt.
Described 20 μ m magnesium oxide are joined in high-speed mixer, then add the weight of 0.5wt%(with respect to boron nitride) described aluminate coupling agent, mix, and then add 20nm aluminum oxide to continue to mix, make nano aluminium oxide evenly adhere to the superficies of boron nitride.Obtain mixture I.
Described 150 μ m boron nitride are joined in high-speed mixer, then add the weight of 0.5wt%(with respect to boron nitride) aluminate coupling agent, mix, obtain mixture II.
Polymeric amide PA10T is added from the main spout of twin screw extruder, in above-mentioned steps, the mixture I of gained adds from main spout and resin simultaneously, short glass fiber is fed mouth from first side in forcing machine downstream and is entered, and mixture II is fed mouth from second side in forcing machine downstream and entered.250 DEG C～320 DEG C of extrusion temperatures, screw speed 400rpm, granulation dry after water cooling excessively.Test according to iso standard injection moulding batten.
The performance data of embodiment 1～embodiment 3 that table 1.2 is heat conduction polymeric amide PA10T.Can be obtained by data in table, the heat conduction polymeric amide PA10T making 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 formula composition
| ? | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Polyphenylene sulfide | 60 | 40 | 20 |
| 100 μ m aluminium nitride | 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 the formula composition of the embodiment 4～embodiment 6 of heat-conducting polyphenyl thioether.Described short glass fiber is that diameter is the chopped strand of 11 μ m; Described aluminium nitride is microcosmic sheet, and median size is 100 μ m, and radius-thickness ratio is 25.Described zinc oxide is that microcosmic is spherical, median size 15 μ m.Described nano magnesia is that microcosmic is spherical, median size 30nm.Described surface-modifying agent is silane coupling agent.
Described 15 μ m zinc oxide are joined in high-speed mixer, then add the weight of 0.8wt%(with respect to zinc oxide) described silane coupling agent, mix, and then add 30nm magnesium oxide to continue to mix, make nano magnesia evenly adhere to the superficies of zinc oxide.Obtain mixture I.
Described 100 μ m aluminium nitride are joined in high-speed mixer, then add the weight of 0.8wt%(with respect to aluminium nitride) silane coupling agent, mix, obtain mixture II.
Polyphenylene sulfide is added from the main spout of twin screw extruder, in above-mentioned steps, the mixture II of gained adds from main spout and resin simultaneously, short glass fiber is fed mouth from first side in forcing machine downstream and is entered, and mixture I is fed mouth from second side in forcing machine downstream and entered.250 DEG C～290 DEG C of extrusion temperatures, screw speed 350rpm, granulation dry after 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 obtained by data in table, the heat-conducting polyphenyl thioether making according to the present invention not only has excellent heat conductivility, and the mechanical property of material is also very good.
Claims (5)
1. a heat conduction moulding compound, is characterized in that comprising 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%
Other additives 0～2 %
Described plastic substrate is one or more the mixture in polyphenylene sulfide, liquid crystalline polymers, polymeric amide, polyester, styrenic polymer and polyolefine;
Described heat conductive filler A is microcosmic sheet structure, and described heat conductive filler A is one or more in graphite, aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, silicon carbide; The median size of heat conductive filler A is at 10 μ m～200 μ m, and radius-thickness ratio is 10～100;
Described heat conductive filler B is spherical, the ellipse ball-like structure of microcosmic, and described heat conductive filler B is the one in aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, and median size is at 1 μ m～20 μ m;
Described heat conductive filler C is that microcosmic is spherical, and described heat conductive filler C is the one in aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, and the median size of heat conductive filler C is at 10nm～100nm.
2. heat conduction moulding compound according to claim 1, is characterized in that described enhancement component is one or more in short glass fiber, carbon fiber, wollastonite fibre, calcium carbonate, talcum powder, silicon-dioxide, mica, potassium titanate crystal whisker.
3. heat conduction moulding compound according to claim 1, characterized by further comprising 0.05～0.5% surface-modifying agent, described surface-modifying agent is one or more in aromatic sulphonate, aromatic sulfonamide, silane coupling agent, aluminate coupling agent, titanate coupling agent.
4. heat conduction moulding compound according to claim 1, is characterized in that other described 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 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, silicone compound.
5. the preparation method of heat conduction moulding compound described in claim 1, is characterized in that comprising the steps:
(1) heat conductive filler B is joined in mixing machine, then add surface-modifying agent to mix, and then add heat conductive filler C to continue to mix, make heat conductive filler C evenly adhere to the superficies of heat conductive filler B, obtain mixture I;
(2) described heat conductive filler A is joined in high-speed mixer, mix, obtain mixture II;
(3) plastic substrate and other additives add from the main spout of twin screw extruder after mixing, and in above-mentioned steps, the mixture I of gained and mixture II add or enter from downstream side hello the mouth of forcing machine from main spout;
(4) feeding mouth by described enhancement component from the downstream opposite side of forcing machine adds separately;
(5) after twin screw extruder melt blending, extrude, pass through water-cooled, pelletizing, sieve, fill job contract order, prepare heat conduction moulding compound.
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