CN101787178B - Heat-conduction electric insulation composite material component and manufacturing method thereof - Google Patents
Heat-conduction electric insulation composite material component and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a heat-conduction insulation composite material and a manufacturing method thereof. The material comprises the components: 1) high-crystallization spherical metallic oxide powder with at least two sizes, wherein the large-grain powder has the size of R, and the small-grain powder has the size of r, and r is more than 0.005R and less than 0.2R; the power is aluminum oxide, magnesium oxide, zinc oxide and the like, the thermal conductivity is more than 10W/m. kilowatt hour, and the powder has electric insulation property; 2) at least one sheet heat-conduction powder such as squamous graphite powder, boron nitride powder and the like, and the thermal conductivity is more than 30W/m. kilowatt hour; and 3) resin such as epoxy, organic silicon, phenolic aldehyde, vinyl resin and the like. The components have the weight percent: 20-60% of spherical powder, 3-30% of sheet heat-conduction powder and 15-65% of resin. Through certain mixing technique, the obtained material has good heat conduction property, the thermal conductivity is more than 0.5W/m. kilowatt hour, the electric insulation property is more than 1012 omega/cm<2>, and the composite material has good injection molding, extruding or hot-pressing forming properties. The invention can be directly used for radiators of an LED, electrical equipment, electronic components and the like, leads heat to be dispersed into colder environment, and reduces the running temperature of electronic devices.
Description
Technical field
Present invention relates in general to a kind of matrix material of modification, especially relate to a kind of high heat-conduction electric insulation composite material that is easy to injection moulding (moldable) or hot press molding (hot press) or extrudes (extrudable).
Background technology
Along with all kinds of electronic devices and components operation high speeds and superpowerization; Equipment can produce relatively-high temperature in use and operational process; Thereby possibly cause the overheated of electronic devices and components and damage its performance, cause safety to reduce, even the life-span of reducing whole system significantly.Conventional engineering plastics comprise thermoplasticity and thermosetting resin, have satisfactory mechanical property; Chemically stable, advantages such as electrical isolation are widely used in fields such as shell such as daily electrical equipment; But because of its thermal conductivity is too low, belong to the poor conductor of heat, not only can not solve high heat dissipation problem; And, possibly make some heat sensitive components and parts overheated, thereby reduce the life-span or the operational efficiency of system significantly because heat can not effectively be discharged.
As everyone knows, metallic substance has extraordinary heat conductivility, but has been applied in the thermal component of semiconductor apparatus assembly. and there is following potential shortcoming in metal:
(1) metal belongs to the good conductor of electricity, at many application occasions, based on security consideration, hopes to use the material of electrical isolation;
(2) the metallic article working (machining) efficiency is lower, generally need or be machined into required complicated shape from the bulk material cutting, needs extraordinary machining apparatus, and unit cost is higher relatively;
(3) metallic substance density is relatively large, usually all greater than 2.4g/cm
3Thereby, cause goods heavy relatively;
(4) metallographic phase is for plastic material, corrosion-vulnerable;
(5) metal processing needs higher relatively temperature, and energy consumption is relatively large.
In sum, develop a kind of low cost, high-level efficiency and the heat-conducting insulation material lighter with respect to metal have huge commercial value.
In existing technology; Chinese patent CN101333434A discloses a kind of nano heat-conductive powder and cubic boron nitride of utilizing thermoplastic material has been carried out modification; Obtain a kind of highly heat-conductive material that carries out thermoplastic molding's processing; But, possibly cause the processing flowability of material to decline to a great extent, and its surface conductivity has reached 10 because a large amount of nanometer powders adds
5Ohm/meter promptly belongs to a kind of semiconductor material.Chinese patent 99815810.0 utilizes the heat conductive filler of two kinds of different length-to-diameter ratios, has obtained one type and has had cancellated highly heat-conductive material.Owing to used a large amount of conductive filler materials, so this type material is non-isolator.Publication number is that CN101225234A has described a kind of have fiber reinforcement or film enhancing structure, is the thermally conductive material of matrix with the silicone resin, has solved the problem of one type of interface heat conduction.In addition, known heat-conductive composite material often uses a large amount of very expensive fillers, as greater than the SP 1 of 30% weight content etc., makes that the overall cost of material is very high.
Simultaneously; Because applied environment needs complicated geometrical shape to realize usually, if in material system, contain a large amount of mineral fillers, its moulding processability; Flowing property possibly fluctuate within the specific limits such as material owing to filler/resin content; Cause its machine-shaping stability lower, in the Application Areas of precision of having relatively high expectations, existing composite property is more very different than expectation.
Present invention relates in general to a kind of improved matrix material.More particularly,, obtain one type high heat-conduction electric insulation material, have overall performances such as maximized thermal conductivity and stable machining moulding, can realize the product of complex geometric shapes through hot-forming or injection moulding with lower cost price.
Summary of the invention
Present invention relates in general to one type of novelty and unique heat-conductive composite material, have and can heat be transferred to the other end quickly from high temperature one end, thereby reach the purpose of heat radiation.Composite system of the present invention is a kind of with the original heat-conductive composite material of making of lower one-tenth, in satisfying the scope of its heat conductivility, can come the processing fluidity of stable material through coupling filler relative proportion.Matrix material of the present invention has thermal conductivity and is higher than 0.5 watt/meter. and degree has electrical insulation capability, its surface resistivity＞10 simultaneously
12Ohm-sq centimetre.Such thermally conductive material component comprises the thermosetting resin of one type of weight content 15-65%.Such thermally conductive material component also comprises first kind of heat conductive filler, and weight content is 20-60%, is the spherical metal oxide powder of high crystal type of at least two kinds of sizes, and its large size powder particle R and small size powder r satisfy: r greater than 0.005R and r less than 0.2R.Such heat conduction component also comprises second type of filler, the sheet heat conductive filler of about 3-30% weight content.Compsn of the present invention, through certain hybrid technique, the flowing property of the heat-conductive composite material that is obtained can be carried out stabilization through the ball filler of coupling different size.In the moulding process of matrix material of the present invention, material can stably join in its process window in the die cavity, can obtain the goods of various complex geometric shapes.
In heat conductive filler, mainly contain aluminum oxide, aluminium nitride AlN, SP 1, heat conduction inorganic powders such as silit.Simple with common micro powder grade mineral filler, often need high filler loading capacity could improve the thermal conductivity of polymkeric substance.Its electrical insulating property of spherical powders such as aluminum oxide is good, has certain thermal conductivity, and with respect to some sheets or fibrous heat conductive filler, it is cheap, and the source is abundant.But its thermal conductivity is still too low, and further improving thermal conductivity can not be merely by improving the filling ratio solve problem of filler.The raising of filling ratio can cause many negative influences, and is too high and influence its processing characteristics and mechanical property etc. like viscosity.
In the matrix material each component of the present invention, the thermal conductivity of resin part is minimum, has only 0.2 watt/meter. about degree; The thermal conductivity of spherical powder electric-insulation heat-conduction filler is about 10-30 watt/meter. degree or higher; Its thermal conductivity of flaky heat conductive filler is about 30 watts/meter. the degree or more than.Therefore, the service efficiency of heat conductive filler be fully improved, just the high thermal resistance problem that produces by resin must be reduced.Oarse-grained spherical heat conduction powder has higher heat transfer efficiency usually under unit volume.But along with the raising of particle size, possibly cause the material surface degraded appearance such as white point, surface irregularity etc., mechanical property descends, so the particle of oversized dimensions will have certain restriction in actual use.
In the present invention, as shown in Figure 1, introduced the heat conductive filler 1 of smaller particle size.When low particle size r have only macrobead size R 20% or more hour, the accumulation homogeneity of raising macrobead heat conductive filler 2 that just might be by a relatively large margin forms articulamentum relatively uniformly thereby resin 3 is distributed around spherical particle.The advantage of this system is the heat conductivility of ability maximum use heat conductive filler, the transmission effects of while maximum use resin counter stress, thereby heat conductivility, mechanical property and the surface property of optimization matrix material.
In the present invention, introduced the heat conductive filler of different size, can keep under the high-heat conductive efficency; Through regulating the ratio of size dimension filler; Viscosity to composite system is regulated, and can obtain the index stable composite material that flows, and helps the forming process property of material.
In the present invention, further introduced the sheet heat conductive filler 4 of 3-30% weight content.Such laminal filler needs weight content greater than 30% in existing technology usually, just can reach preferable heat transfer efficiency.In the present invention; As shown in Figure 1, add the sheet heat conductive filler 4 of (being lower than 30% weight content) on a small quantity, its sheet structure will further make the homogenization that distributes between resin and the ball filler; Fill up the space between the filler, thereby improved the heat conductivility of matrix material.Sheet heat conductive filler 4 in molding process, will be orientated along fluid flow direction, can further improve the final heat conductivility of goods.Simultaneously, the cost of integral material system can be effectively controlled in the laminal filler 4 of lower aq (being lower than 30% weight content).Through the weight content of control sheet heat conductive filler 4, can regulate the conductivity of matrix material, make it have electrical insulating property or electroconductibility.
Therefore, an object of the present invention is to provide the high electric insulation composite material of a kind of heat transfer efficiency;
An object of the present invention is to provide a kind of heat-conductive composite material that is easy to forming process;
An object of the present invention is to provide a kind of heat-conductive composite material with stable machine-shaping property;
An object of the present invention is to provide a kind of heat-conductive composite material cheaply;
An object of the present invention is to provide a kind of heat-conductive composite material that can be shaped to complex geometric shapes;
An object of the present invention is to provide a kind of than the low density heat-conductive composite material of metallic substance;
An object of the present invention is to provide one type of heat-conduction electric insulation material, can be used for thermal components such as LED, electrical equipment, electronic component.
Brief Description Of Drawings
The ideal of the heat conductive filler system of Fig. 1 different size and form in resin piled up synoptic diagram
The test set figure of Fig. 2 equilibrium temperature method assessment material heat conductivility
The mode of embodiment of the present invention
Following examples of implementation just are used for explaining meliority of the present invention.The manufacturing of heat-conducting insulation material of the present invention and practice and be not limited in this.The preparation and the performance test methods of the heat-conducting insulation material in the examples of implementation are following:
The preparation method of heat-conduction electric insulation composite material comprises:
1) resin batching: take by weighing the thermosetting resin each component, stir;
2) take by weighing relevant filler by needed weight percent, place the encloses container pre-mixing;
3) resin and filler are carried out thorough mixing in Banbury mixer, mixing roll or screw extrusion press, process the raw materials mix material.
The hybrid process temperature is according to different resin systems, respectively in processing temperature separately.To being the 20-100 degree in the epoxy vinyl resin/organosilicon-filler systems of following instance.Mixing in an example shown system is the banburying kneader.The bulk plastics that obtained carry out packed for standby use.
4) the raw materials mix material is carried out mold pressing or injection moulding, obtain required product.Condition of molding is regulated according to different resin systems to some extent.In this example, to epoxy vinyl resin-filler systems, it was cured moulding in about 5 minutes in 110 degree hot pressing; To organosilicon-filler systems, it was cured moulding in about 10 minutes in 170 degree hot pressing.
Among the present invention; The epoxy vinyl resin provides Hetron 922 Vinylites by Ashland company; Catalyzer is MEKP (methyl ethyl keton peroxide), and the inner pattern releasing agent applicable and the deaerating agent place of production are that orange industry and trade ltd is built in Shanghai, and consumption is respectively 0.5% and 0.2% weight content.
Among the present invention, methyl vinyl silicon kautschuk is as basic glue, model 110-1, contents of ethylene 0.17%, molecular weight 58-60 ten thousand, fugitive constituent 1.3%, the place of production-Dongjue Silicone Group Company Limited; Vinyl silicone oil: model VM-26, viscosity 2000-5000CS, contents of ethylene 10%, orange industry and trade ltd is built in the place of production-Shanghai; Vulcanizing agent: paste is two two or five, effective constituent 60%, the place of production-chemical plant, the East Sea, Jiangsu.
Two types of heat-conducting type alumina powders, its thermal conductivity are 30 watts/meter. degree.The large-grain alumina powder is that 50% particle average is 20 microns, and superfine type alumina powder 50% particle average is 0.2 micron; The conductive graphite powder is provided by Asbury company, 50 microns of 50% average grains.
The heat conductivility of heat-conduction electric insulation composite material test: adopt constant temperature oil bath heating temperature control system, test specimens is carried out the temperature measurement after the temperature equilibrium.The synoptic diagram of instrument such as Fig. 2: the constant temperature system is controlled at 100 ± 0.2 degree with the temperature of thermostatic bath 1, thermostatic bath 1 and the stable conduction of test specimens 2 through thermofin 3 maintenance temperature.Through heat conduction copper rod 4 test specimens 2 is fixed on the constant position, and the TP that test specimens is demarcated is carried out temperature test.Cage 5 is further isolated whole test zone.The temperature test error of sample is at ± 0.2 degree.Test environment temperature: 25 ± 1 degree, humidity 50%.In addition, the thermal conductivity of material is obtained by the Nanoflash conductometer.
Voyger resistance meter, each 5 test specimens are adopted in the surface resistivity test of material.
The flowing property of material adopts fusion index instrument under the room temperature, and probe temperature is 50 degree, and time of repose is 300 seconds, loads to be 10kg.
Examples of implementation 1: the prescription and the performance of oxyethylene based resin composite material material
Table 1
| The |
1 | 2 | 3 | 4 | 5 |
| Matrix material gross weight (gram) | 650 | 650 | 650 | 650 | 650 |
| Large-grain alumina (gram) | 390 | 325 | 195 | 130 | 0 |
| Ultra-fine grain aluminum oxide (gram) | 0 | 65 | 195 | 260 | 357.5 |
| Graphite (gram) | 97.5 | 97.5 | 97.5 | 97.5 | 97.5 |
| Hetron 922 Vinylites (gram) | 158.05 | 158.05 | 158.05 | 158.05 | 189.66 |
| Superoxide, Methyl ethyl keton peroxide (gram) | 2.822 | 2.822 | 2.822 | 2.822 | 3.387 |
| Releasing agent (gram) | 0.903 | 0.903 | 0.903 | 0.903 | 1.084 |
| Skimmer (gram) | 0.339 | 0.339 | 0.339 | 0.339 | 0.406 |
| Equilibrium temperature (degree) | 68.1 | 70.2 | 70.0 | 71.8 | 71.9 |
| Thermal conductivity (watt/meter. degree) | 2.1 | 2.8 | 2.8 | 2.9 | 3 |
| Mobility-thickness product (restraining/10 minutes) | 16 | 11 | 8 | 3 | ＜2 |
| Surface resistivity (ohm-sq centimetre) | ＞E12 | ＞E12 | ＞E12 | ＞E12 | ＞E12 |
Experiment 1-5 is in the epoxy-resin systems of different alumina particle sizes, the heat conduction of material, and performance with surface conductivity flows.The content of flake graphite is fixed as 15%, and the heat conductive filler total content is 75%.To containing the above-mentioned materials of 75% heat conductive filler of having an appointment, its thermal conductivity is from unfilled 0.2 watt/meter. and degree is increased to rapidly greater than 2.0 watts/meter. degree.To oarse-grained aluminum oxide and graphite system, its thermal conductivity is 2.1 watts/meter. degree, the equilibrium temperature of material are about 68 degree.But when the aluminum oxide that adds a spot of little rate and when keeping the total content of identical heat conductive filler, its equilibrium temperature has promptly improved more than 2 degree, and thermal conductivity raising amount is greater than 30%.Further improve undersized alumina content, the heat conductivility of material will tend to balance.
The flowing property of material can be in the certain heat conductivility of maintenance; Alumina packing through size particles is regulated; In this test, thermal conductivity is at 2.8 ± 0.2 watts/meter. degree, or equilibrium temperature 70 ± 2 is when spending; Flowing property can restrain at 3-11/regulate between 10 minutes, and this provides enough spaces for the stable machine-shaping of product.Cross a high proportion of ultra-fine alumina powder and possibly cause the flowability of material poor excessively, thereby can't process.
Although above-mentioned materials contains the graphite of conductivity, the overall performance of material still keeps electrical insulation capability, and surface resistivity is greater than 10
12Ohm-sq centimetre.
Examples of implementation 2: the prescription of epoxy resin composite material material and performance:
Table 2
| The experiment number | 6 | 7 | 8 | 9 | 10 |
| Matrix material gross weight (gram) | 650 | 650 | 650 | 650 | 650 |
| Large-grain alumina (gram) | 108.3 | 151.7 | 195 | 216.7 | 238.3 |
| Ultra-fine grain aluminum oxide (gram) | 54.2 | 75.8 | 97.5 | 108.3 | 119.2 |
| Graphite (gram) | 97.5 | 97.5 | 97.5 | 97.5 | 97.5 |
| Hetron 922 Vinylites (gram) | 379.3 | 316.1 | 252.9 | 221.3 | 189.7 |
| Superoxide, Methyl ethyl keton peroxide (gram) | 6.77 | 5.65 | 4.52 | 3.95 | 3.39 |
| Releasing agent (gram) | 2.168 | 1.806 | 1.445 | 1.264 | 1.084 |
| Skimmer (gram) | 0.813 | 0.677 | 0.542 | 0.474 | 0.406 |
| Equilibrium temperature (degree) | 64.000 | 64.5.000 | 65.000 | 66.300 | 68.700 |
| Thermal conductivity (watt/meter. degree) | 1.7 | 1.7 | 1.8 | 1.8 | 2.1 |
| Mobility-thickness product (restraining/10 minutes) | Greater than 40.0 | 38.0 | 25.0 | 20.1 | 13.0 |
| Surface resistivity (ohm-sq centimetre) | ＞E12 | ＞E12 | ＞E12 | ＞E12 | ＞E12 |
Table 2_ is continuous
| The experiment number | 11 | 12 | 13 | 14 | 15 |
| Matrix material gross weight (gram) | 650 | 650 | 650 | 650 | 650 |
| Large-grain alumina (gram) | 260 | 303.55 | 455 | 173 | 130 |
| Ultra-fine grain aluminum oxide (gram) | 130 | 151.45 | 0 | 87 | 65 |
| Graphite (gram) | 97.5 | 0 | 0 | 195 | 260 |
| Hetron 922 Vinylites (gram) | 158.1 | 189.7 | 189.7 | 189.7 | 189.7 |
| Superoxide, Methyl ethyl keton peroxide (gram) | 2.822 | 3.387 | 3.387 | 3.387 | 3.387 |
| Releasing agent (gram) | 0.903 | 1.084 | 1.084 | 1.084 | 1.084 |
| Skimmer (gram) | 0.339 | 0.406 | 0.406 | 0.406 | 0.406 |
| Equilibrium temperature (degree) | 70.5 | 60.5 | 61.4 | 72.0 | 72.3 |
| Thermal conductivity (watt/meter. degree) | 2.8 | 0.8 | 1.1 | 3.0 | 3.0 |
| Mobility-thickness product (restraining/10 minutes) | 9.0 | 6.000 | 15.000 | 14 | 16 |
| Surface resistivity (ohm-sq centimetre) | ＞E12 | ＞E12 | ＞E12 | ~E12 | E4 |
The heat conduction of matrix material when experiment 6-11 is different filler content, flow and electrical property.Its total filler content is that the size particles ratio of 40%-75%. aluminum oxide is 2/1, and flake graphite content is 15%.When filler content reaches certain value as 40% the time, its thermal conductivity can improve significantly.Along with the increase of filler content, its thermal conductivity can improve, but its flow capacity also descends thereupon.The conductivity of material still keeps state of insulation.
The material property of experiment 12-15 when adding certain content graphite, graphite weight content 0-40%.A certain amount of graphite adds, and like 15% weight content, can improve the heat conductivility of material very significantly, and thermal equilibrium temperature can improve 10 degree, and thermal conductivity can improve more than 100%, and keeps the electric insulating state of material.But, because graphite has electroconductibility, when content surpasses 30%, promptly might form conductive network, make material have certain electroconductibility.
Examples of implementation 3: the prescription of Zylox-heat-conductive composite material and performance
Table 3
| The experiment number | 16 | 17 | 18 | 19 | 20 | 21 |
| Matrix material gross weight (gram) | 650 | 650 | 650 | 650 | 650 | 650 |
| Large-grain alumina (gram) | 62.5 | 104.9 | 147.4 | 189.9 | 232.4 | 270.9 |
| Ultra-fine grain aluminum oxide (gram) | 31.2 | 52.5 | 73.7 | 95.0 | 116.2 | 137.4 |
| Graphite (gram) | 97.5 | 97.5 | 97.5 | 97.5 | 97.5 | 97.5 |
| Organosilicon 110-1 (gram) | 178.4 | 152.9 | 127.5 | 102.0 | 76.5 | 63.7 |
| Vinyl silicone oil (gram) | 267.6 | 229.4 | 191.2 | 152.9 | 114.7 | 95.6 |
| Releasing agent (gram) | 6.37 | 6.37 | 6.37 | 6.37 | 6.37 | 6.37 |
| Vulcanizing agent (gram) | 6.37 | 6.37 | 6.37 | 6.37 | 6.37 | 6.37 |
| Equilibrium temperature (degree) | 59.1 | 60.7 | 61.4 | 62.1 | 66.5 | 67.1 |
| Thermal conductivity (watt/meter. degree) | 0.8 | 1.1 | 1.2 | 1.4 | 1.8 | 2.0 |
| Mobility-thickness product (restraining/10 minutes) | 17 | 15 | 13 | 8 | 6 | 6 |
| Surface resistivity (ohm-sq centimetre) | ＞E12 | ＞E12 | ＞E12 | ＞E12 | ＞E12 | ＞E12 |
Experiment 16-17 is the performance of above-mentioned filler systems in the organo-silicone rubber system.Filler content is that 30%-75% does not wait.Along with the increase of filler content, equilibrium temperature is rapid ascendant trend, and the thermal conductivity of material can improve more than 100%.Add a certain amount of graphite, material still can keep state of insulation.Above-mentioned trend is consistent with the oxyethylene resin system.
Claims (3)
1. heat-conduction electric insulation material, its characteristic component is:
1) have the spherical metal oxide powder of high crystal type of two kinds of sizes, its thermal conductivity is more than or equal to 10 watts/meter. degree centigrade and have electrical insulation capability; Aforementioned spherical MOX is aluminum oxide or Natural manganese dioxide, and weight percent is 20-60%; In the spherical metal oxide powder of high crystal type of two kinds of sizes, bigger particle size is R, and smaller particles is of a size of r, and r is greater than 0.005R and smaller or equal to 0.2R, and bigger particle size R is 1-200 μ m; In the spherical metal oxide powder of high crystal type of two kinds of sizes, the spherical metal oxide powder content of macrobead is WR, and the spherical metal oxide powder content of small-particle is Wr, 0.6≤WR/ (WR+Wr)≤0.95;
2) at least a sheet heat conduction powder, its thermal conductivity is more than or equal to 30 watts/meter. degree centigrade, sheet heat conduction powder is flaky graphite powder or boron nitride powder, and weight percent is 2%-30%;
3) weight percent is the thermosetting resin of 15%-65%, and thermosetting resin is epoxy resin, silicone resin, resol, thermosetting polyester resin and composition thereof.
2. heat-conduction electric insulation material as claimed in claim 1 is characterized in that, each component is through certain hybrid technique, and the material that is obtained has higher thermal conductivity:＞0.5 watt/meter. degree centigrade, surface resistivity:＞10
12Ohm-sq centimetre.
3. heat-conduction electric insulation preparation methods as claimed in claim 1 is characterized in that, comprises the steps:
1) resin batching: take by weighing the thermosetting resin each component, stir;
2) take by weighing relevant filler by the weight percent in the claim 1, as for pre-mixing in the encloses container;
3) with resin and filler at Banbury mixer, carry out thorough mixing in mixing roll or the screw extrusion press, process the raw materials mix material;
4) the raw materials mix material is carried out mold pressing or injection moulding, obtain required product.
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