CN104530706A - Graphene reinforced organic silicon heat-conductive material and preparation method thereof - Google Patents
Graphene reinforced organic silicon heat-conductive material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene reinforced organic silicon heat-conductive material. The material is prepared from 15-35 parts of organic silicon resin, 25-55 parts of a heat-conductive agent, 1-7 parts of graphene, 0.1-2 parts of a platinum catalyst, 0.1-2 parts of hydrogen-containing silicone oil, 3-11 parts of a coupling agent, 0.5 parts of a flame retardant and 0-3 parts of a release agent. According to the invention, the graphene, the heat-conductive agent and the organic silicon resin are combined in a certain proportion, and the coupling agent, the hydrogen-containing silicone oil curing agent or other auxiliaries are added to form a formula, so that the heat conducting performance of the organic silicon material can be improved, the mechanical performance of the organic silicon material is improved, and the heat conducting performance of the product is further improved due to addition of the graphene, surfaces of the heat-conductive agent particles can be completely covered by the coupling agent due to the surface treatment mode of the heat-conductive agent in the preparation process, the compatibility of the heat-conductive agent and the organic silicon resin can be improved, and a high-quality high-performance product can be obtained.
Description
Technical field
The present invention relates to a kind of organosilicon macromolecule material and preparation method thereof, specifically a kind of Graphene strengthens organosilicon thermally conductive material and preparation method thereof, belongs to technical field of polymer materials.
Background technology
Organosilicon product with silicon-oxygen (Si-O) key for backbone structure, so organosilicon product has, thermostability is high, weathering resistance is high, electrical apparatus insulation performance, low surface tension and the feature such as low surface energy, physiological inertia, because organosilicon has the performance of these excellences above-mentioned, therefore its range of application widely.It not only uses as the special material of aviation, sophisticated technology, military technique department, and for each department of national economy, its range of application diffuses into: building, electric, weaving, automobile, machinery, leather papermaking, chemical industry light industry, metal and paint, medicine are medical.
Domestic and international investigator has carried out a large amount of research and development and modification to organosilicon thermally conductive material, forms a series of thermal conductive silicon material gradually, as heat-conducting silica gel sheet, joint sealant, heat-conducting silicone grease etc.The research adopting mineral filler (glass fibre, carbon fiber, whisker etc.) to prepare super-high heat-conductive matrix material in recent years more and more receives publicity, and is widely used in electron trade.Graphene, because thermal conductivity is up to 5300 W/mK, be greatly improved, and production technique is simple with making polymeric system performance after organosilicon compound.
Meanwhile, in Electronic Packaging and computer chip, the geometrical dimension of equipment constantly reduces, and energy output but constantly increases, and makes the research of heat-conducting insulation material become more and more important in this field.The easy machine-shaping of general thermally conductive material, cheap, but thermal conductivity is lower.By adding the functional stuffing of high heat conductance in organosilicon material, as aluminium nitride, boron nitride, magnesium oxide and aluminum oxide etc., being expected the heat conductivility significantly improving polymkeric substance, the insulating property of polymkeric substance can be kept again simultaneously.
Prior art has reported preparation and the performance thereof of organosilicon thermally conductive material, but add certain proportion grapheme material, and adopt silicone resin to be matrix, high thermal conducting agent, prepare Graphene enhancing heat conductive insulating matrix material situation by the method for calendering few at home.Therefore, the Graphene that the present invention develops strengthens thermally conductive material and has broad application prospects.
Summary of the invention
The object of this invention is to provide a kind of Graphene and strengthen organosilicon thermally conductive material.
Technical scheme of the present invention is as follows: a kind of Graphene strengthens organosilicon thermally conductive material, be made up of by weight ratio silicone resin 15 ~ 35 parts, thermal conducting agent 25 ~ 55 parts, Graphene 1 ~ 7 part, platinum catalyst 0.1 ~ 2 part, containing hydrogen silicone oil 0.1 ~ 2 part, coupling agent 3 ~ 11 parts, fire retardant 0 ~ 5 part, releasing agent 0 ~ 3 part, adopt following steps preparation:
(1) thermal conducting agent powder is blown into confined reaction indoor, by air blast, powder particle is suspended in reaction chamber along with air flowing, after coupling agent is heated, coupling agent after atomization is sprayed in reaction chamber, stop 30s ~ 1min, after the indoor temperature of charge of question response is cooled to room temperature, takes out, obtain surface treated thermal conducting agent;
(2) surface treated thermal conducting agent, Graphene, silicone resin, fire retardant, releasing agent are loaded Banbury mixer banburying 0.5 ~ 1 hour successively, then dry 5min under vacuum tightness is 0.06MPa, continue banburying more blended 0.5 ~ 1 hour, take out dry 5min under vacuum tightness is 0.06MPa, control Banbury mixer temperature is 180 ~ 220 DEG C of control rotor speeds is 30 ~ 45r/min, blended 10 ~ 15 minutes of banburying, obtains mixing raw material;
(3) mixing raw material after banburying, platinum catalyst, containing hydrogen silicone oil are added dispersator successively, after stirring 0.5 ~ 2 hour, take out material with rotating speed 400 ~ 600r/min, through degasification, calendering, obtained Graphene strengthens organosilicon thermally conductive material;
Wherein, the thickness of described Graphene is 1 ~ 3nm, is of a size of 2 ~ 10 μm.
Described thermal conducting agent can be that one or more in talcum powder, aluminum oxide, silicon oxide, zinc oxide, magnesium oxide, calcium oxide, aluminium nitride, boron nitride, silicon carbide are carried out composite.
Preferably, described thermal conducting agent is that magnesium oxide and aluminium nitride carry out composite according to mass ratio 1:1 ~ 4.
Preferred further, described thermal conducting agent is boron nitride or aluminum oxide.
The hydrogen content of described containing hydrogen silicone oil is 0.1 ~ 1.0%.
Described coupling agent is the one in organic complex, silicane, titanate ester or aluminate coupling agent.
Preferably, described coupling agent is methacryloxypropyl silane coupling agent.
The liquid silicone of silicone resin preferably transparent thickness of the present invention.
The present invention is the features such as, temperature coefficient of viscosity little, compressibility high, gas permeability high, high-low temperature resistant, electric insulation, resistance to oxidation stability, weathering resistance, difficult combustion, hydrophobic, corrosion-resistant, nonpoisonous and tasteless and physiological inertia low based on the surface tension of silicone resin, by certain proportion Graphene and high thermal conducting agent and its combination, and add coupling agent, containing hydrogen silicone oil solidifying agent or other auxiliary agents formation formula, can the heat conductivility of organosilicon material improved simultaneously, strengthen its mechanical property, Graphene add the heat conductivility further increasing product; In preparation process, the surface treatment mode of thermal conducting agent can make the covering of completely coupled dose of thermal conductor particles surface, improves the consistency of thermal conducting agent and silicone resin, obtains the high performance product of high quality.
Embodiment
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment 1 adopts following formula: silicone resin 20 parts, 45 parts, aluminum oxide, Graphene (thickness is 1 ~ 3nm, is of a size of 2 ~ 10 μm) 1 part, platinum catalyst 0.2 part, hydrogen content are containing hydrogen silicone oil 0.3 part, silane coupling agent 5 parts, fire retardant 2 parts, the releasing agent 1 part of 0.4%, prepares as follows:
(1) thermal conducting agent powder is blown into confined reaction indoor, by air blast, powder particle is suspended in reaction chamber along with air flowing, after coupling agent is heated, silane coupling agent after atomization is sprayed in reaction chamber, stop 1min, after the indoor temperature of charge of question response is cooled to room temperature, takes out, obtain surface treated thermal conducting agent;
(2) surface treated thermal conducting agent, Graphene, silicone resin, fire retardant, releasing agent are loaded Banbury mixer banburying 1 hour successively, then dry 5min under vacuum tightness is 0.06MPa, continue banburying more blended 0.5 hour, take out dry 5min under vacuum tightness is 0.06MPa, control Banbury mixer temperature is 180 ~ 220 DEG C of control rotor speeds is 30 ~ 45r/min, blended 10 minutes of banburying, obtains mixing raw material;
(3) mixing raw material after banburying, platinum catalyst, containing hydrogen silicone oil are added dispersator successively, after stirring 2 hours, take out material with rotating speed 500r/min, through degasification, calendering, obtained thickness is that the Graphene of 1.0mm strengthens organosilicon thermally conductive material.
Embodiment 2 adopts the raw material of following weight proportion to prepare Graphene of the present invention enhancing organosilicon thermally conductive material: silicone resin 20 parts, 45 parts, aluminum oxide, Graphene (thickness is 1 ~ 3nm, is of a size of 2 ~ 10 μm) 2 parts, platinum catalyst 0.2 part, hydrogen content are containing hydrogen silicone oil 0.3 part, silane coupling agent 5 parts, fire retardant 2 parts, the releasing agent 1 part of 0.4%, and preparation method is with embodiment 1.
Embodiment 3 adopts the raw material of following weight proportion to prepare Graphene of the present invention enhancing organosilicon thermally conductive material: silicone resin 20 parts, 45 parts, aluminum oxide, Graphene (thickness is 1 ~ 3nm, is of a size of 2 ~ 10 μm) 3 parts, platinum catalyst 0.2 part, hydrogen content are containing hydrogen silicone oil 0.3 part, silane coupling agent 5 parts, fire retardant 2 parts, the releasing agent 1 part of 0.4%, and preparation method is with embodiment 1.
Embodiment 4 adopts the raw material of following weight proportion to prepare Graphene of the present invention enhancing organosilicon thermally conductive material: silicone resin 20 parts, 45 parts, aluminum oxide, Graphene (thickness is 1 ~ 3nm, is of a size of 2 ~ 10 μm) 4 parts, platinum catalyst 0.2 part, hydrogen content are containing hydrogen silicone oil 0.3 part, silane coupling agent 5 parts, fire retardant 2 parts, the releasing agent 1 part of 0.4%, and preparation method is with embodiment 1.
At equivalent environment temperature, the thermally conductive material obtained to embodiment 1 ~ 4 detects, and result is as follows.Result shows, what adopt Graphene in the thermally conductive material that obtains of the present invention adds the thermal conductivity that can improve material, and its other performances also improve.
。
Embodiment 5 adopts the raw material of following weight proportion to prepare Graphene of the present invention enhancing organosilicon thermally conductive material: silicone resin 33 parts, thermal conducting agent (magnesium oxide and aluminium nitride carry out composite according to mass ratio 1:3) 55 parts, Graphene (thickness is 1 ~ 3nm, is of a size of 2 ~ 10 μm) 6 parts, platinum catalyst 0.3 part, hydrogen content are containing hydrogen silicone oil 0.5 part, the titanate coupling agent 11 parts of 1.0%, adopt following steps preparation:
(1) thermal conducting agent powder is blown into confined reaction indoor, by air blast, powder particle is suspended in reaction chamber along with air flowing, by titanate coupling agent with after anhydrous solvent dilution, heating atomization, coupling agent after atomization is sprayed in reaction chamber, stops 30s ~ 1min, after the indoor temperature of charge of question response is cooled to room temperature, take out, obtain surface treated thermal conducting agent;
(2) surface treated thermal conducting agent, Graphene, silicone resin, fire retardant, releasing agent are loaded Banbury mixer banburying 1 hour successively, then dry 5min under vacuum tightness is 0.06MPa, continue banburying more blended 1 hour, take out dry 5min under vacuum tightness is 0.06MPa, control Banbury mixer temperature is 180 ~ 220 DEG C of control rotor speeds is 30 ~ 45r/min, blended 15 minutes of banburying, obtains mixing raw material;
(3) mixing raw material after banburying, platinum catalyst, containing hydrogen silicone oil are added dispersator successively, after stirring 1 hour, take out material with rotating speed 600r/min, through degasification, calendering, obtained Graphene strengthens organosilicon thermally conductive material.
Claims (7)
1. a Graphene strengthens organosilicon thermally conductive material, it is characterized in that: be made up of by weight ratio silicone resin 15 ~ 35 parts, thermal conducting agent 25 ~ 55 parts, Graphene 1 ~ 7 part, platinum catalyst 0.1 ~ 2 part, containing hydrogen silicone oil 0.1 ~ 2 part, coupling agent 3 ~ 11 parts, fire retardant 0 ~ 5 part, releasing agent 0 ~ 3 part, adopt following steps preparation:
(1) thermal conducting agent powder is blown into confined reaction indoor, by air blast, powder particle is suspended in reaction chamber along with air flowing, after coupling agent is heated, coupling agent after atomization is sprayed in reaction chamber, stop 30s ~ 1min, after the indoor temperature of charge of question response is cooled to room temperature, takes out, obtain surface treated thermal conducting agent;
(2) surface treated thermal conducting agent, Graphene, silicone resin, fire retardant, releasing agent are loaded Banbury mixer banburying 0.5 ~ 1 hour successively, then dry 5min under vacuum tightness is 0.06MPa, continue banburying more blended 0.5 ~ 1 hour, take out dry 5min under vacuum tightness is 0.06MPa, control Banbury mixer temperature is 180 ~ 220 DEG C of control rotor speeds is 30 ~ 45r/min, blended 10 ~ 15 minutes of banburying, obtains mixing raw material;
(3) mixing raw material after banburying, platinum catalyst, containing hydrogen silicone oil are added dispersator successively, after stirring 0.5 ~ 2 hour, take out material with rotating speed 400 ~ 600r/min, through degasification, calendering, obtained Graphene strengthens organosilicon thermally conductive material;
Wherein, the thickness of described Graphene is 1 ~ 3nm, is of a size of 2 ~ 10 μm.
2. Graphene according to claim 1 strengthens organosilicon thermally conductive material, it is characterized in that: described thermal conducting agent is that one or more in talcum powder, aluminum oxide, silicon oxide, zinc oxide, magnesium oxide, calcium oxide, aluminium nitride, boron nitride, silicon carbide are carried out composite.
3. Graphene according to claim 1 strengthens organosilicon thermally conductive material, it is characterized in that: described thermal conducting agent is that magnesium oxide and aluminium nitride carry out composite according to mass ratio 1:1 ~ 4.
4. Graphene according to claim 1 and 2 strengthens organosilicon thermally conductive material, it is characterized in that: described thermal conducting agent is boron nitride or aluminum oxide.
5. Graphene according to claim 1 strengthens organosilicon thermally conductive material, it is characterized in that: the hydrogen content of described containing hydrogen silicone oil is 0.1 ~ 1.0%.
6. Graphene according to claim 1 strengthens organosilicon thermally conductive material, it is characterized in that: described coupling agent is a kind of in organic complex, silicane, titanate ester and aluminate coupling agent.
7. the Graphene according to claim 1 or 6 strengthens organosilicon thermally conductive material, it is characterized in that: described coupling agent is methacryloxypropyl silane coupling agent.
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