CN112876850A - High-heat-conductivity composition and heat-conducting film - Google Patents
High-heat-conductivity composition and heat-conducting film Download PDFInfo
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Abstract
The invention discloses a high heat conduction composition and a heat conduction film, and the key points of the technical scheme are as follows: comprises the following components by weight: epoxy modified silicone resin: 20-30 parts of a solvent; polymethoxysiloxane: 15-25 parts; silicone oil: 40-60 parts; curing agent: 5-10 parts; heat-conducting filler: 300-1000 parts; the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are adopted as raw materials, and the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are fully fused to have the following advantages: 1. the organic silicon resin provides heat resistance, and the epoxy modified organic silicon resin and the room temperature curing agent are adopted to improve the heat resistance and the strength; 2. the silicone oil provides the fitting property, so that the heat conduction effect of the invention is better; 3. the curing agent can make the system performance of the invention more stable and not easy to embrittle; 4. the roll-to-roll coating mode enables the process of the invention to be simpler, the production efficiency to be higher and the cost to be lower.
Description
Technical Field
The invention belongs to the field of heat-conducting films, and particularly relates to a high-heat-conductivity composition and a heat-conducting film.
Background
The power of electronic components is getting larger and larger, and the heat dissipation capacity is getting larger and larger; with the arrival of the 5G era, consumer electronics develop towards ultra-thinning, intellectualization and multi-functionalization, and the requirement on heat dissipation is higher due to the rapid increase of power density; the thermal conductivity coefficient (2-20w/mk) of the thermal interface material is far lower than that of a metal radiator (higher than 100w/mk), and the thermal resistance of the interface material is a main reason for poor heat dissipation. The thermal resistance is divided into the thermal resistance of the material (inversely proportional to the thermal conductivity coefficient and proportional to the thickness of the interface material) and the interface thermal resistance (the contact thermal resistance of the interface material and the heat dissipation device, which is related to the attachment of the interface material and the surface of the device); the silica gel material has poor strength, thicker interface material thickness and increased thermal resistance, and meanwhile, the silica gel material has poor adhesiveness and poor fitting property with the surface of a device, so that the interface thermal resistance is large; the existing silica gel material is prepared by vinyl organic siloxane and hydrogen-containing silicone oil through a crosslinking reaction under the catalysis of a platinum compound, but the platinum catalyst has high requirements on the environment (the catalyst is easy to be poisoned) and has high cost. In addition, after the liquid heat-conducting silica gel is heated and formed in the first stage, the cross-linking density of the liquid heat-conducting silica gel is insufficient, and secondary vulcanization is needed to achieve the tensile strength, rebound resilience, hardness, swelling degree, density and thermal stability of the heat-conducting silica gel sheet; the existing silica gel sheet is prepared by a calendering mode, so that the efficiency is low and the manufacturing cost is high.
Disclosure of Invention
The present invention is directed to a highly heat conductive composition and a heat conductive film, which are used to solve the above problems.
In order to achieve the purpose, the invention provides the following technical scheme:
a high heat conduction composition and a heat conduction film comprise the following components in parts by weight:
epoxy modified silicone resin: 20-30 parts of a solvent;
polymethoxysiloxane: 15-25 parts;
silicone oil: 40-60 parts;
curing agent: 5-10 parts;
heat-conducting filler: 300-1000 parts.
Preferably, the silicone oil comprises one or more of methyl silicone oil, hydroxyl silicone oil and methoxyl silicone oil.
Preferably, the curing agent includes one or more of a diethylenetriamine curing agent, a triethylenetetramine curing agent, a tetraethylenepentamine-modified aliphatic polyamine curing agent, a polyamide curing agent, an acid anhydride curing agent, and a dicyandiamide curing agent.
Preferably, the heat-conducting filler comprises one or more of aluminum oxide, magnesium oxide, boron nitride and aluminum nitride, and the particle size of the heat-conducting filler is 0.05-0.8 mm.
Preferably, the preparation process of the epoxy modified silicone resin is as follows:
the method comprises the following steps: preparing the following components by weight: 20-45 parts of methyl phenyl cyclosiloxane mixture, 5-15 parts of organic silicon monomer, 4-10 parts of organic silicon end capping agent, 0.5-2 parts of oxidant and 0.2-0.8 part of reducing agent;
step two: placing the weighed methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end-capping agent in a reaction kettle for fully mixing, and reacting to obtain vinyl-terminated organic silicon resin;
step three: and (3) controlling the temperature of the reaction kettle to be 8 ℃, injecting an oxidant into the vinyl-terminated organic silicon resin prepared in the second step, fully reacting, then injecting a reducing agent, controlling the stirring speed of the reaction kettle to be 150-220r/min, continuously mixing for 10min, then extracting and drying to finally obtain the epoxy modified organic silicon resin.
Preferably, the reaction in the second step includes heating the reaction kettle to 60-100 ℃, then reducing the pressure to remove excess water, continuously performing 45-100min, then adding a catalyst accounting for 0.008-0.05% of the total weight of the methyl phenyl cyclosiloxane mixture, the organosilicon monomer and the organosilicon end capping agent, performing heat preservation reaction for 2-5h, controlling the reaction pH value to be 7, finally filtering by using a filtering device, reducing the pressure, then distilling by using a vacuum distillation kettle, and processing the obtained distillate to obtain the vinyl-terminated organosilicon resin.
Preferably, in the third step, the temperature of the reaction kettle is controlled to be 5-10 ℃ before the reducing agent is added, and the reaction is continuously carried out for 25-60min under heat preservation.
Preferably, the oxidizing agent comprises one or more of hydrogen peroxide solution, peracetic acid solution, sodium dichromate solution, chromic acid solution, nitric acid solution, potassium permanganate solution, ammonium persulfate solution, sodium hypochlorite solution, sodium percarbonate solution, sodium perborate solution, potassium perborate solution, bromine solution and iodine solution; the reducing agent comprises one or more of hydrogen, carbon monoxide, scrap iron and zinc powder.
The invention also provides a heat-conducting film, wherein epoxy modified organic silicon resin, polymethoxysiloxane, silicone oil, a curing agent and a heat-conducting filler are sequentially placed into a stirrer according to the component proportion for fully mixing, mixed slurry is taken out after mixing is finished, the mixed slurry is coated on a carrier film containing a fluoride release agent in a coating mode to obtain the heat-conducting film, and the coating thickness is controlled to be 20-100 micrometers.
Preferably, the coating modes include blade coating, screen printing coating and screen roller printing coating.
Compared with the prior art, the invention has the beneficial effects that:
the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are adopted as raw materials, and the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are fully fused to have the following advantages:
1. the organic silicon resin provides heat resistance, and the epoxy modified organic silicon resin and the room temperature curing agent are adopted to improve the heat resistance and the strength;
2. the silicone oil provides the fitting property, so that the heat conduction effect of the invention is better;
3. the curing agent can make the system performance of the invention more stable and not easy to embrittle;
4. the roll-to-roll coating mode enables the process of the invention to be simpler, the production efficiency to be higher and the cost to be lower.
Drawings
FIG. 1 is a process flow diagram of the epoxy modified silicone resin of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high heat conduction composition and a heat conduction film comprise the following components in parts by weight:
epoxy modified silicone resin: 24 parts of (1);
polymethoxysiloxane: 18 parts of a mixture;
silicone oil: 55 parts of (1);
curing agent: 8 parts of a mixture;
heat-conducting filler: 800 parts.
In this embodiment, it is preferable that the silicone oil includes one or more of methyl silicone oil, hydroxy silicone oil, and methoxy silicone oil.
In this embodiment, the curing agent preferably includes one or more of a diethylenetriamine curing agent, a triethylenetetramine curing agent, a tetraethylenepentamine modifier aliphatic polyamine curing agent, a polyamide curing agent, an acid anhydride curing agent, and a dicyandiamide curing agent.
In this embodiment, preferably, the heat conductive filler includes one or more of aluminum oxide, magnesium oxide, boron nitride, and aluminum nitride, and the particle size of the heat conductive filler is 0.15 mm.
In this embodiment, a preferred preparation process of the epoxy modified silicone resin is as follows:
the method comprises the following steps: preparing the following components by weight: 25 parts of methyl phenyl cyclosiloxane mixture, 8 parts of organic silicon monomer, 6 parts of organic silicon end capping agent, 1.2 parts of oxidant and 0.6 part of reducing agent;
step two: placing the weighed methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end-capping agent in a reaction kettle for fully mixing, and reacting to obtain vinyl-terminated organic silicon resin;
step three: and (3) controlling the temperature of the reaction kettle to be 8 ℃, injecting an oxidant into the vinyl-terminated organic silicon resin prepared in the second step, fully reacting, then injecting a reducing agent, controlling the stirring speed of the reaction kettle to be 150r/min, continuously mixing for 10min, then extracting and drying to finally obtain the epoxy modified organic silicon resin.
The self-made epoxy modified organic silicon resin is adopted, the reaction efficiency can be facilitated, the chemical property of the self-made epoxy modified organic silicon resin is more stable than that purchased in the market, the amount of one component can be adjusted through self-making, the single property is improved, the self-made cost in large-scale use is lower, and the production cost can be reduced.
In this embodiment, preferably, the reaction in the second step includes raising the temperature of the reaction kettle to 85 ℃, then reducing the pressure to remove excess water, continuing for 75min, adding a catalyst accounting for 0.04% of the total weight of the methylphenyl cyclosiloxane mixture, the organosilicon monomer and the organosilicon end-capping reagent, reacting for 3h while maintaining the temperature, controlling the reaction pH to 7, finally filtering by using a filtering device, reducing the pressure, and then distilling by using a vacuum distillation kettle, and processing the obtained distillate to obtain the vinyl-terminated organosilicon resin.
In this embodiment, preferably, in the third step, the temperature of the reaction kettle is controlled to be 9 ℃ before the reducing agent is added, and the reaction is kept for 50 min.
In this embodiment, preferably, the oxidizing agent includes one or more of a hydrogen peroxide solution, a peracetic acid solution, a sodium dichromate solution, a chromic acid solution, a nitric acid solution, a potassium permanganate solution, an ammonium persulfate solution, a sodium hypochlorite solution, a sodium percarbonate solution, a sodium perborate solution, a potassium perborate solution, a bromine solution, and an iodine solution; the reducing agent comprises one or more of hydrogen, carbon monoxide, scrap iron and zinc powder.
The invention also provides a heat-conducting film, wherein epoxy modified organic silicon resin, polymethoxysiloxane, silicone oil, a curing agent and a heat-conducting filler are sequentially placed into a stirrer according to the component proportion for fully mixing, mixed slurry is taken out after mixing is finished, the mixed slurry is coated on a carrier film containing a fluoride release agent in a coating mode to obtain the heat-conducting film, and the coating thickness is controlled to be 50 micrometers.
In this embodiment, the coating method preferably includes blade coating, screen printing coating, and screen roller printing coating.
The working principle and the using process of the invention are as follows:
the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are adopted as raw materials, and the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are fully fused to have the following advantages:
1. the organic silicon resin provides heat resistance, and the epoxy modified organic silicon resin and the room temperature curing agent are adopted to improve the heat resistance and the strength;
2. the silicone oil provides the fitting property, so that the heat conduction effect of the invention is better;
3. the curing agent can make the system performance of the invention more stable and not easy to embrittle;
4. the roll-to-roll coating mode enables the process of the invention to be simpler, the production efficiency to be higher and the cost to be lower.
Example 2
A high heat conduction composition and a heat conduction film comprise the following components in parts by weight:
epoxy modified silicone resin: 30 parts of (1);
polymethoxysiloxane: 25 parts of (1);
silicone oil: 60 parts;
curing agent: 10 parts of (A);
heat-conducting filler: 300 parts.
In this embodiment, it is preferable that the silicone oil includes one or more of methyl silicone oil, hydroxy silicone oil, and methoxy silicone oil.
In this embodiment, the curing agent preferably includes one or more of a diethylenetriamine curing agent, a triethylenetetramine curing agent, a tetraethylenepentamine modifier aliphatic polyamine curing agent, a polyamide curing agent, an acid anhydride curing agent, and a dicyandiamide curing agent.
In this embodiment, preferably, the heat conductive filler includes one or more of aluminum oxide, magnesium oxide, boron nitride, and aluminum nitride, and the particle size of the heat conductive filler is 0.8 mm.
In this embodiment, a preferred preparation process of the epoxy modified silicone resin is as follows:
the method comprises the following steps: preparing the following components by weight: 25 parts of methyl phenyl cyclosiloxane mixture, 5 parts of organic silicon monomer, 4 parts of organic silicon end capping agent, 0.5 part of oxidant and 0.2 part of reducing agent;
step two: placing the weighed methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end-capping agent in a reaction kettle for fully mixing, and reacting to obtain vinyl-terminated organic silicon resin;
step three: and (3) controlling the temperature of the reaction kettle to be 8 ℃, injecting an oxidant into the vinyl-terminated organic silicon resin prepared in the second step, fully reacting, then injecting a reducing agent, controlling the stirring speed of the reaction kettle to be 150r/min, continuously mixing for 10min, then extracting and drying to finally obtain the epoxy modified organic silicon resin.
In this embodiment, preferably, the reaction in the second step includes raising the temperature of the reaction kettle to 60 ℃, then reducing the pressure to remove excess water, continuously performing 45min, then adding a catalyst accounting for 0.008% of the total weight of the methylphenyl cyclosiloxane mixture, the organosilicon monomer and the organosilicon end-capping reagent, performing a heat preservation reaction for 4h, controlling the reaction pH value to 7, finally filtering by using a filtering device, reducing the pressure, and then distilling by using a vacuum distillation kettle, and processing the obtained distillate to obtain the vinyl-terminated organosilicon resin.
In this embodiment, preferably, in the third step, the temperature of the reaction kettle is controlled to be 5 ℃ before the reducing agent is added, and the reaction is kept for 25 min.
In this embodiment, preferably, the oxidizing agent includes one or more of a hydrogen peroxide solution, a peracetic acid solution, a sodium dichromate solution, a chromic acid solution, a nitric acid solution, a potassium permanganate solution, an ammonium persulfate solution, a sodium hypochlorite solution, a sodium percarbonate solution, a sodium perborate solution, a potassium perborate solution, a bromine solution, and an iodine solution; the reducing agent comprises one or more of hydrogen, carbon monoxide, scrap iron and zinc powder.
The invention also provides a heat-conducting film, wherein epoxy modified organic silicon resin, polymethoxysiloxane, silicone oil, a curing agent and a heat-conducting filler are sequentially placed into a stirrer according to the component proportion for fully mixing, mixed slurry is taken out after mixing is finished, the mixed slurry is coated on a carrier film containing a fluoride release agent in a coating mode to obtain the heat-conducting film, and the coating thickness is controlled to be 40 micrometers.
In this embodiment, the coating method preferably includes blade coating, screen printing coating, and screen roller printing coating.
The working principle and the using process of the invention are as follows:
the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are adopted as raw materials, and the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are fully fused to have the following advantages:
1. the organic silicon resin provides heat resistance, and the epoxy modified organic silicon resin and the room temperature curing agent are adopted to improve the heat resistance and the strength;
2. the silicone oil provides the fitting property, so that the heat conduction effect of the invention is better;
3. the curing agent can make the system performance of the invention more stable and not easy to embrittle;
4. the roll-to-roll coating mode enables the process of the invention to be simpler, the production efficiency to be higher and the cost to be lower.
Example 3
A high heat conduction composition and a heat conduction film comprise the following components in parts by weight:
epoxy modified silicone resin: 20 parts of (1);
polymethoxysiloxane: 15 parts of (1);
silicone oil: 40 parts of a mixture;
curing agent: 5 parts of a mixture;
heat-conducting filler: 500 parts.
In this embodiment, it is preferable that the silicone oil includes one or more of methyl silicone oil, hydroxy silicone oil, and methoxy silicone oil.
In this embodiment, the curing agent preferably includes one or more of a diethylenetriamine curing agent, a triethylenetetramine curing agent, a tetraethylenepentamine modifier aliphatic polyamine curing agent, a polyamide curing agent, an acid anhydride curing agent, and a dicyandiamide curing agent.
In this embodiment, preferably, the heat conductive filler includes one or more of aluminum oxide, magnesium oxide, boron nitride, and aluminum nitride, and the particle size of the heat conductive filler is 0.8 mm.
In this embodiment, a preferred preparation process of the epoxy modified silicone resin is as follows:
the method comprises the following steps: preparing the following components by weight: 20 parts of methyl phenyl cyclosiloxane mixture, 8 parts of organic silicon monomer, 10 parts of organic silicon end capping agent, 0.5 part of oxidant and 0.2 part of reducing agent;
step two: placing the weighed methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end-capping agent in a reaction kettle for fully mixing, and reacting to obtain vinyl-terminated organic silicon resin;
step three: and (3) controlling the temperature of the reaction kettle to be 8 ℃, injecting an oxidant into the vinyl-terminated organic silicon resin prepared in the second step, fully reacting, then injecting a reducing agent, controlling the stirring speed of the reaction kettle to be 220r/min, continuously mixing for 10min, then extracting and drying to finally obtain the epoxy modified organic silicon resin.
In this embodiment, preferably, the reaction in the second step includes raising the temperature of the reaction kettle to 100 ℃, then reducing the pressure to remove excess water, continuously performing the reaction for 100min, then adding a catalyst accounting for 0.008% of the total weight of the methylphenyl cyclosiloxane mixture, the organosilicon monomer and the organosilicon end capping agent, performing a heat preservation reaction for 5h, controlling the reaction pH value to 7, finally filtering by using a filtering device, reducing the pressure, then distilling by using a vacuum distillation kettle, and processing the obtained distillate to obtain the vinyl-terminated organosilicon resin.
In this embodiment, preferably, in the third step, the temperature of the reaction kettle is controlled to 10 ℃ before the reducing agent is added, and the reaction is kept for 60 min.
In this embodiment, preferably, the oxidizing agent includes one or more of a hydrogen peroxide solution, a peracetic acid solution, a sodium dichromate solution, a chromic acid solution, a nitric acid solution, a potassium permanganate solution, an ammonium persulfate solution, a sodium hypochlorite solution, a sodium percarbonate solution, a sodium perborate solution, a potassium perborate solution, a bromine solution, and an iodine solution; the reducing agent comprises one or more of hydrogen, carbon monoxide, scrap iron and zinc powder.
The invention also provides a heat-conducting film, wherein epoxy modified organic silicon resin, polymethoxysiloxane, silicone oil, a curing agent and a heat-conducting filler are sequentially placed into a stirrer according to the component proportion for fully mixing, mixed slurry is taken out after mixing is finished, the mixed slurry is coated on a carrier film containing a fluoride release agent in a coating mode to obtain the heat-conducting film, and the coating thickness is controlled to be 20 micrometers.
In this embodiment, the coating method preferably includes blade coating, screen printing coating, and screen roller printing coating.
The working principle and the using process of the invention are as follows:
the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are adopted as raw materials, and the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are fully fused to have the following advantages:
1. the organic silicon resin provides heat resistance, and the epoxy modified organic silicon resin and the room temperature curing agent are adopted to improve the heat resistance and the strength;
2. the silicone oil provides the fitting property, so that the heat conduction effect of the invention is better;
3. the curing agent can make the system performance of the invention more stable and not easy to embrittle;
4. the roll-to-roll coating mode enables the process of the invention to be simpler, the production efficiency to be higher and the cost to be lower.
Example 4
A high heat conduction composition and a heat conduction film comprise the following components in parts by weight:
epoxy modified silicone resin: 30 parts of (1);
polymethoxysiloxane: 25 parts of (1);
silicone oil: 60 parts;
curing agent: 10 parts of (A);
heat-conducting filler: 800 parts.
In this embodiment, it is preferable that the silicone oil includes one or more of methyl silicone oil, hydroxy silicone oil, and methoxy silicone oil.
In this embodiment, the curing agent preferably includes one or more of a diethylenetriamine curing agent, a triethylenetetramine curing agent, a tetraethylenepentamine modifier aliphatic polyamine curing agent, a polyamide curing agent, an acid anhydride curing agent, and a dicyandiamide curing agent.
In this embodiment, preferably, the heat conductive filler includes one or more of aluminum oxide, magnesium oxide, boron nitride, and aluminum nitride, and the particle size of the heat conductive filler is 0.05 mm.
In this embodiment, a preferred preparation process of the epoxy modified silicone resin is as follows:
the method comprises the following steps: preparing the following components by weight: 45 parts of methyl phenyl cyclosiloxane mixture, 15 parts of organic silicon monomer, 10 parts of organic silicon end capping agent, 2 parts of oxidant and 0.8 part of reducing agent;
step two: placing the weighed methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end-capping agent in a reaction kettle for fully mixing, and reacting to obtain vinyl-terminated organic silicon resin;
step three: and (3) controlling the temperature of the reaction kettle to be 8 ℃, injecting an oxidant into the vinyl-terminated organic silicon resin prepared in the second step, fully reacting, then injecting a reducing agent, controlling the stirring speed of the reaction kettle to be 150r/min, continuously mixing for 10min, then extracting and drying to finally obtain the epoxy modified organic silicon resin.
In this embodiment, preferably, the reaction in the second step includes raising the temperature of the reaction kettle to 60 ℃, then reducing the pressure to remove excess water, continuing for 45min, adding a catalyst accounting for 0.05% of the total weight of the methylphenyl cyclosiloxane mixture, the organosilicon monomer and the organosilicon end-capping reagent, reacting for 4h while maintaining the temperature, controlling the reaction pH to 7, finally filtering by using a filtering device, reducing the pressure, and then distilling by using a vacuum distillation kettle, and processing the obtained distillate to obtain the vinyl-terminated organosilicon resin.
In this embodiment, preferably, in the third step, the temperature of the reaction kettle is controlled to be 8 ℃ before the reducing agent is added, and the reaction is kept for 50 min.
In this embodiment, preferably, the oxidizing agent includes one or more of a hydrogen peroxide solution, a peracetic acid solution, a sodium dichromate solution, a chromic acid solution, a nitric acid solution, a potassium permanganate solution, an ammonium persulfate solution, a sodium hypochlorite solution, a sodium percarbonate solution, a sodium perborate solution, a potassium perborate solution, a bromine solution, and an iodine solution; the reducing agent comprises one or more of hydrogen, carbon monoxide, scrap iron and zinc powder.
The invention also provides a heat-conducting film, wherein epoxy modified organic silicon resin, polymethoxysiloxane, silicone oil, a curing agent and a heat-conducting filler are sequentially placed into a stirrer according to the component proportion for fully mixing, mixed slurry is taken out after mixing is finished, the mixed slurry is coated on a carrier film containing a fluoride release agent in a coating mode to obtain the heat-conducting film, and the coating thickness is controlled to be 30 micrometers.
In this embodiment, the coating method preferably includes blade coating, screen printing coating, and screen roller printing coating.
The working principle and the using process of the invention are as follows:
the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are adopted as raw materials, and the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler are fully fused to have the following advantages:
1. the organic silicon resin provides heat resistance, and the epoxy modified organic silicon resin and the room temperature curing agent are adopted to improve the heat resistance and the strength;
2. the silicone oil provides the fitting property, so that the heat conduction effect of the invention is better;
3. the curing agent can make the system performance of the invention more stable and not easy to embrittle;
4. the roll-to-roll coating mode enables the process of the invention to be simpler, the production efficiency to be higher and the cost to be lower.
The heat conductive films prepared in examples 1 to 4 and a general film were subjected to a performance test:
the specific method comprises the following steps: the films prepared in examples 1 to 4 with the same specification and the common film are respectively selected, and then the films are sequentially subjected to heat resistance, thermal conductivity, wear resistance, hardness, warping degree and luminescence test, and for convenience of comparison, the test results are shown in the following table:
| heat resistance | Thermal conductivity | Wear resistance | Hardness of | Degree of warp | Luminescence property | |
| Example 1 | 100 | 100 | 100 | 100 | 100 | 100 |
| Example 2 | 99.7 | 98.7 | 98.5 | 99.8 | 99.2 | 98.7 |
| Example 3 | 98.9 | 96.5 | 98.9 | 97.8 | 98.9 | 98.6 |
| Example 4 | 98.6 | 94.6 | 99.8 | 98.3 | 98.2 | 99.7 |
| Plain film | 79.8 | 82.7 | 76.8 | 65.8 | 66.2 | 68.2 |
The larger the numerical value in the table represents the better the performance;
from the above table, it can be seen that the films prepared by the present invention are superior to the conventional films in all properties, and the films prepared in example 1 are optimal in all properties.
The above common films can be selected from Chinese patent with publication number CN 107523237A: a heat-conducting film prepared from the heat-conducting film.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The high-thermal-conductivity composition is characterized by comprising the following components in parts by weight:
epoxy modified silicone resin: 20-30 parts of a solvent;
polymethoxysiloxane: 15-25 parts;
silicone oil: 40-60 parts;
curing agent: 5-10 parts;
heat-conducting filler: 300-1000 parts.
2. A highly thermally conductive composition according to claim 1, wherein: the silicone oil comprises one or more of methyl silicone oil, hydroxyl silicone oil and methoxyl silicone oil.
3. A highly thermally conductive composition according to claim 1, wherein: the curing agent comprises one or more of a diethylenetriamine curing agent, a triethylenetetramine curing agent, a tetraethylenepentamine modifier aliphatic polyamine curing agent, a polyamide curing agent, an acid anhydride curing agent and a dicyandiamide curing agent.
4. A highly thermally conductive composition according to claim 1, wherein: the heat-conducting filler comprises one or more of aluminum oxide, magnesium oxide, boron nitride and aluminum nitride, and the particle size of the heat-conducting filler is 0.05-0.8 mm.
5. A highly thermally conductive composition according to claim 1, wherein: the preparation process of the epoxy modified organic silicon resin comprises the following steps:
the method comprises the following steps: preparing the following components by weight: 20-45 parts of methyl phenyl cyclosiloxane mixture, 5-15 parts of organic silicon monomer, 4-10 parts of organic silicon end capping agent, 0.5-2 parts of oxidant and 0.2-0.8 part of reducing agent;
step two: placing the weighed methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end-capping agent in a reaction kettle for fully mixing, and reacting to obtain vinyl-terminated organic silicon resin;
step three: and (3) controlling the temperature of the reaction kettle to be 8 ℃, injecting an oxidant into the vinyl-terminated organic silicon resin prepared in the second step, fully reacting, then injecting a reducing agent, controlling the stirring speed of the reaction kettle to be 150-220r/min, continuously mixing for 10min, then extracting and drying to finally obtain the epoxy modified organic silicon resin.
6. A highly thermally conductive composition according to claim 1, wherein: and the reaction in the second step comprises the steps of heating the reaction kettle to 60-100 ℃, reducing the pressure to remove excessive water, continuously performing 45-100min, adding a catalyst accounting for 0.008-0.05% of the total weight of the methyl phenyl cyclosiloxane mixture, the organic silicon monomer and the organic silicon end capping agent, performing heat preservation reaction for 2-5h, controlling the reaction pH value to be 7, finally filtering by using a filtering device, reducing the pressure, and distilling by using a vacuum distillation kettle to obtain distillate, and processing the obtained distillate to obtain the vinyl-terminated organic silicon resin.
7. A highly thermally conductive composition according to claim 1, wherein: and in the third step, the temperature of the reaction kettle is controlled to be 5-10 ℃ before the reducing agent is added, and the reaction is continuously carried out for 25-60min under the condition of heat preservation.
8. A highly thermally conductive composition according to claim 1, wherein: the oxidant comprises one or more of hydrogen peroxide solution, peracetic acid solution, sodium dichromate solution, chromic acid solution, nitric acid solution, potassium permanganate solution, ammonium persulfate solution, sodium hypochlorite solution, sodium percarbonate solution, sodium perborate solution, potassium perborate solution, bromine solution and iodine solution; the reducing agent comprises one or more of hydrogen, carbon monoxide, scrap iron and zinc powder.
9. A heat-conducting film is characterized in that: and (2) sequentially putting the epoxy modified organic silicon resin, the polymethoxysiloxane, the silicone oil, the curing agent and the heat-conducting filler into a stirrer according to the component proportion for fully mixing, taking out the mixed slurry after mixing is finished, coating the mixed slurry on a carrier film containing the fluoride release agent in a coating mode to obtain the heat-conducting film, and controlling the coating thickness to be 20-100 microns.
10. The thermally conductive film of claim 9, wherein: the coating modes comprise blade coating, screen printing coating and screen roller printing coating.
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