CN111286308A - Graphene heat-conducting silicone grease and preparation method thereof - Google Patents
Graphene heat-conducting silicone grease and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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Abstract
The invention provides graphene heat-conducting silicone grease and a preparation method thereof. The graphene heat-conducting silicone grease provided by the invention comprises a graphene heat-conducting material containing benzene rings, other fillers and an auxiliary agent, wherein the graphene heat-conducting material has the following structural formula:
x is a graphene structure, R2And R3Is a hydrogen atom, a carbon chain or an aromatic ring structure; the R is1Is a carbon chain with the carbon atom number between 0 and 5, and a is more than or equal to 1. The graphene heat-conducting silicone grease and the preparation method thereof have a good heat-conducting effect.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to graphene heat conduction silicone grease and a preparation method thereof.
Background
The existing preparation methods of graphene heat-conducting silicone grease can be divided into two types: a, directly utilizing the excellent thermal conductivity and the large length-width ratio of graphene as a thermal bridge to connect other heat-conducting fillers; and b, treating the graphene powder by using a wetting agent, a dispersing agent and a surface treating agent, so that the compatibility of the graphene powder in an organic silicon system is improved, the addition amount is increased, and the agglomeration is reduced. For the first utilization mode, the characteristic that the graphene material is neither hydrophilic nor oleophilic is ignored, the viscosity of the heat-conducting silicone grease can be increased violently by adding a small amount of graphene powder/graphene sheets, and the maximum addition amount is further limited, so that the heat conductivity coefficient of the final product is not high. As for the second mode, the conventional surface treatment agent uses alkoxysilane, a coating type auxiliary agent such as stearic acid, etc., and the effect between the alkoxysilane, the coating type auxiliary agent and the graphene powder or graphene sheet is surface coating or hydrogen bond formation or dehydration condensation between hydroxyl groups, and there is no other beneficial effect. Materials such as graphene powder and graphene sheets have inevitable defects in the preparation process, so that the heat conduction effect is poor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the graphene heat-conducting silicone grease with a good heat-conducting effect and the preparation method thereof.
The invention provides graphene heat-conducting silicone grease which comprises a graphene heat-conducting material containing benzene rings, other fillers and an auxiliary agent, wherein the structure of the graphene heat-conducting material has the following structural formula:
x is a graphene structure, R2And R3Is a hydrogen atom, a carbon chain or an aromatic ring structure; the R is1Is a carbon chain with the carbon atom number between 0 and 5, and a is more than or equal to 1.
Preferably, the graphene heat conduction material is 1-110 parts, the other filler is 200-900 parts, and the auxiliary agent is 0.1-10 parts.
Preferably, the carbon-oxygen ratio of the graphene heat conduction material is (50-1000): 1.
preferably, the other thermally conductive filler includes one or more of zinc oxide, aluminum oxide, magnesium oxide, copper powder, silver powder, zinc powder, aluminum powder, and carbon nanotubes.
Preferably, the auxiliary agent comprises one or more of a polyether type defoaming agent, a coating type auxiliary agent and a wetting and dispersing agent.
The invention also provides a preparation method of the graphene heat-conducting silicone grease, which comprises the following steps:
(1) mixing graphene and organic silicon containing benzene rings to obtain a mixture;
(2) adding other heat-conducting fillers and auxiliaries to the mixture.
Preferably, the weight ratio of the organosilicon containing benzene rings to the graphene is (1-20): 1, the carbon-oxygen ratio of the graphene is (8-50): 1.
preferably, the benzene ring-containing organosilicon contains Si-H bonds.
Preferably, in the step (1), after the graphene and the organosilicon containing a benzene ring are mixed, a step of adding a hydrosilation compound is further included, and the hydrosilation compound includes one or more of alkylhydrosilanes such as trimethylhydrosilane and triethylhydrosilane, tetramethylcyclotetrasiloxane, a hydrosiloxane ring body, high-hydrogen silicone oil, phenyltrimethylcyclotetrasiloxane and phenyl-hydrogen silicone oil.
Preferably, the organosilicon containing benzene rings comprises one or more of 1,3, 5-trimethyl-1, 3, 5-triphenyl trisiloxane ring body, 1,3,5, 7-tetramethyl-1, 3,5, 7-tetraphenyl tetrasiloxane ring body, phenyl trimethoxy silane, diphenyl dimethoxy silane and methyl phenyl siloxane ring body.
The graphene heat-conducting silicone grease and the heat-conducting silicone grease prepared by the preparation method provided by the invention have a good heat-conducting effect.
Detailed Description
The technical solutions of the present invention are further described in detail with reference to specific examples so that those skilled in the art can better understand the present invention and can implement the present invention, but the examples are not intended to limit the present invention.
The embodiment of the invention provides graphene heat-conducting silicone grease which comprises a graphene heat-conducting material containing benzene rings, other fillers and an auxiliary agent, wherein the structure of the graphene heat-conducting material has the following structural formula (shown in formula 1):
x is a graphene structure, a is more than or equal to 1, which indicates that the graphene heat conduction material of the embodiment is bonded with one or more structures containing benzene rings on the graphene layer structure. For example as shown in formula 2.
R2Is a hydrogen atom, a carbon chain or an aromatic ring structure; r3Is a hydrogen atom, a carbon chain or an aromatic ring structure; r1Is a carbon chain with the number of carbon atoms between 0 and 5.
In the graphite alkene heat conduction material of this embodiment, the bonding has the structure that contains the benzene ring on the graphite alkene layer, through the conjugation between graphite alkene layer and the benzene ring, strengthens the affinity between organosilicon molecule and the graphite alkene, contains the benzene ring in the graphite alkene heat conduction material, can promote the graphite alkene layer and the separation between the layer of graphite alkene, and effort between reinforcing organosilicon material and the graphite alkene layer slows down the reunion and subside that the attraction between the graphite alkene layer causes. The heat conductivity coefficient of the obtained heat-conducting silicone grease is improved to 3.6W/(m.K) from 1.5W/(m.K), meanwhile, the viscosity is reduced by 50 percent, and the heat-conducting property and the operating property of the heat-conducting silicone grease are greatly improved.
In a preferred embodiment, the graphene heat conduction material comprises 1-110 parts of graphene heat conduction materials, 20-900 parts of other fillers and 0.1-10 parts of auxiliaries. In a further preferred embodiment, the graphene heat conduction material is 10-60 parts, the other fillers are 50-300 parts, and the auxiliary agent is 1-10 parts.
In a preferred embodiment, the carbon-to-oxygen ratio of the graphene thermal conductive material is (8-1000): 1. preferably (50-1000): 1 or (8-100): 1, the more reasonable carbon-oxygen ratio realizes that the heat-conducting silicone grease has better heat-conducting effect.
In a preferred embodiment, the other thermally conductive filler includes one or more of zinc oxide, aluminum oxide, magnesium oxide, copper powder, silver powder, zinc powder, aluminum powder, and carbon nanotubes. Other thermally conductive fillers may be spherical, spheroidal, acicular, or irregular.
The auxiliary agent comprises one or more of polyether defoaming agent, coating auxiliary agent and wetting dispersant, and the coating auxiliary agent comprises stearic acid, sodium stearate, magnesium stearate and the like.
The embodiment of the invention also provides a preparation method of the graphene heat-conducting silicone grease, which comprises the following steps:
(1) mixing graphene and organic silicon containing benzene rings to obtain a mixture, wherein the graphene is graphene micro-sheets or graphene powder. In a preferred embodiment, the organosilicon containing benzene rings and the graphene are mixed according to the weight ratio of (1-20): 1, stirring and carrying out ultrasonic treatment, wherein the carbon-oxygen ratio of the graphene is controlled to be (8-50): 1.
(2) other thermally conductive fillers and auxiliaries are added to the mixture.
In a preferred embodiment, the weight ratio of the organosilicon containing benzene rings to the graphene is (1-10): 1, preferably 1 to 5: 1.
in a preferred embodiment, the carbon to oxygen ratio of the graphene is (8-50): 1. the carbon-oxygen ratio of the graphene is reasonably controlled, and the organic silicon containing benzene rings is matched in a reasonable proportion, so that the benzene rings and the graphene in the prepared graphene heat conduction material can better realize pi-pi conjugation.
In a preferred embodiment, the benzene ring-containing silicone contains Si-H bonds. In a further preferred embodiment, the ratio of the number of moles of Si-H bonds to the number of moles of oxygen atoms in the graphene is (0.5-3): 1. c ═ O double bond in the reduction graphite alkene that can be better plays better repair effect for graphite alkene heat conduction material has better coefficient of heat conductivity.
In a further preferred embodiment, the silicone containing a benzene ring and containing Si-H bonds can be a small molecule material comprising 1,3, 5-trimethyl-1, 3, 5-triphenyltrisiloxane rings, 1,3,5, 7-tetramethyl-1, 3,5, 7-tetraphenyltetrasiloxane rings, or a mixed ring of the two. The method not only can fully utilize the heat in the synthetic process of the organic silicon polymer and reduce the preparation time, but also can realize better dispersion effect by utilizing the characteristic of low viscosity of small molecules.
In another preferred embodiment, the step (1) further comprises adding a hydrosilation compound containing Si — H bonds after mixing the graphene and the benzene ring-containing organosilicon. In a preferred embodiment, the silicon-containing material comprises 80-120 parts by weight of organosilicon containing benzene rings, 20-50 parts by weight of graphene and 10-60 parts by weight of hydrosilicon compound.
In a further preferred embodiment, the ratio of the number of moles of Si-H bonds to the number of moles of oxygen atoms in the graphene is (0.5-3): 1. c ═ O double bond in the reduction graphite alkene that can be better plays better repair effect for graphite alkene heat conduction material has better coefficient of heat conductivity.
In a further preferred embodiment, after the silicon hydride is added, the reaction is carried out for 0.5 to 3 hours at the temperature of between 25 and 40 ℃, the ultrasound is turned off, the temperature is increased to between 80 and 150 ℃, the vacuum pumping is carried out for 2 to 5 hours, and the volatile matter is removed, so that the graphene heat conduction material is obtained.
The structural formula of the hydrosilyl compound in this embodiment can be as shown in formula 3.
In the formula 3, R4Is a carbon chain of 0 to 3 lengths, R5、R6It may be a hydrogen atom, a benzene ring, a carbon chain or a siloxane segment.
The hydrogen atoms on the Si-H bond have electronegativity and strong reducibility, and can perform oxidation-reduction reaction with hydroxyl, epoxy, carbonyl, carboxyl and the like in graphene, so that the defects caused by oxygen atoms on the graphene layer are partially repaired, C-O double bonds in the graphene are completely reduced to C-OH and even C-H, and partial C-OH is reduced to C-H, so that the prepared graphene heat conduction material has a good heat conduction coefficient.
In a more preferred embodiment, the hydrosilane compound may be a silane, for example, an alkylhydrosilane such as trimethylhydrosilane or triethylhydrosilane, a siloxane containing a plurality of active hydrogens such as a hydrosiloxane ring body (trimethylcyclotrisiloxane, tetramethylcyclotetrasiloxane, etc.), a high-hydrogen silicone oil, or a phenyltrimethylcyclotetrasiloxane containing both a benzene ring and an active hydrogen, or a low-viscosity (10-200 mps) phenylhydrosiloxane. The hydrosilation compound may also be a combination of any of the above.
In a preferred embodiment, the silicone containing a benzene ring comprises one or more of 1,3, 5-trimethyl-1, 3,5, triphenyltrisiloxane ring, 1,3,5, 7-tetramethyl-1, 3,5, 7-tetraphenyltetrasiloxane ring, Phenyltrimethoxysilane (PTMS), diphenyldimethoxysilane (DPDS), methylphenylsiloxane ring.
In a preferred embodiment, in the step (1), after the graphene and the organosilicon containing benzene rings are mixed, the temperature is controlled to be 60-80 ℃, and a catalyst is added, wherein the catalyst is a small-molecule cationic catalyst. The small molecule cationic catalyst comprises one or more of tetramethylammonium hydroxide, tetraethylammonium and isopropanol. The addition of small molecular cations can be used as a charge control agent to enable the graphene layer to carry partial positive charges, so that the attractive force between the graphene layers can be weakened, and small-volume cations can enter the graphene layers through intercalation to further separate the graphene layers. And after the graphene heat conduction material is prepared, the small molecules are conveniently removed, and the whole heat conduction system is not affected.
The preparation method of the graphene thermal conductive silicone grease provided by the embodiment comprises the following steps:
(1) mixing graphene and organic silicon containing benzene rings, and stirring and carrying out ultrasonic treatment, wherein the carbon-oxygen ratio of the graphene is controlled to be (8-50): 1, the graphene is graphene nanoplatelets or graphene powder.
(2) Controlling the temperature at 60-80 ℃, and adding a catalyst which is a micromolecular cationic catalyst. Stirring and ultrasonic treatment are continued for 0.5-10 h.
(3) Adding silicon hydride to react at 25-40 deg.c for 0.5-3 hr. And (4) stopping ultrasound, raising the temperature to 80-150 ℃, vacuumizing for 2-5 h, and removing volatile matters to obtain the graphene heat conduction material.
(4) And adding other heat-conducting fillers and auxiliaries into the graphene heat-conducting material.
The foregoing disclosure is further illustrated by the following specific examples in order to provide further understanding and appreciation of the invention and to highlight its progressive effects.
Example 1
Preparing a graphene heat conduction material:
(1) 57 parts of phenyl silicone oil with the viscosity of 200mps and 30 parts of graphene powder with the carbon-oxygen ratio of 20:1 are mixed, and stirring and ultrasonic processing are carried out.
(2) The temperature is controlled between 60 ℃ and 80 ℃, and 0.5 part of tetrapropylammonium hydroxide is added. Stirring and ultrasonic treatment are continued for 2-10 h.
(3) The hydrosil (43 parts diphenylmethylsilane) was added so that the ratio of the number of moles of Si-H bonds to the number of moles of oxygen atoms on the graphene material was (0.8-1.6): 1. Introducing nitrogen, continuously stirring for 0.5-3 h, and keeping the temperature at 25-40 ℃ during the stirring.
(4) And (4) stopping ultrasound, raising the temperature to 80-150 ℃, vacuumizing for 2-5 h, and removing volatile matters to obtain the graphene heat conduction material.
Preparing heat-conducting silicone grease:
(5) adding other heat-conducting fillers (α spherical alumina with the average particle size of 20 mu m) and an auxiliary agent (polyether type defoaming agent) into the step (4), wherein the weight ratio of the graphene heat-conducting materials, the other heat-conducting fillers and the auxiliary agent is 40: 160: 5, adding 1 part of KH550, heating to 60-80 ℃, vacuumizing, and slowly stirring for 1-2 hours.
Example 2
(1) 80 parts of phenyl silicone oil with the viscosity of 200mps and 30 parts of graphene powder with the carbon-oxygen ratio of 10:1 are mixed, and stirring and ultrasonic processing are carried out.
(2) The temperature is controlled between 60 ℃ and 80 ℃, and 0.5 part of tetrapropylammonium hydroxide is added.
(3) The hydrosilation compound (20 parts diphenylsilane) was added so that the ratio of the number of moles of Si-H bonds to the number of moles of oxygen atoms on the graphene material was (0.8-1.6): 1. Introducing nitrogen, continuously stirring for 0.5-3 h, and keeping the temperature at 25-40 ℃ during the stirring.
(4) And (4) stopping ultrasound, raising the temperature to 80-150 ℃, vacuumizing for 2-5 h, and removing volatile matters to obtain the graphene heat conduction material.
Preparing heat-conducting silicone grease:
(5) adding other heat-conducting fillers (α spherical alumina with the average particle size of 20 mu m) and an auxiliary agent (polyether type defoaming agent) into the step (4), wherein the weight ratio of the graphene heat-conducting materials, the other heat-conducting fillers and the auxiliary agent is 20: 160: 5, adding 1 part of KH550, heating to 60-80 ℃, vacuumizing, and slowly stirring for 1-2 hours.
Example 3
(1) 30 parts of phenyl silicone oil with the viscosity of 200mps, 27 parts of dimethyl silicone oil with the viscosity of 100mps and 30 parts of graphene powder with the carbon-oxygen ratio of 10:1 are mixed, and stirring and ultrasonic processing are carried out.
(2) The temperature is controlled between 60 ℃ and 80 ℃, and 0.5 part of tetrapropylammonium hydroxide is added.
(3) Adding hydrosilicon compound (43 parts of diphenylmethylsilane), introducing nitrogen, continuously stirring for 0.5-3 h, and keeping the temperature at 25-40 ℃ during the stirring.
(4) And (4) stopping ultrasound, raising the temperature to 80-150 ℃, vacuumizing for 2-5 h, and removing volatile matters to obtain the graphene heat conduction material.
Preparing heat-conducting silicone grease:
(5) adding other heat-conducting fillers (α spherical alumina with the average particle size of 20 mu m) and an auxiliary agent (polyether type defoaming agent) into the step (4), wherein the weight ratio of the graphene heat-conducting materials, the other heat-conducting fillers and the auxiliary agent is 20: 160: 5, adding 1 part of KH550, heating to 60-80 ℃, vacuumizing, and slowly stirring for 1-2 hours.
Example 4
(1) Mixing 100 parts of 1,3, 5-trimethyl-1, 3,5, triphenyl trisiloxane ring body and 30 parts of graphene powder with the carbon-oxygen ratio of 10:1, and stirring while performing ultrasonic treatment.
(2) Controlling the temperature at 60-80 ℃, adding 0.5 part of tetrapropyl ammonium hydroxide, introducing nitrogen, continuously stirring for 0.5-3 h, and keeping the temperature at 25-40 ℃ during the stirring.
(4) And (4) stopping ultrasound, raising the temperature to 80-150 ℃, vacuumizing for 2-5 h, and removing volatile matters to obtain the graphene heat conduction material.
Preparing heat-conducting silicone grease:
(5) adding other heat-conducting fillers (α spherical alumina with the average particle size of 20 mu m) and an auxiliary agent (polyether type defoaming agent) into the step (4), wherein the weight ratio of the graphene heat-conducting materials, the other heat-conducting fillers and the auxiliary agent is 20: 160: 5, adding 1 part of KH550, heating to 60-80 ℃, vacuumizing, and slowly stirring for 1-2 hours.
Comparative example
Compared with example 1, the phenyl silicone oil and the diphenylmethylsilane in the comparative example are replaced by dimethylsilicone oil, and the rest of the formulation and the preparation method are the same as those in example 1.
Examples of effects
The heat conductive silicone greases prepared in examples 1 to 4 and comparative example were subjected to viscosity and heat conductivity measurement. Specific data are shown in table 1.
TABLE 1
As can be seen from the data in Table 1, the thermal conductivity of the thermal grease prepared in the embodiments 1-4 is 2.3-3.6W/(m.K), which has good thermal conductivity and low viscosity, so that the thermal grease has good operation performance.
The organic silicon in the comparative example adopts organic silicon without benzene rings, and the obtained heat-conducting silicone grease has lower heat conductivity coefficient and higher viscosity. The heat-conducting silicone grease disclosed by the invention is reasonable in formula and preparation method, and the obtained heat-conducting silicone grease has better heat-conducting property and operating performance.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The graphene heat-conducting silicone grease is characterized by comprising a graphene heat-conducting material containing benzene rings, other fillers and an auxiliary agent, wherein the structure of the graphene heat-conducting material has the following structural formula:
x is a graphene structure, R2And R3Is a hydrogen atom, a carbon chain or an aromatic ring structure; the R is1Is a carbon chain with the carbon atom number between 0 and 5, and a is more than or equal to 1.
2. The graphene heat-conducting silicone grease as claimed in claim 1, wherein the graphene heat-conducting material is 1-110 parts by weight, the other fillers are 20-900 parts by weight, and the auxiliary agent is 0.1-10 parts by weight.
3. The graphene thermal silicone grease according to claim 1, wherein the graphene thermal conductive material has a carbon-to-oxygen ratio of (50-1000): 1.
4. the graphene thermal silicone grease of claim 1, wherein the other thermal conductive filler comprises one or more of zinc oxide, aluminum oxide, magnesium oxide, copper powder, silver powder, zinc powder, aluminum powder, and carbon nanotubes.
5. The graphene thermal silicone grease as claimed in claim 1, wherein the auxiliary agent comprises one or more of an antifoaming agent, a coating auxiliary agent and a wetting dispersant.
6. The preparation method of the graphene thermal silicone grease according to any one of claims 1 to 5, comprising the steps of:
(1) mixing graphene and organic silicon containing benzene rings to obtain a mixture;
(2) adding other heat-conducting fillers and auxiliaries to the mixture.
7. The preparation method of the graphene heat-conducting silicone grease as claimed in claim 6, wherein the weight ratio of the silicone containing benzene rings to the graphene is (1-20): 1, the carbon-oxygen ratio of the graphene is (8-1000: 1).
8. The method for preparing graphene thermal silicone grease according to claim 6, wherein the silicone containing a benzene ring contains Si-H bonds.
9. The method according to claim 6, wherein in the step (1), the graphene and the silicone containing a benzene ring are mixed, and then a step of adding a hydrosilation compound is further included, wherein the hydrosilation compound includes one or more of alkylhydrosilanes such as trimethylhydrosilane and triethylhydrosilane, tetramethylcyclotetrasiloxane, hydrosiloxane ring body, high-hydrogen silicone oil, phenyltrimethylcyclotetrasiloxane and phenyl-hydrogen silicone oil.
10. The method according to claim 6, wherein the silicone containing benzene rings comprises one or more of 1,3, 5-trimethyl-1, 3, 5-triphenyl trisiloxane rings, 1,3,5, 7-tetramethyl-1, 3,5, 7-tetraphenyl tetrasiloxane rings, phenyltrimethoxysilane, diphenyldimethoxysilane, and methylphenylsiloxane rings.
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| CN114395254A (en) * | 2022-02-24 | 2022-04-26 | 热领（上海）科技有限公司 | High-thermal-conductivity heat-conducting silicone grease and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395254A (en) * | 2022-02-24 | 2022-04-26 | 热领（上海）科技有限公司 | High-thermal-conductivity heat-conducting silicone grease and preparation method thereof |
| CN114395254B (en) * | 2022-02-24 | 2023-05-26 | 热领(上海)材料有限公司 | High-thermal-conductivity-coefficient heat-conducting silicone grease and preparation method thereof |
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