CN111234536A - Thermal expansion type filler and graphene synergistic electric power composite grease and preparation method thereof - Google Patents
Thermal expansion type filler and graphene synergistic electric power composite grease and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a thermal expansion type filler and graphene synergistic electric power composite grease which comprises the following raw materials in parts by mass: 60-120 parts of silicone oil, 0.1-10 parts of graphene, 5-20 parts of silicon dioxide, 20-80 parts of conductive filler, 0.5-10 parts of thermal expansion type filler, 0.1-5 parts of antioxidant and 1-5 parts of end capping agent; according to the invention, graphene, conductive fillers and the like are dispersed in modified silicone oil to form a stable system, fillers with different morphologies are lapped to form a conductive path, the conduction is realized by utilizing a tunnel effect, the conductive capability under the condition of severe temperature rise is enhanced by utilizing a thermal expansion effect, and the electric composite grease is safer and more energy-saving compared with the traditional electric composite grease.
Description
Technical Field
The invention relates to a thermal expansion type filler and graphene synergistic electric power composite grease and a preparation method thereof.
Background
The electric composite grease (Conductive Paste) is prepared by adding Conductive filler, antioxidant and anti-corrosion oily additive into a high polymer material, is used for improving the electric contact performance, and is also called as Conductive Paste. The product has more types in the market and different performances, the problem of oil content and filler separation loss can occur after a part of products are applied for a long time, the resistance is increased after the running temperature of the existing product is increased, the heating of the contact part can be further activated according to the Joule law, the aging of the high molecular material in the electric composite grease is accelerated, the performance of the electric composite grease is promoted to continue to be reduced, the running safety is reduced, the energy consumption is increased, and the power grid accident is induced. Related patents of the electric composite grease in the prior art include: CN108624226A a graphene power composite grease and a preparation method thereof, CN201710820988.x an irradiation-resistant high-efficiency power composite grease and a preparation method thereof, CN108129985A a polymer power composite grease and a preparation process thereof, and CN107033607A an anticorrosive high-temperature-resistant polymer power composite grease composition and a preparation method thereof, wherein CN108624226A a graphene power composite grease and a preparation method thereof, wherein modified graphene and modified metal powder are adopted to prepare the novel power composite grease; other patents of the invention all adopt the matching of the conductive filler and the lubricating base oil to realize the electric conduction, and the related records of adopting the expansion type filler, the conductive filler and the graphene to cooperate and utilizing the thermal expansion effect to strengthen the electric conduction capability do not appear.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a thermal expansion type filler and graphene synergistic power composite grease which can effectively avoid oil precipitation and has a more stable structural system, and the invention also aims to provide a preparation method of the power composite grease.
The technical scheme is as follows: the invention relates to a thermal expansion type filler and graphene synergistic type electric power composite grease which comprises the following raw materials in parts by weight: 60-120 parts of silicone oil, 0.1-3 parts of gamma-aminopropyltriethoxysilane, 0.1-1 part of gamma-glycidoxypropyltrimethoxysilane, 0.1-10 parts of graphene, 5-20 parts of silicon dioxide, 20-80 parts of conductive filler, 0.5-10 parts of high-molecular thermal expansion microsphere material, 0.1-5 parts of antioxidant and 1-5 parts of end capping agent.
Further, the silicone oil is a mixture of methyl silicone oil and hydroxyl silicone oil, the mixing ratio is preferably 1:1, and the viscosity of the silicone oil mixture is 5000cst-50000 mps; modified silicone oil (ZY-L) with an active reaction structure is used as a continuous phase, has excellent aging resistance and hydrophobicity, and can react with residual hydroxyl, epoxy and the like on the surfaces of graphene and metal powder, so that the problems that the graphene cannot be uniformly and stably dispersed in general silicone oil and the electric composite grease precipitates after long-term operation are solved, and the conductivity of the graphene is exerted to the maximum extent.
Furthermore, the number of the sheets of the graphene is less than 10, and the sheet diameter is 5-80 um.
Furthermore, the silicon dioxide is meteorological silicon dioxide, and the particle size is 5-20 nm.
Further, the conductive filler is one or a combination of silver powder, copper powder, nickel powder and zinc powder, and the particle size of the conductive filler is preferably nano-scale.
Further, the thermal expansion type filler is a high molecular expansion type microsphere with the initial particle size within the range of 10-100 μm, and the particle size of the thermal expansion type filler is increased to 1-5 times of the original particle size after temperature rise; the introduced high-molecular thermally-expansive microspheres and metal zinc with the largest thermal expansion coefficient strengthen a conductive path built by graphene/nano metal under the condition of temperature rise, the electric contact resistance change coefficient is 0.85 in a normal state, the comprehensive performance meets the index requirement in DL/T373 electric composite grease technical condition, and the load is increased differently from the load caused by the increase of the contact resistance after the temperature rise of the traditional conductive paste.
A preparation method of thermal expansion type filler and graphene synergistic type electric power composite grease comprises the following steps:
(1) drying powder: weighing the conductive filler and the silicon dioxide according to the formula proportion, and placing the conductive filler and the silicon dioxide in a vacuum oven for vacuum drying;
(2) preparing modified silicone oil: placing silicone oil, gamma-aminopropyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane in a planetary stirrer, and uniformly dispersing;
(3) planetary stirring: adding the conductive filler, the silicon dioxide, the graphene, the thermal expansion type filler, the modified silicone oil, the antioxidant and the end-capping reagent into a planetary stirrer according to a formula proportion, and uniformly dispersing and mixing;
(4) three-roller grinding: grinding the primary mixed product obtained in the step (3) by using a three-roll grinder;
(5) and (6) filling.
Further, the drying of the powder in the step (1) comprises: respectively putting the conductive filler and the silicon dioxide into a vacuum oven, adding a proper amount of phosphorus pentoxide as a drying agent, setting the temperature at 100 ℃ and the vacuum degree at-0.06-0.09 MPa, maintaining for 1-5h, and cooling to normal temperature under a closed condition.
Further, the preparation of the modified silicone oil in the step (2) comprises: and (2) putting the silicone oil into a planetary stirrer, adding gamma-aminopropyltriethoxysilane (KH550) and gamma-glycidoxypropyltrimethoxysilane (KH560), drying under the protection of nitrogen, dispersing for 2-5 h at normal temperature, and standing for 2 days for use.
Further, the planetary stirring in the step (3) comprises: firstly, adding modified silicone oil and an antioxidant, uniformly stirring, then adding an electric filler, silicon dioxide and graphene, heating to 100-150 ℃, stirring for 0.5-5 h under the vacuum degree of-0.05-0.08 MPa, cooling to below 80 ℃, then adding a thermal expansion type filler, and continuously stirring for 0.5-3 h.
Further, in the step (4), three-roller grinding is carried out for 1-3 times, and the roller spacing is set to be 5-10 um.
Has the advantages that: according to the invention, graphene, conductive fillers and the like are dispersed in modified silicone oil to form a stable system, fillers with different morphologies are lapped to form a conductive path, the conduction is realized by utilizing a tunnel effect, the conductive capability under the condition of severe temperature rise is enhanced by utilizing a thermal expansion effect, and the electric composite grease is safer and more energy-saving compared with the traditional electric composite grease. The silicone oil has reaction activity, can form a chemical linking point with the graphene, the conductive powder and the thermal expansion type filler, a finally formed structural system is more stable, and the oil segregation can be effectively avoided, wherein the structure is similar to a cross-linked network structure, but the paste form is still convenient for construction through process control.
Drawings
FIG. 1 is a schematic diagram of chemical linkage of a molecular chain segment of silicone oil with graphene, an expansion filler and a conductive filler;
FIG. 2 is a schematic view of an electrical landing path prior to temperature rise;
fig. 3 is a schematic view of a conductive landing via after a temperature rise.
Detailed Description
For a further understanding of the present invention, reference will now be made in detail to the embodiments illustrated in the drawings.
Example 1
The thermal expansion type filler and graphene synergistic electric power composite grease comprises the following raw materials in parts by mass: 45 parts of methyl silicone oil, 45 parts of hydroxyl silicone oil, 0.8 part of gamma-aminopropyltriethoxysilane, 0.5 part of gamma-glycidoxypropyltrimethoxysilane, 5 parts of graphene, 12 parts of silicon dioxide, 50 parts of conductive filler, 5.5 parts of thermal expansion type filler, 2 parts of antioxidant (2, 6-di-tert-butyl-4-cresol) and 2.5 parts of end-capping agent (hexamethyldisilazane); wherein the molecular chain of the modified silicone oil simultaneously contains amino, ethoxy and methoxy, and the viscosity is 20000 mps; the graphene is a graphene sheet with the number of layers of 5 and the sheet diameter of 40 um; the conductive filler is nano silver powder; the silicon dioxide is meteorological silicon dioxide, and the particle size is 17 nm; 5 parts of high molecular thermal expansion type microspheres with the particle size of 10 mu m.
The preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease of the embodiment 1 comprises the following steps:
(1) drying powder: respectively putting the conductive filler and the silicon dioxide into a vacuum oven, adding a proper amount of phosphorus pentoxide as a drying agent, setting the temperature at 125 ℃, the vacuum degree at-0.08 MPa, maintaining for 3 hours, and cooling to normal temperature under a closed condition;
(2) preparing modified silicone oil: adding silicone oil into a planetary stirrer, adding KH550 and KH560, drying under nitrogen protection, dispersing at room temperature for 3h, sealing, and standing for 2 days.
(3) Planetary stirring: firstly, adding modified silicone oil and an antioxidant, uniformly stirring, then adding an electric filler, silicon dioxide and graphene, heating to 120 ℃, keeping the vacuum degree at-0.07 MPa, stirring for 2 hours, cooling to below 80 ℃, then adding a thermal expansion type filler, and continuously stirring for 1.5 hours;
(4) three-roller grinding: grinding the primary mixed product obtained in the step (2) for 2 times by using a three-roller grinding machine, and setting the roller spacing to be 8 um;
(5) and (6) filling.
Example 2
The thermal expansion type filler and graphene synergistic electric power composite grease comprises the following raw materials in parts by mass: 30 parts of methyl silicone oil, 30 parts of hydroxyl silicone oil, 0.1 part of gamma-aminopropyltriethoxysilane, 0.1 part of gamma-glycidoxypropyltrimethoxysilane, 10 parts of graphene, 20 parts of silicon dioxide, 80 parts of conductive filler, 10 parts of thermal expansion type filler, 0.1 part of antioxidant and 0.1 part of end-capping agent; wherein the molecular chain of the modified silicone oil simultaneously contains amino, ethoxy and methoxy, and the viscosity is 5000 cst; the graphene is a graphene sheet with the number of layers of 10 and the sheet diameter of 5 um; the conductive filler is nano-grade copper powder; the silicon dioxide is meteorological silicon dioxide, and the particle size is 5 nm; 0.5 part of macromolecular thermal expansion type microspheres with the particle size of 100 mu m.
The preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease of embodiment 2 comprises the following steps:
(1) drying powder: respectively putting the conductive filler and the silicon dioxide into a vacuum oven, adding a proper amount of phosphorus pentoxide as a drying agent, setting the temperature at 100 ℃, the vacuum degree at-0.09 MPa, maintaining for 5 hours, and cooling to normal temperature under a closed condition;
(2) preparing modified silicone oil: putting silicone oil into a planetary stirrer, adding KH550 and KH560, drying under the protection of nitrogen, dispersing at normal temperature for 5h, sealing and standing for 2 days;
(3) planetary stirring: firstly, adding modified silicone oil and an antioxidant, uniformly stirring, then adding an electric filler, silicon dioxide and graphene, heating to 100 ℃, keeping the vacuum degree at-0.08 MPa, stirring for 5 hours, cooling to below 80 ℃, then adding a thermal expansion type filler, and continuously stirring for 3 hours;
(4) three-roller grinding: grinding the primary mixed product obtained in the step (2) for 1 time by using a three-roller grinder, and setting the roller spacing to be 10 um;
(5) and (6) filling.
Example 3
The thermal expansion type filler and graphene synergistic electric power composite grease comprises the following raw materials in parts by mass: 70 parts of methyl silicone oil, 50 parts of hydroxyl silicone oil, 3 parts of gamma-aminopropyltriethoxysilane, 1 part of gamma-glycidoxypropyltrimethoxysilane, 0.1 part of graphene, 5 parts of silicon dioxide, 20 parts of conductive filler, 0.5 part of thermal expansion type filler, 10 parts of antioxidant and 10 parts of blocking agent; wherein the molecular chain of the modified silicone oil simultaneously contains amino, ethoxy and methoxy, and the viscosity is 50000 mps; the graphene is a graphene sheet with the number of layers being 1 and the sheet diameter being 80 um; the conductive filler is nano-grade copper powder; the silicon dioxide is meteorological silicon dioxide, and the particle size is 20 nm; 10 portions of macromolecular thermal expansion type microsphere material with the grain diameter of 50 mu m.
A preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease of embodiment 3, comprising the following steps:
(1) drying powder: respectively putting the conductive filler and the silicon dioxide into a vacuum oven, adding a proper amount of phosphorus pentoxide as a drying agent, setting the temperature at 150 ℃, the vacuum degree at-0.06 MPa, maintaining for 1h, and cooling to normal temperature under a closed condition;
(2) preparing modified silicone oil: putting silicone oil into a planetary stirrer, adding KH550 and KH560, drying under the protection of nitrogen, dispersing at normal temperature for 2h, sealing and standing for 2 days;
(3) planetary stirring: firstly, adding modified silicone oil and an antioxidant, uniformly stirring, then adding an electric filler, silicon dioxide and graphene, heating to 150 ℃, keeping the vacuum degree at-0.05 MPa, stirring for 0.5h, cooling to below 80 ℃, then adding a thermal expansion type filler, and continuously stirring for 0.5 h;
(4) three-roller grinding: grinding the primary mixed product obtained in the step (2) for 3 times by using a three-roller grinding machine, and setting the roller spacing to be 5 um;
(5) and (6) filling.
As shown in fig. 1, modified silicone oil, a graphene sheet 2, a conductive filler 3, and a thermally expansive filler 1 cooperate to construct a conductive path, where the silicone oil has a reactive activity and can form a chemical linking point with the graphene, the conductive filler, and the thermally expansive filler, and a finally formed structural system is more stable and can effectively avoid oil segregation, and the structure is similar to a cross-linked network structure, but is still in a paste form convenient for construction through process control; fig. 2 and fig. 3 are schematic diagrams of conductive lap joint paths before and after the temperature of the electric power composite grease is increased in application, and fig. 4 shows an electric contact fitting, it can be seen that the thermal expansion type filler expands after the temperature is increased, the conductive filler is contacted more tightly, the number of conductive paths is increased, so that the contact resistance is reduced, and the increase of the number of conductive paths in a circuit model is equivalent to the decrease of the total resistance caused by the increase of the number of parallel resistors in a parallel circuit, and the conductive capability is increased before the temperature is increased. The specific properties of the product are shown in Table 1.
Table 1:
Claims (10)
1. the thermal expansion type filler and graphene synergistic electric power composite grease is characterized by comprising the following raw materials in parts by mass: 60-120 parts of silicone oil, 0.1-3 parts of gamma-aminopropyltriethoxysilane, 0.1-1 part of gamma-glycidoxypropyltrimethoxysilane, 0.1-10 parts of graphene, 5-20 parts of silicon dioxide, 20-80 parts of conductive filler, 0.5-10 parts of thermal expansion type filler, 0.1-5 parts of antioxidant and 1-5 parts of end capping agent.
2. The thermal expansion type filler and graphene synergistic electric composite grease as claimed in claim 1, wherein the silicone oil is a mixture of methyl silicone oil and hydroxyl silicone oil, and the viscosity of the silicone oil mixture is 5000cst-50000 mps.
3. The thermal expansion type filler and graphene synergistic electric power composite grease as claimed in claim 1, wherein the number of sheets of the graphene is less than 10, and the sheet diameter is 5-80 um.
4. The thermal expansion type filler and graphene synergistic type electric power composite grease as claimed in claim 1, wherein the silica is fumed silica, and the particle size is 5-20 nm.
5. The thermal expansion type filler and graphene synergistic electric power composite grease as claimed in claim 1, wherein the conductive filler is one or more of silver powder, copper powder, nickel powder and zinc powder.
6. The thermal expansion type filler and graphene synergistic electric power composite grease as claimed in claim 1, wherein the thermal expansion type filler is a high molecular expansion type microsphere with an initial particle size within a range of 10-100 μm, and the particle size of the thermal expansion type filler is increased to 1-5 times of the original particle size after temperature rise.
7. The preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
(1) drying powder: weighing the conductive filler and the silicon dioxide according to the formula proportion, and placing the conductive filler and the silicon dioxide in a vacuum oven for vacuum drying;
(2) preparing modified silicone oil: putting silicone oil, gamma-aminopropyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane into a planetary stirrer, and uniformly dispersing;
(3) planetary stirring: adding the conductive filler, the silicon dioxide, the graphene, the high-molecular thermal expansion type microsphere material, the modified silicone oil, the antioxidant and the end-capping reagent into a planetary stirrer according to a formula proportion, and uniformly dispersing and mixing;
(4) three-roller grinding: grinding the primary mixed product obtained in the step (3) by using a three-roll grinder;
(5) and (6) filling.
8. The preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease as claimed in claim 7, wherein the drying of the powder in the step (1) specifically comprises: respectively putting the conductive filler and the silicon dioxide into a vacuum oven, adding a proper amount of phosphorus pentoxide as a drying agent, setting the temperature at 100 ℃ and the vacuum degree at-0.06-0.09 MPa, maintaining for 1-5h, and cooling to normal temperature under a closed condition.
9. The preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease as claimed in claim 7, wherein the step (2) of preparing the modified silicone oil specifically comprises: and (3) putting silicone oil into a planetary stirrer, adding gamma-aminopropyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane, drying under the protection of nitrogen, dispersing for 2-5 hours at normal temperature, and standing for 2 days for use.
10. The preparation method of the thermal expansion type filler and graphene synergistic type electric power composite grease as claimed in claim 7, wherein the planetary stirring in the step (3) specifically comprises: firstly, adding modified silicone oil and an antioxidant, uniformly stirring, then adding a conductive filler, silicon dioxide and graphene, heating to 100-150 ℃, stirring for 0.5-5 h under the vacuum degree of-0.05-0.08 MPa, cooling to below 80 ℃, adding a high-molecular thermal expansion microsphere material, and continuously stirring for 0.5-3 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112391117A (en) * | 2020-11-06 | 2021-02-23 | 北京国电富通科技发展有限责任公司 | Graphene-carbon nanotube conductive spray for wire clamp contact part of live working robot |
| CN115678228A (en) * | 2022-11-04 | 2023-02-03 | 宁波聚嘉新材料科技有限公司 | Antistatic liquid crystal resin composition and film product thereof |
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| CN115678228A (en) * | 2022-11-04 | 2023-02-03 | 宁波聚嘉新材料科技有限公司 | Antistatic liquid crystal resin composition and film product thereof |
| CN115678228B (en) * | 2022-11-04 | 2023-08-18 | 宁波聚嘉新材料科技有限公司 | Antistatic liquid crystal resin composition and film product thereof |
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