CN111286213A - Chemical and physical treatment method of high-thermal-conductivity filler - Google Patents
Chemical and physical treatment method of high-thermal-conductivity filler Download PDFInfo
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K9/00—Use of pretreated ingredients
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention relates to the field of heat-conducting fillers, in particular to a chemical and physical treatment method of a high heat-conducting filler, which comprises the following steps: (1) carrying out surface chemical modification treatment on the high-thermal-conductivity filler by adopting a modifier to obtain a modified filler; (2) carrying out physical extrusion treatment on the modified filler obtained in the step (1); when the material obtained after the physical extrusion treatment is subjected to soft agglomeration, physical crushing is required. The chemical and physical method of the high-thermal-conductivity filler provided by the invention can realize chemical modification, physical reshaping and self-adaptive grading of the high-thermal-conductivity filler, can be used for preparing composite materials, and can greatly improve the filling amount of the filler in resin and the like or reduce the viscosity of glue solution, thereby improving the thermal conductivity of matrix materials such as resin and the like and ensuring excellent manufacturability.
Description
Technical Field
The invention relates to the field of heat-conducting fillers, in particular to a chemical and physical treatment method of a high-heat-conducting filler.
Background
At present, the high-thermal-conductivity insulating material has very wide application prospect in modern high-tech fields such as electrical equipment, microelectronics, LED illumination, solar energy, transportation, aerospace, national defense and military industry and the like. The research on the high thermal conductivity insulating material is one of the research hotspots in the international electrical and electronic insulation field. The method for improving the thermal conductivity of the polymer material mainly comprises the following two ways: firstly, preparing an intrinsic heat-conducting polymer, namely the polymer has good heat-conducting property, and the method is characterized in that in the preparation and processing processes of the polymer, the molecules and the linked structure of the polymer are changed by a certain means to obtain a special physical configuration so as to improve the heat conductivity of the polymer; and secondly, preparing the filled heat-conducting polymer, namely preparing the heat-conducting insulating polymer composite material by taking the polymer as a matrix, adding high-heat-conducting insulating filler and performing a certain process. The composite material prepared by the method of filling the resin matrix with the inorganic heat-conducting filler has the characteristics of easy processing and forming, low price, good heat conductivity and the like, and is the simplest and most effective method for preparing the heat-conducting material at present. With the increase of the content of the filler in the polymer matrix, part of the heat conduction chains and the heat conduction net can be connected and penetrated through each other to finally form a heat conduction network penetrating through the whole matrix, at the moment, the filler can also become a continuous phase, and the heat conduction performance of the filling type polymer composite material is obviously improved. Therefore, increasing the loading of the filler is the key to increasing the thermal conductivity of the polymer matrix composite. However, the loading of unmodified or chemically modified thermally conductive fillers still cannot meet the requirements of the development of thermally conductive technology. In addition, under a certain filling amount, how to reduce the viscosity of the glue solution is also an important problem in the current development of the heat conduction technology.
Disclosure of Invention
In view of the problems in the prior art, the first aspect of the present invention provides a method for chemically and physically treating a highly thermally conductive filler, comprising the steps of:
(1) carrying out surface chemical modification treatment on the high-thermal-conductivity filler by adopting a modifier to obtain a modified filler;
(2) carrying out physical extrusion treatment on the modified filler obtained in the step (1); when the material obtained after the physical extrusion treatment is subjected to soft agglomeration, physical crushing is required.
As a preferable technical solution of the present invention, the number of times of the physical pressing process in the step (2) is greater than 1.
As a preferable technical solution of the present invention, the high thermal conductive filler is one or more selected from alumina, silicon oxide, aluminum nitride, boron nitride, zinc oxide, and silicon carbide.
As a preferable technical solution of the present invention, the shape of the high thermal conductive filler is selected from one or more of an angle shape, a spherical shape, a sheet shape, a needle shape, and a fiber shape.
As a preferable technical scheme of the invention, the particle size of the high-thermal-conductivity filler is 0.01-500 um.
As a preferable technical scheme of the invention, the modifier is selected from one or more of a coupling agent, a dispersing agent and a surfactant.
According to a preferable technical scheme of the invention, the dosage of the modifier is 0.05-10 w% of the high-thermal-conductivity filler.
As a preferable technical scheme of the invention, the pressure born by the high-thermal-conductivity filler during the physical extrusion treatment in the step (2) is 0.1-200 MPa.
As a preferable technical solution of the present invention, the physical extrusion treatment in step (2) is any one of ball milling, rolling and plate pressing.
As a preferable technical solution of the present invention, the extrusion time of the physical extrusion treatment in the step (2) is 1s to 100 h; the extrusion temperature is-60 to 100 ℃.
The second aspect of the invention provides a modified high thermal conductive filler prepared according to the chemical and physical treatment method of the high thermal conductive filler.
Compared with the prior art, the invention has the following beneficial effects:
the chemical and physical method of the high-thermal-conductivity filler provided by the invention can realize chemical modification, physical reshaping and self-adaptive grading of the high-thermal-conductivity filler, can be used for preparing composite materials, and can greatly improve the filling amount of the filler in resin and the like or reduce the viscosity of glue solution, thereby improving the thermal conductivity of matrix materials such as resin and the like and ensuring excellent manufacturability.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
The first aspect of the present invention provides a chemical and physical treatment method of a highly thermally conductive filler, which comprises the steps of:
(1) carrying out surface chemical modification treatment on the high-thermal-conductivity filler by adopting a modifier to obtain a modified filler;
(2) carrying out physical extrusion treatment on the modified filler obtained in the step (1); when the material obtained after the physical extrusion treatment is subjected to soft agglomeration, physical crushing is required.
Soft agglomeration: soft agglomeration is mainly caused by van der Waals and Coulomb forces between particles, and thus can be largely eliminated by some chemical action or by applying mechanical energy.
Step (1)
In one embodiment, the high thermal conductive filler is selected from one or more of alumina, silica, aluminum nitride, boron nitride, zinc oxide, and silicon carbide.
Preferably, the shape of the high thermal conductive filler is selected from one or more of an angle shape, a spherical shape, a sheet shape, a needle shape and a fiber shape; more preferably, the high thermal conductive filler is shaped like a sheet and/or an angle.
In one embodiment, the particle size of the high thermal conductive filler is 0.01 to 500 um.
The particle size of the high-thermal-conductivity filler can be single particle size or the compounding of multiple particle sizes.
In one embodiment, the modifier is selected from one or more of a coupling agent, a dispersant, a surfactant.
Preferably, the modifier is a coupling agent and a dispersant; more preferably, the weight ratio of the coupling agent to the dispersing agent is 2: 8-10: 0.
In one embodiment, the modifier is used in an amount of 0.05 to 10 w% of the high thermal conductive filler.
The applicant unexpectedly finds that the modifier is used for treating the high-thermal-conductivity filler, and the heat conduction effect is better when the dosage of the modifier is 0.05-10 w% of that of the high-thermal-conductivity filler, and guesses that the possible reason is that the modifier is used for treating the filler, so that the interface thickness of a matrix and the filler is increased, the interface bonding strength is correspondingly increased, the dispersion process of the resin and the heat-conductivity filler is improved, the bonding strength is increased, and the improvement of the heat conduction performance of the final composite material is facilitated. The content of the modifier is increased, the viscosity of the system is increased by excessive modifier, the high-heat-conductivity filler is prevented from playing a role, the content of the modifier is too low, the specific surface energy among the fillers is large, and the fillers are agglomerated in the system to cause the defect of a heat-conducting path.
Step (2)
In one embodiment, the number of times of pressing in the physical pressing process in the step (2) is greater than 1.
Preferably, the pressure born by the high thermal conductive filler during the physical extrusion treatment in the step (2) is 0.1-200 MPa.
Preferably, the physical extrusion treatment in step (2) is any one of ball milling, rolling and plate pressing.
When the physical extrusion treatment mode is ball milling, the chemical modification and the physical modification can be combined, namely: adding a modifier before or during ball milling, or adding the modifier after ball milling for a proper time and continuing ball milling.
In one embodiment, the extrusion time of the physical extrusion treatment in the step (2) is 1s to 100 h; the extrusion temperature is-60 to 100 ℃.
The applicant unexpectedly finds that the high-thermal-conductivity filler is subjected to extrusion treatment, and the extrusion pressure is 0.1-200 MP, so that the tensile strength and the thermal conductivity of the composite material can be further improved, the applicant considers that the possible reason is that after the extrusion treatment, the agglomeration of the filler due to high specific surface energy is reduced, the formation of the filler with a ball-bearing structure or a star-shaped structure is facilitated, the heat conduction is facilitated, the internal friction effect brought to a system by the filler can be reduced, the viscosity of the system can be effectively reduced in the mixing and curing process of the resin and the high-thermal-conductivity filler, and the crosslinking of the resin is facilitated.
The second aspect of the invention provides a modified high thermal conductive filler prepared according to the chemical and physical treatment method of the high thermal conductive filler.
The third aspect of the invention provides a composite insulating material containing a modified high thermal conductive filler.
In one embodiment, the preparation method of the composite insulating material containing the modified high thermal conductive filler comprises the following steps: and mixing the obtained modified high-thermal-conductivity filler with resin, and fully stirring and dispersing to obtain the modified high-thermal-conductivity filler.
Examples
Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not restrictive. The starting materials used in the examples which follow are all commercially available unless otherwise stated.
Example 1
Embodiment 1 of the present invention provides a composite insulating material containing a modified high thermal conductive filler, which includes the following steps:
(1) carrying out surface chemical modification treatment on the high-thermal-conductivity filler by adopting a modifier to obtain a modified filler; the filler is high-thermal-conductivity hexagonal boron nitride, and the sheet diameter is 10 micrometers; the modifier is KH560, and the using amount of the modifier is 2 wt% of the high-thermal-conductivity filler;
(2) carrying out physical extrusion treatment on the modified filler obtained in the step (1) in a ball milling mode; the rotating speed of the ball mill is 1500r/min, the extrusion time is 8h, the extrusion temperature is 60 ℃, and the pressure born by the filler is 120 MPa;
(3) filtering the powder treated in the step (2);
(4) taking 128 epoxy resin as a matrix;
(5) weighing 50g of the filler obtained in the step (3) and 50g of 128-epoxy resin, and fully stirring and dispersing for 20min to obtain a glue solution 1;
(6) replacing the powder obtained in the step (3) with the filler obtained in the step (1), and repeating the step (5) to obtain a glue solution 2;
(7) replacing the powder obtained in the step (3) with the high-thermal-conductivity hexagonal boron nitride which is not processed in the step (1), and repeating the step (5) to obtain a glue solution 3;
(8) the viscosities of the three glues were measured at 80 ℃ using a rotational viscometer. The viscosity of the glue solution 1 was 3500 mPas, the viscosity of the glue solution 2 was 152000 mPas, and the viscosity of the glue solution 3 was 935000 mPas. The viscosity of glue solution 1 is only 1/267 of glue solution 3;
(9) weighing the filler obtained in the step (3), gradually adding the filler into 50g of 128-epoxy resin, continuously dispersing by adopting a centrifugal machine until dry powder appears, recording the content of the added filler, and calculating to obtain the powder filling amount 1;
(10) replacing the filler obtained in the step (3) with the filler obtained in the step (1), and repeating the step (9) to obtain the filler filling amount 2;
(11) replacing the filler obtained in the step (3) with the high-thermal-conductivity hexagonal boron nitride which is not treated in the step (1), and repeating the step (9) to obtain the filler filling amount 3;
the filling amount of the filler 1, 2 and 3 is respectively 60%, 45% and 40% by calculation. This shows that the method of the present invention can significantly increase the filling amount of boron nitride in epoxy resin.
Example 2
Embodiment 2 of the present invention provides a composite insulating material containing a modified high thermal conductive filler, which includes the following steps:
(1) carrying out surface chemical modification treatment on the high-thermal-conductivity filler by adopting a modifier to obtain a modified filler; the filler is angular alumina, the grain diameter of the alumina is 45 μm and 3 μm, and the mixing ratio is 3: 2; the modifier is vinyl siloxane coupling agent, and the using amount of the modifier is 0.5 wt% of the high-thermal-conductivity filler;
(2) carrying out physical extrusion treatment on the modified filler obtained in the step (1) in a rolling manner; the pressure intensity born by the filler is 15MPa, the rotating speed is 2r/min, the temperature is 80 ℃, and the rolling time is 2 h;
(3) crushing the filler treated in the step (2);
(4) repeating the steps (2) and (3), and adjusting the pressure to be 20 MPa;
(5) taking vinyl silicone oil with the viscosity of 500mPa & s as a matrix;
(6) weighing 70g of the filler obtained in the step (4) and 30g of vinyl silicone oil, and fully stirring and dispersing for 20min to obtain a glue solution 1;
(7) replacing the powder obtained in the step (4) with the filler obtained in the step (1), and repeating the step (6) to obtain a glue solution 2;
(8) replacing the powder obtained in the step (4) with angular alumina which is not treated in the step (1), and repeating the step (6) to obtain a glue solution 3;
(9) the viscosities of the three glues were measured at 80 ℃ using a rotational viscometer. The viscosity of the glue solution 1 was 6500 mPas, the viscosity of the glue solution 2 was 46000 mPas, and the viscosity of the glue solution 3 was 168000 mPas. The viscosity of glue solution 1 is only 1/26 of glue solution 3;
(10) weighing the filler obtained in the step (4), gradually adding the filler into 50g of vinyl silicone oil with the viscosity of 500mPa & s, continuously dispersing by adopting a centrifugal machine until dry powder appears, recording the content of the added filler, and calculating to obtain the powder filling amount of 1;
(11) replacing the filler obtained in the step (4) with the filler obtained in the step (1), and repeating the step (10) to obtain the filler filling amount 2;
(12) replacing the filler obtained in the step (4) with angular alumina which is not subjected to any treatment in the step (1), and repeating the step (10) to obtain the filler filling amount 3;
the calculated filling amount of the filler 1, 2 and 3 is 91%, 83% and 75%, respectively. This shows that the method of the invention can significantly improve the filling amount of the mixed alumina in the silicone oil.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. A chemical and physical treatment method of a high thermal conductive filler is characterized by comprising the following steps:
(1) carrying out surface chemical modification treatment on the high-thermal-conductivity filler by adopting a modifier to obtain a modified filler;
(2) carrying out physical extrusion treatment on the modified filler obtained in the step (1); when the material obtained after the physical extrusion treatment is subjected to soft agglomeration, physical crushing is required.
2. The chemical and physical treatment method of a highly thermally conductive filler according to claim 1, wherein the number of times of the physical pressing treatment in the step (2) is more than 1.
3. The chemical and physical treatment method of the high thermal conductive filler according to claim 1, wherein the high thermal conductive filler is one or more selected from the group consisting of alumina, silica, aluminum nitride, boron nitride, zinc oxide, and silicon carbide.
4. The chemical and physical treatment method of highly thermally conductive filler according to claim 1, wherein the highly thermally conductive filler has a shape selected from one or more of angular shape, spherical shape, plate shape, needle shape, and fibrous shape.
5. The chemical and physical treatment method of a highly thermally conductive filler according to claim 1, wherein the highly thermally conductive filler has a particle size of 0.01 to 500 um.
6. The chemical and physical treatment method of highly thermally conductive filler according to claim 1, wherein the surface modifier is selected from one or more of coupling agent, dispersant, and surfactant.
7. The chemical and physical treatment method of a highly thermally conductive filler according to claim 1, wherein the modifier is used in an amount of 0.05 to 10 w% based on the highly thermally conductive filler.
8. The chemical and physical treatment method for the high thermal conductive filler according to claim 1, wherein the pressure applied to the high thermal conductive filler during the physical extrusion treatment in the step (2) is 0.1 to 200 MPa.
9. The chemical and physical treatment method of the high thermal conductive filler according to claim 1, wherein the physical extrusion treatment in the step (2) is any one of ball milling, rolling and plate pressing.
10. The chemical and physical treatment method of the high thermal conductive filler according to any one of claims 1 to 9, wherein the extrusion time of the physical extrusion treatment in the step (2) is 1s to 100 h; the extrusion temperature is-60 to 100 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010107935.5A CN111286213A (en) | 2020-02-21 | 2020-02-21 | Chemical and physical treatment method of high-thermal-conductivity filler |
| PCT/CN2020/110987 WO2021164225A1 (en) | 2020-02-21 | 2020-08-25 | Chemical and physical treatment method for filler with high thermal conductivity |
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| CN202010107935.5A CN111286213A (en) | 2020-02-21 | 2020-02-21 | Chemical and physical treatment method of high-thermal-conductivity filler |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029151A (en) * | 2020-09-09 | 2020-12-04 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity micro-nano boron nitride particles and preparation method and application thereof |
| CN112048270A (en) * | 2020-09-09 | 2020-12-08 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity epoxy composite material and preparation method and application thereof |
| WO2021164225A1 (en) * | 2020-02-21 | 2021-08-26 | 苏州巨峰电气绝缘系统股份有限公司 | Chemical and physical treatment method for filler with high thermal conductivity |
| CN115260793A (en) * | 2022-08-29 | 2022-11-01 | 北京中石伟业科技股份有限公司 | Application of modified zinc oxide filler |
| CN115819979A (en) * | 2022-09-02 | 2023-03-21 | 北京中石伟业科技股份有限公司 | Double-component heat-conducting gel and preparation method and application thereof |
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| WO2021164225A1 (en) * | 2020-02-21 | 2021-08-26 | 苏州巨峰电气绝缘系统股份有限公司 | Chemical and physical treatment method for filler with high thermal conductivity |
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| CN112048270A (en) * | 2020-09-09 | 2020-12-08 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity epoxy composite material and preparation method and application thereof |
| CN112048270B (en) * | 2020-09-09 | 2022-04-12 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity epoxy composite material and preparation method and application thereof |
| CN112029151B (en) * | 2020-09-09 | 2022-04-15 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity micro-nano boron nitride particles and preparation method and application thereof |
| CN115260793A (en) * | 2022-08-29 | 2022-11-01 | 北京中石伟业科技股份有限公司 | Application of modified zinc oxide filler |
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| CN115819979B (en) * | 2022-09-02 | 2023-10-13 | 北京中石伟业科技股份有限公司 | Double-component heat-conducting gel and preparation method and application thereof |
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