CN115850742A - Fiber oriented arrangement composite material and preparation method and application thereof - Google Patents

Fiber oriented arrangement composite material and preparation method and application thereof Download PDF

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CN115850742A
CN115850742A CN202211519966.7A CN202211519966A CN115850742A CN 115850742 A CN115850742 A CN 115850742A CN 202211519966 A CN202211519966 A CN 202211519966A CN 115850742 A CN115850742 A CN 115850742A
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fiber
heat
fiber bundle
composite material
conducting
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王绍凯
叶红利
李敏
顾轶卓
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Beihang University
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Beihang University
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Abstract

The invention provides a fiber oriented composite material and a preparation method and application thereof, belonging to the technical field of functional materials. The invention adopts the heat-conducting fiber with micron-sized diameter as the filler, thereby having lower cost. Meanwhile, the invention utilizes the draftable substrate to drive the fiber bundle to move dispersedly on the premise of ensuring the parallel arrangement of the heat-conducting fibers, and on the basis, the composite material with the heat-conducting fibers arranged directionally along the height (thickness) direction can be prepared by pouring the matrix material. The method of the invention is convenient for regulating and controlling the volume fraction of the heat conducting fiber, is easy to obtain the composite material with higher volume fraction of the heat conducting fiber, has excellent heat conducting performance, avoids the problem that the composite material with high heat conducting filler content is difficult to obtain due to large specific surface area of the nanometer material, and avoids the problem that the heat transfer efficiency of the composite material is influenced due to thermal contact resistance among the nanometer materials. The method provided by the invention is simple to operate and has a wide application prospect.

Description

Fiber oriented arrangement composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of functional materials, in particular to a fiber oriented arrangement composite material and a preparation method and application thereof.
Background
The integration level and power density of electronic devices are gradually improved, and the corresponding heat dissipation problem is increasingly serious. Lightweight, high thermal conductivity Thermal Interface Materials (TIMs) have become an extremely important component in advanced thermal management systems. Meanwhile, in the traditional resin-based composite material, the resin has low heat conductivity, and the researchers pay extensive attention to how to construct a heat transfer path of fibers to improve the heat conductivity of the composite material.
Taking the thermal interface material as an example, the heat conducting gasket completes heat transfer between the heating part and the heat dissipation part by being filled between the heating body and the heat dissipation element, thereby realizing rapid heat dissipation of the equipment. The traditional heat conducting gasket is usually prepared by compounding inorganic heat conducting powder and a matrix, wherein the inorganic heat conducting powder comprises aluminum oxide, aluminum nitride, boron nitride and the like, the heat conductivity of the inorganic heat conducting powder is below 300W/(m.K), and the heat conducting gasket manufactured by filling the inorganic heat conducting powder is usually not higher than 10W/(m.K).
At present, a carbon nanotube, graphene and other nano materials are used as a one-dimensional or two-dimensional heat conduction filler, and an ice template method or a drafting orientation method is adopted to perform orientation regulation on the heat conduction filler, so that a high heat conduction composite material can be obtained. However, these nanomaterials are expensive, and the specific surface area of the nanomaterials is large, and the content of the heat conductive filler is generally not more than 5% by the above method, so that it is difficult to obtain a composite material with a high content of the heat conductive filler.
Disclosure of Invention
The invention aims to provide a fiber oriented composite material, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a fiber oriented composite material, which comprises the following steps:
providing a fiber bundle, wherein the fiber bundle is formed by parallel arrangement of a plurality of heat conducting fibers with micron-sized diameters along the axial direction of the fiber bundle;
vertically adhering the fiber bundle to the surface of a drawable substrate, drawing the drawable substrate, and dispersing heat-conducting fibers in the fiber bundle on the surface of the drawable substrate to obtain a dispersed fiber bundle;
and placing the dispersed fiber bundle in a mold, pouring a matrix material into the mold containing the dispersed fiber bundle, curing and molding, and demolding to obtain the fiber oriented arrangement composite material.
Preferably, the whole fiber bundle is cylindrical, the diameter of the fiber bundle is 8-12 mm, and the height of the fiber bundle is 2-10 mm; the volume fraction of the heat-conducting fibers in the fiber bundle is more than or equal to 60 percent.
Preferably, the thermally conductive fibers comprise carbon fibers, silicon nitride fibers or alumina fibers.
Preferably, the surface of the heat conducting fiber is provided with a protective film; the method further comprises the following steps of before adhesion: and removing the protective film on the surface of the heat-conducting fiber in the fiber bundle.
Preferably, the stretchable substrate comprises a rubber membrane or an extensible sponge.
Preferably, the drawing is mechanical drawing; the speed of the drafting is 3-5 mm/min.
Preferably, the drafting mode comprises annular drafting or unidirectional drafting.
Preferably, the side walls of the fiber bundle have constraining bands for securing the thermally conductive fibers; before the drafting, the method further comprises the following steps: removing the constraining tape from the side wall of the fiber bundle.
The invention provides a fiber oriented composite material prepared by the preparation method in the technical scheme, which comprises a matrix and fiber reinforcements dispersed in the matrix, wherein the fiber reinforcements are formed by orienting and arranging a plurality of heat-conducting fibers with micron-sized diameters along the out-of-plane direction of the fiber oriented composite material; the volume fraction of the heat conducting fiber in the fiber oriented composite material is 10-50%.
The invention provides application of the fiber oriented arrangement composite material in the technical scheme in preparation of a heat conduction gasket or a shielding box shell of an electronic device.
The invention provides a preparation method of a fiber oriented arrangement composite material, which comprises the following steps: providing a fiber bundle, wherein the fiber bundle is formed by parallel arrangement of a plurality of heat-conducting fibers with micron-sized diameters along the axial direction of the fiber bundle; vertically adhering the fiber bundle to the surface of a drawable substrate, drawing the drawable substrate, and dispersing heat-conducting fibers in the fiber bundle on the surface of the drawable substrate to obtain a dispersed fiber bundle; and placing the dispersed fiber bundle in a mold, pouring a matrix material into the mold containing the dispersed fiber bundle, curing and molding, and demolding to obtain the fiber oriented arrangement composite material. The invention adopts the heat-conducting fiber with micron-sized diameter as the filler, thereby having lower cost. Meanwhile, the invention utilizes the draftable substrate to drive the fiber bundle to move dispersedly on the premise of ensuring the parallel arrangement of the heat-conducting fibers, and on the basis, the composite material with the heat-conducting fibers arranged directionally along the height (thickness) direction can be prepared by pouring the matrix material. The method of the invention is convenient for regulating and controlling the volume fraction of the heat conducting fiber, is easy to obtain the composite material with higher volume fraction of the heat conducting fiber, has excellent heat conducting performance, avoids the problem that the composite material with high heat conducting filler content is difficult to obtain due to large specific surface area of the nanometer material, and avoids the problem that the heat transfer efficiency of the composite material is influenced due to thermal contact resistance among the nanometer materials. The method provided by the invention is simple to operate and has a wide application prospect.
Drawings
FIG. 1 is a flow chart of the present invention for preparing a fiber alignment composite;
FIG. 2 is a view showing a physical example of a rod-shaped aggregate and a cylindrical fiber bundle in example 1;
FIG. 3 is a graph comparing the dispersed fiber bundles (drawn 2 and 8 times, respectively) prepared in a unidirectional drawing manner with the fiber bundles (i.e., undrawn) in examples 1 and 2;
FIG. 4 is a side view of the bundle of dispersed fibers obtained after drafting in example 2;
FIG. 5 is a graph comparing the dispersed fiber bundles (drawn 4 and 8 times, respectively) produced in the ring draw mode in examples 3 and 4 with the fiber bundles (i.e., undrawn);
FIG. 6 is a graph showing the results of the thermal conductivity tests of the composite materials prepared in examples 1 to 4 and the silicone rubber and epoxy resin.
Detailed Description
The invention provides a preparation method of a fiber oriented composite material, which comprises the following steps:
providing a fiber bundle, wherein the fiber bundle is formed by parallel arrangement of a plurality of heat-conducting fibers with micron-sized diameters along the axial direction of the fiber bundle;
vertically adhering the fiber bundle to the surface of a drawable substrate, drawing the drawable substrate, and dispersing heat-conducting fibers in the fiber bundle on the surface of the drawable substrate to obtain a dispersed fiber bundle;
and placing the dispersed fiber bundle in a mold, pouring a matrix material into the mold containing the dispersed fiber bundle, curing and molding, and demolding to obtain the fiber oriented arrangement composite material.
In the present invention, the starting materials are all commercially available products well known to those skilled in the art unless otherwise specified.
The invention provides a fiber bundle which is formed by parallel arrangement of a plurality of heat-conducting fibers with micron-sized diameters along the axial direction of the fiber bundle. In the invention, the fiber bundle is preferably cylindrical as a whole; the diameter of the fiber bundle is preferably 8-12 mm, more preferably 9-11 mm, the diameter is too large, the heat conducting fibers are easy to loosen in the subsequent processing process, the diameter is too small, the processing efficiency is low, and the heat conducting fibers are easy to bend and damage; the height of the fiber bundle is preferably 2-10 mm, and more preferably 4-6 mm; the volume fraction of the heat-conducting fibers in the fiber bundle is preferably not less than 60%, and more preferably 60-65%.
In the present invention, the thermally conductive fibers preferably include carbon fibers, silicon nitride fibers, or alumina fibers; the carbon fiber preferably comprises mesophase pitch-based carbon fiber and/or polyacrylonitrile-based carbon fiber, and more preferably one or more of XN-90 mesophase pitch-based carbon fiber, K13C6U mesophase pitch-based carbon fiber and M65J polyacrylonitrile-based carbon fiber; in the examples of the present invention, the mesophase pitch-based carbon fiber used is specifically TC-HC-800 fiber. In the invention, the diameter of the heat-conducting fiber is micron-sized, and the diameter of the heat-conducting fiber is preferably 5-11 μm; the thermal conductivity of the thermal conductive fiber is preferably 100 to 500W/(mK). In the invention, the heat-conducting fiber has high length-diameter ratio and micron-sized diameter, so that the problem that the composite material with high heat-conducting filler content is difficult to obtain due to large specific surface area of the nano material is avoided, and the problem that the heat transfer efficiency of the composite material is influenced due to thermal contact resistance among the nano materials is avoided; the invention preferably adopts the heat conducting fibers of the above type, has excellent axial heat conducting performance, for example, the heat conductivity of the carbon fibers with different microstructures can be changed from 1W/(m.K) to 1000W/(m.K), and the composite material can be prepared through the controllable directional arrangement of the heat conducting fibers, so that the thermal interface material or the resin-based heat conducting composite material with different heat conductivities can be obtained.
In the present invention, the side wall of the fiber bundle preferably has a restraining band for fixing the heat conducting fibers, i.e., the heat conducting fibers are bound and fixed by the restraining band to form the fiber bundle; specifically, the preparation method of the fiber bundle preferably comprises the following steps: binding heat-conducting fibers with a preset length and a preset number into a compact rod shape by using a restraint belt to obtain a rod-shaped aggregate; and the rod-shaped aggregate is sequentially cut and polished to obtain the fiber bundle.
In the present invention, the length of the heat conductive fiber is preferably 8 to 15cm, and more preferably 10cm. In the invention, the number of the heat conducting fibers is calculated according to a formula shown in formula I:
n=(V 1 ×S 2 )/S 1 formula I;
in the formula I, n is the number of the heat-conducting fibers in the fiber bundle, V 1 Is the volume fraction of the heat-conducting fibers in the fiber bundle, S 1 Is the sectional area S of single heat-conducting fiber in the fiber bundle 2 The cross-sectional area of the fiber bundle.
In the present invention, the restraining tape may be specifically an adhesive tape, and the width of the adhesive tape is preferably 1.5 to 2.5cm, and more preferably 2cm. In the present invention, the heat conductive fibers should be prevented from bending during the bundling process. In the present invention, the cutting is preferably performed by cutting the bundled fiber bundle into a plurality of cylinders having a height of 3 to 12mm in a vertical axial direction using a blade. In the present invention, the polishing is preferably performed by polishing the upper and lower surfaces of the cut cylinder with 100-800 mesh sandpaper, and the upper and lower surfaces are smooth and flat, thereby finally obtaining a fiber bundle with a height of 2-10 mm.
After the fiber bundle is obtained, the fiber bundle is vertically adhered to the surface of a drawable substrate, the drawable substrate is drawn, and heat conducting fibers in the fiber bundle on the surface of the drawable substrate are dispersed to obtain a dispersed fiber bundle. In the invention, the surface of the heat-conducting fiber is provided with a protective film, taking the carbon fiber as an example, the protective film formed by sizing agent exists on the surface of the carbon fiber, and the protective film can avoid the problems of abrasion, fluffing and the like of the carbon fiber in the processes of transportation, storage and the like; when the surface of the heat-conducting fiber is provided with a protective film, the method preferably further comprises the following steps before adhesion: and removing the protective film on the surface of the heat-conducting fiber in the fiber bundle. In the invention, the method for removing the surface protective film of the heat-conducting fiber is preferably to soak the fiber bundle by using an organic solvent; the organic solvent is preferably acetone; the soaking is preferably carried out under stirring conditions; the soaking can also preferably be assisted by ultrasound, and when the ultrasonic assistance is adopted, a rigid circular ring is preferably arranged on the side wall of the fiber bundle, and the inner diameter of the rigid circular ring is preferably equal to the diameter of the fiber bundle so as to avoid vibration of the fiber bundle. In the invention, in the soaking process, 1 time of new organic solvent is preferably replaced at intervals of 1 hour; the soaking time is based on the complete removal of the protective film. In the invention, the fiber bundle is soaked in the organic solvent, so that the fiber surface protective film is removed, and simultaneously, the residual scraps in the cutting and polishing processes can be cleaned and removed. After soaking, the fiber bundle is preferably dried; the drying temperature is preferably 50 ℃ and the drying time is preferably 30min.
After the protective film on the surface of the heat-conducting fiber in the fiber bundle is removed, the fiber bundle is vertically adhered to the surface of a drawable substrate, the drawable substrate is drawn, the heat-conducting fiber in the fiber bundle on the surface of the drawable substrate is dispersed, and the dispersed fiber bundle is obtained. In the present invention, the stretchable substrate preferably comprises a rubber film or an extensible sponge; the drafting ratio of the drawable substrate is preferably more than or equal to 10 times; the draft ratio is specifically an area increase magnification after the draft. The fiber bundle is preferably adhered to the surface of the drawable substrate by adopting an adhesive, specifically, the adhesive is atomized and sprayed on the surface of the drawable substrate, and then the fiber bundle is vertically placed on the surface of the drawable substrate coated with the adhesive, and the fiber bundle and the drawable substrate are bonded and fixed; the specific type of the adhesive is preferably spray-type quick-drying adhesive, and the adhesive preferably does not have obvious curing reaction within 20min so as to ensure that the drafting characteristic of the drawable substrate is not influenced.
In the present invention, when the side wall of the fiber bundle has a constraining tape for fixing the heat conductive fiber, the pre-drafting preferably further comprises: removing the constraining tape from the side wall of the fiber bundle. In the present invention, the drawing is preferably mechanical drawing; the rate of the drawing is preferably 3 to 5mm/min, more preferably 4 to 5mm/min. In the present invention, before the drawing, a drawing ratio is preferably determined according to a volume fraction (recorded as a target volume fraction) of the heat conductive fibers in the finally obtained fiber alignment composite material, and the drawing is based on the drawing ratio being satisfied, specifically, the volume fraction/drawing ratio of the heat conductive fibers in the fiber bundle = the target volume fraction. In the present invention, the drawing manner preferably includes ring drawing or one-way drawing; the annular drafting is specifically drafting in the same proportion in all directions in the plane; the unidirectional drafting is specifically drafting along a single direction under the condition of fixing a certain direction size. The principle of the invention is that firstly, a fiber bundle with high volume fraction of heat conducting fibers is prepared, the fiber bundle is adhered to the surface of a drawable substrate, the heat conducting fibers in the fiber bundle are driven to disperse by the deformation of the drawable substrate under the action of drawing, the orientation of the heat conducting fibers is not damaged, and then the fiber oriented arrangement composite material can be obtained by the subsequent operations of matrix material casting, curing forming and the like.
After the dispersed fiber bundle is obtained, the dispersed fiber bundle is placed in a mold, a matrix material is poured into the mold containing the dispersed fiber bundle, and the matrix material is demoulded after solidification and forming to obtain the fiber oriented composite material. According to the invention, preferably, a mould is placed around the dispersed fiber bundle on the surface of the drawable substrate under the condition of keeping the drawable substrate in an extension state, then a matrix material is poured along the edge of the mould until all the dispersed fiber bundle is immersed in the matrix material, then solidification molding is carried out, and the fiber orientation arrangement composite material is obtained after demoulding. In the present invention, the matrix material preferably includes a thermosetting resin or rubber; the thermosetting resin preferably comprises an epoxy resin, a phenolic resin, an unsaturated polyester resin or a bismaleimide resin; the rubber preferably includes natural rubber or silicone rubber, and in the embodiment of the present invention, polydimethylsiloxane (PDMS) is specifically used as the silicone rubber.
In the invention, the curing molding comprises standing, bubble discharging and curing which are carried out in sequence. In the present invention, the time of the standing is preferably 15min, and the standing functions to give a sufficient bubble removal time. In the invention, after standing, preferably placing the whole mould containing the dispersed fiber cluster and the matrix material in a vacuum oven for bubble removal and solidification; the exhaust bubbles are preferably treated for 15min under the conditions of-0.05 MPa and-0.1 MPa in sequence respectively so as to eliminate bubbles in the system; the specific conditions for curing are preferably selected according to the kind of the matrix material, and in particular, when the thermosetting resin is an epoxy resin, the curing conditions for the epoxy resin preferably include: pre-curing at 80 ℃ for 30min, heating to 120 ℃ and further curing for 2h; when the rubber is polydimethylsiloxane, the curing conditions of the polydimethylsiloxane preferably include: pre-curing at 60 deg.c for 1 hr, heating to 100 deg.c and further curing for 1 hr.
In the invention, after demoulding, the surface of the material is preferably polished, so that the composite material with the height of 2-10 mm and the fiber in directional arrangement can be directly obtained; if it is desired to obtain a fiber alignment composite material having a height of 0.5 to 2mm, it is preferably processed to a desired thickness by a mechanical processing method, and the present invention is not particularly limited thereto.
FIG. 1 is a flow chart of the present invention for preparing a fiber-oriented composite material, for example, a rubber film is used as a drawable substrate, a dispersed fiber bundle is prepared by ring-drawing, and then an epoxy resin is used as a matrix material to prepare the fiber-oriented composite material; and if the extensible sponge is used as a drawable substrate, preparing a dispersed fiber bundle in a unidirectional drafting mode, and then preparing the fiber oriented composite material by using the silicon rubber as a matrix material.
The invention provides a fiber oriented composite material prepared by the preparation method in the technical scheme, which comprises a matrix and fiber reinforcements dispersed in the matrix, wherein the fiber reinforcements are formed by orienting and arranging a plurality of heat-conducting fibers with micron-sized diameters along the out-of-plane direction of the fiber oriented composite material; the volume fraction of the heat conducting fibers in the fiber alignment composite material is 10 to 50%, preferably 11 to 32%, more preferably 13 to 25%, and still more preferably 18 to 20%. In the invention, the heat conducting fibers in the fiber oriented arrangement composite material are uniformly distributed, and the fiber oriented arrangement composite material has no obvious pore defect as a whole, and the height can be regulated and controlled within the range of 0.5-10 mm through pretreatment or post-processing according to requirements. According to the invention, the thermal conductivity of the fiber oriented composite material can be regulated and controlled within the range of 1-200W/(m.K), specifically 15-191W/(m.K) and 39-102W/(m.K) according to the difference of the types of the selected heat-conducting fibers and the matrix material and the difference of the volume fraction of the heat-conducting fibers; in particular, considering the matrix thermal conductivity is very low, neglecting the matrix thermal conductivity, the fiber type is selected and the fiber volume fraction is estimated according to the mixing law, i.e. the thermal conductivity of the final fiber aligned composite is approximately equal to the fiber thermal conductivity times the thermally conductive fiber volume fraction.
The invention provides application of the fiber oriented arrangement composite material in the technical scheme in preparation of a heat conduction gasket or a shielding box shell of an electronic device.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
In the present invention, the thermal conductivity of each composite was measured according to the standard test method for the thermal transmission performance of the thermally conductive and electrically insulating material of ASTM D5470.
The TC-HC-800 fibers used in the following examples were provided by Shanxi Tianze New Material science and technology, inc.;
PDMS was purchased from dow corning, usa;
epoxy resins were purchased from Nantong star plastics, inc.;
the extensible sponge is a common commercial compressed sponge;
rubber film was purchased from Changzhou eight zero future Intelligent technology, inc.
Example 1
In this embodiment, a composite material (denoted as TC-HC-800 fiber/PDMS heat-conductive composite material) is prepared from mesophase pitch-based carbon fibers (TC-HC-800 fibers, diameter 11 μm) and silicone rubber PDMS (polydimethylsiloxane), and the steps are as follows:
cutting the carbon fibers into fibers with the length of 10cm, calculating the number of the needed fibers according to a formula I, and then stacking the fibers in parallel; bundling all fibers into a compact rod shape by using an adhesive tape with the width of 2cm, and avoiding bending of the fibers in the bundling process to obtain a rod-shaped aggregate with the diameter of 10mm (as shown in figure 2);
cutting the rod-shaped aggregate into a plurality of cylinders with the height of 6mm along the vertical axial direction by using a blade, then polishing the upper surface and the lower surface of the rod-shaped aggregate by using 100-800-mesh sand paper, wherein the upper surface and the lower surface are smooth and flat, so as to obtain fiber bundles with the height of 4mm and the fiber volume fraction of about 65%, and the fibers in the fiber bundles are all arranged in parallel along the axial direction (as shown in figure 2);
arranging a rigid ring on the side wall of the fiber bundle, wherein the inner diameter of the rigid ring is equal to the diameter of the fiber bundle, then soaking the fiber bundle in acetone, applying mechanical stirring and assisting ultrasonic treatment, and replacing the acetone for 1 time at intervals of 1 hour in the soaking process until the sizing agent on the surface of the fiber in the fiber bundle is completely removed; then drying in a 50 ℃ oven for 30min to obtain a pretreated fiber bundle;
adopting extensible sponge as a substrate, atomizing and spraying an adhesive (spray type quick-drying adhesive) on the surface of the substrate, vertically placing the pretreatment fiber bundle on the surface of the substrate coated with the adhesive, and bonding and fixing the pretreatment fiber bundle and the substrate; then, the rigid circular ring and the adhesive tape on the side wall of the pretreated fiber bundle are removed, and the substrate is mechanically drafted in a one-way drafting mode, wherein the drafting ratio is 2 times (namely the area drafting of the substrate is increased by 2 times), and the drafting speed is 5mm/min, so that a dispersed fiber bundle is obtained (as shown in fig. 3);
keeping the elongation state of the substrate, placing a mold around the dispersed fiber bundle on the surface of the substrate, then pouring PDMS along the edge of the mold until all the dispersed fiber bundles are immersed in the PDMS, standing for 15min, then placing the mold containing the dispersed fiber bundle and the PDMS in a vacuum oven, sequentially and respectively treating for 15min under the conditions of-0.05 MPa and-0.1 MPa to remove air bubbles in the system, then carrying out heating curing according to the curing system of the PDMS (specifically, carrying out heat preservation and pre-curing at 60 ℃ for 1h, then heating to 120 ℃ for further curing for 1 h), and polishing the surface of the obtained cured molding material after demolding to obtain the composite material with the thickness of 4mm, wherein the fiber volume fraction is about 31.8%, and the thermal conductivity is 190.9W/(m.K).
Example 2
A composite was prepared as in example 1, except that the extensible sponge had a draw ratio of 8 times; wherein the side view of the dispersed fiber bundle obtained after drafting is shown in fig. 4, the fiber orientation is good; the actual figure of the dispersed fiber bundle obtained after drafting is shown in figure 3; finally, the composite material with the thickness of 4mm is obtained, the fiber volume fraction is about 8.2%, and the thermal conductivity is 42.0W/(m.K).
Example 3
Preparing a composite material according to the method of the embodiment 1, wherein the difference is that a rubber film is used as a substrate, the drafting ratio of the rubber film is 4 times, the mechanical drafting mode is annular drafting, the matrix material is made of epoxy resin, and the curing condition is specifically that after the temperature is kept at 80 ℃ for 30min, the temperature is raised to 120 ℃ for curing for 2h; wherein the real object diagram of the dispersed fiber bundle obtained after drafting is shown in figure 5; finally, the composite material with the thickness of 4mm is obtained, the fiber volume fraction is about 16.5%, and the thermal conductivity is 102.0W/(m.K).
Example 4
Preparing a composite material according to the method of the embodiment 1, wherein the difference is that a rubber film is used as a substrate, the drafting ratio of the rubber film is 8 times, the mechanical drafting mode is annular drafting, the matrix material is made of epoxy resin, the curing condition is specifically that the composite material is pre-cured for 30min at the temperature of 80 ℃, and then the composite material is further cured for 2h at the temperature of 120 ℃; wherein the real figure of the dispersed fiber bundle obtained after drafting is shown in figure 5; finally, the composite material with the thickness of 4mm is obtained, the fiber volume fraction is about 8.2%, and the thermal conductivity is 39.2W/(m.K).
Example 5
A composite material was prepared as in example 1, except that the carbon fibers were replaced with silicon nitride fibers, and the height of the fiber bundle was 4mm and the fiber volume fraction was about 68%; finally, the composite material with the thickness of 4mm is obtained, the fiber volume fraction is about 34.2%, and the thermal conductivity is 15.5W/(m.K).
Test example
The composite materials prepared in examples 1 to 4 were placed on a hot stage, the lower surface of which was in contact with the hot stage, and the temperature of the upper surface was observed with a thermal infrared imager as a change with time and compared with silicone rubber and epoxy resin. FIG. 6 is a graph showing the results of the thermal conductivity tests of the composite materials prepared in examples 1 to 4, as well as the silicone rubber and the epoxy resin, and the detailed data are shown in Table 1. As can be seen from fig. 6 and table 1, the temperature change rate of the composite materials prepared in examples 1 to 4 is faster than that of the epoxy resin and the silicone rubber reinforced without the thermal conductive fiber, and the final equilibrium temperature is higher, which indicates that the thermal conductive fiber orientation significantly enhances the thermal conductivity.
TABLE 1 temperature Change data for examples 1-4 and neat silicone rubbers and epoxy resins
Figure BDA0003971108360000101
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Figure BDA0003971108360000111
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A method for preparing a fiber orientation arrangement composite material comprises the following steps:
providing a fiber bundle, wherein the fiber bundle is formed by parallel arrangement of a plurality of heat conducting fibers with micron-sized diameters along the axial direction of the fiber bundle;
vertically adhering the fiber bundle to the surface of a drawable substrate, drawing the drawable substrate, and dispersing heat-conducting fibers in the fiber bundle on the surface of the drawable substrate to obtain a dispersed fiber bundle;
and placing the dispersed fiber cluster in a mold, pouring a matrix material into the mold containing the dispersed fiber cluster, curing and molding, and demolding to obtain the fiber oriented arrangement composite material.
2. The method according to claim 1, wherein the fiber bundle is cylindrical as a whole, and has a diameter of 8 to 12mm and a height of 2 to 10mm; the volume fraction of the heat-conducting fibers in the fiber bundle is more than or equal to 60 percent.
3. The production method according to claim 1 or 2, wherein the thermally conductive fiber comprises a carbon fiber, a silicon nitride fiber, or an alumina fiber.
4. The production method according to claim 3, wherein the surface of the heat conductive fiber is provided with a protective film; the method further comprises the following steps of: and removing the protective film on the surface of the heat-conducting fiber in the fiber bundle.
5. The method of claim 1, wherein the stretchable substrate comprises a rubber film or an extensible sponge.
6. The method of claim 1, wherein said drawing is mechanical drawing; the speed of the drafting is 3-5 mm/min.
7. The method according to claim 1 or 6, wherein said drawing comprises ring drawing or unidirectional drawing.
8. The method for preparing a heat conducting fiber bundle according to claim 1 or 6, wherein the side wall of the fiber bundle is provided with a restraining band for fixing the heat conducting fiber; before the drafting, the method further comprises the following steps: removing the constraining tape from the side wall of the fiber bundle.
9. The fiber alignment composite material prepared by the preparation method of any one of claims 1 to 8, which comprises a matrix and fiber reinforcements dispersed in the matrix, wherein the fiber reinforcements are formed by aligning a plurality of heat-conducting fibers with micron-sized diameters along the out-of-plane direction of the fiber alignment composite material; the volume fraction of the heat conducting fiber in the fiber oriented composite material is 10-50%.
10. Use of the fiber alignment composite of claim 9 in the manufacture of a thermal gasket for an electronic device or a housing for a shielding box.
CN202211519966.7A 2022-11-30 2022-11-30 Fiber oriented arrangement composite material and preparation method and application thereof Pending CN115850742A (en)

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