CN114230823A - Dielectrophoresis-based carbon fiber composite material with enhanced interlayer performance and preparation method thereof - Google Patents
Dielectrophoresis-based carbon fiber composite material with enhanced interlayer performance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon fiber composite material with enhanced interlayer performance based on dielectrophoresis and a preparation method thereof. The preparation method comprises the following steps: 1) dispersing metal particles in a resin matrix to form a dispersion; 2) placing the dispersion liquid between carbon fiber layers after defoaming treatment, and arranging electrodes between the carbon fiber layers; 3) alternating current is introduced into the electrodes, and an electric field is applied to assemble metal particles into particle chains between the electrodes; moving the electrode to assemble the metal particle chains at a plurality of positions; 4) removing the upper and lower electrode plates, and carrying out hot-pressing curing to obtain the carbon fiber composite material product. The metal particle chain can be used as a bearing structure to avoid the generation of cracks, the conductivity between carbon fiber layers can be enhanced, and the dispersed particles can toughen the resin and hinder the crack propagation. According to the invention, an electric field is applied to act on metal particles to manufacture a micro-nano composite structure in directional arrangement, and the interlayer performance of the carbon fiber composite material is improved by combining a 'lead-in bearing structure' and 'matrix modification'.
Description
Technical Field
The invention relates to the field of micro-nano manufacturing of composite materials, in particular to a carbon fiber composite material with enhanced interlayer performance by using a dielectrophoresis technology and a method thereof.
Background
In recent years, carbon fiber composite materials have been rapidly developed due to excellent performance, and particularly gradually replace metal structure materials in the field of aerospace. The carbon fiber resin matrix composite has the characteristics of high specific strength, high specific modulus, fatigue resistance, corrosion resistance and excellent structural molding integration, but the conductivity in the thickness direction is poor due to the fact that the composite layers are bonded by resin with brittleness, insulation and low strength. In a complex working environment, the internal temperature and the internal stress are suddenly changed, cracks are easily generated between different layers of the carbon fiber composite material laminated plate and are spread along the layers to form delamination, so that the impact resistance and the fracture toughness of the material are weak, and the performance of the overall performance of the composite material is influenced.
The method for improving the performance between carbon fiber layers mainly comprises two types, namely 'introduction of a bearing structure' and 'toughening of a resin matrix', wherein the former mainly comprises three-dimensional weaving, sewing, z-pining technology and the like, and the introduction of the bearing structure with the dimension similar to that of the fiber in the thickness direction usually damages the fiber, so that the loss of the in-plane performance is caused. The method for modifying nano fiber, adhesive film and particles is gradually developed for resin matrix toughening, interlayer fiber and adhesive film toughening are difficult in the aspects of laying process and large-scale preparation, interlayer particle toughening is the current research hotspot, and excessive particles improve the resin toughness and reduce the structural strength due to the fact that the strength/toughness are usually mutually repellent, so that the balance point needs to be found between the strength and the toughness in the modification research at present. On the other hand, the common method for improving the conductivity of the resin matrix is to add conductive fillers such as metal, carbon nanotubes and the like, the performance optimization degree has a positive correlation with the content of the fillers, and the mechanical strength between the composite layers is still deteriorated if the content of the fillers is too high, so that the contradiction exists between the conductivity and the strength.
Disclosure of Invention
In order to better solve the problem of weak interlayer performance of the existing carbon fiber composite material, the invention provides a method for enhancing the interlayer performance of the carbon fiber composite material.
The invention relates to a method for enhancing interlayer performance of a carbon fiber composite material, which takes metal microparticles as a filler and epoxy resin as a polymer matrix, firstly mixes metal and resin through ultrasonic treatment, uses magnetic stirring to completely disperse the metal particles under heating conditions, uses a vacuum pump to extract bubbles in a solution, compounds the resin and carbon fibers together after cooling, applies an alternating current electric field between carbon fiber layers, performs assembly connection of metal particle chains, and finally cures to obtain a carbon fiber composite material product.
The technical scheme provided by the invention is as follows:
the invention provides a preparation method of a carbon fiber composite material with enhanced interlayer performance based on dielectrophoresis, which comprises the following steps:
1) dispersing metal particles in a resin matrix to form a dispersion;
2) placing the dispersion liquid between carbon fiber layers after defoaming treatment, and arranging electrodes between the carbon fiber layers;
3) alternating current is introduced into the electrodes, and an electric field is applied to assemble metal particles into particle chains between the electrodes; moving the electrode to assemble the metal particle chains at a plurality of positions;
4) and (4) removing the upper electrode plate and the lower electrode plate, enabling most of metal particles in the resin to be in a chain shape and vertical to the fiber laying layer, and then carrying out hot-pressing curing to obtain the carbon fiber composite material product.
Further, the content of the metal particles is 1.4-8% of the mass fraction of the resin matrix, and the particle size of the metal particles is 1-3 μm.
Further, the material of the metal particles includes copper or iron.
Further, the resin is epoxy resin, and the thickness of the resin layer is 10-20 μm. Preferably, the resin is bisphenol A epoxy resin, the viscosity is 11000-15000 cps at normal temperature, the proportion of the resin to a matched curing agent is 100:50, and the curing time is 24 hours at normal temperature or the heating curing is performed for 3 hours at 60 ℃.
Further, the metal particles are uniformly dispersed by ultrasound.
Further, the dispersion method of the metal particles is as follows: dispersing metal particles in an epoxy resin matrix, carrying out ultrasonic treatment for 30-60 minutes by using ultrasonic equipment (1000-2000W) at about 19.75KHz, wherein the solution is quickly heated by high-temperature high-pressure airflow generated by vibration, and the temperature of the dispersion liquid is kept below 70 ℃ during the ultrasonic treatment by adopting flowing condensed water; then a magnetic stirrer is used for stirring for 1-2 hours at the rotating speed of 380-450rpm and the heating temperature of 50-100 ℃, thereby ensuring that the particles can not be agglomerated or settled.
Further, the electrodes are needle-plate copper electrodes, and the electrodes are vertically arranged on two sides of the resin matrix.
Further, the assembling method in the step 3) comprises the following steps: firstly, connecting electrodes with alternating current, and applying high voltage to carry out dielectrophoresis assembly; then reducing the voltage for sintering, and finishing the assembly of the single metal particle chain when the current in the circuit is increased; the voltage application was continued until the current stabilized. High assembly voltage can reduce the movement time of the particles, and lower voltage is needed for sintering chains, so that the particle chains are prevented from being impacted.
Furthermore, a 10k omega protective resistor is connected in series in the dielectrophoresis assembled circuit; the assembly voltage is 40-50V, the frequency is 50-100Hz, and the assembly time is 3-6 minutes; the sintering voltage after depressurization is 10-20V.
Further, the magnitude of the applied electric field depends on the interlayer distance.
Further, the stable resistance of the assembled single metal particle chain is 50-200 omega, and the stable connection current is not more than 10 mA.
In a second aspect of the invention there is provided a dielectrophoresis-based carbon fibre composite having enhanced interlayer properties prepared by the method of the first aspect.
The invention has the beneficial effects that:
(1) according to the carbon fiber reinforced epoxy resin matrix composite material designed by the invention, the particle chains longitudinally connected in the interlayer matrix can serve as a bearing structure, the mechanical strength in the thickness direction is enhanced, and the impact strength of the composite material is improved.
(2) According to the carbon fiber reinforced epoxy resin matrix composite material, the particle chains in the resin matrix are used as good conductive paths among carbon fiber layers, so that the conductive performance of the resin layer is effectively enhanced, and the lightning stroke resistance of the composite material is optimized. And the particles account for the resin matrix in low mass percent, and the adhesive property of the resin cannot be damaged.
(3) According to the carbon fiber reinforced epoxy resin matrix composite material designed by the invention, metal particles with chain structures are not formed in the resin, so that the expansion of cracks in the material is favorably hindered, and the loss of in-plane performance is avoided through matrix modification and toughening of the resin.
(4) The carbon fiber reinforced epoxy resin matrix composite material designed by the invention is simple in operation method and low in cost, and can effectively promote the application of the carbon fiber composite material in the fields of aerospace and the like.
Drawings
FIG. 1 is a schematic representation of the micro-mechanism of the present invention;
FIG. 2 is a schematic view of the moving electrode assembly process of the present invention;
FIG. 3 is a schematic diagram of the process of particle chain formation in epoxy resin.
Detailed Description
The invention will be further illustrated with reference to specific examples, to which the present invention is not at all restricted.
Example 1
1) Dispersing metal copper particles in an E51 epoxy resin matrix, wherein the dispersion concentration is 20mg/ml, carrying out ultrasonic treatment for 30 minutes by using ultrasonic equipment at 19.75KHz, and then stirring for 1 hour at the heating temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of 400rpm to ensure that the particles do not agglomerate or settle.
2) And (2) cooling the mixed dispersion liquid in the step 1), pumping out bubbles of the resin by using a vacuum pump, and preparing the carbon fiber composite material by using the resin. When carbon fiber laying is carried out, an alternating current electric field is applied between carbon fiber layers, and needle-plate copper electrodes with a slightly wider interval than the layers are vertically arranged on two sides of the resin.
3) The voltage is 50V, the frequency is 50Hz, and a protective resistor of 10k omega is connected in series in the circuit. Dielectrophoretic assembly of the metal particles was started after application of the electric field, and the voltage was reduced to 20V after 6 minutes of assembly. When the current in the circuit suddenly increases, the single copper particle chain is assembled between the electrodes, the electric field is continuously applied for 1-2 minutes at the moment, the reading of the current indicator is still stable, the electric field is removed at the moment, the electrodes are moved to the next assembling position, and the step 3) is repeated;
4) the assembly positions are set according to the required particle chain density, after all the positions are assembled, the upper electrode plate and the lower electrode plate are withdrawn, most of metal particles in the resin are in a chain shape and are vertical to the fiber laying layer, dielectrophoresis assembly is completed, and finally, the carbon fiber composite material product is obtained through hot pressing and curing.
Example 2
1) Dispersing metal copper particles in an E51 epoxy resin matrix, wherein the dispersion concentration is 50mg/ml, carrying out ultrasonic treatment for 30 minutes by using ultrasonic equipment at 19.75KHz, and then stirring for 1.5 hours at the heating temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of 400rpm to ensure that the particles do not have agglomeration or sedimentation.
2) And (2) cooling the mixed dispersion liquid in the step 1), pumping out bubbles of the resin by using a vacuum pump, and preparing the carbon fiber composite material by using the resin. When carbon fiber laying is carried out, an alternating current electric field is applied between carbon fiber layers, and needle-plate copper electrodes with a slightly wider interval than the layers are vertically arranged on two sides of the resin.
3) The voltage is 50V, the frequency is 50Hz, and a protective resistor of 10k omega is connected in series in the circuit. Dielectrophoretic assembly of the metal particles was started after application of the electric field, and the voltage was reduced to 10V after 6 minutes of assembly. When the current in the circuit suddenly increases, the single copper particle chain is assembled between the electrodes, the electric field is continuously applied for 1-2 minutes at the moment, the reading of the current indicator is still stable, the electric field is removed at the moment, the electrodes are moved to the next assembling position, and the step 3) is repeated;
4) the assembly positions are set according to the required particle chain density, after all the positions are assembled, the upper electrode plate and the lower electrode plate are withdrawn, most of metal particles in the resin are in a chain shape and are vertical to the fiber laying layer, dielectrophoresis assembly is completed, and finally, the carbon fiber composite material product is obtained through hot pressing and curing.
Example 3
1) Dispersing metal copper particles in an E51 epoxy resin matrix, wherein the dispersion concentration is 80mg/ml, performing ultrasonic treatment for 45 minutes by using ultrasonic equipment at 19.75KHz, and stirring for 1.5 hours at the heating temperature of 80 ℃ by using a magnetic stirrer at the rotating speed of 420rpm to ensure that the particles do not agglomerate or settle.
2) And (2) cooling the mixed dispersion liquid in the step 1), pumping out bubbles of the resin by using a vacuum pump, and preparing the carbon fiber composite material by using the resin. When carbon fiber laying is carried out, an alternating current electric field is applied between carbon fiber layers, and needle-plate copper electrodes with a slightly wider interval than the layers are vertically arranged on two sides of the resin.
3) The voltage is 40V, the frequency is 60Hz, and a protective resistor of 10k omega is connected in series in the circuit. Dielectrophoretic assembly of the metal particles was started after application of the electric field, and the voltage was reduced to 10V after 4 minutes of assembly. When the current in the circuit suddenly increases, the single copper particle chain is assembled between the electrodes, the electric field is continuously applied for 1-2 minutes at the moment, the reading of the current indicator is still stable, the electric field is removed at the moment, the electrodes are moved to the next assembling position, and the step 3) is repeated;
4) the assembly positions are set according to the required particle chain density, after all the positions are assembled, the upper electrode plate and the lower electrode plate are withdrawn, most of metal particles in the resin are in a chain shape and are vertical to the fiber laying layer, dielectrophoresis assembly is completed, and finally, the carbon fiber composite material product is obtained through hot pressing and curing.
Example 4
1) Dispersing metal copper particles in an E51 epoxy resin matrix, wherein the dispersion concentration is 100mg/ml, performing ultrasonic treatment for 60 minutes by using ultrasonic equipment at 19.75KHz, and stirring for 2 hours at the heating temperature of 100 ℃ by using a magnetic stirrer at the rotating speed of 450rpm to ensure that the particles do not agglomerate or settle.
2) And (2) cooling the mixed dispersion liquid in the step 1), pumping out bubbles of the resin by using a vacuum pump, and preparing the carbon fiber composite material by using the resin. When carbon fiber laying is carried out, an alternating current electric field is applied between carbon fiber layers, and needle-plate copper electrodes with a slightly wider interval than the layers are vertically arranged on two sides of the resin.
3) The voltage is 40V, the frequency is 100Hz, and a protective resistor of 10k omega is connected in series in the circuit. Dielectrophoretic assembly of the metal particles was started after application of the electric field, and the voltage was reduced to 10V after 3 minutes of assembly. When the current in the circuit suddenly increases, the single copper particle chain is assembled between the electrodes, the electric field is continuously applied for 1-2 minutes at the moment, the reading of the current indicator is still stable, the electric field is removed at the moment, the electrodes are moved to the next assembling position, and the step 3) is repeated;
4) the assembly positions are set according to the required particle chain density, after all the positions are assembled, the upper electrode plate and the lower electrode plate are withdrawn, most of metal particles in the resin are in a chain shape and are vertical to the fiber laying layer, dielectrophoresis assembly is completed, and finally, the carbon fiber composite material product is obtained through hot pressing and curing.
Example 5
1) Dispersing metallic iron particles in an E51 epoxy resin matrix, wherein the dispersion concentration is 40mg/ml, performing ultrasonic treatment for 60 minutes by using ultrasonic equipment at 19.75KHz, and stirring for 2 hours at the heating temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of 400rpm to ensure that the particles do not agglomerate or settle.
2) And (2) cooling the mixed dispersion liquid in the step 1), pumping out bubbles of the resin by using a vacuum pump, and preparing the carbon fiber composite material by using the resin. When carbon fiber laying is carried out, an alternating current electric field is applied between carbon fiber layers, and needle-plate copper electrodes with a slightly wider interval than the layers are vertically arranged on two sides of the resin.
3) The voltage is 40V, the frequency is 100Hz, and a protective resistor of 10k omega is connected in series in the circuit. Dielectrophoretic assembly of the metal particles was started after application of the electric field, and the voltage was reduced to 10V after 3 minutes of assembly. When the current in the circuit suddenly increases, the single copper particle chain is assembled between the electrodes, the electric field is continuously applied for 1-2 minutes at the moment, the reading of the current indicator is still stable, the electric field is removed at the moment, the electrodes are moved to the next assembling position, and the step 3) is repeated;
4) the assembly positions are set according to the required particle chain density, after all the positions are assembled, the upper electrode plate and the lower electrode plate are withdrawn, most of metal particles in the resin are in a chain shape and are vertical to the fiber laying layer, dielectrophoresis assembly is completed, and finally, the carbon fiber composite material product is obtained through hot pressing and curing.
Example 6
1) Dispersing metallic iron particles in an E51 epoxy resin matrix, wherein the dispersion concentration is 80mg/ml, performing ultrasonic treatment for 60 minutes by using ultrasonic equipment at 19.75KHz, and stirring for 1 hour at the heating temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of 450rpm to ensure that the particles do not agglomerate or settle.
2) And (2) cooling the mixed dispersion liquid in the step 1), pumping out bubbles of the resin by using a vacuum pump, and preparing the carbon fiber composite material by using the resin. When carbon fiber laying is carried out, an alternating current electric field is applied between carbon fiber layers, and needle-plate copper electrodes with a slightly wider interval than the layers are vertically arranged on two sides of the resin.
3) The voltage is 40V, the frequency is 60Hz, and a protective resistor of 10k omega is connected in series in the circuit. Dielectrophoretic assembly of the metal particles was started after application of the electric field, and the voltage was reduced to 10V after 3 minutes of assembly. When the current in the circuit suddenly increases, the single copper particle chain is assembled between the electrodes, the electric field is continuously applied for 1-2 minutes at the moment, the reading of the current indicator is still stable, the electric field is removed at the moment, the electrodes are moved to the next assembling position, and the step 3) is repeated;
4) the assembly positions are set according to the required particle chain density, after all the positions are assembled, the upper electrode plate and the lower electrode plate are withdrawn, most of metal particles in the resin are in a chain shape and are vertical to the fiber laying layer, dielectrophoresis assembly is completed, and finally, the carbon fiber composite material product is obtained through hot pressing and curing.
Fig. 1 shows a microscopic mechanism, taking copper metal particles as an example, the copper metal particles in the carbon fiber interlayer resin are connected with each other after being assembled to form a bearing structure, and dispersed particles can contribute to toughening of a matrix, so that two mechanisms exist to synergistically optimize mechanical properties.
Fig. 2 shows a schematic diagram of the assembly process by moving the electrode, where R1 is a protective resistor to prevent the metal chain from being destroyed by the impact of high current, and the indicator is used to indicate the current value in the circuit, and also as a monitor of the assembly completion of the particle chain, and the needle electrode is moved to assemble the next particle chain after each assembly completion.
Fig. 3 shows the process of particle chain formation in epoxy resins, applying an alternating voltage between the electrodes, creating a non-uniform electric field across the gap, causing the metal particles in the resin dispersion to become polarized, the polarized particles being subjected to dielectrophoretic forces in the non-uniform electric field, moving in the direction of increasing electric field strength, while the polarized particles are subjected to other polarized particles in their attractive region by dipole-dipole attractive forces, until viscous drag and attractive forces are balanced and the velocity no longer increases. Eventually the particles will form a "bridge" between the electrodes, allowing the circuit to be completed. The current does not rise immediately at the beginning of the formation of the particle chains due to the presence of the oxide film on the surface of the copper particles, and the insulating film present at the particle interface causes a high resistance value of the entire particle chain, and the voltage drop between the electrodes is still large, so that a larger electric field is generated across the insulating film between the particle interfaces, and the insulating film breaks down over time, and the current passing through the particle chain gradually increases. Joule heat generated by the increase of the current causes the surface of the copper particles to be sintered, so that the resistance of the particle chain is greatly reduced, the current is increased more quickly, and a positive feedback mechanism is formed. When the current is increased to be approximate to the short circuit of the electrode gap, the voltage between the electrodes is reduced, the particles which are not sintered in the particle chain lose the polarization state, and the particles are gradually loosened in the strong convection near the particle chain, and finally a particle chain with stable resistance is formed.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a carbon fiber composite material with enhanced interlayer performance based on dielectrophoresis is characterized by comprising the following steps:
1) dispersing metal particles in a resin matrix to form a dispersion;
2) placing the dispersion liquid between carbon fiber layers, and arranging electrodes between the carbon fiber layers;
3) alternating current is introduced into the electrodes, and an electric field is applied to assemble metal particles into particle chains between the electrodes; moving the electrode to assemble the particle chains at a plurality of positions;
4) removing the upper and lower electrode plates, and carrying out hot-pressing curing to obtain the carbon fiber composite material product.
2. The method of claim 1, wherein: the content of the metal particles is 1.4-8% of the mass fraction of the resin matrix, and the particle size of the metal particles is 1-3 μm.
3. The method of claim 1, wherein: the material of the metal particles comprises copper or iron.
4. The method of claim 1, wherein: the resin is epoxy resin, and the thickness of the resin layer is 10-20 μm.
5. The method of claim 1, wherein: the metal particles are uniformly dispersed by ultrasound.
6. The method of claim 1, wherein the electrode is a pin-plate copper electrode.
7. The method according to claim 1, wherein the assembling method in step 3) is: firstly, connecting electrodes with alternating current, and applying high voltage to carry out dielectrophoresis assembly; then reducing the voltage for sintering, and finishing the assembly of the single metal particle chain when the current in the circuit is increased; the voltage application was continued until the current stabilized.
8. The method of claim 7, wherein a 10k Ω protective resistor is connected in series in the dielectrophoretic assembled circuit; the assembled voltage is 40-50V, and the frequency is 50-100 Hz; the sintering voltage after depressurization is 10-20V.
9. The method of claim 1, wherein the assembled single metal particle chain has a stable resistance of 50-200 Ω and a stable connection current of no more than 10 mA.
10. A carbon fiber composite material with enhanced interlayer performance based on dielectrophoresis is characterized in that: prepared by the process of any one of claims 1 to 9.
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| US20040026249A1 (en) * | 2000-04-11 | 2004-02-12 | Whatmore Roger W | Electric- field structuring of composite materials |
| JP2010027251A (en) * | 2008-07-15 | 2010-02-04 | Nikon Corp | Laminate, and manufacturing method thereof |
| CN106084264A (en) * | 2016-06-17 | 2016-11-09 | 中国人民解放军装甲兵工程学院 | A kind of composite laminated plate preparation technology of carbon nano-tube oriented arrangement |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040026249A1 (en) * | 2000-04-11 | 2004-02-12 | Whatmore Roger W | Electric- field structuring of composite materials |
| JP2010027251A (en) * | 2008-07-15 | 2010-02-04 | Nikon Corp | Laminate, and manufacturing method thereof |
| CN106084264A (en) * | 2016-06-17 | 2016-11-09 | 中国人民解放军装甲兵工程学院 | A kind of composite laminated plate preparation technology of carbon nano-tube oriented arrangement |
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| CHOUNG-KEUN LEE等: "Nano-Composite Manufacturing Using the Electro-Orientation Method of Micro/Nano-Particles in a Liquid Polymer with Mechanical Characteristics Analysis", 《INTERNATIONAL JOURNAL OF PRECISION ENGINEERING AND MANUFACTURING》 * |
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