CN101250742A - Method for improving interface performance of conductive fiber composite material - Google Patents
Method for improving interface performance of conductive fiber composite material Download PDFInfo
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- CN101250742A CN101250742A CNA2008100525057A CN200810052505A CN101250742A CN 101250742 A CN101250742 A CN 101250742A CN A2008100525057 A CNA2008100525057 A CN A2008100525057A CN 200810052505 A CN200810052505 A CN 200810052505A CN 101250742 A CN101250742 A CN 101250742A
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Abstract
The invention relates to a method for improving interfacial properties of conducting fiber compound materials, which comprises the following steps: firstly, arranging carbon nanometer tubes with functionalized surface into water solution according to the ratio of 0.01-1mg/ml, ultrasonically vibrating for 0.5-3h, then arranging conducting fiber fabric in water solution according to the mass ratio of 100-5:1 between the water solution and the conducting fiber fabric, connecting the conducting fiber fabric to the positive electrode of direct current power supply, negative electrode metallic plates which are connected with the negative electrode of the direct current power supply are arranged around the conducting fiber fabric, connecting the direct current power supply to the positive and the negative electrodes under the voltage of 12-20V, keeping the electric potential difference of 5-15V/cm between the metallic plate and the conducting fiber fabric, taking out the conducting fiber fabric after 0.5-3h, drying, and obtaining the conducting fiber compound materials by compounding and curing molding the conducting fiber fabric and epoxide resin through adopting the vacuum assisted resin transfering mould shaping method. The nanometer tubes comprise a single-wall carbon nanometer tube, a double-wall carbon nanometer tube and a multi-wall carbon nanometer tube, and the average length is 1-20 micrometer.
Description
Technical field
The present invention relates to advanced composite material interface modification technology, be specially a kind of by electrophoresis at conductive fiber surfaces deposition one deck carbon nanotube, and then improve the method for resin base interface performance of conductive fiber composite material.
Background technology
Along with the continuous development of aerospace and modern weapons, material therefor is had higher requirement.For example when the bearing carrier of design guided missile, man-made satellite, aircraft, more and more need the high material of specific tenacity and specific modulus.So lightweight, high-strength resin-based carbon fiber composite occupy more and more important position in high skill field and national defense construction.This matrix material is made up of enhanced carbon fiber and resin matrix, and its performance depends primarily on the mechanical property of carbon fiber, the performance of matrix and the interface performance between carbon fiber and the matrix.But since the interface performance between carbon fiber and the resin matrix a little less than, thereby cause the use range of resin-based carbon fiber composite to be very restricted.
According to composite material interface transition layer theory, at fiber (as carbon fiber) and at the interface resin-based, if there is not transition layer, the rapid sudden change of Young's modulus can take place at phase interface then, phase interface has just become the tensile destination node, becomes formation of crack; If there be the transition layer of one deck modulus between fiber and resin base, the tension variation of phase interface will be slowed down, and has the possibility of stress relaxation, and the probability of crackle formation will be reduced at the interface, and the interface performance of matrix material will be improved accordingly.
Mainly is coating at present, promptly at the functional material of carbon fiber surface coating one deck modulus between fiber and resin, as many structures silsesquioxane, contain nanometer SiO according to the theoretical method that improves the composite material interface performance of transition layer
2Particulate resin and special type phenolic etc.This method can significantly improve the interface performance of matrix material as the method for modifying of important composite material interface, but also exists damage fiber bodies intensity and cause between the fiber shortcoming such as adhesion.
Summary of the invention
At the deficiencies in the prior art, the technical problem that quasi-solution of the present invention is determined is a kind of method that improves interface performance of conductive fiber composite material of research.This method modified effect is remarkable, does not damage the body intensity of carbon fiber simultaneously, can not produce adhesion between the fiber, is of value to the practical ranges that enlarges matrix material.
The technical scheme that the present invention solve the technical problem is, design a kind of method that improves interface performance of conductive fiber composite material, this method places the aqueous solution with the carbon nanotube of functionalisation of surfaces according to the ratio of 0.01～1mg/ml earlier, after leaving standstill 1～3 hour, according to the aqueous solution and electro-conductive fiber fabric quality ratio is that 100～5: 1 ratio places the described aqueous solution with the electro-conductive fiber fabric, and the electro-conductive fiber fabric is connected with the positive pole of direct supply; The negative pole metal sheet that is connected with dc power cathode is installed around the electro-conductive fiber fabric; Positive and negative electrode 12～20V voltage feeds direct current down, and keep the potential difference of 5～15V/cm between negative pole metal sheet and the electro-conductive fiber fabric, 0.5 take out the electro-conductive fiber fabric after～3 hours, after the drying, utilize the vacuum-assisted resin transfer mold shaping method promptly with electro-conductive fiber fabric and the moulding of Resins, epoxy composite curing; Described carbon nanotube comprises Single Walled Carbon Nanotube, double-walled carbon nano-tube and multi-walled carbon nano-tubes, and the mean length of carbon nanotube is 1～20 micron.
Compared with prior art, the method that the present invention improves interface performance of conductive fiber composite material by electrophoresis at composite material reinforcement body conductive fiber surfaces stringer carbon nanotube, after electro-conductive fiber fabric and resin base (Resins, epoxy) are compound, between electro-conductive fiber and resin matrix, formed the nano composite material transition layer of one deck carbon nanotube reinforced epoxy.This transition layer modulus is between carbon fiber and Resins, epoxy, can improve the transmittability of conductive fiber composite material phase interface stress, the mechanical property of reinforced composite phase interface, reduce the probability that the phase interface crackle produces, can not damage simultaneously the body intensity of electro-conductive fiber, can not produce adhesion between the electro-conductive fiber, modified effect is remarkable, helps enlarging the use range of matrix material.
Description of drawings
Fig. 1 improves the principle schematic of the described surface electrical deposition of carbon nanotubes at the electro-conductive fiber fabric of the method for interface performance of conductive fiber composite material for the present invention.
Embodiment
Further narrate the present invention below in conjunction with embodiment and accompanying drawing thereof:
The method (hereinafter to be referred as method, referring to Fig. 1) of the raising interface performance of conductive fiber composite material of the present invention's design, this method is inserted the carbon nanotube 5 of functionalisation of surfaces in the aqueous solution 3 according to the ratio of 0.01～1mg/ml earlier, the preparation electrophoresis aqueous solution; After leaving standstill 1～3 hour, again composite material reinforcement body electro-conductive fiber fabric 4 is inserted in the described aqueous solution 3 according to the aqueous solution 3 and the ratio of electro-conductive fiber fabric 4 mass ratioes 100～5: 1, and electro-conductive fiber fabric 4 is connected with the positive pole 2 of direct supply; Around the electro-conductive fiber fabric 4 negative pole metal sheet 6 is installed, negative pole metal sheet 6 is connected with the negative pole 1 of described direct supply; Positive and negative electrode 12～20V voltage fed direct current 0.5～3 hour down, and keep the potential difference of 5～15V/cm between negative pole metal sheet 6 and the electro-conductive fiber fabric 4, take out this electro-conductive fiber fabric 4 then, at this moment can form the carbon nanotube 5 of skim at the fiber surface of electro-conductive fiber fabric 4, after the drying, utilize the vacuum-assisted resin transfer mold shaping method promptly with electro-conductive fiber fabric 4 and the moulding of Resins, epoxy composite curing.Described carbon nanotube 5 comprises Single Walled Carbon Nanotube, double-walled carbon nano-tube and multi-walled carbon nano-tubes, and the mean length of carbon nanotube 5 is 1～20 micron.
The described electro-conductive fiber fabric 4 of the inventive method comprises the fabric that electro-conductive fibers such as carbon fiber and steel fiber are made, and the existence form of electro-conductive fiber fabric 4 can be planar (two dimension) or three-dimensional form in electrophoresis process.The functionalisation of surfaces of carbon nanotube 5 is meant carbon nanotube 5 after the strong acid oxide treatment, and the treatment process of functional groups such as carboxyl is introduced on the surface.Positive and negative electrode voltage in the electrophoresis process is 12～20V, and size of current decides according to the ionogen situation in the described aqueous solution 3.Described negative pole metal sheet 6 is that general conducting metal gets final product, as copper, aluminium, iron etc.Described assisted resin transfer mould forming method (VARTM) is a prior art.The used solidifying agent of VARTM is a Tetra Hydro Phthalic Anhydride, and its mass percentage content is 30～50%.
The inventive method is further characterized in that and contains the potassium hydroxide that concentration expressed in percentage by weight is 0.05～1wt% in the described aqueous solution, makes aqueous electrolyte liquid.This aqueous electrolyte liquid can shorten the described electrophoretic time.
After the further feature of the inventive method also is to insert in the aqueous solution 3 or the aqueous electrolyte liquid according to the ratio of 0.01～1mg/ml the carbon nanotube 5 of functionalisation of surfaces, with frequency 28kHZ, power is the described aqueous solution 0.5～3h of the ultra-sonic oscillation of 100～600W.After adding ultra-sonic oscillation, can quicken to disperse, described carbon nanotube is well-dispersed in the described aqueous solution, help even electrophoresis.
The present invention does not address part and is applicable to prior art.
Provide the specific embodiment of the inventive method below, but the inventive method is not limited to embodiment, embodiment does not limit claim of the present invention yet.
Embodiment 1
Get 40 milligrams of multi-walled carbon nano-tubes and mix, make aqueous electrolyte liquid with 1000 milliliters of distilled water that contain 0.5wt%KOH; Place frozen water to carry out sonic oscillation in the beaker of described aqueous electrolyte liquid, hunting power is 300 watts, and duration of oscillation is 1 hour, and adds ice cube one time every 20 minutes.The mean length of carbon nanotube is 2 microns, after vibration finishes, leaves standstill 2 hours; 10 gram carbon fiber three dimensional fabrics are placed the described aqueous solution, and insert galvanic positive pole, galvanic negative pole inserts on the aluminium sheet of carbon fibre fabric both sides, and 12V feeds direct current down, and the maintenance potential difference is 12V/cm.Stop energising after one hour, take out carbon fibre fabric, in 110 ℃ vacuum drying oven dry 2 hours, with dried carbon fibre fabric promptly by VARTM technology and Resins, epoxy composite molding.The used solidifying agent of VARTM technology is a Tetra Hydro Phthalic Anhydride, and its mass percentage content is 41%.
After testing, the carbon fiber enhancement resin base three-dimensional composite material interlaminar shear strength of present embodiment gained behind the electrochemical deposition carbon nanotube improved 18%.
Get 100 milligrams of Single Walled Carbon Nanotube and mix, make the electrophoresis aqueous solution with 1000 milliliters of distilled water that contain 0.3wt%KOH; The described aqueous solution is carried out sonic oscillation, and hunting power is 200 watts, and duration of oscillation is 1.5 hours, and every vibration just stopped to cool off 5 minutes in 10 minutes.The mean length of carbon nanotube is 8 microns, after vibration finishes, leaves standstill 1 hour; 10 gram carbon fiber three dimensional fabrics are placed the described electrophoresis aqueous solution, and insert galvanic positive pole, on the iron plate of the both sides of galvanic negative pole access carbon fibre fabric, it is 10V/cm that 15V feeds direct current maintenance potential difference.Stop energising after one hour, take out carbon fibre fabric, drying is 1 hour in 110 ℃ vacuum drying oven; With dried carbon fibre fabric promptly by VARTM technology and Resins, epoxy composite molding.
After testing, the carbon fiber enhancement resin base three-dimensional composite material interlaminar shear strength of present embodiment gained behind the electrochemical deposition carbon nanotube improved 16%.
Get 200 milligrams of multi-walled carbon nano-tubes and mix, make the electrophoresis aqueous solution with 1000 ml distilled waters; The beaker that will contain carbon nano-tube aqueous solutions places frozen water to carry out sonic oscillation, and hunting power is 400 watts, and duration of oscillation is 3 hours.The mean length of carbon nanotube is 12 microns, after vibration finishes, leaves standstill 3 hours; 20 gram carbon fiber three dimensional fabrics are placed the described electrophoresis aqueous solution, and insert galvanic positive pole, galvanic negative pole inserts on the copper coin of carbon fibre fabric both sides, and 20V feeds direct current down, and the maintenance potential difference is 8V/cm; Stop energising after two hours, take out carbon fibre fabric, drying is 1 hour in 110 ℃ vacuum drying oven; With dried carbon fibre fabric promptly by VARTM technology and Resins, epoxy composite molding.
After testing, the carbon fiber enhancement resin base three-dimensional composite material interlaminar shear strength of present embodiment gained behind the electrochemical deposition carbon nanotube improved 20%.
Claims (3)
1. method that improves interface performance of conductive fiber composite material, this method places the aqueous solution with the carbon nanotube of functionalisation of surfaces according to the ratio of 0.01～1mg/ml earlier, after leaving standstill 1～3 hour, according to the aqueous solution and electro-conductive fiber fabric quality ratio is that 100～5: 1 ratio places the described aqueous solution with the electro-conductive fiber fabric, and the electro-conductive fiber fabric is connected with the positive pole of direct supply; The negative pole metal sheet that is connected with dc power cathode is installed around the electro-conductive fiber fabric; Positive and negative electrode 12～20V voltage feeds direct current down, and keep the potential difference of 5～15V/cm between negative pole metal sheet and the electro-conductive fiber fabric, 0.5 take out the electro-conductive fiber fabric after～3 hours, after the drying, utilize the vacuum-assisted resin transfer mold shaping method promptly with electro-conductive fiber fabric and the moulding of Resins, epoxy composite curing; Described carbon nanotube comprises Single Walled Carbon Nanotube, double-walled carbon nano-tube and multi-walled carbon nano-tubes, and the mean length of carbon nanotube is 1～20 micron.
2. the method for raising interface performance of conductive fiber composite material according to claim 1 is characterized in that containing in the described aqueous solution potassium hydroxide that concentration expressed in percentage by weight is 0.05～1wt%.
3. the method for raising interface performance of conductive fiber composite material according to claim 1 and 2, after it is characterized in that the carbon nanotube of functionalisation of surfaces placed the aqueous solution according to the ratio of 0.01～1mg/ml, with frequency 28kHZ, power is the described aqueous solution 0.5～3h of the ultra-sonic oscillation of 100～600W.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877311A (en) * | 2012-10-25 | 2013-01-16 | 哈尔滨工业大学 | Sizing agent for carbon fiber composite repairing and application method thereof |
| CN103554529A (en) * | 2013-10-09 | 2014-02-05 | 西安西热锅炉环保工程有限公司 | Epoxy resin-based conductive composite material and preparation method thereof |
| CN103572351A (en) * | 2012-07-31 | 2014-02-12 | 宝马股份公司 | Carbon fiber reinforced plastic member and method and device for forming anti-corrosion layer |
| CN112409027A (en) * | 2020-11-04 | 2021-02-26 | 南昌航空大学 | Method for improving uniformity of electrophoretic deposits on SiC fiber bundle |
| CN114181494A (en) * | 2020-09-14 | 2022-03-15 | 中国科学院福建物质结构研究所 | Preparation method of anti-delamination high-conductivity polymer matrix composite material prepared by carbon nano tube bucky paper in-situ deposition of carbon fibers |
-
2008
- 2008-03-24 CN CNA2008100525057A patent/CN101250742A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103572351A (en) * | 2012-07-31 | 2014-02-12 | 宝马股份公司 | Carbon fiber reinforced plastic member and method and device for forming anti-corrosion layer |
| CN102877311A (en) * | 2012-10-25 | 2013-01-16 | 哈尔滨工业大学 | Sizing agent for carbon fiber composite repairing and application method thereof |
| CN102877311B (en) * | 2012-10-25 | 2014-06-04 | 哈尔滨工业大学 | Sizing agent for carbon fiber composite repairing and application method thereof |
| CN103554529A (en) * | 2013-10-09 | 2014-02-05 | 西安西热锅炉环保工程有限公司 | Epoxy resin-based conductive composite material and preparation method thereof |
| CN103554529B (en) * | 2013-10-09 | 2016-03-02 | 西安西热锅炉环保工程有限公司 | A kind of epoxy resin based conductive composite material and preparation method thereof |
| CN114181494A (en) * | 2020-09-14 | 2022-03-15 | 中国科学院福建物质结构研究所 | Preparation method of anti-delamination high-conductivity polymer matrix composite material prepared by carbon nano tube bucky paper in-situ deposition of carbon fibers |
| CN114181494B (en) * | 2020-09-14 | 2023-03-28 | 中国科学院福建物质结构研究所 | Preparation method of anti-layering high-conductivity polymer matrix composite material prepared by in-situ deposition of carbon fibers on carbon nanotube base paper |
| CN112409027A (en) * | 2020-11-04 | 2021-02-26 | 南昌航空大学 | Method for improving uniformity of electrophoretic deposits on SiC fiber bundle |
| CN112409027B (en) * | 2020-11-04 | 2023-01-17 | 南昌航空大学 | Method for improving uniformity of electrophoretic deposits on SiC fiber bundle |
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Open date: 20080827 |