CN105200401A - Carbon fiber surface metallization method - Google Patents
Carbon fiber surface metallization method Download PDFInfo
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- CN105200401A CN105200401A CN201510715560.XA CN201510715560A CN105200401A CN 105200401 A CN105200401 A CN 105200401A CN 201510715560 A CN201510715560 A CN 201510715560A CN 105200401 A CN105200401 A CN 105200401A
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Abstract
The invention discloses a carbon fiber surface metallization method. The method is characterized in that carbon fibers undergo early-stage pretreatment degumming activation, and a chemical technology is adopted to realize double nickel plating of the surface of the carbon fibers to form a carbon fiber surface protection layer material; and the method comprises carbon fiber water washing, carbon fiber heating degumming, water washing, carbon fiber coarsening, pickling neutralization, carbon fiber dispersion treatment, primary chemical nickel plating, secondary chemical nickel plating, carbon fiber water washing, hot air drying and quality examination. The carbon fiber water washing adopts deionized water, and is carried out at 30-40DEG C for 10-20min; the carbon fiber heating degumming is carried out at 200-250DEG C; the coarsening adopts a 35% nitric acid solution, and immersion is carried out for 25min; and carbon fiber chemical plating technological parameters comprise 300-400g/L of nickel sulfate, 20-30ml/L of an HF solution, 30-50g/L of nickel chloride, 10-15ml/L of sodium hypophosphite, the pH value of 3.0-4.0, the temperature of 40-50DEG C, the primary nickel plating time of 2-3min and the secondary nickel plating time of 3-4min. The method adopts a double electroplating technology, a nickel plating layer has stable quality and has large bonding force with a substrate, and the thickness of a surface plating layer is uniform and can reach 300[mu]m.
Description
Technical field
The present invention relates to a kind of carbon fiber surface method for metallising.
Background technology
Carbon fiber has high specific tenacity, high ratio modulus, high temperature resistant, resistance to ablation, wear-resistant, conduction, heat conduction and a series of excellent properties such as the coefficient of expansion is little, it is not only the requisite structured material, corrosion resistant material, lagging material and the special type function material that manufacture rocket, guided missile, satellite space shuttle and space station, and be air fighter, airline carriers of passengers, the lightweight of vertisplane, the main reinforcement fibres of high performance, be thus used widely in hi-tech industry.Its demand increases year by year with double-digit growth speed.Carbon fiber industry, in the upgrading of developed country mainstay industry and even overall economic performance raising, is playing more and more important effect, to the adjustment of Industry Structure and the update of traditional material also significant.
A kind of special fibre that carbon fiber is mainly made up of carbon, molecular structure circle is between graphite and diamond, and carbon containing volume fraction is different with kind difference, generally more than 0.9.Carbon fiber is black, and it utilizes the carbonization and obtaining under rare gas element medium and high temperature state of various organic fibre.Carbon fiber has very excellent mechanical property,, in current mass-produced high-performance fiber, there is the highest specific tenacity and the one of the highest specific modulus, particularly 2000 " in the high temperature inert environment of more than C; carbon material is the material that unique intensity does not decline, be other primary structural material (metal and alloy thereof) incomparable.
Carbon fiber is very close with graphite at atomic scale, be made up of the carbon atom arranged with hexangle type from level to level, difference of them is link between layers, graphite is crystalline structure, its layer asks that link is loose, and carbon fiber is not crystalline structure, and it is irregular that interlayer links, so just, prevent slippage, enhancing substance intensity.The most excellent character of carbon fiber is that intensity is high, modulus is high, density is low, and the density of carbon fiber is 1/4 of steel, is 1/2 of aluminium alloy, larger than steel 16 times of its specific tenacity, larger than aluminium alloy 12 times.In addition, carbon fiber also has the various premium propertiess of carbon, and as high temperature resistant, under nonoxidizing atmosphere condition, carbon fiber can use 2000 degree time, and under the high temperature of 3000 degree, not melting is softened; Thermal expansivity is little, thermal conductivity is large, can resistance to rapid heat cycle, also can not burst even if drop to suddenly room temperature from the high temperature of 3000C; Good corrosion resistance, the erosion medium resistance such as ability concentrated hydrochloric acid, phosphoric acid, sulfuric acid, benzene, acetone; Electroconductibility is good.Meanwhile, it has again the flexibility as fiber, can carry out braiding processing and Wrapping formed.Meanwhile, carbon fiber also has some shortcomings, and such as: shock resistance is poor, under air and high temperature, (lower than 600C) can be oxidized.
The production of carbon fiber starts from the beginning of the seventies the 6's Mos of 20th century, is raw material at that time, makes carbon fiber through preoxidation, carbonization, greying with viscose fiber, mainly prevents hot gas flow from conducting at rocket nozzle and uses.
(1) will there is volatile growth in the demand of carbon fiber
According to the relevant dealer's prediction of carbon fiber, in cylinder from now on 8 years, the annual requirement of Global Carbon fiber will there will be volatile growth: namely increase by more than four times from current 100,000,000 pounds (closing 4.54 ten thousand tons), reach 4-5 hundred million pounds, this point has the order of a lot of military products and aircraft industry and some files to testify.Meanwhile, the price of carbon fiber is also in rising, and 5 dollars/pound from the past go up to current 20 dollars/pound.
(2) excellent properties of carbon fiber makes it be widely used
Carbon fiber has the advantages that intensity is high and quality is light, and general and epoxy resin etc. makes matrix material, and for the CFRP of the PAN base usually applied, its proportion is 1.7 stone roller .0, is 1/5th of steel; Tensile strength is 102 kilograms/ram2, similar with steel, and the feature such as high temperature resistant, corrosion-resistant and difficult combustion in addition.From over 35 years of carbon fiber appearance, widespread use in aerospace industry, car industry, yacht industry and aircraft industry, shows light weight and energy-conservation superiority.In aerospace industry, for making satellite, rocket and missile component, in car industry, for making automobile ceiling, engine shield and interior trim etc.In addition, carbon fiber is also for making wind power plant fan blade, pressurized vessel and leisure, sports goods (as Veronicastrum Herb and golf club) etc.
In recent years, carbon fiber develops rapidly in aircraft industry, originally for making machine tail piece, the outside of wing and fuselage and inner parts are now developed into, comprise stopper etc., as Boeing 787 passenger plane manufacturer have employed a large amount of carbon fiber in it makes, waiting in expectation puts into operation can reduce fuel consumption.This passenger plane manufacturer has also signed the supply contract of carbon fiber before 2021 with the Dong Li company of manufacturer one of Japanese textiles, carbon fiber and a resin.A-350 passenger plane also makes whole wing at research carbon fiber.
The material that the mankind use experienced by natural materials, work material, synthetic materials and enter into matrix material epoch of current forth generation.Matrix material is the heterogeneous material be composited by starting material such as organic polymer, inorganic non-metallic and metals.The part of properties that it can not only keep its stock blend to have separately, makes each component property mutually be supplemented, excellent properties not available when even also may to give stock blend be single-material.Along with the development and utilization of high-performance carbon fibre, matrix material is also impelled to enter from the first-generation of glass filament reinforced plastics with the new period of carbon fiber reinforced plastics (CFRF) advanced composite materials (ACM) that is representative.
Although CF has high specific tenacity and specific modulus, it belongs to hard brittle material, only has the Shi Caineng that to be combined with each other securely in it and body material to make it more effectively bearing load.Therefore, CF is mainly still used as strongthener in the composite.The performance of CF reinforced composite except depending on the character of CF itself and matrix, also with the arrangement mode of fiber in matrix, in matrix the volume fraction of fiber and recombining process relevant.Lightweight, the good moldability of all kinds of macromolecule resin, be easy to produce, with low cost, (it is that current processing technology is the most ripe that C deletes to the carbon fiber reinforced plastics be made up of high-performance CF, most popular advanced composite material.In addition, the various matrix materials such as carbon-fiber reinforced carbon, carbon fiber reinforced cement, carbon fiber reinforced metal (CFRM), carbon fibre reinforced ceramics and fibre reinforced rubber are also developed successively according to different characteristic requirements.
Although carbon fiber excellent performance, its extension at break is little, belongs to hard brittle material, cannot stop the expansion of breaking when being used alone, very easily destroyed time bending.Therefore must with the lower body material of modulus and it cohere ~ rise, even if some fibre breakage, the also intensity of unlikely impact entirety like this.Under external force, by matrix, the load of applying is assigned on fiber equably.The material made in this way is called carbon-fibre composite.
The performance suffers of carbon-fibre composite is in the cohesive strength of fiber and matrix.The Surface structure and property of fiber, as the specific surface area, surface energy etc. of the size of surface crystallites, degree of orientation, fiber, all relevant with the cohesive strength of matrix with fiber.The banded aspect of the elongate strip that the structural unit of carbon fiber is made up of hexagonal carbocyclic ring, the carbon atom being in the carbon atom at defectiveness place on the carbon atom at elongate strips edge and face, top layer complete with aspect internal structure is different.Gravitation suffered by the carbon atom of aspect inside is symmetrical, and bond energy is high, and reactive behavior is low.The carbon atom being in marginal surface is stressed asymmetric, and have unpaired electron, activity is higher.Therefore, the surfactivity of carbon fiber is relevant with the carbon atom number being in marginal position, and the carbon atom number of edge is more, and namely specific surface area is larger, and the surfactivity of carbon fiber is larger.When other condition is identical, cohesive strength between carbon fiber with matrix is relevant with pulp freeness, and the specific surface area of fiber is larger, and cohesive strength is higher, thus improving the tensile strength of carbon fibre reinforced composite, this is also carbon fiber towards one of reason of superfluorescent fiber future development.
Electrochemicial oxidation make use of the electroconductibility of carbon fiber, is generally carbon fiber is placed in electrolyte solution as anode, and the active oxygen produced by electrolysis is come carbon oxide fiber surface and introduces polar group, thus improves composite property.Carbon fiber surface oxidation states can control by changing the conditions such as temperature of reaction, electrolyte concentration, treatment time and current density.Identical with other oxide treatment, electrochemical oxidation makes fiber surface introduce various functional group thus improves the infiltration of fiber, is deposited with characteristic and the bonding conditions with matrix, significantly increases the mechanical property of carbon-fibre composite.
The ionogen that electrochemical oxidation uses has nitric acid, sulfuric acid, phosphoric acid, acetic acid, volatile salt, sodium hydroxide, saltpetre etc.Nitric acid is the process ionogen that report is maximum recently.Domestic Fang Kuanjun etc. are studied the electrochemical oxidation of carbon fiber in acid, alkali, salt three class ionogen by the method for orthogonal experiment, think in oxidising process, kind of electrolytes is the main factor of carbon fiber surface acidic functionality after impact process, next is treatment time and current density, and the impact of electrolyte concentration is least remarkable.Beijing University of Chemical Technology Zhuan Yi etc. have studied carbon fiber surface composition and the change of structure and anodized surface process to the Effect and impact of shearing resistance between carbon fiber composite layer, result shows: adopt bicarbonate of ammonia to be after bath surface process, the interlayer shear fracture transition of its matrix material is based on tension rift form, by suitably increasing the hydroxy radical content of carbon fiber surface, improve active atoms of carbon number and nonactivated carbon number ratio, effectively can improve the use properties of carbon-fibre composite, carbon fiber interlaminar shear strength is made to improve 49%, interlaminar shear strength reaches 85.5MPa.The Wang Chengzhong of Beijing University of Chemical Technology etc. carry out electrochemical oxidation surface treatment to isotropic pitch base carbon fibre, analyze the change procedure of carbon fiber surface oxygen-containing functional group and surface microscopic topographic, experimental result shows: carbon fiber is after electrochemical oxidation surface treatment, surface oxygen functional group obviously increases, first the oxide etch of carbon fiber surface occurs in surface imperfection high spot, the result of effect makes carbon fiber surface be tending towards more smooth, continues oxidation and makes carbon fiber surface occur regularly arranged groove.
Summary of the invention
The object of the invention is to propose a kind of carbon fiber surface method for metallising.
For reaching this object, the present invention by the following technical solutions:
A kind of carbon fiber surface method for metallising, carbon fiber is after activation is removed photoresist in pre-treatment in early stage, adopt chemical process in carbon fiber surface twice nickel plating, form carbon fiber surface protection coating materials, comprising: carbon fiber is washed------washing---carbon fiber alligatoring---pickling neutralization---carbon fiber dispersion treatment---a chemical nickel plating---secondary chemical nickel plating---carbon fiber washing---hot blast drying---quality test that carbon fiber heating removes photoresist.Carbon fiber washing adopts deionized water, temperature 30---and 40 degree, washing time 10---20min, carbon fiber heating removes photoresist, and temperature 200---250 degree, alligatoring adopts the salpeter solution of 35%, soaks 25min.Carbon fiber chemical plating technology parameter comprises 300---400g/L single nickel salt, 20---30ml/LHF solution, nickelous chloride 30---50g/L, 10---15ml/L sodium hypophosphite, PH3.0---4.0, temperature is 40---50 degree, first time plating time be 2---3min, second time plating time 3---4min.
Embodiment
Embodiment 1
A kind of carbon fiber surface method for metallising, carbon fiber is after activation is removed photoresist in pre-treatment in early stage, adopt chemical process in carbon fiber surface twice nickel plating, form carbon fiber surface protection coating materials, comprising: carbon fiber is washed------washing---carbon fiber alligatoring---pickling neutralization---carbon fiber dispersion treatment---a chemical nickel plating---secondary chemical nickel plating---carbon fiber washing---hot blast drying---quality test that carbon fiber heating removes photoresist.Carbon fiber washing adopts deionized water, temperature 30 degree, washing time 10min, and carbon fiber heating removes photoresist temperature 200 degree, and alligatoring adopts the salpeter solution of 35%, soaks 25min.Carbon fiber chemical plating technology parameter comprises 300g/L single nickel salt, 20ml/LHF solution, nickelous chloride 30g/L, 10ml/L sodium hypophosphite, PH3.0, and temperature is 40 degree, and plating time is 2min for the first time, second time plating time 4min.
Embodiment 2
A kind of carbon fiber surface method for metallising, carbon fiber is after activation is removed photoresist in pre-treatment in early stage, adopt chemical process in carbon fiber surface twice nickel plating, form carbon fiber surface protection coating materials, comprising: carbon fiber alligatoring---pickling neutralization---carbon fiber dispersion treatment---a chemical nickel plating---secondary chemical nickel plating---carbon fiber washing---hot blast drying---quality test.Carbon fiber adopts without starching carbon fiber, does not need process of removing photoresist, Simplified flowsheet, and carbon fiber washing adopts deionized water, temperature 30 degree, washing time 10min, and alligatoring adopts the salpeter solution of 35%, soaks 30min.Carbon fiber chemical plating technology parameter comprises 400g/L single nickel salt, 15ml/L lactic acid solution, nickelous chloride 35g/L, 20ml/L sodium hypophosphite, PH4.0, and temperature is 40 degree, and plating time is 3min for the first time, second time plating time 3min.
Claims (3)
1. a carbon fiber surface method for metallising, it is characterized in that carbon fiber is after activation is removed photoresist in pre-treatment in early stage, adopt chemical process in carbon fiber surface twice nickel plating, form carbon fiber surface protection coating materials, comprising: carbon fiber is washed------washing---carbon fiber alligatoring---pickling neutralization---carbon fiber dispersion treatment---a chemical nickel plating---secondary chemical nickel plating---carbon fiber washing---hot blast drying---quality test that carbon fiber heating removes photoresist.
2. method according to claim 1, is characterized in that, described carbon fiber washing adopts deionized water, temperature 30---40 degree, washing time 10---20min, carbon fiber heating removes photoresist temperature 200---and 250 degree, alligatoring adopts the salpeter solution of 35%, soaks 25min.
3. method according to claim 1, it is characterized in that, described carbon fiber chemical plating technology parameter comprises 300---400g/L single nickel salt, 20---30ml/LHF solution, nickelous chloride 30---50g/L, 10---15ml/L sodium hypophosphite, PH3.0---4.0, temperature is 40---50 degree, first time plating time be 2---3min, second time plating time 3---4min.
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| CN201510715560.XA CN105200401A (en) | 2015-10-29 | 2015-10-29 | Carbon fiber surface metallization method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106906646A (en) * | 2017-03-02 | 2017-06-30 | 昆明理工大学 | A kind of carbon fiber surface metallization treating method |
| CN107090640A (en) * | 2017-05-11 | 2017-08-25 | 广州市爱因电子有限公司 | The underwear that a kind of use conductive yarn makes |
| RU2698809C1 (en) * | 2018-05-31 | 2019-08-30 | Общество с ограниченной ответственностью "Межотраслевой инжиниринговый центр МГТУ им. Н.Э. Баумана" (ООО "МИЦ МГТУ им. Н.Э. Баумана") | Method of producing composite material based on carbon fibers |
| CN110205611A (en) * | 2019-06-25 | 2019-09-06 | 北京理工大学 | A kind of method of quartz fibre chemical nickel phosphorus plating |
| CN114775274A (en) * | 2022-04-25 | 2022-07-22 | 中国科学院宁波材料技术与工程研究所 | Method and device for continuously metallizing surface of carbon fiber |
Citations (4)
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| US4522889A (en) * | 1983-01-20 | 1985-06-11 | Bayer Aktiengesellschaft | Lightning protection composite material |
| CN102086517A (en) * | 2009-12-08 | 2011-06-08 | 沈阳临德陶瓷研发有限公司 | Chemical nickel-plating method for carbon fiber |
| CN103160826A (en) * | 2013-03-22 | 2013-06-19 | 西北工业大学 | Preparation method of continuous carbon fiber surface pyrolytic carbon/nickel composite coating |
| CN103668134A (en) * | 2013-09-18 | 2014-03-26 | 沈阳工业大学 | Diacid complexing agent method for chemically plating nickel on carbon fiber surface |
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Patent Citations (4)
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| US4522889A (en) * | 1983-01-20 | 1985-06-11 | Bayer Aktiengesellschaft | Lightning protection composite material |
| CN102086517A (en) * | 2009-12-08 | 2011-06-08 | 沈阳临德陶瓷研发有限公司 | Chemical nickel-plating method for carbon fiber |
| CN103160826A (en) * | 2013-03-22 | 2013-06-19 | 西北工业大学 | Preparation method of continuous carbon fiber surface pyrolytic carbon/nickel composite coating |
| CN103668134A (en) * | 2013-09-18 | 2014-03-26 | 沈阳工业大学 | Diacid complexing agent method for chemically plating nickel on carbon fiber surface |
Non-Patent Citations (1)
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| 万里鹰等: ""碳纤维表面连续电镀镍的研究"", 《南昌航空大学学报: 自然科学版》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106906646A (en) * | 2017-03-02 | 2017-06-30 | 昆明理工大学 | A kind of carbon fiber surface metallization treating method |
| CN107090640A (en) * | 2017-05-11 | 2017-08-25 | 广州市爱因电子有限公司 | The underwear that a kind of use conductive yarn makes |
| RU2698809C1 (en) * | 2018-05-31 | 2019-08-30 | Общество с ограниченной ответственностью "Межотраслевой инжиниринговый центр МГТУ им. Н.Э. Баумана" (ООО "МИЦ МГТУ им. Н.Э. Баумана") | Method of producing composite material based on carbon fibers |
| CN110205611A (en) * | 2019-06-25 | 2019-09-06 | 北京理工大学 | A kind of method of quartz fibre chemical nickel phosphorus plating |
| CN114775274A (en) * | 2022-04-25 | 2022-07-22 | 中国科学院宁波材料技术与工程研究所 | Method and device for continuously metallizing surface of carbon fiber |
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Application publication date: 20151230 |