CN101886330B - Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof - Google Patents
Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof Download PDFInfo
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- CN101886330B CN101886330B CN2010101960221A CN201010196022A CN101886330B CN 101886330 B CN101886330 B CN 101886330B CN 2010101960221 A CN2010101960221 A CN 2010101960221A CN 201010196022 A CN201010196022 A CN 201010196022A CN 101886330 B CN101886330 B CN 101886330B
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Abstract
The invention relates to an Fe-Co magnetic alloy plated carbon fiber, a preparation method and application thereof. In the invention, a high-purity metal sheet is used as an anode, continuous carbon fibers oxidized at high temperature by strong acid are used as a cathode, and sulphates of iron and cobalt are used as main salts. In the preparation method, electroplating is carried out under the conditions of constant temperature and electromagnetic stirring, wherein the thickness of the plated layer is controlled through plating temperature and time. The magnetic carbon fiber has uniform and dense magnetic plated layer, the thickness of the plated layer is about 0.5-1.5 mum, and the ingredient of the magnetic plated layer is Co3Fe7. The magnetic carbon fiber has simple preparation process, high production efficiency and excellent magnetic property and is expected to be used as a novel wave-absorbing material having the advantages of high mechanical property and low density.
Description
Technical field
The invention belongs to the electromagnetic wave absorbent material field, particularly a kind of Fe-Co magnetic alloy plated carbon fiber.
Background technology
Inhale wave technology and comprise that coating is inhaled ripple and structure is inhaled ripple.Coating is inhaled ripple and is meant that the coating that has the suction wave energy in surface-coated is to reach the purpose of inhaling ripple; Structure is inhaled ripple and is then given the dual-use function that material is stealthy and carry, and can replace surperficial covering, weight reduction, simplification technology, also keeps the good conformity ability to environment simultaneously easily.It is low that carbon fiber has density, and intensity and modulus are high, no creep, and fatigue durability is good, and specific heat and electric conductivity are between nonmetal and metal, and thermal coefficient of expansion is little, and premium properties such as good corrosion resistance can be used as desirable structural wave-absorbing material.Wave-absorbing mechanism from material; Require material to have high electrical loss and magnetic loss, carbon fiber itself does not have magnetic, therefore passes through coating surface; Promptly obtaining one deck magnetic coating on its surface, is to make the carbon fiber base wave-absorbing material possess a kind of effective way of magnetic loss performance.The Fe-Co alloy as soft magnetic materials have a series of excellent magnetism can, as high saturation and magnetic intensity, high initial permeability and maximum permeability, magnetic hysteresis flexible little, Curie temperature is high.Nanometer iron cobalt powder body has obtained the broad research of researcher as a kind of bandwidth, high decay, resistant to elevated temperatures absorbing material.Therefore, through at carbon fiber surface plating one deck Fe-Co magnetic alloy, be expected to obtain new and effective absorbing material.
The metallization of carbon current fiber surface roughly is divided into physical method and chemical method two big classes: (1) physical method comprises sputtering method, ion plating method, metal powder painting and metal coat etc.(2) chemical method is mainly chemical plating or plating.Galvanoplastic have characteristics such as equipment is simple, cost is low, can produce continuously, are a kind of methods that the applications well prospect is arranged.The research of single metals such as existing a large amount of carbon fiber surface electroplated Ni, Cu, Fe in the document, plating Ni carbon fiber has obtained practical application in the electromagnetic shielding field.Alloy layer compares to the single coat of metal and has more excellent physics, chemistry and mechanics mechanical performances; Thereby obtain broad research and application; It is less that but relevant carbon fiber surface is electroplated the research of function alloy coating; So carbon fiber surface electroplates that Fe-Co is magnetic alloy plated to have important research and an actual application value.
Summary of the invention
The object of the present invention is to provide the Fe-Co magnetic alloy plated carbon fiber.It is the preparation method who deposits the Fe-Co alloy magnetic coating of even compact through galvanoplastic at carbon fiber surface.The present invention utilizes Fe and Co to have the characteristics of close standard electrode potential, on electroplanting device commonly used, carries out the plating of alloy.Technology is simple, and production efficiency is high, is fit to large-scale industrial production.
Fe-Co magnetic alloy plated carbon fiber provided by the invention is magnetic alloy plated at continuous carbon fibre surface electrical deposition Fe-Co, and the coating alloying component is Co
3Fe
7, thickness of coating is 0.5-1.5 μ m.
Continuous carbon fibre is polyacrylonitrile-radical continuous carbon fibre, pitch or gluing basic continuous carbon fibre, more than carbon fibre tow comprises that 1K, 3K, 6K, 12K, 24K reach.
The preparation method of a kind of Fe-Co magnetic alloy plated carbon fiber provided by the invention comprises the steps:
1),, volume fraction soaks 1～2h in being 50% salpeter solution then with continuous carbon fibre 450～500 ℃ of following insulation oxidation 15～20min in Muffle furnace.Purpose is with strong acid carbon fiber surface to be carried out further oxidation.
2) configuration plating bath; Two kinds of salinity of iron and cobalt are 90～100g/L (sulfate), and boric acid concentration is 30～40g/L, and sodium hexadecyl sulfate concentration is that (boric acid is as complexing agent for 0.1g/L; Lauryl sodium sulfate is as dispersant), the pH value is adjusted to 3～4 with dilution heat of sulfuric acid.
3) be that 99.99% metallic plate is an anode with purity, carbon fiber feeds DC current as negative electrode, and electric current 0.5～1A stirs electroplating time 5～10min down at 20-60 ℃.Thickness of coating is controlled through plating time.
4) will electroplate the carbon fiber of accomplishing and use the deionized water rinsing several times, room temperature is placed air dry.
Used anode is pure iron plate, cobalt plate or ferrocobalt plate.
The application of Fe-Co magnetic alloy plated carbon fiber provided by the invention, this material is used for the structural wave-absorbing material field.
Fe-Co magnetic alloy plated carbon fiber provided by the invention is magnetic alloy plated at the Fe-Co that carbon fiber surface obtains even compact through galvanoplastic, makes carbon fiber on the basis that keeps its original performance, has good magnetic.Compare with other magnetic absorbing materials and to have the following advantages:
1. to obtain the technology of magnetic absorbing material simple in the present invention, and production efficiency is high, is fit to large-scale industrial production.
2. carbon fiber original excellent performance is damaged, and the carbon fiber flexibility with magnetic coating is good, can be used as structural wave-absorbing material, and magnetic nano-particle traditionally can only be as the coating absorbing material.
3. this magnetic texure absorbing material density is low, intensity is high, have excellent magnetic characteristics, and is expected to satisfy the absorbing property requirement of aspects such as " thin, light, wide, strong ".
Description of drawings
Fig. 1 is the SEM photo of plating Fe-Co alloy magnetic carbon fiber, and a, b are instance 1, and c, d are instance 2.
Fig. 2 is the X-ray diffractogram of instance 1,2 magnetic carbon fibers.
Fig. 3 is the hysteresis curve under instance 1, the 2 magnetic carbon fiber normal temperature.
Embodiment 1,
With continuous carbon fibre 500 ℃ of following insulation 15min in Muffle furnace,, the 40ml volume fraction soaks the 1h oxidation processes in being 50% salpeter solution then.The configuration plating bath, two kinds of main salt concentrations are 90g/L, and boric acid concentration is 30g/L, and sodium hexadecyl sulfate concentration is 0.1g/L, and pH value use mass fraction is that 10% dilution heat of sulfuric acid is adjusted to 3～4.Plating is that high-purity iron plate of 99.99% is an anode with purity, and the carbon fiber after the oxidation processes is as negative electrode, electric current 0.5A, electromagnetic agitation under the room temperature, electroplating time 5min.Product washes with deionized water repeatedly, air dry 48h under the room temperature.
Embodiment 2,
With continuous carbon fibre 500 ℃ of following insulation 15min in Muffle furnace,, the 40ml volume fraction soaks 1h in being 50% salpeter solution then.The configuration plating bath, two kinds of main salt concentrations are 90g/L, and boric acid concentration is 30g/L, and sodium hexadecyl sulfate concentration is 0.1g/L, and pH value use mass fraction is that 10% dilution heat of sulfuric acid is adjusted to 3～4.Plating is that high-purity iron plate of 99.99% is an anode with purity, and the carbon fiber after the oxidation processes is as negative electrode, electric current 0.5A, 50 ℃ of electromagnetic agitation, electroplating time 5min.Product washes with deionized water repeatedly, air dry 48h under the room temperature.
Product carries out SEM, XRD and magnetism testing.
Test result: Fig. 1 is a SEM pattern photo, and figure a, b are instance 1, and c, d are instance 2, can find out that coating is even, densification, and thickness of coating is about 0.5 and 1.0 μ m respectively.XRD result shows among Fig. 2, and the coating alloy is Co
3Fe
7, do not have other impurity phase.Hysteresis curve shows that coating is typical ferromagnetism under Fig. 3 normal temperature, and it is 31.53 and 49.65emu/g that saturation magnetization Ms is respectively room temperature and 50 ℃, shows that product has good magnetic property.
Claims (5)
1. the preparation method of a Fe-Co magnetic alloy plated carbon fiber, it is magnetic alloy plated at continuous carbon fibre surface electrical deposition Fe-Co, it is characterized in that it comprises the steps:
1),, volume fraction soaks 1～2h in being 50% salpeter solution then with continuous carbon fibre 450～500 ℃ of following insulation oxidation 15～20min in Muffle furnace;
2) configuration plating bath, two kinds of salinity of iron and cobalt are 90～100g/L, and boric acid concentration is 30～40g/L, and sodium hexadecyl sulfate concentration is 0.1g/L, and the pH value is adjusted to 3～4 with dilution heat of sulfuric acid;
3) be that 99.99% metallic plate is an anode with purity, carbon fiber feeds DC current as negative electrode, and electric current 0.5～1A stirs electroplating time 5～10min down at 20-60 ℃;
4) will electroplate the carbon fiber of accomplishing and use deionized water rinsing, room temperature is placed air dry.
2. according to the described preparation method of claim 1, it is characterized in that described coating alloying component is Co
3Fe
7, thickness of coating is 0.5-1.5 μ m.
3. according to the described preparation method of claim 1, it is characterized in that described continuous carbon fibre is polyacrylonitrile-radical continuous carbon fibre, pitch or gluing basic continuous carbon fibre.
4. according to the described preparation method of claim 1, it is characterized in that described anode is pure iron plate, cobalt plate or ferrocobalt plate.
5. according to the described preparation method of claim 1, it is characterized in that described carbon fibre tow comprise 1K, 3K, 6K, 12K, 24K and more than.
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| CN101886330A CN101886330A (en) | 2010-11-17 |
| CN101886330B true CN101886330B (en) | 2012-07-11 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102154816B (en) * | 2011-01-20 | 2012-08-22 | 天津市飞荣达科技有限公司 | FeCo alloy/CuO double-plating magnetic carbon fiber and preparation method and application |
| CN102220689A (en) * | 2011-04-13 | 2011-10-19 | 天津大学 | Device and method for continuously electrodepositing transition metal on surfaces of large-tow carbon fibers of 48K or more |
| CN102628214A (en) * | 2012-04-09 | 2012-08-08 | 天津大学 | Carbon fiber composite material with ZnO layer electrolytically deposited on surface as well as preparation method and application thereof |
| CN102912323B (en) * | 2012-11-20 | 2014-05-07 | 哈尔滨理工大学 | Preparation method of carbon fiber surface nano CoFeB microwave-absorbing coating |
| CN103806042B (en) * | 2014-01-20 | 2016-04-20 | 天津大学 | The preparation method of carbon fiber electroplating iron-nickel alloy |
| CN105908493A (en) * | 2016-04-19 | 2016-08-31 | 郑州四维特种材料有限责任公司 | Metal modified carbon fiber, preparation method and application thereof |
| CN105838324A (en) * | 2016-04-25 | 2016-08-10 | 中国科学院西安光学精密机械研究所 | Preparation method of iron and iron carbide loaded porous carbon sphere composite wave-absorbing material |
| CN105820796A (en) * | 2016-04-25 | 2016-08-03 | 中国科学院西安光学精密机械研究所 | Preparation method of magnetic alloy loaded porous carbon sphere composite wave-absorbing material |
| CN105896099A (en) * | 2016-04-25 | 2016-08-24 | 中国科学院西安光学精密机械研究所 | Preparation method of porous carbon sphere composite wave-absorbing material loaded with magnetic metal simple substance |
| CN114775274B (en) * | 2022-04-25 | 2024-05-31 | 中国科学院宁波材料技术与工程研究所 | Method and device for continuously surface metallizing carbon fiber |
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| CN101591855A (en) * | 2009-06-22 | 2009-12-02 | 万嫣蕊 | The process of electrodepositing transition metal on surfaces of large-tow carbon fibers |
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| JPS5870769A (en) * | 1981-10-22 | 1983-04-27 | 住友電気工業株式会社 | Coated carbon fiber |
| JPH0284540A (en) * | 1988-06-09 | 1990-03-26 | Mitsubishi Rayon Co Ltd | Carbon fiber coated with amorphous alloy |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1741304A (en) * | 2005-07-12 | 2006-03-01 | 北京航空航天大学 | Metal oxide electrode material for producing adulterant utilizing electro-deposition-heat treatment technology |
| CN1844481A (en) * | 2006-03-09 | 2006-10-11 | 上海交通大学 | Metallization treatment method for short carbon fiber |
| CN101591855A (en) * | 2009-06-22 | 2009-12-02 | 万嫣蕊 | The process of electrodepositing transition metal on surfaces of large-tow carbon fibers |
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| Title |
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| 庞永强等.Fe－Co合金和中空碳纤维吸波材料的吸波特性研究.《材料导报：研究篇》.2009,第23卷(第11期),第5－8、14页. * |
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