KR20140015006A - Method for processing conductive of carbon fiber - Google Patents

Method for processing conductive of carbon fiber Download PDF

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Publication number
KR20140015006A
KR20140015006A KR1020120082593A KR20120082593A KR20140015006A KR 20140015006 A KR20140015006 A KR 20140015006A KR 1020120082593 A KR1020120082593 A KR 1020120082593A KR 20120082593 A KR20120082593 A KR 20120082593A KR 20140015006 A KR20140015006 A KR 20140015006A
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KR
South Korea
Prior art keywords
carbon fiber
electroless plating
minutes
swelling
carried out
Prior art date
Application number
KR1020120082593A
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Korean (ko)
Inventor
이종길
허수형
강병록
박민영
류수민
김영규
김진구
Original Assignee
주식회사 불스원신소재
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Priority to KR1020120082593A priority Critical patent/KR20140015006A/en
Publication of KR20140015006A publication Critical patent/KR20140015006A/en

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/165Ethers
    • D06M13/175Unsaturated ethers, e.g. vinylethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M14/00Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/36Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to carbon fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40Fibres of carbon
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2209/00Properties of the materials
    • D06N2209/04Properties of the materials having electrical or magnetic properties
    • D06N2209/048Electromagnetic interference shielding
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00Inorganic fibres
    • D10B2101/10Inorganic fibres based on non-oxides other than metals
    • D10B2101/12Carbon; Pitch
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/16Physical properties antistatic; conductive

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemically Coating (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The present invention relates to a method for conductivity processing of a carbon fiber, capable of improving adhesiveness by minimizing damage to a carbon fiber and capable of obtaining a conductive carbon fiber having a bright tone of color by conducting electroless plating with a bright tone of color. The method for conductivity processing of a carbon fiber according to the present invention comprises the steps of: degreasing epoxy or urethane sized on the carbon fiber using a surfactant; swelling and softening the surface of the carbon fiber using an organic solvent; neutralizing, washing and conditioning the softened carbon fiber using sulfuric acid (H2SO4) and ammonium persulfate; and conducting the electroless plating of the carbon fiber.

Description

Method for processing conductive of carbon fiber

The present invention relates to a conductive treatment of carbon fiber, and more particularly, to maintain the original shape of the carbon fiber, and to eliminate the causes of plating drop and adhesion deterioration, to obtain a conductive fiber by plating electroless Ni of light tones It relates to a conductive treatment method of carbon fiber.

In general, carbon fiber-reinforced composites, which began to develop rapidly with the development of the aerospace and aerospace industries, are now widely used in aerospace and aerospace industries, as well as electrical and electronic materials, civil and building materials, automobiles, ships, military equipment, and sporting goods. It is one of the high-tech materials used in the field.

Carbon fiber as a reinforcing material is divided by the final heat treatment temperature. In general, as the heat treatment temperature increases, the interfacial bond strength tends to decrease. As the heat treatment temperature increases, the crystal structure becomes perfect and the surface energy decreases. Because.

In addition, high-strength carbon fibers carbonized by heating to a temperature of 1000 to 1500 ° C. generally have basic functional groups such as chromene and pyrone, or carbon atom bodies are known to have Lewis basicity. .

Thus, the interfacial bonding strength of carbon fibers can be improved by increasing the surface area of the fibers to provide more contact points or by increasing the physicochemical interaction between the fibers and the resin.

In particular, the highly conductive carbon fiber has excellent properties such as heat resistance, chemical stability, electrical conductivity, and electromagnetic shielding flexibility, and thus can be used as an internal filler of plastic having high conductivity.

Electroless plating is most commonly used as a method of manufacturing such highly conductive carbon fibers. In the case of electroless plating, not only has an excellent shielding effect but also has the advantage of forming a plating layer having a predetermined thickness on the surface of the fiber.

However, the conventional electroless plating method (Korean Patent No. 486,962) is a metal plating solution in which a metal salt, a reducing agent and a complexing agent coexist, and the carbon fiber is nickel-plated on the surface of the carbon fiber by nickel plating of carbon fiber by chemical reduction. Was introduced to form a film of a constant thickness, thereby improving the conductivity of the carbon fiber, but as the phosphorus (P) content in the alloy increased, the specific resistance increased, resulting in a decrease in the conductivity of the carbon fiber. .

In particular, the pretreatment methods are mostly simple, making it difficult to secure the adhesion of carbon fibers, and patents for nickel reducing agents are the mainstay.

Most of them are immersed for 30 minutes using 0.1M HN0 3 or more than 10 minutes using alkaline (NaOH 13-17g).

This has a problem in that the strength of the fiber is weakened by the strong acid strong alkali, and the metal and the fiber is not closely adhered because the adhesion between the metal and the fiber depends on the physical method due to the unevenness.

In addition, there is a problem in time allocation with the next process in the continuous plating process, and the disadvantage is that the tank size is increased, which is disadvantageous in terms of wastewater treatment and cost.

Accordingly, the present invention is to solve all the disadvantages and problems of the prior art as described above, the present invention is to maintain the original shape of the carbon fiber while eliminating the cause of the plating dropout and adhesion is reduced by electroless plating It is an object of the present invention to provide a conductive method for treating carbon fibers from which conductive fibers can be obtained.

The conductive treatment method of the carbon fiber of the present invention for achieving the above object comprises the steps of: degreasing epoxy or urethane sized on the carbon fiber using a surfactant; Swelling and softening the surface of the carbon fiber using an organic solvent; Neutralizing, cleaning, and conditioning the softened carbon fiber by using sulfuric acid (H 2 SO 4 ) and ammonium persulfate ((NH 4 ) 2 S 2 O 8 ); And electroless plating the carbon fibers.

Here, it is preferable to use 47% pure water and 3% NaOH as surfactant.

The organic solvent was 65% diethyl propanediol, 10% dipropylene glycol methyl ether, and 500 ppm non-ionic surfactant (Low Foam). Swelling is preferred.

In addition, the step of coarsening is sodium bisulfite (SODIUM BISULFITE (NaHSO 3 ) 1%, sulfuric acid (H 2 SO 4 ) 0.5%, ammonium persulfate (Amm.persulfate ((NH 4 ) 2 S 2 O 8 )) 15 It is preferable to neutralize alkali, perform cleaning, and condition by using% and 83.5% pure water.

And it is preferable to adsorb Pd-Sn on carbon fiber after a temper action.

Meanwhile, it is preferable to add a sensitizing process and an activation process between the tempering step and the electroless plating step.

Here, swelling is preferably carried out at 50 to 60 ℃ for 1 to 2 minutes.

In addition, the crude is preferably performed for 1 to 2 minutes at 20 to 40 ℃.

In addition, the electroless plating is preferably carried out at 30 to 40 ℃ 10 minutes to 20 minutes.

On the other hand, it is preferable that electroless plating is either nickel or copper plating.

The present invention has the following effects.

First, it is possible to produce conductive carbon fibers close to the original color of Ni.

Second, it contributes to the activation of conductive carbon fiber, which has a gentle working environment and minimizes damage to the fiber, thereby providing excellent adhesion, and thus has a wide range of applications for lightening electric and electronic products and electromagnetic shielding materials.

Third, as a method for lowering the electrical resistance, an excellent effect can be obtained through electroless Cu plating.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

In addition, although the term used in the present invention is selected as a general term that is widely used at present, there are some terms selected arbitrarily by the applicant in a specific case. In this case, since the meaning is described in detail in the description of the relevant invention, It is to be understood that the present invention should be grasped as a meaning of a term that is not a name of the present invention. Further, in describing the embodiments, descriptions of technical contents which are well known in the technical field to which the present invention belongs and which are not directly related to the present invention will be omitted. This is for the sake of clarity of the present invention without omitting the unnecessary explanation.

First, surfactants are used to remove epoxy or urethane sized on the carbon fibers, and at the same time, the surface of the carbon fibers is swelled and softened using an organic solvent.

For example, the surfactant is 25% of the composition using pure water 47% and 3% NaOH, the organic solvent is 65% Diethyl Propanediol, 10% Dipropylene Glycol Methyl Ether. Non-ionic surfactants (Non-Ionic Surfactant (Low Foam)) is used to swell using 500ppm.

This is similar to the method of pretreatment of polycarbonate material. When the material that is not etched is immersed for 1 to 2 minutes at 50 to 60 ° C using an organic solvent (isopropyl alcohol) or the like, it swells on the surface of the polycarbonate material. (Swelling) action will occur.

By treating this in one process, the process of time and washing can be simplified.

Next, neutralize the strong alkali component of NaOH using H 2 SO 4 to reduce the burden on the next process, sensitizing, and utilize ammonium persulfate ((NH 4 ) 2 S 2 O 8 ). To help cleansing and conditioning to strengthen adsorption of palladium.

Specifically, sodium bisulfite (SODIUM BISULFITE (NaHSO 3 ) 1%, sulfuric acid (H 2 SO 4 ) 0.5%, ammonium persulfate (Amm.persulfate ((NH 4 ) 2 S 2 O 8 )) 15% and pure 83.5 Neutralizes alkali by using%, performs cleaning, and plays a pivotal role in securing adhesion, which is a disadvantage of conductive organic fibers by performing conditioning, in which treatment is performed at 20 to 40 ° C. for about 1 to 2 minutes. do.

This crude action serves to reduce the cation bearing carbon fibers to anions to facilitate the adsorption of Pd-Sn.

Then, a typical sensitizing process is performed for 1 to 2 minutes at 25 to 30 ° C., and a typical activating process is performed at 50 to 60 ° C. for 1 to 2 minutes.

Finally, electroless nickel (Ni) or copper is plated at 30 to 40 ° C. At this time, 10 minutes to 20 minutes.

Therefore, in case of nickel plating, electroless plating of light tone is possible, and in the case of copper plating, electrical resistance can be lowered.

While the present invention has been described with reference to the exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Therefore, the examples disclosed in the present invention are not intended to limit the scope of the present invention and are not intended to limit the scope of the present invention. The scope of protection of the present invention should be construed according to the following claims, and all technical ideas within the scope of equivalents should be construed as falling within the scope of the present invention.

Claims (10)

In the method of processing conductivity to carbon fiber,
Degreasing epoxy or urethane sized on the carbon fiber using a surfactant;
Swelling and softening the surface of the carbon fiber using an organic solvent;
Neutralizing, washing and conditioning using sulfuric acid (H 2 SO 4 ) and ammonium persulfate ((NH 4 ) 2 S 2 O 8 ) on the softened carbon fiber; And
Electroless plating of the carbon fibers; conductive treatment method of the carbon fibers comprising a.
The method of claim 1,
47% of pure water and 3% of NaOH are used as the surfactant.
The method of claim 1,
The organic solvent is diethyl propanediol (65%), dipropylene glycol methyl ether (Dipropylene Glycol Methyl Ether) 10%, non-ionic surfactant (Non-Ionic Surfactant (Low Foam)) using 500ppm Swelling is carried out, The electroconductive processing method of carbon fiber characterized by the above-mentioned.
The method of claim 1,
The step of refining is
1% sodium bisulfite (NaHSO 3 ), 0.5% sulfuric acid (H 2 SO 4 ), 15% ammonium persulfate (Amm.persulfate ((NH 4 ) 2 S 2 O 8 )) and 83.5% pure water To neutralize alkali, perform a cleaning action, and perform a conditioning action.
5. The method of claim 4,
Pd-Sn is adsorb | sucked to the carbon fiber after the said temper action, The electroconductive process of carbon fiber characterized by the above-mentioned.
The method of claim 1,
And a sensitizing process and an activation process are added between the tempering step and the electroless plating step.
The method of claim 1,
The swelling is carried out at 50 to 60 ℃ 1 to 2 minutes, characterized in that the conductive treatment method of carbon fiber.
The method of claim 1,
The tempering is carried out at 20 to 40 ℃ 1 to 2 minutes, characterized in that the conductive treatment method of carbon fiber.
The method of claim 1,
The electroless plating is nickel or copper plating.
10. The method of claim 9,
The electroless plating is carried out at 30 to 40 ℃ 10 minutes to 20 minutes characterized in that the conductive treatment method of carbon fiber.
KR1020120082593A 2012-07-27 2012-07-27 Method for processing conductive of carbon fiber KR20140015006A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016010287A1 (en) * 2014-07-17 2016-01-21 (주)크린앤사이언스 Method for plating nonwoven fabric by using continuous electroless and electrolytic plating processes
KR101645944B1 (en) 2016-03-09 2016-08-05 (주)다인스 Metal coated carbon fiber bundle manufacturing process for braid

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016010287A1 (en) * 2014-07-17 2016-01-21 (주)크린앤사이언스 Method for plating nonwoven fabric by using continuous electroless and electrolytic plating processes
US20170204519A1 (en) * 2014-07-17 2017-07-20 Clean & Science Co., Ltd. Method for plating nonwoven fabric by using continuous electroless and electrolytic plating processes
JP2017526816A (en) * 2014-07-17 2017-09-14 クリーン アンド サイエンス カンパニー リミテッド Method for plating non-woven fabric using continuous process of electroless and electrolytic plating
JP2020007639A (en) * 2014-07-17 2020-01-16 クリーン アンド サイエンス カンパニー リミテッド Plating method for nonwoven fabric using continuous process of electroless plating and electrolytic plating
KR101645944B1 (en) 2016-03-09 2016-08-05 (주)다인스 Metal coated carbon fiber bundle manufacturing process for braid

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