CN113502662A - Surface treatment method of asphalt-based graphite carbon fiber - Google Patents

Surface treatment method of asphalt-based graphite carbon fiber Download PDF

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CN113502662A
CN113502662A CN202110906559.0A CN202110906559A CN113502662A CN 113502662 A CN113502662 A CN 113502662A CN 202110906559 A CN202110906559 A CN 202110906559A CN 113502662 A CN113502662 A CN 113502662A
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carbon fiber
asphalt
based graphite
graphite carbon
aqueous solution
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姜海涛
李文泉
周玉柱
田晓峰
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Shaanxi Tiance New Material Technology Co ltd
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    • 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08Organic compounds
    • D06M10/10Macromolecular compounds
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    • 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

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Abstract

The invention relates to a surface treatment method of asphalt-based graphite carbon fibers, which comprises the following steps: before the pitch-based graphitized carbon fiber is subjected to anodic oxidation etching, the surface of the carbon fiber filament is subjected to surface infiltration modification by a polydopamine aqueous solution, an active amino surface layer is formed on the surface of the pitch-based graphitized carbon fiber, and then the pitch-based graphitized carbon fiber enters an electrolytic bath for anodic oxidation treatment. The invention has the advantages that: the oxidation degree of anodic oxidation etching is greatly improved; the types of surface functional groups of the asphalt-based graphite fibers are enriched, so that the asphalt-based graphite fibers are more tightly combined with resin, and higher interlaminar shear strength is endowed to the asphalt-based graphite fibers; and thirdly, the oxygen content increasing effect is obvious, and the surface activity is enhanced. The surface treatment method for introducing the active amino is simple, efficient, easy to operate, free of environmental pollution and convenient for industrial application.

Description

Surface treatment method of asphalt-based graphite carbon fiber
Technical Field
The invention belongs to the technical field of high polymer carbon fiber materials, and relates to a method for treating the surface of asphalt-based graphite carbon fiber.
Background
The carbon fiber is a high-performance fiber with high specific modulus, excellent ablation resistance, high specific strength, excellent fatigue resistance, low thermal expansion coefficient and strong corrosion resistance. The composite material has many advantages and is widely applied to the fields of aerospace, sports equipment, wind power manufacturing industry, automobile manufacturing industry and the like as a reinforcement of an advanced composite material. Compared with polyacrylonitrile carbon fiber, the mesophase pitch-based carbon fiber has higher modulus and higher thermal conductivity, and gives a unique application scene.
The carbon fiber is mainly used as a reinforcement of the composite material, and the interfacial adhesion performance of the composite material is directly influenced by the surface activity of the carbon fiber. After the carbon fiber is subjected to carbonization or graphitization heat treatment, particularly after the asphalt-based carbon fiber is subjected to graphitization treatment, the surface is smooth and compact, the active points are few (the carbon content is more than 98%), and a certain amount of active functional groups need to be introduced to the surface of the graphite fiber through a surface treatment process, so that the bonding strength with a resin matrix is improved conveniently.
The surface treatment method basically used in the carbon fiber industry is an electrochemical anodic oxidation method, and the oxidation reaction is mild, easy to control and remarkable in treatment effect. At present, the anodic oxidation treatment mainly aims at the treatment method of polyacrylonitrile carbon fiber (not graphitized), the carbon content on the surface of the polyacrylonitrile carbon fiber is 90-95%, because the surface has certain activity and the effect of combining with anodic oxidation treatment is obvious, but because of the strong inertia of the surface of the asphalt-based graphitized carbon fiber, the carbon content is more than 99 percent, the surface activation points are less, when the dry tows enter the electrolytic bath, the dry tows cannot be quickly and uniformly wetted by the electrolyte, and the surfaces of the asphalt-based graphite carbon fibers have extremely strong inertia, so that the electrochemical oxidation treatment is not ideal, after single anodic oxidation etching treatment, the introduction amount of functional groups on the surface is still small, so that the interface bonding performance is poor when the carbon fiber is compounded with the resin matrix, therefore, the activity of the carbon fiber surface treatment is improved, and the method has important significance for improving the performance of the asphalt-based graphite carbon fiber.
Disclosure of Invention
The invention aims to solve the problem of insufficient surface activity during the anodic oxidation of the pitch-based graphitized carbon fiber in the prior art, and provides a surface treatment method of the carbon fiber, which improves the activity of the anodic oxidation etching of the surface of the pitch-based graphitized carbon fiber and greatly improves the number of functional groups.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a surface treatment method of asphalt-based graphite carbon fiber comprises the following steps:
the first step is as follows: preparation of aqueous Polydopamine solutions
The mass concentration of the polydopamine aqueous solution is 3.0-6.0%, the pH value is 8-10, and the solution temperature is 20-50 ℃.
The second step is that: firstly, the surface modification of the asphalt-based graphite carbon fiber yarn by the poly-dopamine aqueous solution infiltration
And carrying out surface modification on the asphalt-based graphite carbon fiber filament by using a polydopamine aqueous solution, wherein the modification method is infiltration, the treatment time is 60-180 s, the drying temperature is 110-150 ℃, and the drying time is 60-120 s.
The third step: forming an active amino surface layer on the surface of pitch-based graphitized carbon fibers
The polydopamine forms an active amino surface layer in an adhesion mode, and the amino amount is determined by the concentration of the polydopamine aqueous solution and the infiltration time.
The fourth step: entering an electrolytic bath for anodic oxidation treatment
The method comprises the steps of carrying out electrochemical anodic oxidation by taking asphalt-based graphite carbon fiber as an anode, a graphite plate as a cathode and an ammonium bicarbonate aqueous solution with the mass concentration of 4.0-8.0% as an electrolyte, wherein the applied current density is 1mA/cm2~4mA/cm2And the temperature of the electrolyte is 30-60 ℃ to obtain the asphalt-based graphite carbon fiber after surface treatment.
The preferred mass concentration of the aqueous solution of polydopamine in said first step is 4.0%, the preferred pH is 9, and the preferred solution temperature is 30 ℃.
In the second step, the treatment time is preferably 120s, the drying temperature is preferably 130 ℃, and the drying time is preferably 90 s.
The preferred current density applied in said fourth step is 3mA/cm2Preferably, the electrolyte temperature is 40 ℃.
The invention has the beneficial effects that: (1) the polydopamine with the universal adhesion function is firstly fixed on the inert surface of the asphalt-based graphite carbon fiber in an aqueous solution adhesion mode, so that the surface of the polydopamine is provided with a certain amount of active amino surface layer, the graphite carbon fiber surface has higher activity and better wettability due to the presence of the active amino, and the oxidation degree of anodic oxidation etching is greatly improved. (2) The introduction of active amino enriches the surface functional group types of the asphalt-based graphite fibers, can generate amidation grafting reaction with a resin matrix, is more tightly combined with the resin, and endows the asphalt-based graphite fibers with higher interlaminar shear strength. (3) The introduction of active amino group changes the inert surface of the asphalt-based graphite carbon fiber into an active surface, which has a synergistic promotion effect on anodic oxidation and has an obvious effect of increasing the oxygen content. The surface treatment method for introducing the active amino is simple, efficient, easy to operate, free of environmental pollution and convenient for industrial application.
Drawings
The invention has 1 figure, and can also be used as the figure of the abstract of the specification.
FIG. 1 is a flow chart of the treatment method of the present invention.
Detailed Description
Embodiments of the invention are further described below with reference to the following drawings:
as shown in fig. 1, the surface treatment method of the pitch-based graphite carbon fiber of the present invention comprises the following steps:
the first step is as follows: preparation of aqueous Polydopamine solutions
The mass concentration of the polydopamine aqueous solution is 3.0-6.0%, the pH value is 8-10, and the solution temperature is 20-50 ℃.
The second step is that: firstly, the surface modification of the asphalt-based graphite carbon fiber yarn by the poly-dopamine aqueous solution infiltration
And carrying out surface modification on the asphalt-based graphite carbon fiber filament by using a polydopamine aqueous solution, wherein the modification method is infiltration, the treatment time is 60-180 s, the drying temperature is 110-150 ℃, and the drying time is 60-120 s.
The third step: forming an active amino surface layer on the surface of pitch-based graphitized carbon fibers
The polydopamine forms an active amino surface layer in an adhesion mode, and the amino amount is determined by the concentration of the polydopamine aqueous solution and the infiltration time.
The fourth step: entering an electrolytic bath for anodic oxidation treatment
The method comprises the steps of carrying out electrochemical anodic oxidation by taking asphalt-based graphite carbon fiber as an anode, a graphite plate as a cathode and an ammonium bicarbonate aqueous solution with the mass concentration of 4.0-8.0% as an electrolyte, wherein the applied current density is 1mA/cm2~4mA/cm2And the temperature of the electrolyte is 30-60 ℃ to obtain the asphalt-based graphite carbon fiber after surface treatment.
Example 1
Firstly, an infiltration method is adopted to lead the asphalt-based graphite carbon fiber to pass through polydopamine aqueous solution with the mass concentration of 3.0 percent, the pH value is 8, the solution temperature is 20 ℃, the processing time is 60s, the drying temperature is 150 ℃, the drying time is 120s, then the graphitized carbon fiber is electrochemically anodized through ammonium bicarbonate aqueous solution with the concentration of 4.0 percent, and the applied current density is 1mA/cm2And the temperature of the electrolyte is 60 ℃, so that the asphalt-based graphite carbon fiber after surface treatment is obtained.
Analyzing the change condition of the surface chemical components by adopting a Thermo VG ESCALAB250 type X photoelectron spectrometer; and (3) carrying out interlaminar shear strength test on the asphalt-based graphite carbon fiber after surface treatment, and obtaining a test sample according to the GB3357-82 method. According to the test of the operation method of GB30969-2014 test method of shear strength of short beams of polymer matrix composite materials, an INSTRON-1121 type universal material tester is adopted to test the interlaminar shear strength of the polymer matrix composite materials, and data are recorded.
Example 2
Firstly, an infiltration method is adopted to lead the asphalt-based graphite carbon fiber to be processed for 180s by polydopamine aqueous solution with the mass concentration of 3.0 percent, the pH value is 8, the solution temperature is 20 ℃, the drying temperature is 150 ℃, the drying time is 120s, then the graphitized carbon fiber is electrochemically anodized by ammonium bicarbonate aqueous solution with the concentration of 4.0 percent, and the applied current density is 1mA/cm2The electrolyte temperature was 60 ℃ to obtain the surface areaAnd (4) the treated asphalt-based graphite carbon fiber. The test method was the same as in example 1.
Example 3
Firstly, an infiltration method is adopted to lead the asphalt-based graphite carbon fiber to be processed for 60s by polydopamine aqueous solution with the mass concentration of 6.0 percent, the pH value is 10, the solution temperature is 50 ℃, the drying temperature is 110 ℃, the drying time is 60s, then the graphitized carbon fiber is electrochemically anodized by ammonium bicarbonate aqueous solution with the concentration of 8.0 percent, and the applied current density is 4mA/cm2And the temperature of the electrolyte is 30 ℃, so that the asphalt-based graphite carbon fiber after surface treatment is obtained. The test method was the same as in example 1.
Example 4
Firstly, an infiltration method is adopted to lead the asphalt-based graphite carbon fiber to be processed for 180s by polydopamine aqueous solution with the mass concentration of 6.0 percent, the pH value is 10, the solution temperature is 50 ℃, the drying temperature is 110 ℃, the drying time is 60s, then the graphitized carbon fiber is electrochemically anodized by ammonium bicarbonate aqueous solution with the concentration of 8.0 percent, and the applied current density is 4mA/cm2And the temperature of the electrolyte is 30 ℃, so that the asphalt-based graphite carbon fiber after surface treatment is obtained. The test method was the same as in example 1.
Example 5
Firstly, an infiltration method is adopted to lead the asphalt-based graphite carbon fiber to be processed for 120s by polydopamine aqueous solution with the mass concentration of 4.0 percent, the pH value is 9, the solution temperature is 30 ℃, the drying temperature is 130 ℃, the drying time is 90s, then the graphitized carbon fiber is processed for electrochemical anode oxidation by ammonium bicarbonate aqueous solution with the concentration of 6.0 percent, and the applied current density is 3mA/cm2And the temperature of the electrolyte is 40 ℃, so that the asphalt-based graphite carbon fiber after surface treatment is obtained. The test method was the same as in example 1.
Comparative example 1
Firstly, an infiltration method is adopted to enable the asphalt-based graphite carbon fiber to be processed for 180s by a polydopamine aqueous solution with the mass concentration of 6.0%, the pH value is 10, the solution temperature is 30 ℃, the drying temperature is 130 ℃, and the drying time is 60s, so that the asphalt-based graphite carbon fiber after surface treatment is obtained. The test method was the same as in example 1.
Comparative example 2
The graphitized carbon fiber is subjected to electrochemical anode oxidation by ammonium bicarbonate aqueous solution with the concentration of 8.0 percent, and the applied current density is 4mA/cm2And the temperature of the electrolyte is 40 ℃, so that the asphalt-based graphite carbon fiber after surface treatment is obtained. The test method was the same as in example 1.
Comparative example 3
An unsurfaced pitch-based graphitic carbon fiber. The test method was the same as in example 1.
The test data are shown in table 1:
TABLE 1 statistical table of element contents and interlaminar shear strengths
Figure BDA0003201794510000051
Through comparison of examples 1, 2, 3, 4 and 5 with comparative examples 1, 2 and 3, the samples of comparative examples 2 and 3 have obviously improved interlaminar shear strength when the surface modification treatment of the polydopamine aqueous solution is carried out before anodic oxidation; the sample of comparative example 1 had an oxygen (O) content of only 0.959 after treatment, while the sample of comparative example 2 had an O content of 1.562 after treatment; however, the oxygen content of O in the examples is at least 3.257 and above (greater than the sum of the oxygen contents of O in comparative examples 1 and 2) by the method of surface modification treatment of the aqueous solution of poly dopamine and then anodic oxidation, because the surface activity of the asphalt-based graphite fiber is greatly enhanced due to the introduction of the surface active amino groups, and the introduction of the surface active amino groups has a synergistic promoting effect during anodic oxidation, so that the oxidation degree is enhanced, and the number of oxygen-containing functional groups is increased.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.

Claims (4)

1. A surface treatment method of asphalt-based graphite carbon fiber is characterized by comprising the following steps:
the first step is as follows: preparation of aqueous Polydopamine solutions
The mass concentration of the polydopamine aqueous solution is 3.0-6.0%, the pH value is 8-10, and the solution temperature is 20-50 ℃;
the second step is that: firstly, the surface modification of the asphalt-based graphite carbon fiber yarn by the poly-dopamine aqueous solution infiltration
Carrying out surface modification on the asphalt-based graphite carbon fiber filament by using a polydopamine aqueous solution, wherein the modification method is infiltration, the treatment time is 60-180 s, the drying temperature is 110-150 ℃, and the drying time is 60-120 s;
the third step: forming an active amino surface layer on the surface of pitch-based graphitized carbon fibers
Forming an active amino surface layer by poly-dopamine in an adhesion mode, wherein the amino amount is determined by the concentration of a poly-dopamine aqueous solution and the infiltration time;
the fourth step: entering an electrolytic bath for anodic oxidation treatment
The method comprises the steps of carrying out electrochemical anodic oxidation by taking asphalt-based graphite carbon fiber as an anode, a graphite plate as a cathode and an ammonium bicarbonate aqueous solution with the mass concentration of 4.0-8.0% as an electrolyte, wherein the applied current density is 1mA/cm2~4mA/cm2And the temperature of the electrolyte is 30-60 ℃ to obtain the asphalt-based graphite carbon fiber after surface treatment.
2. The method for surface treatment of an asphalt-based graphite carbon fiber according to claim 1, wherein the aqueous solution of polydopamine in the first step has a mass concentration of 4.0%, a pH of 9, and a solution temperature of 30 ℃.
3. The method for surface-treating an asphalt-based graphite carbon fiber according to claim 1, wherein the treating time in the second step is 120 seconds, the drying temperature is 130 ℃, and the drying time is 90 seconds.
4. The method for surface-treating an asphalt-based graphite carbon fiber according to claim 1, wherein the current density applied in said fourth step is 3mA/cm2The temperature of the electrolyte was 40 ℃.
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CN114634368A (en) * 2022-05-13 2022-06-17 浙江星辉新材料科技有限公司 High-density carbon fiber plate and preparation method thereof
CN115595792A (en) * 2022-10-27 2023-01-13 陕西天策新材料科技有限公司(Cn) Treatment method of ultrahigh-modulus asphalt-based graphite fiber

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CN115595792A (en) * 2022-10-27 2023-01-13 陕西天策新材料科技有限公司(Cn) Treatment method of ultrahigh-modulus asphalt-based graphite fiber

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