CN103087341B - Surface treatment method of carbon fiber epoxy resin composite material - Google Patents
Surface treatment method of carbon fiber epoxy resin composite material Download PDFInfo
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- CN103087341B CN103087341B CN201310030872.8A CN201310030872A CN103087341B CN 103087341 B CN103087341 B CN 103087341B CN 201310030872 A CN201310030872 A CN 201310030872A CN 103087341 B CN103087341 B CN 103087341B
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Abstract
The invention discloses a surface treatment method of a carbon fiber epoxy resin composite material. The surface treatment method comprises steps of: polishing the contact part of a carbon fiber epoxy resin composite material and an electrode, removing oil through a hot alkaline solution, cleaning a surface through water, corroding the surface in a concentrated sulfuric acid and hydrogen peroxide solution, roughening and oxidizing the surface in hot concentrated nitric acid, cleaning the surface through water, coating a layer of conducting adhesive on the surface and curing, polishing the surface of the conducting adhesive, cleaning and polishing the surface through an acetone solution, etc. According to the surface treatment method of the carbon fiber epoxy resin composite material disclosed by the invention, the surface carbon fiber end which is arranged on the carbon fiber epoxy resin composite material and is in contact with the metal electrode is exposed outwards to the greatest extent through mechanical and chemical ways; meanwhile, binding performance of the carbon fiber is improved, and low-resistivity conducting adhesive is used for filling a clearance between the fiber and the resin, so as to reduce a contact resistivity between the fiber and the resin. And the method has the advantages of simple process, low contact resistivity, high binding strength between the conducting layer and the composite material, and the like.
Description
Technical field
The invention belongs to surface treatment technology of material field, particularly relate to a kind of can reduction and the surface treatment method of the carbon fiber ring epoxy resin composite material of metal electrode Contact resistance.
Background technology
The advantages such as carbon fiber ring epoxy resin composite material is because of its specific tenacity and specific modulus is high, fatigue resistance is good, designability is strong, have been widely used in the fields such as aerospace, wind-power electricity generation, building.But the electric conductivity of this type of material is lower, while bearing the current load of the generations such as thunder-strike current, induced current, static charge electric discharge in military service process, the resistance heat of release can damage material production, reduces its mechanical property, threatens structural safety.Thereby carbon fiber ring epoxy resin composite material being connected by electric charge release with metal is to reduce one of important method of damage, but this type of material and metal straight while connecing in succession contact resistance excessive, electric current by time the heat that produces mainly concentrate on both interface, cause junction premature failure.In order to reduce contact resistance, some investigator adopts the method for metallising such as electro-coppering, electroless copper to process the surface of carbon fiber ring epoxy resin composite material, but these class methods exist shortcomings such as technique is cumbersome, liquid waste disposal difficulty is large; Also some investigator is connected with directly adopting conductive resin after the polishing of metallic contact position carbon fiber ring epoxy resin composite material with metal electrode, because does not fully expose some carbon fiber end, carbon fiber and conductive resin wettability is poor etc. that reason exists the excessive problem of contact resistance.
Summary of the invention
In order to address the above problem, the object of the invention is to propose one and can reduce and intermetallic contact resistance, and the surface treatment method of the simple carbon fiber ring epoxy resin composite material of technique.
In order to achieve the above object, the surface treatment method of carbon fiber ring epoxy resin composite material provided by the invention comprises the following step carrying out in order:
1) first will on carbon fiber ring epoxy resin composite material, carry out polishing with flint paper and fine sandpaper successively with metal electrode contact site, until expose all carbon fibers end at this position;
2) with the hot alkaline solution of 50～60 ℃, above-mentioned polished surface is carried out to oil removing 20～30 minutes;
3) water cleans the surface after above-mentioned oil removing;
4) surface after above-mentioned cleaning is put into 98% vitriol oil and the 30% hydrogen peroxide mixed solution within 2: 1 by volume, prepared and corroded 10～20 minutes, to remove carbon fiber part resin around, make carbon fiber be exposed to more surface;
5) then immersing temperature is 80～90 ℃, within the nitric acid that concentration is 40% 20～30 minutes, carries out alligatoring oxidation, to generate the functional group good with conductive resin associativity at carbon fiber surface;
6) water cleans above-mentioned surface after nitric acid treatment;
7) the surface-coated one deck low-resistivity conductive resin after above-mentioned cleaning heating cure and form conductive layer;
8) conductive layer surface of above-mentioned formation is carried out to polishing, until this surperficial roughness is lower than thickness 50～100 μ m of 10 μ m, conductive layer;
9) clean above-mentioned glazed surface with acetone soln, obtain thus the carbon fiber ring epoxy resin composite material of low contact resistance.
Described step 2) in every liter of alkaline solution in containing NaOH, the Na of 15g of 60g
2cO
3na with 30g
3pO
4.
Described step 7) in low-resistivity conductive resin be selected from volume specific resistance lower than 4 × 10
-3epoxy conductive silver glue, the epoxy cupric powder conductive adhesive of Ω cm and fill out the one in silver-colored silicone grease conductive resin.
Carbon fiber ring epoxy resin composite material surface treatment method provided by the invention is to utilize machinery and chemical treatment means to make on carbon fiber ring epoxy resin composite material with the surface carbon fiber end of metal electrode Contact as much as possible to exposing outside, improve the adhesiveproperties of carbon fiber simultaneously, and with low-resistivity conductive resin fiberfill fibers and interlaminar resin space, reduce contact resistance between the two with this.Present method also has that technique is simple, bonding strength advantages of higher.
Accompanying drawing explanation
Fig. 1 is four potentiometry measured resistance value testing apparatus structural representations.
Wherein:
Embodiment
Below in conjunction with the drawings and specific embodiments, the surface treatment method of carbon fiber ring epoxy resin composite material provided by the invention is elaborated.
Embodiment 1
Select T300/914 carbon fiber ring epoxy resin composite material veneer sheet as sample, ply sequence [(0/90)
4]
s, specimen size is 200mm × 10mm × 2mm.Be 200,400,600 sand paper polishing successively by granularity by the surface of above-mentioned T300/914 carbon fiber ring epoxy resin composite material, then after water clean surface, sample is for subsequent use as a comparison.
Be 200,400,600 sand paper polishing successively by granularity by the surface of above-mentioned T300/914 carbon fiber ring epoxy resin composite material; Then with in 50 ℃ every liter containing 60g NaOH, 15g Na
2cO
3with 30g Na
3pO
4hot alkaline solution oil removing 30 minutes; Water clean surface afterwards; 98% vitriol oil and the 30% hydrogen peroxide mixed solution of surface after above-mentioned cleaning being put into preparation in 2: 1 by volume corrode 10 minutes; Immersing temperature is within 20 minutes, to carry out alligatoring oxidation in 40% nitric acid of 80 ℃; Water clean surface; Be not more than 4 × 10 in above-mentioned surface-coated one deck body resistivity after treatment
-4the EPO-TEK H20E epoxy conductive silver glue of Ω cm, and at 80 ℃, be incubated 90 minutes and be cured and form conductive layer; Be that 600,1200 sand paper and the aluminium sesquioxide suspension of 10 μ m carry out polishing to above-mentioned conductive layer by granularity successively, conductive layer final thickness approximately 60 μ m, with acetone soln cleaning polishing surface, obtain thus the carbon fiber ring epoxy resin composite material of low contact resistance.
Be 200,400,600 sand paper polishing successively by granularity by the surface of T300/914 carbon fiber ring epoxy resin composite material; Then with in 55 ℃ every liter containing 60g NaOH, 15g Na
2cO
3and 30gNa
3pO
4hot alkaline solution oil removing 25 minutes; Water clean surface; 98% vitriol oil and the 30% hydrogen peroxide mixed solution of surface after above-mentioned polishing being put into preparation in 2: 1 by volume corrode 20 minutes; Immersing temperature is within 25 minutes, to carry out alligatoring oxidation in 40% nitric acid of 90 ℃; Water clean surface; Be not more than 8 × 10 in above-mentioned surface-coated one deck body resistivity after treatment
-5the Cotronics Duralco120 epoxy conductive silver glue of Ω cm, and at 120 ℃, be incubated 20 minutes and be cured and form conductive layer; Be that 600,1200 sand paper and the aluminium sesquioxide suspension of 10 μ m carry out polishing to above-mentioned conductive layer by granularity successively, conductive layer final thickness approximately 80 μ m, with acetone soln cleaning polishing surface, obtain thus the carbon fiber ring epoxy resin composite material of low contact resistance.
Be 200,400,600 sand paper polishing successively by granularity by the surface of T300/914 carbon fiber ring epoxy resin composite material; Then with in 50 ℃ every liter containing 60g NaOH, 15g Na
2cO
3and 30gNa
3pO
4hot alkaline solution oil removing 25 minutes; Water clean surface; 98% vitriol oil and the 30% hydrogen peroxide mixed solution of surface after above-mentioned polishing being put into preparation in 2: 1 by volume corrode 15 minutes; Immersing temperature is within 25 minutes, to carry out alligatoring oxidation in 40% nitric acid of 85 ℃; Water clean surface; In above-mentioned surface-coated one deck body resistivity 10 after treatment
-4～10
-3the Wuhan DB2012 of the Shuan Jiankaimu sealing material company limited epoxy cupric powder conductive adhesive of Ω cm, is incubated 3 hours at 80 ℃ and is cured and forms conductive layer; Be that 600,1200 sand paper and the aluminium sesquioxide suspension of 10 μ m carry out polishing to above-mentioned conductive layer by granularity successively, conductive layer final thickness approximately 90 μ m, with acetone soln cleaning polishing surface, obtain thus the carbon fiber ring epoxy resin composite material of low contact resistance.
In order to verify the effect of surface treatment method of carbon fiber ring epoxy resin composite material provided by the invention, the inventor has carried out following experiment:
The contrast sample that the carbon fiber ring epoxy resin composite material of the low contact resistance that above-described embodiment 2-4 is made and embodiment 1 make utilizes four potentiometry measured resistance value testing apparatuss shown in Fig. 1 to measure the contact resistance between itself and copper electrode.
As shown in Figure 1, measuring resistance R
mmainly comprise wire resistance R
l, sample resistance R
s, copper electrode resistance R
eand carbon fiber ring epoxy resin composite material and the interelectrode contact resistance R of metallic copper
cif, by wire resistance R
lignore:
R
mR
S+R
e+R
c (1)
Sample resistance can be expressed as:
Wherein ρ
ffor the resistivity of fiber, L
xfor specimen length, V
ffor fiber volume fraction, L
yfor specimen width, e
0be 0
0laying total thickness.The resistivity of the Torayca T300 carbon fiber of selecting in embodiment is about 1.7 × 10
-2Ω mm, in fiber direction, the length of sample is 200mm, and fiber volume fraction is about 0.6, and specimen width is 20mm, and 0 ° of laying total thickness is about 1.0mm, obtains sample resistance R by formula (2)
sbe about 0.28 Ω.The contact pressure applying by above-mentioned testing apparatus is 10N, impressed current 1A, 5 minutes conduction time.Along with the increase of galvanic action time, specimen temperature raises, and now sample resistance can change, and because conduction time is shorter, resistance change can be ignored.The resistivity of copper is about 1.7 × 10
-5Ω mm, therefore copper electrode resistance R
ealso can ignore.According to formula (1), the resistance R of measurement
mdeduct sample resistance R
sbe about contact resistance R
c.
After tested, in embodiment 1, contrast sample and contact the contact resistance R recording with copper electrode
cbe 30.4 Ω; The contact resistance R recording between the carbon fiber ring epoxy resin composite material in embodiment 2-4 after surface treatment and copper electrode
cbe respectively 0.44 Ω, 0.40 Ω and 0.48 Ω, as can be seen here, the carbon fiber ring epoxy resin composite material of low contact resistance provided by the invention is compared than the contact resistance R of sample
chave significantly and reduced.
In addition, the inventor has also carried out the thermal shock test of 150 ℃ ,-100 ℃ to the carbon fiber ring epoxy resin composite material of the above-mentioned low contact resistance of being made up of embodiment 2-4, verifies the bonding strength of conductive layer with this.Result shows, the carbon fiber ring epoxy resin composite material after these conductive processing equal flawless of conductive layer, phenomenon such as come off after 50 thermal shock tests produce, and show that conductive layer has larger bonding strength.
Claims (3)
1. a surface treatment method for carbon fiber ring epoxy resin composite material, is characterized in that: described surface treatment method comprises the following step carrying out in order:
1) first will on carbon fiber ring epoxy resin composite material, carry out polishing with flint paper and fine sandpaper successively with metal electrode contact site, until expose all carbon fibers end at this position;
2) with the hot alkaline solution of 50～60 ℃, above-mentioned polished surface is carried out to oil removing 20～30 minutes;
3) water cleans the surface after above-mentioned oil removing;
4) surface after above-mentioned cleaning is put into 98% vitriol oil and the 30% hydrogen peroxide mixed solution within 2: 1 by volume, prepared and corroded 10～20 minutes, to remove carbon fiber part resin around, make carbon fiber be exposed to more surface;
5) then immersing temperature is 80～90 ℃, within the nitric acid that concentration is 40% 20～30 minutes, carries out alligatoring oxidation, to generate the functional group good with conductive resin associativity at carbon fiber surface;
6) water cleans above-mentioned surface after nitric acid treatment;
7) the surface-coated one deck low-resistivity conductive resin after above-mentioned cleaning heating cure and form conductive layer;
8) conductive layer surface of above-mentioned formation is carried out to polishing, until this surperficial roughness is lower than thickness 50～100 μ m of 10 μ m, conductive layer;
9) clean above-mentioned glazed surface with acetone soln, obtain thus the carbon fiber ring epoxy resin composite material of low contact resistance.
2. the surface treatment method of carbon fiber ring epoxy resin composite material according to claim 1, is characterized in that: described step 2) in every liter of alkaline solution in containing NaOH, the Na of 15g of 60g
2cO
3na with 30g
3pO
4.
3. the surface treatment method of carbon fiber ring epoxy resin composite material according to claim 1, is characterized in that: described step 7) in low-resistivity conductive resin be selected from volume specific resistance lower than 4 × 10
-3epoxy conductive silver glue, the epoxy cupric powder conductive adhesive of Ω cm and fill out the one in silver-colored silicone grease conductive resin.
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| CN103551096B (en) * | 2013-10-25 | 2015-05-27 | 南京工业大学 | Carbon fiber microchip reactor |
| CN107759816B (en) * | 2017-08-31 | 2020-08-28 | 中国石油大学(华东) | Surface treatment method of carbon fiber composite material |
| CN111234657A (en) * | 2020-04-05 | 2020-06-05 | 台州天舒新材料科技有限公司 | Light high-conductivity coating and preparation method and application thereof |
| CN112961385A (en) * | 2021-02-03 | 2021-06-15 | 成都雅印电子科技有限公司 | Method for metalizing surface of three-dimensional non-metal substrate |
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| JP特开2011-76738A 2011.04.14 |
| 纪朝辉.表面预处理对复合材料铝导电涂层性能的影响.《焊接技术》.2009,第38卷(第10期),第16-18页. |
| 表面预处理对复合材料铝导电涂层性能的影响;纪朝辉;《焊接技术》;20091028;第38卷(第10期);第16-17页第1.1节 * |
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