碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面功能涂層制備研究
發(fā)布時(shí)間：2018-07-13 15:43
【摘要】：本研究旨在提高碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料在特殊應(yīng)用下的耐特殊介質(zhì)腐蝕能力,采用等離子體表面技術(shù)在碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面進(jìn)行功能涂層的制備。為了克服碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面極性弱、表面膜層結(jié)合強(qiáng)度低等缺點(diǎn),先使用霍爾源放電等離子體對(duì)碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料進(jìn)行表面活化處理,以提高其表面極性和浸潤(rùn)性,再通過(guò)直流磁控濺射技術(shù)在碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面低溫制備Al涂層。設(shè)計(jì)不同等離子體處理工藝,改變等離子體類型,通過(guò)接觸角測(cè)試、拉伸試驗(yàn)、金相分析、掃描電鏡分析和紅外光譜分析,對(duì)比等離子體處理前后碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面浸潤(rùn)性、表面形貌、力學(xué)性能和表面官能團(tuán)的變化,并探究等離子體處理碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料的最佳工藝。利用X射線衍射(XRD)和掃描電子顯微鏡(SEM)分析碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面Al涂層組織結(jié)構(gòu),自行設(shè)計(jì)垂直拉伸裝置測(cè)定涂層與基體間的結(jié)合強(qiáng)度,并探究不同等離子體處理功率和處理前后不同涂層厚度對(duì)膜基結(jié)合強(qiáng)度的影響。通過(guò)耐含氟介質(zhì)腐蝕性實(shí)驗(yàn),對(duì)比Al涂層制備前后碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料的耐含氟介質(zhì)腐蝕能力,結(jié)果表明： (1)等離子體處理后碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料與蒸餾水的接觸角明顯降低,表面浸潤(rùn)性和自由能顯著提高。等離子體處理效果與工藝參數(shù)和等離子體類型密切相關(guān),接觸角隨處理電流、氣壓的增加先降低后上升,隨處理時(shí)間的延長(zhǎng)先迅速降低后趨于穩(wěn)定,當(dāng)處理電流為1A、氣壓為1Pa、處理時(shí)間為10min時(shí),接觸角達(dá)到極小值,表面浸潤(rùn)性最佳。相同工藝參數(shù)下,不同類型等離子體處理效果依次為：O2N2Ar。 (2)經(jīng)等離子體處理后,碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面的處理效果存在時(shí)效性,即隨著放置時(shí)間的延長(zhǎng)處理效果下降。等離子體處理時(shí)效性與氣體源和保存環(huán)境有關(guān),常溫去離子水中保存可提高時(shí)效性,氧等離子體處理后時(shí)效性較好,氬等離子體次之,氮等離子體最差。 (3)金相顯微鏡和SEM觀察可知,等離子體處理后碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面吸附的雜質(zhì)小顆粒明顯減少,刻蝕痕跡明顯,表面粗糙度增加,纖維樹(shù)脂間粘連程度增加。紅外光譜分析結(jié)果顯示,氬等離子體處理后,碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料表面C-C數(shù)量減少,C-O數(shù)量增加,同時(shí)酯基數(shù)量減少,酮基、羧基和醇羥基數(shù)量相應(yīng)增加；氧等離子體處理后CH2-O-CH2吸收峰強(qiáng)度增大；氮等離子體處理后出現(xiàn)C=N和C≡N兩個(gè)較明顯的含氮吸收峰。 (4)等離子體處理后,Al涂層與碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料間結(jié)合強(qiáng)度顯著上升,且隨處理電流的增大先上升再降低,在電流為1A時(shí)最佳。膜基結(jié)合強(qiáng)度隨涂層厚度增加而降低的趨勢(shì)減弱,在涂層厚度達(dá)到25um時(shí),膜基結(jié)合強(qiáng)度仍較大,為2.88MPa,而未經(jīng)等離子體處理時(shí)僅為1.22MPa。 (5)耐含氟介質(zhì)腐蝕性實(shí)驗(yàn)表明,Al涂層制備后碳纖維增強(qiáng)樹(shù)脂基復(fù)合材料在含氟介質(zhì)中的平均腐蝕速率為4.17×10-3g/m2.h-1,相比較Al涂層制備前的3.78×10-2g/m2·h-1,減小了一個(gè)量級(jí),耐含氟介質(zhì)腐蝕能力顯著提高。
[Abstract]:The purpose of this study is to improve the specific corrosion resistance of carbon fiber reinforced resin matrix composites in special applications. The preparation of functional coatings on the surface of carbon fiber reinforced resin matrix composites by plasma surface technology is used to overcome the weak surface polarity of carbon fiber reinforced resin matrix composites and the bonding strength of the surface film layer. The surface activation of carbon fiber reinforced resin matrix composites was first treated with Holzer source discharge plasma to improve the surface polarity and wettability. The Al coating was prepared at low temperature on the surface of carbon fiber reinforced resin matrix composites by DC magnetron sputtering. Different plasma treatment processes were designed and changed. By means of contact angle test, tensile test, metallographic analysis, scanning electron microscope analysis and infrared spectrum analysis, the surface wettability, surface morphology, mechanical properties and surface functional groups of carbon fiber reinforced resin matrix composites are compared before and after plasma treatment, and the plasma treatment of carbon fiber reinforced resin matrix composites is also explored. X ray diffraction (XRD) and scanning electron microscope (SEM) were used to analyze the structure of Al coating on the surface of carbon fiber reinforced resin matrix composites. The bonding strength between the coating and the substrate was measured by the self designed vertical drawing device, and the strength of different plasma treatment and the bonding strength of different coating thickness to the film base before and after treatment were investigated. The corrosion resistance of carbon fiber reinforced resin matrix composites before and after the preparation of Al coating was compared. The results showed that the corrosion resistance of carbon fiber reinforced resin matrix composites before and after preparation was compared.
(1) the contact angle of the carbon fiber reinforced resin matrix composites and the distilled water decreased obviously after the plasma treatment, and the surface wettability and free energy increased significantly. The plasma treatment effect was closely related to the process parameters and plasma types. The contact angle increased first and then increased with the treatment current. When the current is 1A, the pressure is 1Pa, the treatment time is 10min, the contact angle reaches the minimum and the surface wettability is the best. Under the same process parameters, the effect of different types of plasma treatment is: O2N2Ar.
(2) after the plasma treatment, the treatment effect of the carbon fiber reinforced resin matrix composite surface has the aging effect, that is, the treatment effect decreases with the prolongation of the storage time. The aging property of the plasma treatment is related to the gas source and the preservation environment. The storage of the atmospheric deionized water can be raised to the high aging property, and the aging property after the oxygen plasma treatment is better. The argon plasma is the second, and the nitrogen plasma is the worst.
(3) the metallographic microscope and SEM observation show that the small particles adsorbed on the surface of the carbon fiber reinforced resin matrix composites after the plasma treatment are obviously reduced, the etching marks are obvious, the surface roughness is increased and the degree of adhesion between the fiber resin is increased. The infrared spectrum analysis results show that the carbon fiber reinforced resin matrix composite after the argon plasma treatment. The number of C-C on the surface of the material is reduced, the number of C-O increases, the number of ester groups decreases, the number of ketones, carboxyl and alcohol hydroxyl increases, and the peak intensity of CH2-O-CH2 absorption increases after the treatment of oxygen plasma, and there are two obvious nitrogen absorption peaks of C=N and C N after the treatment of nitrogen plasma.
(4) after plasma treatment, the bonding strength between the Al coating and the carbon fiber reinforced resin matrix composites increases significantly, and increases first and then decreases with the increase of the treatment current. The film base binding strength decreases with the increase of the coating thickness. When the coating thickness reaches 25um, the adhesion strength of the film base is still larger, which is 2.88M. Pa, and only 1.22MPa. without plasma treatment
(5) the corrosion resistance test of fluorine resistant medium shows that the average corrosion rate of the carbon fiber reinforced resin matrix composites in the fluorine containing medium after the preparation of Al coating is 4.17 x 10-3g/m2.h-1, compared with 3.78 x 10-2g/m2 / H-1 before the preparation of Al coating, which is reduced by one order of magnitude and the corrosion resistance of fluorine resistant medium is significantly improved.
【學(xué)位授予單位】：中國(guó)科學(xué)技術(shù)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ327.3;TB33
本文編號(hào)：2119931
[Abstract]:The purpose of this study is to improve the specific corrosion resistance of carbon fiber reinforced resin matrix composites in special applications. The preparation of functional coatings on the surface of carbon fiber reinforced resin matrix composites by plasma surface technology is used to overcome the weak surface polarity of carbon fiber reinforced resin matrix composites and the bonding strength of the surface film layer. The surface activation of carbon fiber reinforced resin matrix composites was first treated with Holzer source discharge plasma to improve the surface polarity and wettability. The Al coating was prepared at low temperature on the surface of carbon fiber reinforced resin matrix composites by DC magnetron sputtering. Different plasma treatment processes were designed and changed. By means of contact angle test, tensile test, metallographic analysis, scanning electron microscope analysis and infrared spectrum analysis, the surface wettability, surface morphology, mechanical properties and surface functional groups of carbon fiber reinforced resin matrix composites are compared before and after plasma treatment, and the plasma treatment of carbon fiber reinforced resin matrix composites is also explored. X ray diffraction (XRD) and scanning electron microscope (SEM) were used to analyze the structure of Al coating on the surface of carbon fiber reinforced resin matrix composites. The bonding strength between the coating and the substrate was measured by the self designed vertical drawing device, and the strength of different plasma treatment and the bonding strength of different coating thickness to the film base before and after treatment were investigated. The corrosion resistance of carbon fiber reinforced resin matrix composites before and after the preparation of Al coating was compared. The results showed that the corrosion resistance of carbon fiber reinforced resin matrix composites before and after preparation was compared.
(1) the contact angle of the carbon fiber reinforced resin matrix composites and the distilled water decreased obviously after the plasma treatment, and the surface wettability and free energy increased significantly. The plasma treatment effect was closely related to the process parameters and plasma types. The contact angle increased first and then increased with the treatment current. When the current is 1A, the pressure is 1Pa, the treatment time is 10min, the contact angle reaches the minimum and the surface wettability is the best. Under the same process parameters, the effect of different types of plasma treatment is: O2N2Ar.
(2) after the plasma treatment, the treatment effect of the carbon fiber reinforced resin matrix composite surface has the aging effect, that is, the treatment effect decreases with the prolongation of the storage time. The aging property of the plasma treatment is related to the gas source and the preservation environment. The storage of the atmospheric deionized water can be raised to the high aging property, and the aging property after the oxygen plasma treatment is better. The argon plasma is the second, and the nitrogen plasma is the worst.
(3) the metallographic microscope and SEM observation show that the small particles adsorbed on the surface of the carbon fiber reinforced resin matrix composites after the plasma treatment are obviously reduced, the etching marks are obvious, the surface roughness is increased and the degree of adhesion between the fiber resin is increased. The infrared spectrum analysis results show that the carbon fiber reinforced resin matrix composite after the argon plasma treatment. The number of C-C on the surface of the material is reduced, the number of C-O increases, the number of ester groups decreases, the number of ketones, carboxyl and alcohol hydroxyl increases, and the peak intensity of CH2-O-CH2 absorption increases after the treatment of oxygen plasma, and there are two obvious nitrogen absorption peaks of C=N and C N after the treatment of nitrogen plasma.
(4) after plasma treatment, the bonding strength between the Al coating and the carbon fiber reinforced resin matrix composites increases significantly, and increases first and then decreases with the increase of the treatment current. The film base binding strength decreases with the increase of the coating thickness. When the coating thickness reaches 25um, the adhesion strength of the film base is still larger, which is 2.88M. Pa, and only 1.22MPa. without plasma treatment
(5) the corrosion resistance test of fluorine resistant medium shows that the average corrosion rate of the carbon fiber reinforced resin matrix composites in the fluorine containing medium after the preparation of Al coating is 4.17 x 10-3g/m2.h-1, compared with 3.78 x 10-2g/m2 / H-1 before the preparation of Al coating, which is reduced by one order of magnitude and the corrosion resistance of fluorine resistant medium is significantly improved.
【學(xué)位授予單位】：中國(guó)科學(xué)技術(shù)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ327.3;TB33
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