Cf/Al复合材料表面稀土膜的表征及耐蚀特性研究
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摘要
碳纤维增强铝基(Cf/Al)复合材料在航天、空间领域有广阔的应用背景,这一材料应用的关键技术之一是耐蚀性能问题。本文在Cf/6061Al复合材料多相表面制备了两种稀土耐蚀膜层,即稀土转化膜和Ni-P/稀土多层膜,系统研究了两种膜层微观组织和耐蚀性能,探索两种稀土膜层的沉积机制和耐蚀特性。
Cf/Al复合材料表面形成的稀土Ce转化膜层是由岛状、凸凹不平的纳米级别球形颗粒层层堆积而成,膜层厚度约3μm,球形颗粒大小在4nm~8nm之间,颗粒团聚明显。TEM测得的晶体结构特征表明,稀土膜层由多种Ce的化合物混合而成, Ce转化膜层主要成分是Ce的氧化物和氢氧化物,化合价态为Ce3+和Ce4+,膜层中还含有少量铝的化合物,表明Ce转化膜成膜过程中伴随着铝基体的溶解。Cf/Al复合材料多相表面的稀土转化膜层沉积机理为:在铝合金基体上成膜符合“微阴极成膜机理”;增强体碳纤维表面稀土化合物沉积以化学吸附和物理吸附为主要形式,而且碳纤维表面的“悬挂键”同稀土元素特有的“剩余化学键”的相互作用也会促进稀土膜层在增强体表面的沉积。稀土化合物在石墨材料表面沉积优先发生在其表面缺陷处,并且这一特性可以修复石墨表面的划伤,对石墨材料表面具有“可修复”作用。
Cf/Al复合材料表面可以镀覆一层均匀的Ni-P合金预镀层,在铝合金表面获得催化活性点,实现了Cf/Al复合材料多相表面化学镀Ni-P合金镀层;增强体碳纤维表面的化学吸附和物理吸附是产生化学镀镍催化活性点的主要原因。Cf/Al复合材料表面预镀的化学镀镍层高的耐蚀性,一方面是镀层含有非晶体成分,腐蚀敏感的晶界少;另一方面,Ni-P镀层减缓了腐蚀介质对Cf/Al复合材料的之间接触,两者协同作用使Cf/Al复合材料耐蚀性大大提高。
化学镀镍和稀土膜层的复合提高了耐蚀膜层的致密性,Ni-P/稀土多层膜微裂纹很少,膜层均匀;电位-pH图结合XPS测试分析发现,Ni-P/稀土多层膜外层稀土化合物的化合价态以Ce4+为主要形式,Ni-P/稀土多层膜的非晶体特征更加明显,加之稀土化合物在化学镀镍膜层微孔处沉积,形成“封孔效应”,进一步提高了Cf/Al复合材料的耐蚀性。
全浸泡腐蚀试验可知,Ni-P/稀土多层膜变化较少,腐蚀程度最轻微;稀土膜层浸泡后膜层颜色变浅,膜层有脱落迹象;化学镀镍膜层腐蚀产物粘附较多;无膜层试样碳纤维的裸露严重。极化曲线对比表明,Ni-P/稀土多层膜处理后的试样腐蚀电势Ecorr相对于无膜层试样增大400mV以上,同时Ni-P/稀土多层膜试样的腐蚀电流密度比无膜层试样的腐蚀电流密度减小了1.32μA·cm-2。稀土膜层的极化曲线阴极分支和阳极分支同无膜层极化曲线相比,都向左移,其阳极反应和阴极反应均被抑制。交流阻抗谱解析结果表明,几种膜层的耐蚀性依次为Ni-P/稀土多层膜>化学镀镍膜层>稀土膜层>无膜层试样,Ni-P/稀土多层膜阻抗值最高,极化电阻为23051Ω,比无膜层试样增高8倍多。
化学镀镍及稀土膜层耐蚀性提高的原因来自膜层晶体结构含有非晶体成分或纳米微晶结构,对腐蚀反应不敏感,膜层阻挡了腐蚀的电化学反应路径。Ni-P/稀土多层膜耐蚀性提高除了化学镀镍膜层的因素外,稀土化合物在化学镀镍膜层微孔处沉积,形成“封孔效应”,并且其表面沉积稀土为Ce4+化合物,抗氧化性更强,从而使Cf/Al复合材料Ni-P/稀土多层膜的耐蚀性高于化学镀镍及单一稀土膜层。
In recent years, carbon fibers reinforced aluminum matrix (Cf/Al) composites are applied in some fields such as aerial material and space technology. It is important to improve corrosion resistance for this composite. For the purpose of improving corrosion resistance of Cf/Al composites, two coatings were prepared by rare earth conversion coating and Ce-rich complex films. The fabrication processes, microstructure and corrosion properties of two coatings were examined, their influencing factors were discussed, the deposition and corrosion resistance mechanics were studied in this paper.
It was found that the Ce conversion coating covered the whole surface of Cf/Al composites as oxidized islands, but some micro-cracks for the coating. The Ce conversion coating was island-like, and it was piled up by spherical Ce-riched particles. The size of Ce-riched particles was about 4nm~8nm, the multiple Ce-rich compounds were mixing in Ce-rich particles, and particles clustering. The thickness of Ce conversion coating is about 3μm, Ce oxides and Ce hydroxides are main composition of Ce conversion coating, which containing Ce3+ and Ce4+ compounds. The little Al compounds in this coating, it is indicated that Al dissolved during processes of formation films.
Uniform Ni-P coating on the surface of Cf/Al composites can be realized by electroless deposition, the catalytic active points for chemical deposition on the Al matrix promoted Ni-P deposition; chemical and physical absorption on the surface of carbon fibers were main reasons for catalytic active points in order to deposit Ni-P alloys. Improvement of corrosion resistance for Ni-P coatings on multi-phases surfaces of Cf/Al composites came from amorphous composition which has insensitive to corrosion reaction in Ni-P coatings, because there were less grain boundary in amorphous films. Moreover, Ni-P coatings can avoid direct touching between corrosion medium and surface of Cf/Al composites. Synergistic effect of them can improve corrosion resistance on Cf/Al composites.
Mechanism of rare earth conversion coating on multi-phases surface of Cf/Al composites is stated that“Mechanism of micro-cathodic deposition”was main factor on the Al matrix, on the other hand, chemical adsorption or physical adsorption was main formed Ce-rich coatings on surface of carbon fibers, therefore, the interactivity“Dangling bonds”on the surface of carbon fibers and“Surplus chemical bonds”belonged to rare earth elements had effect of depositing Ce-rich coating. The behavior of Ce compounds deposition occurred near defects of carbon surface and this characteristic could heal the scratch on carbon surface; this phenomenon can be named“self-healing”on the carbon surface.
The Ce-rich complex films are high condensing coatings which could obtain by Ni-P coatings with rare earth compounds sealing. There are few cracks in Ce-rich complex films and conforming layers. Image of potential-pH combined with XPS analysis can be indicated that the Ce4+ species were main components of Ce compounds in Ce-rich complex films. Microstructure characteristic of complex films is obvious a nano-crystal structure, additionally, the Ce compounds deposit on the sites of micro-porous on the Ni-P coatings,“sealing-effects”is main causes for improving corrosion resistance of Cf/Al composites.
The contrasts of microstructure characterization after immersion testing at the same conditions showed that the corrosion degree of complex films were slightly, the microstructure of coatings changed a little; the Ce conversion coatings had slight loss of color, some evidence supported the existence of coatings exfoliation; the more erosion products adhesive on the electroless plating Ni-P coatings; the carbon fibers had obvious bareness on uncoating samples. The corrosion potential (Ecorr) of complex films has improved more than 400mV as contrast on uncoating samples, the corrosion current density (icorr) of complex films have decreased 1.32μA·cm-2 than uncoating samples. The anodic and cathodic branches of polarization curves of Ce conversion coating were both decreased obviously, the corrosion reaction from anode and cathode were restrained at the same time.
The results of electrochemistry impedance spectra (EIS) indicated that the corrosion resistance of different coatings listed as follows: Complex films > Ni-P coatings > Ce conversion coatings > uncoatings. From EIS simply analysis, the impedance values of polarization resistance for complex films was 23051Ω, which improved 8 times than uncoating samples.
The main reasons for inhibition corrosion came from contents of amorphous structure in Ni-P coatings and rare earth conversion coatings, which structure is insensitive to corrosion reaction; in addition, the coatings inhibit electrochemical reaction. Ce-rich complex films have the best corrosion resistance because it has formed“sealing effects”. Moreover, Ce4+ species deposit surface of Ni-P coatings, there are better oxidation resistance of Ce4+ species than single Ce-rich coating and Ni-P coating.
Cf/Al复合材料表面形成的稀土Ce转化膜层是由岛状、凸凹不平的纳米级别球形颗粒层层堆积而成,膜层厚度约3μm,球形颗粒大小在4nm~8nm之间,颗粒团聚明显。TEM测得的晶体结构特征表明,稀土膜层由多种Ce的化合物混合而成, Ce转化膜层主要成分是Ce的氧化物和氢氧化物,化合价态为Ce3+和Ce4+,膜层中还含有少量铝的化合物,表明Ce转化膜成膜过程中伴随着铝基体的溶解。Cf/Al复合材料多相表面的稀土转化膜层沉积机理为:在铝合金基体上成膜符合“微阴极成膜机理”;增强体碳纤维表面稀土化合物沉积以化学吸附和物理吸附为主要形式,而且碳纤维表面的“悬挂键”同稀土元素特有的“剩余化学键”的相互作用也会促进稀土膜层在增强体表面的沉积。稀土化合物在石墨材料表面沉积优先发生在其表面缺陷处,并且这一特性可以修复石墨表面的划伤,对石墨材料表面具有“可修复”作用。
Cf/Al复合材料表面可以镀覆一层均匀的Ni-P合金预镀层,在铝合金表面获得催化活性点,实现了Cf/Al复合材料多相表面化学镀Ni-P合金镀层;增强体碳纤维表面的化学吸附和物理吸附是产生化学镀镍催化活性点的主要原因。Cf/Al复合材料表面预镀的化学镀镍层高的耐蚀性,一方面是镀层含有非晶体成分,腐蚀敏感的晶界少;另一方面,Ni-P镀层减缓了腐蚀介质对Cf/Al复合材料的之间接触,两者协同作用使Cf/Al复合材料耐蚀性大大提高。
化学镀镍和稀土膜层的复合提高了耐蚀膜层的致密性,Ni-P/稀土多层膜微裂纹很少,膜层均匀;电位-pH图结合XPS测试分析发现,Ni-P/稀土多层膜外层稀土化合物的化合价态以Ce4+为主要形式,Ni-P/稀土多层膜的非晶体特征更加明显,加之稀土化合物在化学镀镍膜层微孔处沉积,形成“封孔效应”,进一步提高了Cf/Al复合材料的耐蚀性。
全浸泡腐蚀试验可知,Ni-P/稀土多层膜变化较少,腐蚀程度最轻微;稀土膜层浸泡后膜层颜色变浅,膜层有脱落迹象;化学镀镍膜层腐蚀产物粘附较多;无膜层试样碳纤维的裸露严重。极化曲线对比表明,Ni-P/稀土多层膜处理后的试样腐蚀电势Ecorr相对于无膜层试样增大400mV以上,同时Ni-P/稀土多层膜试样的腐蚀电流密度比无膜层试样的腐蚀电流密度减小了1.32μA·cm-2。稀土膜层的极化曲线阴极分支和阳极分支同无膜层极化曲线相比,都向左移,其阳极反应和阴极反应均被抑制。交流阻抗谱解析结果表明,几种膜层的耐蚀性依次为Ni-P/稀土多层膜>化学镀镍膜层>稀土膜层>无膜层试样,Ni-P/稀土多层膜阻抗值最高,极化电阻为23051Ω,比无膜层试样增高8倍多。
化学镀镍及稀土膜层耐蚀性提高的原因来自膜层晶体结构含有非晶体成分或纳米微晶结构,对腐蚀反应不敏感,膜层阻挡了腐蚀的电化学反应路径。Ni-P/稀土多层膜耐蚀性提高除了化学镀镍膜层的因素外,稀土化合物在化学镀镍膜层微孔处沉积,形成“封孔效应”,并且其表面沉积稀土为Ce4+化合物,抗氧化性更强,从而使Cf/Al复合材料Ni-P/稀土多层膜的耐蚀性高于化学镀镍及单一稀土膜层。
In recent years, carbon fibers reinforced aluminum matrix (Cf/Al) composites are applied in some fields such as aerial material and space technology. It is important to improve corrosion resistance for this composite. For the purpose of improving corrosion resistance of Cf/Al composites, two coatings were prepared by rare earth conversion coating and Ce-rich complex films. The fabrication processes, microstructure and corrosion properties of two coatings were examined, their influencing factors were discussed, the deposition and corrosion resistance mechanics were studied in this paper.
It was found that the Ce conversion coating covered the whole surface of Cf/Al composites as oxidized islands, but some micro-cracks for the coating. The Ce conversion coating was island-like, and it was piled up by spherical Ce-riched particles. The size of Ce-riched particles was about 4nm~8nm, the multiple Ce-rich compounds were mixing in Ce-rich particles, and particles clustering. The thickness of Ce conversion coating is about 3μm, Ce oxides and Ce hydroxides are main composition of Ce conversion coating, which containing Ce3+ and Ce4+ compounds. The little Al compounds in this coating, it is indicated that Al dissolved during processes of formation films.
Uniform Ni-P coating on the surface of Cf/Al composites can be realized by electroless deposition, the catalytic active points for chemical deposition on the Al matrix promoted Ni-P deposition; chemical and physical absorption on the surface of carbon fibers were main reasons for catalytic active points in order to deposit Ni-P alloys. Improvement of corrosion resistance for Ni-P coatings on multi-phases surfaces of Cf/Al composites came from amorphous composition which has insensitive to corrosion reaction in Ni-P coatings, because there were less grain boundary in amorphous films. Moreover, Ni-P coatings can avoid direct touching between corrosion medium and surface of Cf/Al composites. Synergistic effect of them can improve corrosion resistance on Cf/Al composites.
Mechanism of rare earth conversion coating on multi-phases surface of Cf/Al composites is stated that“Mechanism of micro-cathodic deposition”was main factor on the Al matrix, on the other hand, chemical adsorption or physical adsorption was main formed Ce-rich coatings on surface of carbon fibers, therefore, the interactivity“Dangling bonds”on the surface of carbon fibers and“Surplus chemical bonds”belonged to rare earth elements had effect of depositing Ce-rich coating. The behavior of Ce compounds deposition occurred near defects of carbon surface and this characteristic could heal the scratch on carbon surface; this phenomenon can be named“self-healing”on the carbon surface.
The Ce-rich complex films are high condensing coatings which could obtain by Ni-P coatings with rare earth compounds sealing. There are few cracks in Ce-rich complex films and conforming layers. Image of potential-pH combined with XPS analysis can be indicated that the Ce4+ species were main components of Ce compounds in Ce-rich complex films. Microstructure characteristic of complex films is obvious a nano-crystal structure, additionally, the Ce compounds deposit on the sites of micro-porous on the Ni-P coatings,“sealing-effects”is main causes for improving corrosion resistance of Cf/Al composites.
The contrasts of microstructure characterization after immersion testing at the same conditions showed that the corrosion degree of complex films were slightly, the microstructure of coatings changed a little; the Ce conversion coatings had slight loss of color, some evidence supported the existence of coatings exfoliation; the more erosion products adhesive on the electroless plating Ni-P coatings; the carbon fibers had obvious bareness on uncoating samples. The corrosion potential (Ecorr) of complex films has improved more than 400mV as contrast on uncoating samples, the corrosion current density (icorr) of complex films have decreased 1.32μA·cm-2 than uncoating samples. The anodic and cathodic branches of polarization curves of Ce conversion coating were both decreased obviously, the corrosion reaction from anode and cathode were restrained at the same time.
The results of electrochemistry impedance spectra (EIS) indicated that the corrosion resistance of different coatings listed as follows: Complex films > Ni-P coatings > Ce conversion coatings > uncoatings. From EIS simply analysis, the impedance values of polarization resistance for complex films was 23051Ω, which improved 8 times than uncoating samples.
The main reasons for inhibition corrosion came from contents of amorphous structure in Ni-P coatings and rare earth conversion coatings, which structure is insensitive to corrosion reaction; in addition, the coatings inhibit electrochemical reaction. Ce-rich complex films have the best corrosion resistance because it has formed“sealing effects”. Moreover, Ce4+ species deposit surface of Ni-P coatings, there are better oxidation resistance of Ce4+ species than single Ce-rich coating and Ni-P coating.
引文
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