氨基酸插层水滑石材料的制备及其缓蚀性能研究
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摘要
水滑石(LDHs)作为耐高温、耐辐射、抗老化性能良好的重要无机功能材料,在制备环境友好型缓蚀薄膜材料方面具有十分广阔的前景。目前水滑石薄膜在金属腐蚀与防护领域的应用研究尚处于起步阶段。
本论文旨在利用水滑石材料的特殊结构,将绿色缓蚀剂氨基酸插入水滑石层间,制备皆具水滑石和缓蚀剂优越性能的杂化材料。此类材料克服了常用腐蚀防护方法工艺复杂、污染环境和成本较高等缺点,保护环境的同时节约资金,具有重要的科学意义和实用价值。
首先采用共沉淀法,在弱碱性条件下将氨基酸类绿色缓蚀剂L-谷氨酸、L-天冬氨酸和L-色氨酸插入锌铝水滑石层间,制备氨基酸-LDHs杂化物。通过粉末X射线衍射(PXRD)、傅里叶变换红外光谱(FT-IR)对杂化物的结构进行表征。由PXRD可知,与前驱体水滑石层间距相比,杂化物的层间距明显增大,且003衍射峰向2θ小角度方向移动,说明氨基酸成功插入水滑石层间。杂化物的FT-IR图中也出现了氨基酸特征基团的吸收峰,进一步证明插层反应的成功。
将上述制备的氨基酸-LDHs杂化物通过胶体沉积技术在铜表面成膜,采用扫描电镜(SEM)对其表面形貌进行分析,结果表明,氨基酸-LDHs杂化物在铜表面形成了致密的薄膜。采用电化学阻抗谱(EIS)和极化曲线对铜表面的氨基酸-LDHs薄膜在NaCl溶液中的耐腐蚀性能进行评价,结果表明氨基酸-LDHs具有高的表面覆盖度和缓蚀效率。
最后通过浸泡实验,对氨基酸-LDHs的耐腐蚀机理进行了初步探讨。SEM结果表明,氨基酸-LDHs薄膜在NaCl溶液中浸泡24 h后,薄膜的表面形貌发生显著变化,由于电解质的浸泡,表面的氨基酸-LDHs片状结构排布不再致密。PXRD和能谱(EDS)结果表明浸泡后腐蚀性Cl-插入了水滑石层间,层间氨基酸含量减少,证明氨基酸-LDHs薄膜在腐蚀性介质中发生了离子交换反应。得出如下结论:一方面,溶液中腐蚀性离子Cl-的减少可以减缓介质对基底的腐蚀;另一方面,交换到溶液中的氨基酸也起到了腐蚀抑制作用,两方面的共同作用,使氨基酸-LDHs杂化物薄膜的缓蚀效率提高。
Layered Double Hydroxides (LDHs) are very important inorganic functional materials with high temperature resistance, radiation resistance and good anti-aging performance and they have an extremely good prospect in the preparation of environment-friendly inhibition film materials. Currently, the research of the application of LDHs films in metal corrosion and protection is still in initial stage.
In this study, amino acids, the environment-friendly corrosion inhibitor, were intercalated into LDHs by taking the advantage of the special structure of LDHs to prepare the hybrid materials with superior properties of both LDHs and inhibitors. They overcome the shortcoming of complexity, environmental pollution and high cost in common method of corrosion protection. This method has important scientific significance and practical value.
Firstly, the environment-friendly corrosion inhibitors, L-glutamic acid, L-aspartic acid and L-tryptophan, were intercalated into Zn-Al-LDHs by coprecipitation at alkaline condition. The structure of nanohybirds were characterized by PXRD and FT-IR. The PXRD patterns indicated that the basal spacing of the nanohybirds was obviously larger than pristine LDHs and 003 peak was shifted to the low 2θvalue, which indicated that the nanohybirds were formed by the intercalation of the amino acids into the Zn-Al-LDHs. The successful synthesis of the nanohybirds were also proved by the FT-IR spectra, which indicated the existence of characteristic groups of amino acids.
The nanohybirds were deposited on copper surface by colloid deposition method and the surface morphology was analyzed by scanning electron microscopy(SEM). The results showed that the amino acid-LDHs hybrid materials can form very impact and uniform films on copper surface. The quality and protection performance against corrosion to copper of hybrid films in the NaCl solution were characterized by electrochemical impedance spectroscopy (EIS) and polarization curves. The results showed that hybrid films have high surface coverage and inhibition efficiency.
Finally, the anticorrosion mechanism of amino acid-LDHs hybrid films was studied preliminary by immersion test. The result of SEM showed that the surface morphology of hybrid films changed significantly after the hybrid films were immersed in NaCl solution 24 h. The amino acid-LDHs sheets were not packed densely because of the penetration of NaCl solution into the internal films. The results of PXRD and EDS indicated that Cl- was intercalated into LDHs. It was revealed that NaCl solution penetrated into hybrid films and ion exchange reaction took place in the immersion process. The conclusions are as follows: on the one hand, the reducing of Cl - in the solution can slow down the corrosion of substrate. On the other hand, the release of amino acids from LDHs to solution also prevented the corrosion reaction. So the inhibition efficiency of amino acid-LDHs hybrids was improved.
本论文旨在利用水滑石材料的特殊结构,将绿色缓蚀剂氨基酸插入水滑石层间,制备皆具水滑石和缓蚀剂优越性能的杂化材料。此类材料克服了常用腐蚀防护方法工艺复杂、污染环境和成本较高等缺点,保护环境的同时节约资金,具有重要的科学意义和实用价值。
首先采用共沉淀法,在弱碱性条件下将氨基酸类绿色缓蚀剂L-谷氨酸、L-天冬氨酸和L-色氨酸插入锌铝水滑石层间,制备氨基酸-LDHs杂化物。通过粉末X射线衍射(PXRD)、傅里叶变换红外光谱(FT-IR)对杂化物的结构进行表征。由PXRD可知,与前驱体水滑石层间距相比,杂化物的层间距明显增大,且003衍射峰向2θ小角度方向移动,说明氨基酸成功插入水滑石层间。杂化物的FT-IR图中也出现了氨基酸特征基团的吸收峰,进一步证明插层反应的成功。
将上述制备的氨基酸-LDHs杂化物通过胶体沉积技术在铜表面成膜,采用扫描电镜(SEM)对其表面形貌进行分析,结果表明,氨基酸-LDHs杂化物在铜表面形成了致密的薄膜。采用电化学阻抗谱(EIS)和极化曲线对铜表面的氨基酸-LDHs薄膜在NaCl溶液中的耐腐蚀性能进行评价,结果表明氨基酸-LDHs具有高的表面覆盖度和缓蚀效率。
最后通过浸泡实验,对氨基酸-LDHs的耐腐蚀机理进行了初步探讨。SEM结果表明,氨基酸-LDHs薄膜在NaCl溶液中浸泡24 h后,薄膜的表面形貌发生显著变化,由于电解质的浸泡,表面的氨基酸-LDHs片状结构排布不再致密。PXRD和能谱(EDS)结果表明浸泡后腐蚀性Cl-插入了水滑石层间,层间氨基酸含量减少,证明氨基酸-LDHs薄膜在腐蚀性介质中发生了离子交换反应。得出如下结论:一方面,溶液中腐蚀性离子Cl-的减少可以减缓介质对基底的腐蚀;另一方面,交换到溶液中的氨基酸也起到了腐蚀抑制作用,两方面的共同作用,使氨基酸-LDHs杂化物薄膜的缓蚀效率提高。
Layered Double Hydroxides (LDHs) are very important inorganic functional materials with high temperature resistance, radiation resistance and good anti-aging performance and they have an extremely good prospect in the preparation of environment-friendly inhibition film materials. Currently, the research of the application of LDHs films in metal corrosion and protection is still in initial stage.
In this study, amino acids, the environment-friendly corrosion inhibitor, were intercalated into LDHs by taking the advantage of the special structure of LDHs to prepare the hybrid materials with superior properties of both LDHs and inhibitors. They overcome the shortcoming of complexity, environmental pollution and high cost in common method of corrosion protection. This method has important scientific significance and practical value.
Firstly, the environment-friendly corrosion inhibitors, L-glutamic acid, L-aspartic acid and L-tryptophan, were intercalated into Zn-Al-LDHs by coprecipitation at alkaline condition. The structure of nanohybirds were characterized by PXRD and FT-IR. The PXRD patterns indicated that the basal spacing of the nanohybirds was obviously larger than pristine LDHs and 003 peak was shifted to the low 2θvalue, which indicated that the nanohybirds were formed by the intercalation of the amino acids into the Zn-Al-LDHs. The successful synthesis of the nanohybirds were also proved by the FT-IR spectra, which indicated the existence of characteristic groups of amino acids.
The nanohybirds were deposited on copper surface by colloid deposition method and the surface morphology was analyzed by scanning electron microscopy(SEM). The results showed that the amino acid-LDHs hybrid materials can form very impact and uniform films on copper surface. The quality and protection performance against corrosion to copper of hybrid films in the NaCl solution were characterized by electrochemical impedance spectroscopy (EIS) and polarization curves. The results showed that hybrid films have high surface coverage and inhibition efficiency.
Finally, the anticorrosion mechanism of amino acid-LDHs hybrid films was studied preliminary by immersion test. The result of SEM showed that the surface morphology of hybrid films changed significantly after the hybrid films were immersed in NaCl solution 24 h. The amino acid-LDHs sheets were not packed densely because of the penetration of NaCl solution into the internal films. The results of PXRD and EDS indicated that Cl- was intercalated into LDHs. It was revealed that NaCl solution penetrated into hybrid films and ion exchange reaction took place in the immersion process. The conclusions are as follows: on the one hand, the reducing of Cl - in the solution can slow down the corrosion of substrate. On the other hand, the release of amino acids from LDHs to solution also prevented the corrosion reaction. So the inhibition efficiency of amino acid-LDHs hybrids was improved.
引文
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