不同酸掺杂聚苯胺—环氧涂层对几种金属防腐性能的影响
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摘要
本文选用化学氧化法合成本征态聚苯胺及盐酸掺杂、樟脑磺酸掺杂及氢氟酸掺杂聚苯胺，并用FTIR、XRD及四探针方法对合成的聚苯胺粉末进行表征。结果表明，通过化学氧化法成功合成了本征态聚苯胺及酸掺杂态聚苯胺，酸的主要掺杂部位在醌式结构的氮原子上；经过酸掺杂后，提高了聚苯胺的结晶度和电导率，其中氢氟酸掺杂聚苯胺的电导率较高。
将合成的聚苯胺粉末添加在环氧树脂中，在碳钢、纯铝及铝合金、镁合金表面制备成涂层，在3.5%NaCl溶液中用EIS研究聚苯胺涂层对几种金属的防护性能，用LEIS研究带缺陷的聚苯胺涂层的防护性能。对浸泡后涂层下的金属进行宏观及SEM观察，研究发现：
（1）碳钢表面的环氧清漆涂层在浸泡100天后，阻抗值降低至10~6Ω·cm~2以下，涂层失去了保护作用。而在浸泡175天后，本征态聚苯胺涂层的阻抗值在10~7Ω·cm~2，酸掺杂聚苯胺涂层的阻抗值仍在10~8Ω·cm~2，表明涂层仍有较好的防护作用。其中樟脑磺酸掺杂聚苯胺涂层的阻抗值略高于其它涂层的。经过400天浸泡后，环氧清漆涂层下的碳钢发生了非常严重的腐蚀，并有大量的疏松的产物形成，酸掺杂聚苯胺涂层下的碳钢表面发生了丝状腐蚀，但在腐蚀处形成了一层致密的、连续的产物膜。
（2）纯铝及铝合金表面的环氧清漆涂层分别在浸泡100天和30天后，涂层的阻抗值降低到10~7Ω·cm~2，而此时在两金属基体上的本征态聚苯胺涂层阻抗值仍大于10~8Ω·cm~2。在浸泡215天后，在纯铝及铝合金表面的酸掺杂聚苯胺涂层阻抗值仍维持在10~8Ω·cm~2~109·cm~2，表明涂层对纯铝及铝合金有较好的防护作用，其中氢氟酸掺杂聚苯胺涂层的阻抗值略高于其它涂层的。此外铝合金表面带缺陷的氢氟酸掺杂聚苯胺涂层的阻抗值在浸泡过程中一直高于带缺陷的清漆及本征态聚苯胺涂层的。
（3）镁合金表面的环氧清漆涂层在浸泡42天后，涂层的阻抗值就降低到10~6Ω·cm~2，失去了保护作用。而浸泡400天后，本征态聚苯胺涂层的阻抗值仍在10~7Ω·cm~2，而酸掺杂聚苯胺涂层的阻抗值仍在10~8Ω·cm~2，表明对镁合金仍有较好的防护作用。其中氢氟酸掺杂聚苯胺涂层的阻抗值略高于其它涂层的。酸掺杂聚苯胺涂层下的镁合金表面形成一层非常致密、连续的产物膜。镁合金合金表面带缺陷的氢氟酸掺杂聚苯胺涂层的阻抗值在浸泡过程中一直高于带缺陷的清漆涂层的。
通过原位插层聚合法合成的聚苯胺/有机蒙脱土复合粉末延长了溶液的扩散通道，提高了涂层对侵蚀性离子的屏蔽作用，可以进一步提高聚苯胺涂层的防护性能。
通过综合对涂层的DSC测试、截面的SEM观察，以及聚苯胺涂层在有氧和除氧条件下的EIS测试，并对腐蚀产物膜进行EDS及XPS分析，得出聚苯胺的防护机理为：
（1）聚苯胺的加入提高了涂层的交联密度，在环氧涂层中具有良好的分散性，提高了涂层的屏蔽性能。
（2）氧气参与了聚苯胺的氧化还原作用，使金属表面形成具有保护作用的产物膜。而在无氧条件下聚苯胺涂层的防护性能迅速降低。因此，聚苯胺的氧化还原反应是聚苯胺最主要的防护机理。
（3）酸掺杂提高了涂层的电导率，加速了聚苯胺的成膜过程；掺杂阴离子伴随着聚苯胺的氧化还原过程释放出来，在金属表面与金属形成络合物或不溶物，从而进一步提高了涂层的防护性能。
The emeraldine base polyaniline (PANI) and hydrochloric acid (HCl), camphorsulfonic acid (CSA) and hydrofluoric acid (HF) doped PANI were synthesised by chemicaloxidation method and characterized by FTIR, XRD and four-probe measurements. Theresults of FTIR indicated that the synthesized powders were PANI in emeraldine state oracid doped state. The acid doped location was mainly on nitrogen atoms in the quinoid ringsrather than in the benzenoid ring of PANI. The results of XRD indicated that the crystaldegree of PANI powders was low. The crystal degree and the conductivity of PANI wereincreased by the acid doped anoins. The hydrofluoric acid doped PANI has the highestconductivity among four kinds of PANI powders.
The epoxy resin coatings containing different PANI powders were prepared on thesurface of steel, pure aluminum, aluminum alloy and magnesium alloy. Corrosionprotection of PANI coatings for several metals was studied by EIS in3.5%NaCl solution.The LEIS was used to study the corrosion protection of defected PANI coatings. The metalsurface beneath coatings was observed by the camera and SEM after immersion. The resultswere as follows:
(1)The impedance values of varnish coating on the surface of carbon steel were lessthan10~6Ω·cm~2after100day immersion, which indicated that the coating lost itsanticorrosion properties. After175day immersion, the impedance values of emeraldinebase PANI and acid doped PANI coatings was10~7Ω·cm~2and10~8Ω·cm~2, respectively. Theresults indicated that PANI coating showed high anticorrosion properties. The impedancevalues of CSA doped PANI coating were higher than that of other coatings. After400dayimmersion, lots of pit corrosion and loose corrosion product were formed on the surface ofcarbon steel beneath epoxy varnish. The carbon steel surface beneath acid doped PANIcoating was predominated by filiform corrosion, but a compact and continuous productlayer was detected on the corrosion spots.
(2) The impedance values of varnish coating on the surface of pure aluminium andaluminium alloy were10~7Ω·cm~2after100day immersion and30day immersion,respectively. But the impedance values of emeraldine base PANI were above10~8Ω·cm~2.The impedance values of acid doped PANI coating maintained10~8Ω·cm~2~109·cm~2after 215day immersion. The results indicated that acid doped PANI coating showed highcorrosion protection for pure aluminium and aluminium alloy. The impedance values of HFdoped PANI coating were higher than that of other coatings. The impedance values ofdefected HF acid doped PANI coating on the surface of aluminium alloy were higherthan that of defected emeraldine base PANI coating and defected epoxy varnish coatingduring all immersion time.
(3) The impedance values of varnish coating on the surface of magnesium alloy were10~6Ω·cm~2after42day immersion, which indicated that coating lost its anticorrosionproperties. After400day immersion, the impedance values of emeraldine base PANIcoating and acid doped PANI coating were10~7Ω·cm~2and10~8Ω·cm~2, respectively. Theresults indicated that PANI coating showed high anticorrosion properties. The impedancevalues of HF doped PANI coating were higher than that of other coatings. Compactprotective layer was formed on the surface of magnesium alloy beneath PANI coating. Theimpedance values of defected HF acid doped PANI coating on the surface ofmagnesium alloy were higher than that of defected epoxy varnish coating during allimmersion time.
The polyaniline/organophilic montmorillonite (PANI/OMMT) compound powderswhich were synthesized via in-situ emulsion polymerization increased the tortuosity of thediffusion pathways and improved the barrier properties to the electrolyte solution. Therefore,the corrosion protective properties of PANI coating was improved.
The corrosion protection mechanisms of PANI coating were discussed by the analysisof DSC and SEM of coating, EIS measurements of coatings in deaerated or aerated3.5%NaCl solution, and the SEM, EDS and XPS analyses of the surface of metal beneathcoatings after immersion experiments. The result indicated:
(1) The barrier properties of coating were improved because of the increaseing ofcrosslink density by the addition of PANI powders.
(2) The compact protective layer was formed by the reduction-oxidation reaction ofPANI in the case of oxygen presence. The corrosion protection of PANI decreased rapidly inthe solution without O2. Therefore, the main protection mechanism of PANI coating wasreduction-oxidation reaction of PANI.
(3) The formative speed of protective layer was improved by increased conductance ofacid doped PANI. The doped anions released concomitant redox reaction of PANI andformed protective layer with metal ions. Therefore, the protective effect of coating wasimproved.
将合成的聚苯胺粉末添加在环氧树脂中，在碳钢、纯铝及铝合金、镁合金表面制备成涂层，在3.5%NaCl溶液中用EIS研究聚苯胺涂层对几种金属的防护性能，用LEIS研究带缺陷的聚苯胺涂层的防护性能。对浸泡后涂层下的金属进行宏观及SEM观察，研究发现：
（1）碳钢表面的环氧清漆涂层在浸泡100天后，阻抗值降低至10~6Ω·cm~2以下，涂层失去了保护作用。而在浸泡175天后，本征态聚苯胺涂层的阻抗值在10~7Ω·cm~2，酸掺杂聚苯胺涂层的阻抗值仍在10~8Ω·cm~2，表明涂层仍有较好的防护作用。其中樟脑磺酸掺杂聚苯胺涂层的阻抗值略高于其它涂层的。经过400天浸泡后，环氧清漆涂层下的碳钢发生了非常严重的腐蚀，并有大量的疏松的产物形成，酸掺杂聚苯胺涂层下的碳钢表面发生了丝状腐蚀，但在腐蚀处形成了一层致密的、连续的产物膜。
（2）纯铝及铝合金表面的环氧清漆涂层分别在浸泡100天和30天后，涂层的阻抗值降低到10~7Ω·cm~2，而此时在两金属基体上的本征态聚苯胺涂层阻抗值仍大于10~8Ω·cm~2。在浸泡215天后，在纯铝及铝合金表面的酸掺杂聚苯胺涂层阻抗值仍维持在10~8Ω·cm~2~109·cm~2，表明涂层对纯铝及铝合金有较好的防护作用，其中氢氟酸掺杂聚苯胺涂层的阻抗值略高于其它涂层的。此外铝合金表面带缺陷的氢氟酸掺杂聚苯胺涂层的阻抗值在浸泡过程中一直高于带缺陷的清漆及本征态聚苯胺涂层的。
（3）镁合金表面的环氧清漆涂层在浸泡42天后，涂层的阻抗值就降低到10~6Ω·cm~2，失去了保护作用。而浸泡400天后，本征态聚苯胺涂层的阻抗值仍在10~7Ω·cm~2，而酸掺杂聚苯胺涂层的阻抗值仍在10~8Ω·cm~2，表明对镁合金仍有较好的防护作用。其中氢氟酸掺杂聚苯胺涂层的阻抗值略高于其它涂层的。酸掺杂聚苯胺涂层下的镁合金表面形成一层非常致密、连续的产物膜。镁合金合金表面带缺陷的氢氟酸掺杂聚苯胺涂层的阻抗值在浸泡过程中一直高于带缺陷的清漆涂层的。
通过原位插层聚合法合成的聚苯胺/有机蒙脱土复合粉末延长了溶液的扩散通道，提高了涂层对侵蚀性离子的屏蔽作用，可以进一步提高聚苯胺涂层的防护性能。
通过综合对涂层的DSC测试、截面的SEM观察，以及聚苯胺涂层在有氧和除氧条件下的EIS测试，并对腐蚀产物膜进行EDS及XPS分析，得出聚苯胺的防护机理为：
（1）聚苯胺的加入提高了涂层的交联密度，在环氧涂层中具有良好的分散性，提高了涂层的屏蔽性能。
（2）氧气参与了聚苯胺的氧化还原作用，使金属表面形成具有保护作用的产物膜。而在无氧条件下聚苯胺涂层的防护性能迅速降低。因此，聚苯胺的氧化还原反应是聚苯胺最主要的防护机理。
（3）酸掺杂提高了涂层的电导率，加速了聚苯胺的成膜过程；掺杂阴离子伴随着聚苯胺的氧化还原过程释放出来，在金属表面与金属形成络合物或不溶物，从而进一步提高了涂层的防护性能。
The emeraldine base polyaniline (PANI) and hydrochloric acid (HCl), camphorsulfonic acid (CSA) and hydrofluoric acid (HF) doped PANI were synthesised by chemicaloxidation method and characterized by FTIR, XRD and four-probe measurements. Theresults of FTIR indicated that the synthesized powders were PANI in emeraldine state oracid doped state. The acid doped location was mainly on nitrogen atoms in the quinoid ringsrather than in the benzenoid ring of PANI. The results of XRD indicated that the crystaldegree of PANI powders was low. The crystal degree and the conductivity of PANI wereincreased by the acid doped anoins. The hydrofluoric acid doped PANI has the highestconductivity among four kinds of PANI powders.
The epoxy resin coatings containing different PANI powders were prepared on thesurface of steel, pure aluminum, aluminum alloy and magnesium alloy. Corrosionprotection of PANI coatings for several metals was studied by EIS in3.5%NaCl solution.The LEIS was used to study the corrosion protection of defected PANI coatings. The metalsurface beneath coatings was observed by the camera and SEM after immersion. The resultswere as follows:
(1)The impedance values of varnish coating on the surface of carbon steel were lessthan10~6Ω·cm~2after100day immersion, which indicated that the coating lost itsanticorrosion properties. After175day immersion, the impedance values of emeraldinebase PANI and acid doped PANI coatings was10~7Ω·cm~2and10~8Ω·cm~2, respectively. Theresults indicated that PANI coating showed high anticorrosion properties. The impedancevalues of CSA doped PANI coating were higher than that of other coatings. After400dayimmersion, lots of pit corrosion and loose corrosion product were formed on the surface ofcarbon steel beneath epoxy varnish. The carbon steel surface beneath acid doped PANIcoating was predominated by filiform corrosion, but a compact and continuous productlayer was detected on the corrosion spots.
(2) The impedance values of varnish coating on the surface of pure aluminium andaluminium alloy were10~7Ω·cm~2after100day immersion and30day immersion,respectively. But the impedance values of emeraldine base PANI were above10~8Ω·cm~2.The impedance values of acid doped PANI coating maintained10~8Ω·cm~2~109·cm~2after 215day immersion. The results indicated that acid doped PANI coating showed highcorrosion protection for pure aluminium and aluminium alloy. The impedance values of HFdoped PANI coating were higher than that of other coatings. The impedance values ofdefected HF acid doped PANI coating on the surface of aluminium alloy were higherthan that of defected emeraldine base PANI coating and defected epoxy varnish coatingduring all immersion time.
(3) The impedance values of varnish coating on the surface of magnesium alloy were10~6Ω·cm~2after42day immersion, which indicated that coating lost its anticorrosionproperties. After400day immersion, the impedance values of emeraldine base PANIcoating and acid doped PANI coating were10~7Ω·cm~2and10~8Ω·cm~2, respectively. Theresults indicated that PANI coating showed high anticorrosion properties. The impedancevalues of HF doped PANI coating were higher than that of other coatings. Compactprotective layer was formed on the surface of magnesium alloy beneath PANI coating. Theimpedance values of defected HF acid doped PANI coating on the surface ofmagnesium alloy were higher than that of defected epoxy varnish coating during allimmersion time.
The polyaniline/organophilic montmorillonite (PANI/OMMT) compound powderswhich were synthesized via in-situ emulsion polymerization increased the tortuosity of thediffusion pathways and improved the barrier properties to the electrolyte solution. Therefore,the corrosion protective properties of PANI coating was improved.
The corrosion protection mechanisms of PANI coating were discussed by the analysisof DSC and SEM of coating, EIS measurements of coatings in deaerated or aerated3.5%NaCl solution, and the SEM, EDS and XPS analyses of the surface of metal beneathcoatings after immersion experiments. The result indicated:
(1) The barrier properties of coating were improved because of the increaseing ofcrosslink density by the addition of PANI powders.
(2) The compact protective layer was formed by the reduction-oxidation reaction ofPANI in the case of oxygen presence. The corrosion protection of PANI decreased rapidly inthe solution without O2. Therefore, the main protection mechanism of PANI coating wasreduction-oxidation reaction of PANI.
(3) The formative speed of protective layer was improved by increased conductance ofacid doped PANI. The doped anions released concomitant redox reaction of PANI andformed protective layer with metal ions. Therefore, the protective effect of coating wasimproved.
引文
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