氯离子对热镀锌层在饱和Ca（OH）_2溶液中腐蚀行为的影响
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摘要
钢筋混凝土结构作为应用最为广泛的工程建筑材料之一,它的失效受到人们越来越多的关注。而钢筋混凝土的失效主要是由于埋入其中的钢筋骨架受到了环境中的侵蚀。钢筋腐蚀的介质是以饱和Ca(OH)_2为主的混凝土孔隙液。孔隙液中氯离子造成的点蚀破坏是引起钢筋腐蚀的主要原因之一。关于钢筋的保护,投入使用的有很多种措施,热镀锌作为一种良好的防腐蚀的方法,也有一定范围的应用。本文以热镀锌钢筋在混凝土环境中的应用为背景,探究了热镀锌钢在含不同氯离子浓度的饱和Ca(OH)_2溶液中的腐蚀行为。
在具体实验操作中,主要从热镀锌层对钢基的保护作用和氯离子对热镀锌钢的破坏作用两个方面出发,通过使用高倍率光学显微镜、扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)等仪器对试样表面的腐蚀产物进行各个倍数的形貌观察和结构、成分分析。采用塔菲尔动电位极化曲线(Tafel)和电化学阻抗谱(EIS)等测试了表面腐蚀产物对基体的保护作用,结合形貌图研究了腐蚀产物的结构和生长机理以及遭受到氯离子侵蚀情况下表面状态的变化及作用机制。研究结果表明:
热镀锌层在pH值=12.5的饱和Ca(OH)_2溶液中,表层首先会发生腐蚀并形成腐蚀小孔,锌的晶界是优先腐蚀部位;随后片状锌酸钙在小孔附近形核并逐渐长大。直至覆盖整个锌层表面。作为隔离锌层与腐蚀介质的物理屏障,锌酸钙与锌基体有着良好的粘附性,其覆盖程度决定了对基体的保护性能;随着锌酸钙的生长,覆盖程度增加,试样的自然腐蚀电位正移,EIS的低频端阻抗模值升高,自腐蚀电流减小;经过100h的浸泡,锌酸钙层接近完全覆盖后,自腐蚀电流降至临界钝化值10~(-1)μA/cm~2附近,锌层处于钝化状态。
在含氯离子的混凝土腐蚀环境下,Cl~-的存在会使得镀锌层上覆盖的锌酸钙产生破坏。由于锌酸钙片各自生长彼此连接的覆盖方式,在锌酸钙片的间隙中存在微小的区域,微区里存在着处在不同生长阶段的锌酸钙片或者裸露的锌层,这样锌酸钙保护能力较弱的区域为Cl~-的侵蚀创造了条件。电化学测试结果表明:对应于锌酸钙层受到Cl~-侵蚀的Cl~-浓度是有一定范围的,而且这个范围的氯离子浓度[Cl~-]在0.4mol/L～0.5mol/L之间,当[Cl~-]≤临界值时,钝化膜在锌酸钙保护力较弱的区域受到Cl~-的轻微点蚀,在局部微区生成腐蚀产物碱式氯化锌(ZnCl_2·4Zn(OH)_2·H_2O);另外,锌酸钙覆盖致密保护力较强的区域,不会受到Cl~-的点蚀作用,而且处于生长与溶解动态平衡的锌酸钙释放在表面附近的Ca~(2+)会与溶解在溶液中的CO_2气体反应生成CaCO_3沉积在表面。点蚀生成的具有局部连续性的碱式氯化锌、表面沉积的碳酸钙,连同大面积致密的锌酸钙,仍然可以对热镀锌层提供较好的保护。
当[Cl~-]≥临界值时,自腐蚀电流会超越临界钝化值10~(-1)μA/cm~2,镀锌层的腐蚀程度加剧,Cl~-对钝化膜的破坏由点蚀转变成局部腐蚀破坏:由于Cl~-浓度的增大,在锌酸钙保护力较弱的区域生成的大量的碱式氯化锌,松散堆积的碱式氯化锌与镀层表面结合不紧密,易碎裂脱落,无法体现其微区的保护性能。碱式氯化锌脱落后露出的ZnO基体与周围锌酸钙保护力较强的区域相邻连接但呈现层次, Cl~-通过断层会扩散到锌酸钙底部,并逐渐瓦解锌酸钙致密的结构,从而扩大对镀锌层的侵蚀进而破坏基体金属。
总体上讲,由于在碱性环境中生成致密的锌酸钙覆盖层能有效的延缓氯离子对热镀锌层的侵蚀,并且热镀锌层在自身遭到腐蚀以后可以提供有效的牺牲阳极保护,因而热镀锌防护是一种优良的钢筋防腐蚀方法。
As the most widely used construction materials, the reinforced concrete structure and its failure has attracted more and more attention. The main reason is the attack from the surroundings suffered by the rebars embedded in. One of the most serious attack is brought by the chloride ion. For the protection of rebars, there are already many ways have been taken into use, the galvanized steel ,as an efficient protective measure, also have a range of applications. In this paper, the corrosion behaviour of the galvanized steel in the saturated Ca(OH)_2 solution with different chloride ion has been investigated under the background of the application in the reinforced concrete structure of the galvanized steel.
In the experiment, two aspects ,of both the protection about the galvanizing layer for the steel matrix and the attack about the chloride ion for the protective layer which has grown on the surface of the galvanizing layer immersed in the saturated Ca(OH)_2 solution ,have been investigated. During the process of experiments, high magnification optical microscope, scanning electron microscopy(SEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD) have been used to observe the micro surface appearance under different magnification, study the corrosion products composites as well as various phases respectively. The electrochemical experiments were also employed to detect the protective behaviour of the surface corrosion product on the galvanizing layer via Tafel polarization curves and electrochemical impedance spectroscopy (EIS).The results of both the observation and electrochemical test data have helped to analyse the corrosion mechanism of the two aspects mentioned in the front parts of this passage. The analysed results have summarized as follows:
The saturated Ca(OH)_2 solution’s pH value is 12.5, immersed in which ,the galvanizing layer will be corroded that firstly the corrosion pit hole appears on the surface with a priority of the grain boundary ,then the corrosion product calcium hydroxyzincate (CaHZn) grows from the hole as a way of dense ,each sheet calcium hydroxyzincate connects with the adjacent one, and lastly all of the sheets cover the entire surface of the sample. As a physical barriers of chemical bond with matrix, has good adhesion to the zinc layer, and the percent of coverage area decides the protective property; With the growth of calcium hydroxyzincate ,the coverage area enlarges ,and then the self-corrosion potential shifts towards the positive direction , EIS of the low frequency impedance modulus value increases while the corrosion current decrease; After 100h-immersing, the self-corrosion current is reduced to the vicinity of the threshold value 10~(-1)μA/cm~2 ,the galvanizing layer is passivated then.
If the reinforced concrete structure works in corrosive environment, the existed Cl~- will drive the zinc layer covered with CaHZn to destruction. The way of Independent growing and connected with each other in which CaHZn protect the surface leaves some tiny region on it ,this region facilitated Cl~- to attack the coating. [Cl~-]≤0.5mol/L, the passive film is attacked a little by Cl~- in the weaker protective area with the corrosion product of alkali zinc chloride(ZnCl_2·4Zn(OH)_2·H_2O), while in stronger protective area , the passive film will not be corroded, besides , CaHZn in homeostasis state can release the surrounding Ca~(2+) which will react with the dissolved CO_2 gas to CaCO_3 deposit. The partial continuous ZnCl_2·4Zn(OH)_2·H_2O, surface deposit CaCO_3 ,as well as large area dense CaHZn ,can still provide good protection to the Zinc layer.
[Cl~-]≥0.5mol/L, the self-corrosion current will exceed the threshold value 10~(-1)μA/cm~2 , the corrosion of the surface become more severe, the pitting damage has converted to localized destruction: plenty of ZnCl_2·4Zn(OH)_2·H_2O has appeared because of much more Cl~-, the loose ZnCl2·4Zn(OH)_2·H2O don’t have close combination to the matrix, and easy to crack off that can not play the protective role as in small region. After the Spalling of ZnCl_2·4Zn(OH)_2·H_2O from the matrix .The ZnO layer has exposed out. ZnO layer is adjacent to the CaHZn nearby, however, the junction is not smooth but have gradation ,which can provide a guiding fast path to Cl~- underneath the CaHZn that is collapsed gradually, so the corrosion area is enlarged, and then the metal matrix has destructed.
In conclusion, as the dense CaHZn covered on the Zinc coating can efficiently delay the corrosion of Cl~- to the matrix, in addition ,the Zinc coating can still help to protect the steel as sacrificial anode, the galvanized steel deserve to be endowed as an efficient anti-corrosion methods.
在具体实验操作中,主要从热镀锌层对钢基的保护作用和氯离子对热镀锌钢的破坏作用两个方面出发,通过使用高倍率光学显微镜、扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)等仪器对试样表面的腐蚀产物进行各个倍数的形貌观察和结构、成分分析。采用塔菲尔动电位极化曲线(Tafel)和电化学阻抗谱(EIS)等测试了表面腐蚀产物对基体的保护作用,结合形貌图研究了腐蚀产物的结构和生长机理以及遭受到氯离子侵蚀情况下表面状态的变化及作用机制。研究结果表明:
热镀锌层在pH值=12.5的饱和Ca(OH)_2溶液中,表层首先会发生腐蚀并形成腐蚀小孔,锌的晶界是优先腐蚀部位;随后片状锌酸钙在小孔附近形核并逐渐长大。直至覆盖整个锌层表面。作为隔离锌层与腐蚀介质的物理屏障,锌酸钙与锌基体有着良好的粘附性,其覆盖程度决定了对基体的保护性能;随着锌酸钙的生长,覆盖程度增加,试样的自然腐蚀电位正移,EIS的低频端阻抗模值升高,自腐蚀电流减小;经过100h的浸泡,锌酸钙层接近完全覆盖后,自腐蚀电流降至临界钝化值10~(-1)μA/cm~2附近,锌层处于钝化状态。
在含氯离子的混凝土腐蚀环境下,Cl~-的存在会使得镀锌层上覆盖的锌酸钙产生破坏。由于锌酸钙片各自生长彼此连接的覆盖方式,在锌酸钙片的间隙中存在微小的区域,微区里存在着处在不同生长阶段的锌酸钙片或者裸露的锌层,这样锌酸钙保护能力较弱的区域为Cl~-的侵蚀创造了条件。电化学测试结果表明:对应于锌酸钙层受到Cl~-侵蚀的Cl~-浓度是有一定范围的,而且这个范围的氯离子浓度[Cl~-]在0.4mol/L～0.5mol/L之间,当[Cl~-]≤临界值时,钝化膜在锌酸钙保护力较弱的区域受到Cl~-的轻微点蚀,在局部微区生成腐蚀产物碱式氯化锌(ZnCl_2·4Zn(OH)_2·H_2O);另外,锌酸钙覆盖致密保护力较强的区域,不会受到Cl~-的点蚀作用,而且处于生长与溶解动态平衡的锌酸钙释放在表面附近的Ca~(2+)会与溶解在溶液中的CO_2气体反应生成CaCO_3沉积在表面。点蚀生成的具有局部连续性的碱式氯化锌、表面沉积的碳酸钙,连同大面积致密的锌酸钙,仍然可以对热镀锌层提供较好的保护。
当[Cl~-]≥临界值时,自腐蚀电流会超越临界钝化值10~(-1)μA/cm~2,镀锌层的腐蚀程度加剧,Cl~-对钝化膜的破坏由点蚀转变成局部腐蚀破坏:由于Cl~-浓度的增大,在锌酸钙保护力较弱的区域生成的大量的碱式氯化锌,松散堆积的碱式氯化锌与镀层表面结合不紧密,易碎裂脱落,无法体现其微区的保护性能。碱式氯化锌脱落后露出的ZnO基体与周围锌酸钙保护力较强的区域相邻连接但呈现层次, Cl~-通过断层会扩散到锌酸钙底部,并逐渐瓦解锌酸钙致密的结构,从而扩大对镀锌层的侵蚀进而破坏基体金属。
总体上讲,由于在碱性环境中生成致密的锌酸钙覆盖层能有效的延缓氯离子对热镀锌层的侵蚀,并且热镀锌层在自身遭到腐蚀以后可以提供有效的牺牲阳极保护,因而热镀锌防护是一种优良的钢筋防腐蚀方法。
As the most widely used construction materials, the reinforced concrete structure and its failure has attracted more and more attention. The main reason is the attack from the surroundings suffered by the rebars embedded in. One of the most serious attack is brought by the chloride ion. For the protection of rebars, there are already many ways have been taken into use, the galvanized steel ,as an efficient protective measure, also have a range of applications. In this paper, the corrosion behaviour of the galvanized steel in the saturated Ca(OH)_2 solution with different chloride ion has been investigated under the background of the application in the reinforced concrete structure of the galvanized steel.
In the experiment, two aspects ,of both the protection about the galvanizing layer for the steel matrix and the attack about the chloride ion for the protective layer which has grown on the surface of the galvanizing layer immersed in the saturated Ca(OH)_2 solution ,have been investigated. During the process of experiments, high magnification optical microscope, scanning electron microscopy(SEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD) have been used to observe the micro surface appearance under different magnification, study the corrosion products composites as well as various phases respectively. The electrochemical experiments were also employed to detect the protective behaviour of the surface corrosion product on the galvanizing layer via Tafel polarization curves and electrochemical impedance spectroscopy (EIS).The results of both the observation and electrochemical test data have helped to analyse the corrosion mechanism of the two aspects mentioned in the front parts of this passage. The analysed results have summarized as follows:
The saturated Ca(OH)_2 solution’s pH value is 12.5, immersed in which ,the galvanizing layer will be corroded that firstly the corrosion pit hole appears on the surface with a priority of the grain boundary ,then the corrosion product calcium hydroxyzincate (CaHZn) grows from the hole as a way of dense ,each sheet calcium hydroxyzincate connects with the adjacent one, and lastly all of the sheets cover the entire surface of the sample. As a physical barriers of chemical bond with matrix, has good adhesion to the zinc layer, and the percent of coverage area decides the protective property; With the growth of calcium hydroxyzincate ,the coverage area enlarges ,and then the self-corrosion potential shifts towards the positive direction , EIS of the low frequency impedance modulus value increases while the corrosion current decrease; After 100h-immersing, the self-corrosion current is reduced to the vicinity of the threshold value 10~(-1)μA/cm~2 ,the galvanizing layer is passivated then.
If the reinforced concrete structure works in corrosive environment, the existed Cl~- will drive the zinc layer covered with CaHZn to destruction. The way of Independent growing and connected with each other in which CaHZn protect the surface leaves some tiny region on it ,this region facilitated Cl~- to attack the coating. [Cl~-]≤0.5mol/L, the passive film is attacked a little by Cl~- in the weaker protective area with the corrosion product of alkali zinc chloride(ZnCl_2·4Zn(OH)_2·H_2O), while in stronger protective area , the passive film will not be corroded, besides , CaHZn in homeostasis state can release the surrounding Ca~(2+) which will react with the dissolved CO_2 gas to CaCO_3 deposit. The partial continuous ZnCl_2·4Zn(OH)_2·H_2O, surface deposit CaCO_3 ,as well as large area dense CaHZn ,can still provide good protection to the Zinc layer.
[Cl~-]≥0.5mol/L, the self-corrosion current will exceed the threshold value 10~(-1)μA/cm~2 , the corrosion of the surface become more severe, the pitting damage has converted to localized destruction: plenty of ZnCl_2·4Zn(OH)_2·H_2O has appeared because of much more Cl~-, the loose ZnCl2·4Zn(OH)_2·H2O don’t have close combination to the matrix, and easy to crack off that can not play the protective role as in small region. After the Spalling of ZnCl_2·4Zn(OH)_2·H_2O from the matrix .The ZnO layer has exposed out. ZnO layer is adjacent to the CaHZn nearby, however, the junction is not smooth but have gradation ,which can provide a guiding fast path to Cl~- underneath the CaHZn that is collapsed gradually, so the corrosion area is enlarged, and then the metal matrix has destructed.
In conclusion, as the dense CaHZn covered on the Zinc coating can efficiently delay the corrosion of Cl~- to the matrix, in addition ,the Zinc coating can still help to protect the steel as sacrificial anode, the galvanized steel deserve to be endowed as an efficient anti-corrosion methods.
引文
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[65] Oimellese M, Berra M, Bolzoni F. Corrosion inhibitors for chlorides induced corrosion in reinforced concrete structures[J] . Cement and concrete Research, 2006, 36(3): 536-547
[66] Carmen Andrade, Cruz Alonso. Galvanized steel reinforcement in concrete[M]. Oxford: Elsevier, 2004 : 113-119
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