CN113668031A - 一种在铝合金阳极氧化表面电沉积Ce-MOFs耐腐蚀膜层的制备方法 - Google Patents
一种在铝合金阳极氧化表面电沉积Ce-MOFs耐腐蚀膜层的制备方法 Download PDFInfo
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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Abstract
本发明公开了一种在铝合金阳极氧化表面电沉积Ce‑MOFs耐腐蚀膜层的制备方法。首先通过打磨，除油等前处理操作铝合金基体，然后在一定条件下进行阳极氧化。最后以一定比例配置MOFs电沉积溶液，在恒定电压和温度下进行电沉积反应，得到均匀致密的Ce‑MOFs耐腐蚀膜层。本发明制备工艺绿色环保，操作方法简单。该膜层具有较高的电化学阻抗，较低的腐蚀电流密度，并具有一定疏水性，能较好的提高铝合金的耐腐蚀性能。
Description
技术领域
本发明涉及铝合金金属有机骨架MOFs表面研究领域，特别涉及一种制备铝合金表面Ce-MOFs耐腐膜层的方法。
背景技术
金属有机骨架(Metal-Organic Frameworks，MOFs)材料又称为多孔配位聚合物(Porous Coordination Polymer,PCP)，金属有机框架化合物是主要由含N、O、S的有机配体和金属离子组成，其结构通过配位反应构筑。温度、金属离子与配体摩尔比，反应体系的浓度值，反应溶剂，反应时间等因素不同，都将影响金属有机框架化合物的结构。因而金属有机框架化合物具有多样化的零维笼状、一维链状，二维层状和三维框架结构。并且其结构具有高的比表面积、优良的化学稳定性、热稳定性、大的孔隙率、孔道尺寸均匀且多样、以及仿生催化特性和生物兼容性等特点。比如MOF-177，其孔隙率达到了83％，BET比表面积高达3780m2/g。MOF-200，其孔隙率高达90％，BET比表面积为4530m2/g。Cu2(TMA)2(H2O)2等的孔径为31nm，HKUST-1的介孔孔径为3.9nm。因此金属有机框架化合物被广泛用于储氢和二氧化碳的吸附、电气应用、药物的释放、金属防腐等领域。
现有技术公开了多种MOFs膜层的制备方法，但多数方法制备的MOFs膜层制备过程对环境不够友好，操作复杂，且稳定性不足，效果欠理想。为此，开发一种铝合金表面电沉积MOFs膜的制备方法尤为必要。
发明内容
本发明的目的是提供一种在铝合金阳极氧化表面电沉积Ce-MOFs耐腐蚀膜层的制备方法。
步骤为：
将6061铝合金切割为3mm×15mm×25mm的长方体薄片。采用180#，600#，1000#的砂纸沿一个方向依次打磨铝合金至表面较为光滑，且呈现出光亮的金属光泽同时无明显的划痕，去除覆盖在铝合金表面的自然氧化膜、油污及其他杂质，再用蒸馏水反复冲洗打磨的铝合金并放入鼓风干燥箱烘干。称取0.5-1g硅酸钠和1-2g磷酸钠放入烧杯中，然后量取50-100ml蒸馏水，混合配置除油液。将除油液放入60-80℃的水浴锅中加热，再将前面处理好的铝合金片放入除油液中，浸泡1-5min，进行除油。随后用乙醇和蒸馏水超声冲洗干净后放入50-80℃的鼓风干燥箱进行烘干。
烘干期间称取2-4g氢氧化钠溶于50-100mL蒸馏水配制成碱洗溶液，称取0.5-1mL硝酸溶于50-100mL蒸馏水配制成酸洗溶液，将烘干好的铝合金片在碱洗溶液中超声5-10min，取出立即用蒸馏水冲洗残留的碱洗液，然后再将铝合金片浸入到酸洗溶液中超声5-10min，取出立即用蒸馏水冲洗残留的酸洗液，最后浸入蒸馏水中超声5-10min，放在50-60℃烘箱中烘干以备下一步使用。
0.3M磷酸：0.3M草酸＝4-3：1-2(体积比)混合酸阳极氧化溶液：称取1.8-2g草酸溶于50-60mL蒸馏水配制成草酸溶液，在通风橱中量取2.5-3mL磷酸溶液，将磷酸用玻璃棒引流缓慢倒入140-150mL蒸馏水中，期间需不断搅拌，配制成磷酸溶液，将草酸溶液缓慢倒入磷酸溶液中并超声搅拌2-5min待用。使用直流电源装置，设置电压为50-60V，温度为20-25℃，以高纯铝箔做阴极，对前处理过后并干燥好的铝合金进行阳极氧化1.5-2h，随后蒸馏水冲洗残留在铝合金表面的阳极氧化溶液，并放入50-80℃烘箱中烘干待用。
称取1.5-2g均苯三甲酸(H3BTC)白色粉末并将其溶解在30-40mL的N,N-二甲基甲酰胺(DMF)中，溶解后的液体是无色透明溶液。称取2.5-3gCe(NO3)3·6H2O的无色透明晶体后溶解在30-40mL的去离子水中，溶解后的液体同样是无色透明液体。将H3BTC溶液缓慢到入Ce(NO3)3·6H2O溶液中，得到无色透明混合物液体，配置好电沉积液体。将阳极氧化后的铝片做阴极，石墨电极做阳极，温度25-30℃，电压15-20V，电沉积时间0.5-1h。后用蒸馏水冲洗并放入50-60℃烘箱中烘干待用。具体步骤为：
本发明方法制备工艺绿色环保，操作方法简单，且所制备铝合金阳极氧化表面电沉积Ce-MOFs膜层均匀致密。
附图说明
图1为本发明实施例中阳极氧化后电沉积Ce-MOFs的SEM图
图2为本发明实施例中样品的能谱图。
具体实施方式
实施例：
将6061铝合金切割为3mm×15mm×25mm的长方体薄片。采用180#，600#，1000#的砂纸沿一个方向依次打磨铝合金至表面较为光滑，且呈现出光亮的金属光泽同时无明显的划痕，去除覆盖在铝合金表面的自然氧化膜、油污及其他杂质，再用蒸馏水反复冲洗打磨的铝合金并放入鼓风干燥箱烘干。称取0.5g硅酸钠和2g磷酸钠放入烧杯中，然后量取50ml蒸馏水，混合配置除油液。将除油液放入80℃的水浴锅中加热，再将前面处理好的铝合金片放入除油液中，浸泡2min，进行除油。随后用乙醇和蒸馏水超声冲洗干净后放入50℃的鼓风干燥箱进行烘干。
烘干期间称取4g氢氧化钠溶于100mL蒸馏水配制成碱洗溶液，称取1.4mL硝酸溶于100mL蒸馏水配制成酸洗溶液，将烘干好的铝合金片在碱洗溶液中超声5min，取出立即用蒸馏水冲洗残留的碱洗液，然后再将铝合金片浸入到酸洗溶液中超声5min，取出立即用蒸馏水冲洗残留的酸洗液，最后浸入蒸馏水中超声5min，放在50℃烘箱中烘干以备下一步使用。
0.3M磷酸：0.3M草酸＝3：1(体积比)混合酸阳极氧化溶液：称取1.89g草酸溶于50mL蒸馏水配制成草酸溶液，在通风橱中量取2.6mL磷酸溶液，将磷酸用玻璃棒引流缓慢倒入150mL蒸馏水中，期间需不断搅拌，配制成磷酸溶液，将草酸溶液缓慢倒入磷酸溶液中并超声搅拌5min待用。使用直流电源装置，设置电压为60V，温度为25℃，以高纯铝箔做阴极，对前处理过后并干燥好的铝合金进行阳极氧化2h，随后蒸馏水冲洗残留在铝合金表面的阳极氧化溶液，并放入60℃烘箱中烘干待用。
称取1.5g H3BTC白色粉末并将其溶解在30mL的DMF中，溶解后的液体是无色透明溶液。称取3g Ce(NO3)3·6H2O的无色透明晶体后溶解在30mL的去离子水中，溶解后的液体同样是无色透明液体。将H3BTC溶液缓慢到入Ce(NO3)3·6H2O溶液中，得到无色透明混合物液体，配置好电沉积液体。将阳极氧化后的铝片做阴极，石墨电极做阳极，温度25℃，电压15v，电沉积时间1h。后用蒸馏水冲洗并放入60℃烘箱中烘干待用。从图1中可以看出复合膜层致密均匀，通过图2显示了各元素分布情况。
Claims (1)
1.一种在铝合金阳极氧化表面电沉积Ce-MOFs耐腐蚀膜层的制备方法，其特征在于具体步骤为：
将6061铝合金切割为3mm×15mm×25mm的长方体薄片；采用180#，600#，1000#的砂纸沿一个方向依次打磨铝合金至表面较为光滑，且呈现出光亮的金属光泽同时无明显的划痕，去除覆盖在铝合金表面的自然氧化膜、油污及其他杂质，再用蒸馏水反复冲洗打磨的铝合金并放入鼓风干燥箱烘干；称取0.5-1g硅酸钠和1-2g磷酸钠放入烧杯中，然后量取50-100ml蒸馏水，混合配置除油液；将除油液放入60-80℃的水浴锅中加热，再将前面处理好的铝合金片放入除油液中，浸泡1-5min，进行除油；随后用乙醇和蒸馏水超声冲洗干净后放入50-80℃的鼓风干燥箱进行烘干；
烘干期间称取2-4g氢氧化钠溶于50-100mL蒸馏水配制成碱洗溶液，称取0.5-1mL硝酸溶于50-100mL蒸馏水配制成酸洗溶液，将烘干好的铝合金片在碱洗溶液中超声5-10min，取出立即用蒸馏水冲洗残留的碱洗液，然后再将铝合金片浸入到酸洗溶液中超声5-10min，取出立即用蒸馏水冲洗残留的酸洗液，最后浸入蒸馏水中超声5-10min，放在50-60℃烘箱中烘干以备下一步使用；
0.3M磷酸：0.3M草酸＝4-3：1-2(体积比)混合酸阳极氧化溶液：称取1.8-2g草酸溶于50-60mL蒸馏水配制成草酸溶液，在通风橱中量取2.5-3mL磷酸溶液，将磷酸用玻璃棒引流缓慢倒入140-150mL蒸馏水中，期间需不断搅拌，配制成磷酸溶液，将草酸溶液缓慢倒入磷酸溶液中并超声搅拌2-5min待用；使用直流电源装置，设置电压为50-60V，温度为20-25℃，以高纯铝箔做阴极，对前处理过后并干燥好的铝合金进行阳极氧化1.5-2h，随后蒸馏水冲洗残留在铝合金表面的阳极氧化溶液，并放入50-80℃烘箱中烘干待用；
称取1.5-2g均苯三甲酸(H3BTC)白色粉末并将其溶解在30-40mL的N,N-二甲基甲酰胺(DMF)中，溶解后的液体是无色透明溶液；称取2.5-3g Ce(NO3)3·6H2O的无色透明晶体后溶解在30-40mL的去离子水中，溶解后的液体同样是无色透明液体；将H3BTC溶液缓慢到入Ce(NO3)3·6H2O溶液中，得到无色透明混合物液体，配置好电沉积液体；将阳极氧化后的铝片做阴极，石墨电极做阳极，温度25-30℃，电压15-20V，电沉积时间0.5-1h；后用蒸馏水冲洗并放入50-60℃烘箱中烘干待用。
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