CN108796571A - 一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法 - Google Patents
一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 66
- 239000002096 quantum dot Substances 0.000 title claims abstract description 60
- 238000000576 coating method Methods 0.000 title claims abstract description 54
- 239000011248 coating agent Substances 0.000 title claims abstract description 52
- 238000005260 corrosion Methods 0.000 title claims abstract description 35
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002444 silanisation Methods 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004070 electrodeposition Methods 0.000 claims abstract description 13
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 5
- 229940075397 calomel Drugs 0.000 claims abstract description 4
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 235000011164 potassium chloride Nutrition 0.000 claims abstract 2
- 239000001103 potassium chloride Substances 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 8
- 230000005611 electricity Effects 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 5
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical group CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 229940021013 electrolyte solution Drugs 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 210000004508 polar body Anatomy 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
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- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- LQHZJYFIRFRDKF-UHFFFAOYSA-N gold magnesium Chemical compound [Mg].[Au] LQHZJYFIRFRDKF-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
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- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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Abstract
本发明提供了一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，先以石墨烯量子溶液为电解质溶液，采用三电极系统，以镁合金为工作电极，饱和氯化钾/甘汞电极为参比电极，铂电极为辅助电极，在镁合金表面电化学沉积氮掺杂石墨烯量子点，然后将沉积的氮掺杂石墨烯量子点涂层放置在硅烷化溶液中，硅烷化处理的温度为40～55℃，硅烷化静置时间为1～2h，将经过硅烷化处理的镁合金干燥，即在镁合金的表面设置氮掺杂石墨烯量子点涂层。本发明通过在镁合金表面均匀电沉积氮掺杂石墨烯量子点，随后采用硅烷化处理提高镁合金和氮掺杂石墨烯量子点的结合力，在镁合金表面获得致密度高、结合紧密的氮掺杂石墨烯量子点涂层。
Description
技术领域
本发明属于化工领域，涉及一种金属表面处理技术，具体来说是一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法。
背景技术
镁具有密度低(其密度为1.74g/cm3，仅为铝的2/3和铁的1/4)的特点，并且镁合金比强度比刚度高，具有优良的电磁屏蔽性能和导热导电性能，被称为21世纪的绿色工程材料，在通讯电子汽车制造武器装备和航空航天等领域具有广阔应用前景。但是由于镁合金腐蚀性能差的特点，使得现在对镁合金表面防腐的研究体现的尤为重要。一般镁合金表面耐腐蚀涂层，会有磷酸盐涂层、微弧氧化涂层、超疏水涂层、石墨烯涂层等。在CorrosionScience期刊2016年一篇文献Composite magnesium phosphate coatings for improvedcorrosion resistance of magnesium AZ31alloy，通过化学沉积的方法，在镁合金表面形成磷酸盐涂层，很好的提高了镁合金的耐腐蚀性能。中国科学院长春应用化学研究所在2016年申请的一个专利：镁合金表面功能化石墨烯涂层及其制备方法(CN201610675476.4)，这篇专利就是通过镁合金表面功能化石墨烯涂层，很好地提高镁合金的耐腐蚀性能。
石墨烯量子点作为一种新型的零维石墨烯基材料，其尺寸在100纳米以下，由于其独特的物理化学性质，包括大表面积、低细胞毒性、优良的生物相容性、强量子限制和边缘效应，目前受到越来越多的关注。石墨烯量子点拥有一个石墨烯结构，这使得它们具有石墨烯的一些不寻常的性质。由于存在羟基、环氧和羰基，石墨烯量子点表现出与氧化石墨烯类似的性质；在这方面，石墨烯量子点是亲水的，有很强的溶解倾向，而p-p共轭键的存在为石墨烯量子点提供了粘结能力。
发明内容
针对现有技术中的上述技术问题，本发明提供了一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，所述的这种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法要解决现有技术中的镁合金表面的防腐蚀效果不佳的技术问题。
本发明提供了一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，先以石墨烯量子溶液为电解质溶液，采用三电极系统，以镁合金为工作电极，饱和氯化钾/甘汞电极为参比电极，铂电极为辅助电极，在镁合金表面电化学沉积氮掺杂石墨烯量子点，然后将沉积的氮掺杂石墨烯量子点涂层放置在硅烷化溶液中，硅烷化处理的温度为40～55℃，硅烷化静置时间为1～2h，将经过硅烷化处理的镁合金干燥，即在镁合金的表面设置氮掺杂石墨烯量子点涂层。
进一步的，所述电化学沉积电流为0.20～0.26A，电化学沉积时间为480～600s。
进一步的，所述硅烷化处理的溶液为甲基三甲氧基硅烷、无水乙醇与稀释剂，所述的甲基三甲氧基硅烷、无水乙醇与稀释剂的摩尔比为1:3:5至1:3:6。
进一步的，所述的稀释剂为水。
进一步的，所述的石墨烯量子溶液的浓度为8～15mg/mL。
本发明通过在镁合金表面均匀电沉积氮掺杂石墨烯量子点，随后采用硅烷化处理提高镁合金和氮掺杂石墨烯量子点的结合力，在镁合金表面获得致密度高、结合紧密的氮掺杂石墨烯量子点涂层。
本发明和已有技术相比，其技术进步是显著的。本发明把石墨烯量子点成功应用到耐腐蚀涂层当中，并很好地提高了耐腐蚀性能。本发明的操作步骤及设备要求简单，易于实现，具有氮掺杂石墨烯量子点涂层的自腐蚀电位比无涂层的镁合金的自腐蚀电位更高、自腐蚀电流更小，提高了镁合金的耐蚀性。
附图说明
图1为实施例1中氮掺杂石墨烯量子点涂层断口处扫描电子显微镜图。
图2为实施例1中氮掺杂石墨烯量子点涂层的极化曲线图。
图3位实施例2中氮掺杂石墨烯量子点涂层断口处扫描电子显微镜图。
图4为实施例2中氮掺杂石墨烯量子点涂层的极化曲线图。
具体实施方式
本发明所述的氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法不只局限于该具体实例，所有试验用AZ31镁合金试样。
实施例1
1)预处理，步骤如下：
将AZ31镁合金用砂纸进行打磨，抛光，超声清洗，随后用蒸馏水冲洗，无水乙醇超声清洗10min。
2)电沉积氮掺杂石墨烯量子点涂层：
利用CHI860D型电化学工作站，组装三电极体系，经步骤1)预处理后的AZ31镁合金为工作电极，铂电极为辅助电极，饱和甘汞电极为参比电极。取10mg/mL的氮掺杂石墨烯量子点溶液100ml，进行超声分散30分钟后作为电解质溶液。选择恒电流法，电流为0.26A，电沉积时间为10分钟。经电化学沉积后取出AZ31镁合金放置空间中干燥10分钟，得到AZ31镁合金表面氮掺杂石墨烯量子点涂层。
3)硅烷化处理：硅烷化处理的溶液为甲基三甲氧基硅烷、无水乙醇与稀释剂的摩尔比为1:3:5,将步骤2)得到的氮掺杂石墨烯量子点涂层的AZ31镁合金放置在硅烷化溶液中，硅烷化处理的温度为55℃，硅烷化静置时间为2h，将硅烷化处理的AZ31镁合金放置在60℃下干燥5h，即获得氮掺杂石墨烯量子点涂层。
与现有技术相比，本发明提供的一种氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，解决了氮掺杂石墨烯量子点均匀电沉积在镁合金表面，并且通过硅烷化处理，提高氮掺杂石墨烯量子点涂层与镁合金的结合力。
对本实施例制得的氮掺杂石墨烯量子点涂层进行电化学耐蚀性能测试，采用三电极体系，具体氮掺杂石墨烯量子点涂层的AZ31镁合金为工作电极，铂电极为辅助电极，饱和甘汞电极为参比电极，腐蚀介质为浓度为0.1mol/L氯化钠溶液。图1给出了氮掺杂石墨烯量子点截面扫描电子显微镜图，可以看出，涂层厚度约为23.90μm。图2给出了没有涂层的AZ31镁合金和表面具有氮掺杂石墨烯量子点涂层的AZ31镁合金的极化曲线。可以看出本实施例所获得的氮掺杂石墨烯量子点涂层的自腐蚀电位提高约0.1V，腐蚀电流密度下降了约2个数量级。
实施例2
1)预处理，步骤如下：
本实施例2所采用的试样材料为AZ31镁合金用2000#砂纸进行打磨，抛光，超声清洗，随后用蒸馏水冲洗，无水乙醇超声清洗15min。
2)电沉积氮掺杂石墨烯量子点涂层：
利用CHI860D型电化学工作站，组装三电极体系，经步骤1)预处理后的AZ31镁合金为工作电极，铂电极为辅助电极，饱和甘汞电极为参比电极，取10mg/mL的氮掺杂石墨烯量子点溶液100ml，进行超声分散30分钟后作为电解质溶液。选择恒电流法，电流为0.20A，电沉积时间为8分钟。经电化学沉积后取出AZ31镁合金放置空间中干燥15分钟，得到AZ31镁合金表面氮掺杂石墨烯量子点涂层。
3)硅烷化处理：硅烷化处理的溶液为甲基三甲氧基硅烷、无水乙醇与稀释剂的摩尔比为1:3:6,将步骤2)得到的氮掺杂石墨烯量子点涂层的AZ31镁合金放置在硅烷化溶液中，硅烷化处理的温度为40℃，硅烷化静置时间为1h，将硅烷化处理的AZ31镁合金放置在80℃下干燥8h，即获得氮掺杂石墨烯量子点涂层。
与现有技术相比，本发明提供的一种氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，解决了氮掺杂石墨烯量子点均匀电沉积在镁合金表面，并且通过硅烷化处理，提高氮掺杂石墨烯量子点涂层与镁合金的结合力。
对本实施例制得的氮掺杂石墨烯量子点涂层进行电化学耐蚀性能测试，采用三电极体系，带有涂层的AZ31镁合金为工作电极，铂电极为辅助电极，饱和甘汞电极为参比电极，腐蚀介质为浓度为0.1mol/L氯化钠溶液。图3给出了氮掺杂石墨烯量子点涂层截面扫描电子显微镜图，涂层厚度约为9.5μm。图4给出了没有涂层的AZ31镁合金和表面具有氮掺杂石墨烯量子点涂层的AZ31镁合金的极化曲线。可以看出本实施例所获得的氮掺杂石墨烯量子点涂层的自腐蚀电位提高约0.1V，腐蚀电流密度下降了约5个数量级，明显的提高了镁合金的耐蚀性能。
实施例结果表明，氮掺杂石墨烯量子点在耐蚀涂层方面具有很好的应用前景。
Claims (5)
1.一种采用氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，其特征在于：先以石墨烯量子溶液为电解质溶液，采用三电极系统，以镁合金为工作电极，饱和氯化钾/甘汞电极为参比电极，铂电极为辅助电极，在镁合金表面电化学沉积氮掺杂石墨烯量子点，然后将沉积的氮掺杂石墨烯量子点涂层放置在硅烷化溶液中，硅烷化处理的温度为40～55℃，硅烷化静置时间为1～2h，将经过硅烷化处理的镁合金干燥，即在镁合金的表面设置氮掺杂石墨烯量子点涂层。
2.据权利要求1所述的一种氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，其特征在于：所述电化学沉积电流为0.20～0.26 A，电化学沉积时间为480～600s。
3.根据权利要求1所述的一种氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，其特征在于：所述硅烷化处理的溶液为甲基三甲氧基硅烷、无水乙醇与稀释剂，所述的甲基三甲氧基硅烷、无水乙醇与稀释剂的摩尔比为1:3:5至1:3:6。
4.根据权利要求3所述的一种氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，其特征在于：所述的稀释剂为水。
5.根据权利要求1所述的一种氮掺杂石墨烯量子点涂层提高镁合金耐蚀性的方法，其特征在于：所述的石墨烯量子溶液的浓度为8~15mg/mL。
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