论文中文题名: | 二亚硝基二氨铂的制备及镀铂工艺的研究 |
姓名: | |
学号: | 20213225054 |
保密级别: | 保密(2年后开放) |
论文语种: | chi |
学科代码: | 085600 |
学科名称: | 工学 - 材料与化工 |
学生类型: | 硕士 |
学位级别: | 工学硕士 |
学位年度: | 2023 |
培养单位: | 西安科技大学 |
院系: | |
专业: | |
研究方向: | 铂金属化合物材料 |
第一导师姓名: | |
第一导师单位: | |
论文提交日期: | 2023-06-27 |
论文答辩日期: | 2023-06-05 |
论文外文题名: | Preparation of Dinitrosodiammine Platinum and Study on Platinum Plating Process |
论文中文关键词: | |
论文外文关键词: | Dinitrodiamine Platinum ; Hydrothermal Process ; Platinum ; Platinum Electroplating ; Corrosion Resistance ; Electrochemistry |
论文中文摘要: |
铂是具有优异抗氧化性能和电催化性能的金属,尤其在阳极电化学析氧反应中,铂具有高电位、低腐蚀、高稳定性等优点。因此,铂在燃料电池、电极、催化剂、传感器等领域有着非常广泛的应用。但铂资源有限且开采困难,导致其价格十分昂贵。为解决这一问题,研究者们提出用镀铂材料替代纯铂材料这一方案,以降低成本并保持铂的良好性能。水溶液电镀铂是目前使用最广泛的电镀铂方式,优点在于效率高、镀层质量好、环保性能优良,是未来电镀铂的发展方向,其电镀主盐二亚硝基二氨铂是一种具有良好的电化学性能和稳定性的化合物,在电镀过程中具有高电化学活性和稳定性,可以提高电镀效率和质量。因此,研究二亚硝基二氨铂在电镀上的应用对于推动电镀技术的发展,提高电镀效率和质量,保护环境和人体健康以及促进经济发展具有重要意义。目前,电镀主盐二亚硝基二氨铂的高品质制备技术主要被欧美日等国家垄断,国内主要依靠进口,这一原因限制了其在电镀领域的发展。因此,本论文分别采用常温常压法与水热法在方案A、方案B两种制备条件下制备二亚硝基二氨铂,通过探究反应条件的不同,来寻求最佳制备条件,并对其作为主盐进行电镀实验,探究其电镀性能,达到提升电镀性能的目的,具体开展以下内容: (1)通过常温常压法在两种方案条件下制备出二亚硝基二氨铂,探究氨水添加温度(热浴下、冰浴下、室温下)、不同干燥条件(烘箱干燥、冷冻干燥)对制备二亚硝基二氨铂的影响,通过SEM、XRD、FT-IR 等表征手段研究材料的结构,在最佳防腐电镀工艺条件下,将制备出的二亚硝基二氨铂作为主盐进行电镀,得到镀铂层,并采用SEM、XRD、镀层结合力测试、Tafel、EIS 等手段评价不同镀铂层材料的物理化学性质和电化学性能影响。结果显示:方案A加热情况下添加氨水制备出的二亚硝基二氨铂产率最高,形貌更加均一。电化学研究表明,制备出的二亚硝基二氨铂作为主盐电镀的镀铂层具有更好的防腐蚀性能。方案B冷冻干燥制备出的二亚硝基二氨铂作为主盐电镀出的镀铂层具有更好的防腐蚀性能。 (2)进一步,通过水热法在两种制备方案下成功制备出二亚硝基二氨铂,同时探究不同水热条件对制备二亚硝基二氨铂的影响,通过SEM、XRD、FT-IR 等表征手段研究材料的结构,并采用SEM、XRD、镀层结合力测试、Tafel、EIS 等手段评价不同镀铂层材料的物理化学性质和电化学性能影响。结果显示:水热法下制备出的二亚硝基二氨铂结晶度远好于传统常温常压法,同时水热温度为160℃下制备出的样品其形貌最规整,结晶性最好,同时电镀其防腐性能最佳。 综上,在常温常压条件下合成的二亚硝基二氨铂具有较高的产率,而在水热条件下合成的二亚硝基二氨铂则表现出更好的结晶性,其样品形态也更加均匀规则。水热法是一种便捷、安全的制备高纯度、高结晶度二亚硝基二氨铂的功能材料开发扩展技术。 |
论文外文摘要: |
Platinum is a metal with excellent oxidation resistance and electrocatalytic performance, especially in the anode electrochemical oxygen evolution reaction, platinum has the advantages of high potential, low corrosion, high stability and so on. Therefore, platinum has a wide range of applications in fuel cells, electrodes, catalysts, sensors and other fields. However, platinum is a rare precious metal with limited resources and difficult exploitation, leading to its very high price. To solve this problem, the researchers proposed the idea of using platinum-plated materials instead of pure platinum materials to reduce costs and maintain the good performance of platinum anode. Aqueous solution electroplating platinum is the most widely used platinum plating method at present. Its advantages include high efficiency, good coating quality and excellent environmental protection performance, and it is the development direction of platinum plating in the future. The main salt of its plating, dinitrodiamine platinum, is a compound with good electrochemical performance and stability, with high electrochemical activity and stability, which can improve the plating efficiency and quality. Therefore, it is of great significance to study the application of dinitrodiamine platinum in electroplating to promote the development of electroplating technology, improve the efficiency and quality of electroplating, protect the environment and human health, and promote economic development. At present, the high quality preparation technology of dinitrodiamine platinum, the main salt of electroplating, is mainly monopolized by Europe, America, Japan and other countries, and the domestic mainly relies on imports, which restricts its development in the field of electroplating. Therefore, this paper adopts normal temperature and pressure method and hydrothermal method respectively to prepare dinitrodiamine platinum under the two preparation conditions of plan A and plan B. By exploring the difference in reaction conditions, the best preparation conditions are sought, and electroplating experiments are conducted on it as the main salt to explore its electroplating performance and achieve the purpose of improving. The following contents are specifically carried out: (1) Dinitrodiamine platinum was successfully prepared by normal temperature and pressure method under the conditions of two schemes. At the same time, the influence of different ammonia adding temperatures and different drying conditions on the preparation of dinitrodiamine platinum was explored. The structure of the material was studied by SEM, XRD, FT-IR and other characterization methods, and the best anticorrosive electroplating process was explored. Under the optimal conditions of anti-corrosion electroplating, the prepared dinitrodiamine platinum was used as the main salt for electroplating to obtain the platinized layer. The physicochemical properties and electrochemical properties of different platinized layer materials were evaluated by means of SEM, XRD, coating adhesion test, Tafel, EIS, etc. The results showed that under the condition of scheme A, the yield of dinitrodiamine platinum prepared by adding ammonia water under heating was the highest. At the same time, the morphology is more uniform. Electrochemical studies show that the prepared dinitrodiamine platinum as the main salt electroplating platinum layer has the best corrosion resistance. Under the condition of scheme B, the platinum layer prepared by freeze-drying as the main salt has the best anti-corrosion performance. (2) Further, dinitrodiamine platinum was successfully prepared by hydrothermal method under two preparation schemes. At the same time, the influence of different hydrothermal conditions on the preparation of dinitrodiamine platinum was explored. The structure of the material was studied by SEM, XRD, FT-IR and other characterization methods. The physicochemical properties and electrochemical properties of platinized materials were evaluated by means of SEM, XRD, coating adhesion test, Tafel and EIS. The results show that the crystallinity of dinitrodiamine platinum prepared by hydrothermal method is much better than that by traditional normal temperature and atmospheric pressure method. At the same time, the sample prepared at 160℃ hydrothermal temperature has the most regular morphology and the best crystallinity. At the same time, electroplating has the best corrosion resistance. In conclusion, dinitrodiamine platinum synthesized under normal temperature and pressure has higher yield, while dinitrodiamine platinum synthesized under hydrothermal conditions shows better crystallinity, and its sample morphology is more uniform and regular. Hydrothermal method is a convenient and safe development and expansion technology for the preparation of high purity and high crystallinity dinitrodiamine platinum functional materials. |
参考文献: |
[2]刘以柔, 黄安达, 高书刊, 等. 贵金属纳米复合材料的制备工艺及应用研究[J]. 热加工工艺, 2022, 51(20): 4. [15]何建平. 无氰电镀工艺的研究现状及解决问题的途径[J]. 电镀与涂饰, 2005, 24(7): 4. [17]杜继红, 李晴宇. 稀有金属表面电镀铂研究现状[J]. 贵金属, 2014, 004(004): 65-69, 74. [21]杨凡, 巩加芳, 郭乃华, 等. 一种水热制备立方体结构二亚硝基二氨铂的方法和应用, CN113979490A[P]. 2022. [22]巩加芳, 杨凡, 贾伟航, 等. 一种水热法制备球形二亚硝基二氨铂的方法和应用, CN114057242A[P]. 2022. [24]吴聪, 李治宇, 贺昕. 一种顺式二亚硝基二氨铂的制备方法. CN202211137784.3[P]. 2023. [27]徐明玥, 申兵伟, 王塞北, 等. 贵金属阳极材料的应用与研究进展[J]. 贵金属, 2022, 43(4):10. [30]叶小凤, 何援利, 付霞霏, 等. 骨髓间充质干细胞移植治疗顺铂致卵巢的化疗性损伤[J]. 中国组织工程研究, 2015, 19(10): 1597. [31]吴化平, 颉彦华, 赵其景, 等. 卵巢癌对顺铂耐药机制的研究进展[J]. 中国肿瘤临床, 2006, 33(021): 1256-1259. [32]周友珍, 陈惠祯, 杨庆忆, 等. 人卵巢癌顺铂耐药细胞株的建立及其耐药机制的研究[J]. 中华医学杂志, 1996, 76(9): 680-683. [33]洪祥乐. 金属钨表面电镀的研究[J]. 佛山科学技术学院学报: 自然科学版, 1999, 17(3): 1-5. [34]张玉萍, 鞠鹤, 武宏让, 等. 钛基镀铂工艺研究进展[J]. 钛工业进展, 2002 (2): 7-9. [35]林福文. 电镀铂的研究[J]. 材料开发与应用, 1992, 7(4): 26-30. [36]林华水, 陈华毅. 钛电极脉冲电镀铂及镀层性能[J]. 厦门大学学报: 自然科学版, 1992, 31(4): 379-382. [37]张玉萍, 鞠鹤, 武宏让, 等. 铂复合电极研究进展[J]. 表面技术, 2005, 34(5): 16-18. [39]Compton R G, Dai X. Electrochemical detection of arsenic: US08016998B2[P]. 2017 [41]汪欣, 李晴宇, 马秀芬, 等. 用于镍基高温合金表面电镀铂层的电镀液及其电镀方法, CN108130566A[P]. 2018. [42]何远怀, 周生刚, 竺培显, 等. 新型钛-铜基复合基体阳极的制备及性能研究[J]. 昆明理工大学学报: 自然科学版, 2015, 40(3): 5. [52]杨晓明. 血小板形态学分析[J]. 分子生物学方法,2013, 992: 207-25. [53]宋玉来. 纯铁液凝固形核机理和铁—氧化物界面结构研究[D]. 辽宁科技大学, 2016. [54]蔡文斌, 田中群. 铂电极表面拉曼增强因子的初步研究[C]. 第九届全国分子光谱学术报告会. 1996. [55]陈晓明. 电镀层的检测项目与检测标准汇总[J]. 表面技术, 2018, 2: 1-6. [56]陈晓明. 电镀基础知识之八: 影响镀层厚度分布均匀性的因素[N]. 表面技术网, 2019-12-04 [57]覃奇贤, 刘淑兰. 镀层与基体的结合力[J]. 电镀与精饰, 2010, 1: 3. [58]丁昊冬, 胡荣宗, 吴辉煌, 等. 碱性镀浴中钛基体化学镀铂的研究[J]. 材料保护, 2008, 41(5): 29-32. [60]姜义, 王久胜, 李雪松. 工艺参数对 Ni-Fe-Co 三元合金镀层形貌及耐蚀性的影响[J]. 电镀与环保, 2015, 35(6): 5-7. [61]张进红, 林启美, 赵小蓉, 等. 水热炭化温度和时间对鸡粪生物质炭性质的影响[J]. 农业工程学报, 2015, 24: 6. [62]刘爽, 刘俊刚, 杨家德, 等. 常规XRD对超薄PtSi/Si膜的表征技术的研究[J]. 半导体光电, 1999, 4: 285-288. [63]李美芬, 曾凡桂, 齐福辉, 等. 不同煤级煤的Raman谱特征及与XRD结构参数的关系[J]. 光谱学与光谱分析, 2009, 29(9): 4. [64]崔启明, 潘惟期, 王金城. 电沉积铂研究Ⅰ工艺条件与镀层性能[J]. 电镀与涂饰, 2005, 05: 1-5. [65]李向悦. 铝合金耐蚀复合涂层的制备与防护性能研究[D]. 华中科技大学, 2016. [67]黄佳妮, 潘锗航, 凌国平. 不锈钢氧化膜去除率及对铝镀层形貌的影响[J]. 材料科学与工程学报, 2021, 39(04): 615-621+691. [69]黄素清, 黄钊, 谷铁安, 等. 电镀铂/金的金电极上As 电化学行为的电化学石英晶体微天平研究[J]. 分析化学, 2011, 7: 978-984. [71]李强. 超声辅助喷射电沉积Ni-TiN纳米复合镀层的制备及表征[D]. 东北石油大学. [72]陈宏伟, 王建国, 张光辉, 等. 电沉积铂纳米线阵列及其催化性能[J]. 中国稀土学报, 2011, 29(3): 321-325. [73]刘冰洋, 周根树, 任颖, 等. 镀层厚度对铝基化学镀镍磷导电性和耐蚀性的影响[J]. 表面技术, 2020, 49(6): 8. [76]CAI W Y. A preparation method of dinitrodiaminoplatinum. CN102285693 A[P]. 2011. [77]金永中, 杨奎, 曾宪光, 等. 温度对化学镀 Ni-P 合金层形貌, 硬度及耐蚀性的影响[J]. 表面技术, 2015, 44(4): 23-26. |
中图分类号: | TQ183 |
开放日期: | 2025-06-28 |