安宁-毕业论文 - 图文

化学沉积中磷含量Ni-W- P合金晶化

及耐蚀性研究

作 者 姓 名 安 宁 专 业 材料成型及控制工程06-1 指导教师姓名 刘 宏 专业技术职务 教 授

目 录

摘 要 ........................................................... 1

第一章 绪论 ............................................... 3

1.1 化学镀技术的研究及发展趋势 ................................ 3 1.1.1 化学镀的基本原理 .......................................... 3 1.1.2 化学镀镀液组成及作用 ..................................... 4 1.1.3 化学镀技术研究概述 ........................................ 6 1.1.4 化学镀技术在国内的发展 .............................. 8 1.1.5 化学镀技术的应用 .......................................... 9 1.1.6 化学镀的发展趋势 ......................................... 10 1.2 化学沉积层晶化转变机理 .................................... 11 1.3 企业设备腐蚀的现状及危害 .................................. 11 1.4 本文的目的、意义及研究内容 ............................... 12 1.4.1 研究目的及意义 ........................................... 12 1.4.2 研究内容 .................................................. 12

第二章 混晶态Ni-W-P合金镀层的制备与实验方法 .... 14 2.1 实验材料与仪器 ............................................. 14 2.2 化学镀镀液的组成及配制工艺 ............................... 14 2.2.1 化学镀镀液的组成 ......................................... 14 2.2.2 化学镀镀液的配制工艺 .................................... 14 2.3 实验方法 .................................................... 14 2.3.1 镀前处理 .................................................. 15 2.3.2 化学沉积过程 .............................................. 15 2.4 沉积层检测及性能测试 ...................................... 15 2.4.1 沉积层的结构测试 ......................................... 15 2.4.2 沉积层的形貌观察及成分测试 ............................. 16 2.4.3 沉积层耐蚀性能测试 ....................................... 17 2.4.4 热处理后沉积层的性能测试 ................................ 17

第三章 实验结果与分析 ................................. 19 3.1 化学沉积中磷含量Ni-W-P合金镀层的微观分析 .............. 19 3.1.1 镀层的X射线（XRD）衍射分析 .......................... 19 3.1.2 镀层热处理前后的表面形貌及成分分析 .................... 23 3.1.3 镀层的晶化过程及晶粒尺寸 ................................ 25 3.2 热处理前后镀层耐蚀性分析 .................................. 26

第四章 结论 .............................................. 28

参考文献 ........................................................ 29 致 谢 ........................................................... 31

山东轻工业学院2010届本科生毕业设计（论文）

摘 要

本文采用化学镀的方法制备了混晶态Ni-W-P合金镀层。通过扫描电镜（SEM）、能谱仪(EDS)及X射线衍射（XRD）法，分析研究了Ni-W-P合金镀层的微观组织结构、成分和形貌特征，并利用Jade软件对XRD衍射图谱进行晶粒尺寸计算。通过对Ni-W-P合金镀层进行腐蚀测试，研究了镀层热处理前后的耐蚀性能。旨在从Ni-W-P镀层宏观性能和微观组织的对比分析中获得两者之间的具体联系,从热处理的Ni-W-P合金沉积层结构、晶化程度、Ni及Ni3P晶粒尺寸及耐蚀性的变化中，探索Ni-W-P合金沉积层耐蚀性的影响机制，为研究材料的性能和组织的关系提供更详实的数据。其研究结果包括以下几个方面：

1. 化学沉积中磷含量（5.89%）的Ni-W-P合金镀层为混晶态结构，经热处理后逐

渐向稳定的晶态结构转变，形成含钨的Ni固溶体晶体和Ni3P组成的混合组织。 2. 在混晶态Ni-W-P合金镀层的晶化过程中，温度低于300℃时只有单一的Ni(W)

固溶体析出，其晶粒尺寸小于12.5nm；温度达到400℃直至500℃时，Ni3P开始析出，且Ni3P的晶粒尺寸大于Ni的晶粒尺寸；温度超过500℃时，析出物聚集粗化，Ni的晶粒尺寸反过来大于Ni3P的晶粒尺寸，但直到600℃时两相的晶粒尺寸仍保持在纳米级。

3. 混晶结构的镀态镀层耐蚀性最低，热处理温度低于300℃时，镀层的耐蚀性有

所提高。温度超过300℃直至500℃时，镀层的耐蚀性呈下降趋势。热处理温度高于500℃，则镀层的耐蚀性显著提高。

4. 化学沉积中磷含量Ni-W-P合金镀层的耐蚀性与镀层的组织结构、晶化程度、镀

层的应力，析出相的晶粒尺寸及其相对大小等因素有关。在400-500℃之间镀层的晶化过程中，所形成的Ni小Ni3P大的尺寸特征是影响镀层耐蚀性的重要因素。

关键词：化学镀 Ni-W-P合金镀层 混晶态 热处理 晶化 耐蚀性

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山东轻工业学院2010届本科生毕业设计（论文）

ABSTRACT

The electroless plating method was employed to plate Ni-W-P ternary mix-structure alloy on low carbon steel surface. Scanning electron microscope and laser microscope observations ,X-ray diffraction were performed to examine the microstructure(grain size)and phase composition of the coatings. And Jade software was used to calculate grain size. The corrosion resistance of the coating was estimated by 50%HNO3 solution immergence test. What had been done above was to obtain the relationship between the properties and microstructure of the coating and search the mechanism of corrosion resistance of Ni-W-P alloy coating by analysizing the Ni-W-P alloy deposition layer structure ,degree of crystallization, the grain size of Ni and Ni3P. What had studied in this paper can provide more detailed datas and theories for our study of the relationship between the properties and microstructure of the materials.The results were as follows:

As-plated Ni-W-P alloy coating with P content 5.89％has mixture of nanocrystalline and amorphous structure. After heat treatment, the Ni-W-P alloy deposition layer structure has gradually transmitted into crystalline structure, forming Ni and Ni3P after crystallization.

1. In the process of crystallization of the mix-structure Ni-W–P alloy, when the

teampreature was lower than 300℃, it had only Ni(W) solid solution, its grain size was smaller than 12.5nm;further heating until 500℃, Ni3P existed in the coating, its grain size was bigger than that of Ni; when the teampreature higher than 500℃, Ni3P began to coarsen, in turn, the grain size of Ni was bigger than that of Ni3P. Until 600℃, the grain size of Ni and Ni3P remained nanocrystalline. 2. The corrosion resistance of as-plated Ni-W-P alloy coating with mix-structure

was worst. When the heat treatment teampreature was lower than 300℃, the corrosion resistance of the alloy increased slightly, between 300℃ and 500℃, it decreased; when higher than 500℃, it increased dramatically.

3. The deposition layer structure, degree of crystallization, stress, the grain size of

Ni and Ni3P had great effect on the corrosion resistance of the alloy. When heat treatment teampreature between 400℃and 500℃, the grain size of Ni was smaller than that of Ni3P. This is a significant factor for its corrosion resistance.

Key words：electroless plating; Ni-W–P alloy coating; mix-structure; heat treatment; crystallization; corrosion resistance

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