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（题目）Ni-PTFE化学复合材料镀层的研究

（作者不用译）K. N. Srinivasan* S. John

摘要：镍基复合材料的化学镀层具有出色的摩擦行为。这些复合镀层的形成除了通过材料以粉末形式在化学镍溶液中共沉积和还要通过在沉积过程中的悬浮态下使之加入到镀层中。最常用的硬度高的弥散化合物是碳化硅，金刚石粉末，氧化铝，碳化钛，氮化硼，碳化铬或碳化钨。最近，含PTFE的化学镍做为复合材料被使用是因为它是均匀的，高粘附的，耐磨的，干润滑的，无擦伤的具有较低的摩擦系数和优良的抗腐蚀性。本论文研究了PTFE在化学镍酸溶液中对沉积速率的影响，PTFE的聚合和镀层中磷含量，耐磨性和抗腐蚀性。

关键词：化学复合材料；化学沉积；Ni-P-PTFE复合材料；复合镀层

1. 引言

电沉积复合镀层是均匀离散的小颗粒物分布在金属镀层里的[1-3]。化学镍磷镀层有许多性能都优于其它镍镀层[4]。由于磷的含量，化学镍镀层有更好的硬度和更好的耐腐蚀性[5]。化学镍复合镀层结合了传统化学镍镀层特有的性能例如复杂铸型中的沉积均匀性，高硬度和优良的耐蚀性带有研磨材料的所拥有的耐高温和其它摩擦性能。

值得注意的是在化学沉积中它有可能达到一个高比例的聚合甚至在镀液中低浓度的颗粒，与电镀相比，高浓度的颗粒必将出现高比例的聚合。近年来复合材料在工程工业中取得重要地位，尤其在高技术领域比如发动机领域，现代燃气涡轮发动机，汽车等等[6]。在化学材料领域，基体不是纯镍，而是其它Ni-P或Ni-B，依于还原剂被用于镀液中。最常用的硬度高的弥散化合物是碳化硅，金刚石粉末，

氧化铝，碳化钛，氮化硼，碳化铬或碳化钨[1-9]。在化学共沉积中的最新发展就是PTFE与镍共沉积。共沉积PTFE颗粒以水分散的形式被添加到溶液中[10,11]。

化学Ni-PTFE镀层的性能如耐磨性，耐蚀性，摩擦系数，显微硬度和所有其它性能都是非常优秀的[12-18]。化学Ni-PTFE复合镀层的制作，性能和应用都是良好的[19,20]。PTFE颗粒被均匀分布在化学镍复合镀层中[21,22]。Duncan[13]沉积的镀层其中包含10-30vol.-%（体积浓度）的直径为0.3-0.4的5-10wt-%磷含量的PTFE 颗粒。在非润滑条件下摩擦系数通常为0.1-0.2。从显微硬度测试和耐磨性能测试中发现含量为14-16%PTFE的复合镀层的硬度通常为250-400HV，而含量为26%PTFE的复合镀层硬度只有275HV。二者通过大于300℃的热处理后硬度值分别增高到625-700HV和400HV。Hadley 和Harl[17]描述了含量达到25wt-%PTFE 均匀分布在含量为84.6Ni-7P-8.4PTEF的化学Ni-P基体上比重为6.5。他们也发现硬度依赖于热处理。Nishira等人[23]研究发现在化学Ni-P镀液中悬浮的PTFE颗粒受非离子和阳离子表面活性剂的影响。Matsuda等人[24]发现PTFE颗粒被共沉积在化学Ni-P镀膜上。这种沉积取决于表面活性剂类型，即在镀液中颗粒表面的电动势和镀膜上颗粒的含量。

PTFE作为一种多功能材料被用于保护工件被腐蚀和磨损[25]。Daniels 和Harme[26]发现Ni-PTFE镀层提高了使用寿命和在塑料制造方面的产品质量[26]。Zhengshan等人[27]报道了Ni-P-PTFE镀层的形态和结构。这赋予了镀层相当多的非擦伤和干润滑性能和较低的摩擦系数。由于颗粒尺寸小，不存在与粗糙度相关的问题，可以以正常方式过滤溶液。Tulsi[28,29]制备的Ni-PTFE镀层基于6.5-11g/dm 的PTFE（60%活性）的添加剂，PTFE颗粒尺寸达到1在88-92的温度下和pH

值为4.7-5.2并伴随搅拌。PTFE共沉积的体积浓度为25-30%。电镀工件具有具体的磨损率和摩擦系数。它被用于各种橡胶和塑料模具，蝶阀，石油和天然气工业紧固件，铝制液化气瓶和化油器节流阀。Pearce[30]概述了制备Ni-PTFE镀层的问题。他在92至95℃下以12mm/h的沉积速率成功得到了25-30%的PTFE镀层。

12.5的镀层是光滑灰暗的，而更厚的镀层会起皮。镀层在350℃下处理1小时能被沉淀和硬化。Roberto[31]描述了一个典型的85Ni-6.6P-8.4PTFE复合镀层。他也发现这些类型的镀层被用做液压离合器组件、工具、安全带组件、机械齿轮和汽车燃料系统元件[32,33]。

Przybylska和Raczynaska[34]能够得到PTFE含量在2.5-11wt-%的镍镀层，即产率不同的分散镀层。含有75Ni-7.9P-6-8PTFE的镀层有良好的结合力和耐磨性。Zhao等人[35]研发了Ni-P-PTFE的分级镀层技术，这大大提高了镀层的附着能力。Liu和Zhao[36]研究了在化学Ni-P系统中表面活性剂对PTFE颗粒大小的影响，并发现镀层中PTFE含量的最大值主要取决于表面活性剂浓度与镀液中PTFE颗粒浓度的比例。Huang等人[37,38]研究了Ni-P化学镀系统中SiC和PTFE在镀层腐蚀，磨损和防粘性能反面的协同作用。Rossi等人[39]评估了Ni-PTFE，P/M O S2和C u/PTFE 化学镀层的服饰行为，用以提高碳钢的耐磨性。本论文作者研究了镀液温度，PTFE 的浓度和PH值对电镀过程中PTFE沉积和聚合速率的影响。镀层的性能如硬度，耐磨性，防腐性和表面形貌的研究用过扫描电镜在有或无热处理条件下得到的。

2. 实验部分

2.1电极制备

低碳钢和不锈钢被用作电极。电极被加工成合适的尺寸和机械抛光。被抛光

的试件用三氯乙烯去垢并浸在稀盐酸中腐蚀。不锈钢试件只能用于磷分析。

2.2镀液的重点

文献中所写道的多种多样的实验方案是在不同温度下选择和研究试件的电镀速率。在这些方案中，如下所述的镀液都是基于柠檬酸钠，次磷酸钠和硫酸镍三者之间被选择用作进一步研究：

（i）硫酸镍30g/L

（ii）柠檬酸三钠50g/L

（iii）次磷酸钠25g/L

（iv）PTFE 添加剂.

为了在90℃下获得具有相对较高的沉积速率，需要改变镀液的组成成分以得到最合适的镀液组成。

2.3镀液的制备与净化

化学药品先被称量再溶解于蒸馏水中（大约为总需求量的75%）。溶液用G.4坩埚过滤并加入蒸馏水混合至需求量。PTFE以离散形式加入到水中。溶液的pH 值用氨电解调节。

2.3镀液维护与控制

镀液的温度用保护系统保持，它能使温差保持在正负2摄氏度。溶液的pH值用PH计不断监视，酸或碱的加入取决于镀液的pH值。镀液的成分主要是硫酸镍和次磷酸钠，二者的比例取决于溶液中沉积的镍。承装镀液的容器要定期更换，并用硝酸清洗。镀液要定期用G.4坩埚过滤，从溶液中去除金属镍。溶液通过磁力搅拌器被搅拌，为保持颗粒悬浮和保持温度均匀。

3. 镀液的参数对沉积速率的影响

3.1 温度的影响

取10×10mm的低碳钢钢板，与三氯乙烯进行皂化作用，在稀盐酸中浸蚀，用碱液碱洗，再用清水清洗，烘干并称重。然后这些钢板在不同温度下被EN/PTFE 复合镀，即60℃，70℃，90℃，在pH值为5.5的酸碱环境下进行2小时。用搅拌器搅拌使得PTFE分散在镀液中。2小时候取出钢板，进行清洗，烘干和称重。依照处理前后的重量差来估算出Ni-PTFE复合镀层的重量。依照镀层重量来估算镀层厚度。

3.2 电镀时间的影响

把经过预处理和称重的钢板在pH值为5.5的酸碱环境中以不同时间进行电镀，即1h，2h，3h，4h和5h。在规定时间过后，钢板被取出并用清水清洗，烘干和称重。依照不同的重量，不同电镀时间下的镀层厚度可以被估算出来。

3.3 PTFE浓度的影响

低碳钢钢板在PTFE浓度为5g/L和20g/L的电镀液中用EN/PTFE复合材料电镀，其镀层厚度能被估算。

3.4 硬度的测定

清洗过的低碳钢钢板用EN/PTFE电镀，其硬度用维氏硬度方法测定。菱形对角线型的压痕是在已知载荷和确定时间下压出的并用装有校准目镜的显微镜测试。依照菱形的长度来估算维氏硬度。

3.5用泰伯耐磨测试仪测量耐磨性

EN/PTFE电镀试件先被称重，然后把试件放在一对较重的有严格控制结构的

研磨轮（每个500g）下，这对研磨轮在这种方式以导致研磨轮与工件表面之间发生侧滑。试件经过称重后，研磨轮每1000转在试件上转换一次。重量差就是磨损指数（泰伯指数）或磨损率。进行两次实验，取平均值。在用只镀镍的试件进行相同的实验，比较镀层含PTFE和不含PTFE的试件的耐磨性。

3.6热处理对硬度的影响

取两个相同的试件。一个只镀镍，另一个镀Ni-PTFE复合镀层。二者均在400℃下进行一个小时的热处理。然后用泰伯测试仪测定耐磨性。

3.7分析镀层中的镍和磷

不锈钢钢板在多种环境下镀EN/PTFE镀层。钢板浸蚀在浓盐酸中1-2min并在氯化钯溶液中活化。然后镀上EN/PTFE复合镀层。把镀层从钢板上取下并称重，溶解于20ml 40%浓度的硝酸中，在倒入100ml的标准测量烧瓶中。溶液中的镍含量通过EDTA法（乙二胺四乙酸胰蛋白酶法）分析，磷含量通过铵磷方法。

3.8极化电位测量腐蚀速率

两块低碳钢被截取成75×15mm规格，进行机械抛光，与三氯乙烯进行皂化作用，60℃下浸蚀在浓度20%的硫酸中2分钟。一块钢板只镀镍而另一块镀EN/PTFE 复合镀层在90℃和pH5.5的环境下电镀2小时。在每个（含PTFE和不含PTFE）镀件的1cm2区域上用恒电位进行稳态极化测量。铂用作辅助电极，饱和甘汞电极作参比电极。研究中电解液是3%浓度的氯化钠溶液。阳极极化和阴极极化都进行。图标显示出了电流密度与电位的关系。用塔菲尔推算法，腐蚀电流和腐蚀电位被确定。毫升每年的腐蚀速率被计算出。

4. 结果和讨论

4.1温度的影响

温度对腐蚀速率的影响如图表1所示。腐蚀速率随温度升高而增高。溶液的温度的升高是溶液发生对流，使溶液流向电极。因为金属电镀总是涉及到以有限扩散速率发生的反应过程，溶液温度的升高有利于镍离子向电子移动，因而导致高沉积率。PTFE共沉积的体积百分数也随温度上升而增加。

表1. pH5.5的镀液中温度对沉积速率的影响

温度，℃沉积速率，

60 70 80 90 3.7 5.0 8.0 10.5

4.2沉积时间的影响

图表2展示了沉积厚度随沉积时间的变化。结果表明，随沉积时间的增加，镀层厚度也增加。

表2. 90℃，pH5.5的镀液中沉积时间对沉积厚度的影响

沉积厚度，沉积时间，h

10.5 17.9 25.9 30.8 38.11 2 3 4 5

4.3镀液中PTFE含量的影响

镀液中PTFE的含量在5g/L至20g/L之间变化，镀层中镍和磷的含量是分析过的。分析结果表明次磷酸盐的增加来减少镍离子，使磷含量达到8%。镀层中镍的数量随PTFE含量的增加而减少。可以明确的是PTFE的体积分数随其含量的增加而增加。PTFE的体积分数得到了15g/L的恒定值。PTFE含量的影响在图表3中给出。

表3. 镀液中PTFE浓度的影响

聚四氟乙烯浓度，g/L聚四氟乙烯在EN /聚四氟乙烯沉积vol.-%

5 7 9 11 13 15 17 19 18.0 20.8 22.

6 24.0 24.8

24.9

25.0 25.0

4.4嵌入的PTFE和热处理对镀层硬度和耐磨性的影响

比较镀镍试件和镀复合物试件的硬度。这些测试证实了镀镍过程加入聚四氟乙烯颗粒会减少镀层硬度，以为它减少电镀的有效承载区域。这两个试件在400℃环境下进行一小时的热处理。热处理导致EN和EN/PTFE复合镀层硬度的增加。然而，发现EN/PTFE镀层的硬度比EN镀层的硬度低。PTFE颗粒通过热处理过程

被烧结，这使得在镀层表面留下富PTFE的膜，因为高温将PTFE颗粒压到顶部。结果列于图表4。EN/PTFE复合镀层的耐磨性比镍镀层的耐磨性有所提高。PTFE 作为干润滑剂，因此增加了耐磨性。经过400℃、1小时的热处理产生更好的性能。热处理前后的磨损率平均值在图表5中给出。

镍镀层和EN/PTFE复合镀层的腐蚀行为通过塔菲尔极化曲线比较。镍磷化学镀层在恶劣环境中有较高的耐蚀性。EN/PTFE共镀据报告也有相似行为。图表6展示了结果。有时候自由的双层PTFE复合镀层是可取的低或高含量磷层紧挨着EN/PTFE复合镀层能提高基体金属的保护性。图1为热处理前EN/PTFE复合镀层的显微照片。从图中明显得知PTFE颗粒被聚合在Ni-P集体上。

表6. pH5.5的3%氯化钠中的腐蚀数据

基体

/corr,μA /CM 腐蚀速率,ml/year 镍镀层

EN/PTFE

25.7 25.18 10.918 10.670

a ×2000；

b ×5000

图1.Ni-P-PTFE 化学复合镀层SME 照片

4.5 Ni-PTFE 化学复合镀层的应用

EN/PTFE 复合镀层主要被用作润滑镀层。EN/PTFE 在不同温度下保护不受润滑剂作用的元件不受溶剂作用。该镀层一般用于阀门，铝筒，泵叶轮和模芯。EN/PTFE 性能有自润滑和低摩擦表面，优良的耐磨和耐蚀性，镀层厚度均匀性。

5. 结论

（1）低碳钢的Ni-PTFE 复合镀层镀液的制定是通过计算的，沉积速率10.5，90℃，pH5.5。镀液的组成：（i ）硫酸镍30

（ii ）柠檬酸50 （iii ）次磷酸钠

（iv ）分散的聚四氟乙烯（60%活性）

（2）研究发现PTFE 共沉积的体积分数随着温度升高和溶液中PTFE 的浓度升高

而升高。

（3）研究发现镍镀层中18-25%的共沉积PTFE减少耐磨性，通过400℃热处理可以进一步减少PTFE的量。

（4）研究发现共沉积PTFE能减少硬度，但通过400℃的热处理能再提高。（5）PTFE共沉积对镍的腐蚀行为无影响。

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[36] Y. Liu Q. Zhao: Trans. Inst. Met. Finish., 2003, 81, 168.

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[38] Y. S. Huang, X. T. Zeng, X. F. Hu F. M. Liu: Electrochim. Acta, 2004, 49, 4313.

[39] S. Rossi,. F. Chini, G. Straffelini, P. L. Bonora, R. Moschini A. Stampali: Surf. Coat. Technol., 2003, 173, 235.

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外文文献及翻译

外文文献及翻译 题目：利用固定化过氧化氢酶 回收纺织品漂染的废水 专业食品科学与工程 学生姓名梁金龙 班级B食品072 学号0710308119 指导教师郑清

利用固定化过氧化氢酶回收纺织品漂染的废水 Silgia A. Costa1, Tzanko Tzanov1, Filipa Carneiro1, Georg M. Gübitz2 &Artur Cavaco-Paulo1,? 1纺织工程系, 米尼奥大学, 4810吉马尔, 葡萄牙 2环境生物技术系, 格拉茨技术大学, 8010格拉茨, 奥地利 ?作者联系方式(Fax: +351 253 510293; E-mail: artur@det.uminho.pt) 关键词：过氧化氢酶的固定化，酶稳定，过氧化氢，纺织印染 摘要 过氧化氢酶固定在氧化铝载体上并用戊二醛交联，在再循环塔反应器和CSTR反应器中研究贮存稳定性，温度和pH值对酶的活性。固定化酶的在的活性维持在44％，pH值11（30?C），对照组是活性为90％，pH值7（80?C），过氧化氢酶固定化的半衰期时间被提高到2小时（pH12，60?C）。用过氧化氢漂白织物后，洗涤过程中的残留水被固定化酶处理，可以用于再次印染时，记录实验数据。 1 序言 由于新的法规的出台，从生态经济的角度来看（Dickinson1984年），对于纺织行业中存在的成本和剩余水域的污染问题，必须给予更多的关注。过氧化氢是一种漂白剂，广泛应用于工业纺织工艺（Spiro & Griffith1997年）。在去除H2O2时，会消耗大量的水和能源（Weck 1991, St?hr & Petry 1995），以避免对氧气敏感的染料（Jensen 2000）产生后续问题。过氧化氢酶可用于降低过氧化氢的含量（Vasudevan & Thakur 1994, Emerson et al. 1996），从而减少水分消耗或方便回收印染洗涤液。过氧化氢酶的使用主要问题出在漂白时温度和清洗液碱度过高。以前，我们试图通过筛选新的嗜热嗜碱的微生物（Paar et al. 2001）或使用不同的酶稳定剂（Costa et al. 2001）来解决此问题。但是染料与蛋白质之间的潜在相互作用（Tzanov et al. 2001a, b）表明，可溶性过氧化氢酶的使用是不恰当的。固定化过氧化氢酶的使用还有一种选择(Costa et al. 2001, Amar et al. 2000)。在这项研究中，我们对氧化铝进行共价固定并使用戊二醛作为交联剂，这种方法在商业中得到验证。本项研究的目的就是探讨过氧化氢酶的固定化动力学，及其稳定性和工艺条件，这将使我们能够应用此系统，以处理可能被用于清洗染色的反复使用的酒。 2 材料和方法 2.1 酶 Terminox（EC1.11.1.6），50L以上，由AQUITEX- Maia提供，葡萄牙产。 2.2 过氧化氢酶的固定化 取Al2O3颗粒或薄片（Aldrich），直径分别为3和7毫米，在45摄氏度下，先经浓度4%的γ-氨丙基三乙氧基硅烷(Sigma)烷基化，再放入丙酮中浸泡24小时。用蒸馏水洗涤硅烷化载体后，放入浓度为2％戊二醛水溶液中室温下浸泡2小时（Aldrich），重复清洗一次并在60?C下干燥1小时。取五克的烷基化载体，室温24?C下浸泡在25毫升粗酶制剂中（Costa et al. 2001）。得出，每克Al2O3

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Dashboard From Wikipedia, the free encyclopedia This article is about a control panel placed in the front of the car. For other uses, see Dashboard (disambiguation). The dashboard of a Bentley Continental GTC car A dashboard (also called dash, instrument panel (IP), or fascia) is a control panel located directly ahead of a vehicle's driver, displaying instrumentation and controls for the vehicle's operation. Contents 1.Etymology 2.Dashboard features 3.Padding and safety 4.Fashion in instrumentation 5.See also 6.References Etymology Horse-drawn carriage dashboard Originally, the word dashboard applied to a barrier of wood or leather fixed at the front of a horse-drawn carriage or sleigh to protect the driver from mud or other debris "dashed up" (thrown up) by the horses' hooves.[1] Commonly these boards did not perform any additional function other than providing a convenient handhold for ascending into the driver's seat, or a small clip with which to secure the reins when not in use. When the first "horseless carriages" were constructed in the late 19th century, with engines mounted beneath the driver such as the Daimler Stahlradwagen, the simple dashboard was retained to protect occupants from debris thrown up by the cars' front wheels. However, as car design evolved to position the motor in front of the driver, the dashboard became a panel that protected vehicle occupants from the heat and oil of the engine. With gradually increasing mechanical complexity, this panel formed a convenient location for the placement of gauges and minor controls, and from this evolved the modern instrument panel,