高磷化学镀镍光亮剂的研究

研究了无机、有机、复合光亮剂对高磷化学镀镍镀层外观、表面微观形貌、沉积速度、磷含量、孔隙率及耐蚀性的影响。试验证明:添加无机光亮剂时,镀层光亮,但存在微孔结构,导致孔隙率升高,耐蚀性大幅下降;添加有机光亮剂时,镀层光亮性略有下降,但镀层均匀性好,缺陷少;而复合光亮剂则可以实现较理想的效果,其镀层外观光亮,表面平整细致,沉积速度快,整体性能优良,复合光亮剂组成为:2mg/L Ce(SO4)2、3 mg/LTe(SO4)2、30 mg/L C6H5SO2Na、2 mg/L N,N-二乙基丙炔胺(DEP)。     

AlCl3·6H2O在盐酸体系中的结晶行为

研究了AlCl₃·6H₂O在盐酸体系中的结晶行为,考察了铁、钙、镁、钾、钠等杂质对AlCl₃·6H₂O结晶行为的影响,并利用聚焦光束反射测量技术（FBRM）和颗粒录影显微镜（PVM）探讨了不同盐酸滴加速度下AlCl₃·6H₂O的结晶粒度分布及形貌。结果表明,AlCl₃·6H₂O的结晶量随着盐酸加入量的增加而增加,当浓盐酸加入量为AlCl₃饱和溶液体积的2.25倍时,25℃时的结晶效率可达到80%。溶液中Fe的存在可促进AlCl₃·6H₂O的结晶,在1.5 mol·kg^-1的AlCl₃溶液中,当铝铁摩尔比低于3：1时,得到的AlCl₃·6H₂O晶体中铁的含量小于0.1%。钾、钙、镁、钠等杂质对AlCl₃·6H₂O的结晶影响不大。盐酸添加速度影响AlCl₃·6H₂O的形貌,快的盐酸添加速度易使晶体发生团聚,颗粒粒径小,盐酸添加速度较慢时,可得到颗粒较大、形貌好的单晶。     

脉冲电沉积Ni-Al2O3复合镀层的工艺参数及性能研究

利用脉冲电沉积在304不锈钢上制备了Ni-Al2O3纳米复合镀层,通过正交试验法确定了最佳工艺参数为:硫酸镍280 g/L,氯化镍45 g/L,硼酸40 g/L,十二烷基硫酸钠0.1 g/L,平均电流密度4 A/dm2,占空比40％,脉冲频率600 Hz,纳米Al2O3颗粒质量浓度5 g/L,温度45～55°C,pH 3～4,搅拌速率约220 r/min,电沉积时间60 min.用扫描电子显微镜分析镀层表面形貌,用能谱仪确定镀层中Al2O3含量,用显微硬度计测试镀层的显微硬度,用数码显微镜测量镀层的表面粗糙度,用电化学工作站分析镀层的耐蚀性.结果表明:与直流电沉积复合镀层相比,脉冲复合镀层晶粒尺寸较小、结合紧密,纳米Al2O3颗粒均匀分散,显微硬度和纳米Al2O3颗粒含量高,表面平整,耐蚀性好.     

锌-镍/纳米氧化铝复合电沉积及镀层结构性能研究

以冷轧钢板为基材,研究了Zn-Ni/纳米Al2O3复合镀层的电沉积工艺,分析了复合镀层的成分和晶体结构.通过中性盐雾试验,考察了复合镀层的耐蚀性.采用X射线衍射和扫描电镜,分别表征了复合镀层腐蚀产物的微观结构以及镀层的表面形貌.结果表明:Zn-Ni/纳米Al2O3复合镀层的结晶比Zn镀层及Zn-Ni合金镀层更细致,晶粒排布更均匀、整齐.当Zn-Ni/纳米Al2O3复合镀层中Ni和Al2O3的质量分数分别为13%左右和0.40%～0.60%时,其耐蚀性最好.Al2O3颗粒的掺入可降低镀层的孔隙率,使镀层平整、致密,从而提高了镀层的耐蚀性.     

镍基氧化铝纳米微粒复合电镀的研究现状

以Al2O3纳米微粒为复合材料的复合电镀是一种取代镀硬铬的极有价值的复合表面技术。Al2O3微粒与镍金属共沉积可明显提高镀层的硬度、耐磨性与耐蚀性。主要阐述了Al2O3纳米微粒与金属镍共沉积的工艺条件对沉积速率和镀层性能的影响。并且指出Al2O3纳米微粒复合镀镍中关键问题是如何提高复合镀层中纳米微粒的含量及镀层形貌对镀层性能的影响,以寻找控制镀层表面形貌的条件。     

纯Fe在酸性AlCl3-EMIC离子液体中的阳极行为

重点研究了纯铁（Fe）在2∶1酸性AlCl₃-氯化1-甲基-3-乙基咪唑（AlCl₃-EMIC）中的阳极行为。通过三电极体系测定了Fe在AlCl₃-EMIC中的阳极极化和不同电位下的电流-时间曲线,利用恒电位溶解计算了Fe溶解的价态,最后通过扫描电子显微镜（SEM）观察了不同电流密度下Fe的溶解形貌。结果表明：Fe表面的氧化膜会阻碍Fe的溶解,在去除氧化膜后,当电位达到-0.35 V时,Fe开始发生活性溶解,产物为Fe（Ⅱ）。Fe的阳极电流密度随电位的增加而增加,达到峰值后显著下降。小电流密度下（如2 mA·cm^-2）,Fe的溶解形貌随时间的延长,呈现先点状腐蚀再均匀腐蚀的特点;而大电流密度下（如15 mA·cm^-2）,Fe电极表面会生成一层固态物质,同时可见清晰的划痕,即不发生明显的腐蚀。     

全光亮化学镀镍磷合金新工艺

研制开发了一种新型的全光亮化学镀镍磷合金工艺,光亮剂对磷的沉积起到积极的促进作用,能够提高镀层中的磷含量。光亮剂的添加使镀液出光速度快、镀层光亮均匀,可以获得全光亮的镍磷合金镀层。扫描电镜和X 射线衍射分析结果表明,高磷合金镀层为非晶态结构。测试表明,镍-磷合金镀层的硬度介于290～490HV之间,且随光亮剂加入量的增加而降低。镀层磨损率在0 00396～0 00498mg/(cm2·h)之间。镀液中光亮剂含量为2mL/L时,所得镀层在10%的HCl介质中腐蚀率最低为0 0002mg/cm2·h。     

纳米颗粒对复合电刷镀过程中镀液特性及镀层沉积速度的影响

本文研究了特快镍刷镀液(TK-Ni)及两种不同纳米颗粒含量的纳米Al2O3／特快镍复合刷镀液(10n／TK-Ni和30n／TK-Ni，其中前者纳米颗粒含量较少)在刷镀过程中的温度和密度变化及复合镀层厚度的变化，解释了纳米颗粒的加入对镀液温度和密度的影响及对镀层沉积速率的影响。试验结果表明：刷镀过程中含纳米颗粒的复合镀液的温度和密度均较高，且二者均随纳米颗粒含量的增大而升高；随刷镀过程的进行，镀液温度升高，密度减小，复合镀液密度在刷镀时间达30min后出现回升现象；复合镀层沉积速度较快，且镀层沉积速度随镀液中纳米颗粒含量增加而增大。     

三价铬电沉积机理研究及镀层表征

在硫酸盐三价铬电沉积体系中,通过赫尔槽实验对不同络合剂含量进行了筛选,得到络合剂最佳含量配比为甲酸铵80 g/L、草酸铵20 g/L以及尿素30 g/L,最佳电流密度范围为5.11 A/dm²～20.68 A/dm²;通过循环伏安曲线和阴极极化曲线分析三价铬电沉积机理,发现三价铬的沉积过程分两步进行：第一步为Cr³⁺+e→Cr²⁺,过程不可逆;第二步为Cr²⁺+2e→Cr,可逆;草酸铵会增大阴极极化,甲酸铵和尿素会降低阴极极化;电沉积20 min得到的铬镀层,XPS分析表面镀层由单质Cr、Cr₂O₃及Cr(OH)₃构成;微观结构观测发现,随着电沉积时间增加,镀层由表面平整形貌逐渐转变为瘤状结构形貌;镀层呈现明显的(110)择优取向;电化学研究表明,相比20 min铬镀层,5 min铬镀层的耐蚀性较好,腐蚀电位由-0.6377 V提高至-0.5633 V,腐蚀电流由6.1030×10^-6 A/...     

电流密度对硫酸盐光亮镀锡的影响

在电流密度为0.01～0.05 A/cm~2的条件下进行光亮锡镀。研究了电流密度对阴极过电位、电流效率及镀层厚度的影响,并用SEM和XRD对镀层的表面形貌和晶粒的择优取向进行了表征。结果表明:随着电流密度的增大,阴极过电位和镀层厚度不断增加,电流效率先增大后减小。在较低的电流密度下得到的镀层表面较为均匀、致密;当电流密度高于0.03 A/cm~2时,镀层表面出现较多孔隙,粗糙度增加。不同电流密度下,晶粒的择优取向不同。当电流密度高于0.03 A/cm~2时,晶粒的择优取向由(101)晶面和(211)晶面向(220)晶面转变。     

Effects of additive NaI on electrodeposition of Al coatings in AlCl3-NaCl-KCl molten salts

Effects of NaI as an additive on electrodeposition of Al coatings in AlCl₃-NaCl-KCl(80-10-10 wt-%)molten salts electrolyte at 150°C were investigated by means of cyclic voltammetry,chronopotentiometry,scanning electron microscopy and X-ray diffraction(XRD).Results reveal that addition of NaI in the electrolyte intensifies cathodic polarization,inhibits growth of Al deposits and increases number density of charged particles.The electrodeposition of Al coatings in the AlCl₃-NaCl-KCl molten salts electrolyte proceeds via three-dimensional instantaneous nucleation which however exhibits irrelevance with NaI.Galvanostatic deposition results indicate that NaI could facilitate the formation of uniform Al deposits.A compact coating consisting of Al deposits with an average particle size of 3μm was obtained at a current density of 50 mA?cm^?2 in AlCl₃-NaCl-KCl molten salts electrolyte with 10 wt-%NaI.XRD analysis confirmed that NaI could contribute to the formation of Al coating with a preferred crystallographic orientation along(220)plane.     

硫酸铝铵-氯化氢反应制备六水氯化铝过程中晶体形貌的研究

以十二水合硫酸铝铵为原料,采用氯化氢通气结晶法制备了六水氯化铝晶体,考察了通气速率、通气时间、反应温度、铝离子初始浓度对六水氯化铝晶体形貌的影响。结果表明,50 mL硫酸铝铵酸溶液中,当通气速率为60 mL/min、通气时间为2 h、反应温度为30 ℃、铝离子初始质量浓度为20 g/L时,可以得到形貌比较规整的棱柱形六水氯化铝晶体。该研究为提取、制备高品质六水氯化铝晶体提供了技术参考。     

Surface tension studies of additives in acrylic resin-based powder coatings using the Wilhelmy balance technique

A modified Wilhelmy balance technique using thin fibers as solid probes has been applied to study the effect of silicone additives in acrylic resin-based powder coatings on the surface tension of non-reactive binder systems. By measuring the temperature dependence of the surface tension in the temperature range between 140 and 180°C, it could be shown that the silicone additives investigated had a very different surface activity in the molten acrylic resin. Due to the high accuracy of the measuring technique and the good reproducibility of the experiments the influence of different additive concentrations on the surface tension was detectable even at very low concentrations (below 1 wt.%).

Compared to the pure powder coating binder which has a surface tension of about 30 mN/m the values decreased between 2–15 mN/m depending on the type of the silicone additive. In addition, the temperature coefficient −(dγ/dT) of the surface tension of the binder melt was changed. In the case of two additives, the surface tension of the powder coating and its temperature coefficient were lowered considerably. This effect of additives is desirable to reach good wetting and leveling of the powder coating.     

Electrodeposition of Cu–Zn alloy coatings from citrate baths containing benzotriazole and cysteine as additives

Alternative electrolytes, such as citrate baths, are now studied, aiming to reduce the toxicity and the cost of the electroplating process while maintaining the decorative qualities and anticorrosive properties of the coatings. For this purpose, brightening and/or leveling compounds are usually added to the base citrate bath. In this work, Cu–Zn alloys were electroplated on mild steel substrates from electrolytes containing sodium citrate and additives (benzotriazole and cysteine) at constant stirring speed. The results showed that coatings produced from baths containing additives were brighter than those obtained from the base citrate bath. Additionally, the presence of benzotriazole directly influenced the coating composition and the properties of the deposited alloy: the amount of zinc in this coating increased excessively, and the coating/substrate corrosion presented a poor anticorrosive performance.     

Assessment of Oxide Debond Coatings for Metal-Toughene Intermetallics

The interfacial debond characteristics of sputtered Al₂O₃ and Y₂O₃, coating were assessed in a γ-TiAl/Nb composite. The preferred debond coating identified for this composite system was Y₂O₃, which also protected the ductile reinforcing phase from reaction with the matrix. Tension tests on a model laminate specimen were performed to characterize the toughening behavior and showed that interfacial debonding promoted extensive plastic deformation of the ductile phase over a large volume. The coatings were characterized to understand the debonding behavior. Comparison is made with other metal/oxide system.     

AlCl3·6H2O在FeCl3、CaCl2、KCl及KCl–FeCl3溶液中溶解度的实验及预测

如何将AlCl₃·6H₂O从众多组分中选择性地结晶分离是从煤矸石中提Al的关键,而AlCl₃·6H₂O在煤矸石酸浸体系中的热力学平衡数据对于结晶过程的控制至关重要。在25～85℃的温度范围内,测定了不同温度和溶液浓度下AlCl₃·6H₂O在FeCl₃、CaCl₂、KCl及KCl-FeCl₃溶液中的溶解度。实验发现温度对AlCl₃·6H₂O在所有溶液体系中溶解度的影响均不明显,溶解度只随温度的升高略有增加;溶液浓度是影响溶解度的主要因素,AlCl₃·6H₂O在所有溶液体系中的溶解度均随溶液浓度的升高而明显下降,分析其原因是由于溶液浓度的增大使得Cl^–同离子效应增强。为了提高OLI软件预测结果的准确性,对其嵌入Bromley-Zemaitis模型中“Al³⁺–Cl<...     

氯铝酸盐离子液体催化甲苯与氯代叔丁烷烷基化反应合成对叔丁基甲苯

合成[Me3NH]Cl-2.0AlCl3、[PyH]Cl-2.0AlCl3、[Bmim]Cl-2.0AlCl3以及[Et3NH]Cl-2.0AlCl3氯铝酸盐离子液体,对[Et3NH]Cl-2.0AlCl3和[PyH]Cl-2.0AlCl3两种离子液体进行系列改性,并考察氯铝酸盐离子液体催化甲苯与氯代叔丁烷的烷基化反应,反应合成对叔丁基甲苯的催化性能。结果表明,未经改性的氯铝酸离子液体催化烷基化反应,对位产物选择性均较低,经FeCl3、CuCl以及CH3NO2改性的[Et3NH]Cl-2.0AlCl3离子液体对叔丁基甲苯选择性显著提高,而[PyH]Cl-2.0AlCl3离子液体经CuCl改性后的对叔丁基甲苯选择性则提高到85%以上。采用乙腈、吡啶为探针的红外光谱对离子液体酸性表征的结果表明,改性后离子液体的L酸和B酸均有所降低,其中B酸是影响对叔丁基甲苯选择性的主要因素,并对离子液体酸性催化甲苯与氯代叔丁烷烷基化反应合成对叔丁基甲苯的作用机制进行分析。     

Effects of the structure of organic additives in the electrochemical preparation and characterization of CoFe film

The use of organic additives is widespread in the manufacturing of thin films by electrochemical deposition. Common additives like saccharin (SAC) were used as leveling and brightening agents in the cobalt-iron deposits. In the present work, effects of additives molecular structure on the CoFe deposits from sulfate electrolytes at pH 3 were investigated. Phthalimide (PHTA) and a new additive (OAS) were tested like organic additives to understand the influence of different functional groups of these compounds. The composition and the morphology of the binary alloy were examined by SEM. The corrosion properties were characterized by voltammetry. The main results revealed that the presence of the sulfonamide in the structure of organic additives does not play the role in brightening and leveling agent, but this function seems to be important for CoFe deposit corrosion resistance even if all additives change the deposit corrosion resistance properties. Moreover, the complexation between the iron ion and the organic additive seems to be affected by the presence of the carbonyl group.