因瓦合金箔电沉积的制备及其微观结构和耐蚀性

在含有复配稳定剂和添加剂的高铁硫酸盐氯化物电解液中,电沉积得到因瓦合金箔。研究电沉积过程中对合金箔组成的影响因素以及合金箔的耐腐蚀性能。研究结果表明:电解液组成、电流密度、温度及pH值对合金箔组成的影响较大;在阴、阳极面积比为1.0∶2.0,镍、铁阳极面积比为1.8∶1.0的条件下,因瓦合金箔组成稳定,Fe的质量分数为(64±2)%;合金箔晶粒细小,尺寸均匀,结构紧密,表面光滑平整,无孔洞和裂纹,呈铁镍固溶体和面心立方晶体结构,表现出较强的(111)和(200)晶面择优取向;因瓦合金箔分别在10%硫酸溶液、10%氢氧化钠溶液和3.5%氯化钠溶液中钝化稳定,钝化电位较宽,表现出良好的耐蚀性能。     

阿维菌素-羟丙基-β-环糊精包合物的制备

对羟丙基-β-环糊精包合阿维菌素进行了研究.通过应用溶液搅拌法制取包合物,采用单因素试验和正交试验确定的最佳工艺条件为:主客体投料质量比为100∶3,包合温度为50℃,包合时间为8h.在最佳工艺条件下,用HPLC法确定包合率为39.6%,用称重法确定收率为81.1%,并对包合物做了TG分析.结果表明:被包合后的阿维菌素的水溶性、光稳定性显著提高,同时提高了阿维菌素杀虫杀螨的长效性.     

6-甲基-2(1H)-吡啶酮的合成

以2-氨基-6-甲基吡啶为初始原料,通过重氮化水解反应合成了6-甲基-2(1 H)-吡啶酮.研究了反应条件对合成产率的影响,确定了最佳反应条件:反应时间3h,温度0～5℃;光照条件下水解;饱和碳酸钠溶液调节溶液的pH值至7.合成产物的结构经熔点测定、1 H-NMR、13 C-NMR表征得到证实,产率达到91.7%.     

光亮微晶态镍铁合金箔电沉积

在氯化物-硫酸盐体系中, 采用电沉积的方法制得了光亮Ni-Fe二元合金箔. 研究了Ni2 与Fe2 的摩尔比(n(Ni2 )/n(Fe2 ))及Cl-、硼酸、柠檬酸、糖精和十二烷基硫酸钠对电沉积Ni-Fe合金箔的铁含量和电流效率的影响规律. 当电流密度为10～13 A/dm2, pH值为3.17, 温度为50～55 ℃, 时间为10 min时, 得到了Fe含量(质量分数)为23.2%～63.0%, Ni含量为37.0%～76.8%, 厚度为30 μm左右的纳米微晶态Ni-Fe合金箔镀层. X射线衍射结果表明: 合金箔为NiFe固溶体织构, 晶粒细化, 属于纳米微晶体;合金箔表面光亮平滑;显微硬度(HR30T)为17.2～19.5, 抗拉强度为779.66 Mpa, 延伸率为1%, 电阻率为29.56～62.99 μΩ·cm, 其具有较强的韧性和耐腐蚀性能.     

负载型钒-钛体系催化剂合成反式-1,4-聚异戊二烯

研究了复合负载型钒催化剂VCl3/MgCl2·SiO2-Al(i-Bu)3-TiCl4/MgCl2·SiO2体系合成反式-1,4-聚异戊二烯的基本规律.当采用单体-Al-V-Ti的加料顺序时,温度为50 ℃,最大催化剂效率可达10～11 kgTPI/gV.结果表明最佳工艺条件为:n(Al)/n(V)/n(Ti)=10:1:0.5,n(V)/n(Ip)=1～2.60×10-4,反应温度50 ℃.温度和时间对聚合产物的结构无影响,所得产物的反式-1,4结构含量均大于95%.     

浊点萃取-分光光度法测定水中痕量镍

采用十二烷基磺酸钠(SDS)和Triton X-100的混合表面活性剂,以1-(2-吡啶偶氮)-2-萘酚(PAN)为络合剂,加入电解质NaCl溶液,通过紫外-可见分光光度法测定水中痕量镍.在室温下,考察影响浊点萃取、分离和富集金属离子镍的影响因素及适宜的反应条件.结果表明,在饱和NaCl的加入量为5.5 mL,体积分数为0.1%的PAN加入量为0.125 mL,SDS和Triton X-100的摩尔比在0.38～1.39时,所形成的体系对Ni2 -PAN络合物具有较好的萃取效果.最佳条件下,方法的线性范围为0.1～1.0 mg·L-1,相关系数R2＝0.999 8,检测限为18.9 μg·L-1,镍的加标回收率达97%～99%,相对标准偏差为2%～4%.     

溶胶-凝胶法制备ITO薄膜及其光电特性研究

以InCl3·4H2O和SnCl4·5H2O为主要原料,采用溶胶一凝胶法和旋转涂膜工艺,在玻璃基片上制备掺锡氧化铟透明导电薄膜(ITO).用紫外-可见透射光谱和四探针技术,研究了不同掺Sn量、不同热处理温度和热处理时间对薄膜光学和电学性能的影响.实验结果表明,最佳工艺条件为掺Sn量11%,热处理温度480℃,热处理时间60min.在最佳工艺条件下制备的ITO薄膜可见光透过率达82%以上,薄膜的方块阻为390Ω/□.     

固体超强酸SO2-4/ZrO2催化α-蒎烯异构反应

研究了固体超强酸SO2-4/ZrO2催化剂的制备条件(硫酸浸渍浓度、焙烧温度等)对其催化性能的影响.结果表明,催化剂的制备条件不同,对莰烯选择性和α-蒎烯转化率有较大影响.适宜的催化剂制备条件是: 硫酸浓度0.5～1.0 mol/L,焙烧温度650 ℃.对所制备的SO2-4/ZrO2固体超强酸作为α-蒎烯异构反应的催化剂,以及对影响反应过程的主要因素进行探讨.优化的工艺条件为:反应时间1～3 h,反应温度(130±2)℃,催化剂质量分数3%～4%.该条件下α-蒎烯转化率96.4%,莰烯选择性49.7%.此外,还分析了催化剂放置时间对异构产物的影响及催化剂重复使用情况.     

三价铬镀液中电沉积纳米晶体Fe-Ni-Cr合金箔

在氯化物—硫酸盐镀液体系中,以柠檬酸为络合剂,通过电沉积的方法获得厚度约为30μm的Fe-Ni-Cr合金箔。研究了电流密度、温度、pH值以及镀液中三氯化铬和柠檬酸含量对Fe-Ni-Cr合金箔成分的影响。确定了最佳工艺条件,即电流密度为10~20 A/dm2,pH值为1.60~2.70,温度为20~30℃。采用能量损失谱测定镀层成分,采用X射线衍射和扫描电镜分别测定镀层的晶体结构和表面形貌。研究结果表明,电沉积得到的合金箔成分为31.13%~54.24%Fe,44.64%~65.36%Ni,1.11%~3.52%Cr,镀层表面光亮平滑,抗拉强度为900.2~996.0 MPa,电阻率为61.3~95.4μΩ.cm;Fe-Ni-Cr合金箔的晶粒尺寸小于10 nm,为纳米晶体结构,具有良好的韧性和耐腐蚀性。     

固体超强酸SO4^2-／ZrO2催化α-蒎烯异构反应

研究了固体超强酸SO2-4/ZrO2催化剂的制备条件(硫酸浸渍浓度、焙烧温度等)对其催化性能的影响.结果表明,催化剂的制备条件不同,对莰烯选择性和α-蒎烯转化率有较大影响.适宜的催化剂制备条件是 硫酸浓度0.5～1.0 mol/L,焙烧温度650 ℃.对所制备的SO2-4/ZrO2固体超强酸作为α-蒎烯异构反应的催化剂,以及对影响反应过程的主要因素进行探讨.优化的工艺条件为反应时间1～3 h,反应温度(130±2)℃,催化剂质量分数3%～4%.该条件下α-蒎烯转化率96.4%,莰烯选择性49.7%.此外,还分析了催化剂放置时间对异构产物的影响及催化剂重复使用情况.     

Annealing crystallization and catalytic activity of ultrafine NiB amorphous alloy

Annealing crystallization of ultrafine NiB amorphous alloy prepared by the chemical reduction method was studied by DTA, XRD and XAFS techniques. The XRD and XAFS results have revealed that the crystallization process of ultrafine NiB amorphous alloy proceeds in two steps. First, ultrafine NiB amorphous alloy is crystallized to form metastable nanocrystalline Ni₃B at an annealing temperature of 325℃. Second, the nanocrystalline Ni₃B is further decomposed into crystalline Ni at 380℃ or higher tempera ture, the local structure around Ni atoms in resultant product is similar to that in Ni foil. It was found that the catalytic activity of nanocrystalline Ni₃B for benzene hydrogenation is much higher than that of ultrafine NiB amorphous alloy or crystalline Ni. The result indicates that the active sites of nanocrystalline Ni₃B for benzene hydrogenation are composed of both Ni and B with proper geometry configuration.     

反相微乳液法制备Ni-B非晶态合金团簇

采用W/O型微乳液法,用KBH4还原Ni(Ac)2制备Ni-B非晶态合金团簇.扫描电镜(SEM)和透射电子显微镜(TEM)测试表明,团簇形貌呈球形,尺寸为10~15 nm,分布较均匀,基本达到单分散.热分析(DSC)测试表明,Ni-B样品的热稳定性明显高于水溶液体系用KBH4还原Ni(Ac)2制得的Ni-B非晶态合金纳米颗粒.热处理实验及XRD测试结果表明,Ni-B非晶态合金团簇的晶化过程包括两个步骤,即Ni-B非晶态合金晶化成晶态Ni-B合金和Ni-B晶态合金分解成纳米晶Ni和单质B.     

化学镀Ni-Mo-P纳米晶镀层腐蚀性能研究

通过化学镀获得了混晶(非晶+微晶)和纳米晶态两种结构的Ni-Mo-P合金镀层,并将混晶态镀层进行晶化处理得到一种单相和一种双相的纳米晶镀层。通过阳极极化曲线分析了各镀层在5%H2SO4溶液的耐蚀性能并与Ni-P镀层进行对比,结果发现,镀态Ni-Mo-P纳米晶镀层的耐蚀性能优于镀态Ni-P纳米晶镀层;经退火处理后获得的两种纳米晶镀层的耐蚀性能比镀态混晶和纳米晶镀层均要好;同时还发现退火处理获得的Ni-Mo-P双相（Ni+Ni3P）纳米晶镀层与退火处理后获得的Ni-Mo-P单相(Ni)纳米晶镀层的耐蚀性能相当。     

Corrosion-wear behavior of nanocrystalline Fe_(88)Si_(12) alloy in acid and alkaline solutions

The corrosion-wear behavior of a nanocrystalline Fe_(88)Si_(12) alloy disc coupled with a Si_3N_4 ball was investigated in acid(pH 3) and alkaline(pH 9) aqueous solutions. The dry wear was also measured for reference. The average friction coefficient of Fe_(88)Si_(12) alloy in the pH 9 solution was approximately 0.2, which was lower than those observed for Fe_(88)Si_(12) alloy in the pH 3 solution and in the case of dry wear. The fluctuation of the friction coefficient of samples subjected to the pH 9 solution also showed similar characteristics. The wear rate in the pH 9 solution slightly increased with increasing applied load. The wear rate was approximately one order of magnitude less than that in the pH 3 solution and was far lower than that in the case of dry wear, especially at high applied load. The wear traces of Fe_(88)Si_(12) alloy under different wear conditions were examined and analyzed by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. The results indicated that the tribo-chemical reactions that involve oxidation of the worn surface and hydrolysis of the Si_3N_4 ball in the acid solution were restricted in the pH 9 aqueous solution. Thus, water lubrication can effectively improve the wear resistance of nanocrystalline Fe_(88)Si_(12) alloy in the pH 9 aqueous solution.     

Corrosion-wear behavior of nanocrystalline Fe88Si12 alloy in acid and alkaline solutions

The corrosion?wear behavior of a nanocrystalline Fe88Si12 alloy disc coupled with a Si3N4 ball was investigated in acid (pH 3) and alkaline (pH 9) aqueous solutions. The dry wear was also measured for reference. The average friction coefficient of Fe88Si12 alloy in the pH 9 solution was approximately 0.2, which was lower than those observed for Fe88Si12 alloy in the pH 3 solution and in the case of dry wear. The fluctuation of the friction coefficient of samples subjected to the pH 9 solution also showed similar characteristics. The wear rate in the pH 9 solution slightly increased with increasing applied load. The wear rate was approximately one order of magnitude less than that in the pH 3 solution and was far lower than that in the case of dry wear, especially at high applied load. The wear traces of Fe88Si12 alloy under dif-ferent wear conditions were examined and analyzed by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. The results indicated that the tribo-chemical reactions that involve oxidation of the worn surface and hydrolysis of the Si3N4 ball in the acid solution were restricted in the pH 9 aqueous solution. Thus, water lubrication can effectively improve the wear resistance of nanocrystalline Fe88Si12 alloy in the pH 9 aqueous solution.     

晶粒细化对Cu-20Ag-30Cr合金在HCl溶液中腐蚀电化学行为的影响

采用机械合金化通过控制球磨时间制备不同晶粒尺寸的三元合金粉末,然后分别以真空热压工艺制备常规晶粒尺寸和纳米晶粒尺寸的Cu-20Ag-30Cr合金块状合金。并且利用PARM273A和M5210电化学综合测试系统对两种合金进行电化学腐蚀测试,通过测定电化学极化曲线和交流阻抗谱研究了常规晶粒尺寸和纳米晶粒尺寸的Cu-20Ag-30Cr合金在不同浓度HCl溶液中的腐蚀电化学行为。结果表明随着HCl浓度的增加,腐蚀电流密度随之持续增大,自腐蚀电位持续负移,传递电阻持续减小,表明合金的腐蚀程度加剧,合金的耐腐蚀性能减弱;在相同浓度的HCl溶液中,纳米晶粒尺寸的Cu-20Ag-30Cr合金的腐蚀电流密度明显高于高于Cu-20Ag-30Cr合金,表明经过晶粒细化合金腐蚀速度加快,其耐腐蚀性能下降。     

FeNiPB(Cu,Nb)纳米晶软磁材料的研究

通过扫描电子显微镜、透射电子显微镜及场发射扫描子显微镜并借助X－ray衍射仪分析研究了Fe基纲米晶软磁材料，结果表明：用机械合金化法可以合成FeNiPB(Cu,Nb）非晶合金，非晶粉末经晶化处理可以得到FeNiPB(Cu,Nb）纳米晶组织。     

机械合金化Fe40Ni40Si20纳米晶固溶体

机械合金化方法制备了Fe—Ni—Si三元系合金,利用X射线衍射仪研究了合金化过程中的 相变行为,计算了晶粒尺寸及微观应变。结果表明,经36小时球磨可形成α-Fe(bcc)和γ-Fe(fcc) 两相混合纳米晶固溶体;继续球磨,过饱和α相逐渐分解并向γ相转化,72小时后可得单相γ-Fe纳 米晶固溶体。球磨晶粒尺寸可达12 nm,微观应变随球磨时间先增加后减小。     

电刷镀纳米晶Ni-Co合金镀层组织结构与性能的研究

采用可溶性阳极电刷镀技术制备Ni-Co合金镀层,利用用X射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)等方法研究合金元素钴对镀层组织结构和性能的影响.结果表明:刷镀工艺下制备的镍钴合金镀层的晶粒尺寸都是纳米级;镍钴合金镀层都是单相面心立方固溶体结构,合金元素Co在镀层中具有固溶强化和细化晶粒的作用,随Co含量的增加,刷镀层的晶粒尺寸减小,硬度提高,耐磨性与耐腐蚀性能提高.