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1.
提出用溶胶粒子表面修饰方法,结合溶胶凝胶技术制备无机催化膜.该方法的基本原理是利用合适的金属配合物在胶粒表面的吸附作用,经溶胶凝胶过程,将活性组分结合到无机膜中.实验测定结果表明:(NiEDTA)2-,VO-3,MoO2-4,(Pd(NH3)4)2+,PdCl2-4,PtCl2-6和RhCl3-6可用来修饰AlOOH溶胶.以Pd/γAl2O3催化膜的制备为例,经三次溶胶凝胶过程,可制得无裂缺的厚度为9μm的Pd/γAl2O3催化膜,膜材料的平均孔直径为6nm,Pd被均匀地分布在膜的顶层,其平均粒径为23nm.  相似文献   

2.
本文研究了Pd(Ⅱ)与meso-四(4-甲基-3-磺基苯)卟啉(T(4M3SP)P)的显色反应在表面活性剂十二烷基磺酸钠(SDS)和抗坏血酸存在下,pH48的HAc-NaAc介质中,沸水浴加热,Pd(Ⅱ)与T(4M3SP)P形成1∶1(M∶L)配合物配合物最大吸收波长414nm,表观摩尔吸光系数ε=20×105L·mol-1·cm-1钯量在0-2.25μg/10μL范围内符合比耳定律本法应用于催化剂中痕量钯的测定,结果满意  相似文献   

3.
以银氨络离子和氯钯酸铵为前驱体制备了5%Ag01%Pd/γAl2O3催化剂,其低温深度氧化性能明显优于Ag或Pd单组分催化剂;T50和T95(CH3OH)分别为125℃和170℃,且不受O2及CO的阻抑.O2TPD的结果表明,随着在Ag组分中加入Pd及Pd加入量的增加,O2的低温脱附峰(Tp<200℃)逐渐减弱至消失;中温脱附峰(250℃<Tp<400℃)则向低温位移;高温脱附峰(Tp>500℃)峰面积逐渐增大,峰温比单组分钯的氧脱附峰高.Pd与Ag的相互作用(电荷转移)是造成上述现象的原因.  相似文献   

4.
低磷化学镀镍层性能的研究   总被引:8,自引:0,他引:8  
郭慧林  胡信国 《电化学》1996,2(1):84-88
低磷镀层(LP)在碱性和中性盐水条件下的耐蚀性较高磷镀层好,当LP镀层在350℃下热处理1h后,镀层在显微硬度从454Hv增加到890Hv。差热分析研究发现,在341.6℃和406.2℃有两个放热峰,分别对应于新相Ni5P2和Ni3P的形成,利用X射线衍射对镀层的结构进行分析,发现该镀层由非常细的微晶构成。  相似文献   

5.
利用恒电流沉积法,在p-Si上制备出不同W含量和不同结构的Ni-W薄膜,研究了镀液温度,pH值,电流密度对镀层组成的影响,结果表明,提高温度有利于获得高W含量的合金.随着镀层中W含量的增加,Ni面心立方晶格f.c.c发生正畸变,晶粒平均尺寸变小,当W含量达到56%以上时,晶粒小于2nm,薄膜呈非晶态结构.  相似文献   

6.
CeO2在Pd/γ-Al2O3催化剂中的助剂作用   总被引:11,自引:0,他引:11  
用色谱微反流动法技术考察了富氧和贫氧条件下,添加CeO2对Pd/γAl2O3催化剂上CO氧化反应的影响,并运用TPR、TPDMS及SEM等技术研究了CeO2Pd/γAl2O3催化剂.结果表明:CeO2、Pd的共助作用使CeO2Pd/γAl2O3催化剂TPR还原峰温向低温方向移动;CeO2的存在使Pd/γAl2O3催化剂表面的吸附氧容易脱出,从而改善了催化剂的氧化活性;CeO2、Pd间的强相互作用使催化剂上Pd元素的分散程度增加.  相似文献   

7.
研 究 了 Cu、 La、 Ba、 Ce 和 Co 等 多 种 金 属 氧 化 物 对 Pd / γAl2 O3 催 化 剂 在 3, 5二 羟 基 苯 甲 酸 转 移 加 氢 制 备3, 5二 氧 代 环 己 烷 羧 酸 反 应 中 的 活 性 影 响 , 发 现 镧 的 改 性 效 果 最 明 显 . 得 到 的 PdLaOx / γAl2 O3 催 化 剂 在 150 ℃下 还 原 , 催 化 3, 5二 羟 基 苯 甲 酸 转 移 加 氢 反 应 的 转 化 率 和 选 择 性 分 别 达 到 了 90. 6% 和 98. 2% . 在 150 ℃ 下 PdCl2被 还 原 为 Pd, 而 La 保 持 氧 化 态 . 经 TPR、 SEM、 TEM、 XPS 等 手 段 分 析 后 认 为 , 引 入 的 La 使 Pd 具 有 适 宜 的 粒 度 ,低 温 还 原 时 保 持 氧 化 态 的 La 与 载 体 产 生 相 互 作 用 , 并 对 Pd 的 转 移 加 氢 活 性 的 提 高 有 利 , 而 高 温 下 被 还 原 的 La则 对 提 高 Pd 的 活 性 不 利 .  相似文献   

8.
电沉积Ni-PSZ梯度镀层过程中阴极电流效率的研究   总被引:1,自引:0,他引:1  
李君  王殿龙  陈莉  胡信国 《电化学》1997,3(1):61-66
采用动电位扫描,电化学交流阻抗及扫描电子显微镜研究电沉积Ni-PSZ梯度镀层过程中阴极电流效率的变化规律及其机理.结果表明,Ni-PSZ复合镀层对氢的析出反应具有催化作用,在镀液中加入PSZ微粒后,能增大镍还原过电位,降低氢析出过电位,从而不断降低电沉积梯度镀层过程中的阴极电流效率.在电沉积Ni的过程中,有中间吸附相Ni+ads生成,PSZ微粒的加入能优先催化Hads,加速氢气析出  相似文献   

9.
电沉积Ni—Mo—P合金镀层在NaCl溶液中的腐蚀特性   总被引:1,自引:0,他引:1  
曾跃  姚素薇 《电化学》1998,4(4):380-387
用失重法,阳极率曲线,X-光电子能谱(XPS)以及俄歇电子能谱(AES)研究了电沉积Ni-Mo-P合金镀层在5%NaCl溶液中的腐蚀特性,非晶态Ni-Mo-P合金镀层比晶态Ni-Mo-P合金镀层有较低的腐蚀速度阳极极化曲线表明,Ni-Mo-P合金镀层中,镍的摩尔分数国0.719~0.868时,随镀层中磷含量的增加,腐蚀电位正移,而活化区的峰电流随镀层中钼含量的增加而增加,磷含量的活化区的峰电流以及  相似文献   

10.
甲醇羰基化制醋酸镍基双金属催化剂的研究   总被引:7,自引:3,他引:7  
在NiC催化剂中分别添加了九种不同的金属组分,在加压和碘甲烷助剂的存在下考察了第二金属组分及含量对甲醇羰基化反应性能的影响。结果表明:分别添加Pd、Mo、La三种组分可不同程度地提高NiC催化剂的羰基化活性,其中以Pd的效果最佳,Ni和Pd之间存在着明显的相互作用。Pd含量为1%时,羰基化活性达到最高,甲醇转化率和醋酸收率分别为9240%和4973%。Ni-PdC双金属催化剂的活性中心主要为Ni0,还有少量Pd0存在,Pd能够显著促进NiO的还原,这可能是氢溢流现象所致  相似文献   

11.
The effects of the Pd content (0–1 wt %) and the synthesis method (joint impregnation with Ni + Pd and Pd/Ni or Ni/Pd sequential impregnation) on the physicochemical and catalytic properties of Ni–Pd/CeZrO2/Al2O3 were studied in order to develop an efficient catalyst for the conversion of methane into hydrogen-containing gas. It was shown that variation in the palladium content and a change in the method used for the introduction of an active constituent into the support matrix make it possible to regulate the redox properties of nickel cations but do not affect the size of NiO particles (14.0 ± 0.5 nm) and the phase composition of the catalyst ((γ + δ)-Al2O3, CeZrO2 solid solution, and NiO). It was established that the activity of Ni–Pd catalysts in the reaction of autothermal methane reforming depends on the method of synthesis and increases in the following order: Ni + Pd < Ni/Pd < Pd/Ni. It was found that, as the Pd content of the Ni–Pd/CeZrO2/Al2O3 catalyst was decreased from 1 to 0.05 wt %, the ability for self-activation, high activity, and operational stability of the catalyst under the conditions of autothermal methane reforming remained unaffected: at 850°C, the yield of hydrogen was ~70% at a methane conversion of ~100% during a 24-h reaction.  相似文献   

12.
非晶态Ni-Ce-P合金的共沉积与耐蚀性能   总被引:8,自引:0,他引:8  
刘江  蒋雄  江琳才  朱则善 《电化学》2001,7(3):294-301
采用恒电位沉积、循环状安等方法研究了在水溶液中电沉积稀土合金的可能性 ,首次在含有CeCl3的弱酸性NaH2 PO2 镀液中获得了不同铈含量的Ni Ce P合金镀层 ,XPS、AES、XRD和SEM等实验技术表征了镀层的组成和结构 ,极化电阻和腐蚀电位的测试数据表明此镀层与Ni P无定形合金相比 ,具有更强的耐腐蚀能力 ,同时 ,讨论了沉积条件与镀层耐蚀性能的关系 ,结论是 :镀层中铈含量越高 ,其耐腐蚀性能越好 ,此外还对Ni Ce P的共沉积机理进行了初步探讨 ,指出在所研究的电沉积条件下 ,Ni Ce P合金共沉积可以用“诱导共沉积理论”合理解释  相似文献   

13.
Electroless Zn–Ni–P thin films were deposited on low carbon steel from an alkaline non‐cyanide aqueous electrolyte. The newly developed ternary alloys structure and microstructure investigations were carried out via X‐ray diffraction and SEM. Chemical composition of the coatings was investigated via energy dispersive spectroscopy. Polarization tests were used to study the corrosion properties of the coatings in a 3.5 wt.% NaCl solution. The results confirmed the high corrosion resistance of Zn–Ni–P alloy plated steel sheet. The surface analysis of the thin film samples before and after corrosion was performed by XPS. The incorporation of Zn in Ni–P thin film is proven for all initial samples to be as a mixture of zinc and zinc oxide, while nickel exists in +2 and +3 oxidized states. A passive film of a mixture of oxide and hydroxide of zinc and nickel forms on the surface and prevents the Zn–Ni–P thin films from corrosion. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

14.
Electroless deposition of Ni–Zn–P thin film was considered as a barrier film on a galvanic Zn or Ni–Zn sacrificial layer in a multicomponent corrosion protective coating on steel. The incorporation of zinc on the chemical composition of electroless Ni–Zn–P coating was studied. The effect of operating conditions such as temperature, pH value and concentration of zinc sulphate was investigated. Some physical characteristics such as morphology, structure, corrosion properties of Ni–Zn–P coatings were assessed in parallel with those of Ni–P. Inclusion of Zn to Ni–P is accompanied by the transformation of the coating structure from amorphous to crystalline. The effect of adding nonionic surfactant to the plating solution on the composition and surface morphologies was also investigated. The results indicate that nonionic surfactant has no effect on the Zn % in the deposit layer, but it affects the surface morphology and improves the corrosion resistance of Ni–Zn–P layers. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

15.
以磷酸氢二铵为磷源,硝酸镍为镍源,硝酸铝为助剂铝源,制备了nP/nNi=0.8,Al含量为1.06wt%~6.35wt%的一系列Al-Ni2P/SBA-15催化剂。采用XRD、TEM和N2吸脱附等技术对催化剂的结构进行了表征研究,以二苯并噻吩(DBT)作为模型化合物,在微型固定床反应器上对催化剂的加氢脱硫(HDS)性能进行了评价。结果表明,Al修饰的Al-Ni2P/SBA-15催化剂仍然保持介孔结构,当Al含量低于5.29wt%时,催化剂的物相主要是Ni2P,当Al含量在5.29wt%-6.35wt%之间时,催化剂的物相为Ni2P和Ni12P5。Al含量为4.24wt%的3-Al-Ni2P/SBA-15催化剂具有最好的二苯并噻吩加氢脱硫催化活性,在反应温度为360 ℃,反应压力为3.0 MP的条件下,3-Al-Ni2P/SBA-15催化剂对二苯并噻吩的转化率可达99.0%。  相似文献   

16.
Pure Ni and electroless Ni‐P coating (ENPC) were passivated by a chemical conversion treatment. The passive films formed on pure Ni and ENPCs (with content of P 2.9, 7.2 and 11.7 at.% respectively) were analyzed by X‐ray photoelectron spectroscopy (XPS). High‐resolution XPS was also used to analyze the chemical states of the elements detected in the passive films. The results indicated that the detected Ni and P were in elemental states, and no compound with Ni and P element was detected in passive film, meaning that Ni and P did not participate in the formation of the passive film. The content of film‐forming reaction product in passive film increases with the content of element P in Ni‐P coating, suggesting that the nonmetallic P in Ni‐P coating played an important role in the formation of the passive film. The XPS results were used to analyze the formation mechanism of the passive film. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

17.
Pinhole-free palladium/nickel (Pd/Ni) alloy membranes deposited on a porous stainless steel (SUS) support have been fabricated. The deposition was made by vacuum electrodeposition technique which could produce the alloy film less than 1 μm thick. This technique allows for the Pd/Ni alloy by employing Pd/Ni complex reagent, and typical Pd/Ni plating had compositions of 78% Pd and 22% Ni. In order to make the surface smooth and enhance the adhesive bond between the top layer and the substrate, a nascent porous SUS disk was treated sequently with submicron nickel powder and CuCN solution. The important parameters that can affect deposition were pore size, defects, and surface roughness of substrate. The membranes were characterized by permeation experiments with hydrogen and nitrogen at temperatures ranging from 623 to 823 K and pressures from 10.3 to 51.7 cmHg. The composite membranes prepared in this technique yielded excellent separation performance for hydrogen: hydrogen permeance of 5.79×10−2 cm3/cm2 cmHg s and hydrogen/nitrogen (H2/N2) selectivity was 4700 at 823 K.  相似文献   

18.
Carbon supported Palladium–Nickel alloys with various compositions (Pd–Ni/C) were synthesized by chemical reduction of the co-precipitated Pd and Ni hydroxides on carbon. The structure of these alloys was characterized using X-ray diffraction (XRD) analysis. The catalytic activity of Pd–Ni/C for oxygen reduction reaction (ORR) in alkaline media was studied using a glassy carbon rotating disk electrode (RDE). Pd/C showed ORR activity close to that of Pt/C. The activities of Pd–Ni (3:1)/C and Pd–Ni (1:1)/C were found unchanged compared with that of Pd/C. Ni/C showed about 175 mV lower onset potential than Pt/C, and the activity of Pd–Ni (1:3)/C was observed to be between that of Pd/C and Ni/C.  相似文献   

19.
通过两步还原法制备了Pd/Ni双金属催化剂.由于金属Pd原子在先行还原的Ni纳米粒子表面的外延生长以及其在Ni表面及Pd表面生长表现出的吉布斯自由能差异,最终导致了异结构Pd/Ni纳米粒子的形成.高分辨电子透射显微镜结果证实了异结构的存在,然而X射线衍射测量表明Pd/Ni纳米粒子具有类似于Pd的面心立方结构.制备的Pd/Ni纳米粒子与同等条件下合成的Pd纳米粒子相比对甲酸氧化呈现了更高的电催化活性,而且电催化稳定性也要明显优于纯Pd纳米粒子,证明Pd/Ni双金属催化剂是可选的直接甲酸燃料电池阳极催化剂.双金属催化剂对甲酸氧化电催化活性和稳定性增强可能是Ni原子的修饰改变了Pd粒子表面配位不饱和原子的电子结构所致.  相似文献   

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