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1.
利用表面活性剂十二烷基磺酸钠(SDSN)的调控合成不同粒径的硒模板和铂纳米空球(Pthollow),并将其修饰于玻碳(GC)基底即可制得Pthollow/GC电极;采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HR-TEM)和X射线光电子能谱等观察表征了Pthollow样品的形貌与组成;以甲醇为探针分子,研究Pthollow/GC和电沉积铂电极(Ptnano/GC)对甲醇氧化的电催化活性. 结果表明,由铂原子簇团构筑的多孔铂纳米空球粒径均匀,分散性好;用4 μmol·L-1 SDSN控制合成的直径为130 nm的Pthollow制备的Pthollow/GC电极对甲醇氧化的电催化活性最佳.  相似文献   

2.
本文以约120nm的α-Se球为模板,抗坏血酸为还原剂,H2PtCl6为前驱体,通过改变氯铂酸的用量可控合成了不同壳厚的纳米铂空球(Pthollow)及其修饰玻碳(GC)电极(Pthollow/GC);采用扫描电子显微镜(SEM)、高分辨透射电子显微镜(HR-TEM)、能量色散X射线(EDX)谱、X射线衍射(X-ray diffraction,XRD)谱和选区电子衍射(SAED)图等表征其形貌、组成与结构;以甲酸为探针分子,采用循环伏安和计时电流法研究了甲酸在Pthollow/GC电极上的电催化氧化行为.结果表明,所制备的Pthollow分散性好、粒径比较均匀,其多孔球壳是由多维多级的铂原子团簇所构建,呈现多晶铂的结构与性质;当RPt/Se=1.2时,所合成Pthollow。对甲酸的电催化氧化活性最高,且明显优于电沉积铂(Ptnano)修饰GC电极(Ptnano/GC),为直接甲酸燃料电池(DFAFC)阳极材料的优化制备提供了一定的实验与理论依据,有潜在的应用推广价值.  相似文献   

3.
以粒径为100nm的硒球作模板,在室温下批量合成了粒径约110nm、壳厚约5 nm的铂空球.采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HR-TEM)、选区电子衍射(SAED)、X射线衍射(XRD)、能量色散X射线谱(EDX)等检测技术表征了其形貌与结构;以甲醇为探针分子研究了铂纳米空球修饰玻碳电极对甲醇电氧化的催化性能.结果表明,由铂原子簇团构筑的多孔铂空球粒径均匀、分散性好、结构稳定、比表面积大、传质性能好,是甲醇氧化的理想催化材料.循环伏安(CV)结果表明:当甲醇氧化的电流密度0.10 mA·cm-2,正扫时,铂纳米空球的氧化电位与实心铂纳米粒子及铂黑相比,分别负移了约110和64mV;负扫时,前者比后两者分别负移了约51与13 mV.经800圈循环伏安扫描后,正扫时,甲醇在铂纳米空球上氧化峰的电流密度为实心铂纳米粒子及铂黑上的13和15倍;负扫时,前者为后两者的19和38倍.表明铂纳米空球对甲醇氧化具有较好的催化活性和稳定性.  相似文献   

4.
以无定形硒溶胶为模板制备了不同硒覆盖度(θSe)(θSe=0.49,0.39,0.06,0)的Pt-Se和Pt纳米空球(分别记为(Pt-Se)HN和PtHN),发展了利用亚硫酸盐彻底除去核壳纳米粒子上Se的方法.对获得的纳米空球进行了形貌和结构的表征,结果表明所制备的(Pt-Se)HN粒径均匀,分散性好,球壳呈多孔结构.以其作为电催化剂制备了(Pt-Se)HN修饰的玻碳(GC)电极((Pt-Se)HN/GC),利用常规电化学方法比较该电极与PtHN/GC和商用碳载铂(Pt/C)修饰GC(Pt/C/GC)电极对甲酸的催化氧化作用,发现对甲酸氧化的活性顺序为(Pt-Se)HN/GCPtHN/GCPt/C/GC.三种电极催化甲酸氧化的机理有所不同:前者更倾向于通过弱吸附中间体直接氧化成CO2的单途径机理进行,后两者则通过强吸附和弱吸附中间体的双途径机理进行.在一定Se覆盖度条件下,(Pt-Se)HN/GC对甲酸的氧化有助催化作用.  相似文献   

5.
王洁莹  陈燕鑫  陈声培  王鹏  孙世刚 《应用化学》2010,27(11):1296-1300
通过循环伏安法(CV)在玻碳(GC)电极表面电沉积出分布较为均匀的纳米Fe粒子,制得纳米Fe粒子修饰的GC(纳米Fe/GC)电极,再经“电荷置换”制得具有Fe核Pt壳结构的纳米粒子修饰的(纳米PtFe/GC)电极。 SEM结果显示,纳米Fe/GC和纳米PtFe/GC表面粒子的形貌均呈立方体形,分布较为均匀,粒径在60 nm左右。 纳米PtFe/GC电极对亚硝酸盐的还原具有很高的电催化活性。 3种电极的电催化活性顺序依次为:纳米Fe/GC<纳米Pt/GC<纳米PtFe/GC。 相对于纳米Pt/GC电极,纳米PtFe/GC电极的起始还原电位(Ei)正移了0.14 V,还原峰电流(ip)增大了3倍。  相似文献   

6.
以100 nm的Au粒子为核,抗坏血酸为还原剂,H2PtCl6·6H2O为前驱体,合成了Pt包Au核壳结构纳米粒子( Au@ Pt)及其修饰的玻碳(GC)电极(Au@ Pt/GC).采用旋转圆盘电极等常规电化学方法,比较了Au@ Pt/GC和商用碳载铂(Pt/C)修饰的玻碳电极(Pt/C/GC)催化O2还原反应活性及耐甲醇性能,发现Au@ Pt纳米粒子在铂用量很低的情况下,其催化O2还原反应活性仍与商用Pt/C相当,而且还具有优良的耐甲醇性能;其催化O2还原反应机理按O2直接还原成H2O的四电子历程进行.  相似文献   

7.
采用绿色还原剂抗坏血酸,一步法制备纳米铂/石墨烯。对其进行X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)形貌结构表征,铂纳米粒子均匀分散于纳米石墨烯片层褶皱间,有效减少了团聚现象。运用循环伏安法(CV)和计时电流法(CA)研究纳米铂/石墨烯对甲醇电催化氧化活性和稳定性,通过交流阻抗(EIS)定量测定,发现铂/石墨烯比铂具有更优异的电荷传输性能,电荷转移阻抗下降了34.8%。计时电量法(CC)测定得到甲醇在铂/石墨烯电极的表面扩散系数为1.42×10~(-9) cm~2·s~(-1)。与铂纳米粒子相比,纳米铂/石墨烯对甲醇电催化氧化具有更高的活性和稳定性,显著提高电极催化活性表面积和电荷传输及转移性能。  相似文献   

8.
以Keggin结构硅钨杂多酸H4SiW12O40(SiW12)为光催化还原剂,通过光化学还原法制备Au/Ag核壳结构纳米粒子. 透射电子显微镜分析显示,所得纳米粒子粒径为30~40 nm,呈均匀分散的球形颗粒,该制备方法的特点是可以较好的避免单金属纳米粒子的形成. 将Au/Ag核壳纳米粒子修饰到具有PVP膜的玻碳电极表面,得到SiW12-(Au/Ag)-PVP多层膜修饰电极. 该修饰电极在0.5 mol/L H2SO4介质中具有良好的电化学响应,在0~-0.75 V电位范围内,出现了3对归属于SiW12的氧化还原峰,且电极性能稳定,灵敏度高. 对H2O2的电催化还原性能明显优于单金属Ag纳米粒子修饰电极,说明Au核的存在可以很好的改善Ag的电催化性能,Au和Ag之间存在相互协同催化作用.  相似文献   

9.
应用循环伏安法(CV),扫描电子显微镜(SEM)和电化学原位红外反射光谱(in situFTIRS)研究了不同介质对碳载铂纳米薄膜电极(Pt/GC)的表面结构以及该薄膜电极对甲酸电催化氧化性能的影响.结果表明,使用不同介质的镀铂溶液,均可电沉积出分布较为均匀的Pt粒子,但其尺寸与形貌却相差很大.当以H2SO4作介质,由循环伏安法于玻碳电极上电沉积Pt得到的(Pt/GC1)电极,其Pt粒子粒径约100~200 nm;而在HClO4介质得到的(Pt/GC2)电极,则含有两种Pt微晶:其一是立方体形,粒径约200 nm,其二为菜花状,粒径约400 nm.电化学循环伏安和原位红外反射光谱测试指明,不同介质制备的Pt/GC电极对甲酸的电催化氧化均表现出与本体铂电极(Pt)相类似的特性,即可通过活性中间体或毒性中间体将甲酸氧化至CO2,但不同结构的Pt/GC电极具有不同的电催化活性.进一步以Sb或Pb修饰Pt/GC电极,不仅可以有效地抑制毒性中间体CO的生成,而且还能显著提高其电催化活性.比较本文研究的7种电极,其电催化活性顺序依次为:Sb-Pt/GC2>Pb-Pt/GC2>Pb-Pt/GC1>Sb-Pt/GC1>Pt/GC2>Pt/GC1>Pt.  相似文献   

10.
Aucore Ptshell纳米粒子对甲醇氧化的电催化性能研究   总被引:3,自引:0,他引:3  
应用两步化学还原法制备不同厚度的AucorePtshell纳米粒子,经紫外可见光谱(UV-V is)、透射电子显微镜(TEM)表征.该金纳米颗粒经化学还原包裹铂后平均粒径明显增大,调节金与铂的含量可获得不同包裹厚度的AucorePtshell纳米粒子.循环伏安法研究表明,粒径为70~80 nm的AucorePtshell纳米粒子对甲醇的氧化具有较好的电催化活性,并且其电催化性能随着电位循环扫描次数的增加而增强.  相似文献   

11.
An improved method to prepare alkylamine-stabilized Pt and Ru nanoparticles based on the original Brust’s procedure [J. Chem. Soc., Chem. Commun. (1994) 801] has been developed. The new method involves, firstly, mixing an aqueous solution of metal salts such as PtCl62−, PtCl42− or Ru3+ with an ethanol solution of dodecylamine; extracting the metal ions into a toluene layer; and finally reducing the metal ions to their zero valent states using NaBH4. Alkylamine-stabilized Pt nanoparticles prepared this way had a polyhedral or wormlike appearance, depending closely on the chemical nature of the metal precursor salts being used. On the contrary, dodecylamine-stabilized ruthenium nanoparticles were predominantly spherical. The particle formation and growth processes in the hydrocarbon layer could be influenced by the different ways dodecylamine was bound to H2PtCl6, K2PtCl4 or RuCl3 at the precursor stage.  相似文献   

12.
Au/Ag核-壳结构纳米粒子的制备及其SERS效应   总被引:1,自引:0,他引:1  
随着大量有关表面增强拉曼散射 (SERS)的实验和理论研究的开展 ,金属纳米粒子作为一类重要的 SERS增强介质 ,已引起了人们浓厚的研究兴趣 [1] .而 Au和 Ag作为最常用的活性基底物质 ,更是研究的热点 [2 ,3 ] .最近 ,美国印第安那大学的 Nie等 [4 ] 在单个银纳米粒子上 ,观察到高达 1 0 14 ~ 1 0 15的SERS因子 .同时 ,他们的另外一项工作表明银纳米粒子的形状和大小对 SERS活性有很大影响 [5] .但是 ,由于 Ag溶胶制备的重复性较差 ,且粒度分布不均匀 ,通过控制银颗粒大小而调控 SERS活性是相当困难的[6] .与 Ag相比 ,Au在可见光…  相似文献   

13.
食品安全事关人民群众的身体健康和生命安全,而食源性致病菌是食品安全的主要影响因素。由食源性致病菌引起的疾病和死亡持续威胁着全球的公共卫生安全。因此,开发快速、准确且灵敏的食源性致病菌检测方法是预防食源性疾病暴发和确保食品安全的关键。常规检测方法费时费力,需要昂贵的设备和专业的人员,应用受限。近年来,随着纳米技术的快速发展,纳米粒子凭借其小尺寸、高比表面积和高反应活性等理化特性成为食源性致病菌检测领域的研究热点。此外,将识别元件修饰于纳米粒子表面并结合新颖的分析技术,能提高检测的特异性和灵敏度。该综述主要总结和比较了磁性纳米粒子、贵金属纳米粒子、荧光纳米粒子和二氧化硅纳米粒子在食源性致病菌检测中的应用,以期为食源性致病菌的快速分析提供思路。  相似文献   

14.
由于纳米材料独特的表面效应、电子效应及量子尺寸效应 ,已被广泛应用于各个领域 .有关纳米材料研究的报道很多 [1~ 7] ,大部分是关于纳米材料的制备[1~ 4 ] 及其特性研究 .对于纳米金属及纳米氧化物之间相互作用的研究迄今尚未见报道 .本文采用超声分散和机械研磨法物理混合纳米金属铜粉和纳米氧化锌 ,借助 EPR和 XPS技术对样品进行了表征 ,发现混合体系出现了 Cu2 + 的顺磁信号 ,Zn L3M4 5M4 5俄歇动能和 O1s的电子结合能亦发生了变化 ,表明纳米 Cu0 和纳米 Zn O之间存在相互作用 ,作用形式为 Cu— O—Zn.1 实验部分1 .1 样品…  相似文献   

15.
Jans H  Jans K  Demeyer PJ  Knez K  Stakenborg T  Maes G  Lagae L 《Talanta》2011,83(5):5-1585
In this study a double-bead sandwich assay, employing magnetic nanoparticles and gold nanoparticles is proposed. The magnetic nanoparticles allow specific capturing of the analyte in biological samples, while the optical properties of the gold nanoparticles provide the signal transduction. We demonstrated that a major improvement in the assay sensitivity was obtained by selecting an optimal gold nanoparticle size (60 nm). A detection limit of 5-8 ng/mL, a sensitivity of 0.6-0.8 (pg/mL)−1 and a dynamic range of 3 orders of magnitude were achieved without any further amplification using the detection of prostate specific antigen in serum as a model system. The proposed assay has the ability to be easily implemented within a microfluidic device for point-of-care applications whereby the readout can be executed by a fast and cheap optical measurement.  相似文献   

16.
Bottom-up nanoparticle (NP) formation is assumed to begin with the reduction of the precursor metallic ions to form zero-valent atoms. Studies in which this assumption was made are reviewed. The standard reduction potential for the formation of aqueous metallic atoms—E0(Mn+aq/M0aq)—is significantly lower than the usual standard reduction potential for reducing metallic ions Mn+ in aqueous solution to a metal in solid state. E0(Mn+aq/M0solid). E0(Mn+aq/M0aq) values are negative for many typical metals, including Ag and Au, for which E0(Mn+aq/M0solid) is positive. Therefore, many common moderate reduction agents that do not have significantly high negative reduction standard potentials (e.g., hydrogen, carbon monoxide, citrate, hydroxylamine, formaldehyde, ascorbate, squartic acid, and BH4), and cannot reduce the metallic cations to zero-valent atoms, indicating that the mechanism of NP production should be reconsidered. Both AgNP and AuNP formations were found to be multi-step processes that begin with the formation of clusters constructed from a skeleton of M+-M+ (M = Ag or Au) bonds that is followed by the reduction of a cation M+ in the cluster to M0, to form Mn0 via the formation of NPs. The plausibility of M+-M+ formation is reviewed. Studies that suggest a revised mechanism for the formation of AgNPs and AuNPs are also reviewed.  相似文献   

17.
Magnetic nanoadsorbents using Fe3O4 nanoparticles as cores and poly(methyl acrylic acid) (PMAA) as ionic exchange groups were prepared through our novel approach. Two steps were involved in this approach: the first was to functionalize the magnetic nanoparticles (MNPs) with methacrylate double bonds via the combination of ligand exchange and condensation of methacryloxypropyltrimethoxysilane(MPS); the second was to graft PMAA chains onto the surface of MNPs through radical polymerization. The success of the various surface functionalization steps was ascertained using FTIR and XPS. The as‐synthesized PMAA‐coated MNPs were effective in binding bovine serum albumin (BSA) with a high capacity of 1 300 mg · g−1.

  相似文献   


18.
It was established that PbS nanoparticles significantly increase the rate of formation of lead selenide during the reaction of Pb(NO3)2 and Na2SeSO3 in aqueous solutions of polymers. It was shown that the reaction product consists of PbS/PbSe nanoparticles with a “PbS core-PbSe shell” structure. A correlation was found between the forbidden band widths of the PbS nanoparticles and the PbS/PbSe nanostructures formed during the reaction. __________ Translated from Teoreticheskaya i éksperimental’naya Khimiya, Vol. 42, No. 6, pp. 339–344, November–December, 2006.  相似文献   

19.
Nanoparticles sized tens of nm with not only a highly complex but also a highly regular nanostructure, although ubiquitous in nature, are very difficult to prepare artificially. Herein, we report efficient solution‐based preparation of narrow‐disperse ABC three‐segment hierarchical nanoparticles (HNPs) with a size of tens of nm through a three‐level hierarchical self‐assembly of A‐b‐B‐b‐C triblock copolymers in solution. An ABC HNP is composed of three nanoparticles, A, B, and C that are linearly connected; in the ABC HNP, the B nanoparticle is sandwiched between the A and C nanoparticles. The method for the preparation is highly efficient, because all of the A‐b‐B‐b‐C chains in the solution are converted into the ABC HNPs. Furthermore, the ABC HNPs self‐assembled into Θ‐shaped HNPs tens nm in size. Both the ABC and Θ‐shaped HNPs, are highly complex but highly regular, and are novel HNPs, and they should be very promising for addressing various theoretical and practical problems.  相似文献   

20.
电化学沉积法制备金(核)-铜(壳)纳米粒子阵列   总被引:2,自引:0,他引:2  
曹林有  刁鹏  刘忠范 《物理化学学报》2002,18(12):1062-1067
以组装在有机分子自组装膜/金基底电极上的Au纳米粒子阵列为电化学沉积模板,制备了金(核)-铜 (壳)纳米粒子阵列.选用巯基十一胺(AUDT)和巯基癸烷(DT)混合自组装膜作为基底电极与Au纳米粒子的耦联层,可以在一定的电位下实现金属Cu在Au纳米粒子上的选择性沉积.将沉积电位控制在-0.03 V(vs SCE)时,沉积初期(t ≤ 15 s,沉积粒子粒径 ≤ 20 nm )金(核)-铜 (壳)粒子具有良好的单分散性和近似球形,而且粒径实验值同计算值非常吻合.  相似文献   

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