ZnSe/CdSe核壳微球的制备与表征（英文）

在水热条件下,以水热法合成的Zn Se微米球为牺牲模板,成功制备出球形ZnSe/CdSe核壳结构纳米复合材料。讨论反应物ZnSe和Cd(NO3)2的不同摩尔比对最终产物形貌和结构的影响,并借助XRD,SEM,TEM和PL对Zn Se/Cd Se核壳结构纳米复合材料的性能进行表征。结果表明:当n(ZnSe):n(Cd(NO3)2大于1:1时可以制备出核壳结构,n(ZnSe):n(Cd(NO3)2)等于1时为实心球结构。PL光谱表明:Zn Se/Cd Se核壳结构纳米复合材料具有高的PL发射强度,且当n(ZnSe):n(Cd(NO3)2为1:0.5时发光性能最好。     

基于紫外光辐照法制备CuSe/ZnSe核壳结构纳米粒子

本文成功制备出以CuSe为核心、ZnSe为壳层,具有核壳结构的CuSe/ZnSe纳米粒子。首先采用回流冷凝法制备出CuSe纳米粒子（NPs）。然后,采用一种简单、快速的光化学方法即紫外光辐照法,室温下在CuSe NPs外包覆ZnSe壳层,最终得到CuSe/ZnSe核壳结构纳米粒子。利用X射线衍射(XRD)、能量色散谱仪(EDS)、透射电镜(TEM)、高分辨透射电镜(HRTEM)和光致发光光谱(PL)对合成的CuSe/ZnSe核壳NPs进行了表征。结果分析表明,合成的CuSe纳米粒子具有六方相结构,粒径平均大小在12 nm。制备出的CuSe/ZnSe纳米粒子的核壳结构清晰,生长的ZnSe壳层为立方闪锌矿结构,粒径大小约为15~45 nm。通过ZnSe壳层的包覆使CuSe在475 nm处产生蓝光发射,同时荧光强度显著增强。     

原位一步法合成Ag/Fe2O3磁性核壳纳米粒子

采用原位法在低温下一步合成Ag/Fe2O3磁性核壳纳米粒子,并采用XRD,TEM和UV光谱研究了Ag-Fe2O3核壳纳米复合材料的结构。结果表明,纳米银粒子表面被Fe2O3层包覆,Ag核的平均粒径大约为35nm,Fe2O3壳层平均厚度约为7.5nm或15nm,形成了核壳结构的电磁复合纳米粒子。在室温下,饱和磁化强度达到0.98(A·m2)·kg-1,矫顽力8.48×103A/m;Ag/Fe2O3核壳粒子的导电率达到0.62S/cm。通过此法可以比较容易的控制核和壳的尺寸以及复合粒子的单分散性,并得到较高的产率,在催化剂、医药、光电等领域有着广阔的应用前景。     

CdSe/ZnS/SiO_2多层核壳结构量子点材料的制备

纳米粒子表面包覆二氧化硅层形成的核/壳结构能减少表面缺陷,改善发光性能,保护纳米粒子核不受外界环境的影响。本实验在液体石蜡-油酸介质中首先制备CdSe量子点,再通过直接在反应体系中加入硫源和锌源的方法,在CdSe量子点的表面原位组装ZnS纳米层,得到CdSe(核)/ZnS(壳)结构量子点材料;然后利用反相微乳液方法在CdSe(核)/ZnS(壳)复合量子点的表面继续包覆SiO2层,得到CdSe/ZnS/SiO2多层核壳结构量子点材料。化学性质稳定的ZnS及SiO2材料的包覆使CdSe量子点材料的毒副作用降低,且没有降低单纯CdSe的发光效率,这种CdSe/ZnS/SiO2多层核壳结构量子点材料在探索新型载体、生物传感器、生物医疗、肿瘤的早期诊断和治疗等方面有广泛的应用前景。     

基于纳米晶的低温离子渗硫层油润滑条件下摩擦磨损性能

利用预压力滚压技术在堆焊修复层表面制备纳米晶层,用低温离子渗硫技术在纳米晶层表面制备Fe S固体润滑膜。利用CETR-3型多功能摩擦磨损试验机考察油润滑条件下堆焊层表面纳米晶/Fe S复合层的摩擦磨损性能。采用SEM、EDS、XRD和XPS对摩擦磨损前后的硫化层微观组织结构进行分析。结果表明:与原始低温离子渗硫层相比,基于纳米晶的渗硫层厚度增加了40%,硫化层更为密实,基于纳米晶的低温离子渗硫层摩擦因数明显降低,磨损量降低40%左右,承载能力明显提高。耐磨减摩性能提高是纳米晶层作用的结果,基于纳米晶的硫化层硫化物含量较高,Fe S相所占比例较高,高硬度的纳米晶层为表面润滑层起到良好的支撑,对于减摩性能的提高起到积极作用。     

电催化氧化甲醇反应低成本高活性的Pd核@Pt壳纳米粒子的光化学合成与表征研究(英文)

研究了PEG-丙酮体系中光化学合成Pd纳米粒子并在同一体系内在获得的Pd纳米粒子表面光化学还原Pt(IV)离子获得Pd核@Pt壳纳米粒子。通过改变Pd晶种对Pt(IV)的比例,能够有效调节复合粒子的Pt壳厚度。经HR-TEM和XPS分析,结果表明,获得的纳米粒子的平均粒径为5.3~7.1 nm,具有核-壳复合结构。电化学分析表明Pd:Pt摩尔比1:1、4:1的Pt核@Pt壳纳米粒子具有与Pt相似的催化活性和稳定性,且成本更低,可能被用作直接甲醇燃料电池阳极催化材料。     

PS@Au核壳复合粒子的可控合成及粒径对催化性能的影响

采用适当的化学镀工艺,通过对核层聚苯乙烯微球粒径的调制,可控合成了粒径连续可调的PS@Au核壳复合粒子,其球形度较高,无团聚,催化活性优良。利用SEM、XRD和UV-Vis,结合催化性能测试,研究了粒径对PS@Au核壳复合粒子催化性能的影响。结果表明:PS@Au核壳复合粒子较大的比表面积是其取得优良催化性能的物理本质,此外,粒径对其表面微观形貌、Au纳米粒子的生长方式及其催化性能都有显著影响。粒径较小时,核层曲率较大,Au纳米粒子呈发散式生长,表现出孤立的纳米颗粒状结构。此时,比表面积和表面能最大,催化活性最高。随着粒径增大,曲率逐渐减小,Au纳米颗粒表现出近似的薄膜状结构,比表面积和表面能逐渐降低,催化性能逐渐下降。核壳复合粒子的粒径达到400 nm时,Au纳米粒子的表面形貌开始由孤立的颗粒状结构向连续薄膜状过度。     

SnO_2@TiO_2核-壳纳米线的制备及其光催化性能

通过固-液-气(VLS)生长机制,利用化学气相沉积法(CVD)制备SnO_2纳米线。利用原子层沉积(ALD)以钛酸四异丙酯为前驱体在SnO_2纳米线表面沉积不同厚度的TiO_2壳层,形成SnO_2@TiO_2核-壳纳米线结构。通过中间Al_2O_3插层,分别制备出金红石和锐钛矿2种不同晶型的TiO_2,从而制备出2种不同复合结构的SnO_2@TiO_2核-壳纳米线。实验研究该复合结构中TiO_2的厚度与晶型对紫外光下光催化降解甲基橙溶液活性的影响。     

核/壳结构Fe/FeS_2纳米线结构与磁性能

利用电沉积及热硫化法制备了核/壳结构Fe/FeS2纳米线,研究了硫化过程对纳米线体系磁特性的影响。试验中,通过直流电沉积方法,可以在纳米孔洞高度有序排布的阳极氧化铝模板中制备Fe纳米线,之后部分溶去模板,再经450℃硫化处理,Fe纳米线表面可形成＂毛刷＂绒状物FeS2,从而形成核/壳结构Fe/FeS2纳米线。结果表明,随着高温硫化处理,Fe纳米线直径略有减小,且择优取向发生变化,并引起复合纳米线饱和磁化强度及矫顽力增强,主要认为是由于核/壳复合结构的形成引起纳米线体系静磁耦合作用降低所致。     

改进型原位限制聚合法制备纳米LiFePO_4/C核-壳材料及其电化学性能研究（英文）

采用改进型原位限制聚合法制备具有核-壳结构的纳米LiFePO_4/C颗粒.。并通过XRD,HRTEM,电化学工作站等测试手段研究了所制备粉体的相组成,微观结构和电化学性能。XRD结果表明所制备的LiFePO4/C具有晶型完整的橄榄行结构,壳层炭为作晶。HRTEM照片显示所制备的LiFePO4/C粒径在18.2~54.5 nm之间,炭层均匀包覆在LiFePO4颗粒外表面,厚度在2~10nm之间。700℃合成的LiFePO_4/C核-壳材料的首次放电容量为142 mAh/g,经过40次充放电循环后,容量保持在132 mAh/g,容量保持率在93.0%。其充放电容量受电子导电、锂离子扩散速率的共同影响。     

Synthesis and characterization of ZnSe/ZnS core/shell nanocrystals by aqueous reflux route

ZnSe/ZnS core/shell nanocrystals (NCs) with strong photoluminescence (PL) intensity and improved photochemical stability are synthesized through a simple water bath reflux route. Diffraction peaks can be indexed by zinc blend structure of ZnSe and ZnS. Transmission electron microscope (TEM) images reveal that each ZnSe NC (27 nm) is coated by a ZnS epitaxial shell. The ZnS shells are constitutive of crystalline and amorphous ZnS NC film with average thickness of 5 nm thick. The photoluminescence of ZnSe/ZnS core/shell NCs is also remarkably improved, which can be approved by the PL spectrum and laser-scanning confocal microscope test.     

Fe:ZnSe semiconductor nanocrystals: Synthesis, surface capping, and optical properties

Water-soluble Fe-doped ZnSe (Fe:ZnSe) nanocrystals (NCs) were synthesized by aqueous synthesis approach using thioglycolic acid (TGA) as capping agent. The undoped ZnSe and Fe:ZnSe NCs were well retained in the zinc blende structure, and the Fe dopants were well doped into the ZnSe NCs, as confirmed by X-ray photoelectron spectroscopy (XPS). The lattice constant of Fe:ZnSe NCs decreases slightly by the introduction of Fe, and Fe:ZnSe NCs exhibit a uniform size distribution with average grain size of ∼5 nm. The thioglycolic acid (TGA) was successfully capped on the surface of Fe:ZnSe NCs, confirmed by Fourier-transform-infrared (FT-IR) spectroscopy. The absorption edges of pure ZnSe and Fe:ZnSe NCs are blue-shifted compared to that of corresponding bulk ZnSe, indicating the quantum confinement effect, and the absorption edge of Fe:ZnSe NCs shows a slightly red shift with respect to the pure ZnSe NCs. The as-prepared Fe:ZnSe NCs exhibits an emission peak at ∼425 nm, and the photoluminescence (PL) intensity of the NCs has the maximum value when the Fe-doping concentration reaches 1.0 at%. It is of interest to note that the concentration quenching effect appears when the Fe-doping concentration is larger than 10.0 at%, and the underlying physical mechanisms were discussed.     

Facile and green route to highly luminescent ZnS-shelled CdSe nanocrystals

Highly luminescent CdSe/ZnS nanocrystals were obtained by adapting non-TOP-based synthesis and a subsequent two-phase ZnS shelling procedure:the core CdSe nanocrystals were synthesized in sole solvent paraffin liquid with cadmium oxide,elemental sele-nium,and oleic acid; the deposition of the ZnS shell was conducted by using zinc stearate in toluene and sodium sulfide in deionized water. The green and low-cost route was proved to be more efficient to constrain the size of core nanocrystals while tuning the ...     

ZnSe微球在不同水热条件下的制备与表征(英文)

以Zn(NO3)2·6H2O和Na2SeO3作为原料,通过水热法制备ZnSe纳米晶。探讨了水热反应温度、反应时间、NaOH浓度和N2H4·H2O的添加量对最终产物的相组成、显微形貌和颗粒尺寸的影响,并借助XRD、SEM、TEM、PL等测试手段对产物的相组成、显微形貌和颗粒尺寸进行表征。添加20 mL 1 mol/L NaOH溶液和10 mL N2H4·H2O溶液,在180°C的温度下水热反应4 h制备的产物主要是立方闪锌矿结构的ZnSe微球,所得的ZnSe微球从内到外是由平均尺寸约20 nm的ZnSe纳米晶组成。结果表明:较低的水热温度和较短的反应时间都不利于得到结晶好的纯相ZnSe,产物结晶性不好,而且还会产生杂相和有较多缺陷。添加适量浓度的NaOH和水合肼才能确保得到形貌均匀、发光性能好的ZnSe微球。     

ZnS纳米微晶的合成与光学性能的研究

采用离子络合法和自组装法在丙烯酸／2-丙烯酰胺-2-甲基丙烷磺酸／丙烯酸羟丙酯（Aa-AMPS-hT）三元嵌段共聚物中原位合成了ZnS纳米微晶。用TEM，SED，紫外可见吸收光谱分析仪，荧光光谱分析仪等手段对纳米晶的微观形貌、结构、光学性能进行表征。结果表明：所得产物为六方晶型纤锌矿结构，粒度随着硫化时间的延长而增大；随着硫化时间的缩短，紫外可见吸收光谱的吸收边和结构峰蓝移，荧光光谱的峰位逐渐蓝移，量子尺寸效应显著。     

A facile method to synthesize high-quality ZnS(Se) quantum dots for photoluminescence

Colloidal zinc sulfide (ZnS) quantum dots are synthesized by a solvothermal route from Zn(Ac)₂·2H₂O, sulfur powder and oleylamine at 120-240 °C. Microstructural, morphological, and optical properties of the as-synthesized ZnS quantum dots are characterized by X-ray diffraction analysis, transmission electron microscopy, UV-vis absorption spectroscopy, and photoluminescence spectroscopy. Results indicate that the obtained ZnS quantum dots distribute uniformly, the particle size is in the range between 1.7 nm and 3.1 nm, and the band gap decreases from 4.16 eV to 3.90 eV with an increase of the particle size. The size-dependent photoluminescence exhibits a strongly broadened peak accompanied by a pronounced blue-shift. It is also found that the size of the ZnS nanocrystals can be effectively controlled by adjusting synthesis temperature. It is shown that the present method is also applicable to synthesize other binary II-VI semiconductor materials, such as ZnSe quantum dots.     

Photoluminescence behavior and visible light photocatalytic activity of ZnO,ZnO/ZnS and ZnO/ZnS/α-Fe2O3 nanocomposites

In order to achieve effective, economic, and easily achievable photocatalyst for the degradation of dye methyl orange (MeO), ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe₂O₃ nanocomposites were prepared by simple chemical synthetic route in the aqueous medium. Phase, crystallinity, surface structure and surface behavior of the synthesized materials were determined by X-ray diffraction (XRD) and Brunauer–Emmett–Teller analysis (BET) techniques. XRD study established formation of good crystalline ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe₂O₃ nanomaterials. By using intensity of constituent peaks in the XRD pattern, the compositions of nanocomposites were determined. From the BET analysis, the prepared materials show mesoporous behavior, type IV curves along with H4 hysteresis. The ZnO/ZnS/α-Fe₂O₃ composite shows the largest surface area among three materials. From the UV–visible spectra, the band gap energy of the materials was determined. Photoluminescence spectra (PL) were used to determine the emission behavior and surface defects in the materials. In PL spectra, the intensity of UV peak of ZnO/ZnS is lowered than that of ZnO while in case of ZnO/ZnS/α-Fe₂O₃, the intensity further decreased. The visible emission spectra of ZnO/ZnS increased compared with ZnO while in ZnO/ZnS/α-Fe₂O₃ it is further increased compared with ZnO/ZnS. The as-synthesized materials were used as photocatalysts for the degradation of dye MeO. The photo-degradation data revealed that the ZnO/ZnS/α-Fe₂O₃ is the best photocatalyst among three specimens for the degradation of dye MeO. The decrease of intensity of UV emission peak and the increase of intensity of visible emission cause the decrease of recombination of electrons and holes which are ultimately responsible for the highest photocatalytic activity of ZnO/ZnS/α-Fe₂O₃.     

Fabrication and characteristics of spindle Fe2O3@Au core/shell particles

The fabrication and characteristics of spindle Fe2O3@Au core/shell particle were investigated, and the effect of the core/shell nanoparticles as the surface enhanced Raman spectroscopy (SERS)-active substrates was studied. By using the seed-catalyzed reduction technique, anisotropic Fe2O3@Au core/shell particles with spindle morphology were successfully prepared. The Fe2O3 particles with spindle morphology were initially prepared as original cores. The Au nanoparticles of 2 nm were attached onto the Fe2O3 particles through organosilane molecules. Uniform Au shell formed onto Fe2O3 core modified by Au nanoparticles through the in-situ reduction of HAuCl4. The shell thickness was controlled through regulating the concentration of HAuCl4 solution. The results of TEM, XRD and UV-vis characterization show that the core/shell particles with the original shape of the Fe2O3 particles are obtained and these surfaces are covered by Au shell completely. The surface enhanced Raman spectrum of the probe molecules adsorbed on these core/shell substrates is strong and the intensity is enhanced with the increase of the thickness of Au shell or the aspect ratio of particles. The spindle Fe2O3@Au core/shell particles exhibit optimum (SERS) activity.     

Synthesis and optical properties of yttria-doped ZrO2 nanopowders

Yttria-doped zirconia (YDZ) nanopowders were synthesized via a solvothermal route using ethanol as solvent. Evolution of crystal phases for different amount of yttria-doped samples were studied by X-ray diffraction (XRD). Morphology and component of the as-synthesized cubic YDZ were characterized by scanning electron microscopy (SEM) and energy dispersion spectrum (EDS). Defects of the sample were detected using ultraviolet–vis (UV–vis) absorption spectrum and photoluminescence (PL) spectrum. The results indicated that cubic structured nanocrystals can be obtained through doping 4 mol% Y₂O₃ into ZrO₂ lattice. The particles had sphere morphology with an average crystal size of 10 nm and agglomerated into bigger spheres with a diameter of about 120 nm. Mechanism of the agglomeration was also discussed. UV spectra showed two absorption peaks, red shift for both of the adsorption edges was observed. PL spectra with excitation wavelength of 260 and 420 nm revealed six fluorescence peaks which were regarded as various energy levels in the band gap and as the evidence of existence of oxygen vacancies in the as-synthesized sample.