海胆状ZnO纳米线阵列的制备及其光学性能

采用一种低成本的有效方法制备出了有序排列的海胆状ZnO纳米线阵列。首先利用自组装的方法得到了单层的聚苯乙烯(PS)小球,以其为模板用水热法在小球表面生长ZnO纳米线,得到了由PS小球和ZnO纳米线构成的海胆状结构。纳米线的直径均一,长度可通过水热反应时间进行控制。利用这种方法制备的一维ZnO纳米结构在传感器、太阳能电池及光催化领域有潜在的应用价值。     

Zno纳米粒子在PS中空微反应器中的合成与光学性能

通过种子乳液聚合合成核壳结构的聚甲基丙烯酸甲酯/聚苯乙烯(PMMA/PS)复合微球,通过酸碱溶胀法进一步制备出次微米级的PS中空微球. 将此中空微球作为微反应器,使在ZnO纳米粒子前驱体溶液中溶胀, 最终ZnO纳米粒子在PS中空微球中原位生成. 实验表明, 组成ZnO纳米粒子前驱体溶液的两种组 分(CH₃COO)₂Zn和LiOH的滴加顺序不同对最终生成的ZnO纳米粒子的尺寸和负载效率有很大的影响,但并不改变ZnO纳米粒子的晶型. 复合物的光致发光和UV-Vis吸     

疏水基团修饰的核-壳型NaYF_4/NaLuF_4∶Yb~(3+),Tm~(3+)纳米粒子设计制备

通过异质核诱导,利用溶剂热法在较低温度下合成了具有疏水表面的上转换发光稀土核-壳Na YF4/Na Lu F4∶20%Yb,1%Tm纳米粒子,并利用X射线衍射仪、透射电子显微镜、傅里叶变换红外吸收光谱仪以及荧光光谱仪等测试设备对其进行了结构、形貌和上转换光谱的表征。测试结果表明,纳米粒子核为立方相,壳层为六角相。核-壳型纳米粒子的尺寸平均在20 nm以下,分布较为均匀。在980 nm近红外光激发下,核-壳型纳米粒子发射出较强的紫色和紫外荧光,且发光强度明显高于同尺寸立方相Na Lu F4∶20%Yb,1%Tm纳米粒子。这表明利用异质核诱导的方法制备的核-壳型纳米粒子在生物医学领域具有更高的应用价值。     

甘氨酸燃烧法合成纳米ZnO-MgO及其紫外光发射

利用甘氨酸燃烧法制备了ZnOMgO纳米复合材料,并在不同温度进行热处理.通过X射线衍射、扫描电子显微镜和傅里叶变换红外吸收谱,对其升温过程中的结构变化进行了表征,研究了热处理温度对样品室温光致发光行为的影响.结果表明,复合材料的发光性能与纯ZnO相比有很大改善,经900℃热处理的纳米复合材料,其发射谱由一个强紫外发射带(峰值385nm)构成;当热处理温度低于900℃时,发光强度随热处理温度的升高而增强,进一步将热处理温度升至1000℃时发光强度又明显降低.发光强度主要受ZnO、MgO纳米晶的粒子尺寸、结晶完善程度,尤其是受两相纳米粒子之间相互作用的影响.同时发现选择合适的甘氨酸与硝酸根离子的摩尔比,对改善样品紫外发光特性也很重要.     

溶剂对石墨烯量子点荧光性质的影响

采用柠檬酸热解法制备了石墨烯量子点(GQDs),研究了非极性溶剂戊烷,极性溶剂乙醇、丙酮、乙二醇对GQDs荧光性质的影响。透射电子显微镜(TEM)和原子力显微镜(AFM)图像表明,制备的GQDs尺寸分布在2~12 nm(平均尺寸为4.9 nm),分散均匀,高度分布在0.5~2 nm。吸收光谱表明,GQDs具有明显的紫外吸收特性,吸收峰位于259 nm和274 nm。光致发光谱表明,GQDs的发光具有明显的溶剂依赖性。GQDs在极性溶剂乙醇、丙酮、乙二醇中,发光峰的位置依赖于激发波长,发射波长在可见光区。而在非极性溶剂戊烷中,GQDs表现出对激发波长不依赖的荧光性能,且发射波长在近紫外。     

离子注入及后退火方法制备SiO2基质中镶嵌ZnO纳米粒子的结构和光学性质

利用离子注入及后退火方法在光学纯的石英基片中注入3×1017cm-2剂量的Zn离子,然后在不同的退火条件下制备了高质量的镶嵌在SiO2基质中的ZnO纳米粒子.X射线衍射光谱的实验结果表明在氧气气氛、700℃退火温度和2小时退火时间条件下,得到了(002)择优取向镶嵌在SiO2基质中的ZnO纳米粒子;而在700℃退火温度、N2和O2气氛下顺次退火1小时,得到了比上述条件(002)择优取向更好的ZnO纳米粒子.室温下对用上述两种条件制备的镶嵌在SiO2基质中的ZnO纳米粒子观察到了自由激子吸收峰.室温光致发光谱中观察到了ZnO纳米粒子位于3.29eV处的强紫外发射,紫外发射强度与深能级发光强度之比为40,紫外发射峰的半高宽为96meV,晶体质量类似于分子束外延方法生长的ZnO.在低温(77K)光致发光谱中,较强的自由激子的紫外发光峰仍然存在.     

Al纳米颗粒表面等离激元对ZnO光致发光增强的研究

基于聚苯乙烯球自组装法,在P型氮化镓(P-GaN)衬底上制备了有序致密的掩模板;采用热蒸发法在该模板上沉积金属Al薄膜,通过甲苯溶液去除聚苯乙烯球,得到了金属Al纳米颗粒阵列;采用原子层沉积法,在Al纳米颗粒阵列表面依次沉积氧化铝(Al_2O_3)和氧化锌(ZnO).通过测试Al纳米颗粒阵列的消光谱以及ZnO薄膜的光致发光谱,研究了Al纳米颗粒表面等离激元与ZnO薄膜激子之间的耦合效应.实验结果表明:引入Al纳米颗粒后,在约380 nm位置附近的ZnO近带边发光峰积分强度增强了1.91倍.对Al纳米颗粒表面等离激元增强ZnO光致发光的机理进行探讨.     

La、Ce掺杂ZnO纳米晶的发光特性

共沉淀法制备了稀土镧、铈掺杂的ZnO半导体纳米晶。X射线衍射(XRD)结果表明:掺杂的ZnO纳米晶为六方纤锌矿结构,随掺杂浓度增加ZnO粒径减小。对铈掺杂纳米ZnO,以波长380nm激发,在443nm处出现了半峰宽较窄的强的蓝光发射峰;镧掺杂ZnO纳米晶则为从418~610nm的多峰宽带发射。     

ZnO/MCM-41复合材料的制备及其光谱性质

以硅酸钠(NaSiO3·9H2O)为硅源,三甲基十六烷基溴化铵(CTAB)为模板剂在碱性条件下水热合成介孔分子筛MCM-41,然后以其为主体,采用锌盐浸渍-灼烧的方法.在介孔分子筛MCM-41上负载了氧化锌(ZnO)纳米微粒,并通过扫描电子显微镜,红外光谱(1R).紫外可见吸收光谱(UV-Vis),N2-吸附脱附和荧光光谱等手段对产品进行了系列表征.结果表明,分子筛平均直径约为1.7μm,对不同温度下灼烧后得到的ZnO/MCM-41组装体的光谱性质进行研究表明介孔分子筛MCM-41的尺寸所限,制备出的ZnO粒子粒径小于2 nm.量子尺寸效应使得ZnO/MCM-41组装体中的ZnO纳米粒子的紫外可见吸收光谱及荧光光谱均发生蓝移.通过红外光谱分析得知ZnO负载到MCM-41上并没有改变介孔分子筛原有的骨架结构.     

纳米氧化锌的IR及其薄膜的UV光谱研究

采用溶胶-凝胶浸渍提拉法制备了纳米氧化锌薄膜。ZnO为六方晶系纤锌矿型,薄膜表面均匀致密,粒径尺寸约为10nm,400℃焙烧后的粉体在451cm-1处出现Zn-O伸缩振动,较体相材料向低波数移动了约29cm-1,膜中ZnO粒子的带边吸收位于363nm,其吸光度值与膜层数间的较好线性关系说明可以将氧化锌溶胶中的纳米粒子较好地转移到基片上。     

Influence of nanoparticle size on the pH-dependent structure of adsorbed proteins studied with quantitative localized surface plasmon spectroscopy

We have studied p H-dependent conformational transitions of Bovine Serum Albumin adsorbed onto different sizes of gold nanospheres. For larger spheres (D > 10 nm) there is evidence for a path-dependent extended state near p H 4, over a very small p H range. For smaller nanospheres (5nm and 10nm) the evidence for such a transition is either much weaker or completely suppressed. We suggest that the absence of the transition on small spheres is due to the fact that the protein adsorbed on such small spheres has already lost at least some of its tertiary structure. The results have important implications for the functionality of proteins adsorbed onto nanospheres or surfaces with nm scale roughness.     

Using sonochemistry for the fabrication of hollow ZnO microspheres

Hollow ZnO microspheres assembled by nanoparticles have been prepared by a sonochemical synthesis at room temperature using carbon spheres as template. The growth process of the precursor was investigated. The prepared hollow spheres were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM). The diameter of the obtained hollow spheres is about 500 nm, and the walls are composed of numerous ZnO aggregate nanocrystallines with diameters of 90 nm. A possible growth mechanism for the formation of ZnO microspheres has been proposed, in which carbon spheres play a crucial role in the formation of the wurtzite hollow ZnO microspheres. The specific structure of the hollow spheres may find applications in nanoelectronics, nanophotonics and nanomedicine.     

Controlling oxygen vacancies and properties of ZnO

Intrinsic defects in semiconductors play crucial roles on their electrical and optical properties. In this article, we report on a facile method to control concentration of oxygen vacancies inside ZnO nanostructures and related physical properties based on adjustment of thermal transformation conditions from ZnO₂ to ZnO, including annealing atmosphere and temperature. ZnO₂ spheres assembled with nanoparticles were formed through the reaction between zinc nitrate and hydrogen peroxide. Significantly, it was found that the adopted temperature and atmosphere have remarkable impact on the concentration of oxygen vacancies, which was revealed by the variations of featured Raman scattering peaks at 584 cm⁻¹. Furthermore, with the increase of oxygen vacancies inside ZnO, the optical band-gap was found to red-shift 350 meV and the room-temperature ferromagnetism became stronger up to 1.6 emu/mg. The defect formation and evolution were discussed according to the chemical equilibrium of decomposition reaction under special local heating environment. This work demonstrated that ZnO₂ decomposition is an effective process to control the defect states inside ZnO and related properties.     

二维氧化锌纳米阵列的制备及光学吸收特性研究

采用漂移法,在玻璃衬底上制备出粒径分别为117,350和500 nm单层、大面积的聚苯乙烯胶体球掩膜板,在已制得的掩膜板上用射频磁控溅射的方法沉积一层氧化锌薄膜,最后用有机溶液四氢呋喃(THF)浸泡去除聚苯乙烯胶体球,获得不同粒径的二维氧化锌纳米团簇。通过扫描电子显微镜和能量色散X射线光谱仪对样品的形貌及成份进行表征,表明所制得样品为有序分布的蜂窝网状氧化锌纳米阵列。在室温下,通过吸收光谱仪测试样品在300～800 nm波长范围内的吸收光谱,结果表明对于具有不同尺寸晶粒的氧化锌纳米团簇样品,随着所采用的聚苯乙烯胶体球粒径的增大,即氧化锌纳米团簇粒径的增加,光吸收峰出现了宽化和红移;随着溅射时间的延长,即氧化锌薄膜膜厚的增加,光吸收率提高。此外,对氧化锌纳米团簇阵列的光吸收特性进行了基于离散偶极子近似的理论计算从而获得任意形状和尺寸粒子的吸收。目前,文献报道中用此理论计算各种形状的纳米金、银等金属的结果与实验结果相符,但是应用离散偶极子的近似理论计算氧化锌纳米颗粒的报道很少。应用此理论计算三角棱台形状的氧化锌光学吸收特性,根据氧化锌薄膜介电常数和膜厚的变化进行光吸收特性的模拟,并解释了实验结果。     

Synthesis of Na-doped ZnO nanowires and their photocatalytic properties

Na-doped ZnO nanowires with an average diameter of ∼40 nm have been fabricated by a thermal decomposition route at temperature around 400 °C. Their properties have been investigated using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), UV-visible spectroscopy, Raman spectra, and photoluminescence (PL) spectroscopy. Room temperature photoluminescence (RT-PL) showed that the as-synthesized ZnO samples exhibited strong visible emission with a major peak at 420 nm. Furthermore, intensity of the visible emission increased and then decreased with increase in Na concentration. The improvement of visible emission at 420 nm in the Na-doped ZnO samples should be a result of the surface defects increased by doping of Na in zinc oxide. In addition, photocatalytic studies indicated that these nanomaterials showed good photocatalytic performance for organic pollutants in water.     

Sol–gel derived zinc oxide films: Effect of deposition parameters on structure, microstructure and photoluminescence properties

ZnO films were prepared by sol–gel method and deposited onto glass substrates with spin coating system. XRD patterns and FESEM analysis were used to investigate the effect of deposition parameters such as spin speed and molar concentration on the crystallinity and surface morphology of the films. XRD patterns show that ZnO films are polycrystalline with type-wurtzite hexagonal structure. The film which is deposited at 4000 rpm and with 0.5 M sol has the best crystallinity. The FESEM micrographs showed that the surface morphology of the films was not significantly affected from the spin speed. FESEM micrographs showed that the crystallite sizes of 1000, 4000 and 5000 rpm are almost same. But 2000 and 3000 rpm have lower crystallite sizes than the others. Also, the amount of voids in the 1 M was found higher. The effect of spin speed and molar concentration on the optical properties of ZnO films was investigated by PL spectroscopy. The electrical properties of the ZnO films were investigated by using two probe methods in dark. The highest conductivity values were obtained for ZnO films prepared by 4000 spin speed and 0.5 M of concentration.     

ZnO spheres and nanorods formation: their dependence on agitation in solution synthesis

ZnO nanostructures including nanorods, dense, and partially hollow spheres were synthesized via a solution synthesis method with temperature ranging from 65 to 95 °C. Scanning electron microscopy (SEM) revealed that the diameter of the spheres is in the range of 200–500 nm. Transmission electron microscopy (TEM) showed that some of the spheres are hollow or partially hollow. Powder X-ray Diffraction (XRD) and TEM-Selected area electron diffraction (SAED) analysis showed that the spheres consist of polycrystalline nanoparticles. It was found for the first time that the agitation during the synthesis plays a critical role on morphology of the ZnO nanostructures formed in solution. The oriented attachment of nanocrystals without agitation during the synthesis could guide the nanocrystals to form an ordered nanorod structure. However, the disordered aggregation of the nanocrystals under shear force resulted in a spherical morphology. It was also found that the composition of spheres is different from that of nanorods: the spheres consist of both ZnO and Zn(OH)₂, but nanorods consist of single-crystal ZnO only. Zn(OH)₂ presented in the spheres could decompose to ZnO by calcination, resulting in the formation of hollow spheres.     

ZnO纳米/微米结构传感器对乙醇气敏性研究

采用化学气相法分别在石英舟内表面和单晶硅衬底上制备了ZnO微米片、纳米线、微米四足体以及微米球4种结构,并制作了相应的气敏传感器。扫描电子显微镜、气敏测试仪等结果显示：合成的ZnO纳米/微米结构尺寸在200 nm~100 μm之间,传感器最佳工作电流区间为120~130 mA,其中微米四足体制备的传感器灵敏度高达127,展现出优异的气敏特性。在4种结构中,微米四足体材料内部的V_O缺陷含量最高,结合气敏测试与荧光光谱结果,我们认为材料内部的V_O缺陷含量是影响材料气敏特性的最重要因素。     

Preparation and photocatalytic properties of hybrid core–shell reusable CoFe2O4–ZnO nanospheres

Magnetically separable and reusable core–shell CoFe₂O₄–ZnO photocatalyst nanospheres were prepared by the hydrothermal synthesis technique using glucose derived carbon nanospheres as the template. The morphology and the phase of core–shell hybrid structure of CoFe₂O₄–ZnO were assessed via TEM, SEM and XRD. The magnetic composite showed high UV photocatalytic activity for the degradation of methylene blue in water. The photocatalytic activity was found to be ZnO shell thickness dependent. Thicker ZnO shells lead to higher rate of photocatalytic activity. Hybrid nanospheres recovered using an external magnetic field demonstrated good repeatability of photocatalytic activity. These results promise the reusability of the hybrid nanospheres for photocatalytic activity.     

Controlled synthesis of cuprous oxide nanospheres and copper sulfide hollow nanospheres

Uniform Cu₂O nanospheres have been successfully synthesized by reducing CuSO₄ with ascorbic acid in sucrose solution at room temperature. The diameter of the Cu₂O nanospheres can be tuned from 90 to 280 nm by adding different amounts of sucrose in the solution. Furthermore, CuS hollow nanospheres with different diameters have been obtained based on the Kirkendall effect using the as-prepared Cu₂O nanospheres as sacrificial templates. Cu₂O/Cu_7.2S₄ core/shell nanospheres and Cu_7.2S₄ hollow nanospheres are obtained as the intermediate products at different stages of the conversion process. Through the post-treatment of sodium citrate solution, Cu_7.2S₄ hollow nanospheres can be changed into CuS hollow nanospheres. The products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field-emission scanning electron microscopy (FESEM). Optical properties of the products have also been studied.