电爆炸丝法制备纳米Al2O3粉末

 设计了电爆炸金属丝产生纳米金属氧化物粉末的实验装置，金属丝电爆炸腔采用圆筒结构，纳米粉末经过微孔滤膜过滤收集。成功制备了纳米Al₂O₃粉末，其平均粒度达到64.9 nm。对电爆炸金属丝产生纳米Al₂O₃粉末的物理条件进行了研究。结果表明实验条件对粉末粒度有重要影响：随气压的增加粉末平均粒度变大；随金属丝直径增大粉末平均粒度变大；粉末的平均粒度与电容器的初始储能也有一定的关系。     

Ba0.98Ce0.8Tm0.2O3-α的离子导电性及其燃料电池性能

用高温固相反应法制备了Ba_0.98Ce_0.8Tm_0.2O_3-α钙钛矿型氧化物固溶体,粉末X射线衍射表明该固溶体为单相. 用交流阻抗谱技术和气体浓差电池方法研究了样品在500～900 oC、不同气体气氛中的导电性,以及该样品为固体电解质的氢-空气燃料电池性能. 该电池能稳定地工作,在900 oC时,电池的最大功率密度为110.2 mW/cm²,高于以Ba_xCe_0.8RE_0.2O₃^- (x≤1, RE=Y, Eu, Ho)为固体电解质的氢-空气燃料电池的功率密度     

掺杂质子化石墨相氮化碳增强碳基太阳能电池中钙钛矿的结晶

钙钛矿层的品质极大影响钙钛矿太阳能电池性能. 然而,在溶液法生成多晶钙钛矿膜过程中会不可避免地形成缺陷和陷阱位. 通过在钙钛矿层中嵌入添加物改善钙钛矿晶化,用于减少和钝化缺陷是非常重要的. 本文合成一种环境友好的二维纳米材料质子化石墨相氮化碳(p-g-C₃N₄),并掺杂于碳基钙太阳能电池的钙钛矿层中. 实验证明,在钙钛矿前驱体溶液中添加p-g-C₃N₄不仅能调解碘铅甲胺(MAPbI₃)结晶的成核和生长速率,获得大晶粒尺寸的平滑表面,还能减少钙钛矿层的本征缺陷. 质子化过程在氮化碳表面引入活性基团-NH₂/-NH₃,它们和钙钛矿晶体表面N-H键发生强化学作用,有效地钝化电子陷阱,提高钙钛矿结晶质量. 结果表明,与不掺杂的对照电池(效率为4.48%)和掺杂石墨相氮化碳(g-C₃N₄)电池(效率为5.93%)相比,掺杂质子化石墨相氮化碳(p-g-C₃N₄)的电池获得了6.61%的较高效率. 本工作展示了一种通过掺杂改性添加物改善钙钛矿膜的简单方法,为碳基钙钛矿太阳能电池的低成本制备提供了建议.     

金属醇盐法制备Ta2O5气凝胶

 以乙醇钽为前驱物,采用金属醇盐溶胶-凝胶技术,获得了Ta₂O₅湿凝胶,分析了不同条件下的溶胶-凝胶过程,并初步探讨了凝胶过程机理。Ta₂O₅的溶胶-凝胶过程主要受到水量、催化剂用量及钽源浓度等因素的影响：体系在强酸性条件下凝胶,且随着酸性的增强,体系凝胶时间明显缩短;当水量较少时,凝胶时间随水量的增加而增加,但当水量增加到一定程度时,体系凝胶时间基本不变;实验证明,通过增大溶剂用量,体系凝胶时间延长,气凝胶理论密度降低。通过对溶胶-凝胶过程的控制,结合超临界干燥技术,获得了密度低至44 mg/cm³的Ta₂O₅气凝胶样品。     

Gd2O3:Eu3+纳米晶的燃烧合成及光致发光性质

采用柠檬酸作燃烧剂用燃烧合成法制备了Gd₂O₃:Eu³⁺纳米晶.用X射线衍射仪(XRD)、高分辨透射电子显微镜(HRTEM)和荧光分光光度计等对Gd₂O₃:Eu³⁺纳米晶的结构、形貌和发光性能进行了分析.结果表明：不同柠檬酸与稀土离子配比(C/M)制备的样品经800℃ 退火1 h后，均得到了纯立方相的Gd₂O₃:Eu³⁺纳米晶，晶粒尺寸约为30 nm，尺寸分布较窄，其中以C/M=1.0时制备的纳米晶结晶性最好，发光强度最大.Gd₂O₃:Eu³⁺纳米晶主发射峰位置均在612 nm处 (⁵D₀→⁷F₂跃迁)，激发光谱中电荷迁移态发生红移，观察到Gd³⁺向Eu³⁺的有效能量传递.对柠檬酸与稀土离子配比(C/M)对结晶度、发光性质等的影响也进行了分析和讨论.     

压力对纳米CoFe2O4/SiO2复合材料结构的影响

 采用溶胶-凝胶工艺和高温高压实验技术,制备了纳米CoFe₂O₄/SiO₂复合材料。利用X射线衍射仪、扫描电子显微镜和振动样品磁强计,对样品的结构、微观形貌和磁性进行了研究,并对CoFe₂O₄中阳离子的占位情况进行了讨论。结果表明,随着处理压力的升高,样品的晶粒尺寸增大,晶格常数减小,比饱和磁化强度增大。通过计算结果可以推断,压力的升高导致CoFe₂O₄中的部分Fe³⁺从A位移向了B位,而部分Co²⁺则从B位移向了A位。     

不同粒径纳米Y2Ba4CuBiOy 相掺杂对TSIG法单畴YBCO超导块材性能的影响

本文采用顶部籽晶熔渗方法(TSIG), 研究了不同粒径纳米Y₂Ba₄CuBiO_y粒子对单畴YBCO超导块材的生长形貌、微观结构及其磁悬浮力的影响.实验所用纳米Y₂Ba₄CuBiO_y粉体的平均粒度分别为283.0 nm, 170.4 nm以及82.5 nm, 每种粉体在YBCO超导块材中的含量均为2 wt%. 研究结果表明: 在掺杂量为2 wt%的情况下, Y₂Ba₄CuBiO_y粉体的粒度并不影响样品的宏观形貌, 均可制备出单畴YBCO块材; 并且成功地将纳米Y₂Ba₄CuBiO_y粒子引入单畴YBCO块材中, 且使其均匀分布, 但样品中的Y₂Ba₄CuBiO_y粒子均小于其初始粉体的粒度, 分别减小到270 nm, 150 nm和50 nm; 随着Y₂Ba₄CuBiO_y粉体初始粒度的减小, 样品的磁悬浮力逐渐增大, 分别为10 N, 17 N, 22 N. 该结果为进一步研究纳米磁通钉扎中心的引入方法及提高YBCO超导块材的性能有重大意义.     

BiVO4空心微球的合成及其光催化降解亚甲基蓝的性能研究

以BiNO₃·5H₂O和NH₄VO₃为原料,柠檬酸为络合剂,成功合成了BiVO₄空心纳米球．采用TEM、XRD、UV-Vis等测试技术对样品的形貌、相结构以及光吸收性能等进行了表征．结果表明,所制备的BiVO₄空心微球在紫外区和可见区均有较强的光吸收,空心球平均粒径为160 nm,空腔直径为10～80 nm．以亚甲基蓝染料溶液的脱色降解实验为模型反应研究了样品的光催化性能．光催化实验结果表明,在可见光照射下,反应150 min后,样品对亚甲基蓝溶液的脱色率可达到95%以上．此外,考察了柠檬酸添加量对空心球形貌的影响,并提出了BiVO₄空心纳米球的可能形成机理．     

不同氮流量制备Mn3CuNx薄膜及其电、磁输运性质的研究

采用对靶磁控溅射方法在单晶Si(100)基片上制备了反钙钛矿结构的Mn₃CuN_x薄膜.通过控制制备过程中的反应气体氮气(N₂) 流量(N₂/Ar+N₂), 研究了氮含量对Mn₃CuN_x薄膜结构及物理性能的影响.分别利用X射线衍射仪、俄歇电子能谱、 原子力显微镜、X射线光电子能谱、物理性能测试系统和超导量子干涉仪, 对所制备薄膜的晶体结构、成分、表面形貌和电、磁输运性质进行了测试.结果表明:制备的薄膜均为反钙钛矿立方结构,且沿 (200) 晶面择优生长.随着氮含量的增大,薄膜表面粗糙度和颗粒度尺寸逐渐增大, 导致电阻率增加.氮含量对薄膜的电输运性质没有影响,所有薄膜电阻率均随着温度的降低逐渐增大, 呈现半导体型导电行为,这与对应的块体材料结果相反.Mn₃CuN_x薄膜随着测试温度的增大发生了 亚铁磁到顺磁的磁转变,且N含量的增大降低了磁有序转变温度,主要是由于N缺陷对Mn₆N八面体结构中 磁交换作用的影响所致.     

La0.3Sr0.7CrO3钙钛矿化合物高压合成和物性

 采用高压高温方法合成了单相的带宽调控型La_0.3Sr_0.7CrO₃ Mott化合物,对其晶体结构和磁学性质进行了研究。结果表明：La_0.3Sr_0.7CrO₃化合物具有立方钙钛矿晶体结构,温度在170 K以上其磁性为顺磁性,满足居里-外斯定律,温度低于20.7 K发生了自旋玻璃转变。     

Luminescent properties and the morphology of SrMoO<Subscript>4</Subscript>:Eu<Superscript>3+</Superscript> powders synthesized <Emphasis Type="Italic">via</Emphasis> combining sol-gel and solid-state route

SrMoO₄:Eu³⁺ red phosphors were prepared by combining sol-gel and solid-state route. Citric acid and ethylenediaminetetraacetic acid (EDTA), employed as the chelating agents, were added to the aqueous solutions of metal nitrates. X-ray diffraction (XRD) and photoluminescent spectra techniques (PL) were used to characterize the resultant powders. The results indicated the obtained SrMoO₄:Eu³⁺ phosphors were fine powders with a particle size of 50 nm. The effects of synthesizing conditions were also investigated and optimized, which included the synthesis temperature and the activator concentration on the luminescent intensity. Compared with SrMoO₄:Eu³⁺ phosphors prepared by Solid-state reaction SrMoO₄:Eu³⁺ phosphors prepared by combining sol-gel and solid-state route showed appropriate particle size and a higher emission intensity.     

Fuel additives and heat treatment effects on nanocrystalline zinc ferrite phase composition

Nanocrystalline ZnFe₂O₄ powder was prepared by the auto-combustion method using citric acid, acetic acid, carbamide and acrylic acid as fuel additives. Pure spinel zinc ferrite with the crystallite size of about 15 nm can be obtained by using acrylic acid as fuel additive. Samples prepared using other fuel additives contain ZnO impurities. In order to eliminate ZnO impurities, the sample prepared with citric acid as fuel additive was annealed at different temperatures up to 1000 °C in air and in argon. Annealed powders have pure ZnFe₂O₄ phase when annealing temperature is higher than 650 °C in air. Sample annealed at 650 °C in air is paramagnetic. However, annealed powders become a mixture of Fe₃O₄ and FeO after annealing at 1000 °C in argon atmosphere due to Zn volatility and the reduction reaction.     

Electrochemical behavior of carbonic precursor with Na<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript>nanostructured material in hybrid battery system

The nanostructured Na₃V₂(PO₄)₃ (NVP) cathode material has been synthesized using the sol-gel route for different molar fractions of citric acid as a carbon source during the synthesis. The nanostructured NVP as cores with carbonic shell structures are fabricated with two different citric acid molar ratios. The thermal treatment has been optimized to convert the amorphous carbon shell into graphitic carbon to realize the better electrical conductivity and thus effective electron transfer during the electrochemical charge transfer process. The X-ray diffraction measurements confirmed the rhombohedral crystallographic phase (space group R-3c) with average crystallite size ~28 ± 5 nm. The coin cells are assembled in a hybrid rechargeable electrochemical cell configuration with lithium as a counter electrode and LiPF₆-EC:DEC:DMC (1:1:1 ratio) as the electrolyte. The electrochemical charge/discharge measurements are carried out at C/10 and C/20 rates and the measured specific capacities are 80 and 120 mAhg^?1 for samples with lower and higher citric acid molar ratios, respectively. The studies suggest that NVP can be used as an effective cathode material in hybrid electrochemical cells, and a higher concentration of citric acid may result in the effective carbonic shell for optimal electron transfer and thus enhanced electrochemical performance.     

Sinter-active nanocrystalline CeO<Subscript>2</Subscript> powder prepared by a mixed fuel process: Effect of fuel on particle agglomeration

A modified combustion process, namely a mixed fuel process making use of a mixture of two fuels, such as citric acid and glycine has been developed to prepare nanocrystalline ceria powders. The effect of the mixed fuel and the different fuel to oxidant ratios on the decomposition characteristics of the gels were investigated by simultaneous thermal analysis experiments. It was established from various characterization techniques that the ceria powder prepared through the mixed fuel process has got the optimum powder characteristics, namely, a surface area of 33.33 m²/g and a crystallite size of 14 nm compared to the powders produced through the combustion process using a single fuel like glycine or citric acid. Such powders when sintered at 1250°C resulted in pellets with densities in the range of 94–96% of theoretical density. In this paper, we have carried out systematic studies on the sintering of ceria powders prepared by different approaches. The sintered ceramic from mixed fuel batch, exhibited and retained relative density more than 95% up to 1250°C and this data clearly underscores the ability of this process in developing ceria ceramics with increased stability against reduction.     

Concentration effect of Tm on cathodoluminescence properties of SiO2:Tm and SiO2:Ho,Tm systems

Cathodoluminescence (CL) properties of SiO₂ powders activated with thulium (Tm³⁺) and holmium (Ho³⁺) ions prepared by a sol–gel process were investigated. Different molar concentrations of Tm³⁺ co-doped with Ho³⁺ were studied. The 460 nm peak was monitored and the influence of the beam energy and concentration of Tm³⁺ ions on the emission properties of this peak was also monitored. The peculiar behavior whereby the 460 nm emission peak decreases and the increase in the 705 and 865 nm peaks with the increase in the concentration of Tm³⁺ ions is reported. The relationship between the accelerating beam voltage and the CL intensity of the blue emission peak (460 nm peak) is established. Morphology, particle size and optical properties were characterized with Scanning electron microscopy (SEM), UV/VIS Lambda 750 S spectrometer and Auger electron spectroscopy (AES) equipped with Ocean Optics S2000, respectively.     

Effect of citric acid on photoelectrochemical properties of tungsten trioxide films prepared by the polymeric precursor method

Effect of citric acid (CA) on microstructure and photoelectrochemical properties of WO₃ films prepared by the polymeric precursor method was investigated. The obtained materials were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and high-resolution transmission electron microscopy (HRTEM). The results showed that samples prepared with adding different amounts of citric acid had a pure phase of cubic. The addition of citric acid could significantly increase the particle size and change the surface of WO₃ films. The photoelectrochemical measurements were performed using a standard three-electrode system cell. The films prepared from mass ratios of CA/PEG (R = 0, 0.2, 0.4, 0.6 and 1) showed 1.0, 1.4, 1.7, 2.1 and 0.9 mA cm⁻² at 1.2 V under illumination with a 500 W xenon lamp (I₀ = 100 mW/cm²), respectively.     

Er3+，Er3+/Yb3+掺杂氟化镧超微材料的光谱特性与上转换发光

采用共沉淀法制备了Er³⁺掺杂和Er³⁺/Yb³⁺共掺杂LaF₃超微材料,所制备的样品的颗粒呈球形,尺寸为250nm左右.计算得到Er³⁺单掺杂样品中对应着⁴S_3/2和⁴F_9/2能级的发光量子效率分别为67.0%和71.9%.研究发现,随着Yb³⁺离子浓度的增加 关键词： 3+')" href="#">Er³⁺ 3+')" href="#">Yb³⁺ 发光 能量传递     

Structural,morphological and photoluminescence characteristics of sol-gel derived nano phase CeO<Subscript>2</Subscript> films deposited using citric acid

Homogenous nano structured CeO₂ films have been prepared by a sol-gel process using different mole ratios of citric acid as additive. XPS studies clearly illustrate an increase in Ce³⁺ proportion upon the use of higher citric acid content for the deposition of films. The crystallite sizes in the films lie in the nanorange. Photoluminescence emission in the films is attributed to various defects resulting from crystallization. Lowest transparency, high Ce³⁺ content and optimum sized crystallites in CeO₂ (1:1.5) films have led to its highest PL characteristics. Ce³⁺ chemical state is the major contributor to the PL activity of these films. The SEM micrographs show a reduced level of CeO₂ agglomeration in the films deposited using higher citric acid contents. A comparison of different properties of CeO₂ films deposited using citric acid and CeO₂–TiO₂ films has also been made.      

Size dependent structural and magnetic behaviour of CaFe2O4

CaFe₂O₄ nanocrystalline powders were synthesized through sol–gel treatment in which the stoichiometric mixing of various nitrates involving calcium and iron in presence of citric acid was performed. Subsequently, the as prepared sample was annealed at various temperatures in order to obtain the fine distribution of size including the bulk counterpart. The samples were then characterized using powder X-ray diffraction followed by ⁵⁷Fe Mössbauer spectroscopy, SQUID as well as vibrating sample magnetometry. The results of spectroanalyses revealed that the samples were formed in single phase cubic spinel structure and exhibits room temperature superparamagnetism, except the bulk one, which crystallizes in characteristic orthorhombic structure of CaFe₂O₄ and displays trivial coercivity and remanent magnetization at room temperature.     

Effect of aluminum substitution on the structural and magnetic properties of cobalt ferrite synthesized by sol-gel auto combustion process

Aluminum substituted cobalt ferrite powders (CoFe_2−xAl_xO₄) with varying composition from 0.0 to 1.0 in the step of 0.2 have been obtained by sol-gel auto combustion technique using citric acid as a fuel. The metal nitrate to fuel ratio was maintained 1:4 throughout the synthesis of CoFe_2−xAl_xO₄. The thermal analysis of as prepared samples is done by TGA technique. The compositional stoichiometry of the prepared samples is confirmed by Energy dispersive X-ray analysis technique. Single phase cubic spinel structure and nano phase structure of the synthesized powders were confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallite size of 16-26 nm was obtained using Scherrer formula. SEM analysis shows the formation of uniform grain growth. The grain size obtained from SEM results is of the order of 30 nm. Maximum specific surface area was observed to be of the order of 52 m²/gm. The highest value of saturation magnetization and coercivity was observed for pure cobalt ferrite sample and it decreases as the aluminum content x increases. A strong co-relation between the saturation magnetization and aluminum content was observed. The decrease in magnetic properties is due to the substitution of aluminum ions in place of Fe³⁺.