钛合金微弧氧化膜微晶生长特性的研究

在Na₂CO₃-NaOH溶液中, 采用自制多功能单极性脉冲微弧氧化电源在TC4钛合金上制备了TiO₂薄膜. 利用XRD和SEM分别对氧化膜的相组成和表面形貌进行了分析. 结果表明, 在脉冲频率和电流密度分别固定为5000Hz和20A/dm²时, 氧化膜主要含锐钛矿和金红石相TiO₂,随着处理时间的延长, 金红石TiO₂的相对含量逐渐增加; 氧化膜呈多孔结构, 表面布满了尺寸在300nm～1μm之间的TiO₂颗粒, 随着处理时间的延长, 这些颗粒微孔的尺寸明显变大, 其密度逐渐减小.     

等离子喷涂HA/TiO2复合涂层

采用大气等离子喷涂方法,成功地制备了HA／TiO₂复合涂层,对复合涂层的结合强度、微观结构、水浸渍下的表面形貌进行了较为深入的研究．结果表明,由于TiO₂的加入,HA／TiO₂涂层的结合强度明显高于纯HA徐层,而且导致涂层破坏机理由粘合破坏向内聚破坏转化．这是由于HA／TiO₂的复合缓和了涂层与基体间的膨胀系数失配现象,改善了涂层与基体之间的结合．SEM观察显示,HA／TiO₂涂层表面有一些细小的裂纹,但在去离子水中浸泡后就会消失,而且不容易产生新的裂纹,这说明TiO₂的加入不但改善了涂层与基体之间的结合,同时增强了涂层内部颗粒的结合．     

电解液性质对TiO2纳米管阵列形貌及生长机理的影响

采用电化学阳极氧化法在纯钛片表面制备出了结构整齐有序的TiO₂纳米管阵列, 主要研究了电解液的性质、浓度以及氧化时间对TiO₂纳米管阵列形貌的影响, 并对不同电解液中TiO₂纳米管阵列的形成机理进行了初步探讨. 结果表明：在不同浓度的HF酸电解液中均可制备出规则、均匀的TiO₂纳米管阵列, 管径均匀, 表面平整, 但是纳米管的长度均较短, 约为300～350nm. 在高浓度HF电解液中, 同时获得了规则的纳米管阵列和纳米棒阵列. 在0.5wt% NaF和1mol/L Na₂SO₄中性电解液中也可以制备出表面光洁、排列整齐有序的TiO₂纳米管阵列, 纳米管长度明显长于HF酸电解液中获得的纳米管阵列, 达到了700nm, 但是阵列的表面平整度较差. 在乙二醇+0.6wt% NH₄F+2vol% H₂O有机电解液体系中可以制得超长的TiO₂纳米管阵列, 管径在150nm左右, 管长可达6μm.     

水热法制备过程中TiO2纳米纤维成形机理研究

采用水热法制备出φ20～30nm, 长度达微米级的TiO2纳米纤维, 以XRD、TEM、IR等手段对不同工艺条件下获得的产物晶型结构、微观形貌以及化学组成进行了表征, 对TiO₂纳米纤维成形机理进行探讨, 并就洗涤过程中pH值对纤维结构的影响进行分析. 结果表明, TiO₂纳米纤维的形成机理可能是锐钛矿型TiO₂纳米颗粒在强碱作用下生成K₂Ti₆O₁₃颗粒, 小颗粒沿一定晶轴生长, 遵循溶解-生长机理, 逐渐长成纳米纤维. 清洗溶液的pH值对产物的成分和结构有较大影响, 通过控制清洗溶液的pH值和热处理温度, 可以获得组成分别为K₂Ti₆O₁₃、H₂Ti₃O₇和TiO₂的纳米纤维. 在pH=7、80℃烘干条件下得到的主要是H₂Ti₃O₇纳米纤维, 400℃煅烧后转变为TiO₂纳米纤维.     

Ag/TiO2薄膜结构和光催化性能研究

采用溶胶-凝胶技术制备了Ag掺杂的TiO₂薄膜.用XRD、氮吸附法、UV-VIS-NIR分光光度计以及XPS对Ag掺杂后TiO₂薄膜结构的变化进行了分析;用分光光学法通过在紫外光照下分解亚甲基蓝的实验比较了TiO₂薄膜与Ag/TiO₂薄膜的光催化性能.结果发现,掺杂适量的Ag有助于TiO₂薄膜光催化氧化性能的提高,原因在于:（1）Ag通过引入耗尽层提高了TiO₂的电荷分离能力,并吸引空穴向薄膜表面移动,结果使薄膜表面空穴的浓度提高,薄膜光催化效率提高;（2）Ag减小了TiO₂粒子的粒径,使TiO₂禁带宽度增大,薄膜光催化氧化的能力提高;（3）Ag掺杂后,TiO₂薄膜表面对-OH基和水的吸附增加,使光照后TiO₂薄膜表面活性自由基·OH的浓度增加,空穴向薄膜所吸附物质的转移能力提高.     

高度有序钛基体阳极氧化钛纳米管阵列的制备与表征

室温下在NH₄F、乙二醇的混合溶液中采用阳极氧化法在纯Ti片表面组装一层结构高度有序且表面光滑的TiO₂纳米管阵列．对TiO₂纳米管阵列进行扫描电子显微镜(SEM)、X射线衍射(XRD)检测; 且检测了TiO₂纳米管(锐钛矿型)在锂离子电池和光催化降解甲基橙等应用性能．结果表明, 制备得到了高密度排列的TiO₂纳米管阵列; TiO₂纳米管在锂离子的脱嵌过程中表现出较好的可逆性质. 溶液中加入H₂O₂可以提高TiO₂纳米管光降解催化活性．     

纳米TiO2/Sb2O5涂层的光生阴极保护研究

采用溶胶凝胶法在304不锈钢表面制备了纳米TiO₂/Sb₂O₅叠层涂层. 用扫描电子显微镜（SEM）、X射线衍射（XRD）、X射线光电子能谱(XPS)对涂层表面形貌、晶体结构以及组成进行表征. 采用电化学方法研究涂层的光电化学性能与光生阴极保护特性. 结果表明,所制备的纳米TiO₂/Sb₂O₅叠层涂层表面连续、均匀、致密;XRD分析表明纳米TiO₂为锐钛矿型;XPS分析表明纳米涂层表面与内层均由Ti、Sb、O、C四种元素组成;稳定电位与极化曲线测试表明,在3%NaCl溶液中,纳米TiO₂/Sb₂O₅叠层涂层的光电化学性能低于纯纳米TiO₂涂层,但纳米TiO₂/Sb₂O₅涂层经紫外光照1h,停止紫外光照后的延时阴极保护作用可达4h. 通过研究分析,提出了一种新的纳米叠层涂层光生阴极保护作用机理.     

掺钒二氧化钛中空微球的制备和光催化性能研究

以聚苯乙烯微球为模板,钛酸四丁酯为前驱体制备了掺钒TiO₂中空微球,并用FT-IR,SEM,TEM,XRD,UV-Vis等技术对样品进行了表征. 研究结果表明,掺杂少量钒到体系中,TiO₂微球形貌没有发生明显变化,得到壳层厚度约为20~30nm的TiO₂中空微球. 但钒的引入使得TiO₂中空微球从锐钛矿相向金红石相转变. 随着掺钒量的增加,TiO₂中空微球吸收边向长波方向移动增强. 光催化降解甲基橙溶液实验结果表明,掺杂1.0%钒的TiO₂中空微球表现出更好的光催化性能.     

铝硅酸盐中间体对TiO2纳米粒子团聚及相转变的抑制

以粉煤灰为原料, 通过与NaOH煅烧、水解合成铝硅酸盐中间体(ASI), 向sol-gel法制备的TiO₂溶胶中加入ASI, 经处理得到钛铝硅酸盐复合材料(TiO₂/ASI). X射线衍射分析(XRD)和紫外-可见漫反射光谱(DRS)研究ASI对sol-gel方法制备TiO₂纳米晶形成过程和相转变的影响. 研究结果表明: 铝硅酸盐中间体不但能抑制TiO₂纳米粒子的团聚, 而且能够有效地抑制TiO₂由锐钛矿型向金红石型的相转变, 由此所制备TiO₂与ASI的钛铝硅酸盐复合材料(TiO₂/ASI)对溶液中亚甲基蓝的吸附性能高于单一的TiO₂或铝硅酸盐中间体.     

钒掺杂纳米TiO2薄膜的结构和光吸收性能

采用磁控溅射法制备了不同V含量的纳米TiO₂薄膜,利用SEM、XRD、Raman光谱和UV-vis吸收光谱对V掺杂TiO₂薄膜的表面形貌、结晶特性、晶格应力和光吸收性能进行了分析.结果表明,V掺杂可促进TiO₂薄膜晶粒的定向生长,得到尺寸分布较均匀的哑铃状晶粒,且可抑制薄膜的晶格膨胀和金红石型晶粒的生成.V掺杂TiO₂薄膜处于压应力状态,且应力随V含量增加而增大.V掺杂使导带底向带隙延伸,TiO₂薄膜光学带隙变窄,光响应范围从紫外区红移到可见光区域,提高了薄膜对可见光的吸收率.     

去甲斑蝥素PLA-PEG纳米微球的制备研究

采用复乳法和相分离法两种方法制备去甲斑蝥素的聚乳酸-聚乙二醇嵌段共聚物(PLA-PEG)纳米微球.对比了两种不同方法对制得的含药微球在粒径、包封率以及缓释性能方面的差异.用激光粒度分析仪表征了微球的粒径及其分布,并用透射电镜观察了微球的形貌,其结果表明:复乳法与相分离法制备的微球粒径均在100nm左右,并且成球性好;相对于复乳法,相分离法制备的微球分布较宽,包封率较高,可达到50%左右;体外释放实验表明两种方法制备的微球都具有缓释作用.     

Investigation on one-pot hydrothermal synthesis,structural and optical properties of ZnS quantum dots

The advantage of hydrothermal synthesis of semiconductor quantum dots (QDs) over the control of particles size, morphology and stability is reported here. In a typical synthesis procedure, the zinc and sulfur precursor molar ratio of 1:3 was used in an aqueous solution at 150 °C. The cubic phase of ZnS with average particles size of 5 nm was confirmed and estimated from the X-ray diffraction (XRD) analysis. The composition and purity of the sample were analyzed from (energy dispersive-ray analysis) EDAX and (X-ray photoelectron spectroscopy analysis) XPS spectra. The absorption spectrum shows the large shift in the absorption band over 90 nm due to the quantum confinement of carriers. The emission spectrum of quantum dots carry more evidence on the presence of shallow trap, deep trap in the band gap of the material responsible for weak emission in the spectral region of 450–500 nm. High resolution transmission electron microscope and scanning electron microscope studies reveal the structural and morphological features of ZnS with slightly distorted spherical morphology. We found that the coordinating ability of solvent strongly influences the reaction process and morphology of the products.     

钯纳米颗粒的形貌控制合成

为优化钯纳米颗粒的化学还原法制备工艺,本文以氯钯酸(H₂PdCl₄)为前驱体,抗坏血酸(C₆H₈O₆)为还原剂,聚丙烯酸钠(PAAS)为表面活性剂制备钯纳米颗粒。采用正交实验探究不同工艺参数对钯纳米颗粒粒径和形貌的影响。通过 X射线粉末衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)及电化学工作站对制备产物的结构、物相、形貌、电催化性能进行了表征。结果表明:在相同的工艺体系下,通过温度的改变,40 ℃条件下可以得到粒径大小为64.5 nm,球形度较好,分散性高的钯纳米颗粒;90 ℃条件下可以得到粒径大小为45.9 nm的立方体钯纳米颗粒。所制备的球形和立方体钯纳米颗粒对甲酸的电氧化催化活性分别为商业钯黑的1.57倍和1.49倍,在催化剂制备领域有广泛的应用前景。     

Influence of acid precursors on physicochemical properties of nanosized titania synthesized by thermal-hydrolysis method

The influence of nature and concentration of acid species on surface morphology and physicochemical properties of titania particles synthesized by direct thermal hydrolysis of titanium tetrachloride was investigated. The acids used were hydrochloric acid, nitric acid, sulfuric acid, and perchloric acid with a concentration of 3 M. Thermal hydrolysis of titanium tetrachloride in hydrochloric acid and perchloric acid with molar ratios of [H⁺]/[Ti⁴⁺] = 0.5, 1.0, 1.5, and 2.0, respectively, was used to study the effect of acid concentration. The synthesized materials were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, dynamic light scattering, and thermogravimetric analysis. Characterization of the samples by X-ray diffraction studies revealed the influence of acid species on the phase transformation of titania. Samples prepared by hydrochloric acid, nitric acid, and perchloric acid formed rutile phase with rhombus primary particles, while sulfuric acid resulted in anatase phase with flake-shaped primary particles. Transmission electron microscopy and dynamic light scattering results confirmed the nanosized titania particles and the agglomeration of primary particles to form secondary particles in spherical shape. The particle size of titania prepared using perchloric acid was smaller than those prepared with other acid sources. A direct correlation between [H⁺]/[Ti⁴⁺] ratio and particle size of titania was observed.     

Synthesis and characterisation of ferromagnetic hexagonal cobalt nanoparticles

Ferromagnetic hexagonal cobalt nanoparticles are synthesised via reduction of cobalt acetate tetrahydrate by using sodium borohydride as a reducing agent. The morphology, crystal structure and magnetic properties of as synthesised particles are characterised by using transmission electron microscopy (TEM), powder X-ray diffraction (XRD) and vibratory sample magnetometer (VSM). The results show that the particles are spherical in shape with a size of 5?nm. These particles show ferromagnetic behaviour with magnetic coercivity of 583?Oe at room temperature. Oleic acid acts as the surfactant and its bonding nature on the cobalt nanoparticles is studied by Fourier transform infrared spectrometry.     

Deposition of gold nanoparticles on electrospun MgTiO3 ceramic nanofibers

A simple method to deposit spherical gold nanoparticles on the surface of MgTiO3 ceramic nanofibers is presented. Electrospun MgTiO3/poly(vinyl acetate) (PVAc) hybrid nanofibers were calcined at 650 degrees C to obtain phase pure ceramic MgTiO3 nanofibers with 100-150 nm diameters. These ceramic nanofibers were immersed in an aqueous solution of HAuCl4 containing poly(vinyl alcohol) (PVA) as capping agent followed by photoreduction at 365 nm to get a novel Au-MgTiO3 nanocomposite. The formation of gold nanoparticles upon irradiation was confirmed by the appearance of a surface plasmon band (SPB) at 590 nm in the UV-visible absorption spectra. The surface morphology and elemental compositions were analyzed by the scanning electron microscope (SEM) equipped with energy dispersive X-ray (EDX), and transmission electron microscope (TEM). X-ray diffraction (XRD) and selected area diffraction (SAED) pattern in TEM revealed the crystallization of gold by exhibiting strong diffractions correspond to Au(111) and Au(200) crystalline planes in addition to the MgTiO3 diffraction.     

碳酸铅纳米粉体的制备及其表征

在溶液结晶体系中加入适当的添加剂可改变晶体的生长环境,影响晶体的生长、团聚行为,从而得到理想的晶形及晶粒尺寸。本研究在化学沉淀法制备碳酸铅的反应体系中加入适量表面活性剂,通过表面活性剂对晶粒生长和团聚的抑制作用,制备了疏松的碳酸铅纳米粉体。XRD和TEM分析表明,反应体系中加入表面活性剂后,制备的碳酸铅纳米粉体的晶形发生了改变,纳米碳酸铅颗粒呈球形,粒度均匀,为60 nm左右。     

溶胶-凝胶模板法制备有序大孔TiO_2微球

以无皂乳液聚合方法自制的单分散聚苯乙烯(PS)微球乳液为原料,利用PS自组装制备了有序胶体晶体模板("蛋白石"),采用溶胶-凝胶模板法制备了有序大孔TiO2微球("反蛋白石"),其孔呈六边形,孔径分布均一,约为200nm。运用扫描电镜(SEM)、X射线衍射(XRD)对其形貌特征及晶型进行了表征,结果表明,采用表面含有羧基的单分散聚苯乙烯微球及高的硅油黏度制得的模板有序度高;通过控制煅烧温度可以改变有序大孔TiO2微球的晶型,当煅烧温度为500℃时,其晶型为锐钛型,当煅烧温度为700℃时,其晶型则为金红石型。     

Improvement of morphology and luminescence of CaS:Eu<Superscript>2+</Superscript> red-emitting phosphor particles via carbon-containing additive strategy

CaS:Eu²⁺ red-emitting phosphors particles, were prepared by the precipitation method, followed by sintering in the atmosphere over the mixture of sulfur powder, Na₂CO₃, and carbon-containing compounds such as tartaric acid, citric avid, glucose, and cane sugar. The structure, morphology and photoluminescence performance of the as-prepared samples were investigated by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence spectrum (PL), respectively. The influences of carbon-containing additives on its crystallization behavior, morphology, and enhancement in luminescence of CaS:Eu²⁺ particles were studied. CaS:Eu²⁺ particles without additive show inhomogeneous, rough and aggregation with the size of 75–125 nm, but the spherical particles with mean size of about 110 nm were obtained by adding carbon-containing compounds. Compared with phosphor without additive, the addition of carbon-containing materials induced a remarkable increase of PL, in the order of cane sugar, glucose, citric acid, and tartaric acid. This enhancement is duo to the improvement of crystallinity, particle morphology and size distribution of the samples by adding carbon-containing additive.     

Single step synthesis of indium tin oxide by ultrasonic spray and microwave assisted pyrolysis

Ultrafine indium tin oxide (ITO) powders were successfully synthesised by the combined methods of ultrasonic spray and microwave assisted pyrolysis, which is a single step, facile, rapid and continuous method without post-heating treatment. Crystallinity, morphology and microstructure of the samples were investigated by X-ray diffractometer, scanning electron microscope, transmission electron microscope, energy dispersive X-ray spectroscope, selected area electron diffraction pattern and laser grain size analyser. Results indicate that pure solid solution ITO ultrafine powders with homogeneous and narrow size distribution, highly dense and smooth surface morphology can be obtained under optimum conditions. Each uniform spherical particle consisted of many smaller crystallites with diameter of <10 nm.