酸诱导液相沉积法制备二氧化锗基空芯光波导

采用酸诱导液相沉积法在石英玻璃管内壁生长了二氧化锗内反射膜,GeO2能够与OH-离子反应生成可溶性锗酸根离子,从而使GeO2在氨水和氢氧化钠溶液中的溶解度大大提高。通过向所合成的锗酸根离子前驱液中加入酸,使锗酸根离子被逐步分解为GeO2溶质析出。将酸化的锗酸根离子水溶液通入石英毛细管,可在毛细管内壁上逐渐液相沉积生长出GeO2陶瓷膜。将试样在GeO2的熔点(1 115℃)附近热处理,可以得到致密的GeO2膜。实验结果表明GeO2-氨水体系制备的GeO2空心光波导对二氧化碳激光的直线传输损耗为0.9～2.44dB.m-1。当前驱体的固含量(质量分数,下同)从5%增大到7%制备的二氧化锗空芯光波导的传输损耗降低,前驱体的固含量为8%和9%制备的空芯光波导的传输损耗大于固含量为7%。     

碱金属离子对二元锗酸盐玻璃结构的影响

基于拉曼光谱、红外光谱、密度测试分析了不同的碱金属氧化物对二元碱金属锗酸盐玻璃红外拉曼光谱的影响。结果表明:1)Li+,Na+,K+对xR2O-(1-x)GeO2(R=Li、Na、K)玻璃的红外光谱的影响规律相同:高频区吸收峰700~900 cm-1随R+含量的增加逐渐向低频移动,低频区吸收峰500~700 cm-1逐渐向高频移动,但是当R+含量足够大时转而向低频移动;Rb+,Cs+对xR2O-(1-x)GeO2(R=Rb、Cs)玻璃红外光谱的影响相同:高频区吸收峰700~900 cm-1随R+含量的增加向低频移动,低频区吸收峰500~700 cm-1以锗反常点附近为中心先升高后降低。2)从xR2O-(1-x)GeO2(R=Li、Na、K)玻璃拉曼光谱可以看出,当R2O的量分别达到其对应的锗反常点时,网络结构中仍然存在[GeO4]六元环。而在xR2O-(1-x)GeO2(R=Rb、Cs)玻璃拉曼光谱中,在锗反常点时,435 cm-1散射峰完全消失,表明网络结构中已不存在[GeO4]六元环。继续增加R2O的量,Ge—O—Ge键的弯曲振动开始显示拉曼活性。3)xR2O-(1-x)GeO2(R=Li、Na、K)体系...     

二元Li_2O-GeO_2体系玻璃的结构和锗反常现象

利用密度、红外和拉曼光谱等方法研究了二元Li2O-GeO2体系玻璃的结构和锗反常现象。结果表明:1)当Li2O摩尔含量低于20%时,网络结构中存在非桥氧,其含量随Li2O含量的增加而增加,但含量仍然很少。2)当Li2O摩尔含量增加到约20%时,Li2O-GeO2体系玻璃结构能容纳的[GeO6]八面体数量和三元环数量达到最大值;3)当Li2O摩尔含量高于20%时,随着Li2O含量的增加,由[GeO4]四面体和[GeO6]八面体参与构成的三维网络结构不断解聚,复杂大阴离子团变成小阴离子团,网络结构中产生大量间断点,[GeO6]转变成[GeO4],使得析晶活化能大大降低,从而导致熔体在冷却过程中的析晶;4)Li2O-GeO2系玻璃的锗反常归因于[GeO4]与[GeO6]之间的转变、Ge—O-非桥氧的产生、六元环向三元环的转变三者之间的交互作用。当Li2O摩尔含量≤20%时,[GeO4]向[GeO6]的转变占主导地位,伴随着六元环向三元环的转变。而当Li2O摩尔含量高于20%时,Ge—O—Ge的断裂(或非桥氧的形成)和[GeO6]向[GeO4]的转变占主导地位。     

溶致富勒烯C_(60)片状晶体向晶须的转变

将采用液-液界面析出法在甲苯/叔丁醇体系中培养的二维(2D)富勒烯C_(60)片状晶体置于含2%(体积分数)间二甲苯的异丙醇中24 h,则该2D片状晶体转变成一维(1D)晶须。通过光学显微镜,扫描电子显微镜,红外光谱,拉曼光谱,X-射线衍射法对其形貌及组成、晶型进行了表征。结果表明:1D富勒烯C_(60)晶须与2D C_(60)片状晶体具有相同的分子组成和晶型。     

钠钙玻璃负载TiO_2薄膜光催化性能影响因素研究

以普通钠钙玻璃片为载体,采用溶胶—凝胶法,经胶液配制、膜的涂覆与焙烧等工序,制备TiO2催化膜。通过正交实验,考察胶液配比、涂覆次数、升温程序等因素对TiO2薄膜光催化降解苯酚性能的影响,在选定个因素各水平下,在普通钠钙玻璃片上负载TiO2催化膜的影响因素主次顺序为:硝酸体积涂覆次数焙烧温度V乙醇∶V酞酸丁酯,最优条件为:涂覆次数=4次;焙烧温度=450℃;V乙醇∶V酞酸丁酯∶V硝酸(1∶4)∶V水=400∶40∶1∶4。通过扫描电子显微镜(SEM)可以观察到玻璃片表面明显负载着厚实的薄膜,最优条件下制备的TiO2颗粒粒径在100nm左右。     

外源低分子有机酸对纯化磷酸铁中磷释放的影响

运用高压溶液法对磷化渣进行3次提纯,获得高纯度的磷酸铁样品,采用扫描电子显微镜、X射线衍射仪对其进行表征。比较3种低分子有机酸(甲酸、乙酸、草酸)、混合酸及硫酸对纯化磷酸铁中水溶性磷释放的影响。研究结果表明,不同的低分子量有机酸对纯化磷酸铁具有不同的释放磷的能力,各有机酸对磷元素释放的作用依次表现为草酸混合酸甲酸≈乙酸;在5 g磷酸铁和500 m L去离子水的混合液中加入10 mmol的草酸时,水溶性总磷的析出效率最大。磷酸盐释放磷主要与有机酸的酸强度(pH)以及络合作用有关。     

KNN粉体水热法制备及生长机制研究

以NaOH、KOH、Nb_2O_5为原料,采用合成温度较低的水热法合成铌酸钾钠(KNN)无铅压电陶瓷粉体。通过X射线衍射技术(XRD)和扫描电子显微镜(SEM)对KNN粉体的物相、形貌及生长机制进行研究。结果表明所得KNN粉体为正交结构,由微米级斜方柱小颗粒构成,KNN粉体为层层台阶生长方式,并在颗粒表面留有大量生长台阶。     

氧化物对(111)锗片表面少子寿命的影响研究

为了提高(111)锗片表面少子寿命,分别采用体积分数30％过氧化氢和硝酸作为氧化剂,对试样表面进行湿化学氧化,得到表面的氧化层.利用微波光电导衰减仪测量试样在氧化反应前后的少子寿命变化情况,采用X射线光电子能谱测试样的Ge3d谱图,并进行机理分析.结果发现:经过过氧化氢处理的试样少子寿命得到很大提高,分析是由于GeO2钝化了锗表面悬挂键而达到了钝化效果.     

17-4PH不锈钢时效析出相的形成过程

对17-4PH(0Cr17Ni4Cu4Nb)马氏体不锈钢进行了3种不同条件下的时效处理。利用透射电子显微镜(TEM)技术详细分析了17-4PH不锈钢时效处理后析出相的形成过程。实验结果表明,时效条件为442℃,8h空冷时,在马氏体内部析出弥散的、尺寸小于10nm的ε-Cu、Nb6C(N)5和Nb2C(N)型亚稳相颗粒;时效条件为465℃,4h空冷时,析出尺寸为10～15nmε-Cu和稳定的NbC(N)相;时效条件为480℃,1h空冷时,析出尺寸为20～25mm的ε-Cu+NbC(N)相,且析出相NbC(N)与马氏体为共格析出,取向关系为NbC[001]//α-Fe[001]。     

BaO-Ga2O3-GeO2玻璃的析晶机理研究

钡镓锗玻璃是一种性能优异的中红外透过材料,而较差的机械性能严重制约了其应用。研究了钡镓锗玻璃的析晶动力学及其微晶化行为,阐明了析晶机理,为制备透明钡镓锗微晶玻璃提供理论指导。采用非等温方法研究了钡镓锗玻璃的析晶动力学,利用Kissinger模型,计算出析晶活化能Ec,两个析晶峰对应的Ec1=318kJ/mol和Ec2=515kJ/mol。通过Augis-Bennett方程获得了两个析晶峰对应的析晶指数,n-≈3。当低于1 187K(Tc2)进行晶化处理时,钡镓锗微晶玻璃中仅析出ZrO2晶体;随着晶化温度的升高,玻璃的热能持续增大,Ge2Al6O13晶体开始从母体玻璃中孕育并长大。     

Preparation and Characterization of Monodisperse Nickel Nanoparticles by Polyol Process

Polymer-protected monodisperse nickel nanoparticles were synthesized by a modified polyol reduction method in the presence of poly（N-vinyl-2-Pyrrolidone）.These nanoparticles were characterized by transmission electron microscopy（TEM）,X-ray diffraction（XRD）,selected area electron diffraction（SAED）,as well as vibrating sample magnetometer（VSM）.The experimental results show that the addition of PVP and the concentration of NaOh have strong influences on the size.agglomeration and uniformity of nanoparticles.In the presence of PVP and NaoH with low concentration.smonodisperse nickel nanoparticles with average diameters about 42 nm were obtained and characterized to the pure nickel crystalline with foc structure.Secondary structures such as clusters.loops.and strings resulted from magnetic interactions between particles were observed.The chemical interaction between the PVP and nickel nanoparticles was found by FTIR.The saturation magnetization（Ms）.remanent magnetization（Mr）and coercivity（Hc）of these nickel nanoparticles are lower than those of bulk nickel.     

Hydrothermal synthesis and photoluminescence behavior of CeO2 nanowires with the aid of surfactant PVP

Well-crystalline CeO_2 nanowires were prepared via a surfactant-assisted hydrothermal process.Reaction temperature and reaction time were changed for the determination of optimal synthesis parameters.The as-obtained products were characterized by X-ray diffraction (XRD),high-resolution transmission electron microscopy(HRTEM),and field emission scanning electron microscopy(FESEM).The results show that single crystal CeO_2 nanowires with high yield and good uniformity can be obtained hydrothermally at 180℃...     

Cl~- induced synthesis of submicron cubic copper particles in solution

Submicron copper microcrystal was synthesized by reducing Cu2O with hydrazine hydrate as reducer in aqueous solution,and was characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The shapes of copper microcrystal depend on additives. Cubic copper particles were observed when the inorganic salt containing Cl^-,such as NH4Cl,NaCl,or KCl,was added into the reaction system. By combined use of NH4Cl and polyvinylpyrrolidone （PVP）,the proportion of cubic copper particle number exceeded 90%,and the particle size is 0.1-0.5μrn. While other inorganic salt without Cl^-,such as Na2SO4 or （NH4）2SO4,had little effect on the shapes of the copper particles. The growth mechanism of metallic copper crystal in aqueous solution was analyzed. It is suggested that the formation of cubic copper crystals is ascribed to the selective adsorption of Cl^-on copper crystal （100） faces.     

Precipitation characteristic of high strength steels microalloyed with titanium produced by compact strip production

Transmission electron microscopy (TEM) and physics-chemical phase analysis were employed to investigate the precipitates in high strength steels microalloyed with Ti produced by compact strip production (CSP). It was seen that precipitates in Ti microalloyed steels mainly included TiN, Ti4C2S2, and TiC. The size of TiN particles varied from 50 to 500 nm, and they could precipitate during or before soaking. The Ti4C2S2 with the size of 40-100 nm might precipitate before rolling, and the TiC particles with the size of 5-50 nm precipitated heterogeneously. High Ti content would lead to the presence of bigger TiC particles that precipitated in austenite, and by contrast, TiC particles that precipitated in ferrite and the transformation of austenite to ferrite was smaller. They were less than 30 nm and mainly responsible for precipitate strengthening. It should be noted that the TiC particles in higher Ti content were generally smaller than those in the steel with a lower Ti content.     

Corrosion Behavior of Low Alloy Pipeline Steel in Saline Solution Saturated with Supercritical Carbon Dioxide

The carbon dioxide corrosion behavior of low alloy pipeline steel was investigated by immersion experiment. Optical microscopy(OM), scanning electron microscopy(SEM), transmission electron microscopy(TEM), and X-ray diffraction(XRD) were used to reflect the microstructure of the tested material and the corrosion morphology characterization. Results show that precipitate particles may accelerate the iron cabonate crystal formation process of the nucleation growth and promote the formation of compact layer. The major corrosion phases are Fe CO_3 and complexity compound containing Fe and Cr. The corrosion behavior consists of three stages. At the first stage, a thin inner layer and an inhomogeneous outer layer have appeared. At the second stage, the outer layer becomes homogeneous and compact, which prevents corroding the steel substrate further. At the third stage, iron carbonate crystal tends to nucleate and grow locally. The corrosion rate obtained by weight loss method increases abruptly first and then decreases quickly with increasing corrosion time. The mutual relation among microstructure, corrosion surface morphology, corrosion phases and corrosion kinetics is discussed.     

聚乙烯吡咯烷酮与柠檬酸钠的加入量对葡萄糖还原法制备Cu_2O颗粒形貌的影响

利用葡萄糖与本尼迪特试剂反应制备Cu2O颗粒,以X射线衍射、扫描电镜为表征手段,研究了聚乙烯吡咯烷酮(PVP)与柠檬酸钠的加入量对Cu2O颗粒形貌的影响。结果表明,通过改变PVP量可调控Cu2O的形貌与大小,即随着PVP量的增加,Cu2O颗粒由边长约为500nm的立方体变为大小约为1μm的切角八面体再演变为大小约为2μm的八面体。研究结果还表明,在没有柠檬酸钠存在的情况下,产物是由Cu2O小纳米晶自组装而成的、大小不均的球形颗粒;柠檬酸钠的加入有助于Cu2O晶体的生长,随着柠檬酸钠加入量的增加,球形Cu2O颗粒逐渐变为大小均一的晶体。     

Formation mechanism of gradient-distributed particles and their effects on grain structure in 01420 Al-Li alloy

Fine-grained 01420 Al-Li alloy sheets were produced by thermo-mechanical processing based on the mechanism of particle stimulated nucleation of recrystallization. The thermo-mechanically processed sheets were observed to contain layers of different microstructures along the thickness. The precipitate behavior of the second phase particles and their effects on the distribution of dislocations and layered recrystallized grain structure were analyzed by optical microscopy（OM）, scanning electron microscopy（SEM）, transmission electron microscopy（TEM） and X-ray diffractometry（XRD）. The formation mechanism of the gradient particles was discussed. The results show that after aging, a gradient distribution of large particles along the thickness is observed, the particles in the surface layer（SL） are distributed homogeneously, whereas those in the center layer（CL） are mainly distributed parallel to the rolling direction, and the volume fraction of the particles in the SL is higher than that in the CL. Subsequent rolling in the presence of layer-distributed particles results in a corresponding homogeneous distribution of highly strained regions in the SL and a banded distribution of them in CL, which is the main reason for the formation of layered grain structure along the thickness in the sheets.     

燕窝状TiO_2纳米构筑体的制备及其光催化性能

以Ti(SO4)2·2H2O为主要反应物,在雪碧(碳酸饮料)介质中通过水热法制得燕窝状构筑体的锐钛矿型TiO2。运用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线衍射分析仪(XRD)等表征手段证实,此组装结构受雪碧中的蔗糖、柠檬酸等成分及PVP含量控制,并阐明其形成过程。制得的燕窝状TiO2显示出较好的光催化性能。     

One-pot synthesis of Sb-Fe-carbon-fiber composites with in situ catalytic growth of carbon fibers

A Sb-Fe-carbon-fiber (CF) composite was prepared by a chemical vapor deposition (CVD) method with in situ growth of CFs us-ing Sb2O3/Fe2O3 as the precursor and acetylene (C2H2) as the carbon source. The Sb-Fe-CF composite was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM), and its electrochemical per-formance was investigated by galvanostatic charge-discharge cycling and electrochemical impedance spectroscopy. The Sb-Fe-CF composite shows a better cycling stability than the Sb-amorphous-carbon composite prepared by the same CVD method but using Sb2O3 as the precur-sor. Improvements in cycling stability of the Sb-Fe-CF composite can be attributed to the formation of three-dimensional network structure by CFs, which can connect Sb particles firmly. In addition, the CF layer can buffer the volume change effectively.     

TiO_2/NiO复合纳米纤维制备及光催化性能研究

通过溶胶-凝胶过程,采用静电纺丝技术,以聚乙烯吡咯烷酮（PVP,Mn=900 000）和钛酸正丁酯为前驱物,制备了PVP/Ti（OPr）4/Ni（CH3COO）2复合一维纳米纤维材料。经控温缓慢氧化分解,在600℃的条件下成功制备了直径50～100 nmTiO2/NiO纳米纤维。采用扫描电镜、红外光谱、X射线粉末衍射、拉曼等分析手段对样品进行了表征,系统地介绍了TiO2光催化作用机理并在紫外灯下使用样品对罗丹明B溶液进行降解实验。结果显示,0.5%TiO/NiO复合纳米纤维具有良好的光催化活性。