反应时间对溶剂热法制备Bi_2Se_3纳米片的影响

以BiCl3和Se粉为原料,二甘醇(DEG)作为溶剂,Na2SO3作为还原剂,碱性条件,在160℃的反应温度下,利用溶剂热法成功地合成Bi2Se3纳米片,并研究不同反应时间(20,22,24h)作用下所得产物结构形貌的变化。利用XRD和SEM对所合成产物的晶相结构及表面形貌进行表征。结果显示:在不同反应时间下所合成的粉体均为纯物相(均为六方晶相)的纳米片状Bi2Se3,且反应22h条件下所得产物形貌为大小均一、分散性良好的六边形片状结构,其厚度为10～50nm。并分析片状结构Bi2Se3的形成机制。     

真空熔炼及热压烧结Sb2Se3热电材料的微结构研究

采用石英管真空封装高纯度的Sb粉和Se粉,在800℃下熔炼8h,冷却后制成Sb2Se3粉末,在真空下进行热压烧结(470℃,60 MPa)并保温0.5 h,制备出Sb2Se3块体材料。运用XRD、SEM和EDS法对材料物相、形貌和成分进行了表征。结果表明,真空熔炼合成粉末和热压烧结块体材料的XRD图谱与Sb2Se3的标准衍射图谱(01-072-1184)相对应;Sb2Se3热压块体材料在平行和垂直于热压方向的断面上都分布着大量的层片状结构,平行于热压方向的断面上层片状结构沿某一方向择优生长,而在垂直于热压方向的断面上层片状结构分布更均匀,结晶更充分;材料中Sb和Se的原子百分比分别为40.68%、59.32%,接近于2∶3。     

Sb_2Se_3单晶纳米带的水热制备、表征及性能

采用水热法制备大量高长径比的Sb2Se3纳米带。十六烷基三甲基溴化铵(CTAB)作为形貌控制剂在纳米带的形成过程中起了至关重要的作用,借助X射线粉末衍射(XRD)仪、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和高分辨透射电镜(HRTEM)等对所得产物进行系统表征。结果表明,所制备出的Sb2Se3纳米带是沿[001]晶面方向生长的,带的宽度在1μm以内,厚度有100nm左右,长度可达几十个微米。对Sb2Se3纳米带的生长机制和光学性质进行了初步的讨论和研究。     

Sb2Se3热电材料的真空熔炼合成及微结构研究

采用石英管真空封装高纯度的Sb、Se粉末,在800℃下熔炼12 h,冷却后制成Sb2Se3粉末,在真空下进行热压烧结(470℃,60 MPa)并保温0.5 h,成功制备出Sb2Se3块体材料。运用XRD,SEM和EDS方法对材料的物相、成分和形貌进行了表征。结果表明,真空熔炼合成粉末和热压烧结块体材料的XRD图谱峰与Sb2Se3的标准衍射图谱(01-072-1184)相对应。Sb2Se3热压块体材料在平行于热压方向的断面上分布着大量的层片状结构,但少量片状结构变得粗大,层片状结构厚度约在1μm以下,并沿某一方向择优生长;垂直于热压方向的断面上微观形貌主要是层片状结构,并出现少量近似球形的结构,层片状结构短而薄,部分变得粗大,晶粒结构不均匀。热压烧结块体材料中Sb和Se的原子分数分别为40.68%,59.32%,接近2∶3。     

Sb2S3纳米线的制备和表征

以硫化钠(Na2S)和氯化锑(SbCl3)为原料,采用水热法在240 ℃下反应12 h 制备了大量高长径比的Sb2S3纳米线.X射线粉末衍射测试结果表明,所制备的产物是正交Sb2S3晶相,其晶胞参数为:a=1.123 nm,b=1.131 nm,c=0.3840 nm.通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)和高分辨透射电镜(HRTEM)分析表明:所制备的Sb2S3纳米线为单晶并且沿[001]晶面生长,其直径为100～250 nm,长为100 μm.初步讨论了Sb2S3纳米线的生长机制.     

Sb掺杂量对ATO纳米颗粒结构及激光吸收性能的影响(英文)

以SnCl4·5H2O和SbCl3为原料,采用共沉淀法制备不同Sb掺杂量的氧化锡锑(ATO)纳米粉末。分别采用XRD、FESEM、紫外可见分光光度计和激光器对晶体结构、形貌、激光反射率进行表征,研究Sb掺杂量对ATO纳米颗粒的结构、晶粒尺寸和激光反射性能的影响。结果表明:共沉淀法制备的ATO纳米颗粒为四方相金红石结构,粒径大小约为几十纳米;随着Sb掺杂量的增加,ATO的晶粒尺寸减小,晶胞体积则逐渐增大;与未掺杂的SnO2粉末相比,Sb掺杂后的ATO粉末在1.06μm激光波长处的反射率明显低于未掺杂的SnO2的反射率;随着Sb掺杂量的增加,反射率值呈先减小后增大的趋势,在Sb掺杂量为20%时,ATO粉末在1.06μm激光波长处的反射率低于0.02%,激光隐身性能最佳。     

电弧等离子体合成Sb2Te3粉末材料的微结构研究

以单质sb、Te粉末为原材料,采用直流电弧等离子体蒸发法制备Sb<,2>Te<,3>纳米粉末,当Sb:Te的原子比为5.5:4.5时,合成了Sb<,2>Te<,3>纳米粉末.通过XRD、SEM和EDS分析法对Sb<,2>Te<,3>粉末的物相结构、形貌和化学成分进行了表征.结果表明,Sb<,2>Te<,3>粉末的晶格常数为a=4.267 A,c=30.469 A;Sb<,2>Te<,3>粉末的形貌大部分为六角形片状结构,说明其形貌为单一的Sb<,2>Te<,3>纳米粉末;Sb<,2>Te<,3>纳米粉末中Sb和Te的含量为41.3at%和58.7at%,与Sb<,2>Te<,3>的含量接近.     

一种性能优良的ZnO纳米线的水热法生长

以醋酸锌(Zn(CH3COO)2·2H2O)和氢氧化钠(Na(OH)2)作为实验反应前驱物,聚乙二醇(HO(CH2CH2O)13H)作为表面活性剂,采用低温水热法在60 ℃条件下,合成了不同形貌的ZnO纳米线和纳米棒材料,并对样品结构和形貌进行了XRD、SEM等分析.结果显示,ZnO纳米结构都具有六方纤锌矿结构,主要是由单晶纳米棒状组成的"菊花状"ZnO纳米団簇,団簇中的单晶在不同反应条件下合成了线形、尖细、平面等不同形貌,但主要粒子基本为棒状和菊花状.合成方法可作为制备形貌可控的金属氧化物的参考.     

Cu_3SbS_3纳米棒的制备及形成机理

以CuCl2作为铜源,SbCl3作为锑源,L-胱氨酸作硫源和模板剂,采用生物分子辅助溶剂热法在200℃下反应12h,合成了Cu3SbS3纳米棒状结构。探讨了反应温度、反应时间等因素对产物的物相、结构形貌的影响,通过X射线粉末衍射仪(XRD)、扫描电镜(SEM)、X射线能谱仪(EDS)、高分辨透射电子显微镜(HRTEM)和选区电子衍射(SAED)等仪器对所得产物进行了表征,结果表明:所合成的产物Cu3SbS3为典型的立方结构,纳米棒的长度为数微米,直径为100～150nm,并探讨了生物分子辅助溶剂热法合成Cu3SbS3纳米棒可能的形成机理。     

微波法合成纳米羟基磷灰石晶体及表征

以Na3PO4·12H2O,Ca(NO3)2·4H2O为前驱体,通过调节pH值控制PO43-的生成,利用微波液相法合成针状纳米羟基磷灰石(n-HA),采用X射线衍射(XRD)仪、拉曼光谱(RS)、红外光谱(FT-IR)、透射电镜(TEM)等对粉体相组成和形貌进行分析。结果表明,微波液相法可以快速合成类骨n-HA晶体,合成的n-HA晶体呈针状,尺寸在(10~20)nm×(50~70)nm之间,随着微波加热时间的延长,n-HA晶体的结晶程度升高,晶体形貌从针状向短柱状转变。     

Preparation and characterization of nanostructured Bi_2Se_3 and Sn_(0.5)-Bi_2Se_3

Nanostructured Bi2Se3 and Sn0.5·Bi2Se3 were successfully synthesized by hydrothermal coreduction from SnCl2-H2O and the oxides of Bi and Se. The products were characterized by X-ray diffraction (XRD),transmission electron microscopy (TEM),and field emission scanning electron microscope (FESEM). Bi2Se3 powders obtained at 180°C and 150°C consist of hexagonal flakes of 50-150 nm in side length and nanorods of 30-100 nm in diameter and more than 1 μm in length. The product obtained at 120°C is composed of thin...     

Simple hydrothermal synthesis and sintering of Na0.5Bi0.5TiO3 nanowires

Single-crystalline Na_0.5Bi_0.5TiO₃ (NBT) nanowires, with diameters of 100 nm and lengths of about 4 μm, were synthesized by using a simple hydrothermal method. Phase composition, morphology and microstructure of the as-prepared powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). The effects of reaction temperature and reaction time on precipitation of the NBT nanowires were investigated. It was found that reaction time significantly influenced the growth behavior of the powders in the hydrothermal system. Based on the experimental results, the one-dimensional (1D) growth mechanism of the NBT was governed by a dissolution-recrystallization mechanism. NBT ceramics derived from the nanowires showed typical characteristics of relaxor ferroelectrics, with diffuseness exponent γ of as high as 1.73.     

氨化Ga2O3 /Nb膜制备的GaN纳米线的光学和微观结构特性的研究

采用射频磁控溅射技术在硅衬底上制备Ga2O3/Nb薄膜,然后在900℃下于流动的氨气中进行氨化制备GaN纳米线.用X射线衍射(XRD)、透射电子显微镜(TEM)和高分辨透射电子显微镜详细分析了GaN纳米线的结构和形貌.结果表明:采用此方法得到的GaN纳米线有直的形态和光滑的表面,其纳米线的直径大约50nm,纳米线的长约几个微米.室温下以325nm波长的光激发样品表面,只显示出一个位于367 nm的很强的紫外发光峰.最后,简单讨论了GaN纳米线的生长机制.     

Synthesis and characterization ofsingle-crystalline alumina nanowires

Alumina nanowires were synthesized on large-area silicon substrate via simple thermal evaporation method of heating a mixture of aluminum and alumina powders without using any catalyst or template. The phase structure and the surface morphology of the as-grown sample were analyzed by X-ray diffractometry(XRD) and scanning electron microscopy (SEM), respectively. The chemical composition and the microstructure of the as-grown alumina nanowires were characterized using transmission electron microscope(TEM). The nanowires are usually straight and the single crystalline has average diameter of 40 nm and length of 3 - 5μm. The growth direction is along the [002] direction. Well aligned alumina nanowire arrays were observed on the surface of many large particles. The catalyst-free growth of the alumina nanowires was explained under the framework of a vapor-solid(VS) growth mechanism. This as-synthesized alumina nanowires could find potential applications in the fabrication of nanodevices.     

三维形貌ZnO一维纳米结构的微波水热合成、机理及性能研究

以Zn(NO3)2·6H2O和NaOH为原料,采用微波水热法成功合成了具有三维形貌的单晶ZnO一维纳米结构。采用XRD、SEM及紫外-可见光谱分析等手段对ZnO纳米结构及性能进行了表征;探讨了ZnO复杂纳米结构的形成机理。结果表明:在不同工艺条件下可分别合成ZnO纳米棒、纳米线、纳米推进器、纳米蒲公英及纳米纺锤等结构;微波在合成复杂ZnO纳米结构中起非常重要的作用;纳米ZnO紫外-可见光谱吸收带边出现红移现象。该法没有引入任何金属催化剂、模板或者表面活性剂,从而避免了去除残余添加剂的后续复杂工序。另外,与传统水热法相比,该法可以显著减少反应时间和降低反应温度。     

Chemical synthesis of nanocrystalline ZrO_2-SnO_2 composite powders

ZrO_2-SnO_2 composite nanoparticles were prepared by heating the hydrate precursors synthesized by the chemicalco-precipitation reaction of ZrOCl_2 and SnCl_4. The precursors were examined by differential thermal analysis (DTA) andthermogravimetric analysis (TGA). The composite powder was characterized using X-ray diffraction (XRD), transmissionelectron microscopy (TEM) and desorption isotherm (Barrett-Joyner-Halenda method). The average crystal size of thenanoparticle ranges from 15 to 30 nm for the sample containing 5%-25% ZrO_2 (mass fraction). Most of the pores in theZrO_2-SnO_2 nanoparticles are about 10-20 nm in diameter. The composite powder is promising for chemical sensors.     

氨化Si基Ga2O3/V膜制备GaN纳米线

氨化硅基钒应变层氧化镓膜制备了大量氮化镓纳米线,X射线衍射、扫描电子显微镜和透射电子显微镜观察发现,纳米线具有十分光滑且干净的表面,其直径为20～60 nm左右,长度达到十几微米.高分辨透射电子显微镜和选区电子衍射分析结果表明,制备的氮化稼纳米线为六方纤锌矿结构.光致发光谱显示制备的氮化稼纳米线有良好的发光特性.另外,简单讨论了氮化稼纳米线的生长机制.     

Effects of Growth Parameters on the Morphology of CNTs/Cu Composite Powder Prepared Using Cr/Cu Catalyst by Chemical Vapor Deposition

采用化学共沉淀法制备了Cr/Cu复合粉体催化剂,并用化学气象沉淀法（CVD）原位合成CNTs/Cu复合粉末。利用SEM, TEM和Raman光谱分别对其微观形貌和结构进行表征。结果表明：采用化学气相沉淀法,使用10 wt%Cr/Cu 的催化剂,在混合气体(Ar/H2/C2H4) 流量2450/300 mL/min下,于1073 K 温度生长30 min,可以得到优质、结晶良好的 CNTs/Cu 复合粉末     

纳米Ba_3Ti_4Nb_4O_(21)微波介质陶瓷粉体制备及表征

以铌柠檬酸盐、乙酸钡和钛酸正四丁酯为原料,采用溶胶-凝胶法,通过控制反应条件,在700℃的温度下获得Ba3Ti4Nb4O21纳米粉体,比采用普通固相法合成的温度低400℃左右。用红外光谱,差热-热重,X射线衍射以及透射电镜等手段表征Ba3Ti4Nb4O21柠檬酸盐前驱体以及煅烧后粉体的各项特性。结果表明:用柠檬酸盐溶胶-凝胶法制得的前驱体在700℃煅烧2h后,可获得纯Ba3Ti4Nb4O21纳米粉体,其平均粒径在30～50nm,适合于微波介质陶瓷的制备。     

PREPARATION OF MULTI-WALLED CARBON NANOTUBES USING NiO CATALYST SYNTHESIZED BY HYDROTHERMAL METHOD

The Ni(OH)2/SiO2 binary colloid was prepared using Ni(NO3)2.6H2O and (C2H5O)4SiO4 as starting materials and was used to form NiO/SiO2. composite powder by hydrothermal method and desiccant method in open air respectively. Multi-walled carbon nanotubes (MWCNTs) were synthesized respectively by chemical vapor deposition using the NiO/SiO2 catalyst prepared by different methods. The phase and morphology of the catalysts and the morphology, output yield and purity of MWCNTs were compared by XRD, TEM and SEM. The results show that the catalyst powder prepared by hydrothermal method, compared with that by desiccant method, is smaller, better dispersion and has stronger catalytic activity. Pure MWCNTs with smaller tube diameter and narrow range could be obtained at a high yield using that NiO/SiO2 powder prepared by hydrothermal method as catalyst.