反应温度和时间对纳米氧化镁形貌和结构的影响

以六水合氯化镁(MgCl2·6H2O)为镁源,水合肼(N2H4·2H2O)为沉淀剂,采用化学共沉淀法制备纳米氢氧化镁前驱体煅烧得到分散性良好的不同纳米结构的氧化镁(MgO)纳米片.通过XRD、SEM、TEM对产物的结构和形貌进行分析,初步研究了反应温度和时间对MgO纳米片的形貌和结构影响,分析了MgO多孔纳米片的生长机理.结果表明:25℃,24h下MgO纳米片大小均一尺寸在20～40 nm;当温度升高到100℃,72 h生长的多孔MgO纳米片缺陷多,是晶粒相互连接起来的,纳米孔洞在10 nm;140℃72 h制备的多孔纳米片尺寸均一在100～200nm.因此可以通过调节反应温度和时间来控制多孔氧化镁纳米片结构.     

球磨增强液相剥离法制备h-BN纳米片的工艺研究

针对异丙醇溶液中高质量、高产率六方氮化硼(h-BN)纳米片的制备工艺开发问题,本文在研究h-BN粉在异丙醇(IPA)溶液中分散工艺及其悬浮稳定性的基础上,采用球磨与超声相结合的方法研究其剥离工艺,系统研究超声时间、功率、h-BN浓度及球磨时间对h-BN剥离效果的影响.采用XRD、扫描电镜(SEM)、透射电镜(TEM)、原子力显微镜(AFM)等对h-BN球磨粉体和所制备的h-BN纳米片进行了表征,并用吸光度表征了h-BN剥离产率.研究结果表明:在异丙醇溶液中加入5wt;的油酸(OA)可以提升h-BN粉的悬浮稳定性,从而提升剥离效果和效率;在液相超声剥离时,提高粉体浓度,纳米片层数提高;提高超声功率,可获得少层h-BN纳米片,但纳米片均匀性下降且制备效率较低.将h-BN粉与异丙醇溶液在300r/min转速下球磨10 h后,以0.25 mg/mL的BN/IPA溶液在350 W功率下超声20h,剥离出的h-BN纳米片为10层以下,层间距为0.33 nm,同时使剥离产率提高6.4倍.     

氧化锌纳米棒的制备及其光电性能的研究

以硝酸锌Zn(NO3)2·6H2O和六次甲基四胺(HMT)为原料,通过水热法制备出氧化锌纳米棒,研究了反应时间和冷却时间对产物形貌和尺寸的影响.采用扫描电子显微镜(SEM)、X射线衍射(XRD)、光致发光谱(PL)、紫外-可见光谱、红外光谱(FT-IR)表征产物的结构和性能.结果表明,反应时间为6 h和急速冷却至室温条件下合成样品为六方纤锌矿氧化锌纳米棒,平均直径为300 nm;样品具有良好的结晶质量和发光性能,样品在200～400nm有较强的紫外吸收性能;FT-IR图谱表明产物在430 cm-1左右出现了Zn-O特征吸收峰,并有所红移;样品的开启场强为2.2 V/μm,场增强因子为2550,当场强为4.75 V/μm时,电流密度可以达到0.7 mA/cm2,是一种性能优良的冷阴极电子发射源.     

γ-AlOOH纳米晶的微波水热法制备及表征

以Al(NO3)·9H2O和en(乙二胺)为起始反应物,用微波水热法制备出单相纳米晶γ-AlOOH.用XRD和TG-DTG对合成产物进行了表征.结果表明:在200 ℃反应20 min,可获得平均晶粒度8.5 nm的γ-AlOOH.随着合成温度升高或反应时间延长,产物的晶粒度增加,晶胞参数减小,有助于获得热稳定性高的γ-AlOOH.     

新型SiC/SiBCN复合陶瓷的析晶性能

通过热解聚碳硅烷(PCS)和聚硼硅氮烷(PBS)两种有机先驱体混合物,制得非晶态SiC/SiBCN复合陶瓷,然后对复合陶瓷进行高温热处理,研究其析晶规律及影响因素.利用热分析(TG-DTA)、X射线衍射(XRD)及透射电子显微镜(TEM)分别研究先驱体的热解机理,先驱体的组成、热解温度和时间对SiC/SiBCN复合陶瓷结晶性的影响,以及复合陶瓷的微观结构.结果表明,先驱体的组成和热处理温度对复合陶瓷的析晶行为有重要影响.当PBS/PCS=1(w/w),1100 ℃/2 h制得非晶态SiC/SiBCN复合陶瓷;1400 ℃/4 h PCS热解转变的非晶SiC开始结晶,晶粒尺寸～3 nm;1500 ℃/4 h 得到产物的相结构为～10 nm 的SiC纳米晶均匀弥散在PBS热解得到的非晶态SiBCN中;1700 ℃/2 h SiC的晶粒尺寸～16 nm;1800 ℃/2 h非晶态SiBCN开始析晶,SiC晶粒尺寸～35 nm.     

水热LSS法制备La(OH)3 纳米晶

采用基于在水热合成的过程中发生于液相、固相和溶液相界面处的相扩散和分离机制的液相(Liquid)-固相(Solid)-溶液相(Solution)(LSS)法成功地制备出具有规则形状的La(OH)3纳米晶,主要研究了水热反应釜填充比、水热反应温度等工艺因素对La(OH)3纳米晶的晶粒尺寸及相组成的影响.采用X射线衍射仪、纳米粒度分析仪和透射电子显微镜对所制备的La(OH)3纳米晶进行表征.结果表明:所制备的La(OH)3由直径约为10～40nm的纳米晶组成,晶粒尺寸分布均匀;随着水热反应温度从120℃增加到220℃,La(OH)3纳米晶结晶程度提高,晶粒的平均尺寸从14nm增加到40nm;在60～80;范围内,水热反应釜填充比对La(OH)3纳米晶的粒度影响不大.     

微波水热法制备ZnO纳米晶

采用微波水热(microwave hydrothermal,M-H)法在MDS-6型温压双控微波水热反应仪中成功地制备出平均晶粒尺寸为30 nm且呈现棒状形貌的ZnO纳米晶.并在一定的水热温度和反应时间下系统研究了微波水热反应过程中[Zn2+]离子浓度、反应釜填充比、反应物浓度比[Zn2+]/[OH]等工艺因素对ZnO纳米晶的晶粒尺寸及形貌的影响.采用X射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)和透射电子显微镜(TEM)对所制备的ZnO纳米晶进行表征.结果表明:所制备ZnO的平均晶粒尺寸约为30 nm,ZnO纳米晶呈现棒状形貌.随着[Zn2+]离子浓度的增加,ZnO纳米晶的晶粒尺寸先减小后增大;随着反应釜填充比和反应物浓度比[Zn2+]/[OH]的增大,ZnO纳米晶的晶粒尺寸先减小后增大,并逐渐趋于稳定.制备ZnO纳米晶的最佳反应条件为:[Zn2+]=1.6 mol·L-1;反应釜填充比=70;;[Zn2+]/[OH]=1/2.     

超声波辅助固液反应球磨制备ZnFe2O4纳米晶的研究

以α-Fe2O3和ZnO粉体为原料,在超声波辅助高能球磨作用下通过诱发固液相反应,并在低温下烧结合成了ZnFe2O4纳米晶粉末.采用X射线、透射电镜(TEM)对前驱体和烧结产物进行了表征,分析了球磨过程对粉体晶粒尺寸的影响和znFe2O4的形成过程.实验结果表明:超声波辅助固液球磨能在低温下烧结合成ZnFe2O4纳米晶,纳米晶的晶粒尺寸为15～25 nm;相比无超声波辅助下的固液球磨,超声波球磨降低znFe2O4烧结温度约50℃;同一烧结温度下,球磨时间越长,ZnFe2O4转化率越高,晶粒尺寸越小.     

微波辅助水热合成条件对直接合成纳米HZSM-5晶体性质的影响

利用微波辅助水热合成法直接制备了纳米HZSM-5晶体.采用XRD、FT-IR、SEM、BET和NH3-TPD等手段对合成样品进行了分析表征,研究了晶化温度和时间对合成产物晶体性质的影响.结果表明,晶化温度和时间对微波辅助水热直接合成产物微观形貌、晶粒尺寸和分散度影响明显.较低的晶化温度和较短的晶化时间均难以形成形貌规则的HZSM-5晶体.随着晶化温度的升高,合成样品逐渐变为球形晶粒、晶粒尺寸逐渐增大、分散度逐渐提高,继续提高晶化温度达180 ℃时,晶粒长大使比表面积稍有降低;随着晶化时间的延长,样品的微孔和介孔增多,比表面积和孔容逐渐增大,继续延长晶化时间,晶体内微孔可能的收缩和晶粒的长大使得样品孔容和比表面积减小.160 ℃和1.5 h条件下制备的HZSM-5分子筛晶体形貌呈球形,晶粒尺寸约为60 nm,分散程度较好;其比表面积、孔容和平均孔径分别为398.45 m2·g-1、0.63 cm3·g-1和6.27 nm;晶体表面具有弱酸特征.     

铝诱导纳米硅制备大晶粒多晶硅薄膜的研究

本文以超白玻璃为衬底,利用热丝化学气相沉积和磁控溅射法制备了Glass/nc-Si/Al的叠层结构,然后置于管式退火炉中在H2气氛下进行5h诱导晶化,用XRD、光学显微镜、扫描电镜和拉曼光谱对样品进行了表征.结果表明所有样品都是有(111)择优取向的多晶硅薄膜,在425℃诱导时,多晶硅晶粒尺寸最大达400 μm,但薄膜不连续;随着诱导温度升高到450℃,样品表面已形成了连续的多晶硅薄膜,但晶粒尺寸有所减小;475℃下诱导获得的最大晶粒尺寸约为200μm,此时多晶硅薄膜的结晶质量更好.还从动力学的角度分析了铝诱导纳米硅的晶化机理.     

溶剂热合成氮化硼纳米晶过程中氮源种类的影响

以NaNH2和BC l3为原料,利用溶剂热方法合成了六方氮化硼纳米微晶,并用红外吸收光谱(FTIR)、X射线粉末衍射(XRD)方法分析了微粒的结构,利用透射电子显微镜(TEM)观测了BN微粒的粒度和微观形貌。与早期用L i3N为氮源合成的氮化硼(产物中具有较多纳米棒)相比,本文中制备的氮化硼纳米晶主要呈球形,颗粒粒度明显增大,而且产率有较大幅度的提高。     

Synthesis and characterization of semiconductor metal sulfide nanocrystals using microemulsion technique

The semiconductor nanocrystals ZnS, PbS, CdS and CuS were synthesized via microemulsion technique involving metal acetate, reducing agent (Na₂S) and Triton X‐100 as surfactant. Nanocrystals were characterized by X‐ray diffraction (XRD), transmission electron microscopy (TEM) and dynamic light scattering (DLS). The average size of ZnS, PbS, CdS and CuS nanocrystals were found to be 5.6 nm, 13.3 nm, 11.4 nm and 6.2 nm, respectively. Different parameters like surfactant (Triton X‐100) concentration, water‐to‐surfactant ratio (ω), precursor concentration [zinc acetate, (Zn(AC)₂], reducing agent concentration [sodium sulphide, (Na₂S)] were optimized to synthesize ZnS quantum dots.     

Elimination of Texture Influence in Quantitative Phase Analysis of Boron Nitride Samples

A simple method of texture influence elimination in quantitative phase analysis of boron nitride samples is presented. The method is applicable for the compounds with hexagonal symmetry. The range of validity is discussed and the application in study of phase transitions in boron nitride samples is demonstrated.     

Effect of ferric ions on the morphology and size of magnetite nanocrystals synthesized by ultrasonic irradiation

Two‐dimensional plate‐like Fe₃O₄ nanocrystals and nanoparticles could be synthesized by a simple one‐step sonochemical method through ultrasonic irradiation in reverse co‐precipitation solution at low temperature. This technique provided a facile and rapid way to prepare Fe₃O₄nanocrystals with different morphology and size. Magnetite nanoplates were synthesized with only ferrous salt adding into alkali solution, and adding ferric ions with low molar ratio in the metal salts solution would lead to the formation of very small magnetite nanoparticles (∼10 nm). The size of as‐prepared magnetite nanoparticles increased with increasing reaction temperature and showed narrow size distribution, the standard deviation less than 2 nm. This investigation indicated that ferric ions had significant influence on the morphology of Fe₃O₄ nanocrystals. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Fabrication of CdS nanorods in inverse microemulsion using HEC as a template by a convenient γ-irradiation technique

Cadmium sulfide (CdS) nanocrystals were successfully prepared in inverse microemulsion under γ-irradiation at room temperature. Their shape can be controlled by changing the surfactant concentrations and the addition of hydroxyethyl cellulose (HEC) as the template. CdS nanorods were successfully obtained under γ-irradiation using HEC as the template, which was confirmed by the observation of transmission electron microscopy (TEM). Without the addition of HEC, spherical CdS crystals were formed. X-ray powder diffraction (XRD) pattern and electron diffraction (ED) analysis showed the hexagonal lattice of CdS in the nanorods. Additionally, the optical properties of CdS nanorods were characterized by ultraviolet–visible (UV–Vis) and photoluminescence (PL) spectroscopy.     

Detached solidification of InSb on earth

Detached solidification of lightly gallium-doped indium antimonide was achieved in the laboratory only when the ampoule was coated with hexagonal boron nitride and when the material appeared to be oxide-free. A furnace was constructed with the temperature increasing with height in order to minimize bouyancy-driven convection, so as to maximize transport of segregated dissolved gases into the gap between the growing solid and the ampoule wall. There appeared to be no difference in results with freezing rates of 5 and 10 mm/h. Best results were obtained when the ampoule was backfilled with 20 kPa of Ar-10% H₂ prior to sealing. The detached portions were depressed by several μm from adjacent attached regions, were dull, and sometimes had microfacets and steps.     

表面活性剂对水热法合成ZnS:Cu,Al纳米晶光致发光特性的影响

采用水热法直接合成了ZnS∶Cu,Al纳米荧光粉,并且系统研究了加入表面活性剂在不同S/Zn下,清洗样品和不清洗样品的结晶性、傅立叶红外光谱(FT-IR)及光致发光(PL)光谱.XRD和TEM测试结果表明:合成纳米晶为纯立方相结构,球形纳米晶尺寸约15 nm, 尺寸分布窄,分散性好.未清洗样品的结晶性比清洗样品的好,且加入表面活性剂和未清洗都导致粒径增大,影响纳米材料的表面态.改变[S~(2-)]/[Zn~(2+)]物质的量比、清洗和加入表面活性剂都会影响材料的PL强度.这说明其发光机理为紫外光激发材料表面的发光中心,即PL强度决定于纳米材料的表面态.     

单溶剂体系中CdSe纳米晶体的形貌调控研究

采用非水溶液方法,分别在十六胺(HDA)或邻苯二甲酸辛酯(DOP)的单溶剂体系中,通过调节前体加入速度和反应温度制备出六角形、多臂、短棒、长棒状以及四脚架形CdSe纳米晶体,并用透射电镜(TEM)对所得产品进行了表征.结果表明,前体的过饱和度强烈地影响CdSe纳米晶体的形貌,过饱和度的提高有导致六方纤锌矿结构(011-)方向上择向生长的趋势;两种单溶剂体系中在CdSe纳米晶体的形貌调控上有不同的影响;200 ℃不利于得到高质量的CdSe纳米晶体.     

采用溶胶凝胶前驱物制备氮化镓纳米晶体

采用溶胶凝胶法制备的前驱物进一步在900℃,氨气气氛中氮化得到粒径相对均匀、平均粒径为11.2nm的六方相氮化镓纳米晶体.XRD, HRTEM, SAED, EDS, FTIR被用于表征产物的微结构及组成.室温光致发光光谱显示产物位于3.46eV的带边发光峰和从 2.6～3.2eV 的宽的发光带.产物可直接用于制备氮化镓量子点复合材料和制备高质量的一维氮化镓晶体.     

Synthesis and properties of PbGeO3 nanostructures

PbGeO₃ nanostructures including nanofibers and nanobelts, have been synthesized via a facile hydrothermal method by the reaction between GeO₂ and Pb(CH₃COO)₂·3H₂O in the absence of any surfactant. The influences of synthetic parameters, such as reaction time, reaction temperature, and the concentration of ethylenediamine, on the morphologies and sizes of PbGeO₃ nanostructures have been investigated. It is found that an evolution of PbGeO₃ nanostructures from nanobelts to nanofibers is observed for the first time with the reaction time increased from 1 h to 6 h. The diameters of PbGeO₃ nanofibers can be controled from 300–900 nm to 80–120 nm by adjusting the concentration of ethylenediamine. Under similar conditions, PbGeO₃: Eu³⁺ nanofibers with rough surfaces can also be obtained. The photoluminescent spectra of PbGeO₃: Eu³⁺ nanofibers exhibits two fluorescence emission peaks centered at around 591 and 614 nm as the excitation wavelength is 395 nm. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)