直接沉淀法合成Sc2O3纳米粉

研究了直接沉淀法合成Sc2O3纳米粉的工艺。以硝酸钪[Sc(NO3)3]为母盐,氨水(NH3.H2O)作沉淀剂,采用直接沉淀法合成出网状的前躯沉淀物,同时分析了前驱体的热分解过程。通过X射线衍射和红外光谱对前躯体的物相组成进行了定性分析,结果表明,该前躯沉淀物为γ-ScOOH.nH2O与NH4Sc3(SO4)2(OH)6.nH2O的两相混合物。前躯体经过微化处理后,在1 000℃的温度下煅烧,生成的Sc2O3纳米粉具有纯度较高、颗粒粒度小(40 nm)、粒度分布窄、近似球形Sc2O3的性能,但是粉体产生了轻微团聚的现象。     

均匀沉淀法制备Sc2O3纳米粉

研究以硫酸钪(Sc2(SO4)3)和六次甲基四胺((CH2)6N4)为原料,通过向Sc2(SO4)3溶液中滴加(CH2)6N4溶液,制备出了前驱沉淀物,该前驱沉淀物的化学组成为Sc(OH)2.2(SO4)0.4·0.4H2O,并分析了前驱沉淀物的热分解行为.前驱沉淀物经1100℃煅烧4h后得到了平均粒径为80nm、分散性良好的超细粉体.     

溶胶-凝胶法制备纳米Y2O3粉体

为了改善Y2O3粉体的分散性,提高其烧结活性,试验以三乙醇胺和氨水为凝胶剂,利用溶胶-凝胶方法合成了纳米级Y2O3粉体,采用差热/热重、X射线衍射、透射电镜研究了前驱体的组成、前驱体在不同的煅烧温度下的物相变化以及煅烧粉体的分散性.结果表明,前驱体的组成为Y2(OH)5.14(NO3)0.86H2O,在500℃保温2h可直接生成立方相的Y2O3,煅烧至1000℃保温2h得到了结晶度高、分散性好、平均粒径为50nm、近球形的YO纳米粉体;三乙醇胺的加入有利于提高YO粉体的分散性.     

用微波均相沉淀法合成Sc2O3纳米粉

以硫酸钪为母盐,尿素为沉淀剂,采用微波加热方式合成了水合碱式碳硫酸钪前驱体.用差式扫描量热法(DSC)、热重分析(TG)、红外光谱(IR)、X-射线衍射(XRD)分析了加热过程中前驱沉淀物的物相变化.采用高温煅烧和高能微波辐照两种方法制备了Sc2O3粉体.结果表明,将前驱沉淀物分别在1000℃煅烧3 h和在900℃微波...     

ATO/CaSO4复合导电粉的制备及表征

复合导电粉具有良好的导电性、稳定性和分散性,广泛用于防静电、电磁屏蔽等领域。以硫酸钙晶须为载体,采用共沉淀法在其表面包覆一层锑掺杂氧化锡(ATO)制备了ATO/CaSO4复合导电粉,研究了焙烧温度对导电粉电阻率的影响。运用热重-差热分析(TG-DSC)和X-射线衍射(XRD)对产物进行了表征,并通过扫描电镜(SEM)观察了粉体的形貌。结果表明,最佳的焙烧温度为650℃,与TG-DSC得到的结论相一致。     

尖晶石型LiMn2O4的凝胶燃烧法制备

以硝酸锂、硝酸锰和柠檬酸为原料,采用溶胶-凝胶法制备成前驱体,将该前驱体在空气环境下燃烧得到的粉料在600～900℃焙烧一定时间得到尖晶石型晶体结构的LiMn2O4(空间群为Fd3m)。利用X射线衍射(XRD)、扫描电镜(SEM)、热重-差热分析(TG/DTA)对前驱体及合成的样品进行了测试分析和表征。研究了焙烧温度、时间以及锂锰摩尔比(n(Li)/n(Mn))R等对合成样品的相组成、晶体结构和微观形貌等的影响。合成高纯尖晶石型LiMn2O4的优化条件为焙烧温度800℃,焙烧时间10h,R=1.1/2。     

Co3O4纳米颗粒的制备及表征

以脱脂棉为碳源,硝酸钴为前驱物,采用碳辅助法焙烧制备了粒径为50nm Co3O4纳米颗粒。用X射线衍射(XRD)对不同焙烧温度(200~600℃)下样品的物相、晶粒度进行了研究,并结合傅立叶红外光谱(FT-IR)对Co3O4物相演变进行了分析,确定中间产物前躯体是CoCO3;通过扫描电镜(SEM)和透射电镜(TEM)对制备的Co3O4样品的形貌、粒径进行了分析;同时,X射线能谱(EDS)和氮气吸附-脱附曲线测试等表明制备的Co3O4表面存在碳元素和孔结构,具有较大的比表面积,有利于提升其光解水制氢能力。     

超顺磁性纳米Fe3O4的热分解法制备及表征

以单甲氧基聚乙二醇、对甲苯磺酰氯、邻苯二甲酰亚胺钾等为原料,根据盖布瑞尔合成法原理,合成了一端为氨基的单甲醚聚乙二醇(mPEG-NH2)。并以其为还原剂,聚乙二醇(PEG)为溶剂,利用热分解法制备了水分散性的超顺磁性纳米Fe3O4。采用红外光谱(FT-IR)、X射线衍射(XRD)、透射电镜(TEM)、热重分析(TG)、超导量子干涉仪(SQUID)和纳米粒度与Zeta电位分析仪等测试技术对其性能进行表征,实验结果表明,所制得的纳米Fe3O4粒子结晶度高,粒度均匀,分散良好,平均粒径为(12.2±1.6)nm,具有超顺磁性,饱和磁化强度为54 emu/g,在中性水溶液中其表面带正电,Zeta电位为+33 mV。TG测试结果表明,Fe3O4纳米粒子表面有机物的含量约为28%,Fe3O4的产率为57%左右。     

核壳型Fe3O4/C纳米颗粒的溶剂热法制备及其微波吸收性能

本文以二茂铁为主要原料,通过溶剂热法在190℃反应72h制备了核壳型Fe3O4/C磁性纳米颗粒。通过X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、X-射线能谱仪(EDS)、透射电子显微镜(TEM)、振动样品磁强计(VSM)、矢量网络分析仪对产物进行了表征。结果表明,产物为球形核壳结构的Fe3O4/C纳米颗粒,其尺寸在100~150nm之间,其中碳壳的厚度在10~20nm之间。室温下,产物的矫顽力(Hc)为13.635Oe,剩余磁化率(Mr)为5.00725emu/g,饱和磁化率(Ms)为17.6863emu/g。在2~18GHz范围内,产物厚度为5mm、频率为12.99GHz时,产物的微波反射率为-37.85dB。     

水热-热解法合成不同形貌的α-Al2O3粉体

以Al2(SO4)3·18H2O、尿素为原料,采用水热-热解法制备α-Al2O3粉体。用XRD、SEM对产物进行表征,研究了水热反应时间、表面活性剂PEG2000、添加剂AlF3等因素对产物形貌的影响。结果表明:120℃水热反应6 h,前驱体经1200℃煅烧,用Al2(SO4)3·18H2O/尿素体系得到球形α-Al2O3;分别以表面活性剂PEG2000和AlF3为添加剂,得到纤维状及片状α-Al2O3。讨论了不同形貌α-Al2O3的形成机制。     

Low-temperature performance of Al4B2O9 nanowires

In this paper we report on the synthetic investigation of single-crystalline aluminum borate (Al₄B₂O₉) nanowires in large scale by a direct calcination of a precursor powder made of Na₂B₄O₇·10H₂O and Al (NO₃)₃·9H₂O at a low temperature of 850 °C. The nanowires, with the diameter of 20-40 nm and the length up to several micrometers, possess smooth surfaces and uniform sizes along the entire wire. The growth mechanism of the nanowires is attributed to a solid-liquid-solid process, which controls the nanowire morphology.     

Synthesis of a novel langanite-type compound La3Al5.5Nb0.5O14 by the sol-gel process

Langanite (La₃Ga_5.5Nb_0.5O₁₄, LGN) and its isomorphs are a few piezoelectric materials which have the unique temperature compensation and piezoelectric properties. But the high Ga₂O₃ content makes them very expensive and limits their applications. We reported a new langanite-type compound La₃Al_5.5Nb_0.5O₁₄ (LAN) which has the advantage of no Ga₂O₃ content. Chemically homogeneous La₃Al_5.5Nb_0.5O₁₄ sol was synthesized using La (NO₃)₃·6H₂O, Al (NO₃)₃·9H₂O and niobium citrate as starting materials. Single-phased LAN powder was prepared by decomposition of a citrate polymer precursor and subsequent reactions at high temperatures. TG-DTA, XRD and FTIR were employed to investigate the transformation process of gel to LAN powder. The results showed that, after calcination at 900 °C, pure La₃Al_5.5Nb_0.5O₁₄ polycrystalline powder with a narrow particle size distribution was obtained, which has the same structure with La₃Ga_5.5Nb_0.5O₁₄.     

Synthesis, characterization and magnetic properties of CoFe2O4 nanorods

In this work, we demonstrated a new precursor route to synthesize CoFe₂O₄ one-dimensional (1D) nanorods. CoFe₂O₄ nanorods were prepared via the thermal decomposition of CoFe₂(C₂O₄)₃ nanorod precursor, which was prepared by solvothermal method without the assistance of template or surfactant. The microstructure and magnetic property of the obtained products were characterized by x-ray powder diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), thermogravimetric (TG) and differential thermal analysis (DTA) and vibrating sample magnetometer (VSM). The results showed that the as-prepared CoFe₂O₄ nanorods were built by magnetic nanoparticles after calcining the precursor nanorods at different temperatures, and the size variation of magnetic nanoparticles with calcination temperatures leaded to variable magnetic properties.     

Synthesis of submicron-sized spherical Y2O3 powder for transparent YAG ceramics

Spherical monodispersed, submicron-sized Y₂O₃ powder was prepared via a homogeneous precipitation method using nitrate and urea as raw materials. The structure, phase evolution and morphology of Y₂O₃ precursor and the calcined powder were studied by FTIR, TG/DTA, XRD and SEM methods. The sphere size of the precursor was about 250 nm and that of Y₂O₃ powder calcined at 800 °C for 2 h was about 200-210 nm. With the spherical Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder, high transparent YAG ceramics was fabricated by vacuum sintering at 1780 °C for 6 h through a solid-state reaction method. The in-line transmittances of the as-fabricated YAG ceramics at the wavelength of 1064 nm and 400 nm were 82.8% and 79.5%, respectively, which were much higher than that of the YAG ceramics with a commercial Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder directly. The superior properties are attributed to the good morphology, dispersibility and uniform grain size of the as-prepared spherical Y₂O₃ powder, which matches that of the commercial Al₂O₃ powder.     

Morphotropic phase boundary in Pb(Sc1/2Nb1/2)O3-BiScO3-PbTiO3 high temperature piezoelectrics

The solid solutions in the 0.36BiScO₃-0.64(1 − x)PbTiO₃-0.64xPb(Sc_1/2Nb_1/2)O₃ system were fabricated using wolframite precursor method. A coexistence of rhombohedral and tetragonal phases is formed in the studied compositions range and a wide morphotropic phase boundary region is confirmed by X-ray diffraction results. After the addition of Pb(Sc_1/2Nb_1/2)O₃, a relaxor behavior is induced and the dielectric maximum temperature shifts to higher temperatures with increasing measuring frequencies. The presence of relaxor can be ascribed to the formation of polar nanoregions. The studied composition exhibits the optimal ferroelectric and piezoelectric properties with d₃₃ of 453 pC/N and K_p of 0.58, T_m of 405 °C for x = 0.10 composition, which is suitable for future high-temperature piezoelectric application.     

Low temperature preparation of nanocrystalline Sr0.5Ba0.5Nb2O6 powders using an aqueous organic gel route

Nano-sized Sr_0.5Ba_0.5Nb₂O₆ (SBN50) ceramic powders have been synthesized by an aqueous organic gel route. Homogeneous Sr-Ba-Nb precursor gels are prepared with Ba-EDTA, Sr-EDTA, and Nb-citrate complex as source of Sr, Ba, and Nb, respectively. Citric acid and ethylenediaminetetraacetic acid (EDTA) were used as the chelating agents. The structural variation of the SBN powder with annealing temperature was studied by TG-DTA, FT-IR and XRD. The precursor gel on calcination at 800 °C for 2 h produces a pure tungsten bronze SBN phase and the corresponding average particle size is 30-50 nm. The influences of the pH and the molar ratio of citric acid:Nb cation on the formation of homogeneous Sr-Ba-Nb precursor gels were also studied. The results show that a homogeneous Sr-Ba-Nb precursor gel with no precipitate is formed at pH 8 and the optimum molar ratio of citric acid and the metal cations is 3:1.     

Hydrothermal synthesis, structure and scintillation characterization of nanocrystalline Eu-doped Gd2O3 materials and its X-ray imaging applications

Nanocrystalline Gd₂O₃:Eu scintillators were successfully synthesized using a hydrothermal method and subsequent calcination treatment in the electrical furnace as an X-ray to visible light conversion material for an indirect X-ray image sensor. In this work, various Gd₂O₃:Eu scintillators were prepared in accordance with different synthesis conditions such as doped-Eu concentration, different calcination temperatures of 600-1400 °C and calcination time of 1-10 h. The transition of morphology from nanorods to particles was observed as the calcination temperature of Gd₂O₃:Eu scintillator increased. And the phase transformation of the sample from cubic to monoclinic structure was discovered at 1300 °C calcination temperature. In addition, scintillation properties such as luminescent spectra and light intensity under 266 nm UV illumination were measured as a function of calcination condition of as-synthesized Gd₂O₃:Eu powder. The nanocrystalline Gd₂O₃:Eu scintillator with a strong red light emission at near 611 nm wavelength under photo- and X-ray excitation will be employed for its potential X-ray image sensor applications in the future.     

Facile synthesis of MnCO3 hollow dumbbells and their conversion to manganese oxide

Manganese carbonate (MnCO₃) hollow dumbbells were synthesized via a polyol process. Based on the structural analysis of the samples obtained at different reaction times, a mechanism of nucleation-growth-aggregation-ripening was proposed to account for the formation of the hollow dumbbells. Moreover, the manganese oxide has also been obtained from the MnCO₃ crystals after thermal transformation in laboratory air, and the phase of final product could easily be controlled to be either MnO₂ or Mn₂O₃, simply by altering the calcination conditions. The manganese oxide powder products possessed mesoporosity and essentially preserved the pristine morphology of the MnCO₃ precursor.     

Compounds in the system BaOSc2O3

The occurrence of compounds in the system BaO-Sc₂O₃ has been investigated. Apart from the already known compounds Ba₃Sc₄O₉ and BaSc₂O₄, tetragonal Ba₂Sc₂O₅ has been found. This phase is the only compound formed at low temperature (1000°C). At higher temperatures Ba₂Sc₂O₅ is transformed into the other stable compounds, whereas remaining Ba₂Sc₂O₅ may dissolve excess BaO, changing the unit cell constants. A tetragonal compound Ba₆Sc₆O₁₅, was also observed.     

Preparation and Structure of Ga2 – x Sc x O3 (0.42 ≤ x ≤ 0.52)

The structure of a scandium gallium oxide single crystal grown by the Czochralski process from a charge of composition Ga_1.5Sc_0.5O₃ is determined by x-ray diffraction. The structure is shown to be a superstructure to -Ga₂O₃. The superstructure parameters are found to vary both along the axis of the crystal and radially, which is due to variations in Ga : Sc ratio. A structural model of the Ga_1.5Sc_0.5O₃ crystal is proposed.