Synthesis and microstructure of single-phase BiFeO_3 Powders by Sol-gel Method

The single-phase BiFeO3 powders were prepared by sol-gel method with the starting materials of bismuth nitrate and ferric nitrate, and the effect of the calcined temperature on the phases of BiFeO3 samples was studied. The x-ray diffraction (XRD)showed that the single-phase BiFeO3 powders were obtained with a calcined temperature of 700 ℃. The scanning electron microscope(SEM)analysis indicated that the grain size was around 500 nm in single-phase BiFeO3 powders, and uniform particle size distribution. The FT-IR spectra showed that the BiFeO3 powders began to crystallize at 500℃.

Preparation of Perovskite-Type Oxides La_(1-x)Sr_xFe_(1-y)Co_yO_3 Using EDTA Sol-Gel Method

Two series of perovskite-type oxides with composition (La_(1-x))Sr_xFeO_3(x≤0.8)and La_(1-x)Sr_xFe_(1-y)Co_yO_3(x=0.2; y=0.2, 0.4)powder productions were synthesized by EDTA complexing sol-gel method. The products were characterized by XRD, TEM, SEM, BET method(N_2 adsorption)and laser granularity analysis for different synthesis conditions to obtain the optimum conditions for the preparation process. Single-phased, uniform perovskite-type oxides with small particle size were obtained by EDTA sol-gel process with high stability and repeatability, and the process temperature is much lower than that of solid state reaction method.

Intense up-conversion emissions of yb3＋/Dy3＋ co-doped A12O3 nanopowders prepared by non-aqueous sol-gel method＊

yb3＋/Dy3＋ co-doped A1203 nanopowders have been prepared by the non-aqueous sol-gel method and their up- conversion photoluminescence spectra are measured under excitation by a 980-nm semiconductor laser. The results show that there are comparatively abundant spectra of up-conversion emissions centered at 378, 408, 527 and 543, and 663 nm, corresponding to 4C9/2→ 6H13/2, 4C9/2→ 6Hll/2, 4115/2 → 6H13/2, and 4F9/2 →6Hll/2 transitions of Dy3＋, respectively. Two-photon and three-photon processes are involved in ultraviolet, violet, green, and red up-conversion emissions. The energy transition between Yb3＋ and Dy3＋ is discussed.

Preparation and Magnetic Properties of (Fe_7Co_3)_(0.15)(SiO_2)_(0.85)Granular Solids Using the Sol-Gel Method

(Fe7Co3)0.15(SiO2)0.85 granular alloy solid was prepared successfully using sol-gel method. The samples with different reducing temperatures were investigated by X-ray diffractometer(XRD),transmission electron micrography(TEM) and vibrating sample magnetometer(VSM). The av-erage particIe sizes of the samples were also calculated from Scherrer formula. The magnetic properties of (Fe7Co3 )o. 15 (SiO2)0.85 were studied in detail.

Progress in Research on Nanometer Al_2O_3 Fabricated by Sol-Gel Method

Nanometer Al_2O_3 is one of new types of functional materials with broad application and development prospects in the future. The basic principle and ways of nanometer Al_2O_3 fabricated using sol-gel technique were introduced, and the factors affecting nanometer Al_2O_3 fabricated using sol-gel method were analyzed. The progress in research on nanometer Al_2O_3 and the application fields of nanometer Al_2O_3 were reviewed. The existing problems and the problems prospect for nanometer Al_2O_3 were pointed out.

Electrochemical performance of Al-substituted Li_3V_2(PO_4)_3 cathode materials synthesized by sol-gel method

The effect of Al-substitution on the electrochemical performances of Li3V2(PO4)3 cathode materials was studied.Samples with stoichiometric proportion of Li3AlxV2-x(PO4)3(x=0,0.05,0.10)were prepared by adding Al(NO3)3 in the raw materials of Li3V2(PO4)3.The XRD analysis shows that the Al-substituted Li3V2(PO4)3 has the same monoclinic structure as the un-substituted Li3V2(PO4)3.The SEM images show that Al-substituted Li3V2(PO4)3 has regular and uniform particles.The electrochemical measurements show that Al-substitution can improve the rate capability of cathode materials.The Li3Al0.05V1.95(PO4)3 sample shows the best high-rate performance.The discharge capacity at 1C rate is 119 mA·h/g with 30th capacity retention rate about 92.97%.The electrode reaction reversibility and electronic conductivity are enhanced,and the charge transfer resistance decreases through Al-substitution.The improved electrochemical performances of Al-substituted Li3V2(PO4)3 cathode materials offer some favorable properties for their commercial application.

Effect of Annealing on Ferroelectric Properties of Bi_ (3.25)La_(0.75)Ti_3O_ (12) Thin Films Prepared by the Sol-gel Method

Bi3.25La0.75Ti3O12（BLT）thin films were prepared on Pt/Ti/SiO2/Si substrate by the sol-gel method.The effect of annealing on their structures and ferroelectric properties was investigated.The XRD patterns indicate that the BLT films annealed at different temperatures are randomly orientated and the single perovskite phase is obtained at 550℃.The remmant polarization increnses and the coercive field decreases with the annealing temperature increasing.The leakage current density of the BLT films annealed at 700℃ is about 5.8×10^-8A/cm^2 at the electrie field of 250kv/cm.

Preparation of BaCe_(0.5)Zr_(0.4)Y_(0.1)O_(3-α) by Sol-Gel Method and Its Electrical Properties

A precursor of BaCe0.5Zr0.4Y0. 1O3-α electrolytes was synthesized by the sol-gel method and sintered at temperature which were 150 - 250 ℃ lower than by solid state reaction. The AC impedance spectrums of electrolytes were measured by AUTOLAB PGSTA30 electrochemical measuring device at different temperatures. The conductivities of the electrolytes are 1.62×10^-4 - 6.43×10^-3, 2.52×10^-5 - 3.73×10^-3S·cm^-1 in the temperature range of 350-800℃. The activity energies are 0.54 and 0.84 eV. At the same time BaCe0.9Y0.1O3-α was prepared by direct solid state reaction. The conductivity of BaCe0.9Y0.1O3-α is 1 × 10^-4- 4×10^-3 S·cm^-1 and the activation energy is 0.50 eV at the same condition. The results show that conduction of electrolyte prepared by sol-gel method is higher than the one by solid state reaction. As far as BaCe0.9Y0.1O3-α concerned, its conductivity of the Zr-substituted specimens is decreased.

BiFeO3-Bi24Fe2O39复合物的制备及可见光催化性能研究

以硝酸铁(Fe(NO3)3·9H2O)硝酸铋(Bi(NO3)3·5H2O)为原料,酒石酸作络合剂,聚乙二醇6000作分散剂,用溶胶-凝胶法制备了BiFeO3-Bi24Fe2O39复合催化剂。用XRD、FT-IR、UV-vis、PL光谱、TG-DSC等对其结构进行了表征。以亚甲基蓝为目标化合物,评价了样品的可见光催化活性。结果表明,500℃煅烧2 h的复合催化剂热稳定性好,荧光强度最强,禁带宽度最小,用500 W的长弧氙灯照射6 h,亚甲基蓝降解率达到93.11%。

Preparation of Al_2O_3-SiO_2-TiO_2-ZrO_2 Composite Ceramic Membranes by Sol-Gel Method

Al 2O 3-SiO 2-TiO 2-ZrO 2 supported membranes were prepar ed by Sol-Gel method. These composite ceramic membranes are level, even and no macro crack. There exist several crystalline phases such as Al 2O 3, TiO 2(a natase), Al 2SiO 5, and ZrO 2 in these membranes. Changing the molar ratio of Al∶Si∶Ti∶Zr,the kinds and content of crystal phases of composite membranes could be different, which may lead to a variety of microstructure of membranes. The surface nanoscale topography and microstructure of membranes were investiga ted by XRD,SEM,AFM,EPMA. The effects of additives and heat treatments on the sur face nanoscale topography and microstructure of composite ceramic membranes were also analyzed.

Anticorrosion of WO₃-Modified TiO₂Thin Film Prepared by Peroxo Sol-Gel Method

The aim of this study was to develop a method to prepare WO3-TiO2 film which has high anticorrosion property when it was coated on type 304 stainless steel. A series of WO3-modified TiO2 sols were synthesized by peroxo-sol gel method using TiCl4 and Na2WO4 as the starting materials. TiCl4 was converted to Ti(OH)4 gel. H2O2 and Na2WO4 were added in Ti(OH)4 solution and heated at 95°C. The WO3-TiO2 sol was transparent, in neutral (pH^7) solution, stable suspension without surfactant, nano-crystallite and no annealing is needed after coating, and very stable for 2 years in stock. WO3-TiO2 sol was formed with anatase crystalline structure. These sols were characterized by XRD, TEM, and XPS. The sol was used to coat on stainless steel 304 by dip-coating. The WO3-TiO2 was anatase in structure as characterized by X-ray diffraction. There were no WO3 XRD peaks in the WO3-TiO2 sols, indicating that WO3 particles were very small, possibly incorporating into TiO2 structure, providing the amount of WO3 was very small. The TiO2 particles were rhombus shape. WO3-TiO2 had smaller size area than pure TiO2. The SEM results showed that the film coated on the glass substrate was very uniform. All films were nonporous and dense films. Its hardness reached 2 H after drying at 100°C, and reached 5 H after annealing at 400°C. The WO3-TiO2 film coated on 304 stainless steel had better anticorrosion capability than the unmodified TiO2 film under UV light illumination. The optimum weight ratio of TiO2: WO3 was 100:4.

Elaboration of an Easy Aqueous Sol-Gel Method for the Synthesis of Micro- and Mesoporous <i>γ</i>-Al₂O₃Supports

An aqueous sol-gel method for the synthesis of γ-Al2O3 supports has been developed for the use in tar reforming applications. It was determined the influences of two different aluminum precursors (aluminum sec-butoxide (Al[OCH(CH3)CH2CH3]3) and aluminum nitrate (Al(NO3)3)) on the textural and crystallographic properties of Al2O3 supports. Only the formation of γ-Al2O3 is aimed in order to use these alumina materials as catalytic supports, because it presents high specific surface area and pore volume values. Additionally, the synthesis of γ-Al2O3 was realized with the use of a functionalized silicon precursor, [3-(2-aminoethylamino)propyl]trimethoxysilane, called EDAS. By the presence of an ethylenediamine group in this molecule, it is possible to chelate metallic ions and to highly increase their dispersion at a molecular level during the synthesis of metallic catalysts supported on alumina, which is an asset for catalytic applications. So it was developed a synthesis sol-gel procedure for the cogelation between the functionalized silicon alkoxide EDAS and alumina precursor. The alumina supports synthesized with Al(NO3)3 as precursor presented higher porous values than the ones obtained with aluminium sec-butoxide precursor. Since nitrate salts are much easier to handle than alkoxides, these observations allowed validating Al(NO3)3 as aluminum source for the future synthesis procedures for metallic catalysts supported on alumina.

不同水热反应条件下BiFeO3颗粒的制备及其光催化性能研究

采用水热法在不同条件下制备BiFeO3光催化剂,利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和紫外-可见漫反射光谱(UV Vis DRS)等对其进行表征,并以罗丹明B(RhB)溶液为降解物,研究BiFeO3的可见光光催化性能.研究结果表明:制备的BiFeO3光催化剂具有单一的晶相,粒径为几微米至几十微米,颗粒团聚,吸收的截止波长约为600 nm.BiFeO3颗粒的催化性能表明:中性环境下BiFeO3颗粒对RhB的降解能力很弱,基本对RhB无降解.将体系引入酸性环境,当体系的pH=5时,RhB经过90 min照射,降解率为89.2%;当体系的pH=3时,经过90 min照射,RhB完全降解.说明在模拟太阳光光照下,BiFeO3颗粒对酸性环境下的RhB有良好的光催化降解作用.

Sb2O3掺杂BiFeO3-BaTiO3压电陶瓷的结构及电性能研究

采用传统固相烧结法合成了0.7BiFeO_(3)-0.3BaTiO_(3)+x%Sb_(2)O_(3)(质量分数)陶瓷(BFO-BTO+x Sb,x=0.00~0.20),研究了Sb_(2)O_(3)掺杂对BFO-BTO陶瓷的晶相结构、介电、导电以及压电和铁电性能的影响,并对影响机理进行探讨。结果表明:Sb掺杂导致陶瓷的晶体结构由伪立方相向菱形相转化。Sb的B位取代增加了BFO-BTO+x Sb陶瓷的铁电弛豫性,降低高温损耗,并使居里温度Tc有所降低。导电特性的研究表明,Sb掺杂改变了V×O和Fe 2+的浓度,降低了电导率,但没有改变陶瓷的导电机制,其主要载流子是氧空位。Sb掺杂量x=0.05时,BFO-BTO+x Sb陶瓷表现出最佳的综合电性能:d 33=213 pC/N,k p=28.8%,Q m=38,T c=520℃,P r=24.7μC/cm^(2)。

Structural,morphological and photoluminescence characterizations of Sm^(3+) doped Y_(2)O_(3) nano-sized phosphors synthesized by ultrasound assisted sol-gel method

Nanosized 1 at% Sm^(3+)doped Y_(2)O_(3)powders were prepared by an ultrasound assisted sol-gel method.Y_(2)O_(3):Sm^(3+)powders crystallize in Y_(2)O_(3)pure cubic phase and XRD analysis shows that the as-used agitation protocol affects strongly the crystallite’s shape and mean size.The recorded emission spectra under λ_(em)=600 nm exhibit two absorption bands;the first one is assigned to O^(2-)→Sm^(3+)charge transfer state(CTS) with a maximum absorption at 223 nm,and the second is due to intraconfigurational transition 4f^(5)-4f^(5) of Sm^(3+) with a maximum absorption at 407 nm.The 223 and 407 nm transitions are attributed to characteristics intra-configurational transitions of Sm^(3+).All emission spectra are dominated by reddish/orange luminescence located at 606 nm and assigned to ^(4)G_(5/2)→^(6)H_(7/2) transition.It is found that the photoluminescence intensity of samples obtained under excitation at 407 nm is 60 times smaller than that obtained under 223 nm excitation.Decay time measurements of the ^(4)G_(5/2)→^(6)H_(7/2) luminescence transition indicate that decay time of nano-sized powder is significantly shorter than bulk material one.

Comparative structural and electrochemical properties of mixed P2/O′3-layered sodium nickel manganese oxide prepared by sol-gel and electrospinning methods:Effect of Na-excess content

The effect of Na-excess content in the precursor on the structural and electrochemical performances of sodium nickel manganese oxide(NNMO)prepared by sol-gel and electrospinning methods is investigated in this paper.X-ray diffraction results of the prepared NNMO without adding Na-excess content indicate sodium loss,while the mixed phase of P2/O′3-type layered NNMO presented after adding Na-excess content.Compared with the sol-gel method,the secondary phase of NiO is more suppressed by using the electrospinning method,which is further confirmed by field emission scanning electron microscope images.N_(2) adsorption-desorption isotherms show no remarkably difference in specific surface areas between different preparation methods and Na-excess contents.The analysis of X-ray absorption near edge structure indicates that the oxidation states of Ni and Mn are+2 and+4,respectively.For the electrochemical properties,superior electrochemical performance is observed in the NNMO electrode with a low Na-excess content of 5wt%.The highest specific capacitance is 36.07 F·g^(-1)at0.1 A·g^(-1)in the NNMO electrode prepared by using the sol-gel method.By contrast,the NNMO electrode prepared using the electrospinning method with decreased Na-excess content shows excellent cycling stability of 100%after charge-discharge measurements for 300 cycles.Therefore,controlling the Na excess in the precursor together with the preparation method is important for improving the electrochemical performance of Na-based electrode materials in supercapacitors.

室温下Sol-Gel法制备BiFeO_3薄膜的铁电和介电性

采用溶胶-凝胶(Sol-Gel)法,在LaNiO3包覆的SiO2/Si衬底上采用不同退火工艺制备了BiFeO3薄膜。原子力显微镜研究表明,薄膜表面光滑,并由不同大小的晶粒组成。X-射线表明不同样品结晶程度不同,并根据不同的退火工艺分别呈(010)择优取向和随机取向。2种取向的薄膜的双剩余极化强度分别为2.84μC/cm2和2.56μC/cm2。择优取向的薄膜在低频下的介电常数和介电损耗较大,且其薄膜中观察到大漏电流。并对两薄膜的导电机制用空间电荷限制的电导理论进行了分析。

Effect of Annealing Temperature on the Ferroelectric Properties of BiFeO_3 Thin Films Prepared by Sol-gel Process

Sol-gel process was adopted to prepare BiFeO3 films.BiFeO3 films were deposited on LaNiO3 coated Si（100） substrates annealed at 500 and 550 ℃,respectively.The X-ray diffraction results reveal that BiFeO3 film has a rhombohedrally distorted perovskite structure with space group R3c.The film annealed at 500 ℃ has larger remnant polarization（Pr） of 35.3 μC/cm2.For the film annealed at 550 ℃,smaller remnant polarization of Pr=4.8 μC/cm^2 is observed for its low breakdown electric field.Lower leakage conduction is observed in the film annealed at 500 ℃ at low applied field.

Preparation and properties of nanocrystal SmBO_3 by nitrate-citrate sol-gel combustion method

Nanocrystal SmBO3 powders were synthesized by nitrate-citrate sol-gel combustion method. The phase evolution, morphologies and absorbency of the synthesized powders were characterized by X-ray diffraction （XRD）, Field emission scanning electronic microscope （FESEM）, Fourier transform infrared spectroscopy （FFIR） and UV-3101PC spectrophotometer （UVPC）, respectively. XRD and FESEM results showed that pure SmBO3 phase was obtained at 750 ℃, with an average original particle size of about 100 nm. FTIR showed that there were apparently concentrated absorbent peaks between 500 and 1400 cm^-1. Moreover, the reflectivity of the powders apparently decreased at the wavelength between 1.05 and 1.15 μm. Therefore, SmBO3 might be a kind of absorbent material for infrared laser.

Ferroelectric properties of Bi_(3.25)La_(0.75)Ti_(3)O_(12) thin films prepared by sol-gel method

The Bi3.25La0.75Ti3O12 thin films were fabricated on the Pt/Ti/SiO2/Si substrates using sol-gel method. The structure and morphology of the films were characterized us-ing X-ray diffraction and atomic force microscopy. The thin films showed a perov- skite phase and dense microstructure. The 2Pr and 2Vc of the Bi3.25La0.75Ti3O12 thin films annealed at 700℃ were 18.6 μC/cm2 and 4.1 V, respectively, under an applied voltage 10 V. After the switching of 1×1010 cycles, the Pr value decreased to 90% of its pre-fatigue values. The films showed good insulating behavior according to the test of leakage current. The dielectric constant and the dissipation factor of the Bi3.25La0.75Ti3O12 thin films were about 176 and 0.046 at 1 kHz, respectively.