熔盐法制备Bi1.5ZnNb1.5O7陶瓷粉体

以Bi2O3,ZnO和Nb2O5为原料,KCl为熔盐,用熔盐法合成了单相Bi1.5ZnNb1.5O7陶瓷粉体.XRD和SEM分析表明,在950～1000 ℃,合成了单相Bi1.5ZnNb1.5O7粉体,粉体呈颗粒状,尺寸约2～5 μm.研究了合成温度、熔盐含量和保温时间对粉体颗粒形貌和尺寸的影响.结果表明,合成温度对Bi1.5ZnNb1.5O7粉体形貌和尺寸影响较大,熔盐含量和保温时间对其形貌和尺寸的影响相对较小.     

Bi1.5ZnNb1.5O7纳米粉体的水热合成与表征

以分析纯的Bi(NO_3)_3·5H_2O,ZnO和Nb_2O_5为初始原料,KOH为矿化剂,采用水热法合成立方焦绿石结构的Bi_(1.5)ZnNb_(1.5)O_7纳米粉体。通过XRD分析其物相组成,TEM分析其形貌和尺寸,Scherrer公式计算其晶粒的大小。结果表明,在KOH浓度为1.8mol/L,温度为180～220℃反应6～48h,可以合成立方焦绿石结构的Bi_(1.5)ZnNb_(1.5)O_7纳米粉体,粉体颗粒尺寸约30～50nm,形貌呈较为规则的颗粒状。合成温度和反应时间对合成粉体的物相和粒径都有一定的影响,并讨论了水热法合成Bi_(1.5)ZnNb_(1.5)O_7纳米粉体的机理。     

水热法制备BiFeO3粉体的工艺研究

以Bi(NO)3·5H2O和Fe(NO)3·9H2O为初始原料,KOH、NaOH和LiOH·H2O为矿化剂,乙二醇、浓度为65％ ～68％硝酸和氨水为辅助试剂,水热合成BiFeO3粉体.X-射线衍射图表明,当采用不同的矿化剂合成样品时,可以得到不同的铋铁系化合物,采用KOH为矿化剂时,更容易得到单相BiFeO3粉体;另外发现不使用辅助剂溶解硝酸铋,不仅容易得到单相BiFeO3粉体样品,而且工艺简单.在此基础上,进一步研究了KOH浓度、反应时间、反应温度和前驱物浓度对合成单相BiFeO3粉体的影响.     

钛酸铋钾纳米粉体的水热法制备和表征

以Bi(NO3)3·5H2O和纳米Ti O2作为铋源和钛源,KOH作为钾源和矿化剂,采用水热法制备钛酸铋钾,(K,Bi)Ti O3(KBT)纳米粉体,并对样品进行了XRD和SEM表征。结果表明,在反应温度为180℃时保温24 h,能够得到单一晶相的KBT粉体。KOH浓度由6 mol/L增加到8 mol/L时,KBT由赝立方晶相变为四方晶相,说明粉体粒径尺寸明显增大;KOH浓度为6 mol/L时,粒径尺寸约50 nm。     

CoFe2O4纳米颗粒的溶液合成及磁性能

以Co(NO3)2.6H2O和Fe(NO3)3.9H2O为原料,采用直接溶液合成法制备CoFe2O4纳米粉体。分析了纳米粉体的物相结构、微观形貌及合成机理,研究了热处理温度对粉体磁性能的影响。结果表明:所得CoFe2O4粉体为立方尖晶石铁氧体,颗粒细小、分散均匀,平均粒径约为5nm。500℃以下热处理的粉体表现出良好的超顺磁性;500℃以后,随热处理温度上升,颗粒尺寸变大,粉体的比饱和磁化强度Ms、比剩余磁化强度Mr和矫顽力Hc均增大。室温下CoFe2O4粉体的Ms为3.4A.m2/kg。当热处理温度为900℃时,Ms增大到59.5A.m2/kg,Hc增大到97.0kA/m。     

纯相BiFeO_3微晶的水热合成及表征

以Bi(NO3)3.5H2O和Fe(NO3)3.9H2O为原料,KOH为矿化剂,聚乙二醇6000为分散剂,水热合成BiFeO3粉体,XRD和Raman光谱对粉体的表征说明在200℃反应6 h可以得到纯净的单相BiFeO3粉体,热分析结果得到BiFeO3粉体的磁相变温度——尼尔温度(TN)和铁电相变温度——居里温度(Tc)。     

液相沉淀法制备HfO2纳米粉体

以HfOCl2·8H2O为原料,采用化学沉淀法在不同的pH值下制备HfO2纳米粉体,并对制备的纳米粉体采用XRD,DSC-TG,TEM,BET等方法进行表征.研究了pH值对粉体比表面积、粒径的影响.结果表明:本方法制备的纳米粉体呈简单正交晶型,平均粒径为10m,粒度分布窄,随着pH值的增加,粉体有比表面积增大,平均粒径减小的趋势,但变化幅度较小.     

Bi4Si3O12纳米粉体的制备与表征

以正硅酸乙酯和Bi2O3为原料,采用溶胶-凝胶法制备了硅酸铋(Bi4Si3O12)纳米粉体.通过X射线衍射和电子显微镜分析了合成粉体的相结构和形貌,测定了粉体的粒度分布曲线,研究了正硅酸乙酯用量对产物相组成的影响.结果表明:干凝胶粉末在750℃热处理2 h,得到了粒径为40～100nm的粉体.正硅酸乙酯的实际用量为理论用量的6倍时,可以制备出相组成为Bi4Si3O1 2的纳米粉体.纳米尺度的Bi4Si3O12材料的激发光谱和发射光谱相对于晶体材料发生了蓝移.     

熔盐法合成片状SrBi2Nb2O9粉体

以分析纯的Bi2O3,Nb2O5和SrCO3为原料,以NaCl和KCl为熔盐,采用熔盐法在800～1150℃合成了单相生长的各向异性的片状SrBi2Nb2O9陶瓷粉体.X射线衍射分析表明:熔盐法合成的陶瓷粉体为单相SrBi2Nb2O9,没有其它杂相生成.扫描电镜分析显示:所得粉体呈明显的片状,无团聚现象.研究了合成温度、熔盐含量对粉体颗粒形貌和尺寸的影响.结果表明:在熔盐与原料的质量比≤1的情况下,随着合成温度的升高和熔盐含量的增加,片状粉体尺寸增大.探讨了熔盐法合成SrBi2Nb2O9陶瓷粉体的机理.     

水热法制备ZrO2(3Y)纳米粉体中复合矿化剂的作用

本文以K2CO3／KOH复合矿化剂水溶液作为反应介质，水热制备四方相ZrO2（3Y）纳米粉体，并借助XRD、TEM、BET等测试手段，对粉体的性能进行表征。实验结果表明：随着K2CO3/KOH浓度（0．1M、0．3M、0．5M、0．7M）的增加，ZrO2（3Y）粉体的比表面积呈下降趋势，对应的等比表面积当量球径呈上升趋势，晶粒尺寸增大；随着K2COJKOH比率（1，2，3）的增加，粉体的比表面积由于矿化剂浓度的增加而下降的趋势更加明显。     

Ce3+掺杂的Ca1.5Y1.5Al3.5Si1.5O12荧光粉发光性能研究

采用高温固相法合成白光LED用Ca1.55Y1.5Al3.5Si1.5O12:x Ce3+黄绿色荧光粉,利用X-射线粉末衍射和荧光光谱进行表征。实验结果表明,在紫外近紫外区(200~380nm)激发下荧光粉发射光谱主峰位于402nm,在蓝光454nm激发下荧光粉发射光谱主峰位于530nm。当灼烧温度为1623K,Ce3+掺杂浓度为10%,发光强度最高。随着Ce3+的掺杂增加会发生浓度猝灭。该荧光粉与商业近蓝光芯片发射相匹配,是一种优秀的白光LED用黄绿色荧光粉。     

Comparison of microwave dielectric behavior between Bi1.5Zn0.92Nb1.5O6.92 and Bi1.5ZnNb1.5O7

The microwave dielectric, Bi_1.5ZnNb_1.5O₇ exhibits low-temperature dielectric relaxation. To find the origin of the dielectric relaxation of Bi_1.5ZnNb_1.5O₇, we studied the structure and dielectric behavior of Bi_1.5ZnNb_1.5O₇ in detail. The Bi_1.5ZnNb_1.5O₇ is not composed of a single phase pyrochlore structure. Instead, it consists of unusual structure of Bi_1.5Zn_0.92Nb_1.5O_6.92 and ZnO. The ZnO is distributed evenly in the grain and at the boundary of the Bi_1.5Zn_0.92Nb_1.5O_6.92 structure. Many small voids (<1 μm) were observed in the samples due to the loss of volatile Bi during sintering. The Bi_1.5Zn_0.92Nb_1.5O_6.92 exhibited a broad dielectric relaxation between 100 and 400 K at 1.8 GHz, peaking around 230 K. The Fourier transformation IR spectra predict that dielectric relaxation may occur near room temperature during extremely high frequencies (THz). The substitutional point defects in Bi_1.5Zn_0.92Nb_1.5O_6.92 provide room for dielectric relaxation at microwave frequencies. The low quality factor Q × f (∼520 GHz) of Bi_1.5Zn_0.92Nb_1.5O_6.92 results from both the dielectric relaxation of the material and the voids within its microstructure. The presence of ZnO phase in the Bi_1.5ZnNb_1.5O₇ produces interstitial defects that further enhance the dielectric relaxation with reduced quality factor Q × f (∼426 GHz).     

CeO2–YO1.5–NdO1.5 system: An extensive phase relation study

The sub-solidus phase relations in the CeO₂–YO_1.5–NdO_1.5 system have been studied. About 45 compositions in the series Ce_1?x(Y_0.70Nd_0.30)_xO_2?0.5x, Y_1?x(Ce_0.50Nd_0.50)_xO_1.5+0.25x and Nd_1?x(Ce_0.55Y_0.45)_xO_1.5+0.275x were prepared and characterized by powder XRD. In the Ce_1?x(Y_0.70Nd_0.30)_xO_2?0.5x series, there was a gradual transformation from the defective F-type cubic lattice to an ordered C-type phase with increasing x, whereas in the Y_1?x(Ce_0.50Nd_0.50)_xO_1.5+0.25x series, the C-type cubic lattice of yttria was retained over the entire range. In the Nd_1?x(Ce_0.55Y_0.45)_xO_1.5+0.275x system, the compositions with NdO_1.5 content greater than 95 mol% showed coexistence of hexagonal, monoclinic and cubic phases. A biphasic region of monoclinic and C-type cubic phases was observed as NdO_1.5 decreases from 90 to 70 mol%. All the compositions below 70 mol% NdO_1.5, were found to be C-type cubic solid solutions. The phase relations are distinctly characterized by an extensive range of cubic solid solutions, stable under the slow-cooled conditions. To the best of our knowledge, this is the first detailed sub-solidus study reported in CeO₂–YO_1.5–NdO_1.5 system.     

Dielectric properties and electrical behaviors of tunable Bi1.5MgNb1.5O7 thin films

The Bi_1.5MgNb_1.5O₇ (BMN) thin films were prepared on Au-coated Si substrates by rf magnetron sputtering. We systematically investigated the structure, dielectric properties and voltage tunable property of the films with different annealing temperatures. The relationships of leakage current and breakdown bias field with annealing temperature were firstly studied and a possible explanation was proposed. The deposited BMN thin films had a cubic pyrochlore phase when annealed at 550 °C or higher. With the increasing of annealing temperature, the dielectric constant and tunability also went up. BMN thin films annealed at 750 °C exhibited moderate dielectric constant of 106 and low dielectric loss of 0.003–0.007 between 10 kHz and 10 MHz. The maximum tunability of 50% was achieved at a bias field of 2 MV/cm. However, thin films annealed at 750 °C had lower breakdown bias field and higher leakage current density than films annealed below 750 °C. The excellent physical and electrical properties make BMN thin films promising for potential tunable capacitor applications.     

Ni替代Nb对Bi1.5ZnNb1.5O7陶瓷介电性能的影响

以分析纯级原料,按照一定比例混合,利用固相反应制备Bi1.5ZnNb1.5O7陶瓷.研究结果表明:Ni掺杂样品能够有效地降低烧结温度至960℃;样品相结构保持立方焦绿石相;随着Ni3+替代量的增加,介质材料的介电常数及介电损耗逐渐增大;在-195～150℃的温度范围内,介电常数存在明显的弛豫现象,随Ni3+的掺杂量增加,逐渐向高温方向移动,在1 MHz下其峰值温度为:-98.1℃,-97.7℃,-97.1℃,-94.2℃.     

Green emitting Ba1.5Lu1.5Al3.5Si1.5O12: Ce3+ phosphor with high thermal emission stability for warm WLEDs and FEDs

By hetero-valence substituting Ba²⁺-Si⁴⁺ for Lu³⁺-Al³⁺ pair in Lu₃Al₅O₁₂: Ce³⁺, a new green phosphor Ba_1.5Lu_1.5Al_3.5Si_1.5O₁₂: Ce³⁺ (BLAS: Ce³⁺) has been obtained. It crystallizes in garnet structure with space group Ia-3d (230). In the structure, Ba²⁺ ions are incorporated into both dodecahedral Lu³⁺ and octahedral Al³⁺ sites while Si⁴⁺ ions only occupy tetrahedral Al³⁺ sites. Under the blue light irradiation of 450 nm, an intense green light peaking at 520 nm was observed and the PL spectrum can be fitted in two Gaussian components, due to the crystal field splitting of Ce³⁺ 5d states under D₂ symmetry constrains. The optical doping concentration of BLAS: Ce³⁺ is 6% mol, of which the IQE and EQE are 89.1% and 51.8%, respectively. Furthermore, this sample exhibits an extremely good thermal stability, i.e. the integrated emission intensity is still more than 90% of the initial intensity at 480 K. Then, a w-LED device was fabricated from this new green phosphor BLAS: Ce³⁺ and commercial red phosphor (Ca,Sr)AlSiN₃: Eu²⁺, which shows a quite high color rendering (Ra = 88.2) and a relatively low color temperature 4772 K. Besides, the phosphor exhibits a stable chromaticity under different acceleration voltages. The phosphor may be promising material for the development of solid-state lighting and display systems.     

Cold sintering process of Li1.5Al0.5Ge1.5(PO4)3 solid electrolyte

The recently developed technique of cold sintering process (CSP) enables densification of ceramics at low temperatures, i.e., <300°C. CSP employs a transient aqueous solvent to enable liquid phase‐assisted densification through mediating the dissolution‐precipitation process under a uniaxial applied pressure. Using CSP in this study, 80% dense Li_1.5Al_0.5Ge_1.5(PO₄)₃ (LAGP) electrolytes were obtained at 120°C in 20 minutes. After a 5 minute belt furnace treatment at 650°C, 50°C above the crystallization onset, Li‐ion conductivity was 5.4 × 10^?5 S/cm at 25°C. Another route to high ionic conductivities ~10^?4 S/cm at 25°C is through a composite LAGP ‐ (PVDF‐HFP) co‐sintered system that was soaked in a liquid electrolyte. After soaking 95, 90, 80, 70, and 60 vol% LAGP in 1 M LiPF₆ EC‐DMC (50:50 vol%) at 25°C, Li‐ion conductivities were 1.0 × 10^?4 S/cm at 25°C with 5 to 10 wt% liquid electrolyte. This paper focuses on the microstructural development and impedance contributions within solid electrolytes processed by (i) Crystallization of bulk glasses, (ii) CSP of ceramics, and (iii) CSP of ceramic‐polymer composites. CSP may offer a new route to enable multilayer battery technology by avoiding the detrimental effects of high temperature heat treatments.     

Structure,dielectric and optical properties of Bi1.5+xZnNb1.5O7+1.5x pyrochlores

Non-stoichiometric pyrochlore ceramics with formula Bi_1.5+xZnNb_1.5O_7+1.5x were systematically investigated. Crystal structures of the compounds were studied by X-ray diffraction (XRD) technique. The structures were identified as pure cubic pyrochlores when |x| < 0.1. Dielectric and optical properties of the compositions when x = −0.1, 0 and 0.1 were studied. All samples have high resistivities and low dielectric loss. With increasing x in Bi_1.5+xZnNb_1.5O_7+1.5x, the lattice constant, permittivity, temperature coefficient of permittivity and thermal expansion coefficient increased, while dielectric loss decreased. Raman spectra indicated that the intensity of Bi–O stretching become stronger with increasing x. A vibration mode emerging at 861 cm⁻¹ when x = −0.1 means that the B–O coordination environment is significantly more disordered. Absorption spectra suggested that the bandgap energy become lower from 2.86 to 2.70 eV as lattice constants increased. Strong absorption occurs at wavelengths from 433 to 459 nm, shows that samples have the ability to respond to wavelengths in the visible light region.