Preparation of nano-sized cerium and titanium pyrophosphates via solid-state reaction at room temperature

Nano-sized cerium-titanium pyrophosphates Ce1-xTixP2O7 （with x = 0, 0.2, 0.5, 0.7, 0.9, and 1.0） were obtained by grinding a mixture of Ce（SO4）2·4H2O, Ti（SO4）2, and Na4P2O7·10H2O in the presence of surfactant PEG-400 at room temperature, washing the mixture with water to remove soluble inorganic salts, and drying at 100℃. The products and their calcined samples were characterized using ultraviolet-visible spectroscopy （UV-vis）, thermogravimetry and differential thermal analyses （TG/DTA）, X-ray powder diffraction （XRD）, and transmission electron microscopy （TEM）. The results show that nano-sized Ce1-xTixP2O7 behave as an excellent UV-shielding material. Thereinto, the CeP2O7 has the most excellent UV-shielding effect, and the amorphous state of Ce0.8Ti0.2P2O7 can keep at a higher temperature than CeP2O7. Therefore, the stabilization of the amorphous state of the cerium pyrophosphates was carded out by doping titanium. This stabilization is a significant improvement, which enables to apply these amorphous pyrophosphates not only to cosmetics and paints, but also plastics and films.

Preparing Nano-ZnS by Solid State Reaction at Room Temperature

ZnS nanoparticles were prepared by using solid-state reaction method at room temperature in agate mortar for the first time. The average particle size was about 20nm. This reaction is affected by the structure of reactant, crystal water and defects.

Synthesis of Mesoporous Chromium Aluminophosphate (CrAlPO) via Solid State Reaction at Low Temperature

Mesoporous chromium aluminophosphate （CrAIPO） was successfully synthesized via solid state reaction （SSR） route at low temperature in the presence of a cationic surfactant cetyltrimethyl ammonium bromide （CTAB） and inorganic sources such as A1C13 · 6H20, CrCI3 · 6H20 and NaH2PO4 · 2H20. Characterizations by means of powder X-ray diffraction （XRD）, N2 adsorption- desorption, high resolution transmission electron microscopy （HR-TEM）, scanning electron micrography （SEM）, energy dispersion spectroscopy （EDS）, thermo-gravimetry （TG）, Fourier transform infrared spectroscopy （FT-IR）, and ultraviolet visible light spectroscopy （UV-Vis） were carried out to understand both the pore characteristics and electron transition route of these obtained materials. The experimental results show that the meso-CrA1PO materials with various Cr/A1 molar ratios possess a mesostructure and a specific surface area of 193 to 310 m2/g corresponding to an average pore size of 5.5 to 2.2 rim, respectively. The maxium content of Cr in meso-CrA1PO materials synthesized via SSR route can achieve 16.7wt%, being significantly higher than that of the meso-CrA1PO prepared via a conventional sol-gel route. Meanwhile, the formation mechanism of the meso-CrA1PO was also proposed.

Salt-assisted Low Temperature Solid State Synthesis of High Surface Area CoFe_2O_4 Nanoparticles

A novel salt-assisted low temperature solid state method using CoCl2.6H2O, FeCl3.6H2O and NaOH as precursor and using NaCI as a dispersant to synthesize high surface area CoFe2O4 nanoparticles, has been investigated. The effects of the molar ratio of added salt and calcination temperature on the characteristics of the products were investigated by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, vibrating sample magnetometer （VSM） and Brunauer, Emmett and Teller （BET） surface area analysis. Results showed that the introduction of leachable inert inorganic salt as a hard agglomeration inhibitor in the mixture precursor led to the formation of high dispersive CoFe2O4 nanoparticles; and the increase in specific surface area from 28.28 to 73.97 m^2/g, and the saturation magnetization is 84.6 emu/g.

Preparation of transparent yttrium aluminum garnet ceramics by relatively low temperature solid-state reaction

A new preparation method for a highly sinterable Y 2O 3 powder was developed, using the mixture of the powder with Al 2O 3 powder, a transparent yttrium aluminum garnet(YAG) ceramic was prepared at relatively low temperature by a solid state reaction method. Yttrium nitrate was used as a mother salt, and aqueous ammonia was used as a precipitant reagent, the fine and dendritic precursor crystalline was prepared by adding 0.5% ammonium sulfate into the precipitation reaction system. The highly pure and low agglomerated Y 2O 3 powders were obtained by calcinating the precursor at 1 100 ℃, the primary particles are spherical and 60 nm in diameter. The mixture of Y 2O 3 and Al 2O 3 powders was calcinated, and the resulting mixture compact pressed in mold could be sintered to transparency under vacuum at 1 700 ℃. The sintered transparent YAG polycrystalline exhibits a homogeneous microstructure and its transmittance reaches 45% in the visible light region and 70% in the near infrared wavelength region.

Microstructural evolution of NiFe_2O_4-10NiO powder prepared by high temperature solid state reaction

The NiFe2O4-10NiO powder for inert anode of aluminium electrolysis was prepared by high temperature solid state reaction. The microstructural evolution from the raw materials NiO and Fe2O3 to the NiFe2O4-10NiO powder was studied by SEM. The results show that the domain structure making up of the agglomerate particles of Fe2O3 remains after high temperature solid state reaction, and the diffusion of Ni2+ into Fe2O3 structure is the control step of the reaction process. A microstructure with compact structure and fine grain inside the particle results from the sintering of NiFe2O4-10NiO powder.

Solid-state synthesis of Sr-and Co-doped LaMnO_3 perovskites

The synthesis process for La 1- x Sr x Mn 1- y Co y O 3- δ ( x = 0.2, 0.3; y = 0.2, 0.8, designated as LSMC below) perovskite oxides prepared by solid state reaction was investigated using DSC/TG, XRD, EPMA and particle size analysis methods. It was found that LSMCs were all of single phase and the synthesis process might be divided into three stages: the decomposition of reactants, the formation of LaMn(Co)O 3 based oxides, and the formation of LSMC solid solution. Typical average and the peak value of particle size, and the specific surface area are 14.65?μm, 16.4?μm and 1.38?m 2/mL, respectively, for mixed reactants and are 23.81?μm, 32.11?μm and 0.5?m 2/mL, respectively, for powder synthesized at 1?200?℃ for 8?h in air.

Room-temperature strong coupling between dipolar plasmon resonance in single gold nanorod and two-dimensional excitons in monolayer WSe_2

All-solid-state strong coupling systems with large vacuum Rabi splitting energy have great potential applications in future quantum information technologies, such as quantum manipulations, quantum information storage and processing,and ultrafast optical switches. Monolayer transition metal dichalcogenides（TMDs） have recently been explored as excellent candidates for the observation of solid-state strong coupling phenomena. In this work, from both experimental and theoretical aspects, we explored the strong coupling effect by integrating an individual plasmonic gold nanorod into the monolayer tungsten diselenide（WSe2）. Evident anti-crossing behavior was observed from the coupled energy diagram at room temperature; a Rabi splitting energy of 98 meV was extracted.

Fabrication and characterization of SmO_(0.7)F_(0.2)FeAs bulk with a transition temperature of 56.5 K

The superconductivity of iron-based superconductor SmO 0.7 F 0.2 FeAs was investigated. The SmO 0.7 F 0.2 FeAs sample was prepared by the two-step solid-state reaction method. The onset resistivity transition temperature is as high as 56.5 K. X-ray diffraction （XRD） results show that the lattice parameters a and c are 0.39261 and 0.84751 nm, respectively. Furthermore, the global J c was more than 2.3 × 10 5 A/cm 2 at T = 10 K and H = 9 T, which was calculated by the formula of J c = 20ΔM/[a（1-a/（3b））]. The upper critical fields, H c2 ≈ 256 T （T = 0 K）, was determined according to the Werthamer-Helfand-Hohenberg formula, indicating that the SmO 0.7 F 0.2 FeAs was a superconductor with a very promising application.

液相Y、Nb共掺杂BaTiO_3基PTC陶瓷的制备与性能

本文以Ba(OH)2.8H2O、Sr(OH)2.8H2O、TiCl4、NbCl5、YCl3和Mn(Ac)2为原料,采用室温研磨、低温固态反应合成了一系列的纳米钛酸钡基PTCR陶瓷粉,首先实现了Y和Nb双施主以离子的形式共掺杂。采用XRD,TEM对样品进行了表征。研究表明,产品为立方晶系的完全互溶取代固溶体。粒子基本成球形,分布均匀,粒径大约60 nm。通过优化Y和Nb的掺杂量,使材料的室温电阻得到了进一步降低,并提高了材料的升阻比。当Y、Nb和Mn的用量分别为0.2 mol%、0.18 mol%和0.04 mol%时,加入定量的AST烧结助剂,控制最高烧结温度为1310℃,制备出了室温电阻17.6Ω,正温度系数为18.6%/℃,升阻比为6.5×104的性能优异的PTCR电阻材料。另外还就烧结条件对材料PTC性能的影响进行了讨论。

NaYSiO_(4)∶Ce^(3+)蓝色荧光粉的发光性质及其在白光发光二极管上的应用

采用高温固相法合成了NaYSiO_(4)∶xCe^(3+)(0.01≤x≤0.05)系列蓝色荧光粉。NaYSiO_(4)∶xCe^(3+)荧光粉在250~360 nm之间的宽带吸收能与紫外LED芯片很好地匹配。NaYSiO_(4)∶xCe^(3+)荧光粉中存在多个Ce^(3+)离子荧光中心,且在紫外光激发下表现出峰值波长位于414 nm附近的宽带蓝光发射。NaYSiO_(4)∶0.02Ce^(3+)荧光粉在300~350 nm紫外光激发下量子效率在25%以上。NaYSiO_(4)∶0.02Ce^(3+)荧光粉表现出优良的化学稳定性,在水中浸泡14 d后荧光强度和量子效率几乎不变。将NaYSiO_(4)∶0.02Ce^(3+)蓝色荧光粉、商用(Sr,Ba)_2SiO_(4)∶Eu^(2+)绿色荧光粉和商用(Ca,Sr)AlSiN_(3)∶Eu^(2+)红色荧光粉涂覆于310 nm紫外LED芯片上制备得到了显色指数高达95的LED器件。当驱动电流从50 mA逐渐增大到300 mA时,制备的LED器件表现出稳定的暖白光发射,其色坐标几乎不变。上述结果说明,本研究报道的NaYSiO_(4)∶0.02Ce^(3+)蓝色荧光粉在紫外LED芯片驱动的白光发光二极管照明上有着潜在应用价值。

Preparation and gas sensing properties for acetone of amorphous Ag modified NiFe_2O_4 sensor

Nickel ferrite nano-powders were prepared by microwave radiating low-temperature solid-state reaction method, and then modified with Ag by dipping method. The crystal structure and morphology of the samples were characterized by means of X-ray diffraction（XRD）, scanning electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS）. The gas sensing properties of the samples were also investigated. The results reveal that the Ag, as amorphous structure, can efficiently prevent the reuniting and growing-up of nanosized NiFe2O4 grains, and 1.5% Ag modified NiFe2O4 sensor has a better sensitivity, up to 43, for acetone gas than 1.5%Ag mixed NiFe2O4 sensor prepared by low-temperature solid-state reaction, at an optimal working voltage of 4.5 V. The quick response time （1 s） and fast recovery time （～10 s） are the main characteristics of this sensor.

Bi掺杂BaTiO_3基PTC陶瓷的制备、微结构和电性能

采用液相掺杂及低温固相反应法制备了Bi掺杂BaTiO3纳米晶体,然后经烧结制得了Bi掺杂BaTiO3基PTC陶瓷。分析了所制Bi掺杂BaTiO3晶体的物相、晶粒大小及微结构,研究了烧结条件对所制PTC陶瓷电性能的影响。结果表明:Bi掺杂BaTiO3晶体在常温下为立方晶系,颗粒基本呈球形且大小均匀,粒径约为60 nm;在烧结温度为1 330℃、保温时间为20 min条件下所制PTC陶瓷性能最佳:室温电阻为26.29,升阻比为3.585×104。

无铅高居里点BaTiO_3-Bi_(0.5)K_(0.5)TiO_3陶瓷的制备及其PTC性能的研究

采用固相反应法制备了(1-x)BaTiO3-xBi0.5K0.5TiO3(BT-BKT,x=0,0.1和0.2),对陶瓷样品进行X射线衍射、扫描电镜、介电常数-温度及电阻率-温度测试分析,研究了掺杂BKT对该系统陶瓷相组成、显微结构和电性能的影响。结果表明:BaTiO3陶瓷的晶格参数c轴值随着BKT含量的增加基本不变,而a轴值有所减小。BT-BKT陶瓷的居里温度(Tc)随着BKT的加入向高温移动,当x=0.1和0.2时,Tc分别提高至170℃和185℃左右;但室温电阻率随着BKT含量的增加明显增大。

纳米SiO_(2)包覆Na_(2)Ca_(2.93)Si_(6)O_(16):7% Eu^(3+)荧光粉的制备及性能研究

采用传统高温固相法在1050℃烧结下制备了Na_(2)Ca_(3-x)Si_(6)O_(16)∶xEu^(3+)红色荧光粉,其中Na_(2)Ca_(2.93)Si_(6)O_(16)∶7%Eu^(3+)荧光粉的发光性能最好。采用溶胶-凝胶法制备出纳米SiO_(2)并包覆在Na_(2)Ca_(2.93)Si_(6)O_(16)∶7%Eu^(3+)荧光粉表面,包覆量为2%~10%(wt,质量分数,下同)。通过X射线衍射仪、激发-发射光谱分别对荧光粉物相结构和发光性能进行表征,采用CIE色度坐标分析软件对样品的色度图进行绘制。结果表明纳米SiO_(2)包覆量不同的荧光粉其基质结构未发生改变,纳米SiO_(2)包覆膜是无定型的,样品的发射峰位置没有变化,但发射强度不同;当纳米SiO_(2)包覆量为8%时,荧光粉发射强度最高,比Na_(2)Ca_(2.93)Si_(6)O_(16)∶7%Eu^(3+)荧光粉的发光强度明显提高,且此时色纯度更高,更接近正红色,CIE色度坐标为(0.5282,0.3210)。

红色荧光粉CaWO_(4)∶Eu^(3+),Bi^(3+)的制备和光学性能的研究

本文采用高温固相法合成了一系列红色荧光粉CaWO_(4)∶Eu^(3+),Bi^(3+)。通过X射线衍射仪、扫描电子显微镜和荧光分光光度计等手段,对样品的晶体结构、微观形貌、光学性能、能量传递方式、荧光寿命和热稳定性进行了表征。结果表明,当Eu^(3+)和Bi^(3+)的掺杂浓度分别为7%和2%时(摩尔分数),荧光粉红色发光(615 nm)最强,理论计算得到荧光粉的平均颗粒尺寸为50.27 nm,这与电子显微镜观察结果相符合。能量传递方式以电偶极-电四极相互作用为主,对CaWO_(4)∶7%Eu^(3+),yBi^(3+)(y=0~6%)系列荧光粉进行了荧光寿命测量,发现它们荧光寿命基本相同,都在0.56 ms左右。对CaWO_(4)∶7%Eu^(3+),2%Bi^(3+)荧光粉在不同温度下的光谱进行比较,并且计算相应的色度坐标,当温度升高时,色度坐标整体左移,发光强度有所变弱,但整体来说热稳定性较好。较好的热稳定性和明亮红光发射表明该荧光粉可以作为潜在商用红光荧光粉。

La和Y掺杂对BaTiO_3基PTC陶瓷性能的影响

采用低温固相反应法(800℃)合成了一系列纳米掺杂BaTiO3基PTC瓷粉。经XRD分析,产品为立方晶系的完全互溶取代固溶体。分别研究了La和Y双施主掺杂以及烧结条件对材料PTC性能的影响,实验表明,以La和Y进行双施主掺杂可使材料的室温电阻进一步降低,升阻比提高。通过合理地调整双施主的相对含量,优化烧结制度,制备出了室温电阻为14.25?,升阻比达3.7×104的PTCR材料。

Ba/Fe双掺LaCoO_(3)热敏陶瓷材料低温离子传输机制研究

为了开发电学性能优异的深低温材料,采用传统高温固态法制备了Ba/Fe双掺杂的LaCoO_(3)负温度系数热敏陶瓷材料,结合XRD、SEM、XPS等测试手段,研究了材料的物相结构、微观形貌、离子价态分布等,并在22—80 K和80—290 K范围内进行了低温电学性能测试。结果表明:双掺杂改性降低了LaCoO_(3)材料的应用温区,ρ(22 K)在1.85×10^(5)—6.94×10^(6)Ω·cm范围内变化,材料常数B(22—100 K)在146.09—162.75 K范围内变化;在深低温环境下,材料的导电机理由80 K以上时的小极化子跳跃导电转变为80 K以下时的双交换导电,导致了材料常数B发生突变。由此证明,该双掺杂热敏陶瓷材料在极低温测试中具有可开发的应用潜力。

室温固相反应助力制备氮硫共掺杂碳限域的FeCoS_(2)复合物用于高性能钠离子电池负极

利用室温固相自组装反应制备Co和Fe双席夫碱配合物,随后在硫粉存在下中温热处理,使该配合物同时发生热解碳化和固相硫化反应,从而获得N、S共掺杂碳限域的FeCoS_(2)纳米复合物(记为FeCoS_(2)■NSC)。通过粉末X射线衍射、透射电镜、X射线光电子能谱和热重分析技术分别对纳米复合物的物相、形貌结构、组分和含量等进行物理表征,并通过循环伏安、恒电流充放电技术测试其电化学储钠性能。研究结果表明,最优化条件下制备的复合物(FeCoS_(2)■NSC-7001)中FeCoS_(2)粒子的平均尺寸约为3.4 nm,且被均匀限域在N、S共掺杂的碳基体中;该复合物作为钠离子电池负极时,在0.1 A·g^(-1)的电流密度下经过300次充放电循环,其可逆充电比容量仍高达310.4 mAh·g^(-1);即使在5 A·g^(-1)的大电流密度下,其充电比容量也高达146.0 mAh·g^(-1),呈现优异的电化学储钠性能。

修饰四氧化三锰对尖晶石锰酸锂电化学性能的影响

以硫酸锰为原料,以十六烷基三甲基溴化铵为修饰剂,通过络合沉淀法制备四氧化三锰,再通过高温固相法合成锰酸锂正极材料,探讨了修饰剂用量对四氧化三锰形貌、粒度和锰酸锂正极材料放电比容量的影响。结果表明:未加修饰剂时,制备的四氧化三锰颗粒团聚现象严重;当修饰剂十六烷基三甲基溴化铵质量浓度为3.0 g/L时,制备的修饰四氧化三锰颗粒大小均匀、分散无团聚。用自制的修饰四氧化三锰制备尖晶石锰酸锂,并与市场销售的3种四氧化三锰制备的尖晶石锰酸锂进行了性能对比,结果表明,修饰四氧化三锰制备的锰酸锂电化学性能更优,首次放电比容量达到120.43 mAh/g,1C下循环50次容量保持率为96.79%。