Thermal expansion properties and hygroscopicity of Y2-xSmxW3O12 (x = 0.0-0.4) compounds

A novel class of solid solutions of Y2-xSmxW3O12 (x = 0.0-0.4) were synthesized and studied by means of powder X-ray diffraction. All samples crystallize in an orthorhombic space group Pnca. The lattice parameters a, b and c of Y2-xSmxW3O12 increase with increasing Sm content. Since the compounds of this series hydrate at room temperature, thermogravimetric (TG) analysis was carried out. The result shows that the compound stores less water with increasing Sm content. The thermal expansion properties of Y2-xSmxW3O12 (x = 0.1, 0.3 and 0.4) were investigated with high temperature X-ray diffraction. Negative thermal expansion coefficient -α becomes less negative from -6.644×10-6 to -6.211×10-6℃-1 when x changes from 0.1 to 0.4.     

Al/Y_2W_3O_(12)复合材料的制备、热膨胀及电性能研究

采用固相法制备Al/Y_2W_3O_(12)复合材料,研究了Al与Y_2W_3O_(12)以不同质量比合成样品的特性。X射线衍射表明:样品只含有Al和Y_2W_3O_(12),不存在Al对Y的取代。SEM和EDS分析表明:小颗粒Y_2W_3O_(12)嵌入在块状Al基底中,为嵌入式复合结构。热膨胀性能和电导率测试分析表明:当Al与Y_2W_3O_(12)的质量比7∶3时,Al/Y_2W_3O_(12)样品的线膨胀系数14.76×10-6/K(RT~600℃)约为Al的一半,呈现良好的导电性,其导电率为18.2 S/m可达Al的电导率的1/2,且Al/Y_2W_3O_(12)样品几乎不表现出吸水性。研究认为,该复合材料具有低膨胀和较高导电性是由于其特有的嵌入式结构所致。     

Effect of Li content on the microstructure and properties of lead-free piezoelectric （K0.5Na0.5）1-xLixNbO3 ceramics prepared by SPS

Lead-free piezoelectric （K0.5sNa0.5）1-xLixNbO3 （x = 0at%-20at%） ceramics were synthesized by spark plasma sintering （SPS） at low temperature and the effects of LiNbO3 addition on its crystal structure and properties were also studied. When the Li content was less than 6at%, a single proveskite phase with the similar structure of （K0.5Na0.5）NbO3 was formed; and a secondary phase with K3Li2Nb5O15 structure was observed in the 6at% 〈 x 〈 20at% compositional range. Furthermore, LiNbO3 existed as the third phase when the Li content was higher than 8at%. The grain sizes increased from 200-500 nm to 5-8 μm when the K3Li2Nb5O15 and LiNbO3 like phases were formed. With increasing Li content, the relative density of the ceramics first decreased from 97% to 93% and then kept constant. The piezoelectric coefficient d33, dielectric constant, and planner electromechanical coupling factor exhibited a decreasing tendency with increasing Li content because of the decrease in density and the formation of the secondary phase such as K3Li2Nb5O15 and LiNbO3. The formation of dense microstructure with a single phase is necessary in improving the properties of the （K0.5Na0.5）1-xLixNbO3 ceramics.     

(1-x)Ca_5Zn_4(VO_4)_6-xCa_(0.8)Sr_(0.2)TiO_3陶瓷微波介电性能研究

采用传统固相法制备(1-x)Ca5Zn4(VO4)6-xCa0.8Sr0.2TiO3(0.5≤x≤0.8)系陶瓷,并研究其烧结特性、晶相组成、显微组织和微波介电性能变化规律。用X射线衍射仪(XRD)和扫描电子显微镜(SEM)分析陶瓷的晶相组成和显微组织,采用闭腔法测量其微波介电性能。研究表明,随着Ca0.8Sr0.2TiO3含量增加,陶瓷的εr和τf值逐渐增大,而Q×f值逐渐减小。875℃/5h烧结0.3Ca5Zn4(VO4)6-0.7Ca0.8Sr0.2TiO3名义陶瓷具有最佳微波介电性能,即εr=13.5,Q×f=12 800GHz,τf=3ppm/℃。     

Mn3(Cu0.6Si0.15Ge0.25)N/Ag复合材料的负热膨胀与物理性能

采用机械球磨加固相烧结法合成Mn3(Cu0.6Si0.15Ge0.25)N/Ag复合材料。在77K-300K温度范围内,分别研究了Mn3(Cu0.6Si0.15Ge0.25)N/Ag复合材料的热膨胀性能,电导性能和热导性能。当含Ag量分别为1,5,10和20 wt%时,所有样品在有效的温度区间205K-275K表现出负热膨胀。随着Ag含量的增加,有效温度区间向室温方向移动。另外,和Mn3(Cu0.6Si0.15Ge0.25)N材料相比,Mn3(Cu0.6Si0.15Ge0.25)N/Ag复合材料具有更高的电导率1?0-6（Ohm.m）-1和热导率10.5W/(mK)。     

A位Y^（3＋）替代α-BZN陶瓷结构及介电性能研究

采用传统的固相反应法制备了（Bi1.5-xYxZn0.5）（Zn0.5Nb1.5）O7（BYZN,0≤x≤0．2mol）陶瓷,借助XRD、SEM和Agilent4284A测试仪,研究了A位替代对OL—BZN结构和介电性能的影响。研究表明：当掺杂量xY^（3＋）〈0．15mol时,样品相结构中没有出现其他杂相,为单一立方焦绿石相;随掺杂离子的进一步增加,样品中出现少量第二相。陶瓷样品的晶粒尺寸和介电性能随着Y^（3＋）掺杂量的增加而呈现有规律的变化;低温介电弛豫峰的峰形逐渐宽化;xY^（3＋）≤0．15mol时,1MHz下弛豫峰峰值温度Tm由-117℃逐渐增加到-108℃。     

Superparamagnetism in Zn Substituted Copper-gallate Ferrite

Solid solution of spinel ferrite Cu1-xZnxFe2-yGayO4 with (0.0≤x≤0.5 and y=0.1) are synthesized. XRD measurements confirm the presence of single-phase tetragonal structure with c/a>1 for CuFe2O4 and samples with (x=0.0 and 0.1). The tetragonal phase is attributed to the presence of the cooperative Jahn-Teller Cu ions in the octahedral B-site in the spinel lattice. Tetragonal-to-cubic transformation is occurred at the compositional parameter x≥0.2 and the lattice parameter a is found to decrease with increasing Zn content x. 57Fe M(o)ssbauer measurements at 293K for these compounds reveal superparamagnetic phase for samples with (0.0≤x≤0.2). In contrast, M(o)ssbauer spectra at 12K for these materials show well ordered spectra where, the cation distribution and the hyperfine parameters are determined.     

Effects of yttrium on the formation and magnetic properties of bulk metallic glassy （Fe, Co）-B-Si-Nb alloys

The bulk metallic glassy (BMG) rods of [(Fe0.5Co0.5)0.72B0.192Si0.048Nb0.04]100-xYx (x=0-6) and [(FexCo1-x)0.72B0.192Si0.04]Nb0.04]96Y4 (x=0.5-0.8) were prepared by copper mold casting. The structure, thermal stability,and magnetic properties of the samples were studied by X-ray diffraction (XRD), differential scanning calorimetry (DSC), and vibrating sample magnetometer (VSM). Adding lat% to 6at% of yt-trium, the bulk glassy alloy rods of [(Fe0.5Co0.5)0.72B0.192Si0.048Nb0.04]100-xYx (x=0-6) with the diameter of 3 mm were not formed, and the sample with 4at% of yttrium showed less crystalline phase than others. When the Fe/Co atomic ratio was between 5:5 and 7:3, the bulk glassy alloy rods of [(Fe1-xCox)B0.192Si0.048Nb0.04]96Y4 (x=0.5-0.8) with the diameter of 2 mm were fabricated. In the (Fe, Co)-B-Si-Nb-Y BMGs, when the Fe content increased, the thermal stability, the supercooled liquid region, and the glass-forming ability (GFA) decreased, but the saturation magnetization (Ms) increased.     

热压合成Ti_4AlN_3及其物理性能研究

以摩尔比为Ti ◇Al ◇TiN=1 1.2 2.7的混合粉为原料,采用真空热压烧结工艺在1400℃保温2 h成功合成了高纯Ti4AlN3块体材料,Ti4AlN3烧结试样结晶良好,晶粒发育完善,内部较为均匀致密,相对密度达到98.5%,具有较高的抗弯强度（384 MPa）、抗压强度（523 MPa）和断裂韧性（6.5（MPa.m1/2））,较低的维氏硬度（2.9 GPa）和抗破坏能力,具备良好的机械加工性能。Ti4AlN3常温电导率和热导率分别为4.6×105（Ω-1.m-1）和12（W.m-1.K-1）,其热导率在25～600℃范围呈上升趋势;25～1100℃的线膨胀系数为9.0×10-6K-1,良好的导热性能和高温热稳定性使其可以应用于高温领域。     

一个簇基无机-有机杂化材料的合成与表征

对簇基无机-有机杂化材料的制备方法及表征手段进行了研究。利用水热合成技术制备了一个具有新颖结构的簇聚物(H_2en)_2(H_3O)_(12)[Si_2Mo_(14)~(VI)Mo_2~VV_2~VV_(10)~(IV)O_(84)](1,en=乙二胺),采用元素分析、红外光谱、X射线光电子能谱、电子顺磁共振、TG及X射线单晶衍射等技术对晶体结构进行了分析。结构分析显示,簇基杂化材料是由两个高还原态的二帽Keggin型簇阴离子[Si(1)Mo_6~(VI)Mo_2~VV_6~(IV)O_(42)]~(10-)和[Si(2)Mo_8~(VI)V_2~VV_4~(IV)O_(42)]~(6-)通过(μ_2-O)_2双桥氧原子连接成以簇阴离子二聚体为结构单元的1-D链,相邻的1-D链再经质子化的水分子通过氢键连接成新颖的3-D簇阴离子超分子网络,质子化的乙二胺和水分子填充于网络之中。磁性研究表明化合物1金属离子间存在反铁磁性相互作用。     

ZrW2-xMoxO8的合成、表征与热膨胀特性

立方结构的ZrW2-xMoxO8氧化物材料具有各向同性负热膨胀效应，但难以用固相化学反应法制备．采用水热法合成了Zr(W，Mo)2O7(OH)2(H2O)2，热重-差热分析(TG—DTA)表明，Zr(W，Mo)2O7(OH)2(H2O)2的DTA曲线上有明显的ZrW2-xMoxO8结晶转变点，且结晶点随Mo含量的增加而降低．严格控制加热工艺条件，将Zr(W，Mo)2O7(OH)2(H2O)2作为前驱体低温合成了ZrW2-xMoxO8系列氧化物材料，高温X射线衍射分析表明ZrW2-xMoxO8具有强烈的负热膨胀效应．     

Microstructure, crystalline phase and electrical properties of Li0.06（Na0.5K0.5）0.94Nb（1-2x/5）MgxO3 lead-free piezoelectric ceramics

MgO-modified Li0.06(Na0.5K0.5)0.94NbO3(L6NKN) lead-free piezoelectric ceramics were synthesized by normal sintering at a relatively low temperature of 1000°C.The crystalline phase,microstructure,and electrical properties of the ceramics were investigated with a special emphasis on the influence of MgO content.The addition of MgO effectively improves the sinterability of the L6NKN ceramics.X-ray diffraction analysis indicates that the morphotropic phase boundary(MPB) separating orthorhombic and tetragonal ph...     

掺杂氧位Bi_(1.5)ZnNb_(1.5)O_7陶瓷结晶化学与介电性能

用F-替代氧离子O2-,采用固相反应法制备Bi1.5-xCaxZnNb1.5O7(0.00≤x≤0.30,简称C-x)、Bi1.5-x CaxZnNb1.5O7-yFy(0.00≤x≤0.20,简称CF-x)陶瓷样品,研究F-添加的缺陷补偿形式、替代位置,以及对Ca2+掺杂的Bi1.5ZnNb1.5O7(简称α-BZN)陶瓷的相结构、结晶化学和介电性能的影响。结果表明:F-的引入降低了Ca2+在α-BZN陶瓷的固溶度,替代八面体BO6的氧位;在等量Ca2+掺杂的情况下,引入F-进入体系后,样品的介电常数减小,介电损耗下降,这与F-引入α-BZN陶瓷后,四面体A4O'键价和比Ca2+单独掺杂时高一致;F-替代导致介电峰值温度均向高温移动,这可能与F-的添加导致激活能增加有关。     

连续变温下早龄期混凝土应变时变规律试验研究

针对早龄期混凝土开裂现象,为掌握其应变变化规律,通过日大气温度变化影响下早龄期混凝土应变随时间变化的模拟试验,采集试件的应变及重量数据,分析早龄期混凝土在日气温变化影响下的应变变化规律.研究结果表明:在日气温变化的升温和降温过程中,早龄期(3d内)混凝土均数次出现量级达1 00×10-6的剧烈收缩,受到约束时可产生易使混凝土开裂的应力;不同水灰比混凝土之间的膨胀应变差值、收缩应变差值分别可达100×10-6、200×10-6.     

Ti掺杂Te置换型CoSb_3的高压合成及电热输运性能研究

Co Sb3基方钴矿化合物具有优良的电输运性能,是一种极具潜力的新型中温热电材料,但其相对较高的热导率限制了它在热电方面的应用和发展。针对方钴矿化合物特殊的笼状晶体结构,本文采用高温高压合成方法制备了具有Skutterudite结构的Ti掺杂Te置换型方钴矿热电材料,利用X射线衍射以及扫描电镜对该类样品的晶体结构和断面微观形貌进行了分析。分析结果表明高温高压合成方法可以快速的制备出单相Skutterudite结构、晶界明显且晶粒较小(1~3μm)的方钴矿热电材料。研究了室温情况下合成压力与Ti原子的掺杂浓度对所得样品热学与电学输运性能的影响规律。所得结果表明:通过高压快速制得的Ti掺杂Te置换型样品呈n型传导,与预期相同,Ti掺杂Te置换型Co Sb3样品的Seebeck系数随合成压力的升高而升高;不同掺杂浓度的样品获得最大功率因子(~10μWcm-1K-2)的合成压力均在1.5GPa左右;样品的热导率和晶格热导率整体上随着合成压力升高而降低。     

高岭土掺杂NASICON固体电解质及全固态电池性能

针对LiTi2(PO4)3基固态电解质电导率低的问题,采用浙江三门高岭土矿作为主要原料,以高温固相法制备铝、镁、硅共掺杂钠超离子导体(NASICON)型快离子导体Li1+2x+2yAlxMgyTi2-x-ySixP3-xO12.研究掺杂比例、温度对固态电解质离子电导率的影响.结果表明,组成为Li1.8Al0.1Mg0.3Ti1.6Si0.1P2.9O12固体电解质在423 K时有最高离子电导率7.86×10-4 S·cm-1.以该组成固态电解质为基片,喷雾热解原位制备Al/ Li1+xV3O8/ Li1.8Al0.1Mg0.3Ti1.6Si0.1 P2.9O12 /C全固态电池并在1.8～3.9 V电压区间进行50次充放电测试.该电池具有较好的稳定性及循环容量保持能力.30次循环以后放电容量基本稳定在190～205 mAh·g-1之间,充放电效率大于90%.     

Thermal expansion behavior of KZr2P3O12-SrZr4P6O24 ceramics

The relationships between thermal expansion and density,microcracking,stress and phase transition in K1/2Sr1/4Zr2P3O12(K2) and with K2 containing 2 mass fraction of MgO (K2M2) have been studied.The materials showed a little thermal expansion anisotropy,hysteresis,and microcracking Thermal shock-induced cracks resulted in a decrease of the coefficient of thermal expansion.Phase transition caused crack healing resulting in a decrease in specimen size.     

（0.82-x）Bi0.5Na0.82Ti O3-0.18Bi0.5K0.18TiO3-xBiFeO3（x=0.01-0.07）无铅压电陶瓷的制备及其电学性能的研究

采用传统的固相烧结法于1120℃烧结2 h得到（0.82-x）Bi0.5Na0.82Ti O3-0.18Bi0.5K0.18TiO3-xBiFeO3（x=0.01-0.07）无铅压电陶瓷,并对该体系陶瓷的微观结构和电学性能进行了研究。结果表明,BiFeO3的引入量x为0.01-0.07时,样品均为具有MPB准同型相界（三方相和四方相共存）的钙钛矿结构。BiFeO3的引入使陶瓷的晶粒度略有增加;当x=0.03时,样品达到最大致密度。为97.7%;陶瓷的压电常数d33随BiFeO3的引入而降低。陶瓷的相对介电常数εr和居里温度随BiFeO3的引入而明显增大,在x=0.03时达到最大值。     

Effect of aluminum addition on microstructure and properties of SiO<Subscript>2</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-CaO vitrified bond

Influence of aluminum addition on the structures and properties of SiO₂-B₂O₃-Al₂O₃-CaO vitrified bond at low sintering temperature and high strength was discussed. FTIR and XRD analyses were used to characterize the structures of the basic vitrified bond with different contents of aluminum. The bending strength and the thermal expansion coefficients were also tested. Meanwhile, the microstructures of composite specimens at sintering temperature of 660 °C were observed by scanning electron microscope (SEM). The experimental results showed that the properties of vitrified bond with 1wt% aluminum were improved significantly, where the bending strength, Rockwell hardness, and thermal expansion coefficient of the vitrified bond reached 132 MPa, 63 HRB, and 6.73×10^-6 °C^-1, respectively.     

Ti/RuO_2-Co_3O_4阳极析氧性能

为制备高性能析氧电极,采用热分解法在400℃温度下制备Ti/RuO2(x)-Co3O4(1-x)(0≤x≤1,x为Ru的摩尔分数)复合氧化物电极,通过电极开路电压、循环伏安曲线及极化曲线等分析其在1.0mol/LKOH溶液中的析氧催化活性及析氧动力学.结果表明,摩尔分数为10%的RuO2使电极催化活性急剧变化,摩尔分数为50%的RuO2复合氧化物电极具有最大的伏安电荷(429.63mC.cm-2)、最高的表面粗糙度(1786),其析氧性能最佳;Ti/Co3O4在高、低过电位区域电极对OH-的反应级数分别近似为1.0和2.0,含RuO2电极反应级数均为1.0.