MnO2掺杂对Sr1.95Ca0.05NaNb5O15无铅压电陶瓷微观结构及电学性能的影响

采用固相反应法制备了MnO2掺杂Sr.95Ca0.05.osNaNbsO15+y wt;MnO2(SCNNM)无铅压电陶瓷.研究了MnO2掺杂对SCNNM陶瓷显微结构及电学性能的影响.结果表明:当y≤0.7时,SCNNM陶瓷为单一的四方钨青铜结构,当y≥1.0时有第二相生成;少量MnO2掺杂能有效降低烧结温度,促进晶粒长大,显著提高SCNNM陶瓷的介电、压电性能,降低矫顽场和居里温度,当y＞0.7时,陶瓷烧结恶化,性能降低.当y＝0.5时,SCNNM陶瓷具有较好的介电、压电和铁电性能:介电系数εr＝2123,介电损耗tanδ＝0.038,平面伸缩振动机电耦合系数Kp＝13.4;,厚度伸缩振动机电耦合系数K1＝36.5;,矫顽场E.＝12.68 kV/cm,剩余极化强度Pr＝4.76 μC/cm2,压电系数d33＝190 pC/N,机械品质引因数Qm＝1455,居里温度Tc＝260℃.     

具有倍频效应的硼酸盐Pb2 [B5O9]Br化合物的合成、晶体生长及其性质研究

利用高温固相反应法合成出Pb2 [B5O9]Br硼酸盐粉末.采用PbO-NaF做复合助熔剂,利用顶部籽晶法获得了3 mm ×3 mm ×1.5 mm的透明单晶,X射线粉末衍射数据显示,该晶体属正交晶系,Pnn2空间群,晶胞参数为a=1.1524(1) nm, b=1.1431(1) nm, c=0.65399(3) nm. 红外光谱测量证实晶体结构中含有BO3-3和BO5-4基团.反射光谱表明Pb2 [B5O9]Br的紫外吸收边在250 nm左右.Pb2 [B5O9]Br粉末倍频效应(SHG)测试表明该化合物具有非线性光学效应,信号强度约等同于β-BaB2O4.     

La2Ca1-xSrxB10O19(Sr2+∶LCB)晶体的生长及光学性质

通过顶部籽晶法生长出掺5;和8;Sr2+的La2CaB10O19(LCB)晶体,ICP测得LCB晶体中Sr2+掺入量分别为1.75;和2.02;.XRD证实Sr2+的掺入对LCB晶体晶胞参数的影响较小.摇摆曲线测得Sr2+∶LCB晶体半高宽为36",表明晶体具有较高质量.Sr2+∶LCB晶体在300～2000 nm波段具有较高的透过率,紫外截止边为172 nm.拟合的色散方程符合Sr2+∶LCB晶体折射率的实验值,理论计算表明Sr2+∶LCB晶体可实现相位匹配,其最短二倍频波长小于LCB晶体.     

稀土掺杂Sr5(PO4)2SiO4发光材料的制备工艺研究

采用高温固相法制备了稀土掺杂Sr5(PO4)2SiO4发光材料,研究了样品的发光性能,研究了预烧结温度、烧结温度、烧结时间对样品发光性能的影响.Sr4.975(PO4)2SiO4∶0.025Eu2荧光粉能够被400 nm左右的近紫外光激发,发射光谱受基质品格结构影响呈现双峰发射现象.实验结果表明,预烧结温度选择850℃,烧结温度选择1400℃,烧结时间选择600 min,制得的样品的发光性能最佳.     

(Nb2O5)1-x(TiO2)x陶瓷的制备及其介电性能的研究

我们采用传统固态反应方法烧结制备(Nb2O5)1-x(TiO2)x陶瓷,给出了掺杂量x从0.01到0.13陶瓷的介电性能.在本工艺条件下,所有样品的介电系数均大于120.当样品中TiO2的掺杂量为5mol;时,陶瓷的介电性能最佳:介电系数和损耗分别为217和0.078.XRD测试实验给出,当x≤0.05时,陶瓷的主要相结构为Nb2O5;当x≥0.07时,主相为TiNb24O62.     

La1-x CaxAl0.8Cr0.2O3/CaZrO3(0≤x≤0.2)复相陶瓷材料发射率的研究

以La2O3、Al2O3、ZrO2、Cr2O3、CaCO3为原料,通过高温固相反应法制备La1-xCaxAl0.8 Cr0.2O3/CaZrO3(0≤x≤0.2)复相陶瓷材料,分别通过XRD、SEM和EDS等仪器对试样的物相组成和显微结构进行分析,利用紫外可见近红外分光光度计测量其红外吸收曲线.结果 表明:当CaZrO3理论生成量和La1-xCaxAl0.8Cr0.2O3的摩尔比小于0.20时复相陶瓷材料在0.76～2.5 μm的发射率较La0.8 Ca0.2Al0.8Cr0.2O3得到进一步提高,当CaZrO3理论生成量和La1-xCaxAl0.8Cr0.2O3的摩尔比为0.04时发射率最佳.     

Nb2O5掺杂对Pb(Mg1/3Nb2/3)O3-PbZrO3-PbTiO3陶瓷组织与性能的影响

采用固相烧结法制备Nb2O5掺杂的Pb(Mg1/3Nb2/3) O3-PbZrO3-PbTiO3+ 0.5mol; ZnO(PMN-PZT)压电陶瓷,研究了不同Nb2O5掺杂量对材料结构及压电介电性能的影响.实验结果表明,随着Nb2O5掺杂量的增加(0～1 mol;),PMN-PZT陶瓷的晶界强度提高,断裂模式由沿晶断裂逐渐转变为穿晶断裂,而且陶瓷的压电介电性能升高.当Nb2O5掺杂量为1mol;时,1250℃烧结的陶瓷样品性能参数为:d33=430 pC/N,Qm=60,kp=0.52,kt=0.38,εr=3620,tanδ=0.017.     

Pb0.92Sr0.08-xBax(Sb2/3Mn1/3)0.05Zr0.48Ti0.47O3的制备与性能研究

采用传统固相烧结法制备了Pb0.92Sr0.08-xBax(Sb2/3 Mn1/3)005Zr0.48Ti0.47O3(PSBSM-PZT)压电陶瓷样品.研究了不同Sr2+、Ba2+掺杂含量对样品的相结构、微观形貌、压电和介电性能的影响.结果显示:所有样品均为钙钛矿结构.而当x=0.02～0.06时,陶瓷样品组分位于准同型相界区(MPB).由于位于准同型相界区域的陶瓷样品对于电畴的转向具有促进作用,所以处于MPB区域的陶瓷样品具有较大的压电和介电性能,但同时由于电畴转向带来的较大内摩擦和结构损耗,从而提高了材料的机械损耗和介电损耗.当x=0.02时的陶瓷样品获得最佳的综合性能:d33=346 pC/N,kp=0.58,Qm=1217,εr=1724,tanδ=0.774;.     

CaGd2(MoO4)4:Sm3+,La3+荧光粉的 制备及发光性能研究

采用高温固相法合成了CaGd2-x(MoO4)4:xSm3+(x=0.1、0.3、0.5、0.7、0.9)橙红色荧光粉.研究了样品的X射线衍射谱(XRD)、激发光谱和发射光谱.从XRD图谱测试结果表明,在900℃下烧结6 h后得到的样品为纯CaMnO4晶相,样品CaGd2(MoO4)4:Sm3+的激发光谱由两部分组成:一部分(250～340)nm为属于O2--M6+O的电荷迁移带;另一部分(350～450)nm的系列线状峰是Sm3+的f-f跃迁特征激发峰.样品在405 nm(6H5/24F7/2)下激发得到的发射光谱,其主发射峰位于646 nm(6 G5/26 H7/2)处.当Sm3+掺杂浓度高于2;时,样品CaGd2-x(MoO4)4:xSm3+发生浓度猝灭现象,该现象是由于离子间的能量传递.在CaGd1.5(MoO4)4:0.5Sm3+样品中掺入一定浓度La3+,掺入La3+并没有改变CaGd2(MoO4)4:Sm3+光谱峰的形状和位置,当y=0.8时,荧光粉的发光强度最好.通过测量计算GIE在405 nm激发下的色坐标,显示色坐标均在橙红色区域移动,表明荧光粉的光色性较好.     

La6-xSr4(SiO4)6F2∶xCe3+荧光粉的制备及发光性能研究

采用高温固相法合成了一种新型荧光粉La6-x Sr4(SiO4)6F2∶xCe3+,并通过X射线粉末衍射(XRD)、荧光光谱、荧光寿命等测试手段,对其进行了性能测试及表征.通过分析该荧光粉的荧光光谱,初步研究了其发光性能.结果表明:产物晶体属于六方晶系,磷灰石结构;所得样品在紫外线照射后发蓝光,发射峰位于413 nm,Ce3+的掺杂浓度为10mol;时发光强度最强.     

Czochralski Growth of Potassium Lithium Niobate Single Crystals with Low Li Content and Their Characterization

Single crystalline and crack free potassium lithium niobate (KLN) single crystals with low Li content were grown by the Czochralski method. The crystal composition can be written as K_2.60Li_1.17Nb_5.44O₁₅ (=K_2.95Li_1.33Nb_6.17O₁₇) which contain relatively fewer Li ions than ferroelectric K₃Li₂Nb₅O₁₅ crystals. All experimental results show that the deficiency of the Li ions in the KLN crystals strongly influences their physical properties. Especially, the as‐grown crystals do not indicate any signature for a ferroelectric phase transition in contrast to the ferroelectric K₃Li₂Nb₅O₁₅ crystals. However, due to ionic conduction, the temperature dependence of the dielectric constant of such KLN‐2 crystals show a broad anomaly near 300°C. In addition, the existence of proton defects can be revealed by infrared absorption spectroscopy near 3500 cm^‐1 in as‐grown crystals.     

An effective growth method to improve the homogeneity of relaxor ferroelectric single crystal Pb(In1/2Nb1/2)O3‐ Pb(Mg1/3Nb2/3)O3‐PbTiO3

Compositional segregation usually has negative effects on the growth of solid solution ferroelectric single crystals of Pb(In_1/2Nb_1/2)O₃‐Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ (abbr. PIN‐PMN‐PT or PIMNT). A modified Bridgman method was adopted in this work to control the segregation and improve the compositional homogeneity significantly. The characteristic of this work is to use multiround growths and gradient composition raw materials in order to keep the PbTiO₃ concentration constant during the crystal growth. As an example, the two‐round growth of ternary PIN‐PMN‐PT single crystal is conducted in the same Pt crucible with gradient raw materials, where the first‐round boule was used as the seed crystal for the second‐round growth. Our results show that the as‐grown (Ф80 mm × 270 mm) PIN‐PMN‐PT crystals exhibit higher phase transition temperatures (T_c∼180 °C, T_r/t∼110 °C) and larger coercive field (E_c∼5–5.5 kV/cm), which are much better than the performances of Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ crystals, and similar dielectric and piezoelectric performances (ε∼5000, tanδ∼1.25%, d₃₃∼1500 pC/N, k_t∼60%). And about 85 percent of the crystal boule grown by the two‐round growth technique could maintain its compositions around the morphotropic phase boundary.     

(1-4x)NBT-3xKBT-xBT系压电陶瓷电性能研究

采用传统固相法制备了(1-4x)NBT-3xKBT-xBT(x=0.020～0.035)体系压电陶瓷.采用XRD分析发现该体系陶瓷都能形成单一的钙钛矿型固溶体,并在0.025≤x≤0.032范围内具有三方和四方共存结构,为该体系的准同型相界.当x=0.028时,d33=162 pC/N,Qm=203.29,kp=0.234.电滞回线分析表明,(1-4x)NBT-3xKBT-xBT体系陶瓷随着KBT和BT含量的增加具有从铁电体向反铁电体转变的趋势.     

K2O助溶剂提拉法和富锂提拉法生长的近化学计量比LiNbO3晶体性质的比较

分别采用K2O助溶剂提拉法和富锂提拉法生长了近化学计量比LiNbO3晶体.比较了两种方法生长的晶体紫外吸收边和红外吸收谱的差别,光谱结果表明,K2O助溶剂提拉法生长的晶体组成非常均匀,而富锂提拉法生长的晶体组成不均匀,沿晶体生长方向,Li2O含量逐渐增加.另外,两种生长方法中,籽晶表面均看到螺旋状环,分析了其产生原因.     

Y0.145Gd0.855Ca4O(BO3)3混晶的晶体生长和压电、热膨胀性能

利用提拉法成功生长出了Y0.145Gd0.855Ca4O(BO3)3(Y0.145Gd0.855COB)混晶.对其压电系数和热膨胀系数进行了测量,测得压电系数d26为9 pC/N,计算得到热膨胀系数α11,α22 α33分别为12.97×10-6/℃,5.94×10-6/℃,8.03×10-6/℃.通过与YCa4O(BO3)3和GdCa4O(BO3)3晶体的对比,分析了Re3+半径和Re3+、Ca2+的无序分布对于Y0.145 Gd0.855COB混晶的压电性能和热膨胀性能的影响.     

Li_(0.067)Na_(0.933)Tb(MoO_4)_2磁光晶体的生长与磁光性能

采用Czochralski法生长了Li_(0.067)Na_(0.933)Tb(MoO_4)_2晶体,并测试了Li~+在NaTb(MoO_4)_2晶体中的有效分凝系数.由粉末X射线衍射数据计算了晶体的晶胞参数.室温下,采用消光法测试了Li_(0.063)Na_(0.933)Tb(MoO_4)_2晶体在532 nm、633 nm和1064 nm处的费尔德常数,分别为-293.6 rad·m~(-1)·T~(-1)、-200.5 rad·m~(-1)·T~(-1)和-68.6 rad·m~(-1)·T~(-1),与纯NaTb(MoO_4)_2相比,其费尔德常数均有所增加.结果表明,在1064 nm处Li_(0.067)Na_(0.933)Tb(MoO_4)_2晶体有较高的磁光优值.     

Transport Properties of (NH4)2 CuCl4.2H2O Low Dimensional Single Crystals

The X‐ray diffraction and Infrared (IR) spectral studies of (NH₄)₂ CuCl₄.2H₂O single crystals reveals that these crystals contains tetragonal crystal structure with the unit cell dimensions of a = 7.58Å, c = 7.95Å, z= 2, β =90° and two water molecules in the unit cell. The temperature dependence of thermally stimulated depolarization current (TSDC) and dc electrical conductivity (σ) studies of this two‐dimensional (NH₄)₂ CuCl₄.2H₂O single crystal have been carried out in 77K–300K temperature region. The TSDC thermograph shows only one sharp peak at 248K with a peak current of 130nA, which is attributed to the Maxwell‐Wagner peak. The activation energy (U), relaxation time (τ) are calculated as 0.78eV and 3.44×10^‐15 s respectively. Dc electrical conductivity studies of these crystals show a first order phase transition at about 248K.     

Synthesis and single crystal X‐ray structure of the tetragonal tungsten bronze Pb0.91K1.72Li1.46Nb5O15

Crystals of Pb_0.91K_1.72Li_1.46Nb₅O₁₅, belonging to tetragonal tungsten bronze materials, were grown by the slow cooling technique, and characterized by means of single crystal X‐ray diffraction: the structure was solved in the P4bm tetragonal space group, with the following unit cell parameters: a = 12.548(5), c = 4.042(5) Å, V = 636.4(9) ų. The three‐dimensional framework can be described as a layered structure down crystallographic axis c, with arrays of NbO₆ octahedra, whose corner sharing makes up the formation of tunnels filled up by Li, Pb and K displaying complex cation‐oxygen coordinations. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

CsB3O5(CBO)晶体生长和形貌研究

本文采用籽晶浸没法,在Cs2O过量3;的Cs2O-B2O3体系中生长了CsB3O5单晶.生长参数如下:液面以下温度梯度为0.5℃/cm, 晶体旋转速度为12r/min,降温速率0.2℃/d,可获得透明、无包裹体、无开裂、最大尺寸达65×44×49mm3的CsB3O5单晶.研究了CsB3O5的生长形貌,CsB3O5生长没有明显的方向性,总是呈现长柱状,最易出现的晶面是(011)和(101)晶面.     

Growth and characterization of ferroelectric‐ferroelastic Tb2(MoO4)3 crystals

Transparent and nearly colorless ferroelectric‐ferroelastic β′‐Tb₂(MoO₄)₃ (TMO) single crystals have been grown by the Czochralski (CZ) method. The single crystal structure was investigated by X‐ray powder diffraction and was shown to be a single phase with the structure similar as the β′‐Gd₂(MoO₄)₃ crystal. The optical transparency of the TMO crystal has been measured and the crystal is almost transparent in the visible and near infrared regions. The defects of TMO crystal were evaluated by etching technique and the ferroelectric domain structures were observed by an optical microscope. A high‐resolution X‐ray diffraction analysis demonstrates that the as‐grown TMO crystal possesses relatively high optical quality. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)