聚合物前驱体法制备铌酸钾钠纳米粉体

采用聚合物前驱体法,以柠檬酸(CA)为络合剂,乙二醇(EG)为酯化剂合成了纳米级(Na0.35K0.65)NbO3。研究了乙二醇用量对聚合物前驱体稳定性的影响,结果表明n(EG):n(CA)为2时能得到稳定凝胶,与乙二醇和柠檬酸聚酯化反应得到凝胶的理论配比一致。XRD分析表明聚合物前驱体在650℃煅烧2h可制得平均晶粒尺寸为24nm左右,纯单斜相结构的(Na0.35K0.65)NbO3纳米粉体,该合成温度比传统固相法降低了约300℃。     

用聚合物前驱体法低温合成铌酸锂纳米粉体

用聚合物前驱体法,以柠檬酸为配位剂．乙二醇为酯化剂．水为溶剂合成纳米铌酸锂（LiNbO3）粉体。研究发现：当柠檬酸和金属离子的摩尔比（下同）为3：1,柠檬酸和乙二醇的为1：2时,可形成稳定的Li-Nb前驱体溶液和凝胶。用差热-热重分析研究凝胶前驱体的热分解历程。用X射线衍射分析和红外光谱分析研究凝胶前驱体及其不同温度下煅烧所得粉体的相组成和结构。结果表明：Li-Nb凝胶前驱体在加热过程中分解形成LizCO3相．Li2CO3与Nb2O3发生固相反应生成LiNbO3。凝胶前驱体经800℃煅烧2h可以制备纯钙钛矿型的纳米LiNbO3粉体。     

聚合物前驱体法制备ZnTiO3粉体的影响因素

聚合物前驱体法已成为制备微波介质陶瓷重要方法之一.本文以制备ZnTiO3粉体为例,系统地研究了pH值,乙二醇与柠檬酸的摩尔比和柠檬酸与金属离子的摩尔比对ZnTiO3晶相的形成过程和显微结构的影响.pH值5～6之间时,能形成淡黄色透明溶胶;乙二醇与柠檬酸的摩尔比为2时,前驱体树脂为多孔的海绵状;柠檬酸与金属离子的摩尔比为2,前驱体合成的ZnTiO3粉体最佳.     

铌酸锂铁电薄膜的制备与表征

采用柠檬酸盐法制备铌酸锂铁电薄膜。探讨了柠檬酸（CA）和乙二醇（EG）的用量、pH和水浴温度等工艺参数对溶胶性能的影响。采用XRD和TG—DTA研究了铌酸锂（LiNbO3）晶相的形成过程，用XRD和AFM对所制得薄膜的物相组成和表面形貌进行了表征。结果表明，当前驱体溶胶的pH为7．5，水浴温度大于80℃，n（CA）：n（Li＋Nb）=3：1，n（CA）：n（EG）=1：2时，可以获得稳定性好的溶胶。薄膜经缓慢升温至800℃热处理，可以获得单相、表面光滑、晶粒大小均匀、晶粒大小为70nm的LiNbO3铁电薄膜。     

流延法制备铌酸钾钠无铅压电陶瓷的工艺研究

以Na2CO3,K2CO3,Nb2O5等为原料,采用固相法合成了K0.5Na0.5NbO3的粉体,并以此粉体为主要原料,添加适量的分散剂、粘结剂及除泡剂制备浆料,采用流延法制备K0.5Na0.5NbO3膜片,研究了K0.5Na0.5NbO3固相含量、分散剂、粘结剂及除泡剂的种类及含量对流延浆料流延性能和对K0.5Na0.5NbO3陶瓷的影响。实验结果表明:流延膜的厚度在0.3mm时,选用三乙醇胺作分散剂效果最好,当固相含量在55wt%时,分散剂用量在2%时浆料的粘度为2000mPa.s,适合于流延工艺;粘结剂PVB的含量在8%时膜片强度较高。     

过量Na~+对(K_(0.5)Na_(0.5))NbO_3-LiNbO_3无铅压电陶瓷相组成及结构的影响

通过固相反应法预合成0.94(K0.5Na0.5)NbO3-0.06LiNbO3(KNLN6)无铅压电陶瓷粉体。采用X线衍射仪(XRD)、扫描电子显微镜/能谱仪(SEM/EDS)和高分辨透射电子显微镜(HRTEM)对KNLN6试样进行性能表征。结果表明:按化学计量配比合成的KNLN6粉体中含有K3Li2Nb5O15(KLN)第二相;Na2CO3摩尔分数过量5%时,可有效地消除第二相KLN,从而获得单一钙钛矿结构的KNLN6粉体,同时,粉体的预烧温度降低了50℃;在1070℃下烧结2 h制备的Na2CO3过量5%的无铅压电陶瓷中,KNLN6晶体具有A位无序的单一正交钙钛矿结构,晶粒呈立方体状,平均尺寸约为10μm。     

制备工艺对0.95(K_(0.5)Na_(0.5))NbO_3-0.05CaZrO_3基无铅陶瓷压电性能的影响

采用传统陶瓷工艺制备了0.95(K0.5Na0.5)NbO3-0.05CaZrO3无铅压电陶瓷。研究了烧结温度和极化工艺对陶瓷压电性能的影响。结果表明:随着烧结温度的提高,0.95(K0.5Na0.5)NbO3-0.05CaZrO3陶瓷的体积密度增大,在1170℃时达到最大值,同时d33和kp,在此温度也分别达到他们的最大值210pC/N和0.40。极化工艺对0.95(K0.5Na0.5)NbO3-0.05CaZrO3陶瓷的压电性能有明显的影响,0.95(K0.5Na0.5)NbO3-0.05CaZrO3陶瓷的最佳极化温度是70℃,最佳极化电场是4kV/mm。     

MgO掺杂铌酸钾钠基晶体材料的制备、结构及性能EI北大核心CSCD

采用无籽固相晶体生长法制备MgO掺杂的K0.5Na0.5NbO3基无铅压电单晶。采用X射线衍射仪、扫描电子显微镜和压电铁电测试仪等研究了MgO掺杂对K0.5Na0.5NbO3基晶体的生长、微结构和压电铁电性能的影响。结果表明:添加MgO后,仍可采用无籽固相晶体生长法制备出K0.5Na0.5NbO3基单晶;MgO的加入没有明显改变K0.5Na0.5NbO3基单晶的晶体结构,MgO溶入铌酸钾钠晶格形成了均匀的固溶体;适量MgO的添加有利于提高K0.5Na0.5NbO3基单晶的压电和铁电性能、降低介电损耗,当MgO的掺杂量为0.6%(质量分数)时,K0.5Na0.5NbO3基单晶的压电常数d33=203 pC/N,介电损耗tanδ=0.028,介电常数ε=221,矫顽电场Ec=7 kV/cm,剩余极化强度Pr=36.5μC/cm^2。     

锂掺杂KNN-BNKT无铅压电陶瓷性能研究

采用液相包覆法制备了结构致密的铌酸钾钠基[(K0.5Na0.5NbO3-K0.1Na0.4Bi0.5TiO3)-xLiNbO3,0≤x≤0.02]无铅压电陶瓷,研究了掺杂Li+对铌酸钾钠钛酸铋钾钠K0.5Na0.5NbO3-K0.1Na0.4Bi0.5TiO3(KNN-BNKT)晶体结构和压电、介电性能的影响。结果表明:当Li+含量在x取0～0.010(摩尔分数)时,陶瓷样品均形成了均一的钙钛矿型结构。Li+掺杂量对陶瓷压电、介电性能有很大的影响,其压电常数(d33)随着Li+掺杂量的增加先升高后降低,并在x=0.010的时候取得最大值。实验表明:当x=0.01时,(K0.5Na0.5NbO3-K0.1Na0.4Bi0.5TiO3)-xLiNbO3无铅压电陶瓷表现出较好的压电性能:d33=173pC/N,相对介电常数εr=620.745,介电损耗tanδ=0.0132,kp=27.35%,kt=26.34%,Qm=48.97。     

EDTA-柠檬酸络合法制备葡萄状硅酸钇纳米晶

分别以硝酸钇(Y(NO3)3·6H2O)和正硅酸乙酯(TEOS)为起始原料,首次尝试采用乙二胺四乙酸(EDTA)-柠檬酸(CA)络合法制备合成硅酸钇(Y2Si2O7)纳米晶陶瓷粉体,研究并讨论了样品前驱体pH值和烧结温度等工艺参数对硅酸钇粉体微观形貌及其合成机理的影响.利用XRD、FE-SEM、T-IR和TGA-DTA等分析方法对制备的样品进行了表征.结果表明,在前驱体溶胶pH值为9.38、煅烧温度为1050℃时的工艺条件下,可以得到晶粒尺寸为50 nm左右、主要组成为α-Y2Si2 O7相硅酸钇粉体;粉体晶粒尺寸随烧结温度升高而增大,且粉体晶粒形貌为葡萄状的组织结构;而在前驱体溶胶pH值为4.00时,采用该方法合成的产物则是物相组成为单硅酸钇(Y2 SiO5)陶瓷粉体.     

Piezoelectric K0.5Na0.5NbO3 Ceramics Textured Using Needlelike K0.5Na0.5NbO3 Templates

Improved performance by texturing has become attractive in the field of lead‐free ferroelectrics, but the effect depends heavily on the degree of texture, type of preferred orientation, and whether the material is a rotator or extender ferroelectric. Here, we report on successful texturing of K_0.5Na_0.5NbO₃ (KNN) ceramics by alignment of needlelike KNN templates in a matrix of KNN powder using tape casting. Homotemplated grain growth of the needles was confirmed during sintering, resulting in a high degree of texture parallel to the tape casting direction (TCD) and the aligned needles. The texture significantly improved the piezoelectric response parallel to the tape cast direction, corresponding to the direction of the strongest <001>_pc orientation, while the response normal to the tape cast plane was lower than for a nontextured KNN. In situ X‐ray diffraction during electric field application revealed that non‐180° domain reorientation was enhanced by an order of magnitude in the TCD, compared to the direction normal to the tape cast plane and in the nontextured ceramic. The effect of texture in KNN is discussed with respect to possible rotator ferroelectric properties of KNN.     

四元复合氧化物La_(0.5)Sr_(0.5)Ni_(0.5)Cu_(0.5)O_3的抗硫性能

以SO2 为毒物 ,采用脉冲中毒方法 ,再以CO氧化反应为探针 ,对三元复合氧化物催化剂La0 .5Sr0 .5NiO3 与La0 .5Sr0 .5CuO3 以及四元复合氧化物催化剂La0 .5Sr0 .5Ni0 .5Cu0 .5O3 等三种催化剂样品的抗硫毒能力、失活曲线、中毒催化剂的再生性能以及毒物残留形态等进行了全面考察和对比分析。实验结果表明四元复合氧化物催化剂La0 .5Sr0 .5Ni0 .5Cu0 .5O3 在SO2 毒物含量是 1 2 2×10 -2 mmol时 ,特别是在高温 (≥ 30 0℃ )条件下 ,具有优异的抗硫性能     

Thermally-stable large strain in Bi(Mn0.5Ti0.5)O3 modified 0.8Bi0.5Na0.5TiO3-0.2Bi0.5K0.5TiO3 ceramics

(1-x)[0.8Bi_0.5Na_0.5TiO₃-0.2Bi_0.5K_0.5TiO₃]-xBi(Mn_0.5Ti_0.5)O₃ (x = 0–0.06, BNKMT100x) lead-free ferroelectric ceramics were prepared via solid state reaction method. Bi(Mn_0.5Ti_0.5)O₃ induces a structure transition from rhombohedral-tetragonal morphotropic phases to pseudo-cubic phase. Moreover, the wide range of compositions within x = 0.03–0.055 exhibit large strain of 0.31%–0.41% and electrostrictive coefficient of 0.027–0.041 m⁴/C². Especially, at x = 0.04, the large strain and electrostrictive coefficient are nearly temperature-independent in the range of 25–100 °C. The impedance analysis shows the large strain and electrostrictive coefficient originate from polar nanoregions response due to the addition of Bi(Mn_0.5Ti_0.5)O₃.     

Na0.5Bi0.5TiO3-Ba0.5Sr0.5Nb2O6无铅压电陶瓷的研究

采用固相法制备了(1-x)(Na0.5Bi0.5)TiO3-xBa0.5Sr0.5Nb2O6(0≤x≤1.0％)(简称(1-x)NBT-xBSN)无铅压电陶瓷,研究了不同BSN含量(x=0,0.1％,0.3％,0.5％,0.7％,1.0％,摩尔分数)样品的物相组成、显微结构及电性能.结果表明:所有样品均为纯钙钛矿结构,随掺杂量x的增加,陶瓷的相对密度pr、压电常数d33和机电耦合系数kp均先增大后降低,机械品质因子Qm和退极化温度Td则逐渐下降.该体系陶瓷具有弥散相变特征,弥散指数介于1.6～1.7.当x=0.5％时,陶瓷获得最佳性能:d33=92pC/N,kp=0.164,Qm=89,εr=650,tanδ=5.47％,pr=96.5％.     

Near-infrared emitting CdTe0.5Se0.5/Cd0.5Zn0.5S quantum dots: synthesis and bright luminescence

We present how CdTe_0.5Se_0.5 cores can be coated with Cd_0.5Zn_0.5S shells at relatively low temperature (around 200°C) via facile synthesis using organic ammine ligands. The cores were firstly fabricated via a less toxic procedure using CdO, trioctylphosphine (TOP), Se, Te, and trioctylamine. The cores with small sizes (3.2-3.5 nm) revealed green and yellow photoluminescence (PL) and spherical morphologies. Hydrophobic core/shell CdTe_0.5Se_0.5/Cd_0.5Zn_0.5S quantum dots (QDs) with tunable PL between green and near-infrared (a maximum PL peak wavelength of 735 nm) were then created through a facile shell coating procedure using trioctylphosphine selenium with cadmium and zinc acetate. The QDs exhibited high PL efficiencies up to 50% because of the formation of a protective Cd_0.5Zn_0.5S shell on the CdTe_0.5Se_0.5 core, even though the PL efficiency of the cores is low (≤1%). Namely, the slow growth process of the shell plays an important role for getting high PL efficiencies. The properties of the QDs are largely determined by the properties of CdTe_0.5Se_0.5 cores and shells preparation conditions such as reaction temperature and time. The core/shell QDs exhibited a small size diameter. For example, the average diameter of the QDs with a PL peak wavelength of 735 nm is 6.1 nm. Small size and tunable bright PL makes the QDs utilizable as bioprobes because the size of QD-based bioprobes is considered as the major limitation for their broad applications in biological imaging.     

K0.5Na0.5NbO3-BaCu0.5W0.5O3无铅压电陶瓷的结构与性能

以传统固相法工艺制备(1-x)K0.5Na0.5NbO3-xBaCu0.5W0.5O3[(1-x)KNN-xBCW]无铅压电陶瓷,研究不同BCW掺量(x=0％,0.1％,0.25％,0.5％,1.0％,摩尔分数,下同)对KNN陶瓷的晶体结构和电性能的影响,结果表明:x＜0.5％时,KNN陶瓷的相结构没有改变,仍为正交相...     

Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3系无铅压电陶瓷的极化工艺研究

主要研究了极化电场,极化时间和极化温度等工艺参数对Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3系无铅压电陶瓷介电和压电性能的影响。结果表明:极化电场和极化温度对压电陶瓷的介电、压电性能影响较大,而极化时间则影响较小。适宜的极化电场是3～3.5kV/mm,极化温度70～80℃,极化时间为10～15min。     

CeO2掺杂钛酸铋钠钾陶瓷的制备工艺与介电性能

为了进一步探索合成工艺对钛酸铋钠系无铅材料的结构及介电特性的影响,本文以甘氨酸为燃料,利用固相-燃烧法制备了CeO2掺杂的Bi0.5Na0.5TiO3-Bi0.5K0.5TiO3 (BNKT)陶瓷.XRD表明,在固相合成工艺中引入燃烧法制备BNKT陶瓷,比传统固相法降低预烧温度150 ℃,掺杂的CeO2扩散进入了BNKT钙钛矿的晶格,且当掺杂量为0%~0.3%时,形成纯的钙钛矿相结构;SEM表明,CeO2掺杂使晶粒尺寸趋于平均,对晶粒生长有抑制作用;介电温谱表明,随着CeO2掺杂量增加,介电常数εr和退极化温度Td、相转变温度Tm降低,介电反常峰逐渐弱化,且室温至300 ℃,介电损耗tanδ始终在0.3%以下,并从微结构缺陷空位形成机制角度,结合铁电畴壁运动状态,分析讨论了对材料介电特性的作用规律.     

Raman spectroscopy of Na0.5Bi0.5TiO3

We have measured the Raman spectra of bismuth sodium titanate in its rhombohedral, tetragonal, and cubic phases, with special attention paid to the phase transitions at 584K and 837K (heating). Both transitions appear to be order-disorder and strongly first order, with large thermal hysteresis. The phonon spectra at temperature slightly below the tetragonal phase are remarkably similar to BaTiO₃ with A₁(To) modes at 130, 269, and 541 cm^-1 (compared with 170, 270, 520 cm^-1 in BaTiO₃) and an E(TO) at 52 cm^-1.     

Characterization of multiferroic PbFe0.5Nb0.5O3 and PbFe0.5Ta0.5O3 ceramics derived from citrate polymeric precursors

Ceramics of the perovskite multiferroics PbFe_0.5Nb_0.5O₃ (PFN) and PbFe_0.5Ta_0.5O₃ (PFT) were synthesized from new citrate polymeric precursors. X-ray tests pointed to trace amounts of the pyrochlore phase. SEM studies revealed the heterogeneous grain size distribution for PFN and the homogeneous one for PFT. Dielectric studies pointed to one diffuse T-C phase transition at 378 K for PFN and two diffuse M-T and T-C phase transitions, at 200 and 235 K, for PFT, respectively. X-ray photoelectron spectroscopy studies of PFN reveal that all ions exist in one valence state, however, with two chemical shifts for Pb²⁺. Two valence states for the majority of ions of PFT seem to be connected with a higher volume fraction of the amorphous grain-boundary phase. The electronic energy band gap for both compounds is approximately 2.8 eV. Two magnetic transitions, ie, from the paramagnetic to the antiferromagnetic phase and then to the spin-glass phase, were observed at 156 and 10 K for PFN, and at 145 and 15 K for PFT, respectively.