铈镧复合氧化物对ZnVCrO陶瓷显微结构及压敏性能的影响

采用混合氧化物工艺经850℃、4h烧结制备了铈镧复合氧化物掺杂的ZnVCrO基压敏陶瓷,综合应用XRD、SEM、EDS和伏安电学特性测试等方法研究了铈镧复合氧化物掺杂在0%~0.6%(质量分数)范围内对显微结构和压敏性能的影响。结果显示,所有样品以ZnO为主晶相,以Zn_3(VO_4)_2、ZnCr_2O_4为第二相,含掺杂样品中还形成Ce(La)VO_4固溶体,其含量随掺杂量增加而升高。铈镧复合氧化物对烧结影响不大,但其含量大于等于0.4%(质量分数)时可大幅提高ZnVO基压敏陶瓷显微组织的均匀性。0.4%(质量分数)铈镧复合氧化物掺杂样品压敏性能最优:非线性系数为24.7,压敏电压为1 029V/mm,漏电流为92μA/cm~2。     

镧、铈掺杂TiO_2超滤膜的制备

考察了镧、铈掺杂对二氧化钛(TiO2)超滤膜的影响。镧掺杂可以有效抑制TiO2晶型随烧结温度增加的急剧转变。镧、铈掺杂可以有效控制膜层的粒径和孔径,并提高其抗酸碱性能。TiO2膜层粒径为60~80nm,孔径为10~60nm,抗酸碱性能较差;而经镧、铈掺杂后的TiO2膜层粒径为50nm左右,孔径为10~20nm,抗酸碱性能较好,其中镧掺杂效果优于铈掺杂。     

ZnS∶La纳米晶的制备及其光学性质研究

采用醋酸锌、醋酸镧和硫代乙酰胺(TAA)为原料,水热合成法制备了粒度分散均匀的镧掺杂硫化锌纳米晶.粉末X-射线衍射(XRD)和透射电子显微镜(TEM)测试结果表明合成的样品为立方闪锌矿结构;纳米晶为近球形的多晶粒子,平均粒径在25nm左右且分布较窄.从纳米晶紫外-可见(UV-vis)光谱数据计算的半导体带宽(Eg)相对于体相材料有较大的蓝移,表现出明显的量子尺寸效应.用荧光光谱(PL)研究了ZnS∶La纳米晶的光致发光能力,结果表明产物的荧光发射峰位于465nm左右,且具有良好的发光性能.此外,通过改变镧的掺杂量和反应的时间来研究发光强度的变化,随着掺杂量的提高和反应时间的延长,纳米晶的发光强度都呈现出先增强后减弱的趋势,并对具体原因进行了探讨.     

镧掺杂TiO2/膨润土复合光催化材料的制备及性能

以钠基膨润土为载体,钛酸丁酯和硝酸镧为原料,采用溶胶-凝胶法制备镧掺杂TiO2/膨润土复合光催化剂,采用X射线衍射(XRD)和红外光谱(IR)对复合催化剂进行了表征,在紫外光照射下,通过对TNT废水的光催化降解,考察其光催化活性。实验结果表明,掺杂镧与未掺杂镧的TiO2/膨润土复合光催化剂中TiO2主要以锐钛矿型存在;掺杂镧的TiO2/膨润土复合光催化剂的光催化性能明显优于未掺杂镧的TiO2/膨润土复合光催化剂,当镧的掺杂量为1%(原子分数),焙烧温度为500℃时,其光催化活性达到最佳效果。     

氧化物掺杂钼丝中掺杂颗粒的特性

钼丝和钼箔广泛用于白炽灯作冷却芯杆、灯丝支架和箔封.掺杂钼具有很高的高温强度和再结晶温度,高温应用中已大量取代未掺杂的钼材.掺杂铝-钾-硅(AKS)的钼由于细小钾泡对晶界的钉扎作用,再结晶温度可达1 800℃(未掺杂的钼仅为1 200℃),而氧化镧掺杂的钼,再结晶温度更高.为了弄清掺杂剂的作用,美国通用电气环球研究所的L.E.Iovio等人对AKS掺杂钼丝和氧化镧掺杂钼丝中的掺杂颗粒的特性进行了研究,制作了直径为0.18 mm和0.41 mm的AKS掺杂钼丝,并分别用2 000℃,10 min和2 350℃,30 min的工艺制度进行再结晶热处理.还制作了直径为0.51 mm,0.62 mm和0.64 mm的氧化镧掺杂钼丝,分别用1 800℃,30 min和2 350℃,30 min的工艺制度进行再结晶热处理.用透射电镜(TEM)对两类掺杂钼丝的加工态和退火态进行了分析.     

RF溅射稀土掺杂ZnO薄膜的结构与发光特性

通过射频磁控溅射技术在Si(111)衬底上制备了未掺杂和La、Nd掺杂ZnO薄膜.XRD分析表明,ZnO薄膜具有c轴择优生长,La、Nd掺杂ZnO薄膜为纳米多晶薄膜.AFM观测,La、Nd掺杂ZnO薄膜表面形貌较为粗糙.从薄膜的室温光致光谱中看到,所有薄膜都出现了395 nm的强紫光峰和495 nm的弱绿光峰,La掺杂ZnO薄膜的峰强度增大,Nd掺杂ZnO薄膜的峰强度减弱,分析了掺杂引起PL峰强度变化的原因.     

纳米La-TiO2光催化降解甲基橙废水的研究

采用溶胶-凝胶法制备了纯TiO2和La掺杂TiO2复合纳米粉体,通过XRD,UV-Vis等测试手段分析了在紫外光照射下,以降解甲基橙为探针反应研究其可见光催化性能。结果显示样品均为锐钛矿相纳米TiO2,稀土元素镧掺杂后纳米TiO2特征衍射峰宽化,强度降低;掺入的La主要以La2O3的形式存在,同时有一部分形成Ti-O-La键;La掺杂可减小TiO2晶粒尺寸及增大催化剂比表面积;与未掺杂的二氧化钛相比较,适当含量的镧掺杂可有效促进TiO2表面光生载流子的分离,从而显著提高其光催化活性。当La/Ti的摩尔比为0.010时,可见光催化性能最好。     

La3+-Pr3+共掺杂纳米TiO2粉体的光催化性能

以钛酸四丁酯(TBT)为原料, 采用溶胶-凝胶法制备了纯TiO₂和La³⁺-Pr³⁺共掺杂复合粉体(La³⁺-Pr³⁺/TiO₂), 采用XRD、 UV-Vis和TEM等测试手段分析了在紫外光照射下, 以降解甲基橙为探针反应研究其可见光催化性能。结果显示: 所有样品均为锐钛矿相纳米TiO₂, 稀土元素镧和镨掺杂后TiO₂特征衍射峰宽化, 强度降低; 与纯TiO₂、 镧掺杂TiO₂与镨掺杂TiO₂相比, 光催化剂La³⁺-Pr³⁺共掺杂TiO₂颗粒的粒径更小, 比表面积更大, 光吸收边红移程度更显著; 与未掺杂和单一掺杂的TiO₂相比较, 共掺杂的TiO₂具有更高的可见光催化性能。当La³⁺与TiO₂和Pr³⁺与TiO₂的摩尔比分别为1.0%和0.2%时, 可见光催化性能最好。可见光催化性能的提高归因于镧和镨的协同作用。     

尖晶石相型LiM_(0.2)Mn_(1.8)O_4(M=Mg、Cd)相的晶格畸变与红外吸收峰频移

通过室温固相法制备了不同元素掺杂的前驱体,并采用分步煅烧法获得了尖晶石型LiMn2O4和LiM0.2Mn1.8O4(M=Mg、Cd)相。采用XRD和FTIR技术就元素掺杂对产物晶格畸变、Mn—O键长和键能强度等微观结构参数和光谱频移现象进行分析。结果表明,不同元素掺杂导致产物产生不同程度的晶格畸变。Mg元素掺杂使晶格收缩,Mn(Ⅳ)—O和Mn(Ⅲ)—O键收缩和键能强度增加,对应吸收峰发生蓝移;Cd元素掺杂使晶格膨胀,Mn(Ⅳ)—O和Mn(Ⅲ)—O键增长和键能强度降低,对应吸收峰发生红移。     

RF溅射稀土（La，Nd）掺杂ZnO薄膜的结构

通过射频磁控溅射技术在Si(111)衬底上制备了未掺杂和镧、钕掺杂ZnO薄膜.XRD分析表明,ZnO薄膜具有c轴择优生长,镧、钕掺杂ZnO薄膜为自由生长的纳米多晶薄膜.用AFM观测薄膜的表面形貌,镧、钕掺杂ZnO薄膜表面形貌粗糙.     

Microstructural characterization of donor-doped lead zirconate titanate films prepared by sol–gel processing

Lanthanum and niobium-doped lead zirconate titanate, Pb(Zr,Ti)O₃, (PZT) thin films were prepared on Pt/Ti/SiO₂/Si substrates by sol–gel processing. Films have a Zr/Ti ratio of 52:48 and tetragonal perovskite phase structure. The influence of donor dopants on the morphology, texture and defects of PZT films was studied using X-ray diffraction, X-ray photoelectron spectroscopy, atomic force microscopy, scanning electron microscopy, breakdown field strength and fatigue. Donor doping of PZT films results in increased breakdown field strength and improved fatigue properties. These originate from (i) the reduction of texture in the [111] and increase in the texture in [100]; (ii) lower porosity, smaller grain size and smoother surfaces; (iii) granular grain structure; and (iv) reduction in the oxygen vacancy concentration in the films.     

Ultrasonically assisted hydrothermal synthesis of polycrystalline PZT thin film on titanium substrate

Ultrasonically assisted hydrothermal synthesis of PZT thin films was performed using an ultrasonic transducer integrated into the lid of an autoclave. Direct ultrasonic irradiation of 23 W at 53 kHz was carried out during the hydrothermal synthesis at a reaction temperature of 140°C for 24 h. The resultant PZT thin film was characterized using scanning electron microscopy (SEM) and x-ray diffraction (XRD). The PZT thin film had fine nanoparticles of approximately 100 nm in diameter when the substrate was placed perpendicular to the plane of ultrasonic irradiation. The film exhibited predominantly (001) orientation when the substrate was placed parallel to the plane of ultrasonic irradiation.     

Electric and magnetic properties of Pb(Zr0.52Ti0.48)O3-CoFe2O4 particle composite thin film on the SrTiO3 substrate

We deposited a thin epitaxial Pb(Zr_0.52Ti_0.48)O₃ (PZT) layer on the (0 0 1) SrTiO₃ (STO) substrate doped with Nb (0.5 wt.%), then grew composite thin film of CoFe₂O₄ (CFO) and PZT phases on it. X-ray diffraction and high resolution transmission electron microscopy showed that the PZT and CFO phases in the film had perfect epitaxial structures. CFO nanoparticles were embedded in PZT matrix randomly, which was useful to enhance the insulativity of the composite film. The composite thin film exhibited good ferromagnetic and ferroelectric properties. The dielectric constants of the composite thin film kept unchangeable in a wide bias electric field, but increased in a magnetic field, namely, magnetodielectric effect. The possible reasons for the magnetodielectric effect were discussed.     

Effect of heat-treatment on LaNiO3 film electrode of PZT thin films derived by a sol–gel method

Lanthanum nickel oxide (LaNiO₃ or LNO) conducting thin films that could be used as electrodes for improving fatigue and aging properties of ferroelectric thin films were investigated. In this paper, LNO films were directly spin-coated onto SiO₂/Si(1 0 0) substrates followed by thermal treatment in air and in oxygen. It was found that crack-free dense and uniform films with good crystallinity and medium grains were obtained, preferentially (1 0 0)-oriented LNO thin films could be formed at a lower annealing temperature of 550 °C and that with the increase in thermal annealing temperature the LNO thin film possessed better electrical properties especially at 750 °C. However, the LNO film displayed a structure transformation above 850 °C. A phenomenon was found that the first heat-treatment temperature and time played a key role to determine the crystallite size of LNO films. A subsequent deposition of a sol–gel derived Pb(Zr_0.53Ti_0.47)O₃ (PZT53/47) thin film on the LNO-coated SiO₂/Si(1 0 0) substrates was also found to have a (1 0 0)-oriented texture. Moreover, the Au/PZT/LNO capacitor was found to significantly improve the fatigue and the effects of the LNO electrodes to the fatigue were discussed.     

Effect of heat-treatment on LaNiO3 film electrode of PZT thin films derived by a sol–gel method

Lanthanum nickel oxide (LaNiO₃ or LNO) conducting thin films that could be used as electrodes for improving fatigue and aging properties of ferroelectric thin films were investigated. In this paper, LNO films were directly spin-coated onto SiO₂/Si(1 0 0) substrates followed by thermal treatment in air and in oxygen. It was found that crack-free dense and uniform films with good crystallinity and medium grains were obtained, preferentially (1 0 0)-oriented LNO thin films could be formed at a lower annealing temperature of 550 °C and that with the increase in thermal annealing temperature the LNO thin film possessed better electrical properties especially at 750 °C. However, the LNO film displayed a structure transformation above 850 °C. A phenomenon was found that the first heat-treatment temperature and time played a key role to determine the crystallite size of LNO films. A subsequent deposition of a sol–gel derived Pb(Zr_0.53Ti_0.47)O₃ (PZT53/47) thin film on the LNO-coated SiO₂/Si(1 0 0) substrates was also found to have a (1 0 0)-oriented texture. Moreover, the Au/PZT/LNO capacitor was found to significantly improve the fatigue and the effects of the LNO electrodes to the fatigue were discussed.     

磁控溅射工艺参数对Pb(Zr,Ti)O3薄膜织构的影响

利用RF磁控溅射法制备了Pb(Zr,Ti)O3(PZT)铁电薄膜,利用X射线衍射(XRD)法研究了薄膜的相组成及溅射工艺参数对薄膜织构的影响.结果表明,在小靶基距时,过高溅射功率不利于获得纯钙钛矿相的PZT铁电薄膜.溅射功率及溅射气压影响PZT薄膜的织构及其织构散漫度,提高溅射气压及溅射功率,(111)织构漫散度随之提高.在靶基距为80mm时,选择150w、0.7Pa的溅射工艺可获得具有最佳(100)织构的PZT薄膜.     

Effects of frequencies of AC modulation voltage on piezoelectric-induced images using atomic force microscopy

Lead zirconate titanate (PZT) thin film is prepared by sol-gel method on Pt/Ti electrode/SiO₂/Si wafer. Local poling is performed on the PZT film using an atomic force microscope (AFM). The topography and piezoelectric-induced (PEI) images on the polarized PZT film are recorded using AFM at piezo-responsive mode, operated with an AC voltage at varying frequencies. The best PEI image was obtained at the frequency around 300 kHz. It is explained that the change of piezoelectric vibrations and input noise signals with the frequency of AC modulation voltage affects the intensity of PEI images.     

The thickness effect of Bi3.25La0.75Ti3O12 buffer layer in PbZr0.58Ti0.42O3/Bi3.25La0.75Ti3O12 (PZT/BLT) multilayered ferroelectric thin films

A series of PbZr_0.58Ti_0.42O₃ (PZT) thin films with various Bi_3.25La_0.75Ti₃O₁₂ (BLT) buffer layer thicknesses were deposited on Pt/TiO₂/SiO₂/p-Si(100) substrates by RF magnetron sputtering. The X-ray diffraction measurements of PZT film and PZT/BLT multilayered films illustrate that the pure PZT film shows (111) preferential orientation, and the PZT/BLT films show (110) preferential orientation with increasing thickness of the BLT layer. There are no obvious diffraction peaks for the BLT buffer layer in the multilayered films, for interaction effect between the bottom BLT and top PZT films during annealing at the same time. From the surface images of field-emission scanning electron microscope, there are the maximum number of largest-size grains in PZT/BLT(30 nm) film among all the samples. The growth direction and grain size have significant effects on ferroelectric properties of the multilayered films. The fatigue characteristics of PZT and PZT/BLT films suggest that 30-nm-thick BLT is just an effective buffer layer enough to alleviate the accumulation of oxygen vacancies near the PZT/BLT interface. The comparison of these results with that of PZT/Pt/TiO₂/SiO₂/p-Si(100) basic structured film suggests that the buffer layer with an appropriate thickness can improve the ferroelectric properties of multilayered films greatly.     

Effect of microwave annealing temperatures on lead zirconate titanate thin films

Lead zirconate titanate (Pb(1.1)(Zr(0.52)Ti(0.48))O(3)) thin films of thickness 260?nm on Pt/Ti/SiO(2)/Si substrates were densified by 2.45?GHz microwave annealing. The PZT thin films were annealed at various annealing temperatures from 400 to 700?°C for 30?min. X-ray diffraction showed that the pyrochlore phase was transformed to the perovskite phase at 450?°C and the film was fully crystallized. The secondary (again pyrochlore) phase was observed in the PZT thin films, which were annealed above 550?°C. The surface morphologies were changed above 550?°C of the PZT thin films due to the secondary phase. Higher dielectric constant (ε(r)) and lower dielectric loss coercive field (E(c)) were achieved for the 450?°C film than for the other annealed films.     

Lanthanum concentration dependence of electrical properties in tin oxide thin films

Lanthanum doped tin oxide thin films were prepared on boron-silicon glass substrates by spray pyrolysis. Lanthanum concentration was varied from 0 to 1.0 wt%. The microstructures, sheet resistance and thermal stabilities of the lanthanum doped tin oxide thin films have been investigated in order to determine the role of this dopant on electrical properties. X-ray diffraction (XRD) result shows the deposited thin film is mainly rutile SnO₂. And atomic force microscopy (AFM) reveals that the thin film has smooth surface with no cracks and defects. And it exhibits a typical bimodal grain size distribution with an average grain size of 95 nm. The sheet resistances of the thin films have a complex dependence on the lanthanum concentration. With increasing lanthanum concentration, the sheet resistances of tin oxide thin films were slightly increased and then abruptly decreased. Moreover, when the lanthanum concentration of 0.5 wt% was reached, the specimen exhibits excellent electrical properties. Because of its effectiveness in improving homogeneity of operating surface temperature and thermal stability, lanthanum appears to be an attractive additive for the tin oxide thin films.