Nd：YAG粉体的分散性研究

钇铝石榴石(YAG)单晶因其优良的光学性能和稳定的化学性能被广泛用作激光和其它发光基础材料.掺Nd的YAG透明陶瓷激光材料的研究,是十几年来在激光工作物质制备技术领域最为重要的创新.与单晶相比,陶瓷具有容易制造、成本低、尺寸大和掺杂浓度高、可大批量生产等优点,最重要的是陶瓷可以达到与单晶一样的光学和机械性能,然而合成化学纯度高、分散性能好、无团聚、粒度均匀的纳米原料粉体是制备透明YAG陶瓷的关键.Nd: YAG陶瓷粉体制备可采用固相法[1]、溶胶-凝胶法[2]、喷雾热解法[3、4]、共沉淀法[5]、机械化学法[6]等多种合成方法.这些方法中各有优缺点,共沉淀法是一种方法简单,易于控制,成本低廉的一个体系,郭旺[7]、王宏志[8]等所在的研究组对YAG的纯相、前驱体的组成、控制溶液的浓度和沉淀剂的pH值也进行了分析,在这些研究中,虽然都能形成较纯的YAG相,但其颗粒间也有较多的团聚,所以本文着重研究了不同分散剂对YAG粉体分散性的影响.采用共沉淀法合成粉体,在合成粉体时加入不同的分散剂,研究获得分散、无团聚的粉体.     

溶胶-凝胶法制备钛酸钡超细粉体的研究

钛酸钡是一种非常重要的铁电材料 ,其合成方法主要分为固相反应法和液相反应法。传统的固相反应法是以ＴｉＯ2 和ＢａＣＯ3 经高温反应制取钛酸钡粉体 ,该法产品杂质含量高 ,颗粒粗 ,均匀性差 ,粉体烧结温度高。与高温固相反应相比 ,液相法合成的钛酸钡粉体具有化学纯度高 ,颗粒细小 ,粒度分布均匀等优点。特别是以醇盐为原料 ,采用溶胶 凝胶法制备的钛酸钡粉体 ,其性能非常优异 ,已为许多研究者所关注[1,2 ] 。文献[3 ] 报道了以异丙醇钛和醋酸钡为原料 ,采用溶胶 凝胶法制备钛酸钡物体的研究 ,但未见有以钛酸丁酯及醋酸钡为原料制备钛酸钡…     

溶胶-凝胶法合成Li_4SiO_4

Li4SiO4具有有利于离子传导的结构,为锂离子导体理想的基质材料[1].在硅酸盐体系中,硅的聚合态很复杂,难以得到纯相,鉴于固相法操作简单,在已有的文献中,合成方法多为固相法,但固相法不易保证成份的准确性、均匀性且合成温度较高.溶胶-凝胶法是近几年来发展起来的湿化学合成方法,用此法合成离子导体具有纯度高、均匀性好、颗粒小、反应过程易于控制等优点[2],而通常的溶胶-凝胶法是用金属醇盐与有机盐为前驱物,这样成本较高,且易造成污染.本文用金属醇盐及无机盐为前驱物,用溶胶-凝胶法合成了Li4SiO4纯相,并同一般固相法相比较,对合成的…     

质子导体SrCe0.9Y0.1O3-α的柠檬酸法合成研究

采用柠檬酸液相法合成了钙钛矿相SrCe0.9 Y0.1 O-α跃粉体，将所制粉体模压成型后在1450℃烧结10h得到陶瓷膜片。对粉体合成的热处理过程进行了DSC／TG，XRD研究，通过SEM观察了粉体及膜片的微观结构。结果表明，用柠檬酸液相法制备的螫合前驱体在热处理形成srCe0.9 Y0.1 O3-α的过程中，先出现了YxCe1-x O2-x／2复合氧化物、SrCO3及反尖晶石结构的Sr2CeO4相，在1100℃可以完令转变为SrCe0.9 Y0.1 O3-α钙钛矿相；这种方法比传统固相法的合成法温度低，粉体一次粒子粒径小于1μm，分散性差，但烧结性能良好。     

锆钛酸镧铅结构象和缺陷

锆钛酸镧铅(简称 PLZT)是一种十分重要的铁电材料.利用 PLZT 透明陶瓷的场致相变,还有可能在图象存贮和显示中得到应用.目前,在利用 La/Zr/Ti 比为7.9/70/30或8/65/35的 PLZT 透明陶瓷制作平面显示器、散射光开关和电光图象存贮器等方面开展了不少工作.PLZT 透明陶瓷的基本组成是锆钛酸铅掺 La 改性,形成(Pb,La)(Zr,Tj)O_3四元系固溶体.化学式倾向于:Pb_(1-x),La_x(Zr_(1-y),Ti_y)_(1-x/4)O_3.其中,La 的浓度 x 可在2～30％之间改变,而 Zr 与 Ti 的相互比例可连续变化.为了提高 PLZT 性能,人们往往通过改变这一比例加以实现.然而,我们的计算结果指出,这一比例的改变将使晶格能发生变化.我们用高分辨电子显微镜在晶格水平上对配比为8/65/35和7.9/70/30的 PLZT 进行了观察,发现配方7.9/70/30有更多的缺陷.计算表明,这可能是由于7.9/70/30的晶格能比8/65/35相对较低造成的.     

不同干燥过程对超细TiO2粉体性质的影响

考察了采用不同干燥工艺制备的TiO2粉体在粒子形貌、颗粒大小与分布、晶相组成以及比表面积和孔结构等织构和结构性质方面的差异。结果表明，利用常规的干燥方法，由水凝胶脱水所得的颗粒，颗粒间严重团聚，颗粒粒径大且分布不均匀，比表面积和孔体积最小；由醇凝胶直接脱水，则可以显著提高粉体的织构性能．而采用超临界流体干燥法则可以进一步提高粉体的性能，比表面积由水凝胶的4．88m2·g－1增大到113．8m2·g－1，提高了近30倍；孔体积由0．027cm3·g－1增大到0．41cm3·g-1．大约提高了15倍；而且其能够有效地防止粒子间的团聚，较好地保持了湿凝胶的网络结构，使颗粒尺寸降低且分布均匀，可重复性好．     

La0.75Sr0.25Cr0.5Mn0.5O3的制备及其NO2气敏性能

利用高温固相反应法和溶胶-凝胶法制备了La0.75Sr0.25Cr0.5Mn0.5O3钙钛矿复合氧化物粉体。采用XRD,TEM对粉体物相组成及颗粒形貌进行表征,并以制备的两种粉体作为敏感材料分别制成管状传感器,测试了其NO2气敏性能。结果表明：采用高温固相反应法和溶胶-凝胶法在不同焙烧温度下,均可制得单相La0.75Sr0.25Cr0.5Mn0.5O3粉体,采用溶胶-凝胶法在800℃焙烧2 h得到的粉体粒径约为20 nm;传感器输出电动势信号对NO2浓度之间呈良好的线性关系;溶胶-凝胶法制得粉体的气敏性能优于高温固相反应法制得粉体的气敏性能。     

反相微乳液法合成纳米钛酸钡球形颗粒

0引言BaTiO3陶瓷是一种具有高介电常数及优良的铁电、压电和绝缘性能的电子陶瓷材料。不仅是重要的电子陶瓷、PTC陶瓷原料[1],而且也是制备多层陶瓷电容器(M LC C)的必要组分[2,3]。随着现代科学技术的发展,人们更注重材料颗粒的大小和形貌,当材料的粒径达到纳米级时,材料的性能将发生很大的变化。另外,这种具有纳米尺度、球形颗粒的电子陶瓷材料,可能还具有一些新的物理作用,具有潜在的应用价值。B aTiO3粉体的制备方法有:固相煅烧法、化学共沉淀法、溶胶-凝胶法、水热法[4￣11]等。固相法反应温度高(一般1000￣1200℃)、反应活性差…     

微波合成对SrAl2O4:Eu2+, Dy3+晶相和铕的价态的影响

为了在较低温度下合成性能优良的SrAl2O4：Eu^2＋,Dy^3＋（SAO—ED）发光材料,采用溶胶-凝胶-微波法在900℃烧结30min合成SAO—ED发光材料。产品的发光性能优于传统高温固相法1400℃烧结3h制备的产品。根据Henderson和Taylor提出的公式对SrAl2O4的XRD数据进行了量化,计算出单斜晶系（M）和六方晶系的比例;结果表明,溶胶-凝胶-微波法制备的产品中只有单斜晶系存在,而高温固相法制备的产品中有六方晶系存在,六方晶系不发光。另外,产品采用XANES表征了Eu离子存在的价态,发现溶胶一凝胶微波法制备的产品中残留的Eu^3＋的比例远低于传统高温固相法制备的产品。以上两种原因导致了产品的发光性能优于高温固相法制备的产品。     

高效长余辉发光薄膜及粉体的溶胶—凝胶工艺研究

研究了溶胶－凝胶工艺制备SrAl2O4:Eu^2 ,Dy^3 高效长余辉发光薄膜及粉体的工艺条件,以无机盐为原料,成功制备了均一、稳定、透明的SrAl2O4溶胶,并在较低温度下制备了均匀、无裂纹的发光薄膜和颗粒均匀的针状纳米发光粉体。通过热失重和X射线衍射结果分析了样品的结晶过程和晶相组成,并通过扫描电镜、透射电镜和荧光光谱的分析对薄膜和粉体的微结构、表面形态及发光性能进行了表征。结果表明,在本文的工艺条件下,制备的薄膜和粉体的发光特性与传统的高温固相烧结法相似,但烧结温度可降低300℃左右。     

Hydrothermal Synthesis of Pb_(1-1.5x)La_xZr_(0.5)Ti_(0.5)O_3 (x = 0.01-0.06) Nanocrystallites

Lanthanum doped lead zirconate titanate (PLZT) ceramics display excellent electrooptic and photostriction properties because of the existence of cavities in the perovskite structure1-3. The PLZT powders are conventionally prepared by solid state reaction4-5, and the wet chemical methods such as sol-gel techniques are then introduced6-7. However, the homogeneity, morphology and size of the particles, which greatly affect the sinterability and the property of the resulting ceramics, are dif…     

Ce0.35Zr0.55La0.10O1.95对低贵金属Pt-Rh型三效催化剂性能的影响

采用共沉淀技术制备了Ce0.35Zr0.55La0.10O1.95固溶体, 其织构和结构性能以及氧化还原性能分别采用BET、XRD和程序升温(TP)技术进行了表征. 制备了低贵金属Pt-Rh型三效催化剂, 考察了Ce0.35Zr0.55La0.10O1.95对催化剂性能的影响. XRD和BET的结果表明, 经600 ℃焙烧5 h后, Ce0.35Zr0.55La0.10O1.95具有与Ce0.50Zr0.50O2相似的立方结构和高的比表面积；经1000 ℃焙烧5 h后, 仍能保持稳定的立方结构和47.25 m2•g−1的比表面积, 表现出优越的织构性能和高的热稳定性. H2-TPR和O2-TPO的结果表明, Ce0.35Zr0.55La0.10O1.95具有比Ce0.50Zr0.50O2更好的氧化还原性能. 和含Ce0.50Zr0.50O2的催化剂相比, 含Ce0.35Zr0.55La0.10O1.95的催化剂具有较宽的工作窗口, 优越的低温起燃性能, 较强的水气变换能力；催化剂经1000 ℃高温水热老化5 h后, 仍具有良好的催化活性, 表现出了优异的抗老化性能.     

Dependence of dielectric and photovoltaic properties of Pt/PLZT/LNO on the temperature and La doping content

Journal of Sol-Gel Science and Technology - In this study, Pb1?xLax(Zr0.52Ti0.48)O3/LaNiO3 (PLZT/LNO) heterostructures with different doping contents of La (x?=?0.02–0.15)...     

γ-苄基膦酸-磷酸锆的合成、表征及插层性能研究

于220℃水热晶化下制备了高结晶度的γ-ZrP,合成了3种γ-苄基膦酸-磷酸锆层状化合物Zr(PO₄).(H₂PO₄)_0.15(C₆H₅CH₂PO₃H)_0.85·0.4H₂O(1,d=1.86nm),Zr(PO₄)(H₂PO₄)_0.30(C₆H₅CH₂PO₃H)_0.70·0.6H₂O(2,d=1.78nm)和Zr(PO₄)(H₂PO₄)_0.50(C₆H₅CH₂PO₃H)_0.50·0.7H₂O(3,d=1.66nm).用X射线粉末衍射和³¹P固态核磁共振等手段表征其结构,并研究了其与α-苯乙胺的插层性能.     

Role of B-site ion on proton conduction in acceptor-doped Sm2B2O(7-δ) (B = Ti, Sn, Zr and Ce) pyrochlores and C-type compounds

Proton conduction in three pyrochlores, Sm(1.92)Ca(0.08)B(2)O(7-δ), B = Ti, Sn, Zr and one phase with a related C-type fluorite superstructure, B = Ce, has been investigated. The samples were prepared by solid state reaction. Infrared spectroscopy measurements and thermogravimetric analysis were carried out to study the extent of proton dissolution and determine its dependence on the B-site ion. Electrochemical impedance spectroscopy, performed on heating and cooling pre-hydrated samples, confirmed significant levels of proton conduction for Sm(1.92)Ca(0.08)Ti(2)O(7-δ) and Sm(1.92)Ca(0.08)Sn(2)O(7-δ) up to T～ 500 °C. In comparison the B = Zr and Ce samples revealed lower levels of proton conductivity, confined to temperatures below ～ 400 °C. Proton diffusion coefficients of 3.36 × 10(-8), 1.73 × 10(-9), 5.53 × 10(-10) and 2.78 × 10(-11) cm(2) s(-1) were determined at 300 °C for samples with B = Ti, Sn, Zr and Ce respectively. The proton mobility of Sm(1.92)Ca(0.08)Ti(2)O(7-δ) is therefore approximately one order of magnitude lower than that found in yttrium-doped perovskite phases such as BaZrO(3) and BaCeO(3).     

Sol-Gel Processing of Transparent PLZT((Pb,La)(Zr,Ti)O3) Fibers

PLZT((Pb,La)(Zr,Ti)O₃) ceramic fibers were prepared by the sol-gel method from a solution of lead acetate trihydrate, lanthanum isopropoxide, zirconium n-propoxide and titanium isopropoxide containing 2-methoxyethanol as the solvent. The as-drawn gel fibers were pretreated in an autoclave and preheated in flowing H₂O vapor prior to the heat-treatment for crystallization. The effects of autoclaving and preheating in flowing H₂O vapor on the structure and composition of the resultant fibers were investigated. Optically transparent single phase perovskite PLZT fibers of 5–15 m in thickness and 5 cm in length were successfully prepared when the autoclave-treatment and the preheating in flowing H₂O vapor were conducted prior to crystallization. These treatments are thought to promote hydrolysis of the organic groups and polycondensation reaction in the gel fibers, leading to the successful formation of dense, crack-free transparent PLZT fibers.     

可见光下Fe3+掺杂对K2La2Ti3O10分解水制氢性能的影响

采用溶胶-凝胶法制备了Fe3+掺杂的Fe-K2La2Ti3O10光催化剂, 并通过X射线衍射(XRD)、紫外-可见漫反射(DRS)、X射线光电子能谱(XPS)等技术对其进行了表征和分析, 考察了不同掺杂量对K2La2Ti3O10的性质及光催化分解水制氢活性的影响. 结果表明, Fe-K2La2Ti3O10在400-650 nm范围内显示强吸收, 光谱响应扩展到可见光区(λ>400 nm), 掺杂Fe3+后, K2La2Ti3O10的可见光区的光催化制氢活性显著提高, 掺杂量为nFe/nTi=0.04时活性最佳, 当催化剂用量为0.1 g, 反应液为CH3OH(30 mL)+H2O(90 mL)时, 产氢量达到1.92 μmol·h-1, 为未掺杂时的4倍.     

2D-3D transformation of layered perovskites through metathesis: synthesis of new quadruple perovskites A2La2CuTi3O12 (A = Sr, Ca)

We describe the synthesis of two new quadruple perovskites, Sr(2)La(2)CuTi(3)O(12) (I) and Ca(2)La(2)CuTi(3)O(12) (II), by solid-state metathesis reaction between K(2)La(2)Ti(3)O(10) and A(2)CuO(2)Cl(2) (A = Sr, Ca). I is formed at 920 degrees C/12 h, and II, at 750 degrees C/24 h. Both the oxides crystallize in a tetragonal (P4/mmm) quadruple perovskite structure (a = 3.9098(2) and c = 15.794(1) A for I; a = 3.8729(5) and c = 15.689(2) A for II). We have determined the structures of I and II by Rietveld refinement of powder XRD data. The structure consists of perovskite-like octahedral CuO(4/2)O(2/2) sheets alternating with triple octahedral Ti(3)O(18/2) sheets along the c-direction. The refinement shows La/A disorder but no Cu/Ti disorder in the structure. The new cuprates show low magnetization (0.0065 micro(B) for I and 0.0033 micro(B) for II) suggesting that the Cu(II) spins are in an antiferromagnetically ordered state. Both I and II transform at high temperatures to 3D perovskites where La/Sr and Cu/Ti are disordered, suggesting that I and II are metastable phases having been formed in the low-temperature metathesis reaction. Interestingly, the reaction between K(2)La(2)Ti(3)O(10) and Ca(2)CuO(2)Cl(2) follows a different route at 650 degrees C, K(2)La(2)Ti(3)O(10) + Ca(2)CuO(2)Cl(2) --> CaLa(2)Ti(3)O(10) + CaCuO(2) + 2KCl, revealing multiple reaction pathways for metathesis reactions.     

Formation and structure of titanium alkyl phosphates

Titanium alkyl phosphates (TiAP) synthesized by the reactions of Ti(SO(4))(2) with monohexyl, monooctyl, and monodecyl phosphates in aqueous media were characterized by various means. The XRD patterns of TiAP showed a strong diffraction peak and two weak ones below 2theta=15 degrees. The TiAP particle prepared using octyl phosphate gave rise to the lattice patterns having uniform alternating spacings of ca. 0.7 and ca. 2.0 nm. When treated at 900 degrees C, TiAP crystallized as TiP(2)O(7). The chemical formula could be shown as (ROPO(3))(2)Ti.0.44H(2)O. These facts suggest that the TiAP is composed of a multilayer alternating bimolecular layer of alkyl phosphates and hydrated titanium phosphate phase. Alkyl groups in the layers were removed by outgassing above 300 degrees C to give the materials having mesopores with a diameter of ca. 2 nm.     

Photocatalytic hydrogen production from water over M-doped La2Ti2O7 (M = Cr, Fe) under visible light irradiation (lambda > 420 nm)

In the search for efficient photocatalysts working under visible light, we have investigated the effect of cation substitution on a layered perovskite, La2Ti2O7. Among various metal dopants, only Cr and Fe induced intense absorption of visible light (lambda > 400 nm), and only these catalysts produced H2 photocatalytically from water in the presence of methanol under visible light irradiation (lambda > 420 nm). The polymerized complex method was found to be more efficient for fabrication of the present catalysts producing a more homogeneous structure than the solid-state reaction. The characterization by XRD, UV-vis DRS, XPS, and XANES revealed that doped Cr and Fe were present in the Cr3+ and Fe3+ states substituting for Ti sites in the La2Ti2O7 lattice. The theoretical calculation indicated that the most significant feature in the electronic band structure of the metal-doped La2Ti2O7 was the formation of a partially filled 3d band in the band gap of La2Ti2O7, while the contribution of these dopants on the valence band was negligible. Excitation of electrons from this localized interband to the conduction band of La2Ti2O7 was responsible for visible light absorption and the H2 evolution from water under visible light.