凹凸棒土负载CeO2-La2O3复合材料制备表征及催化性能

以凹凸棒土(ATP)为载体, 以Ce(NO₃)₃·6H₂O和La(NO₃)₃·6H₂O为原料, 以C₆H₁₂N₄(HMT)为沉淀剂, 采用均相沉淀法制备了不同铈镧比的CeO₂-La₂O₃/ATP(Ce:La=9:1~3:7, 摩尔比, 下同)复合材料。用TG-DSC、 TEM、 XRD和FTIR对所制备复合材料的微观结构和形貌进行表征, 并分别考察不同铈镧比和H₂O₂添加量对酸性品红模拟废水脱色降解的影响。结果表明, 当Ce:La=5:5时, CeO₂-La₂O₃固溶体颗粒均匀分布在ATP表面, 颗粒尺寸为5~10 nm。随着铈镧摩尔比的增加, 酸性品红的降解率呈先增后减的趋势, 且当Ce:La=5:5、 H₂O₂为10 mL、 酸性品红浓度为100 mg/L时, 降解效果最好, 300 min后的最大降解率达82%。     

Gd3＋掺杂对Sr2FeMoO6结构及电磁性能的影响

采用微波固相烧结法合成了双钙钛矿Sr2-xGdxFeMoO6（x=0.0、0.1、0.2、0.3）。用XRD和VSM对样品的物相结构和电磁性能进行了研究。结果表明所得Sr2FeMoO6为四方晶系结构,空间群为I4/mmm,随Gd3＋掺杂量的增加,Fe、Mo排列的有序度逐渐降低,同时伴有少量Gd2O3杂相生成。样品Sr2-xGdxFeMoO6均表现为铁磁性,磁转变温度均高于室温,Gd3＋掺杂使得样品的室温饱和磁化强度降低,但适量Gd3＋的掺杂（x=0.3）可明显提高样品的室温磁电阻变化率。样品Sr2-xGdxFeMoO6均呈现典型的半导体行为,当x=0.0、0.1、0.2时,在100～300K,其电输运行为服从小极化子变程跃迁导电机制;当x=0.3时,在150～300K,服从小极化子变程跃迁导电机制;在100～150K,则属于绝热小极化子导电机制。     

荧光粉Sr3-x-yAl2O6∶xCe3+,yEu2+的制备及其发光特性

采用高温固相反应法制备了Sr3-x-yAl2O6:xCe3+,yEu2+(x=0,y=0;x=0.04,y=0;x=0.04,y=0.02;x=0.04,y=0.04;x=0.04,y=0.06;x=0.04,y=0.08;x=0,y=0.04)荧光粉,研究其相组成与荧光特性,结果表明,样品具有单相Sr3Al2O6晶体结构。在360nm波长的紫外光激发下,Ce3+离子辐射出峰值在434nm附近的宽谱蓝光。通过能量传递作用,Eu2+离子辐射峰值为517nm左右的宽谱绿光。Ce3+和Eu2+的荧光组合获得了色坐标为(0.2611,0.3313)的近白光发射。样品的激发光谱分布在250～400nm的波长范围,这种荧光粉有望在紫外或近紫外激发的白光LED中获得应用。     

水热合成纳米TiO2-Fe2O3复合材料及其光催化性能

以TiCl4,FeCl3·6H2O和NH3·H2O为原料,把TiCl4和FeCl3·6H2O按照化学计量比共同水解,得到的水合氧化物中间体放入高压釜中在180℃、0.8MPa下进行反应,经过滤、洗涤、烘干,得到纳米TiO2-Fe2O3复合材料.XRD分析证明产品为锐钛矿结构.TEM形貌观察,粒子基本为球形,粒径20～30nm;将样品均匀分散在甘油-水混合液中,利用UV-1200紫外-可见分光光度计测试了样品的光吸收性能,发现该纳米复合材料对紫外光和可见光均有很强的吸收.利用该纳米复合材料作为光催化剂对有机染料溶液进行了降解实验,发现在日光照射180min后,对酸性红B染料的降解率接近100%.     

Tb3+掺杂对Sr2CeO4∶Eu3+发光性能的影响

以尿素为燃料硼酸为助熔剂,采用燃烧法合成了Sr2CeO4∶Eu3+、Tb3+发光材料。测试结果表明,当Tb3+的掺杂为1%(摩尔分数)时,合成的样品为单相Sr2CeO4斜方晶系结构,其样品的激发光谱为240～370nm的宽带双峰,发射光谱为400～550nm宽带峰,余辉衰减曲线的结果显示,适量的掺杂Tb3+可以提高产品的发光性能。与Sr2CeO4∶Eu3+相比,掺杂Tb3+有利于形成结晶度好的固溶体,样品的发光强度明显提高。     

液相直接沉淀法制备Ag3VO4及其可见光催化性能研究

以NH4VO3和AgNO3为原料,采用液相直接沉淀法制备了Ag3VO4粉体,用XRD、SEM、BET和UV-Vis等手段对样品的物相、形貌、比表面积和光学特性进行了表征;以可见光为光源、罗丹明B为目标降解物考察了Ag3VO4的光催化活性。结果表明,反应混合物的pH值对样品的成分有重要的影响,在调节反应混合物的pH值为7时,所制备的样品为单斜相的Ag3VO4;反应时间、反应温度和表面活性剂等对Ag3VO4的尺寸和形貌有较大的影响。UV-Vis分析表明,所得样品在400～680nm有强而宽的吸收,其能带间隙Eg为1.90eV;光催化性能测试表明,样品的可见光光催化活性较高,在35W氙灯照射下,经100min降解,80℃反应8h所得样品对罗丹明B的降解率可达97.7%。     

化合物Sr1.98Nd0.02FeMoO6和Sr1.96Nd0.04FeMoO6的制备及磁学表征

采用溶胶-凝胶法制备了双钙钛矿氧化物Sr1.98Nd0.02FeMoO6和Sr1.96Nd0.04FeMoO6样品。X射线粉末衍射结果表明样品均为纯相,室温下空间群为I4/m,样品有序度随掺杂量的增加而降低。采用多功能振动样品磁强计表征了样品的磁滞曲线和磁热曲线,结果表明样品均具有铁磁性质。H/M-M2曲线表明两个样品均为二级磁相变。Nd掺杂导致样品的居里温度与磁矩降低。不同外磁场下的M-T曲线测量结果表明随着外部磁场的增加样品最大磁矩冻结,阻塞温度降低。     

(Ca,Sr,Ba)3V2O8的制备和发光性能研究

采用微波辅助溶胶-凝胶法制备了自激发钒酸盐A3(VO4)2(A:Ca,Sr,Ba)。采用X射线衍射仪、傅里叶变换红外光谱仪、扫描电镜、透射电子显微镜、荧光谱仪对样品各项参数进行了表征,研究了A3(VO4)2的光致发光特性,探讨了不同制备工艺条件对其发光性质的影响。实验结果表明,Sr3V2O8样品发光强度随退火温度而变化,在680～900℃时,其发射光谱强度随温度上升而单调下降,达到1000℃时开始上升;pH值为4时,样品的发射光谱强度最大。     

发光二极管用荧光材料Sr2CeO4:Sm3+的合成及其发光特性

以具有一维结构的Sr2CeO4化合物为研究对象、Sm3 作为发光中心,探索了其作为LED用荧光材料的可能性.用高温固相法于1200℃、6h合成了Sr2CeO4:Sm3 系列单相粉末样品,并研究了其发光性质.结果表明,在365nm激发下,从荧光光谱中可以看出存在从基质向稀土离子的能量转移.通过调节荧光材料Sr2CeO4:Sm3 中稀土离子Sm3 的掺杂浓度,可以调谐发光体的发光颜色,当Sm3 离子浓度较小(<3%)时,体系发出很强的白光;当Sm3 离子浓度较大(3%～15%)时,体系发出红光.测量了荧光材料的色坐标,发现Sr2CeO4:1%Sm3 的色坐标是(0.334,0.320),接近于纯白色(0.33,0.33),可以作为一种新型的UV-LED用单一白色荧光材料.     

微波辅助熔盐法制备SrFe12O19及其磁性能的研究

以钢厂副产的氧化铁红作为含铁原料,采用微波辅助熔盐法制备了SrFe₁₂O₁₉铁氧体,研究了Fe/Sr摩尔比和微波煅烧温度对样品的物相组成、微观结构及磁性能的影响。采用FullProf软件对样品的XRD数据进行了精修拟合分析,利用扫描电子显微镜(SEM)观察了样品的形貌,用振动样品磁强计(VSM)对样品的磁性能进行了表征。结果表明,Fe/Sr摩尔比对样品的物相组成及样品的晶胞参数有重要影响,当Fe/Sr摩尔比为10.5时,样品获得了较好的磁性能。随着煅烧温度的增加,SrM相的厚度也随着增加,在1373.15 K下微波煅烧2 h, SrM相的厚度最大,此时样品矫顽力最大达到2.69×10⁵ A/m,饱和磁化强度为63.04 A·m²/kg,而在1273.15 K制备的样品最大磁能积最大为9.47×10³ J/m³。     

溶胶-凝胶法制备超细Sr_2FeMoO_6及磁性能研究

以活性炭为还原剂,采用溶胶-凝胶法制备双钙钛矿结构巨磁电阻材料Sr_2FeMoO_6.经XRD物相分析证明,产品为四方晶系Sr_2FeMoO_6,空间群为I4/mmm,晶胞参数:a=0.558nm,c=0.7882nm.SEM形貌分析表明,粉体颗粒分散性较好,粒子基本为球形,尺寸在100nm以下.磁性能测试结果表明,样品的居里温度高于室温,1T磁场下室温饱和磁化强度为13.59A·m~2·kg~(-1).     

煅烧温度对红色长余辉发光材料Sr_3Al_2O_6:Eu~(2+),Dy~(3+)性能的影响

采用溶胶凝胶法合成了Sr3Al2O6:Eu2+,Dy3+长余辉发光材料,利用X射线衍射仪(XRD)对材料的物相进行了分析,采用荧光分光光度计、照度计测定了样品的发光特性。XRD结果表明:随着煅烧温度的升高,SrCO3杂相的衍射峰越来越弱,Sr3Al2O6相的衍射峰越来越强,1200℃时发光基质为纯的Sr3Al2O6相,1250℃时出现新的SrAl2O4杂相。激发光谱和发射光谱结果表明:长余辉发光材料的激发峰位于473nm,发射峰位于612nm,归属于Eu2+的4f65d1→4f7特征发光。温度升至1250℃时,Eu2+的发射峰为612nm和520nm,后者归属于Eu2+在发光基质SrAl2O4中的发光。综合分析得制备Sr3Al2O6:Eu2+,Dy3+发光材料合适的煅烧温度为1200℃,在此温度下,材料具有较好的初始亮度和余辉时间。     

稀土掺杂双钙钛矿结构红色荧光粉的制备及其发光性能

采用高温固相反应法制备了Sr_(2-x)BaxMgMoO_6∶Eu~(3+)(x=0~1)双钙钛矿结构红色荧光粉。探讨了预处理及煅烧制度、Ba取代量对Sr_(2-x)BaxMgMoO_6∶Eu~(3+)荧光粉的相结构和发光性能的影响。Sr_2Mg_(0.94)Eu_(0.06)MoO_6荧光粉最佳制备工艺为:在700℃下预处理1h再升温至1050℃预处理1h并随炉降温后研细,再在1300℃煅烧4h,所得样品主相为双钙钛矿结构的Sr2MgMoO6四方相。其最强发光峰位于617nm附近,对应于Eu3+的5D0→7F2电偶极跃迁。随着Ba2+对Sr2+的取代量的增加晶体对称性提高,晶体结构由四方相变为立方相,样品的激发峰强度显著提高。由于晶体对称性的提高,抑制了荧光粉在617nm处5D0→7F2红光发射,其发光由电偶极跃迁占主导转变为磁偶极跃迁占主导。     

Bulrush-like double perovskite: synthesis, tunneling magnetoresistance, and magnetocaloric effects

The recent observation of room temperature tunneling magnetoresistance (TMR) in half-metallic A2FeMoO6 (A = Ca, Sr, Ba) double perovskites, and their importance to the emerging field of spintronics has led to considerable effort being dedicated to detailed investigations of the physical and chemical properties of these materials. This article will present an review of our recent investigations covering the synthesis, structures, magnetic and transport properties of "bulrush-like" A2FeMoO6 (A = Sr, Ba). Utilizing the high shape anisotropy as well as the reactivity of A2FeMoO6 to water and a sonochemical technique, we managed to manipulate the properties of grain boundary barriers, and thus put forward a new approach for the enhancement of room temperature TMR. The magnetocaloric effects of A2FeMoO6 double perovskites will also be discussed.     

钴掺杂Sr_4Fe_6O_(13)混合导体氧化物结构及透氧测定

用湿化学法合成了Ｓｒ４ＣｏｘＦｅ６－ｘＯ１３±δ系列混合导体氧化物,对其相结构与透氧性能进行了研究．钴离子的引入导致材料中钙钛矿型杂相的出现,Ｘ＝２．０时材料中还产生了ＣｏＯ杂相,ｘ＝２．６时材料呈现钙钛矿型结构．Ｓｒ４Ｆｅ４Ｃｏ２Ｏ１３±δ的相结构还与焙烧温度及环境气氛中的氧浓度密切相关．随着氧浓度的降低,材料从纯相Ｓｒ４Ｆｅ６Ｏ１３结构（纯氧气气氛下）转变为Ｓｒ４Ｆｅ６Ｏ１３结构、钙钛矿型结构和ＣｏＯ共存（空气气氛下）,直至转变为针镍矿结构、 Ｓｒ４Ｆｅ６Ｏ１３结构和 ＣｏＯ共存． Ｓｒ４Ｆｅ６Ｃｏ１３±δ导体膜在ａｉｒ／Ｈｅ氧浓差梯度下的透氧量为 １．５×１０８ｍｏｌ／ｃｍ２·ｓ（８５０℃）,在６５０～８５０℃范围内透氧活化能为７０ｋＪ／ｍｏｌ．     

Visible Light Induced Photocatalysis of Cerium Ion Modified Titania Sol and Nanocrystallites

The cerium ion(Ce4+) doped titania sol and nanocrystallites were prepared by chemical coprecipitation-peptization and hydrothermal synthesis methods, respectively. The X-ray diffraction pattern shows that Ce4+-TiO2 xerogel powder has semicrystalline structure and thermal sintering sample has crystalline structure. Ce4+-TiO2 nanocrystallites are composed of the major anatase phase titania (88.82 wt pct) and a small amount of crystalline cerium titanate. AFM micrograph shows that primary particle size of well-dispersed ultrafine sol particles is below 15 nm in diameter. The particle sizes are 30 nm for xerogel sample and 70 nm for nanocrystallites sample, which is different from the estimated values (2.41 nm and 4.53 nm) by XRD Scherrer's formula. The difference is mainly due to aggregation of nanocrystallites. The experimental results exhibit that photocatalysts of Ce4+-TiO2 sol and nanocrystallites have the ability to photodegrade reactive brilliant red dye (X-3B ) under visible light irradiation with t     

Sintering Behavior and Microwave Dielectric Properties of MgTiO3 Ceramics Doped with B2O3 by Sol-Gel Method

The B2O3-doped MgTiO3 powders and ceramics have been prepared by sol-gel method using Mg(NO3)2·6H2O, Ti(C4H9O)4 and H3BO3 as the starting materials. The sintering behavior and microwave dielectric properties of ceramics prepared from powders with different particle sizes were investigated. The gels were calcined at 650, 700, 750, 800, 850 and 900 C and the derived particle sizes of powders were 20-30 nm, 30-40 nm, 40-60 nm, 60-90 nm, 90-120 nm and 120-150 nm, respectively. The nanoparticles with the size of 30-60 nm benefited the sintering process with high surface energy whereas nanoparticles with the size of 20-30 nm damaged the microwave dielectric properties due to the pores in the ceramics. The addition of B2O3 used as a liquid sintering aid reduced the sintering temperature of MgTiO3 ceramic, which was supposed to enter the MgTiO3 lattice and resulted in the formation of (MgTi)2(BO3)O phase. The B2O3-doped MgTiO3 ceramic sintered at 1100 C and prepared from the nanoparticles of 40-60 nm had compact structure and exhibited good microwave dielectric properties: εr=17.63, Q × f=33,768 GHz and τ f= 48×10 6 C 1.     

微波固相法制备纳米镧锶镍复合氧化物

以硝酸镧、乙酸锶和乙酸镍为原料,应用微波固相法制备了纳米镧锶镍复合氧化物前驱体。研究表明：控制热分解温度是制备超微纳米粒子的关键。最小粒径产物的制备条件是：微波炉加热功率600W,马弗炉热分解温度600℃,热分解时间5h。XRD和TEM分析结果表明,产物主要物相组成为La0.9Sr0.1NiO3,属钙钛矿相斜方六面体结构,空间群R-3c,平均粒径10～25nm。应用DSC—TG技术对纳米镧锶镍复合氧化物前驱物热分解机理进行了初步探索,得两阶段分解机理函数为G（a）=[-ln（ 1-α ） ]^7/12,G（a）=-ln（ 1-α ） ]^4/9。 ：微波固相法;纳米镧锶镍复合氧化物;热分解机理     

Instability of Structural, Magnetic, and Magnetoresistive Properties in Ordered Double-perovskite Sr_2FeMoO_6 Polycrystals

The problem of instability in polycrystalline ordered double-perovskite Sr2FeMoO6, is presented in this paper. By the X-raydiffraction analysis and the measuring of electrical and magnetic transports, it is indicated that the perovskite structure of thecompound is destroyed, and the Sr2FeMoO6 phase is mainly transformed into SrMo04 phase when the samples are exposedin damp atmosphere for several weeks or immersed in water for several hours. Simultaneously, their electrical and magneticproperties obviously change, and the value of magnetoresistance remarkably reduces and even vanishes at room temperature.A possible micromechanism of the instability and an effective method to avoid the problem of instability are also discussed.     

The influence of composition on optical properties of ferroelectric potassium lithium niobate single crystals

Homogeneous crack-free Potassium Lithium Niobate (KLN) single crystals with different Li content were grown up by the TSSG technique. Lattice vibration spectra of these samples were investigated using Raman spectroscopy. The results showed that characteristic Raman spectra of the [NbO₆]⁷⁻ octahedral ions were strikingly influenced by the Li ions. Thus, the symmetric bend vibration mode ν₅ of the KLN sample with higher Li content was split into three Raman peaks, while the sample with lower Li content displayed a single peak, supporting that the bend vibration modes of the [NbO₆]⁷⁻ octahedrons were obviously perturbed by Li ions occupying C-sites. Enhanced Raman peak intensities of the KLN sample post-annealed at 900 °C for 24 h evidenced that content of defects in KLN crystal might be reduced. The transmittance spectra showed that the crystal with higher Li content had better transmittance intensity.