系列层状K2La2Ti3O10的制备及光催化性能

通过固相反应法合成了一系列不同尺寸的K2La2Ti3O10,考察了原料TiO2粒径对固相反应速率及产物尺寸、形貌的影响,得到了不同粒径下原料的最佳配比;以降解甲基橙为探针考察其光催化性能.结果表明:减小原料粒径,反应温度降低、速率加快;有利于合成小尺寸、大比表面积(可达11.83 m2·g-1)的层状K2La2Ti3O10,而且光催化性能提高.     

高分子凝胶法制备纳米ZnO/La2O3及光催化性能

以Zn(CH3COO)2·2H2O,AgNO3为原料,丙烯酰胺为单体,N,N'-亚甲基双丙烯酰胺为网络剂,采用高分子凝胶法在550℃下制得纳米ZnO/La2O3.通过XRD物相分析,得知沉积稀土氧化物La2O3的ZnO纳米粒子样品的物相均是六方晶系纤锌矿结构;TEM形貌观察,粒子基本为球形,纳米ZnO/La2O3的平均粒径约为26 nm,红外光谱分析高分子的分解程度,在550℃时分解完全.水溶液中次甲基蓝染料在ZnO/La2O3半导体光催化条件下,pH值为9时,能迅速分解,在降解90 min时,次甲基蓝的降解率达到81%.     

固相法制备MgO-La2O3纳米晶及表征

以硝酸镧、醋酸镁和酒石酸铵为原料,固相反应法合成白色糊状物,糊状物经400℃时燃烧得到灰白色蓬松絮状多孔性前驱物,前驱物在不同温度下煅烧制备了不同粒径的MgO-La2O3纳米晶,考察研究了煅烧温度和酒石酸铵的用量对MgO-La2O3复合纳米晶的影响,探讨了酒石酸铵的作用.通过XRD、TEM、SEM等手段对纳米晶结构、尺寸形貌进行了表征,样品为立方晶系和六方晶系混合的MgO-La2O3复合纳米晶.     

直接融盐法制备锂离子电池负极材料Li4/3Ti5/3O4及其电化学性能

以CH3COOLi·2H2O和锐钛矿型TiO2为原料,通过直接融盐法合成锂离子电池负极材料Li4/3Ti5/3O4,考察合成条件对材料性能的影响,并通过X射线衍射仪(XRD)和扫描电镜(SEM)对样品进行物相和形貌分析.结果表明,先在70℃保温5 h或10 h,再在800℃煅烧2 h可得到纯相的Li4/3Ti5/3O4粉末,平均粒径在300nm左右,且粒径分布均匀.充放电测试表明在70℃保温5 h、800℃煅烧2 h得到的样品具有最优异的电化学性能.以0.1C倍率充放电,其首次放电容量达到172(mA·h)/g,接近理论容量,20次循环后,容量仍保持在140(mA·h)/g.与传统的固相法相比,用直接融盐法得到的材料具有较大的锂离子扩散速率、高倍率性能和循环可逆性.     

Synthesis and Property of H2La2Ti3O10/CdS Layered Nanocomposite Photocatalyst

H2La2Ti3O10/CdS nanocomposite with er photoactivity was synthesized by a stepwise exchange process from H2La2Ti3O10, which was obtained by H^＋ -exchanging reaction of H2La2Ti3O10 with HCl other than the normally used HNO3. The pillaring process was investigated by XRD, TEM, FT-IR and BET methods. The photocatalytic decomposition of aniline was used as the model system to evaluate the photochemical properties of H2La2Ti3O10/CdS,H2La2Ti3O10 and K2La2Ti3O10. It is found that the photoactivity of layered H2La2Ti3O10 is greatly improved by the intercalation of CdS in the interlayer. In general, the excellent photoactivity of the H2La2Ti3O10/CdS nanocomposite might be attributing to the extremely small particle size of incorporated CdS and good contact between CdS and La2Ti3O10^2- layers. On the other hand, the coupling of two semiconductor particles with different energy gap is useful to achieve effective charge separation. In H2La2Ti3O10/CdS, a photo-generated electron can transfer from CdS to the La2Ti3O10^2- layer, while the holes remain in the CdS particles. This helps to diffuse the electrons and holes before reaching the interface, and the holes and electrons can be effectively captured by the electrolyte in the solution. Simuhaneously, the optimal operating condition of photodecomposition aniline was investigated.     

La2O3/TiO2纳米粒子超声光催化降解邻硝基苯酚

以钛酸丁酯为原料,用溶胶-凝胶(Sol-gel)法制备了La2O3/TiO2纳米粒子.采用X光衍射仪对粉体的粒径、物相进行了表征.研究了超声光催化协同降解水中邻硝基苯酚的效果,考察了超声波声强、反应温度和催化剂投加量对邻硝基苯酚降解速率的影响.研究结果表明,超声光催化协同降解要比单独超声波或光化学处理效果显著,证实了声光联合技术具有明显的协同效应.     

La2O3对ZrO2-Y2O3-Ta2O5陶瓷材料结构及性能的影响

采用固相合成法在氧化钇部分稳定氧化锆(YSZ)陶瓷材料的基础上引入氧化物Ta2O5以及稀土氧化物La2O3取代部分Y2O3,获得一种新型的La2O3-ZrO2-Y2O3-Ta2O5陶瓷材料。分别利用X射线衍射仪、扫描电子显微镜和STA-449C热膨胀仪对材料的物相组成、微观结构及热膨胀性能进行表征。结果表明,陶瓷材料的主晶相仍为四方相,晶粒尺寸减小,在RT～1200℃温度范围内热膨胀系数有所减小。     

镧改性固体催化剂SnO2-WO3/La2O3的制备及其催化性能

500℃焙烧3 h条件下制备了摩尔比nSn∶nW=2∶1,含3.0%(质量分数,下同)La2O3的镧改性固体催化剂SnO2-WO3/La2O3,采用IR分析对其进行了表征。通过改变催化剂用量、30%H2O2用量、反应时间及催化剂重复使用性等因素,系统考察了该稀土改性双金属氧化物催化氧化环己酮合成己二酸的催化性能。实验结果表明,己二酸的适宜合成条件为:100 mmol环己酮,1.25 g催化剂SnO2-WO3/La2O3,50 mL 30%H2O2,回流反应7 h,目的产物己二酸收率达77.7%。SnO2-WO3/La2O3连续使用6次己二酸收率仍可接近40%。     

固相合成In2O3纳米晶及动力学的研究

以InCl3·4H2 O和NaOH为原料 ,利用固相反应合成前驱体 ,再经焙烧合成In2 O3纳米晶。用X射线衍射 (XRD)分析了不同焙烧温度对合成In2 O3晶粒尺寸的影响。研究结果表明 :按Scherrer公式估算合成In2 O3纳米晶的晶粒尺寸在 2 0～ 3 0nm ,焙烧温度越高 ,晶粒尺寸越大 ;根据前驱体不同升温速率下的差热 (DTA)曲线 ,用Kissinger和Ozawa法计算了合成In2 O3纳米晶的活化能分别为 167.0 3和 176.0 6kJ·mol- 1 ,差别不大 ;根据晶粒生长动力学理论计算In2 O3晶粒长大的活化能为 2 .82kJ·mol- 1 ,表明热处理过程In2 O3纳米晶粒的长大主要以界面扩散为主。     

稀土固体超强酸S2O82-/Sb2O3/La3+的制备及催化性能研究

以SbCl3为原料经醇化水解制得Sb2O3前体氧化物,通过浸渍一定量的(NH4)2S2O8和掺杂La(NO3)3制备了一种新型催化剂S2O82-/Sb2O3/La3+.以催化合成乙酸苄酯为探针反应,考察了不同制备条件对催化剂性能的影响.结果表明,1.5 mol/L的(NH4)2S2O8和2.71% La(NO3)3混合溶液浸渍锑前体氧化物,经110℃烘干后,于500℃焙烧3h所得催化剂(SSL2.71-3-500)活性较好.同时,考察了催化剂的稳定性以及对不同酯化反应的作用规律.用Hammett,IR,DTA/TGA,XRD等手段对催化剂进行了表征.     

Mechanochemical Reaction of Lanthanum Carbonate with Sodium Hydroxide and Preparation of Lanthanum Oxide Nanoparticle

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Enhanced photocatalytic activity of Gd~(3+) doped TiO_2 and Gd_2O_3 modified TiO_2 prepared via ball milling method

Gd~(3+)/TiO_2 and Gd_2O_3/TiO_2 nanoparticles were prepared by ball milling method.The effects of Gd~(3+)ion and Gd_2O_3 on the structure and optical property of TiO_2 were studied by XRD and UV-vis DRS.Specific surface area was determined by Brunauer-Emmett-Teller(BET)method.The morphology and elemental composition were characterized by SEM-EDS.XPS was used to determine the surface compositions and chemical character of elements.The sample sizes and microstructures were observed by TEM.The photocatalytic activities of TiO_2 nanoparticles modified with rare earth metal gadolinium(Gd~(3+)ion or Gd_2O_3)were evaluated by degradation of methylene blue(MB)under UV light.Experimental results indicate that 2,5 mol%Gd~(3+)/TiO_2 shows the best photocatalytic activity compared with Gd_2O_3/TiO_2 and pure TiO_2.The existence of gadolinium can exhibit the aggregation and induce lattice distortion of TiO_2 obtained from XRD,SEM and TEM results.The band gap energy of 2.5 mol%Gd~(3+)/TiO_2 decreases to3.07 eV and it leads to visible light absorption response which can be seen from UV-vis absorption spectra.The surface area of 2.5 mol%Gd~(3+)/TiO_2 equals to 85.8 m~2/g and average crystal size is 21.1 nm.EDS and XPS analyses reveal that gadolinium can be introduced either into TiO_2 lattice or adsorbed on the surface of TiO_2.The content of surface OH groups in 2.5 mol%Gd~(3+)/TiO_2 is 50,88%(1.55 times higher than that of pure TiO_2)and the content of lattice oxygen decreases to 11.26%.The MB(25 mg/L)degradation reaction rate constants of 2,5 mol%Gd~(3+)/TiO_2,0.5 mol%Gd_2O_3/TiO_2 and pure TiO_2 were0.0713,0.0588 and 0.0263 min~(-1),respectively.The degradation rates of rhodamine B(30 mg/L)in 60 min are 97,9%,90.1%and 84.6%for 2,5 mol%Gd~(3+)/TiO_2,0.5 mol%Gd_2O_3/TiO_2 and pure TiO_2,respectively.     

ZnO-TiO2体系的固相合成与表征

以分析纯ZnO和TiO2粉体为原料,直接固相法制备钛酸锌粉体.利用X射线衍射（XRD）、扫描电镜（SEM）对粉体物相、形貌进行表征,采用热重-差热（TG-DTA）研究固相反应机理.结果表明：氧化物粉体最低反应温度为800℃,升高反应温度有利于Zn2TiO4相的生成,延长反应时间有利于六方相ZnTiO3生成.在800~900℃保温4 h获得平均粒径为0.3~0.5μm的球形钛酸锌粉体,该晶体生长过程为扩散机制控制,调整温度对产物形貌影响不大.     

A Study on the Thermal Stability of La_2O_3-TiO_2 Supports

In this paper,various techniques including BET,XRD,SEM and XPS were used to study the sintering ofpure and La_2O_3-doped titania.The experimental results show that sintering of titania proceeds via volume diffu-sion.Adding of lanthanum oxide decreases the rate of sintering and hinders the phase transition from anatase torutile crystal by strong surface interaction between the mixed crystals(La_4Ti_9O_(24),La_(0.66)TiO_(2.99))and TiO_2.     

熔盐电解制备钛锆合金及其反应过程研究

采用熔盐电解法由ZrO_2与TiO_2混合氧化物(Ti, Zr原子比为1∶ 1)一步制备出了TiZr合金, 并探讨了反应机制. 温度为900 ℃, CaCl_2熔盐中以烧结的ZrO_2与TiO_2混合氧化物为阴极,石墨棒为阳极, 3.1 V恒电压电解, 制备出了钛锆合金. 结果表明, 所得产物的组分与投料比例一致, 钛、锆为无限互溶的固溶体, 电解反应是由外向内进行的. 其合金化历程为: 部分ZrO_2先生成CaZrO_3, 然后继续脱氧还原为锆的低价氧化物直至还原为金属锆, 一旦有金属锆生成, TiO_2在金属锆上直接电解还原形成钛的低价氧化物, 直至生成金属钛后与锆形成固溶体; 其余ZrO_2, TiO_2先形成CaZr_mTi_nO_x, 然后直接脱氧还原为TiZr.     

Synthesis of Ultrafine K2Ln2Ti3O10 by Microemulsion Method and Its Photoactivity Research

A series of uhrafine K2Ln2Ti3O10（Ln = La, Ce, Pr, Nd, Sm, Eu, Dy）photocatalyst was prepared by microemulsion method based on tetrabutyl titanate reacting with potassium hydroxide and lanthanumoxide. The obtained products were characterized by XRD, TEM and UV-Vis spectra. These results indieate that highly ultrafine K2Ln2Ti3O10 can be accessible at lower fabricating temperature and shorter reation time by this approach. In addition, the investigation on their eatalytieal behavior based on the degradation of methyl orange under UV-Vis light suggests that the degradation rate can reach up to 60%.     

Chemical States of Lanthanum in Carbonized La2O3-Mo Thermionic Cathode Materials

The chemical reaction between lanthanum oxide and molybdenum carbide was studied by thermodynamic calcu-lation, thermal analysis and in-situ X-ray Photoelectron Spectroscopy. The theoretical results show that at the environment allowing for the evaporation of lanthanum, such as in high vacuum, La2O3 in the La2O3-Mo materials can be reduced to metallic lanthanum by molybdenum carbide (Mo2C). To confirm the conclusion, many analysis methods such as XRD, SPS, and TG-DTA were taken. The experimental results show that the chemical state of lanthanum changes during heat-ing. It was proved, for the first time, that reacted metallic lanthanum appears at the surface of this kind of material at high temperature.     

Photocatalytic activity of Lu3+/TiO2 prepared by ball milling method

Ball milling method was applied to prepare Lu~(3+)/TiO_2 photocatalysts. The catalysts were characterized with X-ray powder diffraction(XRD), X-ray photoelectron spectroscopy(XPS), UV-visible diffuse reflectance spectra(UV-vis DRS), energy dispersive X-ray spectrometer(EDS), transmission electron microscopy(TEM) and Brunauer-Emmett-Teller(BET) method. The photocatalytic activities were determined by the degradation of methylene blue(MB) equipped with a 300 W medium pressure mercury lamp. Results show that the first order reaction rate constants of Lu~(3+)/TiO_2 and pure TiO_2 are0.0565 and 0.0263 min-1, respectively, which both were evaluated under the condition of catalysts loading of 0.2 g/L,initial concentration of 25 mg/L for MB, mole ratio of Lu~(3+)/TiO_2 of 1.5% and milling time of 4 h. The average crystal sizes of 1.5 mol% Lu~(3+)/TiO_2 and pure TiO_2 are 18.7 and 19.3 nm, respectively.     

Synthesis of Long Afterglow Phosphor CaAl2Si2O8:Eu2+, Dy3+ via Sol-Gel Technique and Its Optical Properties

The long afterglow phosphor CaAl2Si2O8:Eu2 , Dy3 was prepared by a sol-gel method. The sol-gel process and the structure of the phosphor were investigated by means of X-ray diffraction analysis (XRD). It is found that the single anorthite phase formed at about 1000 ℃, which is 300 ℃ lower than that required for the conventional solid state reaction. The obtained phosphor powders are easier to grind than those of solid state method and the partical size of phosphor has a relative narrow distribution of 200 to 500 nm. The photoluminescence and afterglow properties of the phosphor were also characterized. An obvious blue shift occurs in the excitation and emission spectra of phosphors obtained by sol-gel and solid state reaction methods. The change of the fluorescence spectra can be attributed to the sharp decrease of the crystalline grain size of the phosphor resulted from the sol-gel technique.     

电感耦合等离子体发射光谱法测定石灰石、白云石中的多元素

研究了ICP-AES法同时测定石灰石、白云石中多元素的方法,经试验确定了溶样条件I、CP分析条件及各元素的特征分析谱线。该方法简洁快速,结果满意,适用于石灰石、白云石中SiO2、CaO、MgO、Fe2O3、Al2O3、MnO、P、TiO2、SrO、K2O、和Na2O的同时测定。