聚乙二醇凝胶法制备CeO_2纳米晶

采用聚乙二醇凝胶法制备了不同粒径的单相CeO2 纳米晶。XRD分析表明 ,所合成的CeO2 纳米晶属于立方晶系 ,空间群为O5 H-FM 3M。TEM分析表明 ,CeO2 纳米晶呈球形 ,且随焙烧温度的升高 ,CeO2 纳米晶粒径增大。热失重分析表明 ,样品的失重率主要取决于焙烧温度 ,而焙烧时间的影响较小。密度分析表明 ,CeO2 纳米粉末的密度随焙烧温度的升高、粒径的增大而增加。     

胶溶法合成CeO2纳米晶

用胶溶法合成了不同粒径的CeO2纳米晶,XRD分析表明,所合成的CeO2纳米晶属立方晶系,空间群为O5H-FM3M.计算表明,随着焙烧温度的升高,CeO2晶粒度增大,而平均晶格畸变率则随晶粒度的增大而减小,表明粒子越小,晶格畸变越大,晶粒发育越不完整.TEM分析表明,所合成的CeO2纳米晶呈球形,随焙烧温度的升高,粒子的粒径增大.     

聚乙二醇凝胶法制备CeO2纳米晶

采用聚乙二醇凝胶法制备了不同粒径的单相ＣｅＯ２纳米晶。ＸＲＤ分析表明,所合成的ＣｅＯ２纳米晶属于立方晶系,空间群为Ｏ＾５Ｈ－ＦＭ３Ｍ。ＴＥＭ分析表明,ＣｅＯ２纳米晶呈球形,且随焙烧温度的升高,ＣｅＯ２纳米晶粒径增大,热失量分析表明样品的失重率主要取决于焙烧温度,而焙烧时间的影响较小,密度分析表明,ＣｅＯ２纳米粉末的密主随焙烧温度的升高、粒径的增大而增加。     

沉淀法制备纳米二氧化铈及其表征

利用XRD、SEM和TG-DTA分析手段对用两步沉淀法制备的纳米二氧化铈粉进行了初步表征:XRD分析表明,当焙烧温度为200～600℃时,所合成的CeO2粒子属于立方晶系,空间群为O5hFm3m;SEM微观分析表明,CeO2粒子呈球形,粒度随焙烧温度的升高而增大,在400℃焙烧所得到的粒子粒径≤100nm;TG-DTA分析表明,该方法的前驱体结构为Ce(OH)3OOH和CeO2·2H2O的混合物.     

纳米二氧化铈制备与EPR特性研究

用溶胶-凝胶法制备了CeO2纳米材料，并在不同焙烧温度下得到颗粒大小不同的CeO2材料．分析了CeO2独特结构特点，研究了不同焙烧温度下制备的CeO2材料颜色不同的原因，发现颗粒大小增大、颜色变浅是由于粒子对可见光的吸收能力减弱，其折射、散射光增多的缘故所致；利用电子顺磁共振（EPR）技术研究了不同焙烧温度下制备的CeO2，发现CeO2具有较强的热稳定性；分析了不同样品中的色心和O2^-信号不同的原因．     

沉淀法制备Er2O3纳米晶与表征

在乙醇溶液中,用反向沉淀法制备了Er2O3纳米晶.XRD分析表明,不同温度热处理的Er2O3均为立方晶系,空间群为T5-1213.TEM分析表明,所合成的Er2O3粒子呈球形.实验发现Er2O3晶粒度随焙烧温度的升高而增大,而平均晶格畸变率随焙烧温度的升高,晶粒度的增大而减小,衍射强度随焙烧温度的升高而增大.在酸中溶解性试验和红外光谱分析表明,纳米Er2O3比原料Er2O3具有更高的表面活性,Er-O键的吸收具有微小的蓝移,吸收强度减弱.     

沉淀法制备Er2O3纳米晶与表征

在乙醇溶液中,用反向沉淀法制备了Ｅｒ２Ｏ３纳米晶。ＸＲＤ分析表明,不同温度热处理的Ｅｒ２Ｏ３均为立方晶系,空间群为Ｔ５－１２１３。ＴＥＭ分析表明,所合成的Ｅｒ２Ｏ３粒子呈球形。实验发现Ｅｒ２Ｏ３晶粒度随焙烧温度的升高而增大,而平均晶格畸变率随焙烧温度的升高,晶粒度的增大而减小,衍射强度随焙烧温度的升高而增大。在酸中溶解性试验和红外光谱分析表明,纳米Ｅｒ２Ｏ３比原料Ｅｒ２Ｏ３具有更高的表面活性,Ｅｒ     

水热晶化法制备纳米TiO2的动力学研究

用水热晶化法一步制得D101晶面尺寸为10～16 nm的具有较好结晶度的锐钛矿型的纳米TiO2.XRD结果和热力学分析表明,当水热晶化温度控制在体系的沸点时,所得到的锐钛矿型纳米TiO2的粒度最小.用水热晶化法制得的具有锐钛矿型纳米TiO2在100 ℃焙烧后就开始向金红石型转变.起始相变温度大大地低于文献报道的250 ℃.从而有效地避免了高温焙烧制备金红石型TiO2过程中的粒子团聚现象.动力学分析表明,在实验温度范围内(100～800 ℃)焙烧,低温段(t<500 ℃)的晶粒生长速率大于高温段(t>500 ℃)的晶粒生长速率.其晶粒生长表观活化能分别为:当t<500 ℃时,EA(锐钛矿)＝18.76 KJ/mol,ER(金红石)=38.49 KJ/mol;当t>500 ℃时,EA(锐钛矿)＝70.76 KJ/mol,ER(金红石)=75.66 KJ/mol.低温段(t<500 ℃)有利于锐钛矿型晶粒的生长,相比较而言,高温比低温更有利于金红石型晶粒的生长.     

沉淀法制备La2Sn2O7微粉

用沉淀法制备了La2Sn2O7微粉。XRD分析表明,在1100℃下合成了单相的La2Sn2O7微粉,属于立方晶系,空间群为Fd3m。实验表明,焙烧温度是影响La2Sn2O7相形成的主要因素,而焙烧时间则是次要因素。SEM分析表明,La2Sn2O7粒子基本本呈球形,粒度小于0.5μm。相对密度分析表明,随焙烧温度的增加,粉末的密度增大。     

沉淀法制备La2Sn2O7微粉

用沉淀法制备了La2Sn2O7微粉.XRD分析表明,在1100℃下合成了单相的La2Sn2O7微粉,属于立方晶系,空间群为Fd3m.实验表明,焙烧温度是影响La2Sn2O7相形成的主要因素,而焙烧时间则是次要因素.SEM分析表明,La2Sn2O7粒子基于本呈球形,粒度小于0.5um.相对密度分析表明,随焙烧温度的增加,粉末的密度增大.     

Preparation of Nanocrystalline ZrO2 by Reverse Precipitation Method

Nanncrystalline ZrO2 particulates with different sizes were prepared by precipitation method using ethanol as dispersive and protective reagent. XRD patterns show that the synthesized ZrO2 is monnclinic in structure with space group P21/a when calcination temperature is in the range of 400- 1000 ℃ . It is found that the smaller the particle, the bigger the crystal lattice distortion, the worse the costal growth, and the lower the diffrnction intensity. TEM images reveal that ZrO2 particles are spherical in shape, and the particle size distribution is in narrow range. The mean sizes of the particles increase with the increase of calcination temperatures . It is first to observe tbe streaks of different crystallographic planes. Thermogravimetric analysis indicates that the crystallization temperature of ZrO2 is 461.32 ℃ . Measurement of ZrO2 relative density shows that the relative density of nanocrystalline ZrO2 powders increases witb the increasing of ZrO2 particle sizes.     

制备纳米二氧化铈粉体新工艺的研究

以硝酸铈为原料,柠檬酸为燃烧剂,采用燃烧法制备纳米二氧化铈粉体。考察了反应物配比,不同焙烧时间和焙烧温度对制备纳米二氧化铈粉体的影响。并采用傅立叶变换红外光谱仪（FTIR）、紫外-可见分光光度计（UV-Vis）、差热-热重联用分析仪（TG-DTA）、X射线衍射仪（XRD）和透射电镜（TEM）对产物进行表征分析。研究表明,当硝酸铈和柠檬酸物质的量比为1.7：1.0,焙烧温度为300℃,焙烧时间为2h时,为最佳反应条件。此条件下,CeO2的晶粒大小约为6nm。     

温度及Y_2O_3对SG法制备ZrO_2相结构及粒度的影响

针对纳米ZrO2粉体粒径较小、比表面积大、极易发生团聚问题,以纳米ZrO2为研究对象,采用溶胶-凝胶(SG)法,以氧氯化锆为锆源,水为溶剂,Y2O3为稳定剂,PEG-6000为分散剂,主要研究烧结温度及Y2O3对制成的纳米ZrO2相结构及其粒度的影响.实验结果表明:经XRD分析,所制得的ZrO2试样主要为四方相结构,随着煅烧温度的升高,粉体粒径增大;SEM测试结果表明,在一定ZrO2陶瓷粉体粒度范围内,随着稳定剂Y2O3加入量的增加,粉体颗粒间的分散性有所改善.综合考虑对纳米ZrO2相结构及粒度的影响,确定最佳烧结温度为650℃,稳定剂Y的最佳加入量为7.5mol%,制备的ZrO2纳米粉体粒径尺度最佳,晶型稳定性好且分散性得到改善.     

Preparation of ZAO powder and investigation on its infrared emissivity

According to the basic infrared stealth mechanism of low infrared emissivity powders,the ZAO powder materials were prepared by liquid coprecipitation method,and the starting materials were Zn( NO3) 6H2O and Al( NO3) 39H2O. The process parameters were obtained,and the relationship between technology parameters and infrared emissivity was investigated. The temperature of thermal treatment,crystal structure and surface micrograph of ZAO powder was analyzed by the help of TG-DTA,XRD and SEM. The infrared stealth performance of ZAO powder was studied by IR-2 emissivity spectroscopy. Results showed that the infrared emissivity was the lowest when pH was 8. 0,calcination temperature was 1100 ℃,calcination time was 2 h,and the Al2O3doping content was 3% ( mass percentage) . The crystal structure of doped ZAO powder was lead-zinc, and there exists distortion of crystal lattice in nanocrystalline ZnO. The average particle size was 10 μm. The lowest infrared emissivity reached to 0. 61 at between 8 μm and 14 μm. It means that the ZAO powders will be excellent infrared stealthy materials.     

钨酸盐发光材料MWO_4:Eu~(3+)(M=Ca,Sr)的制备及表征

采用共沉淀法合成了CaWO4:Eu3+和SrWO4:Eu3+荧光粉体.利用荧光光谱仪测定了样品的光谱特性,结果表明,其主要激发波长为393nm和464nm,以393nm为激发波长说明样品能被近紫外光有效激发,并在614nm产生红色荧光;采用XRD分析其物相及晶体结构,发现生成的发光材料的晶型为四方晶系,晶粒均在纳米级,且在焙烧温度为400℃时生成的样品不含杂质,晶粒尺寸较小;扫描电镜显示400℃焙烧温度下生成的发光材料的样品颗粒大小在100~300nm之间,焙烧温度升高时,SrWO4:Eu3+的抗烧结能力弱,样品出现团聚,生成的样品颗粒变大.     

Growth and characterization of doped CeO2 buffers on Ni-W substrates for coated conductors using metal organic deposition method

CeO2 and Ce0.8M0.2O2-d films (M = Mn, Y, Gd, Sm, Nd and La) with (00l) preferred orientation have been prepared on biaxially textured Ni-W substrates by metal organic decomposition (MOD) method. The factors influencing the formation of cracks on the surface of these CeO2 and doped CeO2 films on Ni-W substrates were explored by X-ray diffraction (XRD), scanning electron microscopy (SEM) analysis, atomic force microscopy (AFM) and differential scanning calorimetry (DSC). The results indicate that many factors, such as the change of the ionic radii of doping cations, the transformation of crystal structure and the formation of oxygen vacancies in lattices at high annealing temperature, may be related to the formation of cracks on the surface of these films. However, the crack formation shows no dependence on the crystal lattice mismatch degree of the films with Ni-W substrates. Moreover, the suppression of surface cracks is related to the change of intrinsic elasticity of CeO2 film with doping of cations with a larger radius. SEM and AFM investigations of Ce0.8M0.2O2-d (M = Y, Gd, Sm, Nd and La) films reveal the dense, smooth and crack-free microstructure, and their lattice parameters match well with that of YBCO, illuminating that they are potentially suitable to be as buffer layer, especially as cap layer in multi-layer architecture of buffer layer for coated conductors.