Nd∶Y_3Al_5O_(12)单晶及纳米粉体的Raman光谱分析

测量了YAG（Y3Al5O12）/Nd∶YAG单晶、Nd∶YAG前驱物及其在不同温度下煅烧获得粉体的拉曼光谱,对谱峰的振动模式进行了指认,对结果进行了分析。Nd∶YAG前驱物在煅烧时,有一个由非晶态向晶态的转化过程;700℃下烧结前驱物获得非晶态产物的结构中含有AlO4四面体结构;随着煅烧温度的升高,拉曼光谱的变化主要表现在两个方面：一是谱峰半高宽（FWHM）减小,谱峰强度增大;二是一些拉曼光谱谱峰发生了频移,这是纳米多晶粉体的界面组元的有序度提高所致。另外,800℃下煅烧获得的Nd∶YAG纳米粉体的晶格振动模式与Nd∶YAG晶体的晶格振动模式存在差异,这是纳米多晶粉体的界面组元的贡献所致。     

不同制备条件对Zn2SiO4∶Mn2+粉末发光性能的影响

利用溶胶-凝胶法制备了Zn2SiO4∶Mn2 粉末,探讨了体系pH值、热处理温度、煅烧气氛对材料结构和发光性能的影响。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、光致发光(PL)谱等分析手段对Zn2SiO4∶Mn2 粉末的结构、颗粒大小、形貌、发光性能进行了表征。结果表明:溶胶的pH值影响制备的粉体的结晶性和颗粒大小,当溶胶pH值为4.34时,体系水解缩聚反应充分,所得荧光粉的光致发光强度最强;煅烧气氛显著影响荧光粉的发光强度,前驱体在N2(90%) H2(10%)的还原气氛下煅烧得到的发光粉发光强度最强;最佳热处理温度为900℃。     

YAG及其掺杂纳米粉体的结构与光学特性

由于透明多晶钇铝石榴石(YAG)陶瓷在高功率全固态激光器中巨大的应用价值,所以其研究在近几年引起了广泛的关注。YAG陶瓷与其单晶材料相比,可以实现大尺寸激光晶体,高掺杂浓度,并且制备的成本低。我们报道水热方法制备的纯YAG和硅、铷掺杂YAG陶瓷纳米粉体中掺杂与煅烧温度对陶瓷相组分、晶格参数和晶粒尺寸的影响。通过XRD和透射电子显微镜表征了YAG陶瓷及掺杂粉体的结构及其受到掺杂和烧结的作用,利用光吸收和发射谱研究了共掺杂和煅烧温度对YAG陶瓷粉体光学特性的影响。结果表 Si⁴⁺和Nd³⁺的共掺杂提高了Nd³⁺在YAG纳米体中的可溶度,促进了YAG相的生成,单相纳米Si/Nd:YAG粉体在920℃煅烧温度即可获得。它的光学特性与报道的单晶Nd:YAG一致。     

Nd∶YAG激光透明陶瓷超细粉体的合成及其性能表征

以Al(NO3)3·9H2O和Y2O3为原料,按YAG化学计量比配成相应的硝酸盐混合液,并用一定量的Nd取代Y,加入尿素沉淀剂,利用无机体系均相沉淀法制备了YAG前驱体.对前驱体进行适当处理,并采用高温热解法在1200℃时制备出Nd∶YAG透明陶瓷超细粉体.通过对粉体样品进行XRD,TG-DTA,SEM和红外光谱分析表明,所合成的YAG超细粉为立方晶系石榴石结构,晶格常数a=12.01nm.粉体样品颗粒度小、粒径均匀、流动性好,粒径在150～200nm之间.     

Nd:YAG激光透明陶瓷超细粉体的合成及其性能表征

以Al(NO3)3·9H2O和Y2O3为原料,按YAG化学计量比配成相应的硝酸盐混合液,并用一定量的Nd取代Y,加入尿素沉淀剂,利用无机体系均相沉淀法制备了YAG前驱体。对前驱体进行适当处理,并采用高温热解法在1200℃时制备出Nd∶YAG透明陶瓷超细粉体。通过对粉体样品进行XRD,TG DTA,SEM和红外光谱分析表明,所合成的YAG超细粉为立方晶系石榴石结构,晶格常数a=12.01nm。粉体样品颗粒度小、粒径均匀、流动性好,粒径在150～200nm之间。     

不同助烧剂对Nd∶YAG激光陶瓷前驱粉体烧结活性的影响

采用氨水共沉淀法制备了Nd∶YAG激光陶瓷前驱粉体,并在其中分别加入助烧剂SiO2和CaCO3。利用XRD、SEM及荧光光谱分析了不同助烧剂对Nd∶YAG激光陶瓷前驱粉体烧结活性的影响。XRD测试结果表明,助烧剂SiO2和CaCO3不能促进Nd∶YAG激光陶瓷前驱粉体的结晶。SEM照片观察发现,SiO2的助烧效果较好,能促进Nd∶YAG激光陶瓷前驱粉体的烧结,增加了前驱粉体的烧结活性,并且通过荧光光谱分析发现,助烧剂不改变Nd3+的4F3/2—4I11/2荧光发射。     

Nd:Y3Al5O12单晶及纳米粉体的Raman光谱分析

测量了YAG(Y3Al5O12)/Nd:YAG单晶、Nd:YAG前驱物及其在不同温度下煅烧获得粉体的拉曼光谱,对谱峰的振动模式进行了指认,对结果进行了分析.Nd:YAG前驱物在煅烧时,有一个由非晶态向晶态的转化过程;700℃下烧结前驱物获得非晶态产物的结构中含有AlO4四面体结构;随着煅烧温度的升高,拉曼光谱的变化主要表现在两个方面:一是谱峰半高宽(FWHM)减小,谱峰强度增大;二是一些拉曼光谱谱峰发生了频移,这是纳米多晶粉体的界面组元的有序度提高所致.另外,800℃下煅烧获得的Nd:YAG纳米粉体的品格振动模式与Nd:YAG晶体的晶格振动模式存在差异,这是纳米多晶粉体的界面组元的贡献所致.     

溶剂热-高温煅烧法制备纳米Gd2MoO6:Nd3+近红外发光材料

采用乙二醇-水的混合溶液作为溶剂,用溶剂热法制备了Gd2MoO6∶Nd3+的前驱体,然后对得到的样品在800℃下煅烧1 h。使用X射线衍射仪对样品的结构进行了表征,通过近红外和可见光区的发射光谱和激发光谱以及透射电子显微镜对样品的发光性质以及形貌进行了研究。探究了煅烧温度、Nd3+的掺杂浓度、pH值、乙二醇-水的配比对样品的近红外发光性能以及形貌的影响。实验结果表明,在乙二醇-水的配比为1∶1,Nd3+的掺杂摩尔分数为0.03,pH值为1.5,煅烧温度为800℃时,能得到分散性良好,并具有优良近红外发光性质的纳米粒子。     

光学材料 光学塑料、光学陶瓷

TQ174．758．23 2005043091 Na:YAG激光透明陶瓷超细粉体的合成及其性能表征= Preparation and characteristics of Nd:YAG super-fined powders for laser transparent ceramics[刊,中]／卢利平(长春理工大学材料与化工学院．吉林,长春(130022)),刘景和…／／光学技术,-2005,31(2),-306-308 以Al(NO3)3·9H2O和Y2O3为原料,按YAG化学计量比配成相应的硝酸盐混合液,并用一定量的Nd取代 Y,加入尿素沉淀剂,利用无机体系均相沉淀法制备了 YAG前驱体。对前驱体进行适当处理,并采用高温热解法在1200℃时制备出Nd:YAG透明陶瓷超细粉体。通     

无团聚YAG:Ce~(3+)荧光粉的制备与表征

采用共沉淀-喷雾干燥法制备YAG∶Ce3+荧光粉。前驱体经热处理、研磨、酸洗碱洗后形成荧光粉。研究了前驱体料浆浓度、热处理条件、研磨、酸洗碱洗对粉末晶相、颗粒形貌、粒度和发光性能的影响。研究发现:料浆浓度为0.2,0.4,0.6 mol/L时,前驱体颗粒形貌分别呈碎屑、光滑和褶皱状球形;无团聚光滑球形前驱体经1 100℃热处理4 h后,XRD未检测到杂相;继续升温至1 550℃,荧光粉相对亮度随之提高;酸洗碱洗能够去除碎屑,获无团聚荧光粉,提高相对亮度。     

Nanocrystalline CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> powder by PVA sol–gel route: synthesis,characterization and its giant dielectric constant

Nanocrystalline CaCu₃Ti₄O₁₂ powders were synthesized by a simple PVA sol–gel route and calcined at 700 and 800°C in air for 8 h. The diameter of the powders ranges from 40–100 nm. The calcined CaCu₃Ti₄O₁₂ powders were characterized by TG-DTA, XRD, FTIR, SEM, and TEM. Sintering of the powders was conducted in air at 1100°C for 16 h. The XRD results indicated that all sintered samples had a typical perovskite CaCu₃Ti₄O₁₂ structure although the sintered samples contained some amount of CaTiO₃. SEM of the sintered CaCu₃Ti₄O₁₂ ceramics showed the average grain sizes of 13–15 μm. The samples exhibit a giant dielectric constant, ε′∼10⁵ at 150 to 200°C with weak temperature dependence below 1 kHz in the sample sintered using the powders calcined at 700°C. The Maxwell–Wagner polarization mechanism is used to explain the high permittivity in these ceramics. It is also found that all sintered samples have the same activation energy of grains, which is ∼0.122 eV.     

Mixed-metal carbonates as precursors for the synthesis of nanocrystalline Mn-Zn ferrites

A mixed Mn-Zn-Fe carbonate was prepared by precipitation of metal ions with ammonium carbonate and control of pH=7. Nanocrystalline Mn-Zn ferrite powders were synthesized by thermal decomposition of the carbonate precursor at 500 °C in air. The mean crystallite size of the ferrite particles is 14 nm with a specific surface of 74 m²/g. The magnetization at 5 K of the Mn-Zn ferrite powders (66 emu/g) is smaller than the saturation magnetization of the bulk material. Hysteresis loop measurements indicate ferrimagnetic behavior at 5 and 298 K with a small coercivity at room temperature.     

BaHfO3:Ce sintered ceramic scintillators

Raw powders of BaHfO₃:Ce were prepared with modified Pechini process and were calcined in the 650–1700 °C range of temperatures, at different atmospheres – air, vacuum and nitrogen–hydrogen mixture. The powders were converted into sintered ceramics by vacuum sintering. The materials were characterized by XRD, TEM, photoluminescence and radioluminescence spectroscopy. UV-VUV excitation spectra were recorded using synchrotron radiation. Excitation spectra proved that atmosphere of preparation significantly influences the host-to-activator energy transfer, which is the most efficient for materials made in reducing conditions. Also radioluminescence efficacy was found to be superior for materials prepared in such conditions.     

Yb^3＋：Y2O3超细粉体的低温燃烧法合成及发光性能

以稀土硝酸盐和尿素（摩尔分数为1∶3）为原料,采用低温燃烧法在点火温度为600℃,热处理温度为1 100℃,热处理时间为1 h条件下制备了Yb3＋∶Y2O3超细粉体。利用X射线粉末衍射仪（XRD）、扫描电子显微镜（SEM）和荧光光谱仪（FS）对粉体进行了表征。研究了点火温度、燃料用量和热处理温度对粉体性能的影响。实验结果表明：所制备的Yb3＋∶Y2O3超细粉体的粒径为15～30 nm,颗粒分散性较好,无明显团聚,且粉体的发光性能良好,发射峰位于976,1 030和1 075 nm,适合于制备Yb3＋∶Y2O3透明陶瓷。     

水热法制备不同形貌的GdVO_4:Eu~(3+)纳米发光材料

采用水热法制备了不同形貌的GdVO4:Eu3+纳米晶样品,对其结构以及发光性质进行了表征。XRD结果表明:水热前驱体和经过灼烧之后样品均为四方晶系,具有锆石结构。TEM照片表明:通过改变表面活性剂分别得到了分散性良好的米粒状、六角形和球形的GdVO4:Eu3+纳米晶粒子。发光光谱表明:在288nm的紫外光激发下,不同形貌的GdVO4:Eu3+纳米晶材料均在617nm处产生特征红光发射,归属为Eu3+离子的5D0→7F2跃迁,不同形貌粒子的发光光谱的相对强度有所不同。     

CaS∶Eu~(2+),Sm~(3+)的制备与表征

采用湿法工艺在还原气氛下制备了CaS∶Eu2+,Sm3+光存储材料。研究了灼烧温度和灼烧时间对样品性能的影响。XRD图谱表明,样品在700℃—1200℃均形成CaS晶格。光谱分析表明,在紫外光(295nm)激发后,用980nm半导体激光照射样品,具有光激励发光现象,发射光谱峰值波长为649nm。     

Magnetic behavior and physicochemical properties of Ni and NiO nano-particles

A series of nano-crystalline Ni/NiO particles was synthesized by a combustion route depending upon the glycine-nitrate process. The as prepared samples were characterized by X-ray diffraction (XRD), scanning electron micrograph (SEM), transmission electron micrograph (TEM), nitrogen adsorption isothems at 77 K and vibrating sample magnetometer (VSM) techniques.The XRD results revealed that the Ni powder crystallizes was formed with the cubic phase when the molar ratio of glycine to nitrate is 1.5. Above or below that molar ratio, NiO phase coexists as an impurity along with the Ni phase. The SEM and TEM measurements of the as synthesized powders showed that the particles are irregular in shapes and have porous morphology. Increasing the ratio between glycine and Ni-nitrate resulted in slightly agglomeration and grain growth of nano-particles with subsequent decrease in the value of surface area depending upon high combustion heat. The magnetization value of Ni measured at room temperature is very close to the value observed for commercial Ni powder.     

锐钛矿型二氧化钛纳米粉体的IR光谱与光催化性能研究

采用溶胶-凝胶法制备了TiO2光催化剂,研究了不同温度下焙烧TiO2粉体的XRD和FT-IR光谱。400℃焙烧后,相应有机物的红外吸收峰消失,随着焙烧温度的升高,粉体粒径变大,800-420cm-1之间的吸收峰逐渐锐化,700℃焙烧的FT-IR谱的423cm-1为金红石型TiO2的特征Ti-O键振动。500℃焙烧的锐钛矿型TiO2粉体对水杨酸具有较好的光催化活性。