溶胶-凝胶法制备核级ZrB2粉体

针对核级ZrB₂-IFBA可燃毒物燃料的特点,以硼酸、硝酸氧锆作为B、Zr源,葡萄糖为C源,通过溶胶-凝胶技术和热碳还原工艺制备出核级ZrB₂超微粉体。采用X射线衍射仪、场发射扫描电子显微镜、化学滴定仪等分析了样品的相组成、微观形貌和元素质量分数。结果表明,当Zr:B:C=1:2.2:6.5（摩尔比）时,在1300℃保温2 h后可获得平均粒径为0.41 μm的超微ZrB₂粉体,整个过程B损失率最低为10.6%（质量分数）,与现有工业化ZrB₂粉末制备工艺相比,B损失率显著降低。     

柠檬酸溶胶法制备Bi2WO6粉体及其表征

利用钨酸铵、硝酸铋、柠檬酸和硝酸为原料,柠檬酸溶胶法制备了Bi₂WO₆粉体.热重-差热（TG-DTA）和红外光谱（FT-IR）分析Bi₂WO₆前驱体的热分解过程,X射线衍射（XRD）、场发射扫描电镜（FE-SEM）对Bi₂WO₆粉体结构、形貌进行表征.结果表明,Bi₂WO₆前驱体热分解分为4个阶段,其中Bi₂WO₆粉体开始形成发生在367 ℃. Bi₂WO₆前驱体在400~700 ℃煅烧5 h获得了单一的Bi₂WO₆粉体,当温度低于600 ℃时,产物为球形颗粒,晶粒尺寸随温度升高变化不大,当温度达到700 ℃时,晶粒迅速长大,最终发展成为规则的正交晶系.这表明晶体生长过程发生了由扩散机制向界面反应控制机制的转变,因此通过调整煅烧反应温度和保温时间可以控制产物的尺寸和形貌.      

溶胶-凝胶燃烧合成法制备SmBO3粉体及其性能研究

利用溶胶-凝胶燃烧合成法,在750℃热处理2 h的条件下制备了SmBO3粉体,颗粒大小在100 nm左右.红外吸收光谱显示材料在500～1400 cm-1波数范围内,存在较为集中的吸收峰.此外,由于Sm3+的6H5/2→6F9/2跃迁,使得SmBO3粉体在1.05～1.15μm的范围内反射率降低.因此,SmBO3粉体可能是一种性能较好的针对1.06和10.6μm激光的激光光防护材料和滤光功能材料.     

溶胶凝胶、碳热/硼热还原法制备ZrB2-SiC-LaB6超细复相粉体

以氧氯化锆(ZrOCl₂·8H₂O)、硼酸(H₃BO₃)、水合氯化镧(LaCl₃·7H₂O)、正规酸乙酯(TESO)和葡萄糖(C₆H₁₂O₆)为主要原料,以聚乙二醇(PEG)为分散剂,采用溶胶凝胶法和碳热/硼热还原工艺制备ZrB₂-SiC-LaB₆超细复相粉体。利用X射线衍射、扫描电镜、红外光谱和差示扫描量热分析等对ZrB₂-SiC-LaB₆粉体进行表征,研究烧结温度、原料配比对复相粉体合成过程的影响。结果表明,当原料中n(Zr)∶n(B)∶n(Si)∶n(La)∶n(C)=1∶3∶0.7∶0.16∶8时,在氩气气氛中1 500℃保温2 h,可合成高纯ZrB₂-SiC-LaB₆超细复相粉体。颗粒平均粒径为300 nm,其中ZrB₂相为六方晶...     

溶胶-凝胶法制备工艺参数对Al2O3-SiO2薄膜质量的影响

采用溶胶-凝胶法制备Al2O3-SiO2复合薄膜,研究溶胶成分、水解反应温度、热处理环境及烧结温度对薄膜质量的影响。通过黏度测试、热重分析仪(TG-DTG)、X射线衍射分析仪(XRD)和原子力显微镜(AFM)对样品进行表征。结果表明,溶胶的组成与热处理过程中的应力不均是导致薄膜开裂的主要原因。当Al2O3:SiO2(mol/mol)=1:3或1:2,水解反应温度为40℃,热处理环境湿度70%,温度60℃,以0.5℃/min的升温速率升至600℃焙烧2 h,缓慢升温且适当保温,可得完好的Al2O3-SiO2复合薄膜,所制备的块状薄膜,无裂缝且均匀透明。     

溶胶-凝胶法制备TiO2/硅藻土复合材料及其光催化性能

采用焙烧、酸洗等工艺预处理硅藻土,以改性硅藻土和钛酸丁酯为前驱体,采用溶胶-凝胶法制备TiO₂/硅藻土复合材料,采用XRD、SEM、FT-IR、TG等手段对其进行分析表征,以甲基橙为降解对象考察其光催化性能。结果表明：硅藻土表面均匀负载着锐钛矿型的二氧化钛,晶粒尺寸为35.76 nm。负载比2∶1、pH为>2～3、焙烧温度500℃制备的TiO₂/硅藻土复合材料的光催化性能最好,热稳定性良好。当TiO₂/硅藻土复合材料投入量为1 g/L,对60 mL(10 mg/L)的甲基橙溶液60 min内的降解率达到92%。     

溶胶制备工艺对ZrO2-Y2O3涂层性能的影响

用无机金属盐水解及有机醇盐中间体合成两种不同的工艺路线制备了ZrO₂-Y₂O₃复合Sol(溶胶),对比了通过Dip-Coating的方法在GH220/MCrAlX基体上形成致密ZrO₂-Y₂O₃陶瓷涂层的能力,以及涂层在1000℃的静态抗氧化性能.结果表明,金属有机醇盐工艺制备的ZrO₂-Y₂O₃陶瓷涂层具有极其优越的高温静态抗氧化性能.无机金属盐水解所制备的ZrO₂-Y₂O₃涂层抗氧化能力明显低于金属有机醇盐工艺.可能的原因是残留在涂层内的微量酸根离子使氧化和腐蚀过程加剧.     

溶胶-凝胶法制备Sr2SiO4:Tb3+绿色荧光粉及其发光性能

采用溶胶-凝胶法合成了一系列适合紫外-近紫外激发的(1-X)Sr₂SiO₄:XTb3+(X=0,0.01,0.02,0.03,0.04,0.05,0.06)绿色荧光粉,并采用X射线衍射(XRD)、扫描电子显微镜(SEM)和荧光光谱(PL)研究了样品的结构及发光性能.由XRD的检测结果可知,合成样品属于单斜晶系的β-Sr₂SiO₄相.由SEM图可知,所有样品都呈无规则块状结构.当监测波长为546 nm,样品的激发光谱的主峰位于370 nm处,属于Tb3+的4f-4f特征跃迁吸收.当激发波长分别为285 nm和250 nm,所有样品在488 nm,547 nm,586 nm,623 nm处都出现了1个强发射峰,分别对应Tb3+的5D₄→7F₆、5D₄→7F₅、5D₄→7F₄和5D₄→7F₃电子跃迁.最强发射峰位于547 nm处,呈现特征为绿光发射.随Tb3+掺杂量增大,发射强度呈现出先增大后减小的变化趋势,即存在浓度猝灭效应.当Tb3+掺杂量为X=0.03时,样品的发光强度最大.      

纳米NiO粉体的制备及其表征

采用溶胶转化－凝胶法制备了纳米级NiO粉体。Ni(OH)2粉体的TG－DSC分析表明：在升温速率为10℃/min的条件下，粉体在489K时开始显著分解，626K时分解完毕。X－射线衍射分析表明：分解产物为纯净的NiO2。NiO粉体的化学成分分析表明：其纯度高于国家标准。TEM电镜分析表明：NiO粉体呈单分散的球形或棒状颗粒。对NiO粉体的热敏性能有待进一步研究。     

超细WO3粉体的制备及表征

通过胶溶法、溶胶 凝胶法、聚合 络合法合成了超细三氧化钨粉体。并对 3种制备方法的不同制备条件进行了探讨 ,实验发现不同制备条件对三氧化钨粉体粒径有较大影响 ,研究得出了每种方法的最佳制备条件。胶溶法中pH约为 4.60 ,静置 2 4h ,加入十六烷基三甲基溴化铵(CTAB)浓度为 0 .15mol·L- 1 ;溶胶 凝胶法中pH约为 2 .3 1,加入草酸和CTAB浓度分别为 0 .40和 0 .2 0mol·L- 1 ;而聚合 络合法中前驱体在 2 5 0℃干燥后 ,在 60 0℃煅烧接着再在 65 0℃煅烧。用激光粒度仪、比表面测定仪、XRD和TEM对产品进行了表征 ,结果表明所制三氧化钨为正交晶系 ,平均粒径在 5 0～ 2 0 0nm。团聚粒子大小不均 ,粒径范围较宽 ,颗粒为不规则形状。胶溶法制备的粒子的粒径较其他两种方法更小、更均匀。     

Synthesis and photoluminescence properties of ZnTiO3:Eu3+ red phosphors via sol-gel method

ZnTiO3:Eu3+ phosphors were synthesized with different concentrations of Eu3+ doping through sol-gel method. The samples were calcined at different temperatures for 2 h in air. The synthesized powders were characterized by X-ray diffraction(XRD), scanning electron microscopy-energy dispersive spectroscopy(SEM-EDS), transmission electron microscopy(TEM), Raman and photoluminescence spectroscopy. The XRD results showed that the Zn Ti O3:Eu3+ phosphors doped with different concentrations of Eu3+ ions calcined at 600 oC were of single phase, which indicated that the Eu3+ ions had been successfully incorporated into the Zn Ti O3 host lattice and did not destroy the lattice structure of Zn Ti O3 host. The Raman spectrum, SEM and TEM also proved that the doping of Eu3+ did not change the lattice structure of hexagonal Zn Ti O3 host. The photoluminescence(PL) of Eu3+ ions with the main emission peak at 614 nm was observed to increase with Eu3+ concentrations from 0.5 mol.% to 2.0 mol.% and decreased when the concentration was increased to 2.5 mol.%. The decrease in the PL intensity at higher Eu3+ concentrations could be associated with concentration quenching effect. The CIE1931 chromaticity diagram(x, y) of Zn Ti O3:2.0 wt.%Eu3+ phosphors were located in the red region(x=0.652, y=0.347). The luminescence properties suggested that Zn Ti O3:Eu3+ phosphors might be regarded as a potential red phosphor candidate for light emitting diodes(LEDs).     

Photoluminescent properties of Ca2Gd8（SiO4）6O2： Dy^3＋ phosphor films prepared by sol-gel process

There are growing interests on phosphor thin films owing to their potential application in high-resolution devices such as cathode ray tubes and flat panel display devices. The solution-based sol-gel method is one of the most important techniques for the synthesis of various functional coating films. Compounds with the apatite structure are very suitable host lattices for various luminescent ions. Ca2RE8（SiO4）6O2 （ RE=Y, Gd, La ） is a kind of ternary rare-earth-metal silicate with oxyapatite structure, which has been used as host material for the luminescence of various rare earth and mercury-like ions. In this article, Ca2Gd8（SiO4）6O2：Dy^3＋phosphor films were dip-coated on quartz glass substrates through the sol-gel process. X-ray diffraction （XRD）, atomic force microscopy （AFM）, photoluminescence （PL） spectra, as well as lifetimes were used to characterize the resulting films. AFM study revealed that the phosphor films consisted of homogeneous particles. The Dy^3＋ showed its characteristic emission in crystalline phosphor films, i.e., ^4F9/2-^6H15/2 and ^4F9/2-^6H13/2.     

Al粉添加量对汽车用热压注成形Al2O3粉末组织和性能的影响

选择Al粉作为Al₂O₃粉末材料的改性剂, 采用热压注工艺制备汽车用Al₂O₃粉末材料试样, 研究不同Al粉添加量(质量分数)对Al₂O₃粉末材料组织结构和力学性能的影响。结果表明: Al₂O₃粉末热压注试样最大收缩率出现在长度方向, 最小收缩率出现于高度方向。随着Al粉质量分数的增加, Al₂O₃粉末热压注试样收缩率表现出先减小, 后稳定增加, 最后再减小的变化规律, 弯曲强度和体积密度降低, 气孔率显著升高, 试样挠度增高, 浇注得到更大孔径的结构, 同时试样中大尺寸孔径数量也显著增多。随着Al粉质量分数的增加, 试样中Al₂O₃衍射峰不断上升, 玻璃相的变化不大。加入质量分数8%的Al粉后, 试样断口区域生成了明显的颗粒结构, 说明试样主要发生沿晶断裂。     

Fe2O3转变为Fe3O4粉末的微波碳热还原

以活性炭为还原剂及以氩气为保护气,采用微波碳热还原的方法,将弱磁性的Fe₂O₃还原成强磁性的Fe₃O₄,并研究焙烧温度、保温时间以及SiO₂粉末的加入对其还原焙烧成分及磁化效果的影响规律.结果表明:在配碳量一定的条件下,焙烧温度是微波碳热还原的关键因素,随着温度的升高,还原产物中Fe₃O₄的含量发生有规律的变化;650℃、保温5 min的条件下经微波还原后生成了纯Fe₃O₄粉末,其磁化率和还原度分别达到理论值2.33和11.11%;含SiO₂的Fe₂O₃粉末在750℃以上进行微波还原,会生成大量的硅酸亚铁和氧化亚铁,导致Fe₃O₄含量降低,恶化还原焙烧指标,所以微波磁化焙烧的最佳温度应在570~650℃.     

Luminescent properties of amorphous phosphor 1.4YeO3·2.5Al2O3·0.1Tb2O3 prepared by sol-gel method

Amorphous phosphor 1.4YeO3·2.5Al2O3·0.1Tb2O3 （the same composition as Y2.8Tb0.2Al5O12） was prepared via a sol-gel method at relatively low temperature （i.e., below 650℃）, which is much lower than that for the preparation of polycrystalline Y3Al5O12：Tb^3＋ （above 1400℃）. The amorphous phosphor prepared in the optimized conditions showed a bright green-yellowish luminescence, the intensity of which was comparable with that of polycrystalline sample and the emissions of which were assigned to 5D4 → 7Fj transitions of Tb^3＋. Besides the emissions of Tb^3＋, the amorphous samples prepared at temperatures below 500 ℃ presented a weak blue emission band around 420 nm.     

SPS法制备Al2O3/Cu复合材料研究

将纳米级A12O3以体积分数为1％的配比与微米级Cu粉混合均匀后,采用放电等离子烧结(SPS)法,分别在750、800和850℃进行烧结制备复合材料;将同样的混合粉末采用冷压烧结制备复合材料作为对比.分别测试材料的密度、硬度、导电率,并进行SEM扫描电镜分析.结果表明:在所选择试验参数下,烧结温度为800℃ SPS烧结试样具有最高的相对密度,达到99.17％,硬度与导电率也最高;与冷压烧结制备的材料相比,SPS法制备的试样硬度和导电率更高;SPS烧结试样晶粒均匀细小,并出现了孪晶.     

Characterization of CeO2-ZrO2 mixed oxides prepared by two different co-precipitation methods

A series of cerium zirconium mixed oxides were prepared by two co-precipitation methods using magnesium hydrogen carbonate(MHC)and mixed ammonia-ammonia hydrogen carbonate(AAHC)as precipitant respectively.The crystal structure,BET surface area and morphology of the produced cerium zirconium mixed oxides were characterized by X-ray diffraction(XRD),Brumauer-Emmett-Teller(BET)and scanning electron microscopy(SEM)techniques.The reduction-oxidation behavior and oxygen storage capacity(OSC)performance were also studied by temperature programmed reduction(TPR)and oxygen pulse chemical adsorption methods.The XRD results demonstrated that the cerium zirconium mixed oxides obtained by both methods possessed structure of cubic solid solution phase.The fresh surface area calcinated at 600℃,aged surface area after 1000℃ and OSC at 500 ℃ of cerium zirconium mixed oxides were determined to be 89.337,34.784 m2/g,and 567 μmol O2/g for MHC method and 122.010,46.307 m2/g,and 665 μmol O2/g for AAHC method,respectively.     

Photoluminescent properties of LaF3：Eu^3＋ and GdF3：Eu^3＋ nanoparticles prepared by co-precipitation method

LaF₃:Eu³⁺ and GdF₃:Eu³⁺ nanoparticles were prepared by a co-precipitation method in the presence of the chelating agent, citric acid. The structural properties of the products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The average crystallite size was estimated from the full-width at half-maximum (FWHM) of the diffraction peaks by the Scherrer equation. The sizes of the nanoparticles were 12 nm for LaF₃:Eu³⁺ and 17 nm for GdF₃:Eu³⁺. The luminescent properties of the nanoparticles were investigated by excitation and emission spectra. Energy transfer from Gd³⁺ to Eu³⁺ was observed.