An IR and XPS spectroscopy assessment of the physico-chemical surface properties of alumina–YAG nanopowders

Well-dispersed nano-crystalline transition alumina suspensions were mixed with yttrium chloride aqueous solutions, with the aim of producing by spray-drying Al₂O₃–Y₃Al₅O₁₂ (YAG) composite powders of increasing YAG vol.%. Two samples were prepared, with different Y content, corresponding to 5 and 20 YAG vol.%, respectively. Both samples were then treated at either 600 or 1150 °C. The obtained powders were characterized by X-Ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Fourier Transform Infra Red (FT-IR) spectroscopy and compared to three reference samples: commercial nano-crystalline transition alumina, YAG and Y₂O₃. YAG powders were obtained by co-precipitation route whereas Y₂O₃ powders were yielded by spray-drying of a yttrium chloride aqueous solution. Modification of physico-chemical properties of the surface of alumina nanoparticles were assessed by combining XPS and FT-IR spectroscopies. On the basis of the results obtained, a possible model is proposed for the structure of the obtained composites, in which Y basically reacts with more acidic hydroxyls of alumina, by forming Y-rich surface grains, the extension of which depends on the thermal treatment.     

Influence of AlF3 and ZnF2 on the phase transformation of gamma to alpha alumina

This paper focused on the effect of AlF₃ and ZnF₂ additives on the phase transformation of gamma to alpha alumina. AlF₃ and ZnF₂ were found to be effective accelerating agents on the gamma to alpha phase transformation. A single phase of alpha alumina, with an average particle size of 22 nm, can be obtained at 920 °C with AlF₃additive. ZnF₂ can reduce the gamma to alpha transformation temperature to 900 °C, the average size of the particles is about 40 nm and the morphology of some particles is platelike with an aspect ratio of 2–4. The reduction of the transformation temperature was mainly attributed to the formation of intermediate compound of AlOF, which was considered to accelerate the mass transportation from transition alumina to alpha alumina. Moreover, mechanical milling and introducing alumina seeds uniformly worn from the milling mediums are also beneficial for reducing the transformation temperatures.     

AgCl纳米晶掺杂铌碲酸盐系统非线性光学玻璃材料研究

铌碲酸盐非线性光学玻璃具有优良的三阶非线性光学效应,引入适量纳米晶体后,有望进一步提高玻璃的三阶非线性光学性能.本文采用在辅助电场诱导下的热处理方法在TeO2-Nb2O5-BaO-AgCl系统玻璃中析出AgCl纳米晶体,并研究了AgCl含量、热处理工艺及电场施加工艺对纳米晶析出和三阶非线性光学性能的影响.结果发现,在铌碲酸盐系统玻璃中引入0.1%～0.35%(质量分数)的AgCl,经热处理后可在玻璃中获得AgCl纳米晶体,而辅助电场提供的较小推动力可诱导更多的纳米晶体均匀析出,并且可以将其尺寸控制在20nm以下.采用辅助电场与热处理工艺相匹配的控制技术可以明显提高材料的三阶非线性光学性能.     

Constrained densification in boehmite–alumina mixtures for the fabrication of porous alumina ceramics

It is demonstrated that inherent constrained densification characteristics of the bimodal size distributed powders can be utilized to fabricate porous alpha alumina. Seeded boehmite was mixed with coarse alpha alumina particles to produce various compositions of bimodal mixtures. The densification behaviour of the mixtures was correlated with shrinkage and microstructural evolution. The mixtures sintered at 1200 °C contained more than 30% porosity and the mechanical strength of the mixtures was increased by 2–4 fold relative to the coarse particles alone with similar porosity (<5 MPa). © 1998 Chapman & Hall     

溶胶-凝胶燃烧法制备La_2O_3和La(OH)_3纳米晶的研究

采用燃烧法合成纳米La(OH)3材料,分别以硝酸镧和柠檬酸为镧源和络合剂,以氨水调节pH值为2～4、柠檬酸与硝酸镧的物质的量比为1～1.2∶1之间,加热凝胶至自蔓延燃烧后并在700～750℃煅烧1～2 h,得到膨松粉末状产物,即La2O3纳米晶。利用X射线衍射和透射电镜等测试方法对凝胶热分解过程及最终形成的La2O3纳米晶颗粒进行分析和表征。结果表明:用该方法得到的纳米La2O3产物的平均粒径在30～100 nm之间可控;纳米La2O3在空气中是不稳定的,在自然吸潮情况下和空气中的H2O发生反应生成La(OH)3,控制湿度即可得到纯La(OH)3纳米晶。     

Comparison of zinc oxide nanoparticles and its nano-crystalline particles on the photocatalytic degradation of methylene blue

Comparison of ZnO nanoparticles and its nano-crystalline particles on the photocatalytic degradation of methylene blue was investigated. ZnO nanoparticles and its nano-crystalline particles were synthesized from sprayed droplets of an aqueous zinc nitrate solution by flame spray pyrolysis and spray pyrolysis assisted with an electrical furnace, respectively. ZnO nanoparticles of 20 nm in average diameter and ZnO nano-crystalline particles of 20 nm in the grain size were prepared to compare the photocatalytic activity. The photocatalytic activity of those ZnO particles was evaluated by measuring the degradation of methylene blue in water under the illumination of ultraviolet rays. Effect of the particle morphology, initial concentration of methylene blue, and photocatalyst loading on the degradation of the methylene blue was investigated under the illumination of ultraviolet rays. The photocatalytic degradation capacity of the ZnO nanoparticles was higher than that of the ZnO nano-crystalline particles. The efficiency of photocatalytic degradation of methylene blue increased with increase in photocatalyst loading and decrease in initial concentration regardless of particle morphology.     

Fabrication of nanosized alumina powders by a simple polymer solution route

Nanosized alumina (Al2O3) powders had been successfully fabricated by a simple polymer solution route employing polyvinyl alcohol (PVA) as an organic carrier. The fabricated alumina powders had an average particle size of 6.1 nm with a high specific surface area of 99.5 m2/g. As well, the alumina powders were fully crystallized to alpha phase at a relatively low temperature of 1000 degrees C. The PVA polymer contributed to a soft and porous microstructure of the calcined alumina powders, and ball-milling process with the porous powders was effective in making nanosized alumina powders. In addition, the content and degree of polymerization of the PVA affected the development of crystallization and powder properties. In this study, the simple polymer technique and milling process for the fabrication of nanosized alumina powders are introduced, and the effects of PVA on the property of the synthesized alumina powders are observed. For the study, the characterizations of the synthesized powders are conducted by using XRD, TEM, particle size analyzer, and nitrogen gas adsorption.     

非均相沉淀法制备纳米α-Al2O3/金属复合粉体

利用非均相沉淀法制备了平均粒径小于50 nm的α-Al₂O₃/W(Ni)复合粉体,并研究对比了纳米钨和镍对α-Al₂O₃相转变温度的影响。结果表明:纳米钨和镍的存在均可降低过渡型氧化铝向α型氧化铝转变的相变温度,但降低程度有所不同,含钨氧化铝于1000℃完成相变,而含镍氧化铝于1150℃完成相变;并且纳米第二相体积比越大,对相变温度的影响也越大。     

纳米硅薄膜的镜反射红外光谱研究

研究探讨了镜反射红外光谱在纳米材料方面的应用。通过等离子化学气相沉积法(PECVD),制备本征和掺磷的纳米硅薄膜(nc-Si：H),利用镜反射红外光谱研究了本征和掺磷的纳米硅薄膜的光谱特征。通过实验,发现这两种薄膜中都存在多氢键合方式,PECVD工艺参数如衬底温度、直流电压和掺杂浓度对薄膜结构具有一定的影响。     

Parameters affecting transient oxide formation on FeCrAl based foil and fibre materials

Abstract

The effects of oxidation temperature and atmosphere on the formation of alumina scales on two commercial FeCrAl foil materials have been investigated. The oxidized specimens were characterized using a range of surface analysis techniques including SEM, XRD, laser induced optical spectrometry (LIOS), AES and XPS. During oxidation at temperatures exceeding 1000°C, the protective oxide scales formed on FeCrAl-alloys consist mainly of alpha alumina. At lower temperatures, however, formation of transient alumina modifications, has been observed. Although after longer oxidation times transformation into the stable alpha alumina occurs, the high initial growth rate of the metastable oxide phases could lead to a critical depletion of the Al-reservoir in thin walled (e.g. 20 (m) components, resulting in early breakaway failure. The occurrence of metastable oxides cannot simply be correlated with alloy composition.     

Hydrothermal synthesis of hierarchical titanium silicalite-1 using single template

Hierarchical nano-crystalline TS-1 can be directly synthesized using tetrapropylammonium hydroxide (TPAOH) as single template in the presence of a ‘seed’ gel. The hierarchical nano-crystalline TS-1 was characterized by scanning electron microscopy, transmission electron microscopy, powder X-ray diffraction, UV-Vis diffuse reflectance spectroscopy and nitrogen adsorption-desoprtion. Compared with the conventional TS-1, the hierarchical nano-crystalline TS-1 contained an additional porosity including supermicro/mesopores, which attributed to the interstitial voids existing between the nanocrystals. The secondary porosity in the TS-1 material provided an enhanced external surface area and high mesopore volume in favor of fast diffusion of both reactants and products, which resulted in an enhanced activity in the epoxidation of bulky molecules cyclohexene using aqueous H₂O₂ solution as oxidant.     

纳米晶Al及Al-Mg合金的合成与性能研究进展

主要总结了纳米晶Al及Al-Mg合金的合成与性能研究进展,详尽介绍了用低温球磨法制备纳米晶Al及Al-Mg合金的过程,简要分析了影响低温球磨过程的因素,并探讨了球磨过程对显微组织的影响;介绍和评述了纳米晶Al的热稳定性,并在与粗晶Al及Al-Mg合金对比的基础上,介绍了纳米晶Al及Al-Mg合金的力学性能以及蠕变性能等方面的研究进展.     

机械力化学合成纳米晶体的研究

介绍了机械力化学的概念、作用机理及其表征技术。阐述了机械力化学制备纳米粉体的机理和优越性,并主要以BaTiO3纳米晶为例,研究其合成方法及反应机制。对其未来发展进行了展望。     

Preparation and properties of alumina-ceria nano-nano composites

Alumina-ceria composites were prepared by the calcination in air of gels obtained by homogeneous precipitation from dilute chloride and nitrate solutions, followed by either microwave treatment, autoclave treatment or air-drying. Microwave treatment and air-drying of the gels yielded amorphous powders whereas autoclave treatment yielded well-crystallised boehmite. The phase evolution during calcination was investigated by in-situ X-ray diffraction (XRD) and by differential thermal analysis and thermogravimetry (DTA/TG). The structures of the calcined powder were investigated by transmission electron microscopy (TEM) and high resolution TEM. A variety of morphologies was found depending on the processing route. The calcined microwave treated gels consisted of nano-size particles of ceria in nanostructured transition alumina i.e. a nano-nano composite structure suitable for catalysis applications. In comparison, the calcined autoclave treated gels consisted of a coarser composite of large agglomerates of ceria in transition alumina which, however, was more stable against transformation to alpha alumina at high temperature. Boehmite sols made with the autoclave treated gels were suitable for making thin films by dip-coating. This revised version was published online in September 2006 with corrections to the Cover Date.     

Synthesis and characterization of nanocrystalline mesoporous zirconia using supercritical drying

Synthesis of nano-crystalline zirconia aerogel was done by sol-gel technique and supercritical drying using n-propanol solvent at and above supercritical temperature (235-280 degrees C) and pressure (48-52 bar) of n-propanol. Zirconia xerogel samples have also been prepared by conventional thermal drying method to compare with the super critically dried samples. Crystalline phase, crystallite size, surface area, pore volume, and pore size distribution were determined for all the samples in detail to understand the effect of gel drying methods on these properties. Supercritical drying of zirconia gel was observed to give thermally stable, nano-crystalline, tetragonal zirconia aerogels having high specific surface area and porosity with narrow and uniform pore size distribution as compared to thermally dried zirconia. With supercritical drying, zirconia samples show the formation of only mesopores whereas in thermally dried samples, substantial amount of micropores are observed along with mesopores. The samples prepared using supercritical drying yield nano-crystalline zirconia with smaller crystallite size (4-6 nm) as compared to higher crystallite size (13-20 nm) observed with thermally dried zirconia.     

水热温度对纳米AlOOH成核机理及界面模型的影响

用微观结晶理论解释提高水热温度时出现的纳米AlOOH形貌"逆转"现象,指出升高温度对纳米AlOOH晶体生长速率所具有的"双重"作用;分析温度的改变所引起的体系能量起伏,探讨温度变化直接引起生长基元变化,从而改变成核的机制,最终导致晶体形貌的改变的实质。结果表明:温度的提高激发新的晶核形成,诱导新的生长基元出现,改变原来的界面生长模型,从而彻底改变了晶体生长机制。     

Simultaneous carbothermic reduction of iron and titanium oxides to produce an iron-based composite by mechanically activated sintering method

In this research, for the first time, Fe–TiC nano-crystalline composite was produced via simultaneous reduction of iron and titanium oxides by petrocoke. Powder mixture of Fe₂O₃/TiO₂/petrocoke was mechanically activated in a high-energy ball mill at different times. X-ray diffraction method (XRD) and Scanning Electron Microscopy (SEM) were used to characterize the milled powders. The results showed that new phases were not formed during milling, even after 20 h of milling. However, crystallite size and lattice strain of hematite were remarkably decreased and increased, respectively. Thermogravimetry and Differential Thermal Analysis (TG–DTA) were done on 0, 10 and 20 h mechanically activated powders. These experiments showed a substantial decrease in reduction temperature of iron and titanium oxides as a result of mechanical activation. Then, the powders were cold compacted and sintered at 1200 °C in argon atmosphere for 1 h. XRD results of 20 h milled samples demonstrated that, in this condition, iron oxide was completely reduced to nano-crystalline iron and titanium dioxide was reduced to nano-crystalline titanium carbide and Fe–TiC nano-crystalline composite was successfully formed.     

O/W/O多重乳液法制备毫米级氧化铝空心球

采用O/W/O多重乳液法, 以液体石蜡为内核, 氧化铝溶胶为外壳层组成的复合液滴作为前驱体, 制备毫米级氧化铝空心球, 研究了装置几何结构对前驱体的形成和固化过程对空心球结构的影响。结果表明, 内部油相通过直流通道直接注射到水相液滴内部时, 形成的复合液滴具有均一核壳结构, 壁厚和直径在30~80 μm和800~2200 μm可控。液滴置于水平方向旋转固化, 保持转速在20~60 r/min, 所得凝胶球可以保持完整的球形度和核壳结构。1200℃高温煅烧制备出的氧化铝空心微球维持高的球形度和空心结构, 表面粗糙度大约22 nm, 壁厚达到几十微米, 直径达到毫米级, 主要晶型为稳定的α-Al₂O₃。     

Production of ultrafine alpha alumina powders and fabrication of fine grained strong ceramics

Hydrous alumina powders, pure, seeded with alpha alumina, containing ammonium nitrate and containing both ammonium nitrate and seeds, were prepared by hydroxide precipitation. Their crystallization and sintering behaviour were investigated and mechanical properties of the ceramics were tested. Pure hydrous alumina transformed to alpha alumina crystals, with a size of ca. 200 nm, at 1200°C, after undergoing the usual metastable phase changes during heat-treatment. The powder needed to be sintered at 1600°C to achieve a high density. The ceramic had an average grain size of ca. 9 m. Seeding lowered the transformation temperature to ca. 1120°C and caused the transformation to begin at ca. 600°C. The material could be sintered at 1500°C and had a grain size of 2 m. The nitrate, predominantly present as ammonium nitrate, lowered the transformation temperature to ca. 1150°C and altered the proportion of the intermediate phases. However, the materials still had to be sintered at 1500°C to achieve >97% density. When both seed particles and nitrate ions were present the material almost completely transformed at 950°C to uniform crystals of alpha alumina with a size <60 nm that sintered to >99% theoretical density at 1450°C. The final ceramic had a uniformly grained (<1.0 m) microstructure and exhibited strength up to 800 M Pa.     

Deposition of nano-crystalline graphite films by cathodic plasma electrolysis

Atmospheric pressure plasma deposition of nano-crystalline graphite films on titanium substrates from a predominantly ethanolic liquid phase was carried out under varying applied voltage. A thorough study of the plasma electrolytic deposition mechanisms has been performed. The investigation of the composition, structural properties, and the morphology of these graphite coatings have been performed by visible and ultraviolet Raman spectroscopy, X-ray Photoelectron Spectroscopy, Scanning Electron Microscopy and X-ray elemental microanalysis. The experimental evidence of the reduction of the work function and the enhancement of the plasma intensity with the presence of the carbon film has been reported. These properties make such nano-crystalline graphite coatings very attractive for the production of inexpensive cold cathodes for electronics and plasma devices.