PET/SiO2 nanocomposites prepared by cryomilling

The mixed powders of poly(ethylene terephthalate) (PET) and SiO₂ has been subjected to cryomilling. The evolution of microstructure with time was characterized using scanning electron microscope, transmission electron microscope, field emission scanning electron microscope, and laser diffraction particle size analyzer. It was shown that, upon cryomilling for 10 h, SiO₂ nano particles were well deconglomerated into single particles (～30 nm) that get homogeneously dispersed in PET matrix. The resulted PET/SiO₂ primary particles were flake‐shaped with a size of 400 nm. These primary composite particles agglomerated to form secondary composite particles with an average size about 7.6 μm. A three‐stage model was purposed for the formation mechanism of the nanocomposite structures induced by cryomilling. Our evidences suggest that cryomilling is a capable and promising technique for the production of polymer/inorganic nanocomposites. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 1161–1167, 2006     

Quasi-static deformation and final fracture behaviour of aluminium alloy 5083: influence of cryomilling

The commercial aluminium alloy 5083 was processed via cryomilling to produce nanocrystalline (NC) powders with an average grain size of ～25–50?nm. The powders were subsequently degassed at 723 K (450°C), pre-heated and immediately quasi-isostatic (QI)-forged to produce a thermally stable bulk ultrafine grain (UFG) material having average grain size values ranging from 190 to 350?nm, depending on the processing conditions used. In this paper, the tensile properties and fracture behaviour of the bulk UFG material are presented and compared with the tensile properties of its conventionally processed counterpart. The specific influence of preheat temperature on strength and ductility of the alloy is briefly discussed. Three different pre-heat temperatures of 523, 623 and 723?K (250, 350 and 450°C) were chosen and used with the primary objective of controlling grain growth during forging. The influence of preheat temperature on tensile deformation and final fracture behaviour is highlighted. The macroscopic fracture modes of the bulk nanostructured material (BNM) prepared following three pre-heat temperatures are investigated. The microscopic mechanisms controlling tensile deformation and final fracture behaviour are discussed with regards to the intrinsic microstructural effects in the UFG alloy, nature of loading, and the kinetics and mechanisms of deformation.     

低温球磨制备Mg-4%Ni-1%NiO储氢材料及其性能

采用低温球磨技术制备了Mg-4%Ni-1%NiO储氢材料,主要研究低温球磨时间对材料形貌结构以及储氢性能的影响.采用扫描电子显微镜(SEM)和X射线衍射(XRD)分析材料的形貌和相组成,采用压力-组成-温度(P-C-T)设备研究材料的储氢性能.结果表明:分别经过2、4和7 h球磨后,材料的相组成没有发生明显改变,只有极少量的Mg2Ni合金相生成.随着球磨时间的延长,材料的平均粒度逐渐下降,作为催化剂的Ni、NiO相逐渐揉进基体内部.伴随着上述变化,材料的活化性能、吸氢性能逐渐提高,球磨到7 h后材料仅需活化1次即可达到最大吸放氢速率,初始吸氢温度降为60℃,在4.0 MPa初始氢压和200℃下吸氢量为6.4%(质量分数),60s即可完成饱和吸氢量的80%,10min内完成饱和吸氢量的90%;材料的放氢性能则在球磨4 h后已经基本保持不变,0.1MPa下初始放氢温度为310℃,在350℃、0.1MPa下材料可在500s内释放饱和储氢量的80%.     

Synthesis of nanocrystalline NiCrC alloy feedstock powders for thermal spraying by cryogenic ball milling

Nanocrystalline NiCrC alloy powders with a qualified particle size distribution for thermal spraying were synthesized using the cryogenic ball milling (cryomilling) method. The morphology, microstructure, size distribution, and phase transformation of the powders were characterized by scanning electron microscopy (SEM), laser scattering for particle size analysis, X-ray diffraction (XRD), and transmission electron microscopy (TEM). After cryomilling for 20 h, the average grain size of the as-milled powders approached a constant value of 30 nm by XRD measurement. The average particle size slightly increased from 17.5 to 20.3 μm during the 20-h milling. About 90vol% of the powders satisfied the requirement for thermal spraying with the particle dimension of 10-50 μm, and most of the powders exhibited spherical morphology, which were expected to have good fluidity during thermal spraying. The Cr₂O₃ phase formed during the cryornilling process as revealed in the XRD spectra, which was expected to enhance the thermal stability of the as-milled powders during the followed thermal spraying or other heat treatment.     

低温球磨制备5083超细铝合金及性能研究

本文采用低温球磨的方法制备了5083纳米晶铝合金,并用XRD、SEM和DSC等检测手段对样品粉末的微观结构、组织的变化过程和热稳定性进行了研究。结果表明:随着球磨的进行,球磨混合料中Mg相逐渐减少并逐渐固溶于Al中形成合金,粉末颗粒尺寸不断减小;球磨时间和球磨转速是影响合金结构和性能的主要因素,采用低温高速球磨能使合金纳米晶粒更加均匀,有利于Mg固溶于Al中;能谱分析和DSC分析表明,低温液氮球磨过程中形成的氧化物和氮氧化物颗粒对晶粒的钉扎一定程度的提高了5083铝合金的热稳定性。     

Electromagnetic nanocomposites prepared by cryomilling of polyaniline and Fe nanoparticles

The polyaniline (PANI)/iron nanocomposites have been prepared by high‐energy ball milling under cryogenic temperatures, namely cryomilling, of PANI with Fe nanoparticles. It takes 5 h to refine the Fe into an average grain size of 20 nm and to get homogeneously dispersed in PANI matrix. The obtained PANI/Fe nanocomposites have a maximum conductivity of 0.78 S cm^?1 after 2‐h cryomilling, whereas its coercivity increases monotonously with time in the range of experiment up to 10 h. It is found that the sizes of Fe particles have obvious effects on both electrical and magnetic properties. When compared with micrometer Fe particles as raw materials, Fe nanoparticles result in somewhat lower conductivity but a much higher coercivity exceeding 400 Oe. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 1571–1576, 2008     

低温球磨制备纳米晶Al-Zn-Mg-Cu合金

利用低温液氮球磨技术制备了Al-Zn-Mg-Cu合金纳米晶粉末,并采用X射线衍射(XRD)对材料在球磨过程中的晶粒尺寸和微观应变进行了研究,利用扫描电镜(SEM)、透射电镜(TEM)和差热分析(DSC)等测试方法研究了材料的固态相变以及热稳定性.研究表明,粉末晶粒尺寸随着球磨的进行逐渐减小,球磨10h后晶粒尺寸达到45nm;微观应变随着球磨的进行逐渐增大.粉末球磨过程中,MgZn2相逐渐减少,合金元素过饱和固溶于α-Al晶格之中.球磨10h后仅有少量的MgZn2相存在.制备的Al-Zn-Mg-Cu纳米晶粉末在低于709K下加热,粉末晶粒长大速度较慢,表明Al-Zn-Mg-Cu纳米晶粉末具有较高的热稳定性.     

液氮球磨制备Al-Zn-Mg-Cu纳米晶粉末及组织分析

利用液氮球磨技术制备了Al-Zn-Mg-Cu纳米合金粉末. 采用X射线衍射对材料在球磨过程中的固态相变、晶粒尺寸和微观应变进行了研究,利用金相显微镜和透射电镜观察了微观组织. 研究表明,随着球磨的进行,雾化粉末中的MgZn2第二相逐步减少,并最终完全超饱和固溶于α-Al之中. 低速(200 r·min-1)球磨10 h后仍有少部分粗晶存在于粉末心部;高速(400 r·min-1)球磨能够使粉末纳米晶粒更加均匀. 材料经过低速液氮球磨6 h以后平均晶粒大小稳定在45 nm,并保持到10 h不再变化;增加主轴转速到400 r·min-1继续球磨5 h后,粉末平均晶粒大小降到34 nm. 微观应变随着球磨进行呈现先增大后降低的趋势.     

Catalytic activity of novel thermoplastic/cellulose-Au nanocomposites prepared by cryomilling

Due to environmental concerns, increasing attention has been focused on the application and preparation of biobased polymers and their blends. In this study, cellulose, the most spread biopolymer on Earth, was used in the preparation of novel cotton/polypropylene-Au and cotton/polyethylene-Au nanocomposites via a green mechanochemical approach. First, mechanoradicals were generated by ball milling of the cotton and thermoplastics under cryo conditions, and then, these radicals were used in the reduction of Au ions to Au nanoparticles (Au NPs). Nanocomposites were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The application of mechanochemistry in obtaining the cotton/thermoplastic blends allowed homogenous and fine blending of the samples and in addition, excluded the usage of toxic solvents. Since Au NPs exhibit a wide range of applications, e.g., in catalysis, cotton/thermoplastic-Au nanocomposites were used to catalyze the reduction reaction of 4-nitrophenol to
4-aminophenol, followed by UV-Vis spectroscopy. Finally, the hydrophobicity of the nanocomposites was alternated by tuning the blend composition. In the prepared nanocomposites, cotton and thermoplastics acted as very good supporting matrices for the Au NPs and provided satisfactory access to the NPs.     

Consolidation of cryomilled Al–Si using spark plasma sintering

Cryomilled eutectic aluminum–12% silicon powder was sintered using spark plasma sintering (SPS) to create bulk compacts. The cryomilling serves to break up and disperse the eutectic phase in the powder to create a well-distributed Si phase throughout the matrix and to modify the morphology of the Si phase from plate-like to spherical, whilst refining the aluminium grain size to the nanometric level. The effects of different sintering times and temperatures using SPS on the densification of the powder, the aluminium grain size evolution, the growth of the Si phase and the morphology change of the Si phase were investigated. The compacts were analysed using X-ray diffraction, scanning electron microscopy and optical microscopy. The initial stages of densification appear to be highly dependent on the yield strength of the powder. An estimate of the temperature gradient seen in the powder bed was made and calculated to be near 200?°C at the highest point. The Al and Si phase growth was investigated and it was observed that the Si coarsening rate is increased due to the increased volume of grain boundaries. As the Si coarsens, any pinning effect on the Al grains is lost, resulting in a highly unstable microstructure that coarsens rapidly.