Bulk nanocrystalline Al prepared by cryomilling

Bulk nanocrystalline Al was fabricated by mechanically milling at cryogenic temperature （cryomilling） and then by hot pressing in vacuum. By using X-ray diffraction （XRD）, scanning electron microscopy （SEM）, and transmission electron microscopy （TEM）, the microstructure evolution of the material during cryomilling and consolidation was investigated. With increasing the milling time, the grain size decreased sharply and reduced to 42 nm when cryomilled for 12 h. The grains had grown up, and the columnar grain was formed under the hot pressing and extrusion compared with the cryomilled powders. The grain size of as-extruded specimen was approximately 300-500 nm. The reason of high thermal stability of this bulk was attributed primarily to the Zener pinning from the grain boundary of the AlN arising from cryomilling and the solute drag of the impurity. Tensile tests show that the strength of nanocrystalline Al is enhanced with decreasing grain size. The ultimate tensile strength and tensile elongation were 173 MPa and 17.5%, respectively. It appears that the measured high strength in the cryomilled Al is related to a grain-size effect, dispersion strengthening, and dislocation strengthening.

Surface Passivation of Nanocrystalline Silicon Powder Derived from Cryomilling

The surface passivation mechanism of nanocrystalline silicon powder was studied. The liquid nitrogen/argon was used as the medium to prepare the nanocrystalline silicon powder, using a cryomilling technology. The X-ray diffraction, transmission electron microscopy, plasma emission spectroscopy and infrared spectrum were used to analyze the prepared samples, and density functional theory was used to investigate the cryomilling process. For nanocrystalline silicon powder cryomilled with liquid N2, the amorphous outer layer with N element is formed On the surface, and chemisorption caused by the formation of Si-N-Si bond leads to the surface passivation; although physisorpfion also he confirmed, the Si-N bond is steady after exploded in air for 30 days and no new bond is observed. For nanocrystalline silicon powder cryomilled with liquid At, no new chemical bond is Observed, Ar element absorbs on the surface of the prepared powder only through physisorption, and after exploded in air for 30 days, a Si-O bond can be observed obviously.

A high-Nb-TiAl alloy with ultrafine-grained structure fabricated by cryomilling and spark plasma sintering

In this work,an ultrafine-grained high-Nb-TiAl alloy with a nominal composition of Ti-45Al-8Nb-0.2W-0.2B(at%)was prepared by cryomilling and subsequent spark plasma sintering(SPS)technique.The chemical composition,particle size,morphology and crystallite size of cryomilled powder were studied.It is found that cryomilling can effectively reduce the particle size and enhance grain refinement.The ingots sintered at 900 and 1000℃ show an equiaxed near-γmicrostructure with grain sizes<700 nm,while the sample sintered at 1100℃exhibits duplex microstructure.Especially,the one sintered at 1000℃ has excellent mechanical properties,whose compression yield strength,fracture strength,bending strength and plastic strain achieve 1310,2174,578 MPa and 16.8%,respectively.The reasons for the effect of cryomilling and the mechanical behavior of sintered ingots were discussed.It is suggested that cryomilling in combination with SPS is an effective way to synthesize high-NbTiAl alloy with ultrafine-grained structure.

COMPARISON ON REFINEMENT OF IRON POWDER BY BALL MILLING ASSISTED BY DIFFERENT EXTERNAL FIELDS

The cryogenic milling and milling in conjunction with dielectric barrier discharge plasma (DBDP) have been separately set up. The combined effect of low temperature and plasma on ball milling has been investigated by examining the refinement of particle size and grain size of iron powder using scanning electron microscopy, X-ray diffraction, and small angle X-ray scattering. It was found that the mean size of iron particles could reach 104nm only after 10 hours of ball milling in conjunction with DBDP, whereas a minimum average grain size of 8.4nm was obtained by cryomilling at -20℃; however, it is difficult to refine the particle size and grain size under the same milling condition in the absence of DBDP and cryogenic temperature.

Overview of milling techniques for improving the solubility of poorly water-soluble drugs

Milling involves the application of mechanical energy to physically break down coarse particles to finer ones and is regarded as a“topedown”approach in the production of fine particles.Fine drug particulates are especially desired in formulations designed for parenteral,respiratory and transdermal use.Most drugs after crystallization may have to be comminuted and this physical transformation is required to various extents,often to enhance processability or solubility especially for drugs with limited aqueous solubility.The mechanisms by which milling enhances drug dissolution and solubility include alterations in the size,specific surface area and shape of the drug particles as well as millinginduced amorphization and/or structural disordering of the drug crystal(mechanochemical activation).Technology advancements in milling now enable the production of drug micro-and nano-particles on a commercial scale with relative ease.This review will provide a background on milling followed by the introduction of common milling techniques employed for the micronization and nanonization of drugs.Salient information contained in the cited examples are further extracted and summarized for ease of reference by researchers keen on employing these techniques for drug solubility and bioavailability enhancement.

Thermal stability of nanostructured NiCrC coating prepared by HVAF spraying of cryomilled powders

Thermal stability of nanostructured NiCrC coating prepared by high velocity air-fuel （HVAF） spraying of cryomilled feedstock powders was investigated. Transmission electron microscopy （TEM）, differential scanning calorimetry （DSC）, and X-ray diffraction （XRD） were utilized for characteristic analysis. Recrystallization and normal grain growth occur when isothermal treatment is performed at 923 K （0.55 TM） for up to 100 h, and the average grain size increases from initial 41 nm for as-deposited state to around 100 nm for nearly equilibrium state. Isochronal treatment at 823 K and 1023 K was also conducted for comparison. Accordingly, for 0.49 to 0.61 T/TM, the time exponent n deduced from D^1/n - D0^1/n = kt increases from 0.15 to 0.30. The observed high thermal stability is attributed primarily to a Zener pinning mechanism arising from the fine Cr2O3 dispersions and the solute drag effect as well.

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.