液氮球磨制备纳米SiCp/Al基复合材料的研究

利用液氮球磨技术制备了纳米SiC颗粒增强铝基复合材料粉末,对该纳米粉末进行真空热压和热挤压,获得纳米铝基复合材料块体.采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)研究了纳米SiC粉和Al-Zn-Mg-Cu粉在液氮球磨过程中形貌、组织和相组成等.结果表明,液氮球磨可以使复合材料粉末达到纳米级,且纳米SiC可均匀地分布于铝合金中.     

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.     

Effect of cryomilling on the thermal behaviors of poly(ethylene terephthalate)

We have studied the effect of cryomilling (high‐energy ball milling under cryogenic temperature) on the thermal behaviors of poly(ethylene terephthalate) (PET) by comparing with original PET and quenched PET. Cryomilling induced the amorphization of crystalline PET, but the thermal behaviors of amorphous PET obtained from cryomilling are significantly different to those of amorphous PET obtained from quenching. Unlike amorphous PET obtained from quenching, the heating curve of amorphous PET obtained from cryomilling shows no cold crystallization peak, but evidences are found that its cold crystallization occurs within a wide temperature range. In addition, the stability of amorphous PET obtained from cryomilling is higher than that of amorphous PET obtained from quenching. The difference is proved to be attributed to the stored energy in cryomilled PET. The hot crystallization behaviors of PET improve a lot after cryomilling, and the heat stability of cryomilled PET is also better than those of original PET during reheating. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

Cryomilling-induced solid dispersion of poor glass forming/poorly water-soluble mefenamic acid with polyvinylpyrrolidone K12

The effect of mechanical impact on the polymorphic transformation of mefenamic acid (MFA) and the formation of a solid dispersion of mefenamic acid, a poor glass forming/poorly-water soluble compound, with polyvinylpyrrolidone (PVP) K12 was investigated. The implication of solid dispersion formation on solubility enhancement of MFA, prepared by cryomilling, was investigated. Solid state characterization was conducted using powder X-ray diffraction (PXRD) and Fourier-transform infrared (FTIR) spectroscopy combined with crystal structure analysis. Apparent solubility of the mixtures in pH 7.4 buffer was measured. A calculation to compare the powder patterns and FTIR spectra of solid dispersions with the corresponding physical mixtures was conducted. Solid state characterization showed that (1) MFA I transformed to MFA II when pure MFA I was cryogenically milled (CM); and (2) MFA forms a solid dispersion when MFA was cryogenically milled with PVP K12. FTIR spectral analysis showed that hydrogen bonding facilitated by mechanical impact played a major role in forming solid dispersions. The apparent solubility of MFA was significantly improved by making a solid dispersion with PVP K12 via cryomilling. This study highlights the importance of cryomilling with a good hydrogen bond forming excipient as a technique to prepare solid dispersion, especially when a compound shows a poor glass forming ability and therefore, is not easy to form amorphous forms by conventional method.     

Abs/iron nanocomposites prepared by cryomilling

Acrylonitrile‐Butadiene‐Styrene (ABS)/iron nanocomposites have been prepared by cryomilling (high‐energy ball milling under cryogenic temperature), and a microstructure of iron network in ABS matrix was obtained. The blending scale and homogenization of ABS/iron nanocomposites are observed by Atomic Force Microscope (AFM). The morphology and structure of cryomilled composite powders are characterized by means of Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), and X‐ray Diffraction (XRD). The results indicate that upon cryomilling for 20 h, ABS and Fe are intimately blended with the single composite particle size less than 100 nm, the Fe phase domains less than 50 nm, and Fe grain size reduced to 20 nm. Both the fast rate of homogenization and size reduction are mainly attributed to the introduction of cryogenic temperature and comilling. The evidences suggest that cryomilling is a capable and promising technique for the production of polymer/metal nanocomposites. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 501–505, 2006     

Engineering of Injectable Antibiotic-laden Fibrous Microparticles Gelatin Methacryloyl Hydrogel for Endodontic Infection Ablation

This study aimed at engineering cytocompatible and injectable antibiotic-laden fibrous microparticles gelatin methacryloyl (GelMA) hydrogels for endodontic infection ablation. Clindamycin (CLIN) or metronidazole (MET) was added to a polymer solution and electrospun into fibrous mats, which were processed via cryomilling to obtain CLIN- or MET-laden fibrous microparticles. Then, GelMA was modified with CLIN- or MET-laden microparticles or by using equal amounts of each set of fibrous microparticles. Morphological characterization of electrospun fibers and cryomilled particles was performed via scanning electron microscopy (SEM). The experimental hydrogels were further examined for swelling, degradation, and toxicity to dental stem cells, as well as antimicrobial action against endodontic pathogens (agar diffusion) and biofilm inhibition, evaluated both quantitatively (CFU/mL) and qualitatively via confocal laser scanning microscopy (CLSM) and SEM. Data were analyzed using ANOVA and Tukey’s test (α = 0.05). The modification of GelMA with antibiotic-laden fibrous microparticles increased the hydrogel swelling ratio and degradation rate. Cell viability was slightly reduced, although without any significant toxicity (cell viability > 50%). All hydrogels containing antibiotic-laden fibrous microparticles displayed antibiofilm effects, with the dentin substrate showing nearly complete elimination of viable bacteria. Altogether, our findings suggest that the engineered injectable antibiotic-laden fibrous microparticles hydrogels hold clinical prospects for endodontic infection ablation.     

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 us-ing 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 ap-proached 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 90vo1% of the powders satisfied the requirement for thermal spraying with the particle dimension of 10-50 grn,and most of the powders exhibited spherical morphology,which were expected to have good fluidity during thermal spraying.The Cr2O3 phase formed during the cryomilling 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.     

块体纳米晶Al-Zn-Mg-Cu合金的热处理

利用液氮球磨、真空热压和挤压工艺制备块体纳米晶Al-Zn-Mg-Cu合金,并对其固溶和时效处理进行研究,得到时效硬度曲线。利用X射线衍射仪和透射电镜对该合金热处理前后的微观组织进行分析,结果表明:块体制备过程中析出的MgZn2可以通过固溶处理使其回溶并在时效后沉淀析出;热压后晶粒尺寸为50~100 nm,热处理后晶粒长大到100 nm,部分晶粒达到200 nm。     

Nanostrucmred A1-Zn-Mg-Cu alloy synthesized by cryomilling and spark plasma sintering

Nanocrystallized Al-10.0%Zn-3.0%Mg-1.8%Cu (mass fraction) alloy powder was prepared by cryomilling, and then the nanostructured powder was consolidated into bulk material by spark plasma sintering (SPS). The microstructural evolution and phase transformation were studied. A supersaturated face-centered cubic solid solution is formed after cryomilling for 10 h, and the average grain size is 28 nm. Two typical nanostructures of the bulk nanostructured alloy are observed: primarily equiaxed grains with size of 150 nm, and occasionally occurring sub-micron grains up to 500 nm. Two types of MgZn₂ particles precipitate during consolidation. One is the sub-micron particles distributed along the boundaries of the powders, and the other is fine particles with size of several nanometers in the matrix, especially at the boundaries of sub-micron grains. These second phase particles can be completely dissolved into matrix by proper solid solution treatment.     

Comparison of AC to DC current sources for field-assisted sintering of aluminum alloy 5083 powder

The viability of resistively sintering aluminum 5083 powder with an alternating current (AC) was explored under both as-atomized and cryomilled conditions. Samples were processed under an AC field and a direct current (DC) field. Samples processed by both methods exhibited similar microstructures and densities at different die wall temperatures. For as-atomized powders, similar densities (99% of theoretical [TD]) were achieved at die wall temperatures of 564°C under DC fields and 525°C under AC fields. For cryomilled 5083, densities up to 90% of theoretical were achieved at 550°C under DC fields, while density values 99% of TD were achieved at 500°C under AC fields. Based on these findings, it has been determined that AC fields can be used as an alternative to SPS for achieving optimal density.