Search results for "Ball mill"
showing 10 items of 50 documents
Structural characterization and electrochemical hydrogen storage properties of Ti2LxZrxNi (x [ 0, 0.1, 0.2) alloys prepared by mechanical alloying
2013
International audience; Nominal Ti2Ni was synthesized under argon atmosphere at room temperature using a planetary high-energy ball mill. The effect of milling time and Zr substitution for Ti on the microstructure was characterized by XRD, SEM and TEM, and the discharge capacities of Ti2xZrxNi (x 1/4 0, 0.1, 0.2) were examined by electrochemical measurements at galvanostatic conditions. XRD analysis shows that amorphous phase of Ti2Ni can be elaborated by 60 h of milling, whereas Zr substitution hinders amorphization process of the system. The products of ball milling nominal Ti2xZrxNi (x 1/4 0.1, 0.2) were austenitic (Ti, Zr)Ni and partly TiO, despite the fact that the operation was carrie…
Mechanochemical Access to Defect-Stabilized Amorphous Calcium Carbonate
2018
Amorphous calcium carbonate (ACC) is an important precursor in the biomineralization of crystalline CaCO3. The lifetime of transient ACC in nature is regulated by an organic matrix, to use it as an intermediate storage buffer or as a permanent structural element. The relevance of ACC in material science is related to our understanding of CaCO3 crystallization pathways. ACC can be obtained by liquid–liquid phase separation, and it is typically stabilized with the help of macromolecules. We have prepared ACC by milling calcite in a planetary ball mill. The ball-milled amorphous calcium carbonate (BM-ACC) was stabilized with small amounts of Na2CO3. The addition of foreign ions in form of Na2C…
Correlation between ball milling conditions and planar effects on Cu-nanostructured powders
2002
It is most often proposed that the process of ball milling introduces a variety of defects (vacancies, dislocations, grain boundaries, stacking faults,...) which raise the free energy of the system making it possible to produce metastable phases. But there are very few investigations that deal with the characterization and quantification of the defects produced in milled powders. XRD is really a valuable technique for a characterization in terms of size and morphology of crystallites and imperfections. In this paper, a new line profile analysis method is proposed in order to take into account the dependence of the crystallite size, of the residual strains as well as of the planar defects, o…
Optimization of sample preparation conditions for detecting trace amounts of β-tegafur in α- and β-tegafur mixture.
2012
We report a semiquantitative method for determining trace amounts (<1%) of thermodynamically stable forms in polymorphic mixtures, focusing on sample preparation ef- fects on solid phase transitions. Tegafur (5-fluoro-1-(oxolan-2-yl)-1,2,3,4-tetrahydropyrimidine- 2,4-dione) was used as a model material in this study. The amounts of the thermodynamically stable $ tegafur were increased to levels detectable by powder X-ray diffractometry by grind- ing the samples in a ball mill in the presence of water. The limit of detection for this method was as low as 0.0005% of $ tegafur in " and $ tegafur mixtures. The amount of $ tegafur after sample preparation was found to be proportional to the init…
An experimental investigation on the poor hydrogen sorption properties of nano-structured LaNi5 prepared by ball-milling
2011
Abstract Nano-structured LaNi5 hydrogen storage materials prepared by ball-milling is analysed using differential scanning calorimetry (DSC) and x-ray photoelectron spectroscopy (XPS). DSC results indicate a partial elimination of defects at 500 °C in a more efficient way for the short-time ball-milled powders compared to the long-time ball-milled ones. XPS results show almost no change in the core-level electronic structure for La and Ni of LaNi5 in the bulk and the nano-structured forms, but gives an indication that the self-restoring mechanism of the active surface observed in the bulk sample (Siegmann et al. Phys. Rev. Lett. 40, 972) may not be occurring in the nano-powders. Results fro…
The mechanically activated combustion reaction in the Fe–Si system: in situ time-resolved synchrotron investigations
2002
Mechanical high-energy ball milling of Fe+2Si elemental powder mixtures was used to activate self sustaining combustion reaction in the case of iron disilicide synthesis. The reaction path as well as the influence of the microstructural parameters on phase transformation have been investigated in detail. Time-resolved X-ray diffraction (TRXRD) using the fast recording kinetics offered by the synchrotron radiation was coupled to an infrared camera in order to study the internal structure of the combustion wave. The crystallite size and the amount of mechanically induced phases play an important role during the combustion; the reaction path and the end product composition mainly depend on the…
Enhancement of self-sustaining reaction by mechanical activation: case of an FeSi system
1999
Mechanical high energy ball milling of an Fe2Si elemental powders mixture was used to activate a self sustaining combustion reaction or so-called self-propagating high-temperature synthesis (SHS) to form iron disilicide, a reaction for which the thermodynamic criterion is not favorable. A complete characterization of the milled powders before reaction was performed with energy dispersive X-ray spectrometry, specific surface measurements and X-ray diffraction profile analysis. Thermal and structural information describing the combustion front initiated by heating up a sample to 400°C in a Fe‐Si system is communicated. In order to isolate the phases involved in the gasless reaction, a time-re…
Controlling the Formation of Sodium/Black Phosphorus IntercalationCompounds Towards High Sodium Content
2021
The solid-state synthesis of pure sodium-black phosphorus intercalation compounds (Na-BPICs) has been optimized in bulk for two stoichiometric ratios. Specifically, in-situ X-Ray diffraction (XRD) allowed the precise identification of the optimal temperature range for the formation of Na-BPICs: 94°C–96°C. Moreover, as the undesired formation of Na3P takes place at this very same range, we succeeded in introducing a new synthetic route based on a fast-thermal ball milling implementation that results in the bulk production of BPIC without Na3P in 9 out of 10 cases. Finally, by combining XRD, Raman spectroscopy, and DFT calculations we developed a new structural model for Na-based BPICs showin…
Solid acid-catalyzed depolymerization of barley straw driven by ball milling
2015
This study describes a time and energy saving, solvent-free procedure for the conversion of lignocellulosic barley straw into reducing sugars by mechanocatalytical pretreatment. The catalytic conversion efficiency of several solid acids was tested which revealed oxalic acid dihydrate as a potential catalyst with high conversion rate. Samples were mechanically treated by ball milling and subsequently hydrolyzed at different temperatures. The parameters of the mechanical treatment were optimized in order to obtain sufficient amount of total reducing sugar (TRS) which was determined following the DNS assay. Additionally, capillary electrophoresis (CE) and Fourier transform infrared spectrometr…
Enhanced thermoelectric performance in the p-type half-Heusler (Ti/Zr/Hf)CoSb0.8Sn0.2 system via phase separation
2014
A novel approach for optimization of the thermoelectric properties of p-type Heusler compounds with a C1b structure was investigated. A successful recipe for achieving intrinsic phase separation in the n-type material based on the TiNiSn system is isoelectronic partial substitution of Ti with its heavier homologues Zr and Hf. We applied this concept to the p-type system MCoSb0.8Sn0.2 by a systematic investigation of samples with different compositions at the Ti position (M = Ti, Zr, Hf, Ti0.5Zr0.5, Zr0.5Hf0.5, and Ti0.5Hf0.5). We thus achieved an approximately 40% reduction of the thermal conductivity and a maximum figure of merit ZT of 0.9 at 700 °C. This is a 80% improvement in peak ZT fr…