Focused ion beam milling of carbon nanotube yarns and bucky-papers : correlating their internal structure with their macro-properties

Focused ion beam (FIB) milling through carbon nanotube (CNT) yarns and bucky-papers followed by scanning electron microscopy has recently emerged as a powerful tool for eliciting details of their internal structure. The internal arrangement of CNTs in bucky-papers and yarns directly affects their performance and characteristics. Consequently this information is critical for further optimisation of these structures and to tailor their properties for specific applications. This chapter describes in detail FIB milling of CNT yarns and bucky-papers and gives a range of examples where FIB milling has enabled a better understanding of how processing conditions and treatments affect the internal structure. Emphasis is placed on how FIB milling elucidates the influence of fabrication conditions on the internal arrangement of CNTs and how this influences the material's macroscopic properties.

Stable anode performance of an Sb–carbon nanocomposite in lithium-ion batteries and the effect of ball milling mode in the course of its preparation

Materials that alloy with lithium (Si, Ge, Sn, Sb, and P) are considered as alternatives to graphitic anodes in lithium-ion batteries. Their practical use is precluded by large volume changes (200–370%) during cycling. Embedding nanoparticles into carbon is being investigated as a way to tackle that, and ball milling is emerging as a technique to prepare nanocomposites with enhanced capacity and cyclic stability. Using Sb as a model system, we investigate the preparation of Sb–carbon nanocomposites using a reconfigurable ball mill. Four distinctive milling modes are compared. The structure of the composites varies depending on the mode. Frequent strong ball impacts are required for the optimal electrochemical performance of the nanocomposite. An outstanding stable capacity of 550 mA h g−1 for 250 cycles at a current rate of 230 mA g−1 is demonstrated in a thin electrode (1 mg cm−2) and a capacity of [similar]400 mA h g−1 can be retained at 1.15 A g−1. Some capacity fade is observed in a thicker electrode (2.5 mg cm−2), i.e. the performance is sensitive to mass loading. The electrochemical stability originates from the nanocomposite structure containing Sb nanoparticles (5–15 nm) dispersed in a carbon component.

Electrochemical performance of LiFe1-xMnxPO4/C materials prepared by ball milling

LiFe1-xMnxPO4/C composite materials as cathode materials in Li-ion batteries have been synthesised and their electrochemical properties have been investigated. The samples were synthesised by using high energy ball milling of commercially available precursors (Li2C2O4, FeC2O4.2H2O, MnC2O4.2H2O, NH4H2PO4) and then heated at 600°C. The morphology and structure of the heated samples were analysed by means of SEM and X-ray diffraction. The olivine structure of the LiFe1-xMnxPO4/C composite was obtained. A slight shift of the peaks to smaller 2θ angles with the increasing Mn/Fe ratios is observed due to the increase in lattice parameters. The influence of different Mn/Fe ratios on electrical and electrochemical performances were studied by charge-discharge and cyclic voltammetry (CV) testing. The CV curves of the pure LiFePO4 and LiMnPO4 show the expected Fe2+/Fe3+ peak around 3·5 V and Mn2+/Mn3+ peak around 4·1 V, respectively. The addition of manganese increases the discharge voltage from 3·5 to 4·1 V.

A preliminary assessment of machinability of titanium alloy Ti 6Al 4V during thin wall machining using trochoidal milling

Titanium alloys are of great demand in the aerospace and biomedical industries. Most the titanium products are either cast or sintered to required shape and finish machined to get the appropriate surface texture to meet the design requirements. Ti-6Al-4V is often referred as work horse among the titanium alloys due to its heavy use in the aerospace industry. This paper is an attempt to investigate and improve the machining performance of Ti-6Al-4V. Thin wall machining is an advance machining technique especially used in machining turbine blades which can be done both in a conventional way and using a special technique known as trochoidal milling. The experimental design consists of conducting trials using combination of cutting parameters such as cutting speed (vc), 90 and 120 m/min; feed/tooth (fz) of 0.25 and 0.35 mm/min; step over (ae) 0.3 and 0.2; at constant depth of cut (ap) 20mm and using coolant. A preliminary assessment of machinability of Ti-6Al-4V during thin wall machining using trochoidal milling is done. A correlation established using cutting force, surface texture and dimensional accuracy.

Enhanced lithium storage in ZnFe2O4-C nanocomposite produced by a low-energy ball milling

Preparation of novel nanocomposite structure of ZnFe2O4-C is achieved by combining a sol-gel and a low energy ball milling method. The crucial feature of the composite's structure is that sol-gel synthesised ZnFe2O4 nanoparticles are dispersed and attached uniformly along the chains of Super P Li™ carbon black matrix by adopting a low energy ball milling. The composite ZnFe2O4-C electrodes are capable of delivering a very stable reversible capacity of 681 mAh g-1 (96% retention of the calculated theoretical capacity of ∼710 mAh g-1) at 0.1 C after 100 cycles with a remarkable Coulombic efficiency (82%) improvement in the first cycle. The rate capability of the composite is significantly improved and obtained capacity was as high as 702 at 0.1, 648 at 0.5, 582 at 1, 547 at 2 and 469 mAh g-1 at 4 C (2.85 A g-1), respectively. When cell is returned to 0.1 C, the capacity recovery was still ∼98%. Overall, the electrochemical performance (in terms of cycling stability, high rate capability, and capacity retention) is outstanding and much better than those of the related reported works. Therefore, our smart electrode design enables ZnFe2O4-C sample to be a high quality anode material for lithium-ion batteries.

Preparation of composite electrodes with carbon nanotubes for lithium-ion batteries by low-energy ball milling

Some of the prospective electrode materials for lithium-ion batteries are known to have electronic transport limitations preventing them from being used in the electrodes directly. In many cases, however, these materials may become practical if they are applied in the form of nanocomposites with a carbon component, e.g. via incorporating nanoparticles of the phase of interest into a conducting network of carbon nanotubes. A simple way to prepare oxide-carbon nanotube composites suitable for the electrodes of lithium-ion batteries is presented in this paper. The method is based on low-energy ball milling. An electrochemically active but insulating phase of LiFeTiO4 is used as a test material. It is demonstrated that the LiFeTiO4-carbon nanotube composite is not only capable of having significantly higher capacity (∼105-120 mA h g-1vs. the capacity of ∼65-70 mA h g -1 for the LiFeTiO4 nanoparticles) at a slow current rate but may also operate at reasonably high current rates. © the Partner Organisations 2014.

Structure and characteristics of milled silk particles

This study examined the structure, thermal property, and ion adsorption of silk particles. The particles were prepared by attritor-bead mill combination, using alkaline (pH10) charge repulsion and surfactant steric repulsion methods. Both methods produced particles with a dominant β-sheet structure, similar to the silk fibre. There was no significant difference in the decomposition temperatures for either the silk fibre or the micro/nano silk particles. An important finding from this study is clear evidence of reduction of amorphous content during the final stage of powdering using the bead mill. As a result, despite reduction in β-sheet crystallites with the progressive milling, the relative β-sheet content actually increased during this process. However, intermolecular forces between the β-sheets reduced significantly and hence the XRD results showed significant reduction in crystallinity in nano silk particles but crystal forming segments remained with β-sheet conformations after milling. The structural change influenced the ion-adsorption property where particle-size reduction resulted in a significant increase in both the rate and volume of HCrO4- adsorption. © 2014 Elsevier B.V.

Optimization of milling parameters on the synthesis of stearic acid coated CaCO3 nanoparticles

Surface modification of precipitated calcium carbonate particles (calcite) in a planetary ball mill using stearic acid as a modification agent for making dispersion in hydrocarbon oil was investigated. Different parameters for processing (milling) such as milling time, ball-to-sample ratio, and molar ratio of the reactant were varied and analyzed for optimization. The physical properties of the hydrophobically modified calcium carbonate particles were measured; the particle size and morphology of the resulting samples were characterized by transmission electron microscopy and X-ray diffraction. The surface coating thickness was estimated using small angle X-ray scattering. © 2014 American Coatings Association & Oil and Colour Chemists' Association.

High-efficient production of boron nitride nanosheets via an optimized ball milling process for lubrication in oil

Although tailored wet ball milling can be an efficient method to produce a large quantity of two-dimensional nanomaterials, such as boron nitride (BN) nanosheets, milling parameters including milling speed, ball-to-powder ratio, milling ball size and milling agent, are important for optimization of exfoliation efficiency and production yield. In this report, we systematically investigate the effects of different milling parameters on the production of BN nanosheets with benzyl benzoate being used as the milling agent. It is found that small balls of 0.1-0.2 mm in diameter are much more effective in exfoliating BN particles to BN nanosheets. Under the optimum condition, the production yield can be as high as 13.8% and the BN nanosheets are 0.5-1.5 μm in diameter and a few nanometers thick and of relative high crystallinity and chemical purity. The lubrication properties of the BN nanosheets in base oil have also been studied. The tribological tests show that the BN nanosheets can greatly reduce the friction coefficient and wear scar diameter of the base oil.

Preparation of cellulose nanofiber from softwood pulp by ball milling

This paper reports the possibility of producing cellulose nanofiber from softwood pulp using a simple ball milling technique under ambient pressure and at room temperature. The effects of milling conditions including the ball-to-cellulose mass ratio, milling time, ball size and alkaline pretreatment were investigated. It was found that milling-ball size should be carefully selected for producing fibrous morphologies instead of particulates. Milling time and ball-to-cellulose mass ratio were also found important to control the fiber morphology. Alkali pre-treatment helped in weakening hydrogen bonds between cellulose fibrils and removing small particles, but with the risks of damaging the fibrous morphology. In a typical run, cellulose nanofiber with an average diameter of 100 nm was obtained using soft mechanical milling conditions using cerium-doped zirconia balls of 0.4–0.6 mm in diameter within 1.5 h without alkaline pretreatment.

Compressibility of a Ti-based alloy with varying amounts of surfactant prepared by high-energy ball milling

The combined effects of varying amounts of surfactant (ethylene bis-stearamide; EBS) and milling time on the compressibility of ball-milled Ti-10Nb-3Mo (wt.%) alloy were investigated. Ball milling process was performed on the elemental powders with different amounts of EBS (0-3. wt.%) for 5 and 10. h, and the ball-milled powders were consolidated by a uniaxial cold pressing in the range of 500-1100. MPa. Results indicated that the addition of surfactant in ball milling process lead to significant changes in particle packing density. The relative density was higher for powders ball milled with larger amounts of EBS and for the shorter milling time. The compressibility of powders was examined by the compaction equation developed by Panelli and Ambrosio Filho. The densification parameter (A) increased with the increasing amount of EBS, and decreased with increasing milling time.

Effects of milling time on powder packing characteristics and compressive mechanical properties of sintered Ti-10Nb-3Mo alloy

The influence of milling time on the powder packing characteristics and compressive mechanical properties of a biomedical Ti-10Nb-3Mo alloy (wt.%) was investigated. Ball milling was performed on elemental metal powders at different milling times of 0 (blended), 2, 4, 6, 8, and 10 h. This article demonstrates that despite the beneficial effects of ball milling technique in the mechanical alloying of the Ti-based alloy, the ball-milled powders synthesized at longer milling times can adversely affect the packing density and significantly diminish the compressive mechanical properties of the sintered powders. Crown

Gradient structure produced by three roll planetary milling: numerical simulation and microstructural observations

In this study a gradient grain structure was produced by processing rod billets through three roll planetary milling (also known as PSW process). This kind of gradient structure is reported to provide an excellent combination of strength and ductility owing to an ultrafine-grained surface layer and a coarse-grained interior of the billet. Specifically, copper rod samples were subjected to up to six passes of PSW at room temperature. To study the evolution of the microstructure during the deformation, microhardness measurements and Electron Backscatter Diffraction (EBSD) analysis were performed after one, three and six passes. Additionally, the distributions of the equivalent stress during PSW and the equivalent strain after processing were studied by finite element analysis using the commercial software QFORM. The results showed the efficacy of PSW as a means of imparting a gradient ultrafine-grained structure to copper rods. A good correlation between the simulated equivalent strain distribution and the measured microhardness distribution was demonstrated.

One-hit machining of titanium alloy (Ti-6al-4v) wall component with trochoidal milling

This research will definitely give guidelines to industries associated with titanium slot machining.