Preparation and characterisation of composites from starch and sugar cane fibre

The aim of this study was to prepare and characterise composites of Soluble potato starch or hydroxypropylated maize starch with milled sugar cane fibre (i.e., bagasse). Prior to the preparation of the starch-fibre composites, the ‘cast’ and the ‘hot-pressed’ methods were investigated for the preparation of starch films in order to select the preferred preparation method. The physicochemical and mechanical properties of films conditioned at different relative humidities (RHs) were determined through moisture uptake, crystallinity, glass transition temperature (Tg), thermal properties, molecular structure and tensile tests. Hot-pressed starch films have ~5.5% less moisture, twice the crystallinity (~59%), higher Tg and Young’s modulus than cast starch films. The VH-type starch polymorph was observed to be present in the hot-pressed films. The addition of bagasse fibre to both starch types, prepared by hot-pressing, reduced the moisture uptake by up to 30% (cf., cast film) at 58% RH. The addition of 5 wt% fibre increased the tensile strength and Young’s modulus by 16% and 24% respectively. It significantly decreased the tensile strain by ~53%. Fourier Transform infrared (FT-IR) spectroscopy revealed differences in hydrogen bonding capacity between the films with fibre and those without fibre. The results have been explained on the basis of the intrinsic properties of starch and bagasse fibres.

3D-printing of highly uniform CaSiO3 ceramic scaffolds : preparation, characterization and in vivo osteogenesis

Calcium silicate (CaSiO3, CS) ceramics have received significant attention for application in bone regeneration due to their excellent in vitro apatite-mineralization ability; however, how to prepare porous CS scaffolds with a controllable pore structure for bone tissue engineering still remains a challenge. Conventional methods could not efficiently control the pore structure and mechanical strength of CS scaffolds, resulting in unstable in vivo osteogenesis. The aim of this study is to set out to solve these problems by applying a modified 3D-printing method to prepare highly uniform CS scaffolds with controllable pore structure and improved mechanical strength. The in vivo osteogenesis of the prepared 3D-printed CS scaffolds was further investigated by implanting them in the femur defects of rats. The results show that the CS scaffolds prepared by the modified 3D-printing method have uniform scaffold morphology. The pore size and pore structure of CS scaffolds can be efficiently adjusted. The compressive strength of 3D-printed CS scaffolds is around 120 times that of conventional polyurethane templated CS scaffolds. 3D-Printed CS scaffolds possess excellent apatite-mineralization ability in simulated body fluids. Micro-CT analysis has shown that 3D-printed CS scaffolds play an important role in assisting the regeneration of bone defects in vivo. The healing level of bone defects implanted by 3D-printed CS scaffolds is obviously higher than that of 3D-printed b-tricalcium phosphate (b-TCP) scaffolds at both 4 and 8 weeks. Hematoxylin and eosin (H&E) staining shows that 3D-printed CS scaffolds induce higher quality of the newly formed bone than 3D-printed b-TCP scaffolds. Immunohistochemical analyses have further shown that stronger expression of human type I collagen (COL1) and alkaline phosphate (ALP) in the bone matrix occurs in the 3D-printed CS scaffolds than in the 3D-printed b-TCP scaffolds. Considering these important advantages, such as controllable structure architecture, significant improvement in mechanical strength, excellent in vivo osteogenesis and since there is no need for second-time sintering, it is indicated that the prepared 3D-printed CS scaffolds are a promising material for application in bone regeneration.

Effect of preparation method of palygorskite-supported Fe and Ni catalysts on catalytic cracking of biomass tar

In this study, the effect of catalyst preparation and additive precursors on the catalytic decomposition of biomass using palygorskite-supported Fe and Ni catalysts was investigated. The catalysts were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). It is concluded that the most active additive precursor was Fe(NO3)3·9H2O. As for the catalyst preparation method, co-precipitation had superiority over incipient wetness impregnation at low Fe loadings.

Preparation and characterization of tin oxide nanowires on SiC

Interest in nanowires of metal oxide oxides has been exponentially growing in the last years, due to the attracting potential of application in electronic, optical and sensor field. We have focused our attention on the sensing properties of semiconducting nanowires as conductometric and optical gas sensors. Single crystal tin dioxide nanostructures were synthesized to explore and study their capability in form of multi-nanowires sensors. The nanowires of SnO2 have been used to produce a novel gas sensor based on Pt/oxide/SiC structure and operating as Schottky diode. For the first time, a reactive oxide layer in this device has been replaced by SnO2 nanowires. Proposed sensor has maintained the advantageous properties of known SiC- based MOS devices, that can be employed for the monitoring of gases (hydrogen and hydrocarbons) emitted by industrial combustion processes.

Preparation of metal-TCNQ charge-transfer complexes on conducting and insulating surfaces by photocrystallization

A generic method for the synthesis of metal-7,7,8,8-tetracyanoquinodimethane (TCNQ) charge-transfer complexes on both conducting and nonconducting substrates is achieved by photoexcitation of TCNQ in acetonitrile in the presence of a sacrificial electron donor and the relevant metal cation. The photochemical reaction leads to reduction of TCNQ to the TCNQ- monoanion. In the presence of Mx+(MeCN), reaction with TCNQ-(MeCN) leads to deposition of Mx+[TCNQ]x crystals onto a solid substrate with morphologies that are dependent on the metal cation. Thus, CuTCNQ phase I photocrystallizes as uniform microrods, KTCNQ as microrods with a random size distribution, AgTCNQ as very long nanowires up to 30 μm in length and with diameters of less than 180 nm, and Co[TCNQ]2(H2O)2 as nanorods and wires. The described charge-transfer complexes have been characterized by optical and scanning electron microscopy and IR and Raman spectroscopy. The CuTCNQ and AgTCNQ complexes are of particular interest for use in memory storage and switching devices. In principle, this simple technique can be employed to generate all classes of metal−TCNQ complexes and opens up the possibility to pattern them in a controlled manner on any type of substrate.

Preparation and characterization of composites from starch with sugarcane bagasse nanofibres

This paper reports on the results of using unbleached sugar cane bagasse nanofibres (average diameter 26.5 nm; aspect ratio 247 assuming a dry fibre density of 1,500 kg/m3) to improve the physico-chemical properties of starch-based films. The addition of bagasse nanofibres (2.5 to 20 wt%) to modified potato starch (i.e. soluble starch) reduced the moisture uptake by up to 17 % at 58 % relative humidity. The film’s tensile strength and Young’s modulus increased by up to 100 % (3.1 to 6.2 MPa) and 300 % (66.3 to 198.3 MPa) respectively with 10 and 20 wt% fibre addition. However, the strain at yield dropped by 50 % for the film containing 10 wt% fibre. Models for composite materials were used to account for the strong interactions between the nanofibres and the starch matrix. The storage and loss moduli as well as the glass transition temperature (Tg) obtained from dynamic mechanical thermal analysis, were increased with the starch-nanofibre films indicating decreased starch chain mobility due to the interacting effect of the nanofibres. Evidence of the existence of strong interactions between the starch matrix and the nanofibres was revealed from detailed Fourier transform infra-red and scanning electron microscopic evaluation.

Preparation, characterization of surfactants modified clay minerals and nitrate adsorption

Organic surfactants modified clay minerals are usually used as adsorbents for hydrophobic organic contaminants remediation; this work however has shown organoclays can also work as adsorbents for hydrophilic anionic contaminant immobilization. Organoclays were prepared based on halloysite, kaolinite and bentonite and used for nitrate adsorption, which are significant for providing mechanism for the adsorption of anionic contaminants from waste water. XRD was used to characterize unmodified and surfactants modified clay minerals. Thermogravimetric analysis (TG) was used to determine the thermal stability and actual loading of surfactant molecules. Ion chromatography (IC) was used to determine changes of nitrate concentration before and after adsorption by these organoclays. These organoclays showed different removal capacities for anionic ions from water and adsorption mechanism was investigated.

A thermal expulsion approach to homogeneous large-volume methacrylate monolith preparation; enabling large-scale rapid purification of biomolecules

Numerous efforts have been dedicated to the synthesis of large-volume methacrylate monoliths for large-scale biomolecules purification but most were obstructed by the enormous release of exotherms during preparation, thereby introducing structural heterogeneity in the monolith pore system. A significant radial temperature gradient develops along the monolith thickness, reaching a terminal temperature that supersedes the maximum temperature required for structurally homogenous monoliths preparation. The enormous heat build-up is perceived to encompass the heat associated with initiator decomposition and the heat released from free radical-monomer and monomer-monomer interactions. The heat resulting from the initiator decomposition was expelled along with some gaseous fumes before commencing polymerization in a gradual addition fashion. Characteristics of 80 mL monolith prepared using this technique was compared with that of a similar monolith synthesized in a bulk polymerization mode. An extra similarity in the radial temperature profiles was observed for the monolith synthesized via the heat expulsion technique. A maximum radial temperature gradient of only 4.3°C was recorded at the center and 2.1°C at the monolith peripheral for the combined heat expulsion and gradual addition technique. The comparable radial temperature distributions obtained birthed identical pore size distributions at different radial points along the monolith thickness.

Preparation of macroporous methacrylate monolithic material with convective flow properties for bioseparation : Investigating the kinetics of pore formation and hydrodynamic performance

The preparation of macroporous methacrylate monolithic material with controlled pore structures can be carried out in an unstirred mould through careful and precise control of the polymerisation kinetics and parameters. Contemporary synthesis conditions of methacrylate monolithic polymers are based on existing polymerisation schemes without an in-depth understanding of the dynamics of pore structure and formation. This leads to poor performance in polymer usage thereby affecting final product recovery and purity, retention time, productivity and process economics. The unique porosity of methacrylate monolithic polymer which propels its usage in many industrial applications can be controlled easily during its preparation. Control of the kinetics of the overall process through changes in reaction time, temperature and overall composition such as cross-linker and initiator contents allow the fine tuning of the macroporous structure and provide an understanding of the mechanism of pore formation within the unstirred mould. The significant effect of temperature of the reaction kinetics serves as an effectual means to control and optimise the pore structure and allows the preparation of polymers with different pore size distributions from the same composition of the polymerisation mixture. Increasing the concentration of the cross-linking monomer affects the composition of the final monoliths and also decreases the average pore size as a result of pre-mature formation of highly cross-linked globules with a reduced propensity to coalesce. The choice and concentration of porogen solvent is also imperative. Different porogens and porogen mixtures present different pore structure output. Example, larger pores are obtained in a poor solvent due to early phase separation.

Preparation of lamellar and hexagonal forms of mesoporous silica and zirconiaby the neutral amine route: lamellar-hexagonal transformation in the solid state

The chain length of the surfactant and the solvent composition are two of the factors that determine whether the lamellar or the hexagonal form of mesoporous SiO2 (or ZrO2) is formed by the neutral amine route; a lamellar-hexagonal transformation occurs on removal of the amine from the former.