A series of silicon containing poly(ester imide)s [PEIs] were synthesized using novel vinyl silane diester anhydride (VSEA)
and various aromatic and aliphatic dimines by two-step process includes ring-opening polyaddition reaction to form poly(amic
acid) and thermal cyclo-dehydration process to obtain poly(ester imide)s. VSEA was synthesized by using dichloro methylvinylsilane
and trimellitic anhydride in the presence of K2CO3 by nucleophilic substitution reaction. The PEIs were characterized by FTIR spectroscopy. The thermal properties of PEIs were
investigated by using differential scanning calorimetry (DSC) and thermogravimetric analysis (TG) methods. The prepared PEIs
showed glass transition temperatures in the range of 320–350°C and their 5% mass loss was recorded in the temperature range
of 500–520°C in nitrogen atmosphere. These had char yield in the range of 45–55% at 800°C.
A nanostructured mesoporous MCM-41 supported N-heterocyclic carbene–Pd (NHC–Pd) complex was prepared through the reaction of an ionic liquid immobilized onto MCM-41 with palladium acetate. The MCM-41-supported NHC–Pd complex could serve as a highly effective catalyst for the Suzuki cross-coupling reaction under aqueous conditions. Furthermore, the Pd(II) catalyst was recovered by a simple filtration from the reaction mixture and reused without a significant loss of its catalytic activity. The heterogeneous catalyst was also air-stable and thermally stable to allow its easy use.
The reinforcement of nano-barium titanate in ferrite filled poly-ether-ether-ketone (PEEK) composites caused a shift in the
decomposition temperature, at which maximum mass loss occurred, to higher side and enhancement in char yield in thermogravimetric
analysis. Loss tangent and glass transition temperature of ferrite filled PEEK composites were also found to be increased
with the reinforcement of nano barium titanate. The effect of nano barium titanate on the melting behaviour of ferrite filled
PEEK composites was negligible.
The concentration of radioactive226Ra,232Th and40K in building and ceramic materials of Bangladesh was investigated by γ-spectrometry with two HPGe detectors. Radium equivalent
activities, representative level index values, criterion formula, emanation coefficients and222Rn mass exhalation rates were estimated for the radiation hazard of the natural radioactivity in the materials. The activity
concentrations of the natural radionuclides, radium equivalent activities, emanation coefficients and222Rn mass exhalation rates are compared with the corresponding values for building and ceramic materials of different countries.
The radium equivalent activities in the samples varied between 30.9 (mosaic stone) and 328.0 Bq·kg−1 (gypsum). The emanation coefficient of the materials ranged from 7.83 (cement) to 33.0% (soil) and the222Rn mass exhalation rate ranged from 2.31 (stone chips) to 118.0 μBq·kg−1·s−1 (gypsum).
In this paper we present our recent positron annihilation study of the liquid»solid phase boundary for CO2 confined in nanometer pores of VYCOR glass. We find that CO2 remains liquid in the pores far below the bulk freezing temperature and there is pronounced hysteresis between freezing and melting compared to that seen at the gas-liquid boundary in the pores. On freezing we see evidence of open space created in the pores. This leads to complex melting behaviour possibly involving the formation of gas-liquid interfaces. We see that frezing in the pores is totally irreversible, so that any solid which forms (no matter how small) remains stable up to the higher melting temperature. In contrast melting is more reversible (possibly indicating nucleation centres which permit immediate re-freezing). Finally, the pre-frozen state in the pores is different to the post-melted state.
Polyimides have aromatic moieties in the backbone structure which are responsible for their increased thermal stability. If
phosphorus is introduced in the main chain structure of polyimides, there is further improvement in the thermal stability.
This has been proved by the work carried out in our group. The polyimide having amine termination can be used for crosslinking
of epoxy resins.
In the present study amine terminated phosphorus containing nadicimide were taken as curing agent for DGEBA resins. The curing
characteristics of DGEBA resin were studied by DSC using different amounts of nadic endcapped phosphorylated amines. DSC thermogram
showed the heat of polymerization was lower as compared to system cured with aromatic amines.
The phase behaviour of carbon dioxide confined in VYCOR glass at pressures below that of the bulk triple point (0.51 MPa) has been investigated. The temperature at which freezing occurs appears to be pressure dependent below 0.3 MPa. As experiments are performed at successively lower pressures, the confined phase transitions gradually disappear, due to either partial pore filling, or the proximity of the confined triple point.
In confined (nanometer-scale) geometry, the effects of substrate forces and finite size produce a shift of the gas liquid phase boundary from that found in corresponding bulk. The pore transitions also show marked hysteresis. The phase behaviour of a binary gas mixture in confined geometry is likely to depend on the miscibility of the system and the interaction between the substrate and the individual fluid molecules/atoms. Here, we present the results of a pilot positronium annihilation study of the condensation and evaporation of argon-nitrogen mixtures confined in 4 nm diameter cylindrical pores in VYCOR glass.
Positron lifetime spectroscopy has been applied to estimate the free-volume hole size distribution in glassy polycarbonate (PC) and polystyrene (PS) as well as in plastically deformed and undeformed, semi-crystalline polyethylene (HDPE). The hole radius density distribution is determined from the ortho-positronium lifetime distribution which is obtained via a Laplace-inversion of the positron lifetime spectrum. The hole volume density distribution and the number density distribution of holes is estimated from the hole radius density distribution. In PC and in PS all of the distributions may be well approximated by a single Gaussian. The hole radius and the hole number density distributions have centres <r> and <vn> at 0.29 nm and 0.1 nm3 in PC, and at 0.28 nm and 0.09 nm3 in PS. The FWHM of the corresponding distributions are 0.042 nm and 0.040 nm3 (PC), and 0.039 nm and 0.34 nm3 (PS), respectively. Both, the shape and the width of the distributions correlate well with the free volume theory of BUECHE. In PE the lifetime spectra consist of four components. The o-Ps lifetime distribution is bimodal and may be attributed to o-Ps annihilation in the crystalline and in the amorphous phase of the polymer. The corresponding hole size distributions show definite changes of their position and width following plastic deformation which we attribute to homogeneous crystal lattice dilatation and/or a local disorder in the crystals and to an increase in the eccentricity of holes in the amorphous phase.
In this paper we present a brief review of the current state of positron annihilation research into the phase behaviour of fluids confined within restricted boundaries. We summarise, in the form of selected examples, the work done so far on: (1) fluids confined in the nanometer-size pores of VYCOR glass, with particular emphasis on the confined phase diagram and the mechanisms behind phase transitions compared to bulk. (2) The adsorption/physisorption of gases on internal surfaces of grafoil and the potential of positron technique for revealing physical properties, such as the intricate molecular arrangements during phase transitions of the layered fluid.