Measuring interdiffusion at an interface between two elastomers with tapping-mode and contact-resonance atomic force microscopy imaging

Despite the common use of tapping-mode atomic force microscopy to image composites or polymer blends, very few studies have focused on the measurement of the interdiffusion at an interface between two polymers in contact. In this study, we show how to assess the interphase between two polymers with two methods. First, stable and robust tapping conditions are established, and the problem of the phase contrast is discussed. Second, a contact-resonance method is presented: the tip in contact with the sample is electrostatically excited at its resonance frequency by a self-controlled oscillator. The gain and frequency images allow us to measure the interdiffusion width. Both methods (using high and weak mechanical solicitation) give the same assessment of the interdiffusion width. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and thermomechanical characterization of polyurethane elastomers extended with α,ω‐alkane diols

A series of polyurethane (PU) elastomers was prepared by the reaction of poly(?‐caprolactone) and 4,4′‐diphenylmethane diisocyanate, which was extended with a series of chain extenders (CEs) having 2–10 methylene units in their structure. The completion of the reaction was confirmed by Fourier transform infrared spectroscopy. The chemical structures of the synthesized PU samples were characterized with Fourier transform infrared, ¹H‐NMR, and ¹³C‐NMR spectroscopy, and the thermal properties were determined by thermogravimetric analysis, DSC, and dynamic mechanical thermal analysis techniques. The mechanical properties were also studied and are discussed. The thermogravimetric analysis and DSC analysis showed that CE length had a considerable effect on the thermal properties of the prepared samples. The dynamic mechanical thermal analysis and damping peaks were also affected by the number of methylene units in the CE length. The elastomer extended with 1,2‐ethane diol exhibited optimum thermal properties, whereas the elastomer based on 1,10‐decane diol displayed the worst thermal properties. Tensile strength and elongation at break decreased with increasing CE length, whereas hardness showed the opposite trend. The glass‐transition temperature moved toward lower temperatures with increasing CE length. The decrease in the glass‐transition temperature and tensile properties were interpreted in terms of decreasing hard segments and increasing chain flexibility. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Young’s modulus of crystalline C60 nanotubes studied by in situ transmission electron microscopy

Bending tests of crystalline nanotubes composed of fullerene C₆₀ molecules are performed inside a high-resolution transmission electron microscope. We fixed one side of a C₆₀ nanotube with a body-centered tetragonal structure with typical inner and outer diameters, i.e., 180 nm and 510 nm, respectively, and then applied concentrated forces on the other side using piezomanipulation of a silicon nanotip. The bending process was observed in situ by transmission electron microscopy with simultaneous measurements of the forces by an optical deflection method. It was found that the Young’s modulus of the nanotube was estimated to be 62–107 GPa, which was 1.1–3.3 times larger than that of C₆₀ nanowhiskers. The result concerning the increase in the Young’s modulus of the C₆₀ nanotube provided an experimental evidence for the structural model composed of an inner core and a surface shell for C₆₀ nanowhiskers.     

Flammability characteristics at applied heat flux levels up to 200 kW/m2

This paper documents the first of the two interrelated studies that were conducted to more fundamentally understand the scalability of flame heat flux, the motivation being that it has been reported that flame heat flux back to the burning surface in bench‐scale experiments is not the same as for large‐scale fires. The key aspect was the use of real scale applied heat flux up to 200kW/m² which is well beyond that typically considered in contemporary testing. The main conclusions are that decomposition kinetics needs to be included in the study of ignition and the energy balance for steady burning is too simplistic to represent the physics occurring. An unexpected non‐linear trend is observed in the typical plotting methods currently used in fire protection engineering for ignition and mass loss flux data for several materials tested and this non‐linearity is a true material response. Using measured temperature profiles in the condensed phase shows that viewing ignition as an inert material process is inaccurate at predicting the surface temperature at higher heat fluxes. The steady burning temperature profiles appear to be invariant with applied heat flux. This possible inaccuracy was investigated by obtaining the heat of gasification via the ‘typical technique’ using the mass loss flux data and comparing it to the commonly considered ‘fundamental’ value obtained from differential scanning calorimetry measurements. This comparison suggests that the ‘typical technique’ energy balance is too simplified to represent the physics occurring for any range of applied heat flux. Observed bubbling and melting phenomena provide a possible direction of study. Copyright © 2007 John Wiley & Sons, Ltd.     

Kinetic modelling of textural changes in ready-to-eat breakfast cereals during soaking in semi-skimmed milk

Summary Ready‐to‐eat breakfast cereals immersed in milk undergo undesirable changes in texture because of sudden moisture uptake. The textural changes are ascribable to a plasticizing effect of water, which modifies the mechanical strength of products by softening the starch/protein matrix. In this work, some textural parameters of different cereal flakes were derived from the force–displacement curves monitored during 300 s of immersion in milk. Hardness loss, deformability increment and changes in the force–displacement curve profile were calculated and plotted against soaking time. The application of a sugar coating process to a model cereal flake increased the initial product hardness and improved the preservation of the textural parameters during immersion. The Peleg model closely fitted the experimental data, with regression coefficients from 0.967 to 0.999.     

Design and Characterization of the CLIMPAQ,Chamber for Laboratory Investigations of Materials,Pollution and Air Quality*

A test chamber has been developed in order to provide a small and simple emission testing facility capable of testing construction products in a climate where the important climatic parameters such as temperature, ventilation rate and air velocity can be varied independently around typical indoor values. The test chamber CLIMPAQ is made of panes of window glass. Other main surface materials are stainless steel and eloxated aluminium. The chamber has a volume of 50.9 litres and is designed to meet the requirements for quantifying air pollution. In this investigation human subjects acted as air pollution judges, and chemical characterization of the air pollution was carried out. Carpet, linoleum, wall paint and seal- ant were tested simultaneously in the CLIMPAQ and in four other chambers ranging from a full-scale chamber of 28 m³ to a field and laboratory emission cell of 3.5· 10^?5m³. Product ranking is the same in all chambers for the sensory measurements. Emission rates based on sensory measurements differ for all products less than 100 % except for tests in a 3-litre chamber where emission rates were higher. Chemical measurements differ up to approximately 10 times for the same product in different chambers. Deviations appear to be the result of different environmental parameters in the various chambers. Low air concentrations or high specific ventilation rates seem to increase emissions, while differences in air velocities and sink properties may also be the cause of differences in emission rates.     

Thermal and thermoelastic properties of fast extrusion furnace (FEF) carbon black loaded SBR vulcanizates

The effect of FEF carbon black as filler on the thermal capacity c, diffusivity a, and thermal conductivity λ, of styrene butadiene rubber (SBR) composites in the temperature range 300–420 K was studied. The filler strongly increases the thermal diffusivity, whilst strongly decreasing the thermal capacity and the thermal conductivity (except at high FEF content ≥80 phr). The influence of the filler on the thermoelastic behaviour of the same composites was also investigated. It was found that the thermoelastic temperature change (ΔT) increased with carbon black concentration as well as the entropy change per unit extension.     

Influence of the surface conditions on permeation in the deuterium–MANET system

The condition of the surfaces is of crucial importance for the deuterium permeation through materials. In this work a study of the surface constants for the adsorption (σk₁) and release (σk₂) of deuterium under different surface conditions on the martensitic steel DIN 1.4914 (MANET) has been carried out. The growth of an oxide surface layer (Cr₂O₃) of about 25–30 nm in a MANET sample, heat treated in an oxidizing environment, compared to the bare MANET that have a ‘natural' oxide of about 5 nm has provoked a reduction of both the permeation rate and the recombination coefficient (about 3 orders of magnitude). In addition, the permeation governing process has changed from diffusion-limited to surface-limited. The measurements of the permeation rate of deuterium were performed by a gas-phase permeation technique over the temperature range 574–746 K and for deuterium driving pressures in the range from 3 to 10⁵ Pa.     

Hydrogen and Calcium Ion Concentrations Affect Volume of CO2 Puffed Diced Green Bell Peppers

Diced green bell peppers were soaked in a solution of hydrochloric acid or calcium chloride, air-dried to 50% moisture, held in CO₂ at 5.8 MPa for 1, 3 or 5 min, and puffed by abruptly releasing the CO₂ pressure. Treatment with 1% CaCl₂ increased the size of puffed-dried products as compared to a control; however, HCl treatments did not. The treatment with 1 or 2% CaCl₂ reduced shrinkage as compared to the control. The 1% CaCl₂ treatment may have increased the CO₂ saturation rate.