Residual compressive behavior of alkali‐activated concrete exposed to elevated temperatures

This paper reports the effect of elevated temperature exposures, up to 1200^°C , on the residual compressive strengths of alkali‐activated slag concrete (AASC) activated by sodium silicate and hydrated lime; such temperatures can occur in a fire. The strength performance of AASC in the temperature range of 400–800^°C was similar to ordinary Portland cement concrete and blended slag cement concrete, despite the finding that the AASC did not contain Ca(OH)₂ , which contributes to the strength deterioration at elevated temperatures for Ordinary Portland Cement and blended slag cement concretes. Dilatometry studies showed that the alkali‐activated slag (AAS) paste had significantly higher thermal shrinkage than the other pastes while the basalt aggregate gradually expanded. This led to a higher thermal incompatibility between the AAS paste and aggregate compared with the other concretes. This is likely to be the governing factor behind the strength loss of AASC at elevated temperatures. Copyright © 2008 John Wiley & Sons, Ltd.     

Tape casting of polysiloxane-derived ceramic with controlled porosity and surface properties

Tape casting has been applied to produce porous hybrid and SiOC ceramic tapes using ceramic precursors and commercially available polysiloxanes as polymeric binders. SiC particles of two different mean sizes (4.5 or 6.5?μm) were used as inert fillers to prevent shrinkage and increase mechanical stability. Macroporosity was adjusted by varying the azodicarbonamide (ADA) content from 0 to 30?wt.%. Decomposition of the polysiloxanes at 600?°C resulted in the generation of micropores with high specific surface area (187–267 m²?g^?1) and a predominant hydrophobic behavior. At 1000?°C mainly meso/macroporosity were observed (SSA: 32–162 m²?g^?1) accompanied by increased hydrophilicity. The influence of ADA content, SiC size, and pyrolysis temperature on open porosity (2.5–37%), average pore size (<0.01–1.76?μm), surface characteristics, and flexural strength (10.5–121?MPa) were investigated. The porous tapes with different surface characteristics and controlled structure are highly promising for applications involving membrane processes, particularly microfiltration systems (0.1–10?μm).     

Optimization of structure and properties of polyphenylene sulfide porous membrane by controlling the process of thermally induced phase separation

Polyphenylene sulfide (PPS) porous membranes were successfully prepared from miscible blends of PPS and polyethersulfone (PES) via thermally induced phase separation followed by subsequent extraction of the PES diluent. The morphologies, crystalline structures, mechanical properties, pore structures and permeate fluxes of the PPS porous membranes obtained from different phase separation processes were characterized and are discussed. During the phase separation in the heating process, PPS and PES mainly underwent liquid–liquid phase separation, and then a nonhomogeneous porous structure with a mean pore size of 100 μm and a honeycomb‐like internal structure formed on the membrane surface. The phase separation of PPS/PES occurring in the cooling process was easier to control and the related pore diameter distribution was more regular. In the process of direct annealing, as the phase separation temperature decreased, the pore size distribution became more homogeneous and the mean diameter of the pores also decreased gradually. When the phase separation temperature decreased to 200 °C, PPS membranes with a network structure and a uniform as well as well‐interconnected porous structure could be obtained. In addition, the maximum permeation flux reached 1718.03 L m^–2 h^–1 when the phase separation temperature was 230 °C. The most probable pore diameter was 6.665 nm, and the permeate flux of this membrane was 2.00 L m^–2 h^–1; its tensile strength was 17.07 MPa. Finally, these PPS porous membranes with controllable pore structure as well as size can be widely used in the chemical industry and energy field for liquid purification. © 2020 Society of Chemical Industry     

Cost‐effective porous ceramic tubes fabricated through a phase inversion/casting process using calcined bauxite

Cost‐effective ceramic tubes based on low‐price commercial calcined bauxite for economical separation were fabricated by a new phase‐inversion casting method. The thermal shrinkage and weight loss during heating of the green tubes were characterized by dilatometric analysis and TG, respectively. Three shrinkage stages appear successively, corresponding to the viscous deformation of polymeric binder at 200‐300°C, significant combustion loss of ~5.2 wt% at 500‐620°C and sintering shrinkage over 800°C, respectively. However, due to high enough viscosity of the casting suspension that can guarantee the green tube against collapse or deformation during the phase inversion/casting process, the sintered tubes display nearly uniform microstructure instead of characteristic asymmetrical structure of the phase inversion process. The influence of sintering temperature on the pore property (including pore size and porosity) and mechanical strength was investigated. As the sintering temperature increases from 1200 to 1400°C, the porosity and average pore size decrease from 46.4% to 37.0% and from 0.98 to 0.81 μm, respectively, and the flexural strength increases from 25.8 to 65.1 MPa. The cost‐effective ceramic tube sintering at the range of 1250‐1400°C can be capable of functioning as a microfiltration membrane or an ultrafiltration membrane support.     

Galvanic deposition of silver on 80‐μm‐Cu‐fiber for gas‐phase oxidation of alcohols

Microstructured Ag‐based catalysts were developed by galvanically depositing Ag onto 80‐μm‐Cu‐fibers for the gas‐phase oxidation of alcohols. By taking advantages including large voidage, open porous structure and high heat/mass transfer, as‐made catalysts provided a nice combination of high activity/selectivity and enhanced heat transfer. The best catalyst was Ag‐10/80‐Cu‐fiber‐400 (Ag‐loading: 10 wt%; Cu‐fiber pretreated at 400 °C in air), being effective for oxidizing acyclic, benzylic and polynary alcohols. For benzyl alcohol, conversion of 94% was achieved with 99% selectivity to benzaldehyde at 300 °C using a high WHSV of 20 h^?1. Computational fluid dynamics (CFD) calculation and experimental result illustrated significant enhancement of the heat transfer. The temperature difference from reactor wall to central line was about 10–20 °C for the Ag‐10/80‐Cu‐fiber‐400, much lower than that of 100–110 °C for the Ag‐10‐Cu‐2/Al₂O₃ at equivalent conversion and selectivity. Synergistic interaction between Cu₂O and Ag was discussed, being assignable to the activity improvement. © 2014 American Institute of Chemical Engineers AIChE J, 60: 1045–1053, 2014     

Shrinkage behavior after the heat setting of biaxially stretched poly(ethylene 2,6‐naphthalate) films and bottles

Amorphous preforms of poly(ethylene 2,6‐naphthalate) (PEN) were biaxially drawn into bottles up to the desired volume under industrial conditions. These bottles were used to characterize the shrinkage behavior of the drawn bottles with or without heat treatment and to study structural variations during heat setting. During drawing, a rigid phase structure was induced, and the amount of the induced rigid phase structure was linearly related to the square root of the extra first strain invariant under equilibrium conditions. During the production of these bottles, this equilibrium was not attained because of high stretching conditions and rapid cooling after stretching. The structure after orientation contained a rigid amorphous phase and an oriented amorphous phase. The shrinkage behavior was a function of the temperature and time of heat setting. Long heat‐setting times, around 30 min, were used to characterize the possible structural variations of the oriented PEN after heat setting at equilibrium. Under the equilibrium conditions of heat setting, the start temperature of the shrinkage was directly related to the heat‐setting temperature and moved from 60°C without heat treatment up to a temperature of 255°C by a heat‐setting temperature of 255°C; this contrasted with poly(ethylene terephthalate) (PET), for which the start temperature of shrinkage was always around 80°C. For heat‐setting temperatures higher than 220°C, the structural variations changed rapidly as a function of the heat‐setting time, and the corresponding shrinkage of the heat‐set samples sank below 1% in a timescale of 30–60 s for a film thickness of 500 μm. The heat treatment of the oriented films taken out of the bottle walls with fixed ends stabilized the induced structures, and the shrinkage of these heat‐set films was zero for temperatures up to the heat‐setting temperature, between 220 and 265°C, if the heat‐setting time was sufficient. According to the results obtained, a heat‐setting time of 30 s, for a film thickness of 500 μm, was sufficient at a heat‐setting temperature of 255°C to stabilize the produced biaxially oriented PEN bottles and to take them out the mold without further shrinkage. During the drawing of PEN, two different types of rigid amorphous phases seemed to be induced, one with a mean shrinkage temperature of 151°C and another rigid amorphous phase, more temperature‐stable than the first one, that shrank in the temperature range of 200–310°C. During heat setting at high temperatures, a continuous transformation of the less stable phase into the very stable phase took place. The heat‐set method after blow molding is industrially possible with PEN, without the complicated process of subsequent cooling before the molds are opened, in contrast to PET. This constitutes a big advantage for the blow molding of PEN bottles and the production of oriented PEN films. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 87: 1462–1473, 2003     

Effect of porous properties on self-cooling of fired clay plate by evaporation of absorbed water

Porous ceramic plates were prepared from clay and wood charcoal powder at 900 and 1100?°C and their porous properties, water absorption and the cooling effect of porous plates were investigated to produce eco-friendly porous ceramics for cooling by the evaporation of absorbed water. Porous properties were dependent on the firing temperature, and total pore volume, average pore size and porosity, which were 0.38–0.39 cm³/g, 0.15–0.17 μm and 49–50%, respectively at 900?°C and 0.31–0.33 cm³/g, 2.47–2.59 μm and 43–44%, respectively at 1100?°C. By the addition of wood charcoal powder, the cooling rate of porous plate fired at 1100?°C was 1.7 times faster than that of the plate fired at 900?°C and the cooling temperature difference (?T) was around 2.3?°C at 22.5?°C and 52–54% of relative humidity and around 3.2?°C at 29?°C and 77–80% of relative humidity. The porous ceramic plates developed here are potential materials for cooling buildings.     

Fabrication and Characterization of Anode‐Supported Low‐Temperature SOFC Based on Gd‐Doped Ceria Electrolyte

Large‐size, 9.5 cm × 9.5 cm, Ni‐Gd_0.1Ce_0.9O_1.95 (Ni‐GDC) anode‐supported solid oxide fuel cell (SOFC) has been successfully fabricated with NiO‐GDC anode substrate prepared by tape casting method and thin‐film GDC electrolyte fabricated by screen‐printing method. Influence of the sintering shrinkage behavior of NiO‐GDC anode substrate on the densification of thin GDC electrolyte film and on the flatness of the co‐sintered electrolyte/anode bi‐layer was studied. The increase in the pore‐former content in the anode substrate improved the densification of GDC electrolyte film. Pre‐sintering temperature of the anode substrate was optimized to obtain a homogeneous electrolyte film, significantly reducing the mismatch between the electrolyte and anode substrate and improving the electrolyte quality. Dense GDC electrolyte film and flat electrolyte/anode bi‐layer can be fabricated by adding 10 wt.% of pore‐former into the composite anode and pre‐sintering it at 1,100 °C for 2 h. Composite cathode, La_0.6Sr_0.4Fe_0.8Co_0.2O₃, and GDC (LSCF‐GDC), was screen‐printed on the as‐prepared electrolyte surface and sintered to form a complete single cell. The maximum power density of the single cell reached 497 mW cm^–2 at 600 °C and 953 mW cm^–2 at 650 °C with hydrogen as fuel and air as oxidant.     

Foam processing and cellular structure of polypropylene/clay nanocomposites

Polypropylene (PP)/clay nanocomposites (PPCNs) were autoclave‐foamed in a batch process. Foaming was performed using supercritical CO₂ at 10 MPa, within the temperature range from 130.6°C to 143.4°C, i.e., below the melting temperature of either PPCNs or maleic anhydride‐modified PP (PP‐MA) matrix without clay. The foamed PP‐MA and PPCN2 (prepared at 130.6°C and containing 2 wt% clay) show closed cell structures with pentagonal and/or hexagonal faces, while foams of PPCN4 and PPCN7.5 (prepared at 143.4°C, 4 and 7.5 wt% clay) had spherical cells. Scanning electron microscopy confirmed that foamed PPCNs had high cell density of 10⁷–10⁸ cells/mL, cell sizes in the range of 30–120 μm, cell wall thicknesses of 5–15 μm, and low densities of 0.05–0.3 g/mL. Interestingly, transmission electron microscopic observations of the PPCNs' cell structure showed biaxial flow‐induced alignment of clay particles along the cell boundary. In this paper, the correlation between foam structure and rheological properties of the PPCNs is also discussed.     

Compressive strength of fly‐ash‐based geopolymer concrete at elevated temperatures

This paper presents the compressive strength of fly‐ash‐based geopolymer concretes at elevated temperatures of 200, 400, 600 and 800 °C. The source material used in the geopolymer concrete in this study is low‐calcium fly ash according to ASTM C618 class F classification and is activated by sodium silicate (Na₂SiO₃) and sodium hydroxide (NaOH) solutions. The effects of molarities of NaOH, coarse aggregate sizes, duration of steam curing and extra added water on the compressive strength of geopolymer concrete at elevated temperatures are also presented. The results show that the fly‐ash‐based geopolymer concretes exhibited steady loss of its original compressive strength at all elevated temperatures up to 400 °C regardless of molarities and coarse aggregate sizes. At 600 °C, all geopolymer concretes exhibited increase of compressive strength relative to 400 °C. However, it is lower than that measured at ambient temperature. Similar behaviour is also observed at 800 °C, where the compressive strength of all geopolymer concretes are lower than that at ambient temperature, with only exception of geopolymer concrete containing 10 m NaOH. The compressive strength in the latter increased at 600 and 800 °C. The geopolymer concretes containing higher molarity of NaOH solution (e.g. 13 and 16 m ) exhibit greater loss of compressive strength at 800 °C than that of 10 m NaOH. The geopolymer concrete containing smaller size coarse aggregate retains most of the original compressive strength of geopolymer concrete at elevated temperatures. The addition of extra water adversely affects the compressive strength of geopolymer concretes at all elevated temperatures. However, the extended steam curing improves the compressive strength at elevated temperatures. The Eurocode EN1994:2005 to predict the compressive strength of fly‐ash‐based geopolymer concretes at elevated temperatures agrees well with the measured values up to 400 °C. Copyright © 2014 John Wiley & Sons, Ltd.     

Evaluation and fabrication of pore‐size‐tuned silica membranes with tetraethoxydimethyl disiloxane for gas separation

Organic/inorganic hybrid silica membranes were prepared from 1,1,3,3‐tetraethoxy‐1,3‐dimethyl disiloxane (TEDMDS) by the sol‐gel technique with firing at 300–550°C in N₂. TEDMDS‐derived silica membranes showed high H₂ permeance (0.3–1.1 × 10^?6 mol m^?2 s^?1 Pa^?1) with low H₂/N₂ (～10) and high H₂/SF₆ (～1200) perm‐selectivity, confirming successful tuning of micropore sizes larger than TEOS‐derived silica membranes. TEDMDS‐derived silica membranes prepared at 550°C in N₂ increased gas permeances as well as pore sizes after air exposure at 450°C. TEDMDS had an advantage in tuning pore size by the “template” and “spacer” techniques, due to the pyrolysis of methyl groups in air and Si? O? Si bonding, respectively. For pore size evaluation of microporous membranes, normalized Knudsen‐based permeance, which was proposed based on the gas translation model and verified with permeance of zeolite membranes, reveals that pore sizes of TEDMDS membranes were successfully tuned in the range of 0.6–1.0 nm. © 2011 American Institute of Chemical Engineers AIChE J, 2011     

Physicochemical characterization of maize tassel as an adsorbent. I. Surface texture,microstructure, and thermal stability

In this study, various physicochemical parameters were evaluated for maize tassel, a novel adsorbent. The Brunauer–Emmett–Teller (BET) isotherm was used to experimentally model N₂‐adsorption data (up to a relative pressure of 0.30); the results indicated that the powdered material was mesoporous with a BET specific surface area, total pore volume (up to a relative pressure of 0.98), and average pore width (4V/A by BET) of 2.52 m²/g, 0.0045 cm³/g, and 7.2 nm, respectively, for the 150–300‐μm fraction. Laser diffraction pattern analysis yielded particle size distributions for the 45–50‐, 50–150‐, and 150–300‐μm fractions. High‐resolution scanning electron microscopy revealed a microstructure showing predominantly flattish, rodlike particles. The material exhibited stability to thermal decomposition up to about 230°C, as evidenced by the results obtained from simultaneous thermogravimetry/differential thermal analysis and differential scanning calorimetry. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Initiator‐fragment incorporation radical polymerization of diallyl phthalate: Kinetics,formation of hyperbranched polymer,and iridescent porous film thereof

Diallyl phthalate (DAP) was polymerized in toluene using dimethyl 2,2′‐azobisisobutyrate (MAIB) of high concentrations (0.1–0.9 mol/L) as initiator. The polymerization of DAP of 1.50 mol/L with MAIB of 0.50 mol/L proceeded homogeneously at 80°C without gelation to give soluble polymers in a high yield of 93%. Kinetic results of the homogeneous polymerization at 80°C suggest significant contributions of the degradative chain transfer and the primary radical termination as shown by the rate equation, R_p = k [MAIB]^0.8[DAP]^1.0 (R_p = polymerization rate). The polymer formed in the polymerization of DAP (1.30 mol/L) with MAIB (0.50 mol/L) at 80°C for 8 h consisted of the DAP units with (17 mol %) and without (47 mol %) double bond and the methoxycarbonylpropyl group (36 mol %) as MAIB‐fragment. The large fraction of the incorporated initiator‐fragment as terminal group indicates that the polymer has a hyperbranched structure. The film cast from a solution of the hyperbranched poly(DAP) in tetrahydrofuran showed an iridescent color. The confocal scanning laser microscope image of the film revealed that the iridescent film contained the pores of about 1 μm arranged in an ordered array. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 408–415, 2006     

Ceramic shell foams produced by direct foaming and gelcasting of proteins: Permeability and microstructural characterization by X-ray microtomography

In this work, ceramic shell foams produced by direct foaming and gelcasting of proteins containing 35 vol.% of solids were efficiently tailored through the optimization of suspension parameters, foaming and also according to the gelling temperature. These were key parameters employed for controlling the foamability and foam stability, and hence the foam porosity and pore characteristics after the sintering process. The potential of using microtomography in characterizing the morphometric parameters of foams was explored. Airflow permeability measurements (∼24 °C to 727 °C) were performed in order to investigate the applicability of such materials in the fluid flow field. The samples exhibited a wide range of pore sizes (60 ± 5–1700 ± 90 μm), porosity values higher than 80 %, Darcian (k₁) and non-Darcian (k₂) permeability coefficients values in the ranges of 1.32–1.83 x 10⁻⁹ m² and 8.34–22.46 x 10^-5 m, respectively.     

Effect of elevated temperatures on mechanical properties of high‐strength concrete containing varying proportions of hematite

Aggregates typically constitute 70 to 80 wt% of concrete, and therefore their type, size, and structure play an essential role in modifying the properties of concrete. When concrete is used for shielding nuclear applications, temperature is also a key factor. This study investigates the effects of elevated temperatures (25 °C, 200 °C, 400 °C, 600 °C, and 800 °C), heating durations (1, 2, and 3 h), and cooling regimes (air, and water cooling) on mechanical properties of concrete containing different proportions of hematite. A sample of plain concrete was produced for comparison purposes by using river sand, crushed sand, and crushed aggregates. Replacement ratios of 15%, 30%, 45%, and 60% were used for hematite aggregates. The cement content and water–cement ratio were 450 kg/m³ and 0.38, respectively. Slump values of fresh concretes as well as unit weight, compressive strength, flexural strength, splitting tensile strength, and elasticity modulus values of hardened concrete were determined. The addition of hematite into concrete seems to improve its mechanical properties, and hematite concretes have better thermal stability at elevated temperatures than plain concrete does. Copyright © 2011 John Wiley & Sons, Ltd.     

Mechanical/thermal dewatering of lignite. Part 3: Physical properties and pore structure of MTE product coals

The mechanical thermal dewatering (MTE) process has been shown to effectively dewater high moisture content low rank coals via the application of mechanical force at elevated temperatures.Using mercury intrusion porosimetry (MIP) as an investigative tool, this study examines how MTE processing conditions, such as temperature and pressure, affect the compressibility, pore size distribution, apparent (skeletal) density and shrinkage behaviour of three low rank coals sourced from Australia, Greece and Germany. As both pore filling and sample compression occurred at high mercury intrusion pressures, all MIP data were corrected for compression effects by using compressibility values derived from mercury extrusion data.The MTE process is shown to produce a low porosity coal, which, depending upon the processing conditions used, undergoes further shrinkage upon oven drying at 105 °C. An increase in MTE temperature (above about 85 °C) led to an increase in mesopore volume, which is caused by a hardening of the coal structure, leading to pore volume retention and a consequent reduction in percent shrinkage on oven drying. The increase in measured mesopore volume is also associated with an increase in measured surface area.The reverse trend is seen with increasing MTE pressure, where both the macro and mesopore volume decrease with pressure, causing the percent shrinkage to increase accordingly. This effect may be due to an increase in capillary forces caused by a decrease in the average pore diameter. The percent shrinkage increased up to a pore volume of about 0.1 cm³/g, beyond which no further reduction in pore volume was achieved. The decrease in mesopore volume is also associated with a decrease in measured surface area.Compressibility values derived from mercury extrusion data show that the MTE process has little impact on the network strength of the skeletal network structure of all three coals investigated. Likewise, the skeletal density remained relatively unchanged.The reduction in water content, pore volume and the changes in shrinkage behaviour under increasingly severe MTE conditions are suggestive of the physical changes that accompany increased coalification (rank) within the lignitic range.     

Sulfonated poly(sulfone‐pyridine‐amide)/sulfonated polystyrene/multiwalled carbon nanotube‐based fuel cell membranes

In this study, aromatic sulfonated poly(sulfone‐pyridine‐amide) (S‐PSPA) has been prepared via polycondensation of sulfonated monomer 1‐(4‐thiocarbamoylaminophenyl‐sulfonylphenyl)thiourea and 2,6‐pyridinedicarboxylic acid at high temperature. Mechanically robust and thermally stable hybrid membranes were prepared using non‐functional and functional multiwalled carbon nanotube (MWCNT) i.e., S‐PS/S‐PSPA/MWCNT‐NF and S‐PS/S‐PSPA/MWCNT via solution blending. Field emission scanning electron microscopy exhibited porous membrane structure for 0.1–0.5 wt% nanotube loading, whereas well‐aligned functional MWCNT were observed in 1 wt% loaded sample. Increasing the functional nanotube content from 0.1 to 1 wt% increased tensile strength of functional S‐PS/S‐PSPA/MWCNT hybrids from 62.19 to 65.29 MPa compared with non‐functional hybrid (53.34 MPa) and neat S‐PS/S‐PSPA. 10% decomposition temperature of S‐PS/S‐PSPA/MWCNT 0.1–1 was in the range 491–502°C, while S‐PS/S‐PSPA/MWCNT‐NF showed relatively lower thermal stability (T₁₀ 489°C). Glass transition temperature of functional S‐PS/S‐PSPA/MWCNT was also higher (201–243°C) relative to S‐PS/S‐PSPA/MWCNT‐NF (194°C). Furthermore, functional MWCNT‐based membranes had higher ion exchange capacity (IEC) 3.2–3.6 mmol/g and lower activation energies (95–36 kJ/mol). Novel functional membranes also revealed high proton conductivity 1.68–2.55 S/cm in a wide range of humidity at 80°C higher than that of perfluorinated Nafion® membrane (1.1 ×10^?1 S/cm) at 80°C (94% RH). POLYM. ENG. SCI., 55:1776–1786, 2015. © 2014 Society of Plastics Engineers     

Lipase‐catalyzed synthesis of polyhydric alcohol‐poly(ricinoleic acid) ester star polymers

Polyesters of poly(ricinoleic acid) and polyol acyl acceptors (trimethylolpropane, pentaerythritol, and dimer diol), examples of lipophilic star polymers, were synthesized via bulk polymerization at 70°C in a 1 to 2‐week period, using immobilized lipases from Candida antarctica B, CAL, and Rhizomucor miehei, RML (Novozyme and Lipozyme, respectively, from Novozymes North America, Franklinton, NC). In the screening of several synthesis procedures, the highest molecular weight and degree of conversion occurred when polyricinoleic acid, synthesized previously from ricinoleic acid using CAL as biocatalyst, was mixed with polyol and either CAL or RML. Such a procedure yielded pentaerythritol–poly(ricinoleic acid) tetraester with an average molecular weight of 4850 ± 440 Da, according to ¹H NMR analysis. Seventy‐eight percent of the polyol acyl acceptor's hydroxyl groups were esterified, with the average degree of polymerization for its poly(ricinoleyl) chains being 5.4 ± 0.5. The product mixture contained 83% polyol ester and only 17 wt % nonesterified linear poly(ricinoleic acid). The rate‐limiting step in the formation of poly(ricinoleic acid), propagation, was first‐order with respect to monomer (ricinoleyl acyl groups); and, chain‐transfer reactions were absent. The products formed possessed high viscosity and viscosity indices (155 for the pentaerythritol tetraester) and melting point temperatures below ?7.5°C, suggesting their use as environmentally‐friendly lubricant materials. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 1646–1656, 2006     

Synthesis and Characterization of Ethylene‐Bridged Copolycarbosilazane as Precursors for Silicon Carbonitride Ceramics

An ethylene‐bridged copolycarbosilazane precursor of copolysilylethylenediamine (co‐PSDA) is synthesized by polycondensation of ethylenediamine with the mixture of vinylmethyldichlorosilane and methyldichlorosilane in the presence of triethylamine as acid absorbing agent. Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR, ¹H NMR and ¹³C NMR) spectral analysis of the as‐synthesized co‐PSDA suggests a structure of ethylene‐bridged polycarbosilazane having –Si–N–C–C–N– as backbone chain with –CH=CH₂, –H and –CH₃ attached to Si as side groups. Co‐PSDA can be cross‐linked at 80°C using 2, 2‐azobisisobutyronitrile as initiator through the polyaddition of the vinyl group and dehydrogenation/deamination of Si–H and N–H. Then the cross‐linked co‐PSDA precursor is pyrolyzed at 1000°C in argon, giving out amorphous silicon carbon nitride (SiCN) ceramics with a high ceramic yield of 76 wt%. The obtained SiCN ceramics consist of nitrogen‐rich silicon sites of SiN₄ as predominant component and some SiCN₃ sites, which should arise from the breaking of N–C bonds below 600°C and the formation of active N–Si bonds.     

Porous poly(L‐lactic acid)/poly(ethylene glycol) blend films

Poly(L ‐lactic acid) (PLLA: M_w = 19.4 × 10⁴)/poly(ethylene glycol) (PEG: M_w = 400) blend films were formed by use of a solvent‐cast technique. The properties and structures of these blend films were investigated. The Young's modulus of the PLLA decreased from 1220 to 417 MPa with the addition of PEG 5 wt %, but the elongation at break increased from 19 to 126%. The melting point of PLLA linearly decreased with increases in the PEG content (i.e., pure PLLA: 172.5°C, PLLA/PEG = 60/40 wt %: 159.6°C). The PEG 20 wt % blend film had a porous structure. The pore diameter was 3–5 μm. The alkali hydrolysis rate of this blend film was accelerated due to its porous structure. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 965–970, 2004