Composition optimization of extruded starch foams using response surface methodology

Response surface methodology (RSM) was used to analyse the effect of polyvinyl alcohol (PVA) and calcium carbonate (CaCO₃) on the objective attributes (shipping bulk density, radial expansion ratio, compressibility and spring index) of a biodegradable cushioning extrudate. A rotatable central composite design (CCD) was used to develop models for the objective responses. The experiments were run at 105°C with a feed rate of 27.8 l/h, screw speed 500 r.p.m. and die diameter 3.92 mm. Responses were most affected by changes in polyvinyl alcohol (PVA) levels and to a lesser extent by calcium carbonate (CaCO₃) levels. Individual contour plots of the different responses were overlaid, and regions meeting the optimum shipping bulk density of 6.00 kg/m³, radial expansion ratio of 3.30, compressibility of 43.71 N, and spring index of 0.91 were identified at the PVA level of 20.23% and the CaCO₃ level of 7.89%, respectively. Copyright © 2004 John Wiley & Sons, Ltd.     

Response surface optimization of the feed compositions of biodegradable packaging foams

Response surface methodology (RSM) was used to analyse the effects of polyvinyl alcohol (PVOH) and calcium carbonate (CaCO₃) on the physical and mechanical properties (radial expansion ratio, bulk density, compressibility and spring index) of a biodegradable cushioning extrudate. A rotatable central‐composite design (CCD) was used to develop models for the objective responses. The experiments were run at 125°C with a feed rate of 27.8 l/h, screw speed of 215 r.p.m. and die diameter of 3.92 mm. Responses were most affected by changes in PVOH levels and to a lesser extent by CaCO₃ levels. Individual contour plots of the different responses were overlaid. An optimum radial expansion ratio of 3.39, bulk density of 0.065 (g/cm³), compressibility of 32.27(N), and spring index of 0.906 were identified at 36% PVOH and 5% CaCO₃. Copyright © 2005 John Wiley & Sons, Ltd.     

Influence of pressurized carbon dioxide on ketoprofen-incorporated hot-melt extruded low molecular weight hydroxypropylcellulose

Objectives: The aim of the current research project was to investigate the effect of pressurized carbon dioxide (P-CO₂) on the physico-mechanical properties of ketoprofen (KTP)-incorporated hydroxypropylcellulose (HPC) (Klucel? ELF, EF, and LF) produced using hot-melt extrusion (HME) techniques and to assess the plasticization effect of P-CO₂ on the various polymers tested.

Methods: The physico-mechanical properties of extrudates with and without injection of P-CO₂ were examined and compared with extrudates with the addition of 5% liquid plasticizer of propylene glycol (PG). The extrudates were milled and compressed into tablets. Tablet characteristics of the extrudates with and without injection of P-CO₂ were evaluated.

Results and conclusion: P-CO₂ acted as a plasticizer for tested polymers, which allowed for the reduction in extrusion processing temperature. The microscopic morphology of the extrudates was changed to a foam-like structure due to the expansion of the CO₂ at the extrusion die. The foamy extrudates demonstrated enhanced KTP release compared with the extrudates processed without P-CO₂ due to the increase of porosity and surface area of those extrudates. Furthermore, the hardness of the tablets prepared by foamy extrudates was increased and the percent friability was decreased. Thus, the good binding properties and compressibility of the extrudates were positively influenced by utilizing P-CO₂ processing.     

Physical properties and characterization of biodegradable films using nano-sized TiO2/poly(acrylamide-co-methyl methacrylate) composite

In this study, biodegradable films were prepared by using corn starch, PVA, nano-sized poly(acrylamide-co-methyl methacrylate) (PAAm-co-MMA), nano-sized TiO2(P-25)/PAAm-co-MMA composite, and additives which are harmless to the human body, that is, glycerol (GL) and citric acid (CA). Nano-sized PAAm-co-MMA was synthesized by the method of emulsion polymerization. Also, nano-sized TiO2/PAAm-co-MMA composites were synthesized by wet milling for 48 h. The morphology and crystallinty of nano-sized PAAm-co-MMA and TiO2/PAAm-co-MMA composite was observed by the SEM and XRD. The physical properties such as tensile strength (TS), elongation at break (%E), degree of swelling (DS), and solubility (S) of biodegradable films were investigated. The photocatalytic degradability of starch/PVA/nano-sized TiO2/PAAm-co-MMA composite blended films was evaluated using methylene blue as photodegradation target.     

聚乙烯醇水溶性包装薄膜生物降解性研究

目的研究聚乙烯醇(PVA)水溶性包装薄膜的生物降解性。方法通过培养、筛选、分离、纯化等工序,获得其中降解效率最高的菌株,并对PVA的降解效果进行研究。同时通过控制变量法和正交实验,研究PVA水溶性包装薄膜组分中各种助剂对其降解性的影响。结果青霉菌对PVA水溶性包装薄膜的降解性效果最为明显;PVA水溶性包装薄膜组分中各种助剂含量在一定质量浓度下对PVA的降解效果有促进作用。结论丙三醇的质量分数为1.7%,十二烷基硫酸钠的质量分数为1.2%,吐温的质量分数为1.4%时,青霉菌对PVA降解效果最为明显。     

Effect of degree of saponification on properties of films obtained from PVA/NaCl/H2O system

Properties of the film obtained from the solution of atactic-polyvinyl alcohol (PVA)/NaCl/H₂O system were investigated through changing the degree of saponification (DS) and NaCl concentration. The films had a higher crystallinity as well as a higher draw ratio than pure PVA film. Maximum values of degree of crystallinity and draw ratio of the films were 38.5% and 17.8, respectively. The highest tensile modulus of the films was at DS 99.05 mol% and NaCl concentration 2 wt.%. These results indicated that the NaCl concentration control has a beneficial effect on properties upgrade of PVA film, but the DS control was effective in control of degree of crystallinity.     

Effect of eggshell powder as nucleating agent on the structure,morphology and functional properties of normal corn starch foams

Corn starch and eggshell powder (with particle sizes of 4–5µm and 8–10µm) composite foams were prepared by extrusion. Effects of eggshell on the structure, morphology, physical properties (unit density and expansion ratio), mechanical properties (spring index and compressibility) and thermal behaviour (thermal transition and stability) of the foams were investigated. Foam cell size decreased and cell population increased with addition of eggshell into starch matrix. The foam unit density, expansion ratio and compressibility decreased significantly (p < 0.05), while the spring index increased significantly (p < 0.05) as the eggshell content increased from 0 to 6wt%. Further increasing eggshell content to 10wt% increased the unit density and compressibility and decreased the expansion ratio and spring index. The thermal transition and stability increased with the addition of eggshell. The optimum eggshell content was 6wt% and the smaller‐sized eggshell powder had a favourable effect on the functional properties of the foams. Copyright © 2006 John Wiley & Sons, Ltd.     

Study of some physical properties of biodegradable films based on blends of gelatin and poly(vinyl alcohol) using a response-surface methodology

The aim of this work was to study the effect of the hydrolysis degree (HD) and the concentration (C_PVA) of two types of poly(vinyl alcohol) (PVA) and of the type (glycerol and sorbitol) and the concentration (C_P) of plasticizers on some physical properties of biodegradable films based on blends of gelatin and PVA using a response-surface methodology. The films were prepared with a film forming solutions (FFS) with 2 g of macromolecules (gelatin+PVA)/100 g de FFS. The responses analyzed were the mechanical properties, the solubility, the moisture content, the color difference and the opacity. The linear model was statistically significant and predictive for puncture force and deformation, elongation at break, solubility in water, moisture content and opacity. The C_PVA affected strongly the elongation at break of the films. The interaction of the HD and the C_P affected this property. Moreover, the puncture force was affected slightly by the C_PVA. Concerning the solubility in water, the reduction of the HD increased it and this effect was greater for high C_PVA values. In general, the most important effect observed in the physical properties of the films was that of the plasticizer type and concentration. The PVA hydrolysis degree and concentration have an important effect only for the elongation at break, puncture deformation and solubility in water.     

Solution spinning of high-Tc oxide superconducting filament: Part VIII The effect of degree of saponification of poly(vinyl alcohol) on the critical current density of YBa2Cu3Ox superconducting filament

The precursor YBa2Cu3Ox (Y-123) filaments were prepared by solution spinning through aqueous poly(vinyl alcohol) (PVA) solution containing mixed Y, Ba and Cu acetates. The as-drawn filaments were heated to remove volatile components and to generate a superconducting phase. The effect of degree of saponification (DS) of PVA in the precursor filament on the critical current density, Jc, for the heated filaments was studied. The precursor filaments were successfully prepared using PVA with DSs ranging from 65 to 81 mol%. The liquid-phase sintering throughout the filament occurred for the filament spun from PVA solution with a DS of 71 mol% and sintered at 920°C for 15 min. The filaments were partially melted to enhance Jc. The minimum Jc was observed for the filament with a DS of 67 mol%, and the highest Jc of 3.5×104 A cm-2 at 77 K and 0 T was achieved for the filament with a DS of 81 mol%. A configuration of PVA in the precursor filament affects the superconductivity of the heated filament.     

Study of the effect of DCCA and hydrofluoric acid contents on metric and topological parameters of silica membranes

In this work we studied the effects of drying control chemical additive (DCCA's), for instance formamide, N,N-dimethylformamide and propylene carbonate as well as the effect of hydrofluoric acid on structural parameters related to the evaluation of pore connectivity and permeability of sol-gel membranes. In order to study the effect of drying additives, we used a molar ratio additive/alkoxide of 1/1. We used several molar ratios HF/alkoxide to allow an evaluation of the effect of hydrofluoric acid on the textural properties and permeability of the samples. The influence of those parameters on pores interconnectivity and permeability was studied using a combination of geometric modeling and experimental evaluation of the volume fraction of pores (V _v), the surface area density (S _v), the average pore size and bulk density. Using different DCCA's and different concentrations of hydrofluoric acid we obtained membranes with different textural properties and permeability. The elevated interconnectivity of these membranes suggests the feasibility of their utilization in separation and impregnation processes.     

Structural and thermodynamic properties of antiperovskite SbNMg3

The full potential augmented plane wave plus local orbital (FP-LAPW + lo) method using the generalized-gradient approximation within the framework of density functional theory is applied to the study of the lattice constant, bulk modulus, pressure derivative of the bulk modulus and elastic constants of antiperovskite semiconductor SbNMg₃. The quasi-harmonic Debye model, in which the phononic effects are considered, is applied to the study of the thermodynamic properties. The temperature effect on the structural parameters, bulk modulus, thermal expansion coefficient, specific heats and Debye temperatures in the whole pressure range from 0 to 30 GPa and temperature range from 0 to 1200 K.     

A novel silver–aluminium high-temperature die attach nanopaste system: the effects of organic additives content on post-sintered attributes

An Ag–Al die attach material having a fixed Ag–Al nanoparticles weight percent content (80–20 %), as well as varying organic additives weight percent content was formulated. The total nanoparticle weight percent content was varied between 84.7 and 87.0 %. As the organic additives content in the Ag₈₀–Al₂₀ die attach material decreased from 15.3 to 13.0 %, the nanopaste’s viscosity increased. The die attach material was sintered at 380 °C for 30 min to form Ag₂Al and Ag₃Al compounds. With decreasing organics content from 15.3 to 13.0 %, the porosity of the post-sintered samples also decreased from 30 to 19 %, while the density increased from 2.36 to 6.42 g/cm³. The highest melting point was recorded for the sample with the least organic weight percent content at 519 °C. The coefficient of thermal expansion and electrical conductivity values varied between 6.99–7.74 × 10^?6/ °C and 0.95–1.01 × 10⁵ (ohm-cm)^?1 respectively with decreasing organic content from 15.3 to 13.0 %. The electrical conductivity values recorded were higher than or equal to that of most solder alloy die attach materials. By changing the organic additives content in the Ag₈₀–Al₂₀ die attach material, suitable properties are obtained for high temperature die attach applications.     

A novel technology to manufacture biodegradable polylactide bead foam products

Bead foaming technology with double crystal melting peak structure has been recognized as a promising method to produce high-performance low-density foams with complex geometries. Polylactide (PLA) bead foaming has been of the great interest of researchers due to its origin from renewal resources and biodegradability. However, due to the PLA’s low melt strength and slow crystallization kinetics, the attempts have been limited to the manufacturing methods used for expanded polystyrene (EPS). In this study, we developed microcellular PLA bead foams with double crystal melting peak structure in a large content using a lab-scale autoclave system followed by molding of the beads. PLA bead foams were produced with expansion ratios and average cell sizes ranging from 6 to 31-fold and 6 to 50 μm, respectively. The high-melting point crystals generated during gas-saturation significantly affected the expansion ratio and cell density of the PLA bead foams by enhancing the PLA’s melt strength and promoting cell nucleation around the crystals. The tensile properties of the molded EPLA bead foams showed that EPLA bead foams with double crystal melting peak can be a promising substitute not only for EPS but also for expanded polypropylene (EPP) bead foams.     

Bacterial cellulose-based membrane-like biodegradable composites using cross-linked and noncross-linked polyvinyl alcohol

Bacterial cellulose (BC)-based membrane-like biodegradable composites were produced by immersing wet BC pellicles in polyvinyl alcohol (PVA) solution. The BC content in the BC–PVA composites can be adjusted by varying the concentration of PVA solution. Chemical cross-linking of PVA was carried out using glutaraldehyde to increase the mechanical properties of the composites as well as to make the PVA partially to highly water insoluble. Examination by scanning electron microscopy indicated that the PVA not only penetrated the BC network, but also filled the pores within the BC pellicle. Attenuated total reflectance-Fourier transform infrared spectroscopy showed that acetal linkages could be formed in the BC–PVA composites by a cross-linking reaction. Sol–gel results indicated that cross-linking reaction increasingly made PVA insoluble in water resulting in higher gel (cross-linked fraction) content in the PVA. Wide-angle X-ray diffraction results showed decreased crystallinity in cross-linked BC and PVA, as expected. It was also found that crystal size was smaller in PVA after cross-linking. The BC–PVA composites had excellent tensile properties and cross-linking increased these properties further. Thermogravimetric analysis showed higher thermal stability for BC–PVA composites compared to PVA. The cross-linked specimens, especially the highly cross-linked ones, showed even higher thermal stability. The methods developed in this study make it possible to control the PVA content in the composites as well as the cross-linking level of PVA. These composites could be good candidates for replacing traditional non-biodegradable plastics.     

Fabrication and characterization of biodegradable composites based on microfibrillated cellulose and polyvinyl alcohol

Microfibrillated cellulose (MFC) based thin membrane-like fully biodegradable composites were produced by blending MFC suspension with polyvinyl alcohol (PVA). Desired MFC content in the composites could be easily obtained by varying the PVA solution concentration. Chemical crosslinking of PVA was carried out using glyoxal to increase the mechanical and thermal properties of the composites as well as to make the PVA partially water-insoluble. Examination of composite surfaces and fracture topographies indicated that the MFC fibrils were well bonded to PVA and uniformly distributed. Infrared spectroscopy showed that acetal linkages could be formed in the MFC–PVA composites by a glyoxal crosslinking reaction. Sol–gel and swelling results indicated that crosslinking reaction made PVA partially insoluble and reduced its swelling ability. The MFC–PVA composites had excellent tensile properties which were further enhanced by crosslinking. Thermogravimetric analysis (TGA) showed higher thermal stability for MFC–PVA composites compared to PVA. The crosslinked MFC–PVA composites showed even higher thermal stability. Differential scanning calorimetry (DSC) indicated that crosslinking increased the glass transition temperature and reduced melting temperature and crystallinity of PVA in MFC–PVA composites. Results also indicated that nano- and micro-fibrils in MFC inhibit the crystallization of PVA. These composites could be good candidates for replacing today’s traditional non-biodegradable plastics.     

Densification behaviour analysis of ZrO2 nanopowders for dental applications compacted by magnetic pulsed compaction

Sintered bulks of commercial ZrO₂ nanopowders were produced by combined application of magnetic pulsed compaction (MPC) and subsequent two-step sintering, and finally, their density, hardness, shrinkage and formability were analyzed. The formability tests were conducted by a CAD/CAM system. Nearly fully dense (∼98%) commercial ZrO₂ bulks were successfully obtained. With increasing MPC pressure, there was a decrease in the grain size of zirconia block. The ratio of PVA did not have a remarkable effect on the grain size. The optimum compaction pressure during MPC was 1 GPa and mixing conditions included using 1.0 wt. % PVA. The optimum processing condition included MPC process, followed by two-step sintering (first at 1000 and then at 1450 °C). The bulk under these conditions was found to have good formability, ∼97% density, reasonable hardness (1150 Hv) and ∼19% shrinkage.     

氯化镁/甘油改性羧甲基淀粉/聚乙烯醇共混材料的结构与性能

为获得改性淀粉/聚乙烯醇(PVA)共混材料的结构与性能特征,以氯化镁/甘油为复配改性剂,采用溶液成膜方法制备了羧甲基淀粉(CMS)/PVA,研究了CMS/PVA复合膜的红外吸收特性、结晶性能、微观形貌、热性能、力学性能及生物降解性。研究结果表明,氯化镁和甘油可与CMS/PVA产生电子相互作用和氢键作用,阻碍CMS/PVA分子链的规整排列,提高羧甲基淀粉与PVA的相容性,降低CMS/PVA的结晶度和热稳定性。氯化镁/甘油复配改性剂对CMS/PVA的力学性能影响显著,可使CMS/PVA断裂伸长率和拉伸强度提高。氯化镁/甘油可促进CMS/PVA的降解,增加氯化镁/甘油复配改性剂中氯化镁的含量可提高复合膜的降解率。     

Prediction of the volumetric and thermodynamic properties of some refrigerants using GMA equation of state

The density of 11 refrigerants (hydrochlorofluorocarbon (HCFCs) and hydrofluorocarbon (HFCs)) in the extended ranges of temperature and pressure has been calculated using Goharshadi–Morsali–Abbaspour equation of state (GMA EoS) and the results have been shown as the three-dimensional surfaces of density–temperature–pressure. A wide comparison with experimental data was made. The accuracy of the equation of state in the prediction of density was determined by statistical parameters. The results show that the GMA EoS can reproduce the experimental PVT data of HCFCs and HFCs within experimental errors throughout the liquid phase. The thermodynamic properties such as isobaric expansion coefficient, isothermal compressibility, and vapor–liquid equilibrium (VLE) prediction for these HCFC and HFC refrigerants have been performed using GMA EoS. GMA EoS can predict the characteristic feature of pressure behavior of isobaric expansion and isothermal compressibility coefficients.     

An optical technique forin situ density determination in electrolyte solutions under hydrothermal conditions

We report on a technique which determines the density of hydrothermal solutions through the relationship between density and refractive index given by the Lorentz Lorenz equation. An optical cell is described which allows the refractive index of fluids to be measured at temperatures up to 823 K and pressures up to 1200 bar. The validity of the Lorentz-Lorenz equation is demonstrated for pure water and water/NaCl solutions. New experimental results are presented for the density of water/NaNO₃ solutions at high temperature and pressure. The use of density data to derive other properties such as compressibility, thermal expansion coefficient, and apparent molar volume is demonstrated.     

Low-temperature elastic properties of four wrought and annealed aluminium alloys

The elastic properties of four annealed polycrystalline commercial aluminium alloys were studied between 4 and 300 K using a pulse-superposition method. Results are given for longitudinal sound velocity, transverse sound velocity, Young's modulus, shear modulus, bulk modulus (reciprocal compressibility), Poisson's ratio, and elastic Debye temperature. The elastic stiffnesses of the alloys increase 4 to 13% on cooling from room temperature to liquid helium temperature. The elastic constant-temperature curves exhibit regular behaviour.