Fabrication and enhanced mechanical properties of porous PLA/PEG copolymer reinforced with bacterial cellulose nanofibers for soft tissue engineering applications

A new class of polylactic acid (PLA)/polyethylene glycol (PEG) copolymer reinforced with bacterial cellulose nanofibers (BC) was prepared using a solvent casting and particulate leaching methods. Four weight fractions of BC (1, 2.5, 5, and 10 wt%) were incorporated into copolymer via silane coupling agent. Mechanical properties were evaluated using response surface method (RSM) to optimize the impact of pore size, porosity, and BC contents. Compressive strength obtained for PLA/PEG-5 BC wt% was 9.8 MPa, which significantly dropped after developing a porous structure to 4.9 MPa. Nielson model was applied to investigate the BC stress concentration on the PLA/PEG. Likewise, krenche and Hapli-Tasi model were employed to investigate the BC nanofiber reinforcement and BC orientation into PLA/PEG chains. The optimal parameters of the experiment results found to be 5 wt% for BC, 230 μm for pore size, and 80% for porosity. Scanning electron microscopy (SEM) micrograph indicates that uniform pore size and regular pore shape were achieved after an addition of BC-5% into PLA/PEG. The weight loss of copolymer-BC with scaffolds enhanced to the double values, compared with PLA/PEG-BC % without scaffolds. Differential Scanning Calorimetric (DSC) results revealed that the BC nanofiber improved glass transition temperature (T_g) 57 °C, melting temperature (T_m) 171 °C, and crystallinity (χ %) 43% of PLA/PEG reinforced-BC-5%.     

Synthesis,Characterization, and Hydrolytic Degradation of Polylactide/Poly(ethylene glycol)/Nano-silica Composite Films

Poly(lactic acid) (PLA)/PEG/nano-silica composite degradable films have been prepared by solvent casting method. IR measurements showed that vibration of C–O–C group was confined by silica network. SEM results showed that nano-silica particles were dispersed uniformly in the PLA/PEG matrix. TGA results indicated that the thermal decomposition temperature rose with the increase of nano-silica content. The tensile strength of composite film increased by the addition of nano-silica particles into PLA/PEG matrix. The degradation rate of PLA/PEG/nano-silica composites increased with the acidic medium of degradation. On the other hand, the slower degradation was obtained in the neutral buffer solution. PLA/PEG/nano-silica composites were found to exhibit almost similar degradation behavior as that of PLA/PEG films.     

Characterization of form-stable phase-change material for solar photovoltaic cooling

Solar PV panel cooling is essential to achieve maximum efficiency of PV modules. Phase-change material (PCM) is one of the prominent options to cool the panel and reduce the temperature, since PCMs have low thermal conductivity. Expanded graphite particles are used to enrich the structure and stability as well as to increase the thermal properties. In the present research work, polyethylene glycol (PEG) 1000 is used as a base material and expanded graphite for inclusive particle. A novel form-stable PEG1000/EG composite PCM mixture is prepared, using impregnation and dispersion method. Expanded graphite and PEG1000/EG sample phase compositions are investigated, using X-ray diffraction technique. No new peak is identified in the composite PCM sample. The surface morphology and structure of EG and PEG1000/EG are investigated, using scanning electron microscopy (SEM). Chemical stability analysis is done by Fourier-transform infrared spectroscopy. Thermal properties of the prepared composite PCMs are analysed by differential scanning calorimetry, thermogravimetric analysis (TGA) and KD2 pro analyser. Results show that addition of EG in various propositions (5%, 10% and 15%) enhances the thermal conductivity of PCM samples from 0.3654 to 1.7866 W mK^?1, while melting point and latent heat of fusion of PCM samples are getting reduced. TGA thermographs are used to investigate the thermal stability of the composite PCM samples. TGA curves show that loss of mass happens above the operating temperature, and it is varied with different mass ratios of EG. Characterization of the prepared composite PCM samples is compared and found that PEG1000-85%/EG-15% is the best form-stable PCM, suitable for cooling the solar PV panel as well as to improve the electrical efficiency coupled with a decrease of temperature in the range of 35 °C to 40 °C.

     

Effect of different additives on bacterial cellulose production by Acetobacter xylinum and analysis of material property

Bacterial cellulose (BC) demonstrates unique properties including high mechanical strength, high crystallinity, and high water retention ability, which make it an useful material in many industries, such as food, paper manufacturing, and pharmaceutical application. In this study, different additives including agar, carboxymethylcellulose (CMC), microcrystalline cellulose, and sodium alginate were added into fermentation medium in agitated culture to enhance BC production by Acetobacter xylinum. The optimal additive was chosen based on the amount of BC produced. The produced BC was analyzed by using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), thermogravimetric analysis (TGA), and dynamic mechanical analysis (DMA). Among the evaluated additives, CMC yielded highest BC production (8.2 g/L) compared to the control (1.3 g/L). The results also indicated that CMC-altered BC production increased with CMC addition and reached saturation around 1%. The variation between replicates for all analysis was <5%. From XRD analysis, however, the crystallinity and crystal size decreased as CMC addition increased. FESEM results showed CMC-altered BC produced from agitated culture retained its interweaving property. TGA results demonstrated that CMC-altered BC had about 98% water retention ability, which is higher than BC pellicle produced with static culture. CMC-altered BC also exhibited higher T _max compared to control. Finally, DMA results showed that BC from agitated culture loses its mechanical strength in both stress at break and Young’s modulus when compared to BC pellicle. This study clearly demonstrated that addition of CMC enhanced BC production and slightly changed its structure.     

Morphology and thermal stability of bacterial cellulose/collagen composites

The aim of this paper was to prepare composites of bacterial cellulose (BC) and collagen to evaluate both the effect of collagen on the morphological, mechanical and thermal properties of BC and the effect of BC on the thermal stability of collagen for designing composites with increased potential biomedical applications. Two series of composites were prepared, the first series by immersing BC pellicle in solutions of collagen obtained in three forms, collagen gel (CG), collagen solution (CS) and hydrolysed collagen (HC), followed by freeze drying; and the second series of composites by mixing BC powder in solutions of collagen (CG, CS and HC), also followed by freeze drying. The properties of obtained composites were evaluated by Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), mechanical tests, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The results revealed that BC acts as a thermal stabilizer for CS matrix, while with CG matrix it interacts synergistically leading to composites with improved properties. On the other hand, the BC sheet impregnated with collagen has a significantly improved thermal stability. Collagen (as HC, CS or CG) has also a positive influence on the mechanical properties of lyophilized BC sheet. A four times increase of modulus was observed in BC/HC and BC/CG composites. and an increase of 60 times for BC/CS. The spectacular increase of elastic modulus and tensile strength in the case of BC/CS composite was explained by the easier penetration of collagen solution in the BC network and impregnation of BC fibrils as revealed by SEM and AFM analyzes.

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Nanocomposite films based on TEMPO-mediated oxidized bacterial cellulose and chitosan

Nanobacterial cellulose (BC) and chitosan (CH) have similar molecular structures. In the present work, nanocomposite films based on BC and CH were prepared by stepwise modification instead of by conventional physical blending. First, surface C6-carboxylated BC was prepared in a bromide-free system using 2,2,6,6-tetramethylpyperidine-1-oxyl (TEMPO) as a catalyst. The carboxylate groups of oxidised BC could couple to the amine groups of CH. The composite films were characterised by attenuated total reflectance Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and Carbon-13 solid nuclear magnetic resonance ¹³C NMR. The results showed that a cross-linking reaction occurred between TEMPO-mediated oxidised BC and CH. Even in the absence of cross-linkers, these two biopolymers could interact with each other because of their structural similarity. SEM images and tensile tests showed that the TEMPO-oxidized BC and CH composite film prepared at a 0.5:1 ratio was an exception. The mechanical properties of the composite films decreased with increasing CH content, passed through a minimum, and then increased. To explain this phenomenon, we propose that the hydrogen bonding in the original BC microstructure plays a decisive role in the modified nanocomposites. However, BC/CH composites with excellent properties could be synthesised at appropriate reactant ratios.     

Microstructure and mechanical properties of bacterial cellulose/chitosan porous scaffold

A family of polysaccharide based scaffold materials, bacterial cellulose/chitosan (BC/CTS) porous scaffolds with various weight ratios (from 20/80 to 60/40 w/w%) were prepared by freezing (−30 and −80 °C) and lyophilization of a mixture of microfibrillated BC suspension and chitosan solution. The microfibrillated BC (MFC) was subjected to 2,2,6,6-tetramethylpyperidine-1-oxyl radical (TEMPO)-mediated oxidation to introduce surface carboxyl groups before mixing. The integration of MFC within chitosan matrix was performed by 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC)-mediated cross-linking. The covalent amide bond formation was determined by ATR-FTIR. Because of this covalent coupling, the scaffolds retain their original shapes during autoclave sterilization. The composite scaffolds are three-dimensional open pore microstructure with pore size ranging from 120 to 280 μm. The freezing temperature and mean pore size take less effect on scaffold mechanical properties. The compressive modulus and strength increased with increase in MFC content. The results show that the scaffolds of higher MFC content contribute to overall better mechanical properties.     

层状纳米纤维素膜/PVA复合水凝胶的制备与力学性能研究

采用叠层复合与物理相分离的方法制备了层状纳米细菌纤维素(BC)膜/聚乙烯醇( PVA)复合水凝胶.研究了聚乙烯醇的质量百分数、BC膜的复合层数以及制备条件对复合水凝胶力学性能的影响;通过扫描电镜( SEM)观察比较了复合水凝胶中BC膜层与PVA界面结合情况.结果表明,复合水凝胶的力学性能与PVA的质量百分数和BC膜含水...     

细菌纤维素/聚丙烯酰胺水凝胶的制备及性能表征

通过自由基聚合在细菌纤维素(BC)网络中引入聚丙烯酰胺(PAM),制备了细菌纤维素/聚丙烯酰胺(BC/PAM)复合水凝胶,并采用扫描电子显微镜(SEM)、红外光谱(IR)、热失重分析(TGA)、X射线衍射(XRD)和力学测试等手段对复合凝胶的结构和性能进行了研究.研究结果显示在复合水凝胶中,虽然PAM自身没有交联,但由...     

The electrospun poly(ε‐caprolactone)/fluoridated hydroxyapatite nanocomposite for bone tissue engineering

Biodegradable cell‐incorporated scaffolds can guide the regeneration process of bone defects such as physiological resorption, tooth loss, and trauma which medically, socially, and economically hurt patients. Here, 0, 5, 10, and 15 wt% fluoridated hydroxyapatite (FHA) nanoparticles containing 25 wt% F^? and 75 wt% OH^? were incorporated into poly(ε‐caprolactone) (PCL) matrix to produce PCL/FHA nanocomposite scaffolds using electrospinning method. Then, scanning electron microscopy (SEM), X‐ray diffraction (XRD) pattern, and Fourier transform infrared spectroscopy (FTIR) were used to evaluate the morphology, phase structure, and functional groups of prepared electrospun scaffolds, respectively. Furthermore, the tensile strength and elastic modulus of electrospun scaffolds were investigated using the tensile test. Moreover, the biodegradation behavior of electrospun PCL/FHA scaffolds was studied by the evaluation of weight loss of mats and the alternation of pH in phosphate buffer saline (PBS) up to 30 days of incubation. Then, the biocompatibility of prepared mats was investigated by culturing MG‐63 osteoblast cell line and performing MTT assay. In addition, the adhesion of osteoblast cells on prepared electrospun scaffolds was studied using their SEM images. Results revealed that the fiber diameter of prepared electrospun PCL/FHA scaffolds alters between 700 and 900 nm. The mechanical assay illustrated the mat with 10 wt% FHA nanoparticles revealed the highest tensile strength and elastic modulus. The weight loss alternation of mats determined around 1% to 8% after 30 days of incubation. The biocompatibility and cell adhesion of mats improved by increasing the amounts of FHA nanoparticles.     

Biodegradable polyester/modified mesoporous silica composites for effective bone repair with self‐reinforced properties

A series novel composites based on poly(_L‐lactide) (PLLA) oligomer modified mesoporous silica (MCM41) homogeneous dispersed into poly(_L‐lactide‐co‐trimethylene carbonate‐co‐glycolide) (PLTG) terpolymer has been successfully prepared. The structure of PLTG terpolymer was characterized by ¹H NMR. The structure and properties of modified and unmodified MCM41 were attested by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analyzer (TGA), X‐ray diffraction (XRD), N₂ adsorption–desorption, scanning electron microscope (SEM), and transmission electron microscope (TEM), which demonstrated that the MCM41 was successfully grafted by the PLLA oligomer. The effect of different concentration of modified MCM41 in PLTG matrix on thermal properties, mechanical properties, and hydrophilicity was investigated by TGA, differential scanning calorimetry (DSC), mechanical testing, contact angle measurement, and SEM. The results of mechanical tests showed that 5 wt% of modified MCM41 nanoparticles gave rise to optimal reinforcing effect. The tensile strength, Young's modulus, and elongation at break of the PLTG/PLLA‐MCM41 (5%) composites were 33.2 Mpa, 1.58 Gpa, and 268.7%, respectively, which were all higher than the PLTG/MCM41 (5%) composites and pristine PLTG matrix, which were due to good interfacial adhesion between the PLTG matrix and MCM41 nanoparticles. TGA and DSC have shown that 5% modified MCM41 in the PLTG increased the temperature of composite degradation and T_g. Water contact angle measurement showed the hydrophilicity of the composites increases with the increase of modified MCM41 content. The live/dead assay showed that the modified MCM41 existing on the PLTG matrix presents very excellent cytocompatibility. Therefore, the novel composite material represents promising way for bone tissue engineering application.     

Enhancement of mechanical and thermal properties of oil palm empty fruit bunch fiber poly(butylene adipate-co-terephtalate) biocomposites by matrix esterification using succinic anhydride

In this work, the oil palm empty fruit bunch (EFB) fiber was used as a source of lignocellulosic filler to fabricate a novel type of cost effective biodegradable composite, based on the aliphatic aromatic co-polyester poly(butylene adipate-co-terephtalate) PBAT (Ecoflex?), as a fully biodegradable thermoplastic polymer matrix. The aim of this research was to improve the new biocomposites' performance by chemical modification using succinic anhydride (SAH) as a coupling agent in the presence and absence of dicumyl peroxide (DCP) and benzoyl peroxide (BPO) as initiators. For the composite preparation, several blends were prepared with varying ratios of filler and matrix using the melt blending technique. The composites were prepared at various fiber contents of 10, 20, 30, 40 and 50 (wt %) and characterized. The effects of fiber loading and coupling agent loading on the thermal properties of biodegradable polymer composites were evaluated using thermal gravimetric analysis (TGA). Scanning Electron Microscopy (SEM) was used for morphological studies. The chemical structure of the new biocomposites was also analyzed using the Fourier Transform Infrared (FTIR) spectroscopy technique. The PBAT biocomposite reinforced with 40 (wt %) of EFB fiber showed the best mechanical properties compared to the other PBAT/EFB fiber biocomposites. Biocomposite treatment with 4 (wt %) succinic anhydride (SAH) and 1 (wt %) dicumyl peroxide (DCP) improved both tensile and flexural strength as well as tensile and flexural modulus. The FTIR analyses proved the mechanical test results by presenting the evidence of successful esterification using SAH/DCP in the biocomposites' spectra. The SEM micrograph of the tensile fractured surfaces showed the improvement of fiber-matrix adhesion after using SAH. The TGA results showed that chemical modification using SAH/DCP improved the thermal stability of the PBAT/EFB biocomposite.     

Bacterial cellulose/gelatin composites: in situ preparation and glutaraldehyde treatment

Bacterial cellulose (BC)/GEL composites were prepared in situ by adding gelatin into BC-producing culture medium. The addition of gelatin interfered with the formation of the BC pellicle structure and thus made the BC yield and growth rate quite different from that of pure BC. Scanning electron microscope images showed that the width of cellulose ribbons became narrower than that of pure BC and the gelatin filled in the pores of BC to form a dense structure. The addition level of gelatin significantly influences the yield of BC/GEL composites. An optimum value of 0.5 wt/v% gelatin was attained, with which the highest yield of 0.0541 g/100 mL was achieved. Under this condition, the weight percentage of gelatin in BC/GEL composite was 65 wt%. BC/GEL composites were treated with glutaraldehyde to crosslink BC fibrils and gelatin. The crosslinking degree, determined by the concentration of glutaraldehyde and crosslinking time, could affect the swelling behavior, thermal stability and mechanical properties of composites. With increasing of the crosslinking degree, the crystallinity index and swelling behavior of the composites decreased. The increase in the crosslinking degree also descreased the composite’s strain at break in elongation but increased the compressive and tensile strength. Covalent bonding between BC and gelatin provides good strength retention to the glutaraldehyde-treated composites with a high crosslinking degree. Considering the cytocompatibility and properties of composites, the most appropriate concentration of glutaraldehyde and crosslinking time were 1.0 wt/v% and 24 h, respectively.     

Effects of annealing and the addition of PEG on the PVA based hydrogel by gamma ray

Poly(vinyl alcohol) (PVA) is an interesting material with good biocompatibility, high elasticity and hydrophilic characteristics. PVA hydrogels have been formed through chemical crosslinking with aldehyde, photopolymerization and physical crosslinking with freeze-thawing. In this study, crosslinked hydrogels based on PVA, and poly(ethylene glycol) (PEG) were prepared by gamma-ray irradiation, and then annealed at 120 °C. The properties of a hydrogel such as gel fraction, swelling behavior, gel strength as a function of PEG content and annealing time were investigated. Also, the thermal behaviors were examined by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The gel fraction decreases with an increase in PEG content and decrease in annealing time. The tensile strength increases with an increase in annealing time. The thermal behaviors have shown different patterns according to the annealing time. The improved properties suggest that PVA/PEG blend hydrogel can be a good candidate for applications in the articular cartilage.     

Design of aluminum trihydroxide and P‐N core‐shell structures and their synergistic effects on halogen‐free flame‐retardant polyethylene composites

In order to improve the performance of inorganic/organic composites, aluminum trihydroxide (ATH) core composites with a styrene‐ethylene‐butadiene‐styrene block copolymer grafted with maleic anhydride (MAH‐g‐SEBS) shell phase, and P‐N flame retardant as a synergistic agent, were prepared through an interface design. The effects of polyethylene glycol (PEG) content on the interfacial interaction, flame retardancy, thermal properties, and mechanical properties of high‐density polyethylene (HDPE)/ATH composites were investigated by small angle X‐ray diffraction, rotational rheometer, limiting oxygen index, thermogravimetric analysis (TGA), and tensile testing. The ATH synergistic effects of P‐N flame‐retardant improved the combustion performance of HDPE/ATH/PEG(3%)/MAH‐g‐SEBS/P‐N (abbreviated as HDPE/MH3/M‐g‐S/P‐N) composite by forming more carbon layer, increased the elongation at break from 21% to 558% compared to HDPE/ATH, and increased the interface thickness from 0.447 to 0.891 nm. SEM results support the compatibility of ATH with HDPE increased and the interfacial effect was enhanced. TGA showed the maximum decomposition temperature of the two stages and the yield of the residue at high temperature increased first and then decreased with the increase of PEG content. Rheological behavior showed the storage modulus, complex viscosity, and the relaxation time initially increased and then decreased with the increase of PEG content indicating PEG, M‐g‐S, and ATH powder gradually formed a partial coating, then a full coating, and finally an over‐coated core‐shell structured model.     

Microencapsulated ammonium polyphosphate with polyurethane shell: preparation,characterization, and its flame retardance in polyurethane

A series of polyurethane (PU) microencapsulated ammonium polyphosphate (MCAPP) were prepared by in situ polymerization from toluene‐2,4‐diisocyanate (TDI), polyethylene glycol (PEG), and pentaerythtritol (PER). And the structure was characterized by Fourier transform infrared spectroscopy (FTIR) and X‐ray photoelectron spectroscopy (XPS). Then it chose the optimal PEG constituent to design microcapsule from scanning electron microscopy (SEM) and water solubility test. The combustion and thermal degradation behaviors of PU blended APP or MCAPP were investigated by thermogravimetric analysis (TGA), UL‐94 test, and microcombustion calorimetry. The results showed that the PU/MCAPP had better thermal stability and flame retardance, due to the stable char forming by APP and PU shell. Moreover, the water resistance of flame retarded PU composite was greatly improved. Copyright © 2009 John Wiley & Sons, Ltd.     

Composite polyphosphazene membranes doped with phosphotungstic acid and silica

Poly（bis（phenoxy）phosphazene） （SPBPP）/phosphotungstic acid （PWA）/silica composite membranes for fuel cells were prepared. The composite membranes were characterized by using FTIR, TGA and SEM techniquies. Incorporation of PWA particles and silica particles into the SPBPP polymer matrix and a specific interaction between them were confirmed by FTIR spectra. TGA results showed that the composite membranes had high thermal stability. Homogeneous distribution of PWA and silica particles within the SPBPP matrix was verified by SEM micrographs. The doped membranes showed increased water uptake and proton conductivity.     

氧杂环丁烷/丙烯酸酯混杂体系的光固化性能研究

以氧杂环丁烷和丙烯酸酯为主要原料,加入一定量光引发剂配制成一种新型的光固化混杂体系。研究了混杂体系中引发剂的协同作用,结果显示自由基引发剂对阳离子引发剂有增感作用。通过吸水性测试、红外光谱（FTIR）、热重分析（TGA）、扫描电镜（SEM）等手段研究了固化膜的性能,结果显示混杂固化膜的力学性能、耐溶剂性能和热稳定性要优于自由基固化膜,这是由于混杂体系在固化过程中形成了高分子互穿网络结构（IPN）,其中混杂固化膜的拉伸强度为10.34 MPa,断裂伸长率为10.13%,冲击强度为15 kg·cm,附着力为1级,柔韧性小于3 mm,耐丙酮来回擦拭次数为200次。     

All-cellulose nanocomposites by surface selective dissolution of bacterial cellulose

All-cellulose nanocomposites using bacterial cellulose (BC) as a single raw material were prepared by a surface selective dissolution method. The effect of the immersion time of BC in the solvent (lithium chloride/N,N-dimethylacetamide) during preparation on the nanocomposite properties was investigated. The structure, morphology and mechanical properties of the nanocomposites were characterized by X-ray diffraction, scanning electron microscopy, and tensile testing. The optimum immersion time of 10 min allowed the preparation of nanocomposites with an average tensile strength of 411 MPa and Young’s modulus of 18 GPa. With the longest immersion time of 60 min, the prepared composite sheet turns to express a very high toughness characteristic possessing a work-to-fracture as high as 16 MJ/m³. These biobased nanocomposites show high performances thanks to their unique structure and properties.