scholarly journals Introducing the Newly Isolated Bacterium Aneurinibacillus sp. H1 as an Auspicious Thermophilic Producer of Various Polyhydroxyalkanoates (PHA) Copolymers–2. Material Study on the Produced Copolymers

Polymers ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 1298
Author(s):  
Petr Sedlacek ◽  
Iva Pernicova ◽  
Ivana Novackova ◽  
Xenie Kourilova ◽  
Michal Kalina ◽  
...  
Keyword(s):  
Enzymatic Degradation ◽  
Crystalline Lattice ◽  
Degree Of Crystallinity ◽  
Positive Bacterium ◽  
X Ray ◽  
Moderately Thermophilic ◽  
Monomer Composition ◽  
Cultivation Process ◽  
Pha Copolymers ◽  
Material Study

Aneurinibacillus sp. H1 is a promising, moderately thermophilic, novel Gram-positive bacterium capable of the biosynthesis of polyhydroxyalkanoates (PHA) with tunable monomer composition. In particular, the strain is able to synthesize copolymers of 3-hydroxybutyrate (3HB), 4-hydroxybutyrate (4HB) and 3-hydroxyvalerate (3HV) with remarkably high 4HB and 3HV fractions. In this study we performed an in-depth material analysis of PHA polymers produced by Aneurinibacillus sp. H1 in order to describe how the monomer composition affects fundamental structural and physicochemical parameters of the materials in the form of solvent-casted films. Results of infrared spectroscopy, X-ray diffractometry and thermal analysis clearly show that controlling the monomer composition enables optimization of PHA crystallinity both qualitatively (the type of the crystalline lattice) and quantitatively (the overall degree of crystallinity). Furthermore, resistance of the films against thermal and/or enzymatic degradation can also be manipulated by the monomer composition. Results of this study hence confirm Aneurinibacillus sp. H1 as an auspicious candidate for thermophilic production of PHA polymers with material properties that can be tuned together with their chemical composition by the corresponding adjustment of the cultivation process.

Kinetics of crystallization of biodegradable PHA copolymers: a combined X-ray scattering and micro-indentation study

2011 ◽  
Vol 1301 ◽  
Author(s):  
Maraolina Domínguez-Díaz ◽  
Araceli Flores ◽  
Angel Romo-Uribe ◽  
Rodolfo Cruz-Silva
Keyword(s):  
Room Temperature ◽  
Degree Of Crystallinity ◽  
Indentation Hardness ◽  
X Ray ◽  
X Ray Scattering ◽  
Biodegradable Poly ◽  
Pha Copolymers ◽  
Ice Water ◽  
Kinetics Of ◽  
Ray Scattering

ABSTRACTWide Angle X-ray scattering (WAXS) and indentation hardness have been used to study the development of crystallinity at room temperature of biodegradable poly(hydroxybutyrate) (PHB) and its copolymer with hydroxyvalerate (PHB/HV) containing 12% of valerate. Measurements were carried out immediately after quenching the samples from the molten state (200 ºC) in ice water and over two weeks of storage at room temperature. WAXS showed that the crystallization of the PHB-based polymers initiated within the first minutes of storage at room temperature, the copolymer displaying a higher rate of crystallization than the homopolymer. For all samples, the degree of crystallinity,α, nearly reached a plateau value within the first hour of crystallization. Concurrently to the development of crystallinity, microhardness values,H, clearly rose as crystallization occurred. Monitoring the crystallization for over two weeks showed that after the rapid increase ofαandH, there was a slow monotonic growth of these properties. A correlation between nanostructure and microhardness is found at all stages of the crystallization process.

Synthesis, characterisation and properties of aramid copolymers prepared from AB and AB2 monomers

e-Polymers ◽  
2003 ◽  
Vol 3 (1) ◽  
Author(s):  
Orietta Monticelli ◽  
Stefano Fiori ◽  
Alberto Mariani ◽  
Saverio Russo ◽  
Hartmut Komber
Keyword(s):  
Liquid Crystalline ◽  
Reaction Medium ◽  
Aromatic Polyamide ◽  
Degree Of Crystallinity ◽  
Feed Ratio ◽  
Structure Evolution ◽  
Monomer Composition ◽  
Degradation Temperature ◽  
Monomer Feed ◽  
Monomer Feed Ratio

Abstract Aromatic polyamide (aramid) copolymers having a highly branched architecture were prepared by direct polycondensation of an AB2 monomer (5-(4-aminobenzoylamino) isophthalic acid) with an AB monomer (N-(4-aminophenyl)terephthalamic acid). Two synthetic routes have been followed for copolymer preparation, differing from each other in the overall monomer content and the type of salts added to the reaction medium (LiCl or LiCl + CaCl2). Otherwise, both methods used the same conditions and the same condensing agent (triphenyl phosphite). The feed ratio of the monomers affected the copolymer solubility in aprotic polar solvents such as N,N-dimethylformamide, N-methylpyrrolidone and dimethyl sulfoxide. Only high AB2/AB monomer ratios allowed obtaining completely soluble polymers in the above media. Also copolymer intrinsic viscosity was influenced by that ratio as well as by the polymerisation routes. IR measurements gave an indication of polymer structure evolution as a function of the monomer feed ratio, while 1H NMR experiments verified the actual monomer composition in the synthesized polymers. The monomer feed ratio turned out to influence polymer properties, such as degree of crystallinity, thermal degradation temperature and liquid crystalline behaviour. Some of the characterisation techniques we used (1H and 31P NMR, IR, SEM-EDS) revealed the presence of phosphorus derivatives in the copolymers, despite extensive sample purification. This presence is coming from derivatives of the condensing agent, and is directly related to the content of AB2-type structures present in the copolymers.

X-Ray-Optical Multilayer Structures Studied Using High Resolution Electron Microscopy.

1986 ◽  
Vol 77 ◽  
Author(s):  
Mary Beth Stearns ◽  
Amanda K. Petford-Long ◽  
C.-H. Chang ◽  
D. G. Stearns ◽  
N. M. Ceglio ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
High Resolution ◽  
Substrate Surface ◽  
High Resolution Electron Microscopy ◽  
Atomic Scale ◽  
Degree Of Crystallinity ◽  
Multilayer Systems ◽  
Layer Width ◽  
X Ray ◽  
Resolution Electron

ABSTRACTThe technique of high resolution electron microscopy has been used to examine the structure of several multilayer systems (MLS) on an atomic scale. Mo/Si multilayers, in use in a number of x-ray optical element applications, and Mo/Si multilayers, of interest because of their magnetic properties, have been imaged in cross-section. Layer thicknesses, flatness and smoothness have been analysed: the layer width can vary by up to 0.6nm from the average value, and the layer flatness depends on the quality of the substrate surface for amorphous MLS, and on the details of the crystalline growth for the crystalline materials. The degree of crystallinity and the crystal orientation within the layers have also been investigated. In both cases, the high-Z layers are predominantly crystalline and the Si layers appear amorphous. Amorphous interfacial regions are visible between the Mo and Si layers, and crystalline cobalt suicide interfacial regions between the Co and Si layers. Using the structural measurements obtained from the HREM results, theoretical x-ray reflectivity behaviour has been calculated. It fits the experimental data very well.

Synthesis of Amorphous Zirconium Dioxide from Zirconyl Nitrate in Presence of Oxalic Acid

2021 ◽  
Vol 316 ◽  
pp. 127-133
Author(s):  
Yuriy Velyaev ◽  
Ilona Kometiani ◽  
Olga Miroshnichenko
Keyword(s):  
Oxalic Acid ◽  
Zirconium Dioxide ◽  
Spherical Particles ◽  
Degree Of Crystallinity ◽  
Optimum Temperature ◽  
Sorbed Water ◽  
Zirconyl Nitrate ◽  
X Ray ◽  
Low Degree ◽  
Gel Drying

The article presents the results of studies on preparation of amorphous zirconium dioxide from zirconium nitrate by its hydrolysis in the presence of oxalic acid. It is determined that the balance of reagents taken for synthesis (1 ml 0,025 M ZrO(NO3)2 is 1.35 ml 4 M HOOC-COOH), and the optimum temperature of the received gel drying, which is 230 ̊С, is established, too. Morphology of the obtained ZrO2 samples was explored. It has been found that the calcining temperature is independent of the size and shape forming irregular agglomerates, consisting of smaller spherical particles, whose diameter varies between 50 and 300 nm. The X-ray analysis of the sample is represented, which showed a low degree of crystallinity of the substance. IR spectroscopy data showed the presence of zirconium dioxide-characteristic peaks on the IR spectrum. The same spectrum reflects the presence of a large amount of sorbed water in the obtained sample, as well as peaks characteristic of the gas adsorbed by the sample from the environment.

scholarly journals Effect of indium content on X- ray diffraction and optical constants of InxSe1-x thin films

2019 ◽  
Vol 14 (29) ◽  
pp. 55-72
Author(s):  
Bushra A. Hasan
Keyword(s):  
Thin Films ◽  
Optical Constants ◽  
Indium Content ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Dispersion Energy ◽  
X Ray ◽  
Evaporation Technique ◽  
High Indium Content ◽  
Diffraction Patterns

Alloys of InxSe1-x were prepared by quenching technique withdifferent In content (x=10, 20, 30, and 40). Thin films of these alloyswere prepared using thermal evaporation technique under vacuum of10-5 mbar on glass, at room temperature R.T with differentthicknesses (t=300, 500 and 700 nm). The X–ray diffractionmeasurement for bulk InxSe1-x showed that all alloys havepolycrystalline structures and the peaks for x=10 identical with Se,while for x=20, 30 and 40 were identical with the Se and InSestandard peaks. The diffraction patterns of InxSe1-x thin film showthat with low In content (x=10, and 20) samples have semicrystalline structure, The increase of indium content to x=30decreases degree of crystallinity and further increase of indiumcontent to x=40 leads to convert structure to amorphous. Increase ofthickness from 300 to 700nm increases degree of crystallinity for allindium content. Transmittance measurements were used to calculaterefractive index n and the extinction coefficient k using Swanepole’smethod. The optical constants such as refractive index (n), extinctioncoefficient (k) and dielectric constant (εr, εi) increases for low indiumcontent samples and decreases for high indium content samples,while increase of thickness increases optical constants for all xvalues. The oscillator energy E0, dispersion energy Ed, and otherparameters have been determined by Wemple - DiDomenico singleoscillator approach.

scholarly journals Synthesis and Characterization of alumina nanofiber reinforced Poly ether ether ketone (PEEK)

2014 ◽  
Vol 7 (2) ◽  
Author(s):  
Tg Mahizatulazwa Tg Kamaruddin ◽  
Liew Kong Yong ◽  
Mohd Ridzuan Noordin
Keyword(s):  
Degree Of Crystallinity ◽  
Nano Composites ◽  
Scanning Electron Micrographs ◽  
X Ray ◽  
Alumina Nanofibers ◽  
Transmission Electron ◽  
Ether Ether Ketone ◽  
Poly Ether Ether Ketone ◽  
Ether Ketone

The effects of reinforcing Poly ether etherketone (PEEK) with alumina nanofiber have been studied. The nano-composites were prepared by first dispersing the fibre in solvent and then undertaking the synthesis of PEEK. Nanocomposite materials with 1wt.%, 2.5wt.% and 5wt.% of alumina nanofiber have been prepared successfully by dispersing the alumina nanofiber in Sulfolane as solvent and upon sonication for 30 minutes. Transmission electron microscopy and scanning electron micrographs indicated excellent dispersion and interactions between PEEK matrixes with the added alumina nanofibers. Differential scanning calorimeter shows changes in melting and crystallization point and degree of crystallinity for 1wt.% nanocomposites. The result also indicated that alumina nanofiber serves as nucleating agents in PEEK nanocomposites. The X-ray diffractogram data indicated that the crystallinity of the PEEK nanocomposites was highest for 1wt.% alumina nanofiber. The thermogravimetry analysis, shows that thermal stability for alumina nanofiber/PEEK nano-composites was enhanced compared to that of the pure PEEK.

Preparation of nanocellulose by hydrolysis with ionic liquids and two-step hydrolysis with ionic liquids and enzymes

2021 ◽  
Vol 116 ◽  
pp. 5-14
Author(s):  
Marta Babicka ◽  
Magdalena Woźniak ◽  
Kinga Szentner ◽  
Sławomir Borysiak ◽  
Krzysztof Dwiecki ◽  
...  
Keyword(s):  
Ionic Liquids ◽  
Degree Of Crystallinity ◽  
Cellulolytic Enzyme ◽  
X Ray Diffraction ◽  
Production Methods ◽  
Step Process ◽  
X Ray ◽  
One Step ◽  
Xrd Patterns ◽  
The One

The aim of this study was to compare parameters of nanocellulose obtained by two different procedures: hydrolysis with ionic liquids (1-allyl-3-methylimidazolium chloride and 1-ethyl-3-methylimidazolium acetate) and hydrolysis with ionic liquids in combination with hydrolysis using a cellulolytic enzyme from Trichoderma reesei. Avicel cellulose was treated with two ionic liquids: 1-allyl-3-methylimidazolium chloride (AmimCl) and 1-ethyl 3-methylimidazolium acetate (EmimOAc). In the two-step hydrolysis cellulose after treatment with ionic liquids was additionally hydrolyzed with a solution of enzymes. In order to characterize the obtained material, the following analyses were used: infrared spectroscopy, X-ray diffraction and dynamic light scattering. The results indicated that cellulose obtained by two-step nanocellulose production methods (first hydrolysis with ionic liquids and then with enzymes) showed similar parameters (particle size, XRD patterns and degree of crystallinity) as the material after the one-step process, i.e. hydrolysis with ionic liquids.

scholarly journals Synthesis, Physical Properties and Enzymatic Degradation of Biodegradable Nanocomposites Fabricated Using Poly(Butylene Carbonate-Co-Terephthalate) and Organically Modified Layered Zinc Phenylphosphonate

Polymers ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 2149
Author(s):  
Li-Ying Tseng ◽  
Erh-Chiang Chen ◽  
Jie-Mao Wang ◽  
Tzong-Ming Wu
Keyword(s):  
Nmr Spectra ◽  
Enzymatic Degradation ◽  
Molar Ratio ◽  
Wide Angle ◽  
Mixing Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Organically Modified ◽  
Biodegradable Nanocomposites

A new biodegradable aliphatic-aromatic poly (butylene carbonate-co-terephthalate) (PBCT-85) with the molar ratio [BC]/[BT] = 85/15, successfully synthesized through transesterification and polycondensation processes, was identified using 1H-NMR spectra. Various weight ratios of PBCT/organically modified layered zinc phenylphosphonate (m-PPZn) nanocomposites were manufactured using the solution mixing process. Wide-angle X-ray diffraction and transmission electron microscopy were used to examine the morphology of PBCT-85/m-PPZn nanocomposites. Both results exhibited that the stacking layers of m-PPZn were intercalated into the PBCT-85 polymer matrix. The additional m-PPZn into PBCT-85 copolymer matrix significantly enhanced the storage modulus at −70 °C, as compared to that of neat PBCT-85. The lipase from Pseudomonas sp. was used to investigate the enzymatic degradation of PBCT-85/m-PPZn nanocomposites. The weight loss decreased as the loading of m-PPZn increased, indicating that the existence of m-PPZn inhibits the degradation of the PBCT-85 copolymers. This result might be attributed to the higher degree of contact angle for PBCT-85/m-PPZn nanocomposites. The PBCT-85/m-PPZn composites approved by MTT assay are appropriate for cell growth and might have potential in the application of biomedical materials.

scholarly journals Characterization of Serpentines from Different Regions by Transmission Electron Microscopy, X-ray Diffraction, BET Specific Surface Area and Vibrational and Electronic Spectroscopy

Fibers ◽  
2019 ◽  
Vol 7 (5) ◽  
pp. 47 ◽  
Author(s):  
Miguel A. Rivero Crespo ◽  
Dolores Pereira Gómez ◽  
María V. Villa García ◽  
José M. Gallardo Amores ◽  
Vicente Sánchez Escribano
Keyword(s):  
Electron Microscopy ◽  
Relative Intensity ◽  
Electronic Spectroscopy ◽  
Visible Region ◽  
Band Gap Energy ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Oh Groups ◽  
X Ray ◽  
Xrd Patterns

Serpentinite powdered samples from four different regions were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), SBET and porosity measurements, UV-Vis and Infrared Spectroscopy of the skeletal region and surface OH groups. SEM micrographs of the samples showed a prismatic morphology when the lizardite was the predominant phase, while if antigorite phase prevailed, the particles had a globular morphology. The few fibrous-shaped particles, only observed by SEM and weakly detected by XRD on MO-9C and MO13 samples, were characteristic of the chrysotile phase. All diffraction XRD patterns showed characteristic peaks of antigorite and lizardite serpentine phases, with crystallite sizes in the range 310–250 Å and with different degrees and types of carbonation processes, one derived from the transformation of the serpentine, generating dolomite, and another by direct precipitation of calcite. The SBET reached values between 38–24 m2∙g−1 for the samples less crystalline, in agreement with the XRD patterns, while those with a higher degree of crystallinity gave values close to 8–9 m2∙g−1. In the UV region all electronic spectra were dominated by the absorption edge due to O2− → Si4+ charge transfer transition, with Si4+ in tetrahedral coordination, corresponding to a band gap energy of ca 4.7 eV. In the visible region, 800–350 nm, the spectra of all samples, except Donai, presented at least two weak and broad absorptions centred in the range 650–800 and 550–360 nm, associated with the presence of Fe3+ ions from the oxidation of structural Fe2+ ions in the serpentinites ((MgxFe2+1−x)3Si2O5(OH)4). The relative intensity of the IR bands corresponding to the stretching modes of the OH’s groups indicated the prevalence of one of the two phases, antigorite or lizardite, in the serpentinites. We proposed that the different relative intensity of these bands could be considered as diagnostic to differentiate the predominance of these phases in serpentinites.

Sign in / Sign up

Export Citation Format

Share Document