scholarly journals Influence of Thermal Annealing on the Sinterability of Different Grades of Polylactide Microspheres Dedicated for Laser Sintering

Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 2999
Author(s):  
Małgorzata Gazińska ◽  
Anna Krokos ◽  
Bartłomiej Kryszak ◽  
Paulina Dzienny ◽  
Michał Olejarczyk ◽  
...  
Keyword(s):  
Spherical Shape ◽  
Laser Sintering ◽  
Cold Crystallization ◽  
Scanning Calorimetry ◽  
Residual Solvent ◽  
Crystallinity Degree ◽  
Solvent Content ◽  
Conditioning Temperature ◽  
Powder Characteristics ◽  
Core Powder

We present a comparison of the influence of the conditioning temperature of microspheres made of medical grade poly(L-lactide) (PLLA) and polylactide with 4 wt % of D-lactide content (PLA) on the thermal and structural properties. The microspheres were fabricated using the solid-in-oil-in-water method for applications in additive manufacturing. The microspheres were annealed below the glass transition temperature (Tg), above Tg but below the onset of cold crystallization, and at two temperatures selected from the range of cold crystallization corresponding to the crystallization of the α’ and α form of poly(L-lactide), i.e., at 40, 70, 90, and 120 °C, in order to verify the influence of the conditioning temperature on the sinterability of the microspheres set as the sintering window (SW). Based on differential scanning calorimetry measurements, the SWs of the microspheres were evaluated with consideration of the existence of cold crystallization and reorganization of crystal polymorphs. The results indicated that the conditioning temperature influenced the availability and range of the SWs depending on the D-lactide presence. We postulate the need for an individual approach for polylactide powders in determining the SW as a temperature range free of any thermal events. We also characterized other core powder characteristics, such as the residual solvent content, morphology, particle size distribution, powder flowability, and thermal conductivity, as key properties for successful laser sintering. The microspheres were close to spheres, and the size of the microspheres was below 100 µm. The residual solvent content decreased with the increase of the annealing temperature. The thermal conductivities were 0.073 and 0.064 W/mK for PLA and PLLA microspheres, respectively, and this depended on the spherical shape of the microspheres. The wide angle X-ray diffraction (WAXD) studies proved that an increase in the conditioning temperature caused a slight increase in the crystallinity degree for PLLA microspheres and a clear increase in crystallization for the PLA microspheres.

scholarly journals Influence of Thermal Annealing on Sinterability of Different Grades Polylactide Microspheres Dedicated for Laser Sintering

2021 ◽  
Author(s):  
Małgorzata Gazińska ◽  
Anna Krokos ◽  
Bartłomiej Kryszak ◽  
Paulina Dzienny ◽  
Michał Olejarczyk ◽  
...  
Keyword(s):  
Thermal Conductivity ◽  
Spherical Shape ◽  
Laser Sintering ◽  
Cold Crystallization ◽  
Scanning Calorimetry ◽  
Residual Solvent ◽  
Crystallinity Degree ◽  
Conditioning Temperature ◽  
Powder Flowability ◽  
Core Powder

Comparison of the influence of conditioning temperature of microspheres made of medical grade poly(L-lactide) (PLLA) and polylactide with 4wt.% of D-lactide content (PLA), on its thermal and structural properties is presented. The microspheres were fabricated by solid-in-oil-in-water method for application in additive manufacturing. The microspheres were annealed below glass transition temperature (Tg), above Tg but below onset of cold crystallization, and at two temperatures selected from the range of cold crystallization corresponding to crystallization of α’ and α form of poly(L-lactide) respectively, i.e., at 40°C, 70°C, 90°C and 120°C, in order to verify the influence of conditioning temperatures on sinterability of microspheres set as sintering window (SW). Based on differential scanning calorimetry measurements SW of microspheres were evaluated with consideration of existence of cold crystallization and reorganization of crystal polymorph. The results indicate that the conditioning temperature influence on availability and range of SW that depending on the D-lactide presence. We postulate the need for an individual approach for polylactide powders in determining the SW as a temperature range free of any thermal events. Moreover, other core powder characteristic, such as residual solvent content, morphology, particle size distribution, powder flowability and thermal conductivity, as a key property for successful laser sintering, are characterized. The microspheres are close to sphere and the size of microspheres are below 100 µm. Residual solvents content decreases with the increase of annealing temperature. The thermal conductivity is 0.073 W/mK and 0.064 W/mK for PLA and PLLA microspheres, respectively, and it depends on the spherical shape of the microspheres. Furthermore, the WAXD studies prove that an increase in the conditioning temperature causes a slight increase in crystallinity degree for PLLA microspheres and clear increase in crystallization for PLA microspheres.

scholarly journals Optimization of amorphous solid dispersion techniques to enhance solubility of febuxostat

Folia Medica ◽  
2021 ◽  
Vol 63 (4) ◽  
pp. 557-568
Author(s):  
Vaishali P. Patel ◽  
Anita P. Patel ◽  
Ashish Shah
Keyword(s):  
Dissolution Rate ◽  
Solid Dispersion ◽  
Amorphous Solid ◽  
Amorphous Powder ◽  
Amorphous Solid Dispersion ◽  
Scanning Calorimetry ◽  
Residual Solvent ◽  
Percentage Yield ◽  
Poorly Soluble ◽  
Powder Characteristics

Febuxostat is a selective inhibitor of xanthine oxidase and belongs to BCS class II drugs having low solubility and high permeability. Solubility is the most important parameter which directly affects dissolution, absorption and bioavailability of the drugs. There are different techniques by which we can improve solubility and dissolution rate of poorly soluble drug. Amorphous solid dispersion is one of the methods which can improve solubility as well as powder characteristics. The aim of the present study was to formulate and optimize various methods of formulating solid dispersion by using various drug-to-polymer ratios and identifying the batch which gives higher solubility as well as amorphous powder of the drug febuxostat. Different techniques like hot melt method, solvent evaporation method and spray drying techniques were selected for optimization. Attempts were made to improve solubility of febuxostat by employing Kolliphor P 188, Kolliphor P 237, Eudragit RLPO in different drug-to-polymer ratios (1:1, 1:1.5, 1:2) as carrier. The prepared solid dispersion was characterized for the saturation solubility, percentage yield, using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), powdered X-ray diffraction studies (PXRD), and residual solvent determination. Solid state characterization indicated that febuxostat was present in the amorphous form after mixing with polymeric carrier. In contrast to the pure form of drug, solid dispersion of the drug showed better solubility and amorphous characteristics which can be attributed to decreased crystallinity due to hydrotrophy. Thus, amorphous solid dispersion approach can be used successfully to enhance solubility, dissolution rate and bioavailability of febuxostat.

scholarly journals Production and Processing of a Spherical Polybutylene Terephthalate Powder for Laser Sintering

2019 ◽  
Vol 9 (7) ◽  
pp. 1308 ◽  
Author(s):  
Rob Kleijnen ◽  
Manfred Schmid ◽  
Konrad Wegener
Keyword(s):  
Mechanical Properties ◽  
Thermal Processing ◽  
Selective Laser Sintering ◽  
Spherical Shape ◽  
Laser Sintering ◽  
Polybutylene Terephthalate ◽  
Powder Production ◽  
Injection Molded ◽  
Continuous Extrusion ◽  
Matrix Powder

This work describes the production of a spherical polybutylene terephthalate (PBT) powder and its processing with selective laser sintering (SLS). The powder was produced via melt emulsification, a continuous extrusion-based process. PBT was melt blended with polyethylene glycol (PEG), creating an emulsion of spherical PBT droplets in a PEG matrix. Powder could be extracted after dissolving the PEG matrix phase in water. The extrusion settings were adjusted to optimize the size and yield of PBT particles. After classification, 79 vol. % of particles fell within a range of 10–100 µm. Owing to its spherical shape, the powder exhibited excellent flowability and packing properties. After powder production, the width of the thermal processing (sintering) window was reduced by 7.6 °C. Processing of the powder on a laser sintering machine was only possible with difficulties. The parts exhibited mechanical properties inferior to injection-molded specimens. The main reason lied in the PBT being prone to thermal degradation and hydrolysis during the powder production process. Melt emulsification in general is a process well suited to produce a large variety of SLS powders with exceptional flowability.

scholarly journals Wastes from Agricultural Silage Film Recycling Line as a Potential Polymer Materials

Polymers ◽  
2021 ◽  
Vol 13 (9) ◽  
pp. 1383
Author(s):  
Jerzy Korol ◽  
Aleksander Hejna ◽  
Klaudiusz Wypiór ◽  
Krzysztof Mijalski ◽  
Ewelina Chmielnicka
Keyword(s):  
Vinyl Acetate ◽  
Thermal Performance ◽  
Mechanical Performance ◽  
Ethylene Vinyl Acetate ◽  
Tensile Tests ◽  
Solid Particles ◽  
Polymer Materials ◽  
Slight Reduction ◽  
Scanning Calorimetry ◽  
Crystallinity Degree

The recycling of plastics is currently one of the most significant industrial challenges. Due to the enormous amounts of plastic wastes generated by various industry branches, it is essential to look for potential methods for their utilization. In the presented work, we investigated the recycling potential of wastes originated from the agricultural films recycling line. Their structure and properties were analyzed, and they were modified with 2.5 wt % of commercially available compatibilizers. The mechanical and thermal performance of modified wastes were evaluated by tensile tests, thermogravimetric analysis, and differential scanning calorimetry. It was found that incorporation of such a small amount of modifiers may overcome the drawbacks caused by the presence of impurities. The incorporation of maleic anhydride-grafted compounds enhanced the tensile strength of wastes by 13–25%. The use of more ductile compatibilizers—ethylene-vinyl acetate and paraffin increased the elongation at break by 55–64%. The presence of compatibilizers also reduced the stiffness of materials resulting from the presence of solid particles. It was particularly emphasized for styrene-ethylene-butadiene-styrene and ethylene-vinyl acetate copolymers, which caused up to a 20% drop of Young’s modulus. Such effects may facilitate the further applications of analyzed wastes, e.g., in polymer film production. Thermal performance was only slightly affected by compatibilization. It caused a slight reduction in polyethylene melting temperatures (up to 2.8 °C) and crystallinity degree (up to 16%). For more contaminated materials, the addition of compatibilizers caused a minor reduction in the decomposition onset (up to 6 °C). At the same time, for the waste after three washing cycles, thermal stability was improved. Moreover, depending on the desired properties and application, materials do not have to go through the whole recycling line, simplifying the process, reducing energy and water consumption. The presented results indicate that it is possible to efficiently use the materials, which do not have to undergo the whole recycling process. Despite the presence of impurities, they could be applied in the manufacturing of products which do not require exceptional mechanical performance.

scholarly journals KARAKTERISTIK DAN SKRINING FITOKIMIA EKSTRAK ETANOL 70% BATANG KEPUH (Sterculia foetida L.)

Jurnal Kimia ◽  
2019 ◽  
Vol 13 (1) ◽  
pp. 22
Author(s):  
N. P. S. E. Cahyani ◽  
J. Susiarni ◽  
K. C.S. Dewi ◽  
N. L.P. Melyandari ◽  
K. W.A. Putra ◽  
...  
Keyword(s):  
Moisture Content ◽  
Water Content ◽  
Ethanol Extract ◽  
Phytochemical Screening ◽  
Residual Solvent ◽  
Solvent Content ◽  
Residual Content ◽  
Ethanol Level ◽  
Anti Inflammatory

Kepuh (Sterculia foetida L) is a type of kapok plant that has been scientifically proven to have activity as an anti-inflammatory and analgesic. 70% ethanol extract of stem stem is obtained by maceration using 70% ethanol. Examination of the characteristics of 70% ethanol extract of kepuh stem included organoleptic, of moisture content and determination of residual solvent content. Phytochemical screening of 70% ethanol extract of kepuh bark includes: alkaloid, flavonoid, saponin, tannin , polyphenol, and examination of glycosides. The results of the examination of the characteristics of 70% ethanol extract of kepuh stem obtained water content of 8.66 ± 0.748%, the residual content of the solvent had a 0 (zero) ethanol level. The results of phytochemical screening showed 70% ethanol extract of stem stem containing steroid compounds, triterpenoids, flavonoids, saponins, tannins and polyphenols. The identification using UV-Vis spectrophotometry produced ? 212, the absorbance was 1.8601 and ? 284, the absorbance was 0.42186.

Study in performance and morphology of polyamide 12 produced by selective laser sintering technology

2018 ◽  
Vol 24 (5) ◽  
pp. 813-820 ◽  
Author(s):  
Junjie Wu ◽  
Xiang Xu ◽  
Zhihao Zhao ◽  
Minjie Wang ◽  
Jie Zhang
Keyword(s):  
Selective Laser Sintering ◽  
Polarized Light ◽  
Chain Scission ◽  
High Energy ◽  
Laser Sintering ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Content Type ◽  
X Ray ◽  
Polyamide 12

Purpose The purpose of this paper is to investigate the effect of selective laser sintering (SLS) method on morphology and performance of polyamide 12. Design/methodology/approach Crystallization behavior is critical to the properties of semi-crystalline polymers. The crystallization condition of SLS process is much different from others. The morphology of polyamide 12 produced by SLS technology was investigated using scanning electron microscopy, polarized light microscopy, differential scanning calorimetry, X-ray diffraction and wide-angle X-ray diffraction. Findings Too low fill laser power brought about bad fusion of powders, while too high energy input resulted in bad performance due to chain scission of macromolecules. There were three types of crystal in the raw powder material, denoted as overgrowth crystal, ring-banded spherulite and normal spherulite. Originality/value In this work, SLS samples with different sintering parameters, as well as compression molding sample for the purpose of comparison, were made to study the morphology and crystal structure of sintered PA12 in detail.

scholarly journals Preparation, characterization and scale-up of sesamol loaded solid lipid nanoparticles

2012 ◽  
Vol 2 (1) ◽  
pp. 8 ◽  
Author(s):  
Vandita Kakkar ◽  
Indu Pal Kaur
Keyword(s):  
Solid Lipid Nanoparticles ◽  
Scale Up ◽  
Spherical Shape ◽  
Entrapment Efficiency ◽  
Lipid Nanoparticles ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Solid Lipid ◽  
Transmission Electron ◽  
The Brain

Sesamol loaded solid lipid nanoparticles (SSLNs) were prepared with the aim of minimizing its distribution to tissues and achieving its targeting to the brain. Three scale-up batches (100x1 L) of S-SLNs were prepared using a microemulsification technique and all parameters were statistically compared with the small batch (1x;10 mL). S-SLNs with a particle size of less than 106 nm with a spherical shape (transmission electron microscopy) were successfully prepared with a total drug content and entrapment efficiency of 94.26±2.71% and 72.57±5.20%, respectively. Differential scanning calorimetry and infrared spectroscopy confirmed the formation of lipidic nanoparticles while powder X-ray diffraction revealed their amorphous profile. S-SLNs were found to be stable for three months at 5±3°C in accordance with International Conference on Harmonisation guidelines. The SLN preparation process was successfully scaled-up to a 100x batch on a laboratory scale. The procedure was easy to perform and allowed reproducible SLN dispersions to be obtained.

scholarly journals Microstructure and mechanical properties of slowly cooled Cu47.5Zr47.5Al5

2007 ◽  
Vol 22 (2) ◽  
pp. 326-333 ◽  
Author(s):  
J. Das ◽  
S. Pauly ◽  
C. Duhamel ◽  
B.C. Wei ◽  
J. Eckert
Keyword(s):  
Mechanical Properties ◽  
Fracture Strain ◽  
Volume Fraction ◽  
Spherical Shape ◽  
High Yield ◽  
High Yield Strength ◽  
Scanning Calorimetry ◽  
Arc Melting ◽  
Martensite Matrix

Cu47.5Zr47.5Al5 was prepared by arc melting and solidified in situ by suction casting into 2–5-mm-diameter rods under various cooling rates (200–2000 K/s). The microstructure was investigated along the length of the rods by electron microscopy, differential scanning calorimetry and mechanical properties were investigated under compression. The microstructure of differently prepared specimens consists of macroscopic spherical shape chemically inhomogeneous regions together with a low volume fraction of randomly distributed CuZr B2 phase embedded in a 2–7 nm size clustered “glassy-martensite” matrix. The as-cast specimens show high yield strength (1721 MPa), pronounced work-hardening behavior up to 2116 MPa and large fracture strain up to 12.1–15.1%. The fracture strain decreases with increasing casting diameter. The presence of chemical inhomogenities and nanoscale “glassy-martensite” features are beneficial for improving the inherent ductility of the metallic glass.

scholarly journals Development and evaluation of coenzyme Q10 loaded solid lipid nanoparticle hydrogel for enhanced dermal delivery

2013 ◽  
Vol 63 (4) ◽  
pp. 517-529 ◽  
Author(s):  
Emrah Korkm ◽  
Evren H. Gokce ◽  
Ozgen Ozer
Keyword(s):  
Coenzyme Q10 ◽  
High Speed ◽  
Antioxidant Properties ◽  
Spherical Shape ◽  
Entrapment Efficiency ◽  
Tween 80 ◽  
Trolox Equivalent Antioxidant Capacity ◽  
Scanning Calorimetry ◽  
Transmission Electron Microscopy Analysis ◽  
Solid Lipid

Abstract Coenzyme Q10 (Q10) loaded solid lipid nanoparticles (SLN) were prepared by the high speed homogenization method and incorporated into Carbopol 974P hydrogels. Compritol 888 ATO (C888) was employed as the lipid base; Poloxamer 188 (P188) and Tween 80 (Tw80) were used as surfactant and co-surfactant. Optimum particle size with narrow distribution was obtained as 152.2 nm for blank and 142.4 nm for Q10 loaded SLNs. The overall charge of loaded SLNs was -13.7 ± 1.3 mV. Q10 entrapment efficiency was 89 % and the production yield was 94 %. Transmission electron microscopy analysis provided evidence of colloidal size, spherical shape while differential scanning calorimetry analysis confirmed recrystallization of the lipid after the preparation of SLNs. Trolox equivalent antioxidant capacity (TEAC) analysis has shown that antioxidant potential of Q10 can be protected in SLNs. Rheological characteristics demonstrated that the SLN incorporating gels were shear thinning and the mechanical strength of the gels was suitable for topical application. Diffusion studies from rat abdominal skin revealed that the delivery of Q10 was doubled in SLN incorporating gels, approximately 40 μg cm-2, in comparison with gels prepared with only Q10 (not incorporated in SLNs). As a result, it can be stated that Q10-SLN loaded gels can be successful delivery systems for carrying Q10 efficiently into the skin without losing its antioxidant properties.

scholarly journals Preparation of microencapsulated PCMs for energy saving and thermal comfort of buildings

2021 ◽  
Vol 23 (09) ◽  
pp. 277-287
Author(s):  
Ashraf Mohamed Heniegal ◽  
◽  
Omar Mohamed Omar Ibrahim ◽  
Nour Bassim Frahat ◽  
Mohamed Amin ◽  
...  
Keyword(s):  
Thermal Performance ◽  
Chemical Interaction ◽  
Spherical Shape ◽  
Building Envelope ◽  
Scanning Calorimetry ◽  
Indoor Temperature ◽  
New Techniques ◽  
Consumption Energy ◽  
Local Materials ◽  
Regular Spherical Shape

Energy improvement techniques for buildings are among the modern studies that concentrate on new techniques and methods of saving energy and improving the thermal performance in buildings. This research aims to prepare microencapsulated-PCMs (micro-PCMs) by using local materials and studied the influence of using micro-PCMs on thermal performance improvement and PCMs leakage problems improvement. The micro-PCMs of paraffin wax were prepared as the core PCMs materials while the melamine-formaldehyde polymer as the shell. The micro-PCMs were characterized through scanning electron-microscopy (SEM), energy-dispersive X-ray (EDX) spectrometry, Fourier-transform infrared spectroscopy, and differential scanning calorimetry. Analysis results showed the prepared micro-PCMs present a regular spherical shape and confirm that the formation composite of the shell effectively encapsulated the cores. Furthermore, the absence of chemical interaction between the MF and the PW components. The micro-PCM have potential for architectural applications in the building-envelope to store thermal energy, provide indoor-temperature at the comfortable range, and reduce the consumption energy in buildings.

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