scholarly journals Surface Analysis of Biodegradable Mg-Alloys after Immersion in Simulated Body Fluid

Materials ◽  
2020 ◽  
Vol 13 (7) ◽  
pp. 1740 ◽  
Author(s):  
Darja Steiner Petrovič ◽  
Djordje Mandrino ◽  
Božidar Šarler ◽  
Jelena Horky ◽  
Andrea Ojdanic ◽  
...  

Two binary biodegradable Mg-alloys and one ternary biodegradable Mg-alloy (Mg-0.3Ca, Mg-5Zn and Mg-5Zn-0.3Ca, all in wt%) were investigated. Surface-sensitive X-ray photoelectron spectroscopy analyses (XPS) of the alloy surfaces before and after immersion in simulated body fluid (SBF) were performed. The XPS analysis of the samples before the immersion in SBF revealed that the top layer of the alloy might have a non-homogeneous composition relative to the bulk. Degradation during the SBF immersion testing was monitored by measuring the evolution of H2. It was possible to evaluate the thickness of the sample degradation layers after the SBF immersion based on scanning electron microscopy (SEM) of the tilted sample. The thickness was in the order of 10–100 µm. The typical bio-corrosion products of all of the investigated alloys consisted of Mg, Ca, P and O, which suggests the formation of apatite (calcium phosphate hydroxide), magnesium hydrogen phosphate hydrate and magnesium hydroxide. The bioapplicability of the analyzed alloys with regard to surface composition and degradation kinetics is discussed.

Clay Minerals ◽  
1992 ◽  
Vol 27 (4) ◽  
pp. 413-421 ◽  
Author(s):  
M. Soma ◽  
G. J. Churchman ◽  
B. K. G. Theng

AbstractThe surface composition of some halloysites with different particle morphology has been investigated by X-ray photoelectron spectroscopy (XPS) before and after removal of external Fe. The Fe(III) 2p3/2 binding energy of external Fe is appreciably smaller than that of structural Fe. Particle morphology is influenced by structural Fe content. The long-tubular halloysite has very little surface Fe, and its concentration tends to increase with the proportion of non-tubular particles in the samples. The spheroidal sample contains the most structural Fe which, however, does not appear to influence particle shape directly. Study by XPS indicates that Fe substitutes for Al in octahedral positions in approximately 1 : 2 proportion. As a result, an increase in octahedral vacancies and cation exchange capacity would be predicted. Further, halloysite layers within a crystal are generally inhomogeneous in composition. Built up like “onion skins”, the surface layers would either be enriched or depleted in Fe depending on the chemical environment in which crystal growth occurs.


1999 ◽  
Vol 599 ◽  
Author(s):  
F. Barrère ◽  
P. Layrolle ◽  
C. A. van Blitterswijk ◽  
K. de Groot

AbstractThe aim of this study was to accelerate the formation of biomimetic Calcium-Phosphate (Ca-P) coatings on Ti6Al4V by using a 5 times more concentrated Simulated Body Fluid (SBFx5) than the regular SBF. The production of SBFx5 was possible by decreasing the pH of the solution to approximately 6 with CO2 gas. The release of this mildly acidic gas allowed the formation of a Ca-P film after 4h of immersion at pH=6.8. The structure of this coating was an amorphous carbonated Ca-P. In addition, our experiments showed that the presence of Mg2+ was absolutely necessary for the Ca-P coating formation on Ti6Al4V substrate. Mg2+ is a crystal growth inhibitor and favored the heterogeneous nucleation. Furthermore, depth profile X-Ray Photoelectron Spectroscopy showed that Ca-P nucleation on the passive Titanium oxide (TiO2) passive layer was initiated by Ca2+ and Mg2+. The attachment of this Ca-P coating resulted probably from chemical bonds such as P-O-Ti and Ca-O-Ti. Ca was more present at the coating/substrate interface than P. Thereby Ca-O-Ti seems to be favored.


1986 ◽  
Vol 86 ◽  
Author(s):  
Myra M. Soroczak ◽  
H. C. Eaton ◽  
M. E. Tittlebaum

ABSTRACTThe reactivity of coal fly ash is dependent on the chemical composition of the surface. As reactions occur the ash particle size decreases and new material is available for reaction. This means that the near-surface chemistry can also be important. In the present study the surface chemistries of three ashes are determined by x-ray photoelectron spectroscopy both before and after exposure to a hydrating/leaching environment. Scanning electron microscopy is used to reveal ash morphology. The concentration of sulfur, found at the ash surfaces as a sulfate, and sodium decreased after leaching while the amount of iron and aluminum increased. Other elements, including calcium, increased and decreased with leaching depending on which ash was analyzed. Changes which occurred in the ash morphology after the removal of leachable elements are discussed.


2011 ◽  
Vol 299-300 ◽  
pp. 508-511
Author(s):  
Guo Chao Qi ◽  
Feng Jun Shan ◽  
Qiang Li ◽  
Jing Yuan Yu ◽  
Qu Kai Zhang

Magnesium apatite (MA, (Ca9Mg)(PO4)6(OH)2) and Hydroxyapatite (HA) coatings were synthesized on Ti6Al4V substrates by a sol-gel dip coating method. Glucose and bovine serum albumin (BSA) were added to the standard simulated body fluid (SBF) separately to form organic-containing simulated body fluids. MA and HA coatings were immersed in standard and organic modified SBF for time periods of 4, 7, 14, 21 and 28 days at 37±1°C. The surface dissolution and deposition behavior of the coatings after soaking were examined with Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The results show that glucose in SBF has no apparent effect on the deposition of new apatite from the solution. BSA in SBF shows retardation effect on the deposition of apatite by forming a protein dominant globular layer. This layer inhibits the further deposition of apatite from SBF solution.


Author(s):  
Замир Валериевич Шомахов ◽  
Светлана Сергеевна Налимова ◽  
Рустам Мухамедович Калмыков ◽  
Кирилл Аубекеров ◽  
Вячеслав Алексеевич Мошников

Слои диоксида олова синтезированы гидротермальным методом из водного раствора SnF. Наночастицы серебра осаждены на поверхность полученных слоев методом фотовосстановления. Проведено исследование морфологии поверхности образцов методом атомно-силовой микроскопии. Размер наночастиц серебра зависит от концентрации раствора AgNO, используемого для проведения реакции фотовосстановления. При синтезе из раствора с концентрацией 0,02 М размер полученных наночастиц составляет варьируется от 10 до 100 нм, при увеличении концентрации раствора в два раза размер наночастиц составляет порядка 100 нм. С помощью рентгеновской фотоэлектронной спектроскопии изучен состав поверхности слоев до и после осаждения наночастиц серебра. При выбранных условиях синтеза формируется слой диоксида олова без посторонних включений, и происходит осаждение металлического серебра. Химический сдвиг пиков олова и кислорода после осаждения наночастиц серебра свидетельствует об обмене электронами между оловом и серебром. Полученные слои представляют интерес для применения в области полупроводниковых адсорбционных газовых сенсоров. Tin dioxide layers were synthesized by hydrothermal method from an aqueous solution of SnF. Silver nanoparticles were deposited on the surface of the obtained layers by the photoreduction method. The surface morphology of the samples was studied by atomic force microscopy. The size of the silver nanoparticles depends on the concentration of the AgNO solution used for the photoreduction reaction. When synthesized from 0,02 M solution with a concentration of, the size of the nanoparticles varies from 10 to 100 nm, when the concentration of the solution is doubled, the size of the nanoparticles is about 100 nm. The surface composition of the layers before and after the deposition of silver nanoparticles was studied using the X-ray photoelectron spectroscopy. It was shown that a layer of the tin dioxide is formed without external inclusions, and metallic silver is deposited. The chemical shift of the peaks of tin and oxygen after the deposition of silver nanoparticles indicates the exchange of electrons between tin and silver. The synthesized layers are of interest for application in the field of semiconductor adsorption gas sensors.


2020 ◽  
Author(s):  
Jennifer A. Rudd ◽  
Ewa Kazimierska ◽  
Louise B. Hamdy ◽  
Odin Bain ◽  
Sunyhik Ahn ◽  
...  

The utilization of carbon dioxide is a major incentive for the growing field of carbon capture. Carbon dioxide could be an abundant building block to generate higher value products. Herein, we describe the use of porous copper electrodes to catalyze the reduction of carbon dioxide into higher value products such as ethylene, ethanol and, notably, propanol. For <i>n</i>-propanol production, faradaic efficiencies reach 4.93% at -0.83 V <i>vs</i> RHE, with a geometric partial current density of -1.85 mA/cm<sup>2</sup>. We have documented the performance of the catalyst in both pristine and urea-modified foams pre- and post-electrolysis. Before electrolysis, the copper electrode consisted of a mixture of cuboctahedra and dendrites. After 35-minute electrolysis, the cuboctahedra and dendrites have undergone structural rearrangement. Changes in the interaction of urea with the catalyst surface have also been observed. These transformations were characterized <i>ex-situ</i> using scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. We found that alterations in the morphology, crystallinity, and surface composition of the catalyst led to the deactivation of the copper foams.


Molecules ◽  
2021 ◽  
Vol 26 (12) ◽  
pp. 3588
Author(s):  
Jiayi Chen ◽  
Yansong Liu ◽  
Jiayue Zhang ◽  
Yuanlin Ren ◽  
Xiaohui Liu

Lyocell fabrics are widely applied in textiles, however, its high flammability increases the risk of fire. Therefore, to resolve the issue, a novel biomass-based flame retardant with phosphorus and nitrogen elements was designed and synthesized by the reaction of arginine with phosphoric acid and urea. It was then grafted onto the lyocell fabric by a dip-dry-cure technique to prepare durable flame-retardant lyocell fabric (FR-lyocell). X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) analysis demonstrated that the flame retardant was successfully introduced into the lyocell sample. Thermogravimetric (TG) and Raman analyses confirmed that the modified lyocell fabric featured excellent thermal stability and significantly increased char residue. Vertical combustion results indicated that FR-lyocell before and after washing formed a complete and dense char layer. Thermogravimetric Fourier-transform infrared (TG-FTIR) analysis suggested that incombustible substances (such as H2O and CO2) were produced and played a significant fire retarding role in the gas phase. The cone calorimeter test corroborated that the peak of heat release rate (PHRR) and total heat release (THR) declined by 89.4% and 56.4%, respectively. These results indicated that the flame retardancy of the lyocell fabric was observably ameliorated.


CORROSION ◽  
10.5006/3881 ◽  
2021 ◽  
Author(s):  
Zachary Karmiol ◽  
Dev Chidambaram

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.


Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1725 ◽  
Author(s):  
Xiaohong Liu ◽  
Ming Li ◽  
Xuemei Zheng ◽  
Elias Retulainen ◽  
Shiyu Fu

As a type of functional group, azo-derivatives are commonly used to synthesize responsive materials. Cellulose nanocrystals (CNCs), prepared by acid hydrolysis of cotton, were dewatered and reacted with 2-bromoisobuturyl bromide to form a macro-initiator, which grafted 6-[4-(4-methoxyphenyl-azo) phenoxy] hexyl methacrylate (MMAZO) via atom transfer radical polymerization. The successful grafting was supported by Fourier transform infrared spectroscopy (FT-IR) and Solid magnetic resonance carbon spectrum (MAS 13C-NMR). The morphology and surface composition of the poly{6-[4-(4-methoxyphenylazo) phenoxy] hexyl methacrylate} (PMMAZO)-grafted CNCs were confirmed with Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The grafting rate on the macro-initiator of CNCs was over 870%, and the polydispersities of branched polymers were narrow. The crystal structure of CNCs did not change after grafting, as determined by X-ray diffraction (XRD). The polymer PMMAZO improved the thermal stability of cellulose nanocrystals, as shown by thermogravimetry analysis (TGA). Then the PMMAZO-grafted CNCs were mixed with polyurethane and casted to form a composite film. The film showed a significant light and pH response, which may be suitable for visual acid-alkali measurement and reversible optical storage.


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