Investigations on the Degradation Behavior of Processed FeMnSi-xCu Shape Memory Alloys.

A new functional Fe-30Mn-5Si-xCu (x = 1.5 and 2 wt%) biomaterial was obtained from the levitation induction melting process and evaluated as a biodegradable material. The degradation characteristics were assessed in vitro using immersion tests in simulated body fluid (SBF) at 37 ± 1 °C, evaluating mass loss, pH variation that occurred in the solution, open circuit potential (OCP), linear and cyclic potentiometry (LP and CP), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and nano-FTIR. To obtain plates as samples, the cast materials were thermo-mechanically processed by hot rolling. Dynamic mechanical analysis (DMA) was employed to evaluate the thermal properties of the smart material. Atomic force microscopy (AFM) was used to show the nanometric and microstructural changes during the hot rolling process and DMA solicitations. The type of corrosion identified was generalized corrosion, and over the first 3-5 days, an increase in mass was observed, caused by the compounds formed at the metal-solution interface. The formed compounds were identified mainly as oxides that passed into the immersion liquid. The degradation rate (DR) was obtained as a function of mass loss, sample surface area and immersion duration. The dynamic mechanical behavior and dimensions of the sample were evaluated after 14 days of immersion. The nanocompounds found on the surface after atmospheric corrosion and immersion in SBF were investigated with the Neaspec system using the nano-FTIR technique.

Research on the Quality of Partially Removable Skeletal Prostheses Made Using Classical Versus Modern Sintering Techniques.

Conventional partially removable skeletal dentures are one of the most common therapeutic solutions offered to edentulous patients worldwide. The present study aims to compare the skeleton of removable dentures realized via classical techniques to that realized via modern techniques, represented by the laser sintering technique, with the comparative aspects being realized through the evaluation of atomic force microscopy (AFM). A total of 20 metal frameworks made of Co-Cr were sectioned, representing the infrastructure of partially removable skeletal dentures, developed using the classical technique versus the laser sintering technique. The infrastructures of partially removable skeletal dentures were designed for both the maxilla and the mandible, with the design of each type of denture being identical, and were developed using both techniques. The roughness values are different depending on the technological method used; for the conventional casting technique, we have higher roughness for the component elements of the partially removable skeletal denture that have more stretch, e.g., the major connector, and for the 3D laser sintering technique, lower roughness is obtained for the component elements that have a lower stretch, e.g., the clasp arms, the minor connector, or the junction between the saddles and the major connector. The clinical implications of the presence of roughness at the level of the active arms or at the level of the connector saddle junction are represented by the risk of fracture, which confers real discomfort to the patient.

Interdisciplinary Research on Medieval Fresco Subjected to Degradation Processes in the Corbii de Piatra Cave Church.

This paper presents research on the degradation processes of the fresco painting in the cave church of Corbii de Piatra Hermitage under the influence of meteoric infiltration water and environmental factors. The medieval fresco dates from the end of the 13th century and the beginning of the 14th century, being painted on a sandstone wall. The infiltration of meteoric water through this wall, the temperature variations, the environment and the repeated wetting/drying processes determined the degradation of the fresco, resulting in its detachment from large surfaces. This research established correlations between the processes that take place, the structural transformations, the changes in composition and the adhesion of the fresco to the sandstone wall. The results have been made available to conservation and restoration specialists, in order to choose appropriate materials and technologies. This paper presents findings regarding the pictorial material and introduces new analysis techniques in research on the degradation processes of the fresco painting in the cave church of Corbii de Piatra Hermitage under the influence of meteoric infiltration water and environmental factors.

Influence of Dynamic Strain Sweep on the Degradation Behavior of FeMnSi-Ag Shape Memory Alloys.

Iron-based SMAs can be used in the medical field for both their shape memory effect (SME) and biodegradability after a specific period, solving complicated chirurgical problems that are partially now addressed with shape-memory polymers or biodegradable polymers. Iron-based materials with (28-32 wt %) Mn and (4-6 wt %) Si with the addition of 1 and 2 wt % Ag were obtained using levitation induction melting equipment. Addition of silver to the FeMnSi alloy was proposed in order to enhance its antiseptic property. Structural and chemical composition analyses of the newly obtained alloys were performed by X-ray diffraction (confirming the presence of ε phase), scanning electron microscopy (SEM) and energy-dispersive spectroscopy. The corrosion resistance was evaluated through immersion tests and electrolyte pH solution variation. Dynamic mechanical solicitations were performed with amplitude sweep performed on the FeMnSi-1Ag and FeMnSi-2Ag samples, including five deformation cycles at 40 °C, with a frequency of 1 Hz, 5 Hz and 20 Hz. These experiments were meant to simulate the usual behavior of some metallic implants subjected to repetitive mechanical loading. Atomic force microscopy was used to analyze the surface roughness before and after the dynamic mechanical analysis test followed by the characterization of the surface profile change by varying dynamic mechanical stress. Differential scanning calorimetry was performed in order to analyze the thermal behavior of the material in the range of -50-+200 °C. X-ray diffraction and Fourier transform infrared spectroscopy (FTIR) along with Neaspec nano-FTIR experiments were performed to identify and confirm the corrosion compounds (oxides, hydroxides or carbonates) formed on the surface.

On the Thermomechanical Behavior of 3D-Printed Specimens of Shape Memory R-PETG.

From commercial pellets of recycled polyethylene terephthalate glycol (R-PETG), 1.75 mm diameter filaments for 3D printing were produced. By varying the filament's deposition direction between 10° and 40° to the transversal axis, parallelepiped specimens were fabricated by additive manufacturing. When bent at room temperature (RT), both the filaments and the 3D-printed specimens recovered their shape during heating, either without any constraint or while lifting a load over a certain distance. In this way, free-recovery and work-generating shape memory effects (SMEs) were developed. The former could be repeated without any visible fatigue marks for as much as 20 heating (to 90 °C)-RT cooling-bending cycles, while the latter enabled the lifting of loads over 50 times heavier than the active specimens. Tensile static failure tests revealed the superiority of the specimens printed at larger angles over those printed at 10°, since the specimens printed at 40° had tensile failure stresses and strains over 35 MPa and 8.5%, respectively. Scanning electron microscopy (SEM) fractographs displayed the structure of the successively deposited layers and a shredding tendency enhanced by the increase in the deposition angle. Differential scanning calorimetry (DSC) analysis enabled the identification of the glass transition between 67.5 and 77.3 °C, which might explain the occurrence of SMEs in both the filament and 3D-printed specimens. Dynamic mechanical analysis (DMA) emphasized a local increase in storage modulus of 0.87-1.66 GPa that occurred during heating, which might explain the development of work-generating SME in both filament and 3D-printed specimens. These properties recommend 3D-printed parts made of R-PETG as active elements in low-price lightweight actuators operating between RT and 63 °C.

Heat Treatment and Dynamic Mechanical Analysis Strain Sweep Effects on the Phase Structure and Morphology of an Fe-28Mn-6Si-5Cr Shape Memory Alloy.

Fe-Mn-Si-based shape memory alloys (SMAs) have been extensively investigated since 1982 for various useful properties that enhance the development of different applications such as anti-seismic dampers for very tall buildings, pipe joints, or rail fasteners. In particular, the Fe-28Mn-6Si-5Cr (mass. %) alloy has been mainly used in vibration mitigation or self-adjustable axial displacement applications. Dynamic mechanical analysis (DMA), performed by strain sweeps (SS), enables the monitoring of the evolution of storage modulus and internal friction variations with increasing strain amplitudes at different constant frequencies and temperatures. Thus, applying dynamic bending with various frequencies and amplitudes that actually represents an isothermal mechanical treatment. In the present paper, an Fe-28Mn-6 Si-5Cr (mass. %) SMA was cast by ingot metallurgy, hot-rolled, and water quenched in order to obtain thermally induced martensite and avoid the occurrence of cooling cracks. The influence of the holding time, between 2 and 10 h, at 1050 °C and the effects of DMA-SS performed at three different frequencies were analyzed by a differential scanning calorimetry, an X-ray diffraction, and a scanning electron and atomic force microscopy. The effects of the holding time and mechanical treatment on the structure and morphology of martensite plates were corroborated with the results of the thermal analysis.

Analysis of Degradation Products of Biodegradable ZnMgY Alloy.

Biodegradable metallic materials are increasingly gaining ground in medical applications. Zn-based alloys show a degradation rate between those recorded for Mg-based materials with the fastest degradation rate and Fe-based materials with the slowest degradation rate. From the perspective of medical complications, it is essential to understand the size and nature of the degradation products developed from biodegradable materials, as well as the stage at which these residues are eliminated from the body. This paper presents investigations conducted on the corrosion/degradation products of an experimental material (ZnMgY alloy in cast and homogenized state) after immersion tests in three physiological solutions (Dulbecco's, Ringer's and simulated body fluid (SBF)). Scanning electron microscopy (SEM) was used to highlight the macroscopic and microscopic aspects of corrosion products and their effects on the surface. An X-ray energy dispersive detector (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) provided general information about the compounds based on their non-metallic character. The pH of the electrolyte solution was recorded for 72 h during immersion. The pH variation of the solution confirmed the main reactions proposed for the corrosion of ZnMg. The agglomerations of corrosion products were on the micrometer scale, mainly oxides, hydroxides and carbonates or phosphates. The corrosion effects on the surface were homogeneously spread, with a tendency to connect and form cracks or larger corrosion zones, transforming the pitting corrosion pattern into a generalized one. It was noticed that the alloy's microstructure strongly influences the corrosion characteristics.

Effects of Acidic Challenge on Demineralized Root Surface Treated with Silver Diamine Fluoride and Potassium Iodide.

BACKGROUND: The aim of the study was to assess the protective effect of applying potassium iodide (KI) over silver diamine fluoride (SDF) on demineralized root dentin in the case of a sustained acidogenic attack. METHODS: Forty caries-free third molars were used in the study. A diamond disc was used to separate the roots and the tooth crowns from the roots. Each root fragment was randomly distributed in one of the four study groups: C-samples were not demineralized; DD-demineralized samples; RS1-demineralized samples covered with SDF+KI (RS-Riva Star product, SDI limited, Bayswater, Australia); RS2-demineralized samples covered with SDF+KI and submersed to another acidic challenge for 3 days. SEM and EDX were used for the morphological and elemental analysis. Vickers hardness assessment was performed using a tribometer CETR UMT-2 (Bruker Corporation, Berlin, Germany). One-way ANOVA and post hoc Bonferroni tests were used for the statistical analysis with a significance level of p < 0.05. RESULTS: Morphological and elemental changes were observed on the surface of the study samples. Significant differences were observed between the recorded hardness values of groups C and DD (p = 0.005), C and RS2 (p = 0.002), DD and RS1 (p = 0.011); RS1 and RS2 (p = 0.004). CONCLUSIONS: The application of SDF and KI (Riva Star product) on root dentin caries resulted in the formation of a heterogeneous outer layer that sealed the dentin and increased the microhardness of the treated surface. In the conditions of the present study, this layer did not provide enough protection for root dentin exposed to continuous attacks.

Microstructural, Corrosion Resistance, and Tribological Properties of Al2O3 Coatings Prepared by Atmospheric Plasma Spraying.

An usual material, EN-GJL-250 cast iron, used for automotive braking systems, was covered with a ceramic material (105NS-1 aluminium oxide) using an industrial deposition system (Sulzer Metco). The main reason was to improve the corrosion and wear (friction) resistance properties of the cast-iron. Samples were prepared by mechanical grinding and sandblasting before the deposition. We applied two and four passes (around 12-15 µm by layer) each at 90° obtaining ceramic coatings of 30 respectively 60 µm. The surface of the samples (with ceramic coatings) was investigated using scanning electron microscopy (SEM), dispersive energy spectroscopy (EDS) and X-ray diffraction (XRD). Scratch and micro-hardness tests were performed using CETR-UMT-2 micro-tribometer equipment. The better corrosion resistance of the base material was obtained by applying the ceramic coating. The results present a better corrosion resistance and a higher coefficient of friction of the coated samples.

Structural-Functional Changes in a Ti50Ni45Cu5 Alloy Caused by Training Procedures Based on Free-Recovery and Work-Generating Shape Memory Effect.

Active elements made of Ti50Ni45Cu5 shape memory alloy (SMA) were martensitic at room temperature (RT) after hot rolling with instant water quenching. These pristine specimens were subjected to two thermomechanical training procedures consisting of (i) free recovery shape memory effect (FR-SME) and (ii) work generating shape memory effect (WG-SME) under constant stress as well as dynamic bending and RT static tensile testing (TENS). The structural-functional changes, caused by the two training procedures as well as TENS were investigated by various experimental techniques, including differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), X-ray diffraction (XRD), and atomic force microscopy (AFM). Fragments cut from the active regions of trained specimens or from the elongated gauges of TENS specimens were analyzed by DSC, XRD, and AFM. The DSC thermograms revealed the shift in critical transformation temperatures and a diminution in specific absorbed enthalpy as an effect of training cycles. The DMA thermograms of pristine specimens emphasized a change of storage modulus variation during heating after the application of isothermal dynamical bending at RT. The XRD patterns and AMF micrographs disclosed the different evolution of martensite plate variants as an effect of FR-SME cycling and of being elongated upon convex surfaces or compressed upon concave surfaces of bent specimens. For illustrative reasons, the evolution of unit cell parameters of B19' martensite, as a function of the number of cycles of FR-SME training, upon concave regions was discussed. AFM micrographs emphasized wider and shallower martensite plates on the convex region as compared to the concave one. With increasing the number of FR-SME training cycles, plates' heights decreased by 84-87%. The results suggest that FR-SME training caused marked decreases in martensite plate dimensions, which engendered a decrease in specific absorbed enthalpy during martensite reversion.

Corn Cob Ash versus Sunflower Stalk Ash, Two Sustainable Raw Materials in an Analysis of Their Effects on the Concrete Properties.

The increased CO2 emissions determined by the cement industry led to continuous and intensive research on the discovery of sustainable raw materials with cementitious properties. One such raw material category is agricultural waste. This study involved research on the effects of corn cob ash and sunflower stalk ash, respectively, on compressive strength measured after 28 days and 3 months, the flexural and splitting tensile strengths, the resistance to repeated freeze-thaw cycles, and on the resistance to chemical attack of hydrochloric acid of the concrete. A 2.5% and 5% replacement of the cement volume with corn cob ash (CCA) of A and B quality was applied, and with sunflower stalk ash (SSA) at A and B quality, respectively. The obtained results revealed that CCA and SSA decreased the compressive and tensile strength, but led to higher resistance of the concrete on repeated freeze-thaw cycles and to hydrochloric acid. The mixes with 2.5% SSA at A quality obtained the best results regarding splitting the tensile strength and resistance to repeated freeze-thaw cycles, the mixes with 2.5% SSA at B quality led to the highest resistance to hydrochloric acid, and those with 2.5% CCA at A quality led to the best values of compressive strength and flexural tensile strength.

In-Vitro Analysis of FeMn-Si Smart Biodegradable Alloy.

Special materials are required in many applications to fulfill specific medical or industrial necessities. Biodegradable metallic materials present many attractive properties, especially mechanical ones correlated with good biocompatibility with vivant bodies. A biodegradable iron-based material was realized through electric arc-melting and induction furnace homogenization. The new chemical composition obtained presented a special property named SME (shape memory effect) based on the martensite transformation. Preliminary results about this special biodegradable material with a new chemical composition were realized for the chemical composition and structural and thermal characterization. Corrosion resistance was evaluated in Ringer's solution through immersion tests for 1, 3, and 7 days, the solution pH was measured in time for 3 days with values for each minute, and electro-corrosion was measured using a potentiostat and a three electrode cell. The mass loss of the samples during immersion and electro-corrosion was evaluated and the surface condition was studied by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). SME was highlighted with differential scanning calorimetry (DSC). The results confirm the possibility of a memory effect of the materials in the wrought case and a generalized corrosion (Tafel and cyclic potentiometry and EIS) with the formation of iron oxides and a corrosion rate favorable for applications that require a longer implantation period.

Study of an Ecological Cement-Based Composite with a Sustainable Raw Material, Sunflower Stalk Ash.

The use of plant ash as a sustainable cementitious material in concrete composition is a widely researched subject in the construction domain. A plant studied so far more for its thermal insulation properties, sunflower, was analyzed in this study with regard to its ash effects on the concrete composition. The present research aimed to analyze the effects of a 2.5%, 5%, 7.5%, 10%, 15%, 20%, or 30% volume replacement of cement by sunflower stalk ash (SA), a sustainable cementitious material, on the concrete compressive strength at 28 days and three months, the flexural and splitting tensile strengths, the resistance to repeated freeze-thaw cycles, and the resistance to chemical attack of hydrochloric acid. The elementary chemical composition of the SA and the composites was included also. According to the experimental results, SA decreased the values of the compressive and tensile strength of the concrete, but it improved the concrete behavior under repeated freeze-thaw cycles and under the action of hydrochloric acid. A percent of 10% of SA led to a much more pronounced development of compressive strength over time than conventional concrete (26.6% versus 12%).

New Zn3Mg-xY Alloys: Characteristics, Microstructural Evolution and Corrosion Behavior.

Zinc biodegradable alloys attracted an increased interest in the last few years in the medical field among Mg and Fe-based materials. Knowing that the Mg element has a strengthening influence on Zn alloys, we analyze the effect of the third element, namely, Y with expected results in mechanical properties improvement. Ternary ZnMgY samples were obtained through induction melting in Argon atmosphere from high purity (Zn, Mg, and Y) materials and MgY (70/30 wt%) master alloys with different percentages of Y and keeping the same percentage of Mg (3 wt%). The corrosion resistance and microhardness of ZnMgY alloys were compared with those of pure Zn and ZnMg binary alloy. Materials were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), linear and cyclic potentiometry, and immersion tests. All samples present generalized corrosion after immersion and electro-corrosion experiments in Dulbecco solution. The experimental results show an increase in microhardness and indentation Young Modulus following the addition of Y. The formation of YZn12 intermetallic phase elements with a more noble potential than pure Zinc is established. A correlation is obtained between the appearance of new Y phases and aggressive galvanic corrosion.