Effect of the Axial Profile of a Ceramic Grinding Wheel on Selected Roughness Parameters of Shaped Surfaces Obtained in the Grinding Process with a Dual-Tool Grinding Head.

The use of CNC equipment that integrates several machining operations eliminates downtime due to changes in setup and clamping of workpieces in more than one machining device. A review of CNC equipment and tools known from the literature and from manufacturers' offerings indicates that new technical solutions are being developed to integrate two or more technological operations. However, these examples have numerous limitations and are mostly not suitable for machining surfaces with complex shapes. An example of such solutions is the use of a dual-tool grinding head, which integrates the process of rough grinding with a ceramic grinding wheel and finish grinding with a flexible grinding wheel. Unfortunately, it has the disadvantage of being limited by the angular shape of the ceramic grinding wheel, making it unable to adapt to the complex geometries of the shaped surfaces being ground. The need to overcome this limitation became the motivation for the research work described in this article. By means of experimental research, it was verified what effect the radial outline on the periphery of a ceramic grinding wheel realized by rough grinding would have on the surface roughness parameters obtained in the process of grinding shaped surfaces. For this purpose, grinding processes using a ceramic wheel with a conical and radial outline were compared. The result of the study was a summary of the surface roughness parameters Sa, St, Sq, Spk, Str, and Sds obtained after two-stage machining (rough and finish grinding). The obtained analysis results showed that changing the axial outline of the ceramic grinding wheel makes it possible to significantly expand the range of applications of the dual-tool head without negatively affecting the quality of the machined surface. Thus, such an improvement will make it possible to increase the applicability of the head by grinding shaped surfaces with a radial profile of curvature.

Structure modeling and quantitative X-ray diffraction of C-(A)-S-H.

Quantitative X-ray diffraction of nanocrystalline calcium silicate hydrate (C-S-H) and its aluminium-substituted variants (C-A-S-H) has so far been limited by a lack of appropriate structure models. In this study, atomistic structure models derived from tobermorite were combined with a supercell approach using TOPAS. By accounting for nanostructural features such as isolated layers, turbostratic disorder and, for the first time, fibrils, characteristic reflections and asymmetric bands were more accurately simulated than before, providing the means for phase quantification and refinement of structural sites. This improved methodology is applied to autoclaved aerated concrete and the experimental study of related hydrothermal reactions. Scanning electron microscopy indicated a fibrillar morphology for intermediate C-(A)-S-H, and energy-dispersive X-ray spectroscopy constrained its Ca/Si ratio to 1.31-1.35. As a first step, the direct quantification of C-(A)-S-H via structure models was assessed by a series of X-ray diffraction measurements using corundum as an internal standard. Secondly, the verified structure model was applied to evaluate in situ X-ray diffraction experiments at 457, 466 and 473 K (1.1, 1.35 and 1.55 MPa, respectively). Finally, a quantitative study of industrially produced autoclaved aerated concrete was conducted, determining 20-30 wt% C-(A)-S-H at Ca/Si ratios < 1.0. In general, the developed structure models advance the study of Portland cement concrete and related materials, including autoclaved aerated concrete, and the supercell approach may be universally applicable to other nanocrystalline materials.

In situ monitoring of hydrothermal reactions by X-ray diffraction with Bragg-Brentano geometry.

This note describes an autoclave chamber developed and constructed by Anton Paar and its application for in situ experiments under hydrothermal conditions. Reactions of crystalline phases can be studied by successive in situ measurements on a conventional laboratory X-ray diffractometer with Bragg-Brentano geometry at temperatures <483 K and saturated vapour pressure <2 MPa. Variations in the intensity of X-ray diffraction reflections of both reactants and products provide quantitative information for studying the reaction kinetics of both dissolution and crystal growth. Feasibility is demonstrated by studying a cementitious mixture used for autoclaved aerated concrete production. During a period of 5.7 h at 466 K and 1.35 MPa, the crystallization of torbermorite and the partial consumption of quartz were monitored.

Phosphate Coatings Enriched with Copper on Titanium Substrate Fabricated Via DC-PEO Process.

The present paper covers the possible ways to fabricate advanced porous coatings that are enriched in copper on a titanium substrate through Direct Current Plasma Electrolytic Oxidation (DC-PEO) with voltage control, in electrolytes made of concentrated orthophosphoric acid with the addition of copper(II) nitrate(V) trihydrate. In these studies, solutions containing from 0 to 650 g salt per 1 dm3 of acid and anodic voltages from 450 V up to 650 V were used. The obtained coatings featuring variable porosity could be best defined by the three-dimensional (3D) parameter Sz, which lies in the range 9.72 to 45.18 µm. The use of copper(II) nitrate(V) trihydrate in the electrolyte, resulted, for all cases, in the incorporation of the two oxidation forms, i.e., Cu+ and Cu2+ into the coatings. Detailed X-Ray Photoelectron Spectroscopy (XPS) studies layers allowed for stating that the percentage of copper in the surface layer of the obtained coatings was in the range of 0.24 at% to 2.59 at%. The X-Ray Diffraction (XRD) studies showed the presence of copper (α-Cu2P2O7, and Cu3(PO4)2) and titanium (TiO2-anatase, TiO3, TiP2O7, and Ti0.73O0.91) compounds in coatings. From Energy-Dispersive X-Ray Spectroscopy (EDS) and XPS studies, it was found that the Cu/P ratio increases with the increase of voltage and the amount of salt in the electrolyte. The depth profile analysis by Glow-Discharge Optical Emission Spectroscopy (GDOES) method showed that a three-layer model consisting of a top porous layer, a semi-porous layer, and a transient/barrier layer might describe the fabricated coatings.

Porous Coatings Containing Copper and Phosphorus Obtained by Plasma Electrolytic Oxidation of Titanium.

To fabricate porous copper coatings on titanium, we used the process of plasma electrolytic oxidation (PEO) with voltage control. For all experiments, the three-phase step-up transformer with six-diode Graetz bridge was used. The voltage and the amount of salt used in the electrolyte were determined so as to obtain porous coatings. Within the framework of this study, the PEO process was carried out at a voltage of 450 VRMS in four electrolytes containing the salt as copper(II) nitrate(V) trihydrate. Moreover, we showed that the content of salt in the electrolyte needed to obtain a porous PEO coating was in the range 300-600 g/dm3. After exceeding this amount of salts in the electrolyte, some inclusions on the sample surface were observed. It is worth noting that this limitation of the amount of salts in the electrolyte was not connected with the maximum solubility of copper(II) nitrate(V) trihydrate in the concentrated (85%) orthophosphoric acid. To characterize the obtained coatings, numerous techniques were used. In this work, we used scanning electron microscopy (SEM) coupled with electron-dispersive X-ray spectroscopy (EDS), conducted surface analysis using confocal laser scanning microscopy (CLSM), and studied the surface layer chemical composition of the obtained coatings by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), glow discharge of optical emission spectroscopy (GDOES), and biological tests. It was found that the higher the concentration of Cu(NO3)2∙3H2O in the electrolyte, the higher the roughness of the coatings, which may be described by 3D roughness parameters, such as Sa (1.17-1.90 µm) and Sp (7.62-13.91 µm). The thicknesses of PEO coatings obtained in the electrolyte with 300-600 g/dm3 Cu(NO3) 2∙3H2O were in the range 7.8 to 10 µm. The Cu/P ratio of the whole volume of coating measured by EDS was in the range 0.05-0.12, while the range for the top layer (measured using XPS) was 0.17-0.24. The atomic concentration of copper (0.54-0.72 at%) resulted in antibacterial and fungicidal properties in the fabricated coatings, which can be dedicated to biocompatible applications.

Development of Porous Coatings Enriched with Magnesium and Zinc Obtained by DC Plasma Electrolytic Oxidation.

Coatings with developed surface stereometry, being based on a porous system, may be obtained by plasma electrolytic oxidation, PEO (micro arc oxidation, MAO). In this paper, we present novel porous coatings, which may be used, e.g., in micromachine's biocompatible sensors' housing, obtained in electrolytes containing magnesium nitrate hexahydrate Mg(NO3)2·6H2O and/or zinc nitrate hexahydrate Zn(NO3)2·6H2O in concentrated phosphoric acid H3PO4 (85% w/w). Complementary techniques are used for coatings' surface characterization, such as scanning electron microscopy (SEM), for surface imaging as well as for chemical semi-quantitative analysis via energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), glow discharge optical emission spectroscopy (GDOES), and X-ray powder diffraction (XRD). The results have shown that increasing contents of salts (here, 250 g/L Mg(NO3)2·6H2O and 250 g/L Zn(NO3)2·6H2O) in electrolyte result in increasing of Mg/P and Zn/P ratios, as well as coating thickness. It was also found that by increasing the PEO voltage, the Zn/P and Mg/P ratios increase as well. In addition, the analysis of XPS spectra revealed the existence in 10 nm top of coating magnesium (Mg2+), zinc (Zn2+), titanium (Ti4+), and phosphorus compounds (PO43-, or HPO42-, or H2PO4-, or P2O74-).