A novel multivariate approach using science-based calibration for direct coating thickness determination in real-time NIR process monitoring

This study demonstrates an approach, using science-based calibration (SBC), for direct coating thickness determination on heart-shaped tablets in real-time. Near-Infrared (NIR) spectra were collected during four full industrial pan coating operations. The tablets were coated with a thin hydroxypropyl methylcellulose (HPMC) film up to a film thickness of 28 μm. The application of SBC permits the calibration of the NIR spectral data without using costly determined reference values. This is due to the fact that SBC combines classical methods to estimate the coating signal and statistical methods for the noise estimation. The approach enabled the use of NIR for the measurement of the film thickness increase from around 8 to 28 μm of four independent batches in real-time. The developed model provided a spectroscopic limit of detection for the coating thickness of 0.64 ± 0.03 μm root-mean square (RMS). In the commonly used statistical methods for calibration, such as Partial Least Squares (PLS), sufficiently varying reference values are needed for calibration. For thin non-functional coatings this is a challenge because the quality of the model depends on the accuracy of the selected calibration standards. The obvious and simple approach of SBC eliminates many of the problems associated with the conventional statistical methods and offers an alternative for multivariate calibration.     

Experimental Wear Behavior Analysis of Coated Spindle Hook Teeth under Real Harvesting Work Conditions

This study aimed to investigate the wear failure changes of spindle hook teeth and the reasons for such failure during field work. Spindle samples were obtained from a fixed position of the spindle bar under different field picking area conditions and combined with the spatial distribution characteristics of cotton bolls in Xinjiang. After cutting a spindle sample, a scanning electron microscope and an energy spectrum analyzer were used to characterize the micromorphology and element composition of the hook tooth surface and cross section under different working area conditions. The wear parameters of the hook teeth were then extracted. The results showed that the thickness of the coating on the surface of the hook tooth used in this study was between 66.1 µm and 74.4 µm. The major chemical element was chromium, with a small amount of nickel. During the field picking process, failure of the coating on the surface of the hook teeth initially appeared on the tooth tip and tooth edge, and then spread to the entire hook tooth surface. The wear failure of the hook teeth resulted from abrasive wear, oxidative wear, and fatigue peeling. As the picking area increased, the wear area of the hook teeth increased exponentially, while the wear width increased linearly. When the field picking area reached 533.33 ha, the maximum change rate of the wear area was 2.33 × 10³ µm²/ha, and the wear width was 1.84 µm/ha. During field work, the thickness of the coating decreased from the cutting surface to the tooth edge, and the wear rate gradually increased. The wear rate at Position 1 was the slowest, at 0.01 µm/ha, and the wear rate at Position 5 was the fastest, at 0.25 µm/ha.     

Characteristics of Cr-B Coatings Produced on Vanadis® 6 Tool Steel Using Laser Processing

The paper presents the results of a study of the microstructure, chemical composition, microhardness and corrosion resistance of Cr-B coatings produced on Vanadis 6 tool steel. In this study, chromium and boron were added to the steel surface using a laser alloying process. The main purpose of the study was to determine the impact of those chemical elements on surface properties. Chromium and boron as well as their mixtures were prepared in various proportions and then were applied on steel substrate in the form of precoat of 100 µm thickness. Depending on the type of precoat used and laser processing parameters, changes in microstructure and properties were observed. Coatings produced using precoat containing chromium and boron mixture were characterized by high microhardness (900 HV0.05–1300 HV0.005) while maintaining good corrosion resistance. It was also found that too low laser beam power contributed to the formation of cracks and porosity.     

Multilayer Diamond Coatings Applied to Micro-End-Milling of Cemented Carbide

Cobalt-cemented carbide micro-end mills were coated with diamond grown by chemical vapor deposition (CVD), with the purpose of micro-machining cemented carbides. The diamond coatings were designed with a multilayer architecture, alternating between sub-microcrystalline and nanocrystalline diamond layers. The structure of the coatings was studied by transmission electron microscopy. High adhesion to the chemically pre-treated WC-7Co tool substrates was observed by Rockwell C indentation, with the diamond coatings withstanding a critical load of 1250 N. The coated tools were tested for micro-end-milling of WC-15Co under air-cooling conditions, being able to cut more than 6500 m over a period of 120 min, after which a flank wear of 47.8 μm was attained. The machining performance and wear behavior of the micro-cutters was studied by scanning electron microscopy and energy-dispersive X-ray spectroscopy. Crystallographic analysis through cross-sectional selected area electron diffraction patterns, along with characterization in dark-field and HRTEM modes, provided a possible correlation between interfacial stress relaxation and wear properties of the coatings. Overall, this work demonstrates that high adhesion of diamond coatings can be achieved by proper combination of chemical attack and coating architecture. By preventing catastrophic delamination, multilayer CVD diamond coatings are central towards the enhancement of the wear properties and mechanical robustness of carbide tools used for micro-machining of ultra-hard materials.     

Weldability of Underwater Wet-Welded HSLA Steel: Effects of Electrode Hydrophobic Coatings

The paper presents the effects of waterproof coatings use to cover electrodes on the weldability of high-strength, low-alloy (HSLA) steel in water. With the aim of improving the weldability of S460N HSLA steel in water, modifications of welding filler material were chosen. The surfaces of electrodes were covered by different hydrophobic substances. The aim of the controlled thermal severity (CTS) test was to check the influence of these substances on the HSLA steel weldability in the wet welding conditions. The visual test, metallographic tests, and hardness Vickers HV10 measurements were performed during investigations. The results proved that hydrophobic coatings can reduce the hardness of welded joints in the heat-affected zone by 40–50 HV10. Additionally, the number of cold cracks can be significantly reduced by application of waterproof coatings on the filler material. The obtained results showed that electrode hydrophobic coatings can be used to improve the weldability of HSLA steel in underwater conditions.     

Unusual Dependence of the Diamond Growth Rate on the Methane Concentration in the Hot Filament Chemical Vapor Deposition Process

Although the growth rate of diamond increased with increasing methane concentration at the filament temperature of 2100 °C during a hot filament chemical vapor deposition (HFCVD), it decreased with increasing methane concentration from 1% CH₄ –99% H₂ to 3% CH₄ –97% H₂ at 1900 °C. We investigated this unusual dependence of the growth rate on the methane concentration, which might give insight into the growth mechanism of a diamond. One possibility would be that the high methane concentration increases the non-diamond phase, which is then etched faster by atomic hydrogen, resulting in a decrease in the growth rate with increasing methane concentration. At 3% CH₄ –97% H₂, the graphite was coated on the hot filament both at 1900 °C and 2100 °C. The graphite coating on the filament decreased the number of electrons emitted from the hot filament. The electron emission at 3% CH₄ –97% H₂ was 13 times less than that at 1% CH₄ –99% H₂ at the filament temperature of 1900 °C. The lower number of electrons at 3% CH₄ –97% H₂ was attributed to the formation of the non-diamond phase, which etched faster than diamond, resulting in a lower growth rate.     

Surface Reformation of Medical Devices with DLC Coating

We evaluated the adhesion, friction characteristics, durability against bodily acids, sterilization, cleaning, and anti-reflection performance of diamond-like carbon (DLC) coatings formed as a surface treatment of intracorporeal medical devices. The major coefficients of friction during intubation in a living body in all environments were lower with DLC coatings than with black chrome plating. DLC demonstrated an adhesion of approximately 24 N, which is eight times stronger than that of black chrome plating. DLC-coated samples also showed significant stability without being damaged during acid immersion and high-pressure steam sterilization, as suggested by the results of durability tests. In addition, the coatings remained unpeeled in a usage environment, and there was no change in the anti-reflection performance of the DLC coatings. In summary, DLC coatings are useful for improving intracorporeal device surfaces and extending the lives of medical devices.     

Performance of Green Concrete and Inorganic Coating Materials

Green concrete (GC) was developed for realizing sustainable development, recycling waste materials, and reducing environmental pollution. For the practical use of GC, various harmful materials must blocked from entering its cracks and pores; and its strength and durability must be improved. The use of an inorganic coating material (ICM) for GC effectively prevents the intrusion of harmful materials and repairs the concrete. ICMs can reduce the permeability and increase the durability of concrete. This study investigated GC, construction waste, and ICMs and used recycled sand and gravel as well as construction waste as substitutes for cement. The results indicate that the coarse aggregate substitution, water-binder ratio, and recycled fine aggregate substitution must be controlled suitably in GC. Furthermore, the coating layer, fine aggregate substitution, and aging of the ICM mut be controlled suitably. GC with an ICM showed poorer performance than conventional concrete, mainly because of the high porosity. Nonetheless, the ICM somewhate reduces the porosity and resists the penetration of chloride ions, thereby promoting concrete quality.     

Phase Composition of Al-Si Coating from the Initial State to the Hot-Stamped Condition

The chemical and phase composition of the coating and the coating/substrate interface of an Al-Si-coated 22MnB5 hot stamped steel was investigated by means of SEM-EDS, XRD, micro-XRD and electron diffraction. Moreover, the surface profile was analyzed by XPS and roughness measurements. The XPS measurements showed that the thickness of the Si and Al oxide layers increased from 14 to 76 nm after die-quenching, and that the surface roughness increased as well as a result of volume changes caused by phase transformations. In addition to the FeAl(Si) and Fe₂Al₅ phases and the interdiffusion layer forming complex structures in the coating, electron diffraction confirmed the presence of an Fe₂Al₅ phase, and also revealed very thin layers of Fe₃(Al,Si)C, Fe₂(Al,Si)₅ and Al-bearing rod-shaped particles in the immediate vicinity of the steel interface. Moreover, the scattered nonuniform layer of the Fe₂Al₈Si phase was identified in the outermost layer of the coating. Despite numerous studies devoted to researching the phase composition of the Al-Si coating applied to hot stamped steel, electron diffraction revealed very thin layers and particles on the coating/substrate interface and outermost layer, which have not been analyzed in detail.     

Green Nanocoatings Based on the Deposition of Zirconium Oxide: The Role of the Substrate

Herein, the influence of the substrate in the formation of zirconium oxide monolayer, from an aqueous hexafluorozirconic acid solution, by chemical conversion and by electro-assisted deposition, has been approached. The nanoscale dimensions of the ZrO₂ film is affected by the substrate nature and roughness. This study evidenced that the mechanism of Zr-EAD is dependent on the potential applied and on the substrate composition, whereas conversion coating is uniquely dependent on the adsorption reaction time. The zirconium oxide based nanofilms were more homogenous in AA2024 substrates if compared to pure Al grade (AA1100). It was justified by the high content of Cu alloying element present in the grain boundaries of the latter. Such intermetallic active sites favor the obtaining of ZrO₂ films, as demonstrated by XPS and AFM results. From a mechanistic point of view, the electrochemical reactions take place simultaneously with the conventional chemical conversion process driven by ions diffusion. Such findings will bring new perspectives for the generation of controlled oxide coatings in modified electrodes used, as for example, in the construction of battery cells; in automotive and in aerospace industries, to replace micrometric layers of zinc phosphate by light-weight zirconium oxide nanometric ones. This study is particularly addressed for the reduction of industrial waste by applying green bath solutions without the need of auxiliary compounds and using lightweight ceramic materials.