Wet ball milling of niobium by using ethanol, determination of the crystallite size and microstructures

This study investigates the effect of using ethanol as the process control agent during the wet ball milling of niobium (Nb). Dried nanocrystal Nb powders, of high purity, with particle sizes, ranging from 8.5 to 14.3 nm, were synthesized by ball milling. Commercial Nb powder of particle sizes of − 44 µm was employed by using the planetary ball mill equipped with stainless still vials with still balls in ethanol. A ball-to-powder mass ratio of 10:1 was used at a rotation speed of 400 rpm, an interval of 15 min with an interval break of 5 s, and a milling time of 10 h. The powder was dried in vacutec at a temperature of 100 °C, using a speed of 15 rpm in the vacuum of 250 mbar at a time of approximately 653 min. The crystal phase of the dried powders was analyzed using X-ray diffraction (XRD) with CuKɑ radiation, and by modification of the Scherrer equation, a single crystallite size of 11.85 nm was obtained. The morphology of the particles was observed using scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS). The XRD results show that the pure crystal sizes in nanometre (nm), which decreases as the 2θ and the full width at half maximum (FWHM) increases.

Surface Studies on Glass Powders Used in Commercial Glass-Ionomer Dental Cements

The surface properties of three commercial ionomer glass powders, i.e., Fuji IX, Kavitan Plus and Chemadent G-J-W were studied. Samples were analyzed by X-ray fluorescence spectroscopy (XRF), and the density was determined by gas pycnometry. Morphology was studied using scanning electron microscopy (SEM) and laser diffraction (LD) technique, whereas low-temperature nitrogen sorption measurements determined textural parameters like specific surface area and pore volume. Thermal transformations in the materials studied were evaluated by thermogravimetric analysis (TGA), which was carried out in an inert atmosphere between 30 °C and 900 °C. XRF showed that Fuji IX and Kavitan Plus powders were strontium-based, whereas Chemadent G-J-W powder was calcium-based. Powders all had a wide range of particle sizes under SEM and LD measurements. Specific surface areas and pore volumes were in the range 1.42–2.73 m2/g and 0.0029 to 0.0083 cm3/g, respectively, whereas densities were in the range 2.6428–2.8362 g/cm3. Thermogravimetric analysis showed that the glass powders lost mass in a series of steps, with Fuji IX powder showing the highest number, some of which are attributed to the dehydration and decomposition of the polyacrylic acid present in this powder. Mass losses were more straightforward for the other two glasses. All three powders showed distinct losses at around 780 °C and 835 °C, suggesting that similar dehydration steps occur in all these glasses. Other steps, which differed between glass powders, are attributed to variations in states of water-binding on their surfaces.

In situ measurement and closed-loop control for powder supply processes

The powder mass flow rate is one of the main parameters regarding the geometrical precision of built components in the additive manufacturing process of laser metal deposition. However, its accuracy, constancy, and repeatability over the course of the running process is not given. Reasons among others are the performance of the powder conveyors, the complex nature of the powder behavior, and the resulting issues with existing closed-loop control approaches. Additionally, a direct in situ measurement of the powder mass flow rate is only possible with intrusive methods. This publication introduces a novel approach to measure the current powder mass flow rate at a frequency of 125 Hz. The volumetric powder flow evaluation given by a simple optical sensor concept was transferred to a mass flow rate through mathematical dependencies. They were found experimentally for a nickel-based powder (Inconel 625) and are valid for a wide range of mass flow rates. With this, the dynamic behavior of a vibration powder feeder was investigated and a memory effect dependent on previous powder feeder speeds was discovered. Next, a closed-loop control with the received sensor signal was implemented. The concept as a whole gives a repeatable and accurate powder mass flow rate while being universally retrofittable and applicable. In a final step, the improved dynamic and steady performance of the powder mass flow rate with closed-loop control was validated. It showed a reduction of mean relative errors for step responses of up to 81% compared to the uncontrolled cases.

Correlations between Process and Geometric Parameters in Additive Manufacturing of Austenitic Stainless Steel Components Using 3DPMD

The additive manufacturing of components is characterized by a layered build-up. The stability of the build-up process with regard to the component geometry and the layer thickness is essential for the success of the entire system. A prerequisite for this is the exact knowledge of the interrelationships between the process, construction parameters and the resulting component geometry, respectively. These correlations are determined within the study using the 3D Plasma Metal Deposition Process (3DPMD). For this purpose, the process is first subjected to a system analysis. Possible influencing variables were identified with regard to the question “Which system parameters influence the component geometry?” and then prioritized. Then, the influence of control factors (welding current intensity, welding speed, and powder mass flow) was investigated according to the specifications of the Design of Experiments (DOE) method by means of a full-factorial experimental design and evaluated on the basis of metallographic cross-sections. As a result, it was determined that the system parameter powder mass flow only influences the layer thickness and not the wall thickness and is, therefore, available as a process control variable. In sum, comprehensive knowledge of complex relationships between the control parameters and the component geometry in additive manufacturing using 3DPMD was achieved and forms the basis for further scientific work.

Consolidation of Titanium Powder by Electrical Resistance Sintering: Practice and Simulation

In this work, a commercially pure titanium powder has been consolidated using the Electrical Resistance Sintering (ERS) process. This technique consists in the consolidation of a powder mass by the simultaneous application of pressure (80 MPa, in this work) and heating caused by the passage of a high intensity (3.5-6.0 kA, in this case) and low voltage current (lower than 10 V), during short dwelling times (0.8-1.6 s, in this work). The resulting compacts have been mechanically characterised by measuring their microhardness distribution. The results obtained are compared with the corresponding values of compacts prepared with the same powders following the conventional P/M route of cold pressing and furnace sintering. The results of some simulations are provided to give information about the temperatures reached inside the compacts during the electrical consolidation process.

The mixing of cohesive and flowable powder materials using a common laboratory powder mixer

This study presented the homogeneity obtained when mixing cohesive and flowable powder materials using a laboratory powder mixer. The mixing process parameters studied were the mixing time and the mixer rotational speed (20 rpm, 40 rpm and 60 rpm) at the different ratios (95%: 5%, 50%: 50% and 5%: 95%) of the cohesive cocoa and flowable mannitol powder materials. The homogeneity sampled at the powder bed surface showed that only at the highest rotational speed of 60 rpm used in this work yield acceptable homogeneity at the two extremes of the powder mass ratios; 95%: 5% and 5%: 95% of mannitol: cocoa for some of the locations on the powder bed surface, especially near the wall of the mixer. Other combinations of the experimental conditions did not yield acceptable mixture homogeneity. These results showed the difficulties in obtaining a homogeneous powder mix when mixing cohesive powder materials, especially in academic teaching and research laboratories using a simple powder mixer apparatus.

Uji Efektivitas Cangkang Keong Mas (Pomacea canaliculata L.) Sebagai Biosorben Dalam Menyerap Logam Berat Merkuri (Hg)

Adsorbent is one of the effective solutions to reduce the Hg metal content. The golden snail is a pest for agricultural and contains high of calcium carbonate. However, calcium carbonate can be used as an adsorbent. This study aimed to examine the effectiveness of golden snail shell powder in absorbing Hg metal. This research is a quantitative study consisting of dependent variables and independent variables. The dependent variable involved a concentration of 10 ppm mercury, and 100 rpm stirring time speed while the independent variable included of variations in powder mass and stirring time. The mass of golden snail powder used those are 0 gr, 5 gr, 10 gr, 15 gr, and 20 gr with a variation of stirring time for 15 minutes and 30 minutes for each sample of Hg metals. Each Hg sample was used at a concentration of 10 ppm. The calculation results obtained that the effectiveness of golden snail shell powder in absorbing Hg 10 ppm was the mass of 20 grams of golden snail powder with a stirring time of 30 minutes that was equal to 99.87% with the result of a decrease in concentration of 10 ppm Hg to 0.01 Hg ppm.