Comparison of the Processability and Influence on the Microstructure of Different Starting Powder Blends for Laser Powder Bed Fusion of a Fe3.5Si1.5C Alloy

This paper examines different blends of starting materials for alloy development in the laser powder bed fusion (LPBF) process. By using blends of individual elemental, ferroalloy and carbide powders instead of a pre-alloyed gas-atomized starting powder, elaborate gas-atomization processes for the production of individual starting powders with varying alloy compositions can be omitted. In this work the model alloy Fe3.5Si1.5C is produced by LPBF from different blends of pure elemental, binary and ternary powders. Three powder blends were processed. The base material for all powder blends is a commercial gas-atomized Fe powder. In the first blend this Fe powder is admixed with SiC, in the second with the ternary raw alloy FeSiC and in the third with FeSi and FeC. After characterizing the powder properties and performing LPBF parameter studies for each powder blend, the microstructures and the mechanical properties of the LPBF-manufactured samples were analyzed. Therefore, investigations were carried out by scanning electron microscopy, wave length dispersive x-ray spectroscopy and micro hardness testing. It was shown that the admixed SiC dissolves completely during LPBF. But the obtained microstructure consisting of bainite, martensite, ferrite and retained austenite is inhomogeneous. The use of the lower melting ferroalloys FeSi and FeC as well as the ternary ferroalloy FeSiC leads to an increased chemical homogeneity after LPBF-processing. However, the particle size of the used components plays a decisive role for the dissolution behavior in LPBF.

API Content and Blend Uniformity Using Quantum Cascade Laser Spectroscopy Coupled with Multivariate Analysis

The process analytical technology (PAT) initiative proposed by the US Food and Drug Administration (FDA) suggests innovative methods to better understand pharmaceutical processes. The development of analytical methods that quantify active pharmaceutical ingredients (APIs) in powders and tablets is fundamental to monitoring and controlling a drug product’s quality. Analytical methods based on vibrational spectroscopy do not require sample preparation and can be implemented during in-line manufacturing to maintain quality at each stage of operations. In this study, a mid-infrared (MIR) quantum cascade laser (QCL) spectroscopy-based protocol was performed to quantify ibuprofen in formulations of powder blends and tablets. Fourteen blends were prepared with varying concentrations from 0.0% to 21.0% (w/w) API. MIR laser spectra were collected in the spectral range of 990 to 1600 cm−1. Partial least squares (PLS) models were developed to correlate the intensities of vibrational signals with API concentrations in powder blends and tablets. PLS models were evaluated based on the following figures of merit: correlation coefficient (R2), root mean square error of calibration, root mean square error of prediction, root mean square error of cross-validation, and relative standard error of prediction. QCL assisted by multivariate analysis was demonstrated to be accurate and robust for analysis of the content and blend uniformity of pharmaceutical compounds.

Effect of bimodal powder blends on part density and melt pool fluctuation in laser powder bed fusion

The final part density in laser powder bed fusion is influenced by the powder particle size distribution. Too fine powders are not spreadable, and too coarse powders cause porosity. Powder blends, especially bimodal ones, can exhibit higher packing densities and changes in flowability compared to their monomodal constituents. These properties can influence final part density. Therefore, the influence of bimodal powder on final part density was investigated. Two gas atomized 316L (1.4404) powders with a D50 of 20.3 µm and 60.3 µm were blended at weight ratios of 3:1, 1:1, and 1:3, and the original and blended powders were processed. The results show that the final part porosity increases almost linearly with an increasing volume fraction of coarse powder. Furthermore, the final part density is independent of powder bulk density and flowability. Measurements of the top surface show that an increase of part porosity by coarse powder is caused by an increase in melt pool fluctuation, which in turn causes irregular solidified scan tracks. Additionally, the results show that the powder segregation during coating is stronger for the bimodal powder; however, no influence of the segregation on the part density could be found.