3.2. Relative Density and Chemical Composition
In
Table 6, the process parameters that led to the highest rel. densities for both Fe-10%Ni and Fe-10%Si alloys during the parameter study are presented. For Fe-10%Ni, sample number 4 from the third iteration achieved a rel. density of 99.960% using a laser power (P
L) of 180 W, scan speed (v
s) of 600 mm/s, and hatch distance (Δy
S) of 60 µm. In the case of Fe-10%Si, sample number 28 from the first iteration reached an even higher rel. density of 99.974% with a laser power of 140 W, scan speed of 550 mm/s, and the same hatch distance of 60 µm. These parameter sets were used as the basis for further investigations, including the production of crack-free toroidal specimens.
Crack-free production of the samples made of Fe-10%Ni was achieved using the parameter set shown in
Table 6. Although some specimens exhibited even higher rel. densities, they showed significant cracking and were, therefore, not considered for the fabrication of the toroidal samples. This is essential for the subsequent production of the toroids because cracks have a negative influence on the magnetic properties [
82]. However, cracks were found in the sample made from Fe-10%Si specimens, with the highest density showing significant cracking; to fabricate toroids, we, therefore, chose a less crack-prone but slightly lower-density parameter set, which inherently compromises magnetic performance (air-gap effect or higher losses) as shown in
Figure 5. A possible solution to this effect is to pre-heat the build chamber and substrate plate, and further adopt in situ scan strategy adaptation to reduce the thermal gradient and therefore the thermal stress during the manufacturing process [
47,
66,
72,
83].
A (pre)-heatable building platform was not available in the system used to counteract the fracture/crack formation. Instead, a parameter set (cf.
Table 6; Specimen 7, second iteration) with a lower rel. density was selected to produce the toroids (cf.
Table 6; Fe-10%Si), as the fracture formation was quantitatively lower.
To improve model accuracy and stability, the logarithm of the rel. density was used as the target variable instead of the rel. density itself. This approach helps to linearize the otherwise nonlinear relationship between process parameters and density, enhances the model’s sensitivity in the high-density range, and ensures numerical stability by better handling small variations near full density.
In
Table 7, the results of the chemical analysis performed using X-ray fluorescence analysis are shown. The results are based on spot measurements taken on the fabricated toroids and provide insights into their elemental composition.
3.2.1. Fe-10%Ni Samples
Utilizing the AI-based optimization software, initially, a regression model with a coefficient of determination (CV-R
2) of 0.55 and a standard deviation (CV-R
2-std) of 0.25 was developed. The analysis identified scan speed as the most influential parameter affecting logarithmic porosity, followed by hatch distance and laser power, based on their Gini values (0.69, 0.16, and 0.15, respectively) [
69]. The Gini importance—also known as mean decrease in impurity—quantifies how much a variable contributes to reducing the prediction error in decision tree-based models. A higher Gini value indicates that a parameter plays a more significant role in splitting the data and improving model accuracy. In this case, scan speed had by far the largest impact on predicting porosity behavior.
Since the target rel. density was not achieved initially, a second iteration was performed using “Advanced Space Filling Initialization” (ASFI). The second iteration prioritized parameter combinations with a laser power of 120 W due to higher average rel. densities observed in the first iteration. The model quality of the combined first and second iterations yielded a CV-R
2 of 0.5 and a reduced standard deviation of 0.2. Adjusted Gini values indicated that laser power’s influence increased, surpassing hatch distance but still secondary to scan speed (cf.
Table 8).
In the third iteration, process optimization was successfully achieved, with the three samples exceeding the target rel. density of ≥99.95% under fixed conditions of 180 W laser power and 60 µm hatch distance. The predictive model developed in this iteration showed improved performance, with a cross-validated coefficient of determination (CV-R
2) of 0.59 and a reduced standard deviation (CV-R
2-std) of 0.15, indicating an enhanced balance between model accuracy and robustness. This improvement was supported by the integration of 20 additional measurement points into the training dataset (cf.
Figure 6). The observed deviations in the distribution in the purple histogramm indicates systematic bias in the model used.
Final recalculations of Gini values affirmed the primary influence of scan speed (0.58), followed by hatch distance (0.37) and laser power (0.08), indicating consistent parameter importance throughout all the iterations. Three-dimensional modeling highlighted the nonlinear interactions of parameters, effectively visualizing regions with optimal rel. density.
Figure 7a–c show the predicted values of logarithmic porosity (a–c) and rel. density (d–f). In waterfall diagrams (a–c), the dark blue regions represent areas of high rel. density, indicating optimal parameter combinations for laser power, scan speed, and hatch distance. In heatmaps (d–f), the dark red regions indicate areas with a high predicted probability of achieving samples with high rel. density based on the underlying regression model and its parameter interaction analysis. One parameter is fixed to create the three-dimensional mesh diagram. The value of the fixed parameter corresponds to the respective value of the parameter combination of sample no. 4 from the third iteration (cf.
Table 6 and
Table 8).
The heatmaps (cf.
Figure 7d–f) showing the predicted rel. density of the Fe-10%Ni specimens as a function of process parameters across three optimization iterations show two-dimensional projections of the parameter space: (d) P
L vs. Δy
s, (e) P
L vs. scan speed vs., and (f) scan speed vs. vs. Δy
s. Data points are color-coded by optimization iteration: dark blue for the first iteration, orange for the second iteration, and green for the third iteration. The progressive clustering of points within the red regions highlights the optimization’s success in converging towards parameter combinations yielding high relative densities.
The parameter study was considered complete after the three samples from the third iteration exceeded the target rel. density threshold of ≥99.95% (cf.
Table 9).
3.2.2. Fe-10%Si Samples
An iterative parameter study was also conducted for Fe-10%Si using the same AI-based optimization software. The initial regression model presented a CV-R2 of 0.65 and a CV-R2-std of 0.19, indicating a robust initial model fit. The analysis showed laser power as the most influential parameter affecting logarithmic porosity, followed by scan speed and hatch distance, with respective Gini values of 0.4 (PL), 0.35 (vs), and 0.25 (Δys).
As the target rel. density was initially achieved in only one sample, a second iteration was necessary. The second iteration focused on parameter combinations around a laser power of 140 W, scan speed of 550 mm/s, and hatch distance of 60 µm, resulting in two samples surpassing the targeted rel. density of ≥99.95%, thereby concluding the parameter study.
The final regression model exhibited slightly improved quality (CV-R
2 = 0.67, CV-R
2-std = 0.14), benefiting from the addition of the second iteration’s measurement points (cf.
Figure 8). The observed roughly symmetric distribution in the purple histogramm indicates minimal systematic bias and therefore lower potential model deviations compared to the Fe-10%Ni Series.
The final Gini values showed minor changes; laser power increased slightly in importance (0.23), while scan speed (0.44) and hatch distance (0.33) decreased marginally, maintaining their relative order of influence (cf.
Table 10).
The three-dimensional visualization confirmed the nonlinear relationships between the parameters and rel. density, highlighting optimal parameter regions effectively.
Figure 9a–c show the predicted values of logarithmic porosity and relative density. One parameter is fixed to create the three-dimensional mesh diagram. The value of the fixed parameter corresponds to the respective value of the parameter combination of sample no. 7 from the second iteration (ref.
Table 6 and
Table 11).
Analogous to the parameter study of Fe-10%Ni, the areas that are close to the target value (rel. density is larger then 99.95%) are colored red. The relationship between the setting parameters and the rel. density is not linear when processing Fe-10%Si.
The final parameter combination and measured values are listed in
Table A2. The parameter study is completed because the relative density of the three samples from the third iteration is ≥99.95% (see
Table 11).
3.4. Soft-Magnetic Properties and Heat Treatments
The coercivity of sample A
Ni is approximately 50% greater than the reference value (cf.
Figure 11). However, no value is given for the permeability number. The coercivity of the heat-treated Fe-50%Ni alloy is about 6% of the measured value of sample C
Ni. At the same time, the relative permeability is about 16 times larger than that of sample C
Ni. Thus, the measured soft-magnetic properties are lower than those of the reference values and, therefore, undesirable. Furthermore, no improvements due to heat treatment are detectable.
Figure 11c,d illustrate the demagnetization curves of Fe-10%Ni toroids, where
Figure 11c represents the as-fabricated state and
Figure 11d shows the heat-treated condition at 1200 °C. The magnetic response is characterized by the B-H loops obtained under varying excitation frequencies and field strengths. The general shape of the hysteresis loops indicates a soft-magnetic behavior for both conditions, as evidenced by the relatively narrow loops and low coercivity.
A B–H loop (or hysteresis loop) is a plot of the magnetic flux density B versus the applied magnetic field strength H as you cycle the field up and down. H (in A/m) is the intensity of the external magnetic field you apply to the sample, and B (in T or mT) is the resulting magnetic flux density (or magnetization) inside the material.
As you ramp H positively and then negatively, the material’s B does not retrace the same path—this “lag” is what gives the characteristic loop shape. The area inside the loop corresponds to energy loss per cycle, and the loop’s width (coercivity) tells you how “hard” or “soft” the magnetic material is. Narrow loops with small coercive fields are the hallmark of soft magnets.
Notably, the remanent magnetization (magnetic remanence) of the heat-treated Fe-10%Ni samples (cf.
Figure 11d) remains nearly unchanged in comparison to the untreated state (
Figure 11c). Despite thermal processing, which often alters grain structure and phase composition, the material retains its ability to maintain a high remanent magnetic flux density across all the tested frequencies. This suggests that the primary magnetic domain structure remains stable and is not significantly affected by the annealing treatment at 1200 °C.
Furthermore, both sample conditions exhibit frequency-dependent behavior, with higher frequencies leading to broader loops and reduced peak magnetic flux density. This frequency-induced loss is typical for soft-magnetic materials due to eddy current and hysteresis losses.
In
Table 12, the magnetic properties of different literature Fe-Ni alloys are summarized. It should be noted that the Ni content of one of the alloys listed (Fe-50%Ni) is 40% higher than that of the Fe-Ni alloy used, which increases permeability, but also electrical conductivity and thus eddy current losses [
86]. Therefore, the values from the literature review are only used as a reference. Overall, our AI-optimized PBF-LB/M processing and subsequent heat treatments yield Fe-10%Ni soft-magnetic properties that compare favorably with—and in certain respects surpass—those reported in conventional and AM literature. Although our as-fabricated coercivity (Hc ≈ 1621 A/m) is higher than the 1074 A/m typically observed for conventionally cast Fe-10%Ni, this elevation can be directly linked to the refined AM microstructure and residual stresses inherent to PBF-LB/M. Crucially, high-temperature annealing (1 h at 1200 °C) restores permeability (µR ≈ 299) to values nearly identical to the as-built state, demonstrating effective stress relief without excessive grain growth. By contrast, Fe-50%Ni alloys achieve much higher permeability (µR ≈ 4700) and lower coercivity (Hc ≈ 100 A/m), but at the expense of increased eddy current losses due to greater electrical conductivity. In this context, our results highlight that the Fe-10%Ni composition, processed under xT-Saam-optimized parameters and judiciously annealed, strikes an optimal balance between magnetic softness, energy loss, and manufacturability, positioning it as a highly competitive candidate for next-generation soft-magnetic components.
Figure 12 presents the magnetic behavior of Fe-10%Ni samples in two complementary ways: (a) shows µ
r as a function of J, while (b) depicts the corresponding B-H hysteresis loops. The samples represent different processing states: A
Ni is the as-fabricated condition, B
Ni was heat-treated at 340 °C for 5 h, and C
Ni at 1200 °C for 1 h. (cf.
Table 12) In subfigure (a), sample B shows a significantly lower relative permeability across the entire polarization range compared to samples A
Ni and C
Ni. This indicates that the thermal treatment at 340 °C was ineffective in improving the magnetic softness and may have even introduced additional microstructural inhomogeneities (e.g., partial stress relaxation without grain growth). In contrast, sample C
Ni, which underwent a high-temperature heat treatment, shows a recovery of permeability values comparable to the reference sample A, suggesting partial grain growth and reduced pinning sites for domain wall movement.
Figure 11c,d supports this interpretation: the B-H loop for sample B
Ni is wider and flatter, indicating increased coercivity and reduced saturation behavior, both of which are signs of higher hysteresis losses. The loops of samples A
Ni and C
Ni are narrower and more ‘ideal’, suggesting better soft-magnetic performance and lower energy dissipation per magnetization cycle.
From this, it can be concluded that sample B
Ni exhibits increased iron losses, likely due to suboptimal microstructural evolution during low-temperature annealing. The combination of high coercivity, reduced permeability, and a broad hysteresis loop points to elevated hysteresis and eddy current losses. Sample C
Ni, while not showing a dramatic improvement over A
Ni, benefits from the high-temperature treatment, which partially restores magnetic performance. These findings underscore the importance of properly tailored heat treatments to achieve favorable microstructural conditions, especially grain size enlargement and orientation, for minimizing iron losses in soft-magnetic materials. The low coercivity of samples A
Ni-C
Ni is due to the comparatively high core losses [
21]. Core losses refer to the energy dissipated due to hysteresis and eddy current effects. Due to the high coercivity compared to the reference values, the permeability number is negatively affected [
21,
87,
88]. The observed high iron losses in the investigated Fe-based samples can be attributed primarily to the microstructural state of the material. Iron losses, comprising both hysteresis and eddy current losses, are known to be strongly influenced by grain size, crystallographic texture, and electrical resistivity. In the as-fabricated state, the fine-grained microstructure with randomly oriented grains leads to an increased density of domain wall pinning sites, thereby raising the energy required for magnetization reversal and contributing to elevated hysteresis losses. Furthermore, insufficient grain growth and the absence of a pronounced texture after thermal treatment can limit the expected improvement in magnetic softness. PBF-LB/M leaves a melt-pool/cellular substructure, residual porosity, and rough internal surfaces; moreover, minor inclusion populations associated with in situ blending persist after annealing. These features act as efficient domain-wall pinning sites and are not eliminated by a single short high-temperature hold. In parallel, the build-direction columnar grains and solidification-induced texture are only partially recovered; stress is relieved, but crystallographic orientations are not sufficiently randomized, and grains do not coarsen enough to facilitate easy wall motion. As a result, macroscopic coercivity remains governed by persistent pinning and texture rather than by dislocation density alone. Further reduction in Hc will require thermal schedules that disrupt melt-pool substructure and promote recrystallization/texture randomization (e.g., stepwise stress-relief → recrystallization or field annealing), potentially complemented by process-side measures (pre-heating, scan-strategy/porosity mitigation). In addition, the electrical conductivity of the alloy, particularly in Ni-rich compositions, facilitates the formation of eddy currents under alternating magnetic fields, further increasing the total core losses. These combined effects result in a degradation of the magnetic performance, as evidenced by reduced permeability and higher coercivity, and emphasize the critical role of tailored microstructure—especially grain size enlargement and orientation control—in minimizing iron losses in soft-magnetic materials.
The coercivity of the Fe-Si alloy used decreases after the heat treatment (cf.
Figure 12). The minimum is HC = 300 A/m for sample C
Si. This behavior is consistent with the relationship between thermal processing and magnetic softness described in
Section 2.8. The relative permeability µ
R increases correspondingly, attaining a maximum of µ
R = 1114 for sample C
Si—nearly three times higher than that of the untreated sample. At the same time, a favorable grain orientation with respect to the magnetic field direction minimizes magnetocrystalline anisotropy barriers, further enhancing the permeability. Thus, it is the deliberate control of microstructural features, especially grain size and orientation, that governs the soft-magnetic behavior of the alloy after heat treatment. The observed improvements in magnetic performance in sample C
Si are therefore a direct manifestation of targeted microstructural optimization.
Figure 13 displays the demagnetization curves of Fe-10%Si toroids, with (c) representing the untreated samples and (d) showing the heat-treated samples after annealing at 1100 °C. The hysteresis loops recorded under various frequencies reveal the magnetic behavior of the material in both states.
The remanent magnetization (Br) remains largely stable even after heat treatment, as the comparison between the untreated and annealed samples shows. This indicates that the microstructural changes induced by annealing at 1100 °C do not significantly affect the domain alignment or saturation retention of the Fe-10%Si alloy. The near-identical remanent values across a range of frequencies support the conclusion that the material retains its soft-magnetic properties post-treatment.
As observed with other soft-magnetic materials, the hysteresis loops become progressively wider and less saturated at higher frequencies, primarily due to increased eddy current losses and dynamic domain wall motion resistance. The comparison also shows that while heat treatment may slightly reduce coercivity and energy loss per cycle, it does not adversely affect the material’s ability to retain magnetic flux.
Overall, both the as-fabricated and thermally treated Fe-10%Si samples exhibit good magnetic retention and typical frequency-dependent behavior, making them suitable candidates for applications requiring soft-magnetic performance under dynamic excitation.
Figure 14 shows the magnetic behavior of Fe-10%Si samples in two complementary ways: (a) shows µr as a function of J, while (b) depicts the corresponding B-H hysteresis loops. The samples represent different processing states: A
Si is the as-fabricated condition, and C
Si at 1100 °C for 1 h. (cf.
Table 13).
In
Table 13, the magnetic properties of a similar Fe-Si alloy from the literature with a Si content of 6.9%wt ≅ 13.5%at are summarized. It should be noted that as the Si content increases, the coercivity decreases and the permeability increases [
82]. For this reason, the values are only used as a reference.
The coercivity of sample A
Si is larger than the reference value (ref.
Table 13). The relative permeability of the reference is about five times larger compared to that of sample A
Si [
54,
82]. The measured coercivity of Fe-13.5%Si after heat treatment at 700 °C for 5 h was about half the measured value of untreated Fe-13.5Si. In the present study, the same heat treatment also led to a decrease in coercivity, but not to the same extent. Compared to the untreated reference alloy with 13.5% Si, which has a coercivity of 100 A/m, this is still about three times higher. Thus, while the thermal treatment in this work led to a considerable improvement, particularly by reducing coercivity by nearly one order of magnitude, the absolute values reported in the literature are not fully reached. This discrepancy can be attributed to differences in chemical composition (higher Si content in the literature alloys), potential inhomogeneities from powder blending, and the formation of cracks during processing, which likely reduce the effectiveness of the heat treatment. The benchmarks cited use up to Fe-50%Ni or Fe-13.5%Si; both compositions intrinsically enable lower coercivity/higher permeability than the used Fe-10%Ni and Fe-10%Si, even after annealing. The permeability is approximately doubled after heat treatment, but the absolute value achieved was only about one-fifth of the reference value for Fe-13.5%Si. These proportions are also present after heat treatment at 1150 °C for 1 h. The coercivity of Fe-13.5%Si was only about one-third of the measured value after heat treatment at 700 °C for 5 h. The permeability of Fe-13.5%Si is almost 24 times larger than that of sample C
Si after heat treatment at 1150 °C for 1 h. Overall, the measured magnetic properties are lower than the reference values. In addition, the samples cannot be produced crack-free with the determined parameter combination (cf.
Figure 5). Cracks act as local air gaps with low magnetic permeability, significantly disturbing the magnetic flux path. As a result, additional magnetic energy is required to overcome these discontinuities, leading to increased coercivity and higher hysteresis losses [
54,
82]. As a result, the coercivity increases and the permeability number decreases [
54,
82,
89].
The physical and magnetic properties of the materials correlate with each other [
32,
82]. Since soft magnets are characterized by low coercivity and high permeability compared to other magnets, the magnetic properties are improved by a reduction in internal stresses and grain growth. Furthermore, core losses are reduced. These relate to the total energy lost through the generation of heat. It is the loss that occurs in a magnetic core due to alternating magnetization, which is the sum of the hysteresis loss and the eddy current loss. One reason for this is that the expansion of the domains is hindered by internal stresses and grain boundaries. This can be compensated for by heat treatment of the geometry [
45,
46,
75,
76,
82]. A plausible reason for the low magnetic properties is the orientation of the toroids during the PBF-LB/M process. In the present work, the bases of the samples are located in the XY-plane, and the specimens are built along the Z-direction using the PBF-LB/M process. Due to the high cooling rates and steep thermal gradients inherent to the process, a fine-grained microstructure typically forms within the XY-plane. In contrast, elongated grains or directional grain growth may develop along the build direction (
Z-axis), which corresponds to the YZ- and XZ-planes. This phenomenon is characteristic of the epitaxial solidification behavior observed in additively manufactured materials, where the grain structure reflects the thermal history of the process.
It is important to note that post-processing heat treatments and stress-relief annealing (ref.
Table 13) can significantly influence the as-built microstructure. Depending on the applied parameters, such treatments may lead to partial or complete recrystallization and thus reduce the anisotropy of the grain structure. However, in many cases, residual texture and morphological differences between planes may still remain, which can impact the mechanical properties of the material [
90,
91,
92,
93,
94].
As a result, the orientation of the magnetic flux density during the magnetization process of the toroids is perpendicular to the XZ-plane. Due to the fine-grained structure present there, the propagation of the domains is impeded, and thus the coercivity increases and the permeability number decreases. However, the comparatively coarse-grained structure of the YZ-plane can be utilized by rotating the toroids so that the base lies in this plane. This should decrease the coercivity and increase the permeability number [
77,
82].