Arrays of magnetic nanowires (NWs) are an attractive platform with tremendous potential for developing novel magnetic applications, e.g., next-generation information technologies or sensors [1]. The synthesis of NWs by electrochemistry shows multiple degrees of freedom allowing for tailoring the composition, crystallographic structure and, consequently, magnetic properties [2,3]. Herein, FeNi NWs were grown by electrodeposition into anodized aluminum oxide (AAO) membranes (Fig. 1a). The broad range of electrolytes and voltages used, allowed us to study the anomalous FeNi co-deposition by a compositional analysis, being explained within a modified Bocris-Drazic-Despic (BDD) model [4]. X-ray diffraction patterns showed a change from bcc crystallographic structure for Fe-rich NWs to fcc structure at mid and low Fe content, with biphasic bcc-fcc phase for equiatomic NWs. Tuning the synthesis conditions led to FeNi NWs with a range of magnetic hardness, observing an increase in coercivity (from 0.2 kOe to 1 kOe) for a decreased Fe content (Fig. 1b). Coercivity angular measurements showed that the magnetization reversal is dominated by transverse domain wall reversal and indicated a decrease in magnetostatic interactions among NWs as the source of the coercivity rise. First-order reversal curves (FORCs) highlighted the limited role of the magnetic interactions in the arrays, except for Fe0.80Ni0.20 NWs which showed a FORC diagram for magnetically interacting NWs (Fig. 1c). This study shows how the magnetic properties of the NWs can be tailored through an optimized control of the synthesis conditions and adapted to the requirements of the final application. Fig. 1: (a) SEM image of NWs grown inside the AAO template, (b) Hysteresis loops for FeNi NWs with different compositions, and (c) FORC diagram for Fe0.80Ni0.20 NWs. Acknowledgements Authors acknowledge support from EU M-ERA.NET and MICINN through COSMAG (PCI2020-112143) and NEXUS (PID2020-11521RB-C21). A.J.C.-H. and E.M.P. acknowledge support from "La Caixaâ€ Foundation (ID 100010434) through the Doctoral INPhINIT Incoming program (LCF/BQ/DI20/1178002) and AEI (JdC-I program, IJC2020-043011-I/MCIN/AEI/10.13039/501100011033) and EU by NextGenerationEU/PRTR, respectively.

Analysis of the Magnetic Interactions in FeNi Nanowire Arrays through FORC and Angular Coercivity Measurements

Ferrites and magnetic nanoparticles (NPs) are widely used in sectors such as energy, electronics and biomedicine [1,2]. This work shows an optimum combination of co-precipitation, milling and reduction process of ferrite precursors (CoFe2O4 and NiFe2O4) to obtain CoFe and NiFe NPs, respectively, with tailored magnetic properties and improved heat generation for magneto-thermal applications. Ferrite precursor powders have been synthesized by co-precipitation [3] followed by nanostructuring through self-developed ultrafast milling (24 min). Reduction at different temperatures under Ar+H2 has led to NPs with a tuneable composition going from pure ferrite to CoFe and NiFe NPs, with core-shell nanostructures (CoFe2O4-CoFe and NiFe2O4-NiFe) at intermediate reduction stages. An optimized temperature has resulted in CoFe and NiFe NPs with a high saturation magnetization of 235 and 149 emu/g, respectively. Milling has allowed for diminishing the reduction temperature in 100 °C compared to that required for non-milled particles, which is of relevance in view of upscaling (Fig. 1) [4]. The magneto-thermal response of the NPs has been studied by exposure to alternating magnetic fields at 103 kHz for 5 min. Remarkably, an increase of 28% in the heat generated (under an applied field of 20 mT) has been obtained for the reduced milled CoFe NPs in comparison to the non-milled NPs (Fig. 2), due to particle refinement and high saturation magnetization. The milled NiFe NPs has shown a lower heat generation due to agglomeration effects. This cost-efficient and scalable approach eases the synthesis of NiFe and CoFe NPs for magneto-thermal applications. Acknowledgments. Authors acknowledge financial support from EU M-ERA.NET through COSMAG project (PCI2020-112143); from MICINN through NEXUS project (PID2020-115215RB-C21); and from CM through NanoMagCOST project (P2018/NMT-4321). A.J.C.-H. acknowledges support from "La Caixa" by the Doctoral INPhINIT Incoming program (LCF/BQ/DI20/1178002).

![](https://assets.underline.io/uploads/markdown_image/1/image/3d3878bca20e35efefe648bf0daa5801.jpg)

Fig.1. (a) Room temperature hysteresis loops and (b) XRD patterns of milled cobalt ferrite NPs reduced at different temperatures.

![](https://assets.underline.io/uploads/markdown_image/1/image/1e335e0631e7215287a7642ecf21df92.jpg)

Fig.2. Magneto-thermal measurements of milled and non-milled CoFe NPs.

Scalable Synthesis of CoFe and NiFe Nanoparticles from Ferrite Precursors with Tailored Magneto-Thermal Properties by a Combined Co-precipitation, Milling and Reduction Process

Permanent magnets (PMs) are indispensable in sectors as important as energy and electromobility. MnAlC is an excellent rare earth-free candidate to contribute to fill the gap existing between ferrites and NdFeB magnets, provided a successful development of its PM properties. This will be only possible by combining a high magnetization, through a maximized content of the only ferromagnetic phase in the MnAl system (τ-phase), and an enhanced coercivity, through efficient nanostructuring and phase transformation [1]. We have recently shown the importance of combining the formation of the β-Mn phase and Mn3AlC to increase coercivity -while maintaining a high remanence- in both powder and bulk MnAlC magnets produced by a simplified hot-pressing method [2]. The choice of specific additives may be a successful route to enhance magnetic properties [3]. This study shows the possibility of reaching a coercivity exceeding 2.5 kOe (200 kA/m) for 1 at.% Mo- and Cr-doped MnAlC powder and 3.3 kOe (263 kA/m) for V-doped MnAlC powder. This has been possible by combining gas-atomization and the self-developed flash-milling method (30-240 s) for efficient nanostructuring and promoting the creation of nanoprecipitates acting as pining centers [4]. A five-fold increase in coercivity has been achieved by comparison with that of the unmilled powder (see Fig. 2 for Mo-doped MnAlC). Furthermore, a proper choice of the milling time followed by an optimized annealing has allowed for combining high coercivity with an enhanced remanence (35 emu/g for a Cr-doped MnAlC sample) [4]. This approach opens a new path for engineering novel MnAlC doped nanostructures with promising PM properties. Acknowledgments. Gas-atomized powder was synthesized by Höganäs AB under the industrial project ECNanoManga between Höganäs and IMDEA Nanociencia. IMDEA acknowledges financial support by NEXUS project (PID2020-115215RB-C21) from MICINN.


![](https://assets.underline.io/uploads/markdown_image/1/image/405da192b48636c20674a5c79f4d28da.jpg)

![](https://assets.underline.io/uploads/markdown_image/1/image/1c8762f8591e2521a169282b95770c06.jpg)


Effect of Dopants (Mo, Cr, V) on the Magnetic Properties of Mn-Al-C nanostructured by Flash-Milling

Effect of Dopants (Mo, Cr, V) on the Magnetic Properties of Mn-Al-C nanostructured by Flash-Milling

Ferrites are the most used permanent magnets (PMs) due to their availability and low cost, being an alternative to PMs based on critical rare-earths in new applications such as electromobility [1]. In this work we will show the possibility of 3D-printing objects using strontium ferrite powder obtained by successful recycling of the residue generated from manufacturing commercial ferrite magnets. Tuning the morphology and microstructure of the Sr-ferrite residue by post-processing made possible to end with Sr-ferrite powder with PM properties superior, not only to the residue precursor, but to those of the brand new commercial powder (3.5 fold increase in coercivity and a 25% increase in remanence) [2]. The recycled ferrite was used as precursor for synthesizing composites by the solution casting method [3], and extruding filaments for advanced manufacturing of magnets (with a particle content up to 65 wt%) by Fused Filament Fabrication. Magnetic characterization of composites, filaments and printed objects was performed by Vibrating Sample Magnetometer (VSM), showing that the magnetization scales accordingly to the content of ferrite particles and that there is no deterioration of the PM properties of the starting particles along processing (Fig. 1). Scanning Electron Microscopy (SEM) analysis showed a homogeneous distribution of the particles in the polymer matrix (Fig. 2) [4]. This work has shown an efficient path for developing new and alternative PMs by the combination of recycling and 3D-printing. Acknowledgements. Authors acknowledge financial support from MICINN by NEXUS project (PID2020-115215RB-C21), industrial collaboration PLASMAG with IMA S.L.U. and from the Regional Government of Madrid by NanoMagCOST project (P2018/NMT-4321).

![](https://assets.underline.io/uploads/markdown_image/1/image/ac2f3c775797ab289c0ec1e59559f011.jpg)

Fig. 1. (a) First and second quadrants of the hysteresis loops of starting powder and composites with different content of ferrite. (b) Normalized hysteresis loops of the starting powder, composite and 3D-printed object. Insets show a 3D-printed piece based on ferrite particles.

![](https://assets.underline.io/uploads/markdown_image/1/image/ce076f52b81f87799a6418acd5c64cfb.jpg)

Fig. 2. SEM images of: (a) cross section and (b) closer view of a magnetic filament with a 50 wt% of ferrite; and (c) and (d) inner morphology of a 3D-printed object with a particle content of 65 wt%.

A Sustainable Route for Permanent Magnets Fabrication: Additive Manufacturing Applied to Recycled Ferrite Residues

Additive manufacturing (AM) of composites is attracting much interest in high-tech sectors for fabricating complex high-performance objects with tailored properties [1]. For permanent magnets (PMs), the challenge is to develop magnets by AM with no geometrical restrictions, high filling factor (FF), and non-deteriorated PM properties [2], together with finding alternatives (e.g., improved ferrites and promising MnAlC-based alloys) to rare earth-based magnets [3]. Composites (PM particles/polymer) were synthesized by solution casting, followed by extrusion of filaments for 3D-printing, being reported for the very first time (Fig. 1). Several alternative PM materials were studied (gas-atomized τ-MnAlC, Sr-ferrite and hybrids —Sr-ferrite/NdFeB). Particle size and fine-to-coarse particles ratio (FP/CP) play a key role on the flexibility and powder loading of MnAlC filaments (length&gt;10 m), reaching FF&gt;80% and non-deteriorated PMs properties (Fig. 1) [4]. These results will be compared to the obtained for filaments based on Sr-ferrite (Hc=239 kA/m, FF=92%), NdFeB (Hc=812 kA/m, FF=93%) and hybrids (Hc=629 kA/m, FF=90%) (Fig. 2). MnAlC-based objects were 3D-printed under controlled temperature, proving that alternative PM materials can be efficiently synthesized and processed to develop novel PMs by AM (Fig. 1) [4]. Acknowledgements. Authors acknowledge collaborations with B. Skårman, H. Vidarsson and P.-O. Larsson (Höganäs, Sweden) by the industrial contract GAMMA, and A. Nieto and R. Altimira (IMA, Spain), and financial support from: EU M-ERA.NET by COSMAG project (PCI2020-112143); MICINN by NEXUS project (PID2020-115215RB-C21); CM by NanoMagCOST project (P2018/NMT-4321).

![](https://assets.underline.io/uploads/markdown_image/1/image/3da8e2e0919c7ea3ed6b01fc3af543f4.jpg)

Fig. 1. (a) Gas-atomized MnAlC, polymer, and composite; (b) SEM image of MnAlC particles and size distribution; (c), (d) image and SEM cross section of a MnAlC/ABS filament; (e) MnAlC-based 3D-printed object; (f) normalized magnetic response of MnAlC-based samples; and (g) magnetic flux density of a 3D-printed MnAlC-based disc.


![](https://assets.underline.io/uploads/markdown_image/1/image/b00d3d1a8d0386d3ac76cfe5a8bfe75e.jpg)

Fig. 2. (a) SEM and EDX of a hybrid composite; (b) second quadrant of the hysteresis loops for the hybrid, Sr ferrite- and NdFeB-based materials. Insets show composite pellets and SEM cross section of a Sr ferrite-based filament.

Optimizing the Particle Size Distribution in Permanent Magnet Composites to Extrude Flexible Filaments for Additive Manufacturing

Nowadays the use of permanent magnets (PMs) plays a key role in different applications such as energy and electromobility. In order to obtain a high magnetic performance, the most extended choice is PMs containing rare-earths (REs). Alternative RE-free PM materials are investigated to plug the gap between ferrites and NdFeB magnets [1]. MnAlC alloy is a promising RE-free PM candidate, but further optimization is required in order to achieve a proper combination of saturation magnetization (provided by the only ferromagnetic phase of the system: L10 or τ-MnAl) and coercivity. Studies on MnAl alloys typically focus on obtaining a maximum content of τ-phase, which results in an optimized saturation magnetization [2]. We have recently shown the possibility of developing coercivity in gas-atomized MnAl powder by applying milling times as short as 30-270 s via the self-developed “flash milling” method [3]. A successful combination of nanostructuring and a controlled phase transformation process is behind the observed increase in coercivity [3]. In this study we have used ε-phase MnAlC powder produced by gas-atomization and flash-milling (60 s) to fabricate MnAlC bulk magnets, with no need to transform previously the ε into τ phase. Under the optimal combination of pressure (300 MPa) and temperature (600 °C), hot-pressing applied to ε-phase MnAlC alloy has been able to manage simultaneously the ε-to-τ transformation and the powder compaction to end with a high-density (93%) MnAlC magnet [4]. Figure 1(a) shows the X-ray diffraction pattern of the precursor ε-phase loose powder and the successful transformation into τ-phase after the hot-pressing process. The room temperature hysteresis loops measured for the hot-pressed magnet showed an enhancement of the coercivity of up to 25 % and a slightly superior magnetization at remanence by comparison with the annealed gas-atomized loose powder (Fig. 1 (b)). The large coercivity obtained for the magnet may be explained based on the formation of both β-Mn and Mn3AlC phases together with a reduced mean crystallite size (27 nm) and the induced strain during compaction [4]. On this basis, we have demonstrated that coercivity of the compacted magnet can be further increased in about 15% by starting from flash-milled gas-atomized powder, due to a larger content of β-Mn and Mn3AlC phases. We have obtained comparable magnetization and coercivity values when compacting the starting material with a crystallographic structure based on τ-phase (i.e., involving two steps: annealing for managing ε into τ phase transformation followed by hot-pressing), thus validating our single-step process. This is a promising cost-efficient route which opens the path to new possibilities for the fabrication of MnAlC-based magnets. Acknowledgements IMDEA acknowledges financial support from EU M-ERA.NET and MINECO through the projects "NEXMAG" (Project Success Case at H2020 M-era.Net Programme, Ref. PCIN-2015-126) and "3D-MAGNETOH" (Ref. MAT2017-89960-R); Regional Government of Madrid through "NANOMAGCOST" project (Ref. P2018/NMT-4321); and Höganäs AB through the industrial collaboration "ECNanoManga".

**References:**

[1] J.M.D. Coey, IEEE Trans. Magn., 47, 4671 (2011) [2] V. Øygarden et al., J. Alloys Compd., 779, 776 (2019) [3] J. Rial et al., Acta Mater., 157, 42 (2018); Engineering, 6 (2), 173 (2020) [4] C. Muñoz-Rodríguez et al., J. Alloys Compd., 847, 156361 (2020)

**Images:**

![](https://assets.underline.io/uploads/markdown_image/1/image/ee90b2b1fd40d0e1617728e809b5f480.jpg)
Fig. 1. (a) X-ray diffraction pattern of the ε-phase gas-atomized loose powder and hot-pressed powder. (b) Room temperature hysteresis loops (second quadrant) of the loose annealed powder (ε transformed into τ-phase) and the magnet obtained by hot-pressing the ε-phase powder. Inset shows an image of the resulting compacted MnAlC magnet.

 MnAlC Permanent Magnets Obtained Directly from ε-Phase Gas-Atomized and Milled Powder by Hot-Pressing

Nowadays multi-material additive manufacturing (AM) is attracting much interest in many high technological sectors such as automotive, energy, electronics, aeronautics and medicine. The combination of AM technology with the synthesis of composite materials allows for designing and fabricating objects with complex shapes and tuned properties for reaching high performance [1]. For permanent magnet (PM) applications, a present challenge is developing magnets by AM with no geometrical constrictions, high filling factor (FF) to avoid diluting their magnetic properties, and no deterioration of their PM properties during processing [2]. The industrial fabrication of PM/polymer composites (typically in the shape of pellets) is done by mechanical methods. We showed recently, and for the very first time, the possibility of producing a continuous PM-based filament (meters long) using as a precursor a highly loaded PM/polymer composite synthesized by solution casting [3]. This technique allows for the synthesis of customized composites making possible the choice of the polymer according to the requirements dictated by the final application. Moreover, it is an easily scalable route, which opens a new path to the AM technology of PMs. In this study, different composites (PM particles/polymer) have been analyzed consisting on several PM materials: gas-atomized τ-MnAlC (Fig. 1(a)), Sr-ferrite, NdFeB, and hybrid (NdFeB/Sr-ferrite) powders embedded in different polymer matrix. It is of large scientific and technological interest to consider rare earth (RE)-free PM alternatives such as improved ferrites, and the promising MnAl-based alloys [4]. The starting powders showed different mean particle size ranging from the 5 μm of Sr-ferrite to the 50 μm of NdFeB powders. MnAlC powders showed an intermediate mean particle size between 15 and 30 μm. This work will show the effect of particle size (with special attention to the benefits of combining dissimilar sizes), polymer and fabrication parameters on the properties of the final products, showing that they are key factors to be considered and optimized for obtaining flexible and continuous filaments with a high FF. Particle size plays a key role when extruding the composites in order to obtain flexible filaments with a high FF [3,5,6]. It has been observed that if the mean particle size is larger than 20 μm (coarse particles), the extrusion process is affected by the composite rheology under the exerted pressures and, consequently, the FF of the extruded filament is reduced [5,6]. A key result from this study is the demonstration that, by mixing particles with different size and optimizing the fine-to-coarse particles ratio, it is possible to obtain flexible filaments with increased FF (up to 90%), i.e., leading to an enhanced effectiveness of the extrusion process [5,6]. MnAlC-based composites were synthesized by solution casting (Fig. 1(a)) making possible to tune the FF, reaching extremely high values above 85% [3]. Composites were extruded into continuous and flexible filaments with PM properties (Fig. 1(b)), with a length over 10 m [3,6]. The homogeneity of the composites and filaments has been determined by scanning electron microscopy, SEM (Fig. 1(b)). Processing of SEM images allowed for obtaining the FF of the composites and filaments. Vibrating sample magnetometry (VSM) has been used for accurately determining the FF of composites and filaments, being positioned as a faster technique in comparison with image processing. Moreover, and important in view of practical applications, this technique has demonstrated the no deterioration of PM properties of the starting particles after composite synthesis and filament extrusion processes (Fig. 1(b)) [3,5,6]. We will compare these results with those obtained in the preparation of filament prepared from composites based on: Sr-ferrite (Hc~3 kOe, FF=92%), NdFeB (Hc=10.2 kOe, FF=83%) and hybrid composites containing fine (Sr-ferrite) and coarse (NdFeB) particles (Hc=8 kOe, FF=90%). Optimized MnAlC-based filament (with a high MnAlC content above 80 wt.%) was used for 3D-printing objects as a proof-of-concept (Fig. 2). Magnetic measurements performed on the printed objects (Fig. 2) have proved that alternative PM materials can be efficiently synthesized and processed for developing novel PMs by AM under controlled processing temperature, which might be used in sensing devices [6]. Acknowledgements Authors acknowledge fruitful collaboration and discussions with B. Skårman, H. Vidarsson and P.-O. Larsson from Höganäs AB (Sweden), and A. Nieto and R. Altimira from IMA S.L.U. (Spain). Authors additionally acknowledge financial support from EU M-ERA.NET and MINECO through the projects "NEXMAG" (M-ERA.NET Project Success Case, Ref. PCIN-2015-126) and "3D-MAGNETOH" (Ref. MAT2017-89960-R); Regional Government of Madrid through "NANOMAGCOST" project (Ref. P2018/NMT-4321); and Höganäs AB through the industrial contract "GAMMA".

**References:**

[1] S.A.M. Tofail et al., Mater. Today, 21, 22 (2018) [2] C. Huber et al., Appl. Phys. Lett., 109, 162401 (2016) [3] E.M. Palmero et al., Sci. Technol. Adv. Mater., 19, 465 (2018) [4] A. Bollero et al., ACS Sustainable Chem. Eng., 5, 3243 (2017); J. Rial et al., Acta Mater., 157, 42 (2018); J. Rial et al. Engineering, 6 (2), 173; C. Muñoz-Rodríguez et al., J. Alloys Compd., 847, 156361 (2020) [5] E.M. Palmero et al., IEEE Trans. Magn., 55, 2101004 (2019) [6] E.M. Palmero et al., Addit. Manuf., 33, 101179 (2020)

**Images:**

![](https://assets.underline.io/uploads/markdown_image/1/image/07242cdfa3f27df187acf728ebcc1b22.jpg)
Fig. 1. (a) Composite synthesis by solution casting with representative images of the starting MnAlC powders and the resulting MnAlC/polymer composite. (b) Second quadrant of the hysteresis loops measured at room temperature for the gas-atomized MnAlC particles, MnAlC/polymer composite and extruded filament. Inset shows an extruded MnAlC-based filament together with an SEM image of its circular cross section.

![](https://assets.underline.io/uploads/markdown_image/1/image/313f4a31e639429f97217f5044912754.jpg)
Fig. 2. Magnetic pieces obtained by additive manufacturing using an extruded filament based on MnAlC particles, together with the magnetic flux density measured at the surface of a 3D-printed disc.

 Additive Manufacturing of Rare Earth-free and Hybrid Permanent Magnets: from Composites synthesized by Solution Casting to Magnetic Filament and 3D-printing of Magnets

MOA: Nanocomposite Magnetic Materials

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Presentations

Analysis of the Magnetic Interactions in FeNi Nanowire Arrays through FORC and Angular Coercivity Measurements

Scalable Synthesis of CoFe and NiFe Nanoparticles from Ferrite Precursors with Tailored Magneto-Thermal Properties by a Combined Co-precipitation, Milling and Reduction Process

Effect of Dopants (Mo, Cr, V) on the Magnetic Properties of Mn-Al-C nanostructured by Flash-Milling

A Sustainable Route for Permanent Magnets Fabrication: Additive Manufacturing Applied to Recycled Ferrite Residues

Optimizing the Particle Size Distribution in Permanent Magnet Composites to Extrude Flexible Filaments for Additive Manufacturing

MnAlC Permanent Magnets Obtained Directly from ε-Phase Gas-Atomized and Milled Powder by Hot-Pressing

Additive Manufacturing of Rare Earth-free and Hybrid Permanent Magnets: from Composites synthesized by Solution Casting to Magnetic Filament and 3D-printing of Magnets

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