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Communication

Microwave-Assisted Combustion Synthesized Sm2Co17 Magnetic Particles for Permanent Magnetic Application

by
Yatao Wang
1,2,*,
Xiangyu Ma
3,
Yani Lu
1,
Hui Wen
1,
Guozhe Guo
1,
Yingying Li
1,
Pengming Zhang
1,
Yan Wang
1 and
Zhi Yang
2,*
1
Gansu Key Laboratory of Efficient Utilization of Oil and Gas Resources, College of Petroleum and Chemical Engineering, Longdong University, Qingyang 745000, China
2
Faculty of Materials and Manufacturing, Key Laboratory of Advanced Functional Materials, Ministry of Education of China, Beijing University of Technology, Beijing 100124, China
3
Shanxi Aerospace Qinghua Equipment Co., Ltd., Changzhi 046000, China
*
Authors to whom correspondence should be addressed.
Magnetochemistry 2024, 10(9), 63; https://doi.org/10.3390/magnetochemistry10090063
Submission received: 11 May 2024 / Revised: 5 July 2024 / Accepted: 10 July 2024 / Published: 29 August 2024
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Abstract

:
We reported the new synthesis of Sm2Co17 particles by a microwave-assisted combustion (MACS) method. This process enables the controlled decomposition of Sm(NO3)3 and Co(NO3)2 into SmCo-O particles, followed by calcium reduction-diffusion. This SmCo-O particle provides an approach for achieving high magnetic properties in Sm2Co17 magnetic materials. The rhombohedral Sm2Co17 particles can be incorporated into epoxy resin and oriented, displaying a square-like hysteresis loop. The particles display magnetic properties at room temperature, with a saturation magnetization of 112.3 emu/g, coercivity of 5.6 kOe, and a maximum energy product of 9.4 MGOe. This method improves the synthesis efficiency of rare earth cobalt-based nano-materials, expands the synthesis scope, and provides ideas for the synthesis and applications of other rare earth nano-materials.

1. Introduction

SmCo-based compound is one of the widely used hard magnetic materials due to their exceptionally large magnetocrystalline anisotropy (Ku = 2 × 108 erg/cm3) and high Curie temperatures (Tc = 1020 K) [1,2,3]. The magnetic properties of the alloys can be boosted through precise control of their microstructure on the nanometer level and by synergizing the nanomagnets with soft iron-based phase [4,5,6,7,8,9]. The current studies show that the nanostructured Sm-Co can be synthesized by combining solvo-thermochemistry synthesis with high temperature reduction process [10,11,12].
Abundant research have been worked on the synthesis of SmxCoy nanoparticles with expected magnetic properties adopting chemical method [13,14,15,16,17,18,19,20]. In general, the solvo-thermochemistry mainly includes the following steps. Precursors need to be obtained through the related reaction between salts and bases [21,22,23,24]. After that SmCo-O/CaO core shell nanoparticles were prepared by employing reactants such as Ca(NO3)2, Ca(OH)2 and Ca(Ac)2. However, most available synthesis of SmCoO are very time-consuming and need to be proceeded under very strict conditions. MACS is an economical method compared with various method for preparing metal oxide materials. MACS has many outstanding advantages, such as time saving, low cost and high energy efficiency [25]. When igniting the reaction by microwave radiation, it is necessary to evaporate water, concentrate the reactants, form paste, foam and burn. The reactants will be transformed into black loose particles. The whole reaction can be completed in just a few minutes. CeO2 [26], Y2O3 [27], ZnO [25,28], Nd-Fe-B oxides [29,30] have been successfully synthesized through the MACS method. As we all know, microwave has been widely used as a means of heating materials. It is generally believed that the microwave is one of the most commonly used methods for heating materials. In the MACS process, energy transfer and exchange are embodied at the molecular level [30,31].
The SmCo nanoparticles were obtained by the reduction in the SmCo-O/CaO core–shell particles at a high temperature. The CaO coating helps to inhibit the agglomeration and enlargement of product particles. Particles with different phases and sizes can be synthesized by modifying the initial proportion and types of two metal precursors [24,32,33,34]. Ma [32] reported a method utilizing flame reaction for the amplification synthesis of precursor particles, which resulted in the production of Sm2Co17 particles with Hc of 15.6 kOe, Ms of 103.7 emu/g. Even with advancements in synthesis, achieving desired sizes, compositions, and magnetism controls remains challenging when scaling up the chemical synthesis of REM particles.
Firstly, we synthesized samarium cobalt oxide by the MACS method, which is efficient and environmentally friendly, and the two alloy elements of the precursor are evenly distributed. Then, using calcium nitrate as raw material, SmCo-O particles were coated with a protective layer of calcium oxide, and finally, Sm2Co17 particles were obtained by reduction with Ca at high temperature. The coercivity of the obtained Sm2Co17 magnetic powder after orientation is 5.6 kOe, the saturation magnetization is 112.3 emu/g, and the maximum magnetic energy product is 9.4 MGOe.

2. Experimental

Figure 1 depicts a diagram of the synthesis process of Sm2Co17 nanoparticles. Firstly, the nitrate of samarium and cobalt is transformed into oxide powder under the action of microwave radiation. Secondly, the precursor is coated with a calcium oxide protective layer of calcium nitrate. Then, Sm2Co17 nanoparticles were obtained by high-temperature reduction diffusion technology. Finally, impurities are removed by washing with water. The specific processes for each step areas follows.

2.1. Synthesis of SmCo-O

The MACS method includes taking Sm(NO3)2·6H2O and Co(NO3)2·6H2O as the main reactants, and dissolving urea as a combustion promoter in distilled water. The resulting pasty precursor was heated in a microwave oven (Galanz P70D20N1P-G5(WO)). The detailed experimental procedure is as follows: 3.0 g of Sm(NO3)2·6H2O, 14.142 g of Co(NO3)2·6H2O and 5.353 g of urea were dissolved in 3 mL of deionized water in a porcelain crucible. The paste mixture is placed in the center of a microwave oven, and a microwave field of 700 W is applied to it to decompose. After turning on the microwave, a series of rapid reactions occur. Combustion was completed within just 2–3 min, leaving behind black, loose SmCo-O nanoparticles as residues. The black powder was dispersed in 500 mL of absolute ethanol and then agitated for 70 min to achieve a homogeneous dispersion solution. Then, transfer it into centrifuge tubes and spin at 3000 rpm for 3 min to eliminate any small irregular particles. The powder was dried at room temperature, and about 6.8 g of SmCo-O particles were obtained.

2.2. Synthesis of SmCo-O/CaO

11.5 g Ca(NO3)2·4H2O is weighed and dissolved in 500 mL of absolute ethanol. Then, the SmCo-O particles were dispersed in the ethanol solution of Ca(NO3)2, and treated with ultrasound for 60 min until a uniform black solution was obtained. The above solution was heated on a heating table with strong magnetic stirring, and the temperature was kept at 343 K until the organic solvent had entirely disappeared. The black particles are shifted to a crucible, which is heated in the air. Initially, the temperature was raised to 730 K at the rate of 1 K min−1 and held for 1 h, so that Ca(NO3)2·4H2O was fully melted and wrapped around SmCo-O particles. Then, the temperature was raised to 780 K at the rate of 1 K min−1 and held for 1 h in order for Ca(NO3)2·4H2O to fully decompose into CaO. Cooling to room temperature with the furnace to obtain black SmCo-O/CaO particles.

2.3. Synthesis of Sm2Co17

The fabricated SmCo-O/CaO particles were mixed with 3.5 g KCl and 6.5 g Ca. The mixture was moved into an iron crucible with a cover. The iron crucible was subsequently transferred to a tube furnace. Then, the tube is degassed in order to ensure a vacuum state. Next, the tube furnace was filled with Ar/H2 and heated to 900 °C at a rate of 8 K min−1. The system was maintained for 1.5 h and subsequently cooled down to 25 °C. After removing nonmagnetic substances, Sm2Co17 powder was acquired through centrifugation at a speed of 8000 rpm for 5 min.

2.4. Characterization

X-ray diffraction (XRD, Japan, Rigaku Ultima IV) was employed to investigate the structure of both the oxide and alloy particles. The samples were analyzed for their microstructure and morphology using scanning electron microscopy (SEM, America, FEI, ZEISS-SUPRA55) and transmission electron microscopy (TEM, America, FEI, Tecnai-F20). Sm2Co17 particles with a certain mass were dispersed in epoxy resin and then placed in a cylindrical container together. After that, the container was placed in a static magnetic field of about 2.2 T supplied by a permanent magnet for 4 h. Sm2Co17 particles are arranged in such a way that their longitudinal direction is parallel to the direction of the external magnetic field. After the epoxy resin is fully cured, the cylindrical sample is taken out of the magnetic field. Cuboid samples cut from solidified cylinders were used for PPMS measurement. Magnetic measurements were performed at room temperature (298.15K) with a maximum applied magnetic field of 70 kOe using the vibrating sample magnetometer (VSM) option of a physical property measurement system (PPMS, America, Quantum Design).

3. Results and Discussion

The resulting products were SmCoO3, Co3O4. The gas generated after the combustion reaction is a mixture of N2, CO2, and H2O. The combustion reactions can be expressed as follows [31]:
xSm(NO3)3 + yCo(NO3)2 + zCO(NH2)2 + (9z − 22x − 14y)/3O2→
xSmCo + (y − x)/3Co3O4 + (1.5x + y + z)N2 + zCO2 + 2zH2O
In this case, the molar ratio of Sm/Co is y/x = 7.2, and the necessary amount of urea was calculated based on principles from propellant chemistry [31]. The equation ‘(9z − 22x − 14y)/3 = 0’ indicating that all reactants can provide enough oxygen without the need for external provision. Therefore, the amount of fuel required for the whole reaction can be calculated by Equation (1).
Indeed, the development of SmCo-O nanoparticles comprises two key stages: nucleation and growth. More precisely, urea is essential in controlling the formation and expansion of SmCo-O crystals by modifying the alkaline nature of the initial solution. The hydroxide ions produced by the hydrolysis of urea play a vital role in the nucleation process. In reaction, SmCo-O nucleates from Samarium cobalt basic ion solutions to form polynuclear aggregates. As a result, materials heat in the microwave field faster than in a conventional approach. When the boiling solution is ignited by microwave radiation, polycrystalline SmCo-O nanostructures are produced more rapidly during the combustion process. The reactants will be converted into loose nanocrystalline particles. The whole reaction can be completed in just a few minutes. When the boiling solution is burned by flame, polycrystalline SmCo-O nanostructures are formed at a faster rate in the combustion process [27,30]. The appearance of flaky SmCo-O can be attributed to the release of a large number of gases during the reaction. The XRD pattern of the particles (Figure 2) shows that they mainly consist of SmCoO3 and Co3O4 phases.
The SmCo-O particles were additionally analyzed by the SEM. The SEM image of the SmCo-O particles with loose pore structure is displayed in Figure 3a. The loose structure of oxide powder is due to the release of a large number of gases in combustion reactions. The elemental composition of precursor oxides was analyzed by energy dispersive spectroscopy (EDS) in SEM. Obviously, the Sm, Co, and O (Figure 3b–d) elements exhibit homogenous distribution. The generated gas would head off the growth and reunite of the particles, so loose precursor oxides can be gained [33].
SmCo-O/CaO particles can be prepared by mixing SmCo-O nanoparticles prepared from the above samples with an ethanol solution of calcium nitrate and heat treatment, as shown in Figure 4a. There is an obvious characteristic peak of CaO, which indicates the decomposition of calcium nitrate. Meanwhile, the SmCo-O phase still exists. This method can successfully obtain a stable CaO phase without affecting the crystallinity or phase composition of the oxide. Figure 4b–f shows the SEM image and EDS elemental mapping of SmCo-O/CaO particles. EDS elemental mapping in Figure 4c–f shows that the structure of the SmCo-O particle is well maintained after coating treatment, and the amorphous CaO layer is well-proportioned and coated outside the SmCo-O particle. This specially designed nanostructure helps to obtain ideal particles [32].
The oxide precursor coated with CaO was reduced by Ca at 1173 K and kept for 90 min. Due to the burning loss of samarium in the process of high temperature reduction and diffusion, the ratio of samarium to cobalt in the product is no longer 1:7.2. In order to accurately characterize the structure and properties of the annealed sample, all impurities were removed by washing with deionized water. The Sm2Co17 particles, as shown in Figure 5a, exhibit a Th2Zn17-type rhombohedral structure, which matches the standard card (JCPDSNo. 19-0359). Figure 5b displays the SEM image of the as-prepared Sm2Co17 particles. It is obvious that the obtained particles have good dispersibility and a uniform size distribution. On the basis of the statistical results in Figure 5c, the average particle size is mainly distributed in the range of 400–600 nm. Inevitably, a portion of the nanoparticles aggregated and grew in the process of high-temperature thermal reduction. However, the adhesive strength between particles is not strong, and they are easily dispersed in the ultrasonic process of n-hexane. Figure 5d–i, respectively, show the elemental mapping, HADDF-STEM image, and the corresponding HRTEM lattice image of a single Sm2Co17 nanoparticle after ultrasonic dispersion. The nanoparticles have a diameter of approximately 400 nm, as shown in the HADDF-STEM image in Figure 5f, and elemental mapping in Figure 5g, h shows that two metallic elements are dispersed evenly across each Sm2Co17 particle. The HRTEM image (Figure 5i) further reveals the interplanar distance in the rhombohedral Sm2Co17 of 0.293 nm, corresponding to the (113) plane in Sm2Co17 [35,36,37].
The magnetic properties of Sm2Co17 particles were tested by a physical property measuring system (PPMS) under a magnetic field of 70 kOe. As shown in Figure 6a, the coercivity of the synthesized Sm2Co17 particles was determined to be 5.1 kOe. After orientation, the coercivity of Sm2Co17 particles is 5.6 kOe. Figure 6b is an enlarged scale of the coercive force value in Figure 6a. The room temperature saturation magnetization characteristics of Sm2Co17 particles are 112.3 emu/g, and the Mr at 80.5 emu/g (Mr/M70kOe = 0.72). As shown in Figure 6c, the oriented Sm2Co17 particles show the maximum magnetic energy product (BH) of 9.4 MGOe.

4. Conclusions

In conclusion, Sm2Co17 rhombohedral particles were synthesized by MACS combined with thermal reduction of Ca. MACS is very remarkable in preparing high-quality and uniform samarium cobalt oxide nanoparticles. The key feature of the MACS method is that it converts nitrates of samarium and cobalt into corresponding oxide particles with a gram level in a few minutes. Ca(NO3)2·4H2O was fully melted and wrapped around SmCo-O particles to obtain SmCo-O/CaO particles. The particles were reduced and diffused at high temperatures to form Sm2Co17. The rhombohedral structure of Sm2Co17 particles can be incorporated into epoxy resin and aligned in the presence of an external magnetic field, displaying a square-shaped hysteresis loop with Hc of 5.6 kOe and (BH)max of 9.4 MGOe. This approach expands the synthesis of SmCo-based materials and can be further utilized in microwave communication, aerospace, military, and other application fields because of its high Curie temperature, excellent temperature stability, and corrosion resistance.

Author Contributions

Conceptualization, Y.W. (Yatao Wang) and Z.Y.; methodology, Y.W. (Yatao Wang) and X.M.; software, Y.L. (Yani Lu) and G.G.; validation, Y.W. (Yatao Wang); formal analysis, H.W. and Y.L. (Yani Lu); investigation, Y.L. (Yingying Li) and P.Z.; resources, Y.W. (Yatao Wang) and Z.Y.; data curation, Z.Y.; writing—original draft preparation, Y.W. (Yatao Wang); writing—review and editing, Y.W. (Yatao Wang), H.W. and Z.Y.; visualization, Z.Y.; supervision, Z.Y.; project administration, Y.W. (Yatao Wang); funding acquisition, Y.W. (Yatao Wang), H.W., Y.L. (Yingying Li), G.G. and Y.W. (Yan Wang) All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by [Doctor Funding Project of Longdong University] grant number [XYBYZK2408], [Department of Education of Gansu Province: Youth Doctoral Support Project] grant number [2024QB-116], [Natural Science Foundation of Gansu Province] grant number [23JRRM0754], [Doctor Funding Project of Longdong University] grant number [XYBYZK2224], [Youth Doctoral Project of Gansu province] grant number [2023QB-016], [the Planned Program of Science and Technology in Qingyang] grant number [QY-STK-2022B-148]. And the APC was funded by [Doctor Funding Project of Longdong University] grant number [XYBYZK2408].

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data used to support the findings of this study are included within the article.

Conflicts of Interest

Xiangyu Ma has been involved as a consultant and expert witness in Shanxi Aerospace Qinghua Equipment Co., Ltd. The paper reflects the views of the scientists and not the company.

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Magnetochemistry 10 00063 g001
Figure 1. Schematic illustration of the synthesis of SmCo.
Figure 1. Schematic illustration of the synthesis of SmCo.
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Figure 2. XRD pattern of as-prepared SmCo-O particles.
Figure 2. XRD pattern of as-prepared SmCo-O particles.
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Figure 3. (a) SEM image and elemental mapping of (b) Sm, (c) Co, and (d) O correspond to the SEM image shown in (a).
Figure 3. (a) SEM image and elemental mapping of (b) Sm, (c) Co, and (d) O correspond to the SEM image shown in (a).
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Figure 4. Characterization of SmCo-O/CaO particles. (a) XRD pattern of the particles. (b) SEM image of the particles. Elemental mapping of Sm (c), Co (d) and O (e) and Ca (f) of SmCo-O/CaO particles.
Figure 4. Characterization of SmCo-O/CaO particles. (a) XRD pattern of the particles. (b) SEM image of the particles. Elemental mapping of Sm (c), Co (d) and O (e) and Ca (f) of SmCo-O/CaO particles.
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Figure 5. Characterization of Sm2Co17 particles. (a) XRD pattern of the Sm2Co17 particles. (b) SEM image of the Sm2Co17 particles. (c) The particle size distributions of as-prepared Sm2Co17 particles. (d) Sm, (e) Co, and correspond to the SEM image shown in (b). (f) HADDF-STEM image and elemental mapping of Sm (g), Co (h) of Sm2Co17 particles. (i) HRTEM of a part of a Sm2Co17 particle.
Figure 5. Characterization of Sm2Co17 particles. (a) XRD pattern of the Sm2Co17 particles. (b) SEM image of the Sm2Co17 particles. (c) The particle size distributions of as-prepared Sm2Co17 particles. (d) Sm, (e) Co, and correspond to the SEM image shown in (b). (f) HADDF-STEM image and elemental mapping of Sm (g), Co (h) of Sm2Co17 particles. (i) HRTEM of a part of a Sm2Co17 particle.
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Figure 6. (a) Magnetic hysteresis loop of composed and aligned Sm2Co17 particles. (b) Enlarged view of magnetic hysteresis loop. (c) BH curve of the aligned Sm2Co17 particles.
Figure 6. (a) Magnetic hysteresis loop of composed and aligned Sm2Co17 particles. (b) Enlarged view of magnetic hysteresis loop. (c) BH curve of the aligned Sm2Co17 particles.
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Wang, Y.; Ma, X.; Lu, Y.; Wen, H.; Guo, G.; Li, Y.; Zhang, P.; Wang, Y.; Yang, Z. Microwave-Assisted Combustion Synthesized Sm2Co17 Magnetic Particles for Permanent Magnetic Application. Magnetochemistry 2024, 10, 63. https://doi.org/10.3390/magnetochemistry10090063

AMA Style

Wang Y, Ma X, Lu Y, Wen H, Guo G, Li Y, Zhang P, Wang Y, Yang Z. Microwave-Assisted Combustion Synthesized Sm2Co17 Magnetic Particles for Permanent Magnetic Application. Magnetochemistry. 2024; 10(9):63. https://doi.org/10.3390/magnetochemistry10090063

Chicago/Turabian Style

Wang, Yatao, Xiangyu Ma, Yani Lu, Hui Wen, Guozhe Guo, Yingying Li, Pengming Zhang, Yan Wang, and Zhi Yang. 2024. "Microwave-Assisted Combustion Synthesized Sm2Co17 Magnetic Particles for Permanent Magnetic Application" Magnetochemistry 10, no. 9: 63. https://doi.org/10.3390/magnetochemistry10090063

APA Style

Wang, Y., Ma, X., Lu, Y., Wen, H., Guo, G., Li, Y., Zhang, P., Wang, Y., & Yang, Z. (2024). Microwave-Assisted Combustion Synthesized Sm2Co17 Magnetic Particles for Permanent Magnetic Application. Magnetochemistry, 10(9), 63. https://doi.org/10.3390/magnetochemistry10090063

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