Microstructure and magnetic properties studies of SmCo5 thin films grown on MgO and glass substrates

In this work, SmCo₅ thin films are deposited on single crystal MgO (1 0 0) and amorphous glass substrates with a Cr underlayer at 400 °C by sputtering. A comparison study shows that the microstructures and magnetic properties are different in the two SmCo₅ films on the MgO (1 0 0) and glass substrates, respectively. An epitaxial growth of Cr-(2 0 0)〈1 1 0〉/SmCo₅-(1 1 2¯ 0)〈0 0 0 1〉 is achieved on the MgO (1 0 0) single crystal substrate with an average grain size of 20 nm for SmCo₅. On the amorphous glass substrate, no significant crystallographic texture is found in the Cr underlayer. After the deposition of SmCo₅, a weak texture of (1 1 2¯ 0) is observed with an average grain size of 8 nm. High remanence ratio value in this film is probably due to strong exchange coupling. Both SmCo₅ films show high in-plane coercivity, high in-plane anisotropy and remanence enhancement.     

Ultra-fine grained Nd–Fe–B by high pressure reactive milling and desorption

This paper reports on the grain refinement in dynamic hydrogenation disproportionation desorption and recombination (d-HDDR) processed Nd-rich Nd₂Fe₁₄B and stoichiometric Nd₂Fe₁₄B powders using high pressure reactive milling (HPRM) followed by a subsequent desorption and recombination. In contrast to the dynamic-HDDR processed anisotropic powder with a grain size of the Nd₂Fe₁₄B phase of 300 nm, the new approach yields a further reduction of the Nd₂Fe₁₄B₁ grain size to less than 70 nm. Nd-rich Nd₂Fe₁₄B powder produced by HPRM and subsequent desorption exhibits a coercivity μ_0iH_c=1.35 T and a remanence of 0.80 T. In the stoichiometric material, the reduction of the Nd-content leads to an increase in remanence to 0.85 T. Additionally, it is demonstrated that highly anisotropic powders can also be obtained by dynamic-HDDR processing of stoichiometric Nd₂Fe₁₄B powders.     

Eddy-current-resistant SmCo5/CaF2 magnets produced via high-energy milling in polar and non-polar liquids

Processes of high-energy ball milling of SmCo₅ alloys were compared for three single-liquid environments without using additional surfactants. Both coarsely grained as-cast and nanocrystalline pre-milled SmCo₅ precursors showed tendency toward formation of thin flakes if milled in polar liquids (acetone and ethanol) in a marked contrast to milling in non-polar heptane. CaF₂ dielectric powder added prior to milling in the polar liquids tends to become attached on the flake surfaces. Milling in heptane in the presence of CaF₂ produces flake-like SmCo₅ particles which with increasing the milling time are found to incorporate an increasing amount of CaF₂. The SmCo₅—5 wt% CaF₂ mixtures milled for the optimum time in both the polar and non-polar liquids were successfully hot-pressed into laminated composite magnets having intrinsic coercivity of 25–30 kOe, maximum energy product of approximately 6.5 MG Oe and electrical resistivity of 500–600 μΩ cm, which is more than 7 times the resistivity of conventional Sm–Co magnets.     

Exchange-coupled nanoscale SmCo/NdFeB hybrid magnets

Nanoscale hybrid magnets containing SmCo₅ and Nd₂Fe₁₄B hard magnetic phases have been produced via a novel “in-one-pot” processing route. The grain size of the processed bulk composite materials is controlled below 20 nm. The refinement of the nanoscale morphology leads to effective inter-phase exchange coupling that results in single-phase like magnetic properties. Energy product of 14 MGOe was obtained in the isotropic nanocomposite magnets at room temperature. At elevated temperatures, the hybrid magnets have greatly improved thermal stability compared to the Nd₂Fe₁₄B single-phase counterpart and have substantially increased magnetization and energy products compared to the single-phase SmCo₅ counterpart.     

Effect of hot deformation on texture and magnetic properties of Sm-Co and Pr-Co alloys

Nanocrystalline PrCo₅, SmCo₅ and Sm₂(Co,Fe,Mn)₁₇ alloys were subjected to a high-degree plastic deformation at 950 °C with the height reduction ranging from 70% to 95%. With increasing degree of deformation, the PrCo₅ and SmCo₅ magnets showed improvement of the deformation-induced [0 0 1] texture. The PrCo₅ alloys, known to develop a superior texture at the lower degrees of deformation, showed only modest improvement and their magnetic performance was undermined by a low coercivity. The SmCo₅ alloys had their texture markedly enhanced and, after height reduction by 94.5%, they exhibited a remanence of 8.6 kG, maximum energy product of 18 MGOe and an intrinsic coercivity of 22.8 kOe. No induced texture was found in the alloys based on the Sm₂Co₁₇ structure. The microstructures of the hot-deformed alloys were studied with a transmission electron microscopy, and possible mechanisms of the texture development in the RCo₅ alloys (R=Pr, Sm) are briefly discussed.     

Magnetic properties of anisotropic Sm–Fe–N bulk magnets produced by spark plasma sintering method

Sm–Fe–N powders were consolidated into bulk materials by the spark plasma sintering (SPS) method. Although partial decomposition of the Sm₂Fe₁₇N₃ phase was noted in the magnets, the decomposition was reduced by the addition of a small amount of Zn powder to the Sm–Fe–N powder. The anisotropic Sm–Fe–N magnet obtained from a mixture of Sm–Fe–N and Zn powders exhibited a high remanence of 0.90 T with a coercivity of 0.54 MA m⁻¹.     

Effects of powder flowability on the alignment degree and magnetic properties for NdFeB sintermagnets

The magnetic powders for sintered NdFeB magnets have been prepared by using the strip casting (SC), hydrogen decrepitation (HD) and jet milling (JM) techniques. The effects of powder flowability and addition of a lubricant on the alignment degree and the hard magnetic properties of sintered magnets have been studied. The results show that the main factor affecting powder flowability is the aggregation of magnetic particles for powders in a loose state, but it is the friction between the powder particles for powders that are in a compact state. The addition of a lubricant with suitable dose can slightly prevent the congregating of powders, obviously decrease the friction between the powder particles, improve the powder flowability, and increase the alignment degree, remanence and energy product density of sintered magnets. Mixing a suitable dose of lubricant and adopting rubber isostatic pressing (RIP) with a pulse magnetic field, we have succeeded in producing the sintered NdFeB magnet with high hard magnetic properties of B_r=14.57 KG, _jH_c=14.43 KOe, (BH)_max=51.3 MGOe.     

Structural and magnetic studies on spark plasma sintered SmCo5/Fe bulk nanocomposite magnets

SmCo₅+x wt% Fe (x=0$x=0$, 5 and 10) nanocomposite powders were synthesized by mechanical milling and were consolidated into bulk shape by spark plasma sintering (SPS) technique. The evolution of structure and magnetic properties were systematically investigated in milled powders as well as in SPS samples. A maximum coercivity of 8.9 kOe was achieved in spark plasma sintered SmCo₅+5 wt% Fe sample. The exchange spring interaction between the hard and soft magnetic phases was evaluated using δM–H measurements and the analysis revealed that the SPS sample containing 5 wt% Fe had a stronger exchange coupling between the magnetic phases than that of the sample with10 wt% Fe.     

Improvement of magnetic properties and read/write characteristics in SmCo5 perpendicular thin films

An SmCo₅ alloy is a promising candidate for ultra-high density magnetic recording media because of its strong uniaxial magnetocrystalline anisotropy, whose constant, K_u, is more than 1.1×10⁸ erg/cm³. Recently, we successfully obtained high perpendicular magnetic anisotropy for a sputter-deposited SmCo₅ thin film by introducing a Cu/Ti dual underlayer. However, it is necessary to improve magnetic properties and read/write (R/W) characteristics for applying SmCo₅ thin films to perpendicular magnetic recording media. In this study, we focused on reduction of magnetic domain size and change of a magnetization reversal process of SmCo₅ perpendicular magnetic thin films by introducing carbon (C) atoms into the constituent Cu underlayer. The magnetic domain size became small and the ratio of coercivity (H_c) against magnetic anisotropy (H_k) which is an index of the magnetization reversal process was increased by adding C atoms. We also evaluated the R/W characteristics of SmCo₅ double-layered media including C atoms. The medium noise was decreased and signal-to-noise ratio increased by introducing the C. The addition of C into the Cu underlayer is effective for changing the magnetization reversal process, reducing medium noise and increasing SNR.     

Correlation between microstructure and first-order magnetization reversal in the SmCo5/α-Fe nanocomposite magnets

SmCo₅/α-Fe nanocomposite magnets with different morphology have been fabricated by ball milling of the micrometer sized SmCo₅ and α-Fe powders. The α-Fe grains vary from elongated nano-strips to spherical nanoparticles with increasing milling time. The inter-phase exchange coupling is enhanced with increasing milling time due to reduced grain size. The first-order reversal curves (FORCs) are taken to identify optimal conditions for exchange coupling. It has been found that the stripped morphology results in weak inter-phase exchange coupling, while enhanced exchange coupling is observed with further reduction of the soft-phase grain size. Compared with the measurement of demagnetization curves, FORC analysis provides more information on the magnetostatic as well as the exchange interactions.     

Preparation,microstructure, and magnetic properties of a nanocrystalline Nd12Fe82B6 alloy by HDDR combined with mechanical milling

Nanocrystalline Nd₁₂Fe₈₂B₆ (atomic ratio) alloy powders with Nd₂Fe₁₄B/α-Fe two-phase structure were prepared by HDDR combined with mechanical milling. The as-cast Nd₁₂Fe₈₂B₆ alloy was disproportionated via ball milling in hydrogen, and desorption–recombination was then performed. The phase and structural change due to both the milling in hydrogen and the subsequent desorption–recombination treatment was characterized by X-ray diffraction (XRD). The desorption–recombination behavior of the as-disproportionated alloy was investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The morphology and microstructure of the final alloy powders subject to desorption–recombination treatment were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The results showed that, by milling in hydrogen for 20 h, the matrix Nd₂Fe₁₄B phase of the alloy was fully disproportionated into a nano-structured mixture of Nd₂H₅, Fe₂B, and α-Fe phases with average size of about 8 nm, and that a subsequent desorption–recombination treatment at 760 °C for 30 min led to the formation of Nd₂Fe₁₄B/α-Fe two-phase nanocomposite powders with average crystallite size of 30 nm. The remanence B_r, coercivity H_c, and maximum energy product (BH)_max of such nanocrystalline Nd₁₂Fe₈₂B₆ alloy powders achieved 0.73 T, 610 kA/m, and 110.8 kJ/m³, respectively.     

Microstructures and coercivities of SmCox and Sm(Co,Cu)5 films prepared by magnetron sputtering

We have investigated the influence of composition and annealing conditions on the magnetic properties and microstructural features of SmCo_x films that were prepared by sputtering and subsequent annealing. A huge in-plane coercivity of 5.6 T was obtained from an optimally annealed Sm–Co film, which was attributed to the nanometer sized polycrystalline microstructure of the highly anisotropic SmCo₅ phase. Although a high density of planar defects were observed in the films that were annealed at high temperatures, they did not act as strong pinning sites for domain wall motion. The effect of Cu on [SmCo_4.5(9 nm)/Cu(xnm)]₁₀ multilayer thin films was also studied. An appropriate Cu content increased the coercivity.     

Improvement of magnetic intergranular isolation and evaluation of read/write characteristics on SmCo5 perpendicular magnetic thin films

SmCo₅ alloy is a promising candidate for ultra-high-density perpendicular magnetic recording (PMR) media because of its high uniaxial magnetocrystalline anisotropy K_u of more than 1.1×10⁸ erg/cm³. Previously, we successfully achieved high K_u in a sputter-deposited SmCo₅ thin film by introducing a Cu/Ti dual underlayer. However, in order to apply the SmCo₅ films to practical PMR media, it is necessary to decrease medium noise. A granulated magnetic film comprising of small and magnetically decoupled grains is effective in reducing the medium noise. In this paper, we have proposed a new granular film that is fabricated by partial thermodiffusion of Cu between the Sm-Co continuous layer and the Cu underlayer, which is granulated using compositional segregation caused by the addition of Ta₂O₅. We have analyzed the magnetic properties, magnetic domain size, and magnetization reversal process of the proposed SmCo₅ film. The magnetic domain size decreased and the magnetization reversal process changed from the magnetic-wall-motion mode to a coherent rotation mode to some extent on isolation of magnetic grains. The read/write characteristics of granulated SmCo₅ double-layered media were also evaluated. The medium noise decreased and the signal-to-noise ratio increased for the granulated double-layered (PMR) medium.     

Fabrication of High-performance Sm-Fe-N isotropic bulk magnets by a combination of High-pressure compaction and current sintering

TbCu₇-type Sm-Fe-N coarse powders in the flake form were consolidated without a bonding medium using a low-thermal-load process of current sintering combined with high-pressure compression. When compacted at 1.2 GPa, the relative density of the powder was increased by 80% with close stacking of the flake particles. Although the subsequent current heating was only briefly performed at a low temperature of 400 °C to avoid decomposition, the compact was consolidated into a rigid bulk in which the particles were bonded at the atomic level. Finally, by using cyclic compaction, this process produced bulk magnets with a density of 92% that exhibited the highest maximum energy product (BH)max of 16.2 MGOe, which surpasses that of conventional isotropic Sm-Fe-N bond magnets.     

A study on magnetic properties and structure of SmCo5 thin films on Ni-W underlayers

A systematic study on Ni-W alloy underlayers has shown that a highly textured (2 1 1)-Ni₄W can be formed after deposition at room temperature. Highly textured (0 0 0 1)-SmCo₅ with a high out-of-plane coercivity (over 10 kOe) and large perpendicular anisotropy can be obtained after deposition on the (2 2 1)-Ni₄W underlayer probably due to a small mismatch between (2 2 1)-Ni₄W and (0 0 0 1)-SmCo₅. Our study indicates that the surface roughness of the underlayers also plays a crucial role, that a smooth surface is favorable for a good crystallinity and high coercivity of SmCo₅. Moreover, we found that a highly textured Ni-(1 1 1) can be obtained on the top of the (2 1 1)-textured Ni₄W. The film structure of SmCo₅/Ni/Ni₄W may be interesting as the hard/soft double-layered film for perpendicular magnetic recording or for other applications after a further development.     

Synthesis, structural and magnetic properties of the nanocomposite Fe63B23Nd7Y3Nb3Cr1 magnets

The Fe₆₃B₂₃Nd₇Y₃Nb₃Cr₁ nanocomposite magnets in the form of sheets have been prepared by copper mold casting technique. The phase evolution, crystal structure, microstructural and magnetic properties have been investigated in the as-cast and annealed states. The as-cast sheets show magnetically soft behaviors which become magnetically hard by thermal annealing. The optimal annealed microstructure was composed of nanosize soft magnetic α-Fe (19-29 nm) and hard magnetic Nd₂Fe₁₄B (45-55 nm) grains. The best hard magnetic properties such as intrinsic coercivity, _jH_c of 1119 kA/m, remanence, B_r of 0.44 T, magnetic induction to saturation magnetization ratio, M_r/M_s=0.61 and maximum energy product, (BH)_max of 55 kJ/m³ was obtained after annealing at 680 °C for 15 min. The annealing treatment above 680 °C results in non-ideal phase grains growth, which degrade the magnetic properties.     

The magnetization reversal behaviour for SmCo6.8Zr0.2 and SmCo6.8Zr0.2/α-（Fe,Co） nanocrystalline magnets at low temperature

This paper reports that the SmCo 6.8 Zr 0.2 nanocrystalline permanent magnets and SmCo 6.8 Zr 0.2 /α-(Fe,Co) nanocomposite permanent magnets are successfully produced by mechanical alloying and subsequently annealing at 700 C for 10 minutes.The x-ray diffraction results show that the phase structure of SmCo 6.8 Zr 0.2 nanocrystalline permanent magnets is composed of SmCo 7 phase and SmCo 6.8 Zr 0.2 /α-(Fe,Co) nanocomposite permanent magnets is composed of SmCo 7 and α-(Fe,Co) phases.The mechanism of magnetization reversal is mainly controlled by inhomogeneous domain wall pinning in SmCo 6.8 Zr 0.2 and SmCo 6.8 Zr 0.2 /α-(Fe,Co) magnets.The inter-grain exchange interaction at low temperature is investigated,which shows that the inter-grain exchange interaction of SmCo 6.8 Zr 0.2 /α-(Fe,Co) magnets increases greatly by the decrease of the measured temperature.According to Δm irr-H/H cj,Δm rev-H/H cj and χ irr-H/H cj curves at room temperature and 100 K,the changes of irreversible and reversible magnetization behaviours of SmCo 6.8 Zr 0.2 and SmCo 6.8 Zr 0.2 /α-(Fe,Co) magnets with the decreasing temperature are analysed in detail.The magnetic viscosity and the activation volume of SmCo 6.8 Zr 0.2 and SmCo 6.8 Zr 0.2 /α-(Fe,Co) magnets at different temperatures are also studied.     

Deformation-induced texture in nanocrystalline 2:17, 1:5 and 2:7 Sm-Co magnets

The effect of crystal structures on texture induced by hot plastic deformation was studied for Sm-Co, Sm-Zr-Co, Sm-Zr-Co-Fe and Sm-Co-Fe-Mn nanocrystalline alloys with 9-22 at% Sm. Nanocrystalline precursors were obtained via high-energy ball milling and subsequent hot consolidation; deformation was carried out at 800-1150 °C. The analysis of X-ray diffraction and magnetic measurements showed that the degree of the axial [0 0 1] texture after deformation was negligible for the ordered 2:17 structure, but became increasingly noticeable for the disordered 2:17 (“1:7”), 1:5 and 2:7 structures. Because of interplay of several factors including the [0 0 1] texture, saturation magnetization and magnetocrystalline anisotropy, there was no universal trend in the hard magnetic properties with the Sm content. Optimum compositions for the maximum energy product varied from Sm₁₁(Co, Fe, Mn)₈₉ in the Sm-Co-Fe-Mn series to Sm₁₁Zr₂(Co, Fe)₈₇ in the Sm-Zr-Co-Fe series to Sm₁₇(Co, Fe)₈₃ in the Sm-Co-(Fe) series. Iron substitution for cobalt strongly suppresses the 1:5 structure, whereas the Fe-free magnets based on the SmCo₅ compound showed by far the highest room-temperature coercivity.     

Investigation on magnetic properties of orientated nanocomposite Pr2Fe14B/α-Fe permanent magnets by micromagnetic finite-element method

Demagnetization curves for nanocomposite Pr₂Fe₁₄B/α-Fe permanent magnets with different hard grain alignment are calculated by a micromagnetic finite-element method. The results show that both remanence and coercivity increase with improving hard grains alignment. The demagnetization curves show a single-phase demagnetization behavior for the samples with grain size d of 10 nm and two-phase behavior for the samples with d of 20 and 30 nm. H_ex (reflecting the magnetic hardening of α-Fe) and H_irr (expressing the irreversible reversal of hard phase) are both enhanced with improving the hard grain alignment. The magnetic reversal in orientated nanocomposite permanent magnets is mainly controlled by inhomogeneous pinning of the nucleated type.     

Anisotropic powder from sintered NdFeB magnets by the HDDR processing route

Sintered NdFeB-based scrap magnets were recovered and processed using the HD and HDDR routes. The effects of varying the HDDR processing temperature were investigated (over the range 835-930 °C). The disproportion was carried out with a pressure ramp to a maximum of 1000 mbar hydrogen pressure with a 1 h hold time at each step and the optimum recombination conditions were set at 100 mbar with a 20 min hold time. Anisotropic NdFeB powder was produced in all cases with the best magnetic properties achieved at a processing temperature of 880 °C, producing powder with a remanence of 1.10(±0.02) T and an intrinsic coercivity of 800 (±16) kA m⁻¹ and giving a (BH)_max of 129(±2.5) kJ m⁻³.