Effect of Zn Addition on the Reduction of the Ordering Temperature of FePt Nanoparticles

Monodisperse FePt nanoparticles with an average size of 4.11 nm were successfully synthesized via chemical co-reduction of iron acetylacetonate, Fe(acac)₃, and platinum acetylacetonate, Pt(acac)₂, by 1,2hexadecanediol as a reducing agent. Also (FePt)₈₇Zn₁₃ nanoparticles with average size of 4.24 nm were synthesized using the same method. The structural and magnetic properties of the prepared samples were respectively studied by XRD, TEM and VSM. L1₀ FePt ordered phase is formed at lower annealing temperature by addition of Zn. The (FePt)₈₇Zn₁₃ nanoparticles starts ordering after annealing at 400 °C, whereas FePt nanoparticles at 400 °C are still disordered alloys with superparamagnetic behavior. Additive Zn is very effective in decreasing the ordering temperature and enhancing the chemical ordering in (FePt)₈₇Zn₁₃ particles, So that coercivity 5200 Oe was measured for (FePt)₈₇Zn₁₃ nanoparticles annealed at 500 °C, compared with 1800 Oe for samples without Zn. This reduction in ordering temperature significantly reduces FePt particle coalescence and loss in positional order.     

表面活性剂对FePt纳米颗粒形貌的影响

分别以乙酰丙酮铁(Fe(acac)3)和氯铂酸(H2PtCl6.6H2O)作为Fe源和Pt源,乙二醇作为还原剂和溶剂,通过多元醇还原法制备出单分散的FePt纳米颗粒,并研究了表面活性剂油酸油胺和CTAB对FePt纳米颗粒形貌和磁性能的影响。通过X射线衍射仪(XRD)、透射电子显微镜(TEM)和振动样品磁强计(VSM)对纳米颗粒进行表征。结果表明,表面活性剂油酸油胺和CTAB修饰的FePt纳米颗粒均为面心立方(FCC)结构,分散性良好,粒径分布较未使用表面活性剂时变窄;油酸油胺修饰的FePt形貌主要是球形,但是有四方形纳米结构出现;而CTAB修饰的FePt形貌有蠕虫状产生。VSM结果显示其矫顽力都趋近于零,呈现超顺磁性。     

Reduction of ordering temperature of self-assembled FePt nanoparticles by addition of Au and Ag

The [FePt]94Au6 and [FePt]90Ag10 nanoparticle arrays were synthesized on Si substrates by a reverse micellar method, combined with plasma treatment and in-situ deposition of a SiO2 overlayer, and the post annealing step was performed to drive the face-centered cubic to tetragonal phase transition. These FePt nanoparticles exhibit a quasi-hexagonal order with tailored inter-particle spacing and particle size. The effects of the Ag and Au on the structural and magnetic properties of FePt were investigated. The results indicate that both Au and Ag additives can remarkably enhance the coercivity and reduce the ordering temperature, however, the optimum composition is different for them. The optimum composition is determined to be [FePt]94Au6 and [FePt]90Ag10, respectively, for which the ordering temperature of FePt nanoparticles is reduced by -100 degrees C. After 600 degrees C annealing, the [FePt]94Au6 and [FePt]90Ag10 nanoparticles are totally ferromagnetic with apparent larger coercivities of -7.0 kOe, which is about 3.8 kOe larger than that of the pure FePt nanoparticles. The mechanism of the chemical ordering acceleration may be attributed to the defects and strains caused by the Au/Ag additives.     

Evolution of texture and atomic order in annealed sinter-free FePt nanoparticles

Monodisperse FePt nanoparticles have been synthesized chemically. The spherically shaped as-made nanoparticles were 6.0?nm in size and they were single crystals. The average composition of these particles is determined as Fe(50)Pt(50). The nanoparticles did not show any sign of sintering after annealing at 800?°C for up to 120?min. The texture and order parameters of as-made and annealed FePt nanoparticles were determined from azimuthally integrated selected area electron diffraction patterns. The close to perfect [Formula: see text] axial texture in as-made particles degraded with increasing annealing time, in contrast to the order parameter, which showed a monotonic dependence on annealing time. With 60?min annealing, a 0.8 degree of chemical?ordering has been achieved and the particles were sinter-free as observed from bright field images.     

Effect of Oleic Acid and Oleylamine Surfactants on the Size of FePt Nanoparticles

FePt magnetic nanoparticles have been synthesized by superhydride reduction of FeCl₂ and Pt(acac)₂ at high temperature. Adding superhydride (LiBEt3H) to the phenyl ether solution of FeCl₂ and Pt(acac)₂ in the presence of oleic acid, oleylamine, and 1,2-hexadecanediol at 190?^°C, followed by refluxing at 245?^°C, led to monodisperse 3.5?nm FePt nanoparticles. The effect of oleylamine and oleic acid surfactants on the nucleation and growth of FePt nanoparticles were studied. The size of Pt was controlled by oleylamine surfactant in nucleation stage. To prevent sintering of the FePt nanoparticles, oleic acid surfactant was used in growth stage. The energy dispersive spectroscopy results revealed that the particle composition was first Fe₁₁Pt₈₉ in nucleation stage and after adding superhydride the composition changed to Fe₆₃Pt₃₇ in growth stage. The structural and magnetic measurements indicated that the L1₀ structure of FePt nanoparticles is formed after annealing and the coercivity of superlattice FePt nanoparticles increases to 7.5?kOe after heat treatments.     

Effects of Magnetic Annealing on Structure and Magnetic Properties of L10-FePt/Ag Films

The structural and magnetic properties of L1₀-FePt/Ag films were studied by X-ray diffraction and a vibrating sample magnetometer. The FeAg/Pt films were obtained by depositing FeAg thin films on thermally oxidized Si (001) substrates via magnetron sputtering and Pt layers on their surface after annealing FeAg thin films at 400 °C with and without an out-of-plane magnetic field of 10 kOe. These films were further annealed at various temperatures to obtain L1₀-FePt phase. The results indicated that the pre-annealing of FeAg thin films under 10 kOe magnetic field caused (001) orientation of Fe particles, and the deposition of Pt layer on such orientated underlayers reduced the ordering temperature of FePt in FeAg/Pt films, realizing the L1₀-FePt phase at 400 °C. The higher coercivity and ordering degree were also observed in the samples, compared with those pre-annealed without magnetic field at the same annealing condition.     

Effect of carbon additive on microstructure evolution and magnetic properties of epitaxial FePt (001) thin films

FePt:C thin films were deposited on CrRu underlayers by DC magnetron co-sputtering. The effects of C content, FePt:C film thickness and substrate temperature on the microstructural and magnetic properties of the epitaxial FePt (001) films were studied. Experimental results showed that even with 30 vol.% C doping, the FePt films could keep a (001) preferred orientation at 350 °C. When a FePt:C film was very thin (< 5 nm), the film had a continuous microstructure instead of a granual structure with C diffused onto the film surface. With further increased film thickness, the film started to nucleate and formed a column microstructure over continuous FePt films. A strong exchange coupling in the FePt:C films was believed to be due to the presence of a thin continuous FePt layer attributed to the carbon diffusion during the initial stage of the FePt:C film growth. Despite the presence of a strong exchange coupling in the FePt:C (20 vol.% C) film, the SNR ratio of the FePt:C media was about 10 dB better than that of the pure FePt media. The epitaxial growth of the FePt:C films on the Pt layers was observed from high resolution TEM cross sectional images even for the films grown at about 200 °C. The TEM images did not show an obvious change in the morphology of the FePt:C films deposited at different temperatures (from 200 °C to 350 °C), though the ordering degree and coercivity of the films increased with increased substrate temperature.     

一步法制备L10相FePt纳米颗粒

以乙酰丙酮铁(Fe(acac)3)和氯铂酸(H2PtCl6.6H2O)分别作Fe源和Pt源,三缩四乙二醇(TEG)作溶剂和还原剂,聚乙烯基吡咯烷酮(PVP)作表面活性剂,通过多元醇还原法制备出单分散的FePt纳米颗粒。通过X射线衍射仪(XRD)及透射电子显微镜(TEM)分析表明,所制备的FePt纳米颗粒形状近似球形,分散性较好,平均颗粒粒径约为5.5nm。通过振动样品磁强计(VSM)分析显示所制备FePt纳米颗粒矫顽力为37.64kA/m,这意味着FePt纳米颗粒部分转变为面心四方相(L10相)。     

Structure and properties of nanoporous FePt fabricated by dealloying a melt-spun Fe_(60)Pt_(20)B_(20) alloy and subsequent annealing

A nanoporous FePt alloy has been fabricated by dealloying a melt-spun Fe(60)Pt(20)B(20)alloy composed of nanoscale amorphous and face-centered-cubic FePt(fcc-FePt)phases in H2 SO4 aqueous solution.The nanoporous alloy consists of single fcc-FePt phase with an Fe/Pt atomic ratio of about 55.3/44.7,and possesses a uniform interpenetrating ligament-channel structure with average ligament and pore sizes of 27 nm and 12 nm,respectively.The nanoporous fcc-FePt alloy shows soft magnetic characteristics with a saturation magnetization of 37.9 emu/g and better electrocatalytic activity for methanol oxidation than commercial Pt/C in acidic environment.The phase transformation from disordered fcc-Fe Pt into ordered face-centered-tetragonal FePt(L10-FePt)in the nanoporous alloy has been realized after annealing at823-943 K for 600 s.The volume fraction of the L10-FePt phase in the alloy increases with the rise of annealing temperature,which results in the enhancements of coercivity and saturation magnetization from 0.14 kOe and 38.5 emu/g to 8.42 kOe and 51.4 emu/g,respectively.The ligament size of the samples is increased after annealing.     

Chemically synthesized L1/sub 0/-type FePt nanoparticles and nanoparticle arrays via template-assisted self-assembly

Chemically ordered L1/sub 0/-type FePt nanoparticle agglomerates were synthesized directly by the co-reduction of Fe(III) and Pt(II) acetylacetonates in tetraethylene glycol at 300/spl deg/C in the absence of surfactants. These nanoparticles could be dispersed in n-hexane by coating with oleic acid and oleylamine. However, the dispersed particles exhibited only chemically disordered fcc phase and superparamagnetic behavior. The FePt nanoparticle film composed of dispersed particles and stabilized using amino-silane began to structurally transform to ordered L1/sub 0/ phase at 600/spl deg/C, which is lower compared to that prepared by the hot soap method. Rotational hysteresis loss measurement suggested that the ordering was incomplete at 600/spl deg/C and the nanoparticle film had the distribution of magnetocrystalline anisotropy field values. The FePt nanoparticle array was fabricated using the template-assisted self-assembly technique. To produce periodic dots on a substrate, positive-biased pulse voltage was applied to the substrate coated with octadecyltrichlorosilane monolayer by using a conducting cantilever used in a scanning probe microscope. This process induced electrochemical modification of -CH/sub 3/ groups into polar ones. The resulting template had well-aligned sub-100-nm dot arrays with sub-100-nm periodicity. The FePt nanoparticles were fixed on the patterned areas selectively.     

Nanogranular L1(0) FePt-C-Ta2O5 composite media for perpendicular recording applications

In this report, the effect of simultaneously adding two dopants (C and Ta2O5) in FePt was investigated. (Fe55Pt45)79C21-(x vol%) Ta2O5 films (where x = 0% to 20%) were prepared using both low and high power magnetron sputtering on MgO (2 nm)/CrRu (30 nm) underlayers with in-situ heating at 350 degrees C. Films deposited at low power showed a decrease in exchange coupling with increasing Ta2O5 content. Out-of-plane coercivity of 7.2 kOe was observed even with up to 20 vol% Ta2O5. X-Ray diffraction spectra showed presence of FePt(001) texture for all compositions of Ta2O5 ranging from 0 to 20 vol% suggesting that the perpendicular anisotropy was maintained even with up to 20 vol% of dopant content. Films deposited at high power showed a different behavior with an initial increase in out-of-plane coercivity to 8.2 kOe and a reduction in exchange coupling with loop slope parameter (alpha) approaching a fully decoupled value of 1. Further increase in doping content led to deterioration in the out-of-plane coercivity, as well as an increase in the exchange coupling.     

Controlled synthetic conditions of FePt nanoparticles with high magnetization for biomedical applications

Monodispersed FePt nanoparticles with hydrophobic ligand were chemically synthesized and with controllable surface-functional properties. In order to enhance the saturation magnetization of FePt nanoparticles, the initial mole ratio of Fe to Pt precursors and reaction times were controlled to effectively increase magnetization due to the increased particle size and formation of FePt-Fe3O4 nanocomposites. The surface modification of FePt nanoparticles by using mercaptoacetic acid (C2H4O2S) as a phase transfer reagent through ligand exchange turned the nanoparticles hydrophilic, and the nanoparticles could water-dispersible. The streptavidin-biotin binding pair was used to conjugate with carboxylic acid (COOH) functional group on the surface of FePt nanoparticles that could be further functionalized to provide a biotin moiety for specific interactions with streptavidin protein.     

Effect of sintered grain growth on chemical ordering in binary FePt/Cu nanoparticle arrays

Recent studies have shown a strong correlation between grain growth and chemical ordering in chemically synthesized FePt nanoparticles. In order to study this effect, we have prepared a series of samples in which 3.5 nm FePt nanoparticles are dispersed in a matrix of Cu nanoparticles. The samples were annealed at 600 degrees C and at 800 degrees C. Grain size was determined by XRD Scherrer analysis and time-dependent remanent coercivity measurements were made to determine the intrinsic remanent coercivity, Hcr0. For samples annealed at 600 degrees C, Hcr0 increases strongly with grain size up to approximately 5 nm and increases weakly with additional grain growth. By contrast, after annealing at 800 degrees C, Hcr0 appears nearly independent of grain size. The results suggest that isolated 3.5 nm FePt nanoparticles can be weakly ordered when annealed at 600 degrees C and sintering is necessary for significant chemical ordering.     

Magnetic property of FePt nanoparticles encaged in carbon nanotubes

Encapsulation of FePt nanoparticles in carbon nanotubes (CNTs) was attempted using a thermal chemical vapor deposition technique with a Fe/Pt bilayer catalyst. The metal nanoparticles were encapsulated at the tip of multi-walled CNTs. A selected area electron diffraction measurement of the nanoparticles at CNT tips indicated that diffraction spots attributed to an ordered L1₀ phase. Magnetic hysteresis loops indicated existence of magnetic nanoparticles having various coercivities. From numerical fittings assuming that high and low coercivity components contributed to the hysteresis loops, the high coercivity component was estimated to reach 11.3 kOe (902 kA/m).     

Low temperature magnetic hardening in self-assembled FePt/Ag core-shell nanoparticles

The FePt/Ag core-shell nanoparticles with different Ag shell thickness have been fabricated using a seed mediated technique. The core-shell nanoparticles are annealed at temperatures ranging from 350 to 600 °C for 30 min in vacuum. The magnetic measurement demonstrates that the FePt/Ag core-shell nanoparticles show a better chemical ordering tendency with a magnetic hardening temperature of 400–450 °C, which is almost 100 °C lower than that of pure FePt nanoparticles. Negative peaks on the δM curves of the annealed FePt/Ag core-shell nanoparticles demonstrate that the predominant interparticle interactions are dipolar type rather than exchange coupling one. Besides, the FePt/Ag core-shell nanoparticles show both sensitive plasmonic and superparamagnetic properties. The present results indicate that our composite nanoparticles are very promising from the viewpoint of the optoelectronics and biomedical applications.     

Grain Refining and Decoupling in FePt/SiO2 Nanogranular Films for Magnetic Recording

FePt/SiO₂ nanogranular thin films have been prepared by molecular-beam epitaxy system on MgO (001) substrates with the method of insertion dual SiO₂ layers into Fe/Pt multilayer films. We report the relationships between the inserting thickness of SiO₂ layers and the microstructural and magnetic properties of FePt thin films. It indicated the nanogranular FePt thin films were successfully formed by inserting amorphous SiO₂ layers into the Fe/Pt films. The reduction of grain/domain size and isolation of FePt particles can be achieved by such insertion and maintain (001) texture. The average grain size of FePt films with 5-nm SiO₂ insert layers is estimated to be around 8 nm, while domain rotation is enhanced depicting a decoupling of intergrain interaction. The isolated grains are less magnetically coupled in the rotation mode and the reversal of magnetization is more independent     

Chemically synthesized FePt nanoparticle material for ultrahigh-density recording

We have examined the magnetic anisotropy of the "heat-treated FePt nanoparticles" annealed in a magnetic field. The magnetic easy axis of the "heat-treated FePt nanoparticles" is found to be three-dimensional (3-D) random and a partial ordering fct structure is observed before annealing in the presence of a magnetic field. The value of M/sub r//M/sub s/ obtained is 0.5. After annealing in the presence of a magnetic field, the M-H loop indicates that the easy axis is oriented preferably in the perpendicular direction than along the in-plane direction. The value of H/sub c/(//)/H/sub c/(/spl perp/) at 10 K is 0.62 (1410 Oe/2250 Oe). The value of M/sub r//M/sub s/(/spl perp/) is 0.58 at 10 K larger than the value of M/sub r//M/sub s/(//). Therefore, a weak magnetic easy axis orientation is fundamentally possible on the chemically synthesized FePt nanoparticles. We have studied the recording characteristics of a 3-D random nanoparticle medium using a GUZIK spinstand and observed the recorded patterns for the medium by imaging with a magnetic force microscopy.     

Interfacial magnetic coupling between Fe nanoparticles in Fe–Ag granular alloys

The role of the interface in mediating interparticle magnetic interactions has been analysed in Fe50Ag50 and Fe55Ag45 granular thin films deposited by the pulsed laser deposition technique (PLD). These samples are composed of crystalline bcc Fe (2–4 nm) nanoparticles and fcc Ag (10–12 nm) nanoparticles, separated by an amorphous Fe50Ag50 interface, occupying around 20% of the sample volume, as determined by x-ray diffraction (XRD), x-ray absorption spectroscopy (XAS), and high resolution transmission electron microscopy (HRTEM). Interfacial magnetic coupling between Fe nanoparticles is studied by dc magnetization and x-ray magnetic circular dichroism (XMCD) measurements at the Fe K and Ag L2,3 edges. This paper reveals that these thin films present two magnetic transitions, at low and high temperatures, which are strongly related to the magnetic state of the amorphous interface, which acts as a barrier for interparticle magnetic coupling.     

Structural and Mössbauer effect investigations of amorphous FeCuNbSiB alloys nanocrystallized (VITROPERM) in magnetic field

Melt-spun amorphous ribbons of nominal composition Fe73Cu1Nb3Si16B7, annealed at 560-580 degrees C for 1 hour in a magnetic field (H) applied along the width in the ribbon plane, develop uniaxial magnetic anisotropy with easy axis along H and exhibit several novel attributes. The samples labelled as S20 and S150 are nanocomposites consisting of ferromagnetic nanocrystalline grains (volume fraction approximately equal to 84% and 81%) of mean size d = 13(2) nm embedded in a ferromagnetic amorphous matrix and possess a magnetic permeability as large as 20,000 and 150,000, respectively. While nearly 55% of the nanocrystalline grains have a cubic DO3 Fe3Si-like structure with actual Si concentration of about 22 at.%, the remaining 45% nanocrystalline grains have tetragonal Fe3B and hexagonal Fe2Si structure. Since the crystalline volume fraction of Fe3B and Fe2Si nanocrystals is more in the sample S20, this sample exhibits stronger local magnetic anisotropy and hence lower permeability.     

Onset of hard magnetic L10 FePt phase with (001) texture

The perpendicular anisotropic magnetic properties of in-situ deposited FePt/Pt/Cr trilayer films were elucidated as functions of the deposition temperature and the sputtering rate of the FePt magnetic layer. Ordered L1₀ FePt thin films with perpendicular anisotropy and a (001) texture can be developed at a temperature as low as 300 °C with the sputtering of a FePt layer at a low rate. The larger Pt(001)[100] lattice induced an expansion of the FePt a- and b-axis, leading to the contraction of the FePt c-axis, enabling the epitaxial growth of the L1₀ FePt(001) texture to occur. A low rate of sputtering of the FePt thin film promotes the formation of the magnetically hard FePt(001) texture on the surface of the Pt(001) buffer layer at low temperature, while the high sputtering rate of FePt layer suppresses the phase transformation.