Pulsed fm NMR/on studies of single crystal54MnNi and125SbFe

Precision field shift studies of B_appl-8T using pulsed FM NMR/ON along hard directions (eg <100>⁵⁴MnNi, <112>¹²⁵SbFe and the easy axis (<111>⁵⁴MnNi, <100>¹²⁵SbFe) yield no measurable Knight shifts within the uncertainty allowed by current accuracy of the nuclear moments. This is in striking contrast to earlier measurements with the same apparatus that yielded K=+1.5 (4)% for⁶⁰CoFe. The modulation frequency dependences of the pulsed FMNMR/ON signals are investigated for a variety of rf parameters and compared with model predictions.     

Recent experiments with mapon spectroscopy

Electric quadrupole interactions of impurity nuclei in single crystals of⁵⁴MnNi,¹²⁵SbNi and¹²⁵SbFe have been studied as a function of crystal field direction and applied magnetic field using MAPON. Distributions are in all cases broad compared with the mode values of the EQI's. For⁵⁴MnNi the mode efg is isotropic to better than 5% between the easy <111> axis and a hard <100> axis. The efg is +0.88 (15)x 10¹⁹ Vm⁻². The mode efg for¹²⁵SbFe along its easy <100> axis is one half of that along a hard <112> axis, and one third of that measured along the easy <111> axis of¹²⁵SbNi. The much larger efg mode and distribution seen in¹²⁵SbNi, for four to eight times greater dilution than for¹²⁵SbFe, suggests intrinsic contributions due to valence screening effects in the more itinerant nickel host.     

Mapon and single passage NMRON spectroscopy on125SbFe and125SbNi single crystals

The signs, mode magnitudes and distributions of the electric quadrupole hyperfine interactions (EQI) in single crystal¹²⁵SbFe and¹²⁵SbNi have been examined along a principal hard axis for each system and are compared with earlier easy axis results. The surface preparation was essentially the same for both hosts but the results of the distribution width and anisotropy in the mode values of the measured EQI’s are remarkably different between the two hosts. For¹²⁵SbFe the mode value of the EQI is a factor of two larger along the hard axis <111> and the same sign, negative, as for the easy axis <100>. For¹²⁵SbNi the mode values of the EQI along the same two principal directions are comparable in magnitude but the efg distributions are much broader than in the¹²⁵SbFe case. Single passage results on¹²⁵SbNi provide a weak sweep asymmetry with indications of an apparent change in sign in EQI from negative along the <111> easy axis to positive along the hard <100> axis.     

Magnetic hyperfine fields of Nb andMo in nickel by NMR-ON of90Nb and93mMo

The magnetic hyperfine splitting frequencies of⁹⁰NbNi and^93mMoNi in an external magnetic field of 0.2 T have been determined by the NMR-ON method to be 18.52(7) and23.73(10) MHz, respectively. With the assumption of Knight shift factorK=0 and with the knowng-factors, the hyperfine fields of⁹⁰NbNi and^93mMoNi were deduced asB _HF(⁹⁰NbNi)=-4.118(16) T andB _HF(^93mMoNi)=-3.491(33) T. The rather long spin-lattice relaxation time of 32(5) min was observed for⁹⁰NbNi at an external magnetic field of 0.2T and8 mK.     

NMR-ON measurements of187WFe,182,183,186ReNi,186ReFe and203PbFe

The magnetic hyperfine splitting frequencies of¹⁸⁷WFe,¹⁸²Re(j ^π=2⁺)Ni,¹⁸³ReNi,¹⁸⁶ReNi,¹⁸⁶ReFe and²⁰³PbFe in a zero external magnetic field have been determined by the NMR-ON method at about 7 mK as 225.56(6), 130.9(1), 98.17(4), 136.6(4), 1007.0(3) and 58.43(3) MHz, respectively. With the knowng-factors ofg(¹⁸⁶Re, 1⁻)=1.739(3) andg(²⁰³Pb, 5/2⁻)=0.27456(20), the following hyperfine fields were deduced:B _HF(¹⁸⁶ReNi)=−103.05(35) kG;B _HF(¹⁸⁶ReFe)=−759.7(13) kG;B _HF(²⁰³PbFe)=+279.18(25) kG. Taking hyperfine anomalies into account, theg-factor of¹⁸³Re was deduced as |g(¹⁸³Re, 5/2⁺)|=1.267(6). With the assumption of Knight shift factorK=0, theg-factors of¹⁸²Re and¹⁸⁷W and the hyperfine field of¹⁸⁷WFe were determined as |g(¹⁸²Re, 2⁺)|=1.63(5), |g(¹⁸⁷W, 3/2⁻)|=0.414(10) andB _HF(¹⁸⁷WFe) =−714(18) kG. The large hyperfine anomaly was deduced to be¹⁸³W Δ¹⁸⁷W =−0.124(22).     

Quadrupole interaction studies of Hg in Sb

Time differential perturbed angular correlation and nuclear orientation studies of the electric quadrupole interaction for Hg in Sb have been performed. The effective field gradients |V _zz ^eff (HgSb)|=1.43(18)×10¹⁷V cm^–2 at room temperature andV _zz ^eff (HgSb)=+1.8(2) × 10¹⁷V cm^–2 below 0.05 K have been derived. These two values are no indication for an anomalous temperature dependence of the effective field gradient for Hg in Sb. The value of the electric field gradient fits well into the systematics for Hg in other hosts. It is shown that the electronic enhancements of the field gradients are correlated to the valence of the impurities and are rather insensitive to the host properties.On leave of absence from: University of Lisboa, Portugal     

Recent experiments with transient NMRON

High resolution magnetic and electric hyperfine interaction distributions are determined for single crystal⁵⁴MnNi with diffused impurity concentrations of 0.14 and 0.40 at%, and for a 0.1 µm layer of⁶⁰CoFe co-plated onto single crystal Fe. High quality gamma detected nuclear spin echoes recorded for the⁶⁰CoFe specimen demonstrate that a reduced influence of the RF skin effect far outweighs any magnetic hyperfine field interaction broadening associated with the co-plating process.     

μ+knight shifts and trapping in diluteSbSn alloys

Giant μ⁺ Knight shifts K_μ have been studied previously in Sb andSbBi alloys. Here we report μ⁺SR measurements on Sb with dilute heterovalent Sn impurities. A dramatic concentration dependence is observed: K_μ is increased slightly (relative to the value in pure Sb) by Sn concentrations of <0.1%, whereas larger concentrations cause a drastic reduction of K_μ. One concern could be that K_μ values in the alloy might reflect local band structure in trap sites near Sn impurities rather than the bulk “host” band structure of the alloy. This is indeed the case in bothSbSn (0.03%) andSbSn (0.06%), where a second, lower frequency TF-μSR signal begins to appear for T>60K. The amplitude of the low K_μ signal grows with increasing T at the expense of the amplitude of the high-K_μ, low-T signal, suggesting that the μ⁺ migrates through the host lattice to trap sites. A simple trapping model correctly describes the observed T-dependence of the amplitudes, phases and relaxation rates of the two signals. We conclude that the low-T Knight shift is truly characteristic of the host band structure while the much lower K_μ value of the high-T site is characteristic of a specific trap site, presumably adjacent to a Sn impurity.     

The mapon technique and recent developments

Typical linewidths observed in NMRON on dilute impurities in ferromagnetic metals are of order 1 MHz, making difficult the observation of structure in the resonance with splitting Δv much less than this value. The technique of Modulated Adiabatic Passage on Oriented Nuclei (MAPON) was recently developed as a means of measuring the weak electric quadrupole splitting Δv_Q of the nuclear hyperfine interaction due to an electric field gradient V_zz. MAPON has successfully been applied to measure Δv_Q as low as 4 kHz, i.e. less than 0.5% of the inhomogeneously broadened NMRON CWFM resonance line. The isotopes⁵⁶Co,⁵⁷Co,⁵⁸Co and⁶⁰Co have been studied in iron single crystal hosts, yielding Δv_Q consistent with known and estimated quadrupole moments. In addition the results to date give striking confirmation of analyses based on the single impurity relaxation model. Following a brief summary of the theoretical development of MAPON a review of experimental data is given for the CoFe<100> system. The variation of Δv_Q with direction of magnetization, measured in⁵⁸CoFe and⁶⁰CoFe single crystal samples, is also described. Further MAPON measurements are described for a⁵⁶CoFe polycrystalline sample, for which the most probable value and width of the distribution of V_zz can be described simply in terms of the single crystal principal axis results. The application of the MAPON technique to the measurement of nuclear electric quadrupole moments in implanted and diffused samples is discussed.     

Mössbauer effect study of Ni1−xCuxMnyFe2−yO4 system

The Mössbauer effect technique has been employed for the study of magnetic properties of spinel series Ni_1?xCu_xMn_yFe_2?yO₄ with 0.0≤x≤1.0, and y=0.6. The substitution of Mn³⁺ and Cu²⁺ ions results in a slight decrease of the hyperfine field at B‐ as well as A‐sites. The area ratio of Fe³⁺ ions at the A‐ and B‐site at 77 K indicates that Cu²⁺, Ni²⁺ and Mn³⁺ ions occupy the octahedral sites in an evidence for complete inverse spinel in this system. The temperature dependence of the hyperfine parameters has been studied for composition with x=0.5 where Nèel point T_N and Debye temperature θ_D are found to be 650 and 679 K, respectively. The temperature dependence of the sublattice magnetization σ(T) obeys a one‐third‐power law in the range 0.5N<0.99.     

Magnetic properties of nanocrystalline Ni0.7Mn0.3Gd0.1Fe1.9O4 ferrite at low temperatures

Mössbauer spectra and magnetic measurement of Ni_0.7Mn_0.3Gd_0.1Fe_1.9O₄ ferrite were investigated by Oxford MS-500 Mössbauer spectrometer and superconducting quantum interference device (SQUID) magnetometer with a field 5 T. Ni_0.7Mn_0.3Gd_0.1Fe_1.9O₄ nanoparticles have a considerable coercivity of 1040 Oe when the test temperature is reduced to 2 K. Mössbauer spectra show that Ni_0.7Mn_0.3Gd_0.1Fe_1.9O₄ nanoparticles exhibit superparamagnetism at room temperature and ferrimagnetism at 77 K.     

Hyperfine interactions of light Ir,Re isotopes in iron

The technique of On-line Nuclear Orientation has been applied to light Ir and Re isotopes. Using both¹⁹²IrFe and⁵⁴MnNi thermometers, orientation as a function of temperature was measured over the range 10–100 mK. Pulsed implantation methods were used to obtain spectra with gamma transitions well identified and clear of contaminant activities. Magnetic moment/oriented state spin combinations were obtained for^180,182,183Ir and for^180,179Re. The results are briefly discussed.     

Nuclear magnetic resonance on oriented76,77,82Br in Fe

Nuclear magnetic resonance on oriented^76,77,82BrFe has been measured using recoil-implanted samples. The magnetic hyperfine splitting frequency of⁸²BrFe in a zero external magnetic field has been determined to be 201.90(3) MHz. The resonances of⁷⁶BrFe and⁷⁷BrFe were also observed in an external magnetic field of 0.2 T asv(⁷⁶BrFe)=340.9(3) MHz andv(⁷⁷BrFe)=403.5(2) MHz. With the known values of theg-factors, the hyperfine fields have been deduced:B _HF(⁸²BrFe)=81.397(27) T,B _HF(⁷⁶BrFe)=81.38(7) T. Theg-factor of⁷⁷Br was determined to be |0.6487(4)|.     

Single-crystal EPR studies of transition-metal ions in inorganic crystals at very high frequency

Electron paramagnetic resonance (EPR) single-crystal rotation studies at very high frequency (249.9 GHz) of transition metal ions with electron spins greater than one-half are reported. At 249.9 GHz, the spectra are in the high-field limit despite large zero-field splittings. This leads to a considerable simplification of the spectra, and aids in their interpretation. Single-crystal 249.9 GHz EPR spectra of Ni²⁺ in Ni₂CdCl₆· 12H₂O, Mn²⁺ (0.2%) in ZnV₂O₇, and Fe³⁺ (2%) in CaYA10₄ were recorded at 253 K in an external magnetic field of up to 9.2 T, along with those at X-band and Q-band frequencies at 295 K and lower temperatures. The goniometer used at 249.9 GHz for single-crystal rotation is based on a quasi-optical design and is an integral part of a special Fabry-Pérot resonator. The values of the spin-Hamiltonian parameters were estimated from a simultaneous fitting of all of the observed line positions at several microwave frequencies recorded at various orientations of each crystal with respect to the external magnetic field with least-squares fitting in conjunction with matrix diagonalization. Estimates of zero-field splitting parameterD at room temperature are: for Ni²⁺, about ?31 GHz (site I) and about ?7 GHz (site II); for Mn²⁺, about 6 GHz; and for Fe³⁺, about 29 GHz.     

Magnetic hyperfine fields of Zr in nickel and iron measured by the DPAD method

The magnetic hyperfine fields of Zr in nickel and iron were measured by the DPAD method. Using the 8⁺ isomeric states in⁹⁰Zr and⁸⁸Zr these fields were found to beH _hf(ZrNi)=–4.65(10) T andH _hf(ZrFe)=–27.4(4) T, respectively.     

Satellite line structure in NMR-ON on206BiFe and182ReFe

Nuclear magnetic resonance on oriented²⁰⁶BiFe and¹⁸²ReFe has been measured using recoil implanted samples. Clearly resolved satellite structures were found for both systems. By annealing at an appropriate temperature, the resonance width was reduced. The satellite line structure for¹⁸²ReFe was studied with various annealing temperatures. The ratio of the resonance strength changed with the annealing temperature. The resonances for¹⁸²ReFe were also measured in external magnetic fields of 0.1, 0.2 and 0.4 T. The resonance frequencies for the satellite structure at an external magnetic field of 0.2 T were determined:v ₁=691.7(3),v ₂=684.4(2),v ₃=687.2(2) MHz for²⁰⁶BiFe;v ₁=231.15(5),v ₂=230.20(5) for¹⁸²ReFe. The origin of the satellite structure is discussed. The effective relaxation time of¹⁸²ReFe at 8 mK and external magnetic field of 0.2 T was determined to be 18.6(6) s using a single-exponential fit.     

Magnetocaloric properties in a FeNiGaMnSi high entropy alloy

We investigated a new Fe_26.7Ni_26.7Ga_15.6Mn₂₀Si₁₁ high entropy alloy (HEA) without the rare earth element. The structural, magnetic and magnetocaloric properties of the resulting materials are presented. The HEAs successfully is produced by the arc melting with suction casting method. The crystal structures are characterised through multiphase Rietveld refinement of X-ray diffraction data. The structure of the HEAs was found to be the body centred cubic (bcc). In the magnetic measurements, the ferromagnetic to paramagnetic transition was obtained in the range of 300–400 K. With the employed suction casting method; the Fe_26.7Ni_26.7Ga_15.6Mn₂₀Si₁₁ HEA shows the best magnetocaloric properties as 1.59 Jkg⁻¹K⁻¹ maximum magnetic entropy change (0–2 T) and 75.68 Jkg^-1 refrigeration capacity after the annealing process.     

Homogeneity examination of a disordered magnetic alloy by means of CEMS

The depth sensitivity of the Mössbauer effect conversion electron spectroscopy (CEMS) offers a possibility to check the homogeneity of an alloy as a function of the sample thickness. We present experimental results on (Fe_0.65Ni_0.35)_1-xMn_x (x=0.026) prepared by diffusion of Mn into a Fe_0.65Ni_0.35 foil. On an inhomogeneous sample we determined the diffusion coefficient of Mn in Fe_0.65Ni_0.35 at 1300 K to be about 10^?11 cm²/s.     

Low temperature nuclear orientation of a dilute RhCr alloy

A dilute^101mRhCr alloy has been investigated by means of low temperature nuclear orientation in the temperature range of 6–60 mK. The magnetic hyperfine field has been found proportional to the macroscopic chromium magnetization and follows even at these low temperatures an Overhauser distribution. The maximum hyperfine field value is B_o (T=6 mK)=7.0(5) T. A Knight shift of –16% affects the external magnetic field at the nuclear site.     

Mossbauer effect in (Fe1−xNix)80Mn20 alloys

Mossbauer spectra for Fe⁵⁷ nuclei in (Fe_1?xNi_x)₈₀Mn₂₀ alloys at 300°K and 80°K were measured. It was shown that substitution of Fe atoms by Ni atoms leads to a decrease in the effective magnetic field on the resonance nuclei. The results of these studies are interpreted proceeding on the basis of a model of mixed-exchange interaction. The type of spectra and a detailed analysis of the half-widths of the separate components of the ultrafine magnetic structure does not exclude the influence of relaxation phenomena.