α-Fe2O3磁性微球的合成及磁性能

以氯化铁（FeCl3·6H2O）和氨水（NH3·H2O）为原料,以十六烷基三甲基溴化铵（CTAB）为表面活性剂,采用沉淀法制备了氧化铁磁性微球.所得样品用XRD、SEM及SQUID-VSM等手段进行了表征.结果表明,所得氧化铁磁性微球为斜方六面体结构,其粒径大小在0.5-1.5μm范围,其剩余磁感应强度为0.06emu/g,矫顽力为1700Oe,表现出一定的铁磁性.     

SQUID sensor application for small metallic particle detection

High-Tc superconducting quantum interference device (SQUID) is an ultra-sensitive magnetic sensor. Since the performance of the SQUID is improved and stabilized, now it is ready for application. One strong candidate for application is a detection system of magnetic foreign matters in industrial products or beverages. There is a possibility that ultra-small metallic foreign matter has been accidentally mixed with industrial products such as lithium ion batteries. If this happens, the manufacturer of the product suffers a great loss recalling products. The outer dimension of metallic particles less than 100 μm cannot be detected by an X-ray imaging, which is commonly used for the inspection. Ionization of the material is also a big issue for beverages in the case of the X-ray imaging. Therefore a highly sensitive and safety detection system for small foreign matters is required. We developed detection systems based on high-Tc SQUID with a high-performance magnetic shield. We could successfully measure small iron particles of 100 μm on a belt conveyer and stainless steel balls of 300 μm in water. These detection levels were hard to be achieved by a conventional X-ray detection or other methods.     

The 1.58 μm transparency window of methane (6165-6750 cm): Empirical line list and temperature dependence between 80 and 296 K

The empirical line parameters of over 12,000 methane transitions have been obtained at 80 K in the 1.58 μm transparency window (6165-6750 cm⁻¹) which is of importance for planetary applications. This line list (WKC-80K) was constructed from high sensitivity spectra of normal abundance methane recorded by CW-Cavity Ring Down Spectroscopy at low temperature. The minimum intensity reported is on the order of 5×10⁻³⁰ cm/molecule. High resolution Fourier transform spectra have also been recorded using enriched CH₃D samples at 90-120 K in order to facilitate identification of monodeuterated methane features in the methane line list at 80 K. The CH₃D relative contribution in the considered region is observed to be much larger at 80 K than at room temperature. In particular, CH₃D is found dominant in a narrow spectral window near 6300 cm⁻¹ corresponding to the highest transparency region.Using a similar line list constructed at room temperature (Campargue A, Wang L, Liu AW, Hu SM and Kassi S. Empirical line parameters of methane in the 1.63-1.48 μm transparency window by high sensitivity Cavity Ring Down Spectroscopy. Chem Phys 2010;373:203-10.), the low energy values of the transitions observed both at 80 K and at room temperature were derived from the variation of their line intensities. Empirical lower states and J-values have been obtained for 5671 CH₄ and 1572 CH₃D transitions representing the most part of the absorbance in the region. The good quality of these derived energy values is demonstrated by the marked propensity of the corresponding CH₄ lower state J values to be close to integers. The WKC line lists at 80 K and room temperature provided as Supplementary Material allow one accounting for the temperature dependence of methane absorption between these two temperatures. The importance of the 80 K line list for the study of Titan and other methane containing planetary atmospheres is underlined and further improvements are proposed. The resulting information will advance the theoretical modeling of the methane spectrum in the 1.58 μm transparency window.     

Magnetic properties of ultrathin Ni films

The magnetic properties of Au/Ni/Si(100) films with Ni thicknesses of 8–200 Å are studied at T=77 K using a scanning magnetic microscope with a thin-film high-temperature dc SQUID. It is found that the Ni films, with an area of 0.6×0.6 mm, which are thicker than 26 Å have a single-domain structure with the magnetic moment oriented in the plane of the film and a saturation magnetization close to 0.17 MA/m. For films less than 26 Å thick, the magnetization of the film is found to drop sharply.     

脉冲磁场下水热法制备Cr掺杂ZnO稀磁 半导体晶体

本文以ZnCl₂, CrCl₃. 6H₂O和氨水缓冲溶液为原料, 在4T脉冲磁场下水热法制备了Cr掺杂ZnO稀磁半导体晶体, 通过X射线衍射分析、扫描电子显微镜观察及采用振动样品磁强计进行磁性分析等, 探讨了脉冲磁场对其微观结构及磁性能的影响. 结果表明: Cr掺杂ZnO稀磁半导体晶体仍保持ZnO的六方纤锌矿结构, 脉冲磁场具有促进晶粒生长及取向排列的作用, 4T脉冲磁场条件下合成的Cr掺杂ZnO稀磁半导体具有良好的室温铁磁性, 其饱和磁化强度(M_s)为0.068 emu/g, 而无脉冲磁场情况下制备的样品室温下呈顺磁性, 并且, 脉冲磁场下制备将稀磁半导体的居里温度提高了16 K.     

Characterization of Scanning SQUID Probes Based on 3D Nano-Bridge Junctions in Magnetic Field

We develop superconducting quantum interference device(SQUID) probes based on 3D nano-bridge junctions for the scanning SQUID microscopy. The use of these nano-bridge junctions enables imaging in the presence of a high magnetic field. Conventionally, a superconducting ground layer has been employed for better magnetic shielding. In our study, we prepare a number of scanning SQUID probes with and without a ground layer to evaluate their performance in external magnetic fields. The devices show the improved magnetic modulation up to 1.4 T. It is found that the ground layer reduces the inductance, and increases the modulation depth and symmetricity of the gradiometer design in the absence of the field. However, the layer is not compatible with the use of the scanning SQUID probe in the field because it decreases its working field range. Moreover, by adding the layer, the mutual inductance between the feedback coil and the SQUID also decreases linearly as a function of the field.     

Metallic contaminant detection system using multi-channel high Tc SQUIDs

We have developed the magnetic metallic contaminant detectors using multiple high Tc SQUID gradiometers for industrial products. Finding ultra-small metallic contaminants is a big issue for manufacturers producing commercial products. The quality of industrial products such as lithium ion batteries can deteriorate by the inclusion of tiny metallic contaminants. When the contamination does occur, the manufacturer of the product suffers a great loss to recall the tainted products. Metallic particles with outer dimension less than 50 μm cannot be detected by a conventional X-ray imaging. Therefore a high sensitive detection system for small foreign matters is required. However, in most of the cases, the matrix of an active material coated sheet electrode is magnetized and the magnetic signal from the matrix is large enough to mask the signal from contaminants. Thus we have developed a detection system based on a SQUID gradiometer and a horizontal magnetization to date. For practical use, we should increase the detection width of the system by employing multiple sensors. We successfully realized an eight-channel high-Tc SQUID gradiometer system for inspection of sheet electrodes of a lithium ion battery with width of at least 60 to 70 mm. Eight planar SQUID gradiometers were mounted with a separation of 9.0 mm. As a result, small iron particles of less than 50 μm were successfully measured. This result suggests that the system is a promising tool for the detection of contaminants in a lithium ion battery.     

Impedance measurements on Au microelectrodes using controlled atmosphere high temperature scanning probe microscope

High temperature impedance measurements on Au microelectrodes deposited on polished yttria stabilized zirconia (YSZ) pellets were demonstrated using a newly designed controlled atmosphere high temperature scanning probe microscope (CAHT-SPM). Probes based on Pt_0.8Ir_0.2 were fabricated and employed in all the investigations. The electrical properties of the Au microelectrodes were investigated using CAHT-SPM at various temperatures in air. The influences of the tip-sample force and of the size of the microelectrode on the electrical properties of the Au microelectrodes were also studied. The impedance spectra of circular Au microelectrodes down to 8 μm in diameter at different temperatures were successfully obtained. The CAHT-SPM presented in this paper is capable of obtaining topography images, conductivity images and impedance spectra in-situ in a temperature range from room temperature to at least 650 °C.     

Impact of ligand spacer and counter-anion in selected 1D iron(II) spin crossover coordination polymers

A new 1D coordination polymer [Fe(βAlatrz)₃](ClO₄)₂ ? H₂O (1) with a neutral bidentate ligand, βAlatrz = 4H-1,2,4-triazol-4-yl-propionate, was prepared and its magnetic behavior was investigated by temperature dependent magnetic susceptibility measurements and ⁵⁷Fe M?ssbauer spectroscopy. The temperature dependence of the high-spin molar fraction derived from ⁵⁷Fe M?ssbauer spectroscopy recorded on cooling below room temperature reveals a gradual single step transition with T_1/2 = 173?K between high-spin and low-spin states in agreement with magnetic susceptibility measurements. 1 presents striking reversible thermochromism from white, at room temperature, to pink on quench cooling to liquid nitrogen. The phase transition is of first order as deduced from differential scanning calorimetry, with T_1/2 matching the one determined by both SQUID and ⁵⁷Fe M?ssbauer spectroscopy. A brief assessment has been made among closely related 1D coordination polymers to perceive the effect of ligand spacer length and anion effect on the spin crossover behavior of these new materials.     

Structural, morphological, and magnetic characteristics of Cu-implanted nonpolar GaN films

Diluted magnetic nonpolar GaN:Cu films have been fabricated by implanting Cu ions into unintentionally doped nonpolar a-plane() GaN films and a subsequent thermal annealing process. The structural, morphological and magnetic characteristics of the samples have been investigated by means of high-resolution X-ray diffraction (HRXRD), atomic force microscopy (AFM), and superconducting quantum interference device (SQUID). The sample shows a clear ferromagnetism behavior at room temperature. It is significantly shown that with a Cu concentration as low as 0.75% the sample exhibits a saturation magnetization about 0.65 μ_B/Cu atom. Moreover, the possible origin of the ferromagnetism for the sample was also discussed briefly.     

Characterization of n-GaN dilute magnetic semiconductors by cobalt ions implantation at high-fluence

In this study, we present the structural and magnetic characteristics of cobalt ions implantation at a high-fluence (5×10¹⁶ cm⁻²) into n-GaN epilayer of thickness about 1.6 μm. The n-GaN was grown on sapphire by metal organic chemical vapor deposition (MOCVD). Rutherford backscattering channeling was used for the structural study. After implantation, samples were annealed at 700, 800 and 900 °C by rapid thermal annealing in ambient N₂. XRD measurements did not show any secondary phase or metal related-peaks. High resolution X-ray diffraction (HRXRD) was performed as well to characterize structures. Well-defined hysteresis loops were observed at 5 K and room temperature using alternating gradient magnetometer AGM and Superconducting Quantum Interference Device (SQUID) magnetometer. Temperature-dependent magnetization indicated magnetic moment at the lowest temperatures and retained magnetization up to 380 K for cobalt-ion-implanted samples.     

Synthesis of Fe3O4 hollow microsphere chains and their magnetic properties

Fe₃O₄ hollow microsphere chains with lengths of 8–11 μm have been solvothermally synthesized in the mixed solution of glycerol and water with 1 M NaOH. The hollow microspheres have diameters in the range 0.7–1 μm, and the thickness of the shells is 150–300 nm. The shell of the hollow microspheres is constructed by octahedrons of 100–170 nm. However, when the concentration of NaOH is adjusted to 3 M, the octahedron chains with lengths of 30–50 μm can be obtained. The magnetic saturation values of hollow microsphere chains and octahedron chains are 88.1 and 102.4 emu/g at room temperature, respectively.     

SETUP AND APPLICATION OF SCANNING NEAR-FIELD OPTICAL MICROSCOPY

The research on the setup and application of scanning near-field optical microscopy (SNOM) performed in our laboratory is reviewed in this report. We have constructed a versatile low temperature scanning near-field optical microscope with the capability of near-field imaging and spectroscopy, operating at liquid nitrogen temperature. A special designed coaxial double lens was used to introduce the illumination beam through a 200μm fiber; the detected optical signal was transmitted via a fiber tip to an avalanche photon detector. The performance test shows the stability of the new design. The shear force image and optical image of a standard sample are shown. A system of SNOM working at room temperature and atmosphere was used to characterize semiconductors and bio-molecular samples. It revealed the unique features of semiconductor microdisks in the near-field that is significantly different from that of far-field. The effects of different geographic microstructures on the near-field light distribution of InGaP, GaN, and InGaN multi-quantum-well microdisk were observed.     

Magnetic ordering in the frustrated system FeSc2S4

The sample of FeSc₂S₄ was prepared by solid reaction method. The crystallographic structure and the magnetic properties of the fabricated compound were investigated by X-ray, and superconducting quantum interference device (SQUID) magnetometer and Mössbauer spectroscopy. The polycrystalline FeSc₂S₄ confirmed the normal cubic spinel structure (space group Fd3m). The lattice constants a₀ and anion parameter u are 10.519 Å and 0.255, respectively. The Mössbauer spectroscopy has been studied for the FeSc₂S₄ at various temperatures, ranging from 4.2 K to room temperature. The spectra consist of two doublets at 4.2 K while a single line at room temperature. It is noticeable that the Mössbauer spectra of two doublet patterns with large electric quadrupole splitting (ΔE_Q) remain over the Néel temperature. Those are interpreted as a result of large electric quadrupole interaction compared to magnetic dipole interaction. The magnetic susceptibility measurements were performed with a SQUID magnetometer for temperatures 2<T<320 K, in external fields up to 5 kOe. Magnetic behavior shows antiferromagnetic behavior and the magnetic superexchange interactions between the Fe ions are weakly antiferromagnetic. The paramagnetic susceptibilities follow Curie–Weiss (CW) law with CW temperature Θ_CW=−100 K, and frustration parameter f=−Θ_CW/T_N is of the order of 1000. We conclude that two sublattices are coupled antiferromagnetically, leading to strong frustration effects.     

Synthesis and magnetic properties of ordered barium ferrite nanowire arrays in AAO template

BaFe₁₂O₁₉ nanowire arrays having single magnetic domain size (≤460 nm) in anodic aluminum oxide (AAO) templates were prepared by sol-gel and self-propagating high-temperature synthesis techniques. The diameter of the nanowire arrays is approximately 70 nm and the length is about 2-4 μm. The specimens were characterized using X-ray diffraction, vibrating sample magnetometer, field emission scan electron microscope, atomic force microscopy and microwave vector network analyzer. The magnetic properties of BaFe₁₂O₁₉ nanowire arrays embedded in AAO templates were measured by VSM with a field up to 1274 KA/m at room temperature. The results indicate that the nanowire arrays exhibit large saturation magnetization and high coercivity in the range of 6000 Oe and an obvious magnetic anisotropy with the easy magnetizing axis along the length of the nanowire arrays, probably due to the shape anisotropy and magneto-crystalline anisotropy. Finally the microwave absorption properties of the nanowires were discussed.     

Scanning laser microscope for imaging nanostructured superconductors

The nanofabrication of superconductors yields various interesting features in superconducting properties. A variety of different imaging techniques have been developed for probing the local superconducting profiles. A scanning pulsed laser microscope has been developed by the combination of the XYZ piezo-driven stages and an optical fiber with an aspheric focusing lens. The scanning laser microscope is used to understand the position-dependent properties of a superconducting MgB₂ stripline of length 100 μm and width of 3 μm under constant bias current. Our results show that the superconducting stripline can clearly be seen in the contour image of the scanning laser microscope on the signal voltage. It is suggested from the observed image that the inhomogeneity is relevant in specifying the operating conditions such as detection efficiency of the sensor.     

Crystallographic and magnetic structure of HAVAR under high-pressure using diamond anvil cell (DAC)

Annealed (H1) and cold-rolled (H2) HAVAR has been studied using high-pressure synchrotron X-ray diffraction. A structural phase transformation was discovered at ～13 GPa at ambient temperature, transforming from m ??3 m (S.G. 225) to P 63/m m c (S.G. 194) symmetry. The transition was not reversible on pressure release. The low-pressure cubic phase was found to be more compressible than the high-pressure hexagonal phase. Conventional Mössbauer and NFS shows that the HAVAR is not magnetic at room temperature and no splitting is observed. The SQUID indicates a huge difference in the temperature dependence of the magnetic susceptibility between the cold Rolled HAVAR compared to the annealed HAVAR.     

Influence of annealing temperature on structural, optical and magnetic properties of Mn-doped ZnO thin films prepared by sol-gel method

Thin films of Zn_1−xMn_xO (x=0.01) diluted magnetic semiconductor were prepared on Si (1 0 0) substrates by the sol-gel method. The influence of annealing temperature on the structural, optical and magnetic properties was studied by X-ray diffraction (XRD), atom force microscopy (AFM), photoluminescence (PL) and SQUID magnetometer (MPMS, Quantum Design). The XRD spectrum shows that all the films are single crystalline with (0 0 2) preferential orientation along c-axis, indicating there are not any secondary phases. The atomic force microscopy images show the surfaces morphologies change greatly with an increase in annealing temperature. PL spectra reveal that the films marginally shift the near band-edge (NBE) position due to stress. The magnetic measurements of the films using SQUID clearly indicate the room temperature ferromagnetic behavior, and the Curie temperature of the samples is above room temperature. X-ray photoelectron spectroscopy (XPS) patterns suggest that Mn²⁺ ions were successfully incorporated into the lattice position of Zn²⁺ ions in ZnO host. It is also found that the post-annealing treatment can affect the ferromagnetic behavior of the films effectively.     

Synthesis of magnetic hollow silica using polystyrene bead as a template

In this paper, we report a new route to synthesize novel magnetic hollow silica nanospheres (MHSNs) using polystyrene particles as sacrificial templates, and TEOS and Fe₃O₄ as precursors. TEM, EDS, XRD, and SQUID were applied to characterize MHSNs. TEM and EDS results show that the MHSNs consist of about 200 nm of hollow cores and ∼35 nm shells with ∼10 nm of Fe₃O₄ nanoparticles embedded. The polystyrene beads were successfully removed by immersing the as-prepared silica nanocomposite in a toluene solution. XRD results demonstrate that the Fe₃O₄ magnetic nanoparticles still keep spinel structure even heated at low temperature. The surface status of the polystyrene beads and Fe₃O₄ nanoparticles has an important effect on the formation of the MHSNs. The MHSNs present a superparamagnetism at room temperature by SQUID measurement. The MHSNs have potential applications in biosystem and nanomedicine.