Imaging the Magnetic Reversal of Isolated and Organized Molecular‐Based Nanoparticles using Magnetic Force Microscopy

In the race towards miniaturization in nanoelectronics, magnetic nanoparticles (MNPs) have emerged as potential candidates for their integration in ultrahigh‐density recording media. Molecular‐based materials open the possibility to design new tailor‐made MNPs with variable composition and sizes, which benefit from the intrinsic properties of these materials. Before their implementation in real devices is reached, a precise organization on surfaces and a reliable characterization and manipulation of their individual magnetic behavior are required. In this paper, it is demonstrated how molecular‐based MNPs are accurately organized on surfaces and how the magnetic properties of the individual MNPs are detected and tuned by means of low‐temperature magnetic force microscopy (LT‐MFM) with variable magnetic field. The magnetization reversal on isolated and organized MNPs is investigated; in addition, the temperature dependence of their magnetic response is evaluated.     

A novel imaging tool for hepatic portal system using phase contrast technique with hydrogen peroxide‐generated O2 gas

The objective of this study was to investigate the potential of hydrogen peroxide‐generated oxygen gas‐based phase contrast imaging (PCI) for visualizing mouse hepatic portal veins. The O₂ gas was made from the reaction between H₂O₂ and catalase. The gas production was imaged by PCI in real time. The H₂O₂ was injected into the enteric cavity of the lower sigmoid colon to produce O₂ in the submucosal venous plexus. The generated O₂ gas could be finally drained into hepatic portal veins. Absorption contrast imaging (ACI) and PCI of O₂‐filled portal veins were performed and compared. PCI offers high resolution and real‐time visualization of the O₂ gas production. Compared with O₂‐based ACI, O₂‐based PCI significantly enhanced the revealing of the portal vein in vivo. It is concluded that O₂‐based PCI is a novel and promising imaging modality for future studies of portal venous disorders in mice models.     

Influence of higher harmonics of the undulator in X‐ray polarimetry and crystal monochromator design

The spectrum of the undulator radiation of beamline P01 at Petra III has been measured after passing a multiple reflection channel‐cut polarimeter. Odd and even harmonics up to the 15th order, as well as Compton peaks which were produced by the high harmonics in the spectrum, could been measured. These additional contributions can have a tremendous influence on the performance of the polarimeter and have to be taken into account for further polarimeter designs.     

Upgrade of beamline BL08B at Taiwan Light Source from a photon‐BPM to a double‐grating SGM beamline

During the last 20 years, beamline BL08B has been upgraded step by step from a photon beam‐position monitor (BPM) to a testing beamline and a single‐grating beamline that enables experiments to record X‐ray photo‐emission spectra (XPS) and X‐ray absorption spectra (XAS) for research in solar physics, organic semiconductor materials and spinel oxides, with soft X‐ray photon energies in the range 300–1000 eV. Demands for photon energy to extend to the extreme ultraviolet region for applications in nano‐fabrication and topological thin films are increasing. The basic spherical‐grating monochromator beamline was again upgraded by adding a second grating that delivers photons of energy from 80 to 420 eV. Four end‐stations were designed for experiments with XPS, XAS, interstellar photoprocess systems (IPS) and extreme‐ultraviolet lithography (EUVL) in the scheduled beam time. The data from these experiments show a large count rate in core levels probed and excellent statistics on background normalization in the L‐edge adsorption spectrum.     

In situ X‐ray data collection and structure phasing of protein crystals at Structural Biology Center 19‐ID

A prototype of a 96‐well plate scanner for in situ data collection has been developed at the Structural Biology Center (SBC) beamline 19‐ID, located at the Advanced Photon Source, USA. The applicability of this instrument for protein crystal diffraction screening and data collection at ambient temperature has been demonstrated. Several different protein crystals, including selenium‐labeled, were used for data collection and successful SAD phasing. Without the common procedure of crystal handling and subsequent cryo‐cooling for data collection at T = 100 K, crystals in a crystallization buffer show remarkably low mosaicity (<0.1°) until deterioration by radiation damage occurs. Data presented here show that cryo‐cooling can cause some unexpected structural changes. Based on the results of this study, the integration of the plate scanner into the 19‐ID end‐station with automated controls is being prepared. With improvement of hardware and software, in situ data collection will become available for the SBC user program including remote access.     

Investigation of damaged interior walls using synchrotron‐based XPS and XANES

Evidence of internal sulfate attack in field exposure was demonstrated by the damaged interior wall of a three‐year‐old house situated in Nakhon Ratchasima Province, Thailand. Partial distension of the mortar was clearly observed together with an expansion of a black substance. Removal of the black substance revealed a dense black layer. This layer was only found in the vicinity of the damaged area, suggesting that this black material is possibly involved in the wall cracking. By employing synchrotron‐based X‐ray photoelectron spectroscopy (XPS) and X‐ray absorption near‐edge structure (XANES) techniques, the unknown sample was chemically identified. The S 2p and O 1s XPS results mutually indicated the existence of sulfate species in the materials collected from the damaged area. The XANES results indicated the presence of ferrous (II) sulfate, confirming sulfate‐induced expansion and cracking. The sulfate attack in the present case appeared to physically affect the structure whereas the chemical integrity at the molecular level of the calcium silicate hydrate phase was retained since there was a lack of spectroscopic evidence for calcium sulfate. It was speculated that internal sulfate probably originated from the contaminated aggregates used during the construction. The current findings would be beneficial for understanding the sulfate‐attack mechanism as well as for future prevention against sulfate attack during construction.     

Characteristics of Friedel pairs and diffraction contrast tomography with non‐perpendicular rotation axis

The characteristics of Friedel pairs in diffraction contrast tomography (DCT) are studied in the condition that the rotation axis of the sample is not exactly perpendicular to the incident X‐ray direction. For the rotation axis approximately aligned along the vertical direction, the Friedel pairs close to the horizontal plane are insensitive to the non‐perpendicularity of the rotation axis, and can be used to refine the sample‐to‐detector distance and X‐ray energy, while the Friedel pairs close to the vertical direction are sensitive to the non‐perpendicularity of the rotation axis, and can be used to determine the rotation axis orientation. The correct matching proportion of Friedel pairs decreases with increasing non‐perpendicularity of the rotation axis. A method of data processing considering rotation axis misalignment is proposed, which significantly increases the correct matching and indexing proportions of the diffraction spots. A pure aluminium polycrystalline sample is investigated using DCT at beamline 4W1A of Beijing Synchrotron Radiation Facility. Based on the analysis of Friedel pairs, the sample‐to‐detector distance and X‐ray energy are refined to be 8.67 mm and 20.04 keV, respectively. The non‐perpendicular angle of the rotation axis is calculated to be 0.10°. With these refined geometric parameters, the matching proportion of the spatial position of diffraction spots is 90.62%. Three‐dimensional reconstruction of the sample with 13 grains is realised using the algebraic reconstruction technique. It is demonstrated that the precise correction of the orientation of the sample rotation axis is effective in DCT suffering from rotation axis misalignment, and the higher accuracy in determining the rotation axis is expected to improve the reconstruction precision of grains.     

Combination of HAADF‐STEM and ADF‐STEM Tomography for Core–Shell Hybrid Materials

Characterization of core–shell type nanoparticles in 3D by transmission electron microscopy (TEM) can be very challenging. Especially when both heavy and light elements coexist within the same nanostructure, artifacts in the 3D reconstruction are often present. A representative example would be a particle comprising an anisotropic metallic (Au) nanoparticle coated with a (mesoporous) silica shell. To obtain a reliable 3D characterization of such an object, a dose‐efficient strategy is proposed to simultaneously acquire high‐angle annular dark‐field scanning TEM and annular dark‐field tilt series for tomography. The 3D reconstruction is further improved by applying an advanced masking and interpolation approach to the acquired data. This new methodology enables us to obtain high‐quality reconstructions from which also quantitative information can be extracted. This approach is broadly applicable to investigate hybrid core–shell materials.     

一种裸眼识别Cu~(2+)和Hg~(2+)传感器的合成与性质研究

设计合成了一种香豆素修饰的罗丹明类衍生物L,用作程序型Cu2+与Hg2+检测传感器。采用核磁共振谱、高分辨质谱、红外光谱对其结构进行了表征。利用紫外光谱考察L对不同金属离子的识别作用,研究发现L可以高选择性和高灵敏度识别Cu2+。向L溶液中加入不同的金属离子时(Zn2+,Hg2+,Cu2+,Fe3+,Cd2+,Co2+,Ni 2+,Mg2+,Ca2+,Al 3+,La3+,K+,Na+,Mn2+,Pb2+和Ag+),只有Cu2+的加入会使溶液由无色变为粉色,并且在534nm出现一个新的吸收峰,说明传感器L可以裸眼识别Cu2+。通过紫外滴定得到L可以识别Cu2+的最低检测限为1.9×10-8 mol·L-1。制备了基于L的Cu2+检测试纸,该试纸可以方便快捷的检测水中的Cu2+。通过Job’s曲线和高分辨质谱确定了配合物L-Cu2+之间的结合比为1∶1。另外,若向L-Cu2+的DMSO溶液中加入1equiv.EDTA,溶液瞬间由粉色变为无色,说明EDTA可以取代L并与Cu2+结合,因此传感器L识别Cu2+是可逆的。另外,向L-Cu2+的配合物中加入Hg2+,溶液会由粉色变为无色(而加入其他阳离子没有明显变化),这可顺序实现对Hg2+的裸眼识别。通过紫外滴定计算出L-Cu2+识别Hg2+的最低检测限为2.9×10-7 mol·L-1。因此该程序型传感器L可以有序的裸眼识别Cu2+和Hg2+。