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Pottery excavated from the archeological UNESCO world heritage site Ban Chiang in Thailand stem from distinct periods. Black vessels with cord-mark design from Pre-metal Age (ca. 3000–1000 BC), Bronze Age pottery (ca 1000–300 BC) with yellow-brown surface and Iron Age samples (ca. 300 BC–200 AD) with red pictorial surface patterns. In a previous work [Bismayer U., Srilomsak S., Treekamol Y., Tanthanuch W., Suriyatham K. Artefacts from Ban Chiang, Thailand: pottery with hematite-red geometric patterns. Z. Kristallogr. 2020, 235, 559–568] we studied the mineralogical composition and their surface colour materials of shards from Bronze and Iron Age. In this work we focus on bulk features of the dark Pre-metal Age cord-marked ceramic shard PSN2-S10E13 and compare its elemental and mineralogical composition with bulk composition of sample 5412-S6E15 from Bronze Age. Experimental techniques are electron microprobe, X-ray powder diffraction, FTIR spectroscopy, optical microscopy and X-ray tomographic microscopy (XTM). Sample PSN2-S10E13 contains more quartz than 5412-S6E15. In the bulk of the Pre-metal Age shard, diffraction signals of mullite occur, indicating higher firing temperatures compared to the younger sample. Phyllosilicate signals are seen in FTIR spectra of both shards. E-modes of quartz dominate FTIR spectra of both samples. Optical thin sections show voids around micro-particles in PSN2-S10E13 and XTM indicates that the pore volume percentage of sample PSN2-S10E13 is higher than in 5412-S6E15. Because of the large age gap to younger samples from Ban Chiang, the proper age of our oldest sample PSN2-S10E13 was determined using an accelerator mass spectrometer (AMS) by simultaneous 14C/12C and 13C/12C isotope ratio measurements which yielded a radiocarbon age of 3609 ± 29 BP (resp. 1659 ± 29 BC). [ABSTRACT FROM AUTHOR]

The inner diameter measurement of the micro-hole was performed by a tactile microprobing system using a method of the local surface interaction force detection. The inner diameter of the micro-hole was calculated by the least square method based on the probing coordinates obtained by a custom-made micro-coordinate measuring machine. The dispersion of the probing coordinates was investigated by changing the probe approaching direction with respect to the normal direction of the inner side of the micro-hole. During the probing inside the micro-hole, it was confirmed that the dispersion of the probing coordinates increased when the disagreement between the probe approaching direction and the normal direction of the micro-hole at the measured point became large. The influence of the dispersion of the probing coordinates was evaluated through the uncertainty analysis of the inner diameter measurement. It was revealed that the uncertainty of the inner diameter measurement could be improved when limiting the disagreement between the probe approaching direction and the normal direction of the micro-hole to within ±pi/4 rad. [ABSTRACT FROM AUTHOR]

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Direct sampling of lipids from tissues for direct mass spectrometry (MS) analysis allows a quick profiling of lipidome, which is important for biomedical applications. In this work, we developed a polyporous polymeric membrane (PPM) microprobe for highly efficient sampling of lipids directly from tissue samples. The PPM was prepared by polypropylene with pores as large of 10 ​μm, facilitating the permeation of lipids from tissue surfaces. The PPM was coated onto a stainless steel wire with a thickness of ∼100 ​μm. The entire analysis procedure includes sampling of the lipids in tissue, washing the probe, and extraction spray ionization for MS analysis. The effectiveness was validated by analyzing mouse brain tissue samples. It showed high recoveries for a series of lipid classes in comparison with total lipid extraction method. Further demonstration was carried out with analysis of tissue samples from mouse liver, stomach, kidney and legs. With high physical strength and good chemical stability, the microprobe was also demonstrated for sampling lipids inside mouse kidney tissue samples. By incorporating a photochemical derivatization, a workflow was also developed for fast detection of lipid CC isomers in tissue samples. Finally, a microprobe array was also developed for simultaneous sampling of lipids from multiple sites on tissue surfaces.

Metabolomics is one of the leading approaches for understanding the toxic-mode-of-action of environmental contaminants. Nuclear Magnetic Resonance (NMR) spectroscopy has been commonly used in metabolomic studies; however, its main drawback is its relatively low sensitivity, making it challenging to study mass limited but environmentally crucial samples. In this work a 1 mm microlitre probe modified with a separate lock chamber to address this challenge, provided substantial improvements in mass sensitivity relative to conventional 5 mm NMR probes. The 1 mm probe is used to analyze various components of the model organism Daphnia magna, including hemolymph, parthenogenetic eggs, dormant eggs, and neonates. A μL volume flow system is designed for the 1 mm probe to perform an in-vivo exposure of neonates to high salt concentrations. The metabolic investigation of these samples was only achieved due to the minimum sample requirements and high salt tolerance of the probe, demonstrating that the 1 mm microlitre probe modified with a separate lock chamber holds significant potential for future metabolomic studies of mass limited samples.

The use of the field emission gun in scanning electron microscopy permits the imaging of sub-micrometer-size features. However, achieving sub-micrometer analytical spatial resolution in electron probe microanalysis (EPMA) requires both reducing the electron beam size and reducing the accelerating voltage to achieve the desired sub-micrometer interaction volume. The resulting quantification of the first-row transition metals at low accelerating voltage, i.e., below 7–8 kV, is problematic as the main characteristic X‑ray lines (Kα) cannot be excited at these conditions. Furthermore, the use of the Lα and Lβ soft X‑ray lines for quantification is complicated by bonding and self-absorption effects resulting in not-yet-determined mass absorption coefficients and hence in the failure of the traditional matrix correction procedure. We propose two methods to circumvent these low-kilovolt (low-kV) analysis limitations: using the non-traditional FeLℓ line and using universal calibration curves for the more traditional FeLα and Lβ lines. These methods were successfully applied to Fe-sulfide minerals showing accurate quantification results by EPMA at reduced kV, necessary for accurate quantification of sub-micrometer sulfide grains. [ABSTRACT FROM AUTHOR]

Most interesting materials in nature are heterogeneous, so it is useful to haveanalytical techniques with spatial resolution sufficient to resolve these heterogeneities.This article presents the basics of X-ray photon-in/photon-outchemical imaging. This family of methods allows one to derive images reflectingthe chemical state of a given element in a complex sample, at micronor deep sub-micron scale. X-ray chemical imaging is relatively non-destructiveand element-selective, and requires minimal sample preparation. Thearticle presents the basic concepts and some considerations of data takingand data analysis, along with some examples.

In this article, dynamic behavior of vibratory microprobe is studied based on the strain gradient theory. The microprobe is considered as a piezoelectric actuator attached to a variable cross-section bar. The equation of motion is derived based on the strain gradient theory and solved both analytically and numerically. For analytical approach, a combination of mode summation and Galerkin's technique is used. Moreover, a hybrid finite element/finite difference method is used to calculate the numerical results. Findings show that there is an excellent agreement between the analytical and numerical results. Furthermore, the obtained natural frequencies and dynamic displacements of this work are compared with those of the classical theory and the effects of size dependency on the dynamic behavior of microprobe are discussed. [ABSTRACT FROM AUTHOR]

In this paper, we investigated two originated metamorphosed harzburgites of the metaperidotite complex from the northern part of the Gishaki area. Harzburgite rocks, as main ultramafic complexes of the studied area, have outcrops in the scattered locations of the area. Harzburgitic units were discriminated using petrography and Raman spectroscopy. There are two meta-harzburgite types based on the metamorphic history of their protholites with different mineralogy types. Normal metamorphosed harzburgites (N-Hz) are metamorphosed via phases of retrograde processes and contact metamorphosed harzburgites (C-Hz) metamorphosed visa some different phases containing contact metamorphism. One of the best clues that are different in these two rock types is Antigorite mineral characteristics. Antigorite polymorphs have structural and chemical sensitive characteristics that can discriminate using Raman spectroscopy. It had certain specific chemical differentiation compared with other serpentine polymorphs especially in Silica and molecular water contents. Reviewed antigorites illustrated general differentiations in themselves so that polymorphs hosted by C-HZ rocks could be considered as a group with typical Contact antigorite by geochemical criteria such as lower molecular water, higher Octahedral content and, higher Silica content. An increase in Si and Fe2+ activities cause incurrences octahedral substitutions as temperaturedependent phenomena in Contact antigorites. Diagrams of Silica versus molecular water contents and octahedral contents clearly distinguished modified antigorites from former antigorite polymorphs. Contact antigorite in the Gishaki serpentinites could be considered as metamorphosed products related to metamorphic aureoles. [ABSTRACT FROM AUTHOR]

Ban Chiang () is an extensively studied archeological site in Northeast Thailand, Udon Thani Province, which became a UNESCO world heritage in 1992. Depending on their production period ceramic artefacts show characteristic patterns at the surface which may be interpreted as iconographic motifs for the site. Two ceramic samples, excavated in 2003, from different periods were re-investigated, previously studied by Tanthanuch W., Pattanasiriwisawa W., Somphon W., Srilomsak S. Synchrotron studies of Ban Chiang ancient pottery. Suranaree J. Sci Technol. 2011, 18, 15–28 who focussed on thermal firing and redox-conditions. Shards selected for this study were sample 5412-S6E15 dated from Bronze Age (ca. 1000–300 BC) with yellow-brown, paint-free surface and a younger sample 8027 from Iron Age (ca. 300 BC–200 AD) with red painted design carrying pictorial patterns typical for the Ban Chiang ceramics. The surface material and colour of both shards was studied in detail using optical reflectance, FTIR spectroscopy and X-ray powder diffraction. Thin sections were used to determine the thickness of the red paint and the elemental composition of the surface using an electron microprobe. Chemical composition of sample 5412-S6E15 consists as oxides of elements mainly of SiO2 and Al2O3 (representing ca. 59 and 20 wt. %) and that of the red colour of the youngest sample 8027 consists mainly of SiO2, Al2O3 and Fe2O3 (representing ca. 52, 13 and 13 wt. %), the average composition adjacent to the red painted area has ca. 72 wt. % SiO2, ca. 10 wt. % Al2O3 and only 2 wt. % Fe2O3. X-ray powder diffraction, FTIR spectroscopy and optical reflectance measurements confirm hematite in the mineralogical composition of the red pigment of shard 8027. [ABSTRACT FROM AUTHOR]

Diffusible ions (Na+, K+, Mg2+, Ca2+, Cl–) are vital for healthy function of all cells, especially brain cells. Unfortunately, the diffusible nature of these ions renders them difficult to study with traditional microscopy in situ within ex vivo brain tissue sections. This mini-review examines the recent progress in the field, using direct elemental mapping techniques to study ion homeostasis during normal brain physiology and pathophysiology, through measurement of ion distribution and concentration in ex vivo brain tissue sections. The mini-review examines the advantages and limitations of specific techniques: proton induced X-ray emission (PIXE), X-ray fluorescence microscopy (XFM), secondary ion mass spectrometry (SIMS), laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), and the sample preparation requirements to study diffusible ions with these methods. [ABSTRACT FROM AUTHOR]

This study proposes a novel microprobing system for the surface detection of the side wall of micrometric scale workpieces based on the detection of the local surface interaction force. A spherical tip-shaped glass capillary tube with a micrometric scale diameter was employed as a micro-stylus. To obtain a low measuring force, the local attractive interaction force on the surface of the workpieces was detected by the vibrating micro-stylus and used as the probing trigger signal. The vibration in the main axis direction of the stylus allowed detection of the local surface interaction force in all directions around the stylus shaft. In this paper, the principle and configuration of the developed microprobe are mentioned. Probing detections around the stylus shaft were verified by the surface detection of a pin gauge. Repeatability of the probing by the developed microprobing system was evaluated. [ABSTRACT FROM AUTHOR]

We present two new experimental arrangements designed to study time dependent processes during the irradiation of semiconductor detectors using ion microbeams. The first one is based on an upgraded pulsed beam irradiation setup of the RBI heavy ion microprobe. Controlled time-sequences of sample irradiation and intermediate IBIC probing is used to study dynamics of degradation of charge transport in detectors at different time scales. The second experimental arrangement is a dual ion microbeam irradiation setup that can accept simultaneously the ion beams from the two accelerators. In that case the first ion microbeam may be used as a damaging beam while the second one could be used as a probing beam. Probing techniques that have been used to study induced changes in crystalline materials are based on low microbeam currents and include STIM channeling, IBIC and IL. [ABSTRACT FROM AUTHOR]

The relatively recent entry of field emission electron microprobes into the field of microanalysis provides another tool for the study of small features of interest (e.g., mineral and melt inclusions, ex-solution lamellae, grain boundary phases, high-pressure experimental charges). However, the critical limitation for accurate quantitative analysis of these submicrometer- to micrometer-sized features is the relationship between electron beam potential and electron scattering within the sample. To achieve submicrometer analytical volumes from which X-rays are generated, the beam accelerating voltage must be reduced from 15-20 to ≤ 10 kV (often 5 to 7 kV) to reduce the electron interaction volume from ~3 to ~0.5 µm in common geological materials. At these low voltages, critical Kα X-ray lines of transition elements such as Fe are no longer generated, so L X-ray lines must be used. However, applying the necessary matrix corrections to these L lines is complicated by bonding and chemical peak shifts for soft X-ray transitions such as those producing the FeLα X-ray line. It is therefore extremely challenging to produce accurate values for Fe concentration with this approach. Two solutions have been suggested, both with limitations. We introduce here a new, simple, and accurate solution to this problem, using the common mineral olivine as an example. We also introduce, for the first time, olivine results from a new analytical device, the Extended Range Soft X-ray Emission Spectrometer. [ABSTRACT FROM AUTHOR]

Pitting corrosion of reinforcing steel bar (rebar) imbedded in concrete by chloride ions can cause concrete degradation. It is thus necessary to develop methods to mitigate concrete corrosion which could include using a protective polymer rebar coating. Corrosion studies of polyvinyl butyral‐carbon black polymer‐coated rebar using soft X‐ray fluorescence (XRF) microprobe and micro‐X‐ray absorption near edge spectroscopy (μ‐XANES) are reported in this study. After removal of the polyvinyl butyral‐carbon black polymer coating, Fe Lα1, Mn Lα1, and O Kα1 XRF maps were collected as well as Fe and Mn L3‐edge μ‐XANES spectra from different regions across the whole rebar surface by collection of total electron yield (TEY) and partial XRF yield (PFY) spectra. The distribution of metallic Fe and Fe corrosion products was determined by analysis of the Fe XRF map. The μ‐XANES spectra indicated a higher fraction of Fe (III) phases on the corroded rebar surface, while Fe (II/III) phases were the major corrosion products beneath the surface region. In addition, Mn (II) and Mn (III) were determined as the valence states of the manganese corrosion products. [ABSTRACT FROM AUTHOR]

We present a new calibration for the determination of the iron oxidation state in silicate glasses by electron probe microanalysis (EPMA) with the “flank method.” This method is based on the changes in both intensity and wavelength of the FeLα and FeLβ X-ray emission lines with iron oxidation state. The flank method utilizes the maximum difference for the FeLα and FeLβ spectra observed at the peak flanks between different standard materials, which quantitatively correlates with the Fe2+ content. Provided that this correlation is calibrated on reference materials, the Fe2+/ΣFe ratio can be determined for samples with known total Fe content. Two synthetic Fe-rich ferric and ferrous garnet end-members, i.e., andradite and almandine, were used to identify the FeLα and FeLβ flank method measuring positions that were then applied to the measurement of a variety of silicate glasses with known Fe2+/ΣFe ratio (ranging from 0.2 to 1.0). The measured intensity ratio of FeLβ over FeLα at these flank positions (Lβ/Lα) is a linear function of the Fe2+content (in wt%). A single linear trend can be established for both garnets and silicate glasses with 4–18 wt% FeOT (total iron expressed as FeO). In glasses with up to 18 wt% FeOT and 15 wt% TiO2, no systematic compositional (matrix) effects were observed. A possible influence of Ti on the Fe2+ determination has only been observed in one high-Ti glass with ~25 wt% TiO2, a content that is not typical for natural terrestrial silicate melts. The accuracy of the Fe2+/ΣFe determination, which depends on both the Fe2+ content determined with the flank method and on the total Fe content, is estimated to be within ±0.1 for silicate glasses with FeOT > 5 wt% and within ±0.3 for silicate glasses with low FeOT ≤ 5 wt%. The application of the flank method on silicate glasses requires minimization of the EPMA beam damage that can be successfully achieved by continuous movement of the sample stage under the electron beam during analysis, e.g., with a speed of 2 μm/s. [ABSTRACT FROM AUTHOR]

Abstract A newly developed microprobe-based methodology (the Flank Method) for Fe3+/ΣFe quantification has been successfully applied to some natural garnets from the North Qilian eclogites by JEOL JXA-8100 microprobe at Peking University. The results demonstrated an obvious discrepancy in comparison with the outcomes by conventional stoichiometric calculations. This methodology allows to measure the Fe3+/ΣFe ratio and perform elemental analyses simultaneously in the same condition. Accurate in-situ measurement of Fe3+ content in garnet may bring certain impact on the garnet-based P-T estimation. According to the compositional zonation displayed in the studied eclogitic garnets from North Qilian, a prograde metamorphic PT path from 19.5 kbar, 520 °C to 22 kbar, 600 °C was reconstructed. More interestingly, the measured Fe3+/ΣFe ratios in garnets decreasing from core to rim may probably imply that the oxygen fugacity (fO 2) declines with the depth of the subduction zone. [ABSTRACT FROM AUTHOR]

With the rapid development of the integrated circuit (IC) industry, testing of IC chips is becoming more and more important. A chip probe final test is an important means of final chip testing, which makes use of contacts between probes and bumps on the chip for electrical connections of the test instrument and the chip, through which the electrical characteristics of the chip are tested one by one. The IC final test is directly completed on the entire packaging wafer before the packaging wafer is cut into single die. This complete testing of the whole wafer before dicing can greatly improve the efficiency of the final test. The precise alignment of probe and chip bumps is an important aspect of the final test process. In this paper, image processing is carried out based on the rectangular frame of the chip surface, for which the rectangular box image-processing algorithm is designed. The chip image showing the deflection angle is acquired, and the offset distance is calculated. The rectangular box algorithm based on the principle of the Hough transform detects the orientation that is used to determine the offset of the rectangular frame. The detection accuracy and efficiency of the algorithm is evaluated, and it is shown that the image-processing algorithm of the chip alignment is improved significantly. An efficient automatic probe final test of packaging wafers can finally be achieved. [ABSTRACT FROM PUBLISHER]

In order to investigate the electrical characteristics of microprobe in integrated circuit testing, a wafer probe admittance testing system with motion control and admittance measurement instruments was organized by using pogo microprobe whose impedance characteristics are automatically measured and analyzed. The probe’s admittance characteristics under different loading frequency were explored based on voltammetry. The results show that the probe was resistive when loading frequency was less than 100 kHz, and being inductive when the frequency was larger than 100 kHz. Furthermore, the probe’s admittance was the least when the frequency was between 200 and 400 kHz. Meanwhile, the conductivity of tipped needle is smaller than claw pin when the frequency is between 1 and 500 kHz, whereas the susceptance and resistance of tipped needle is larger than claw pin, which mainly due to the change of contact between probe and the solder. [ABSTRACT FROM PUBLISHER]

The temperature of a minute object is typically measured by an infrared thermograph, a precise and expensive device. This study presents an image–temperature model constructed by particle swarm optimization algorithm to estimate the temperature according to the color image data on object’s surface. The demonstrated case was a palladium alloy microprobe used in wafer testing. Two series of conduction experiments were implemented to imitate the probing condition of the microprobe in wafer testing. Collecting the images captured from a digital video camera and the temperatures measured by the infrared thermograph, the correlations between the color image data and their corresponding temperatures were investigated. An image–temperature model is further constructed by the particle swarm optimization algorithm based on the image components of the RGB and HSV models of the examined pixel. The model developed provides valuable references for making out the electrothermal effect of the palladium alloy microprobe used in wafer testing. [ABSTRACT FROM AUTHOR]

In this work the change in the surface topography of polydimethylsiloxane (PDMS) due to irradiation with 10.5 MeV N 4 + ion microbeam is investigated. Parallel stripes with different widths and different gaps between the stripes were irradiated. The heavy ion beam induced physical and chemical processes caused shrinkage of the irradiated structures. The degree of compaction, and its relation to the irradiation fluence and pattern was studied by means of atomic force microscopy (AFM). Exploiting the compaction effect, arrays of microlenses with different diameters were designed and fabricated in PDMS. We show that regular microlenses can be produced by the adjustment of their size and irradiation fluence. The focal length of the lenses can be tuned with the diameter of the lens and with the delivered ion fluence. [ABSTRACT FROM AUTHOR]

Given that secondary magnetite is common in serpentinites, it is clear that serpentinites are oxidized rocks. Questions remain, however, concerning the distribution of ferric iron among magnetite and serpentine minerals and the role of ferric iron-rich serpentine in the formation of secondary magnetite. Direct determination of ferric iron in serpentine is not possible using an electron microprobe. We show, however, that the stoichiometic effects of ferric iron substitutions are detectable, although not quantifiable, by microprobe. First, we demonstrate that for studies that provide both microprobe analyses of major elements of serpentine and Mössbauer analysis of ferric iron, substitution effects are obvious. Next, it is equally clear that the early veins forming at the onset of olivine hydration (type 1 veins) show no indication of the presence of ferric serpentine, although a small amount of ferric ‘brucite’ may occur. Finally, we show that secondary (type 2) veins, which form as the system becomes open to fluids in equilibrium with plagioclase or pyroxene, contain, in addition to significant alumina, stoichiometric indications of ferric iron substitution. The serpentine in these veins is magnesian, usually with Mg#s around 96–98. Thus, even if a significant proportion of this iron is ferric, it comprises only a small fraction of the total ferric iron budget of the rock. Given that reduced iron is known to be abundant in early-formed brucite and early-formed serpentine and given that brucite, in particular, is absent from evolved serpentine veins, we propose that most magnetite in serpentinites forms as a tertiary product via oxidation of brucite. [ABSTRACT FROM PUBLISHER]

This paper presents a standard-cell-based semiautomatic design methodology for a new conceptual countermeasure against electromagnetic (EM) analysis and fault-injection attacks. The countermeasure, called the EM attack sensor, utilizes LC oscillators that react to variations in the EM field around a cryptographic LSI caused by a microprobe brought near the LSI. A dual-coil sensor architecture with digital calibration based on lookup table programming can prevent various microprobe-based EM attacks that cannot be thwarted by conventional countermeasures. All components of the sensor core are semiautomatically designed by standard electronic design automation tools with a fully digital standard cell library and hence minimum design cost. This sensor can therefore be scaled together with the cryptographic LSI to be protected. The sensor prototype is designed based on the proposed methodology together with a 128-bit-key composite AES processor in 0.18- $$\upmu \hbox {m}$$ CMOS with overheads of only 2 % in area, 9 % in power, and 0.2 % in performance, respectively. The countermeasure has been validated against a variety of EM attack scenarios. In particular, some further experimental results are shown for a detailed discussion. [ABSTRACT FROM AUTHOR]

A motor-based microprobe is proposed using a tubular microengine powered by bio-assembled enzyme as catalyst and exploited for washing-free detection of DNA through motion readout. The microprobe is fabricated by assembling a catalase layer on the inner surface of poly(3,4-ethylenedioxythiophene)/Au (PEDOT/Au) microtube through DNA conjugate, which is responsible for the biocatalytic bubble propulsion. The sensing concept of the microprobe relies on the target-induced release of catalase through the DNA strand-replacement hybridization, which decreases the amount of enzyme assembled on microtube to slow down the movement of the microprobe. Therefore, the motion speed is negatively correlated with the target concentration. At the optimal conditions, the microprobe can conveniently distinguish the concentration of specific DNA in a range of 0.5–10 µM without any washing and separation step. This microprobe can be prepared in batch with good reproducibility and stability, and its motion speed can be conveniently visualized by optical microscope. The proposed motor-based microprobe and its dynamic sensing method provide a novel platform for the development of intelligent microprobe and clinical diagnostic strategy. [ABSTRACT FROM AUTHOR]