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[Analysis Case] Evaluation of Surface Deterioration of Polycarbonate

Structural analysis of resin surface degradation using TOF-SIMS.

Polycarbonate (PC) is a type of thermoplastic that has excellent transparency, impact resistance, and heat resistance. It has been reported that degradation occurs due to hydrolysis, leading to the generation of the raw material bisphenol A (BPA). Particularly in solar panels, it is important to understand how the surface of the material changes under UV (ultraviolet) irradiation. Below, we present a case study that evaluated the degree of degradation of the PC surface due to UV irradiation using TOF-SIMS.

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[Analysis Case] Indoor Air Quality Measurement Case

It is possible to analyze aldehydes and VOCs (volatile organic compounds) in indoor air.

Formaldehyde and volatile organic compounds (VOCs: Volatile Organic Compounds, such as toluene, xylene, and para-dichlorobenzene) emitted from building materials, adhesives, and preservatives are considered to be causes of sick house syndrome and sick school syndrome. This report introduces a case study analyzing the concentrations of formaldehyde and toluene in indoor air sampled using passive methods.

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[Analysis Case] High-Precision Quantification of the sp2/(sp2+sp3) Ratio of DLC Films

High-precision analysis using XAFS

DLC (diamond-like carbon) films, which are widely used as coating materials in various fields, are composed of a mixture of carbon elements with sp3 hybrid orbitals corresponding to a diamond structure and carbon elements with sp2 hybrid orbitals corresponding to a graphite structure when viewed from a microscopic perspective. One indicator that determines the properties of DLC films is the sp2/(sp2+sp3) ratio. High-precision quantification of the sp2/(sp2+sp3) ratio in DLC films is possible using XAFS.

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Precautions for Low-Temperature Photoluminescence Measurement

Photoluminescence method

- Photoluminescence measurement (PL measurement) can be conducted not only at room temperature but also by placing the sample in a cryostat for low-temperature measurements. Low-temperature measurements tend to show an increase in peak intensity and a decrease in peak full width at half maximum compared to room temperature measurements, which may provide insights into various energy levels. - Below, we will explain the precautions for low-temperature measurements and the differences in spectral shapes between room temperature and low-temperature measurements.

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[Analysis Case] Evaluation of GaN Crystal Growth by XRD and EBSD

Cross-sectional mapping allows for the evaluation of the crystal growth of GaN.

Gallium nitride (GaN) is used as a material for LEDs and power devices due to its high thermal conductivity and high breakdown voltage characteristics. In the manufacturing process of these products, it is essential to produce high-quality GaN crystals without crystal defects that can affect device characteristics. This document presents a case study evaluating the crystal state of samples in which c-GaN crystals were grown at high speed on c-plane GaN substrates (c-GaN substrates).

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Valence evaluation of metal oxides by chemical shift

XPS: X-ray Photoelectron Spectroscopy

In XPS analysis, the binding state evaluation of the material surface is conducted by observing the energy of photoelectrons obtained through X-ray irradiation. It allows for the assessment of whether metal elements are in an oxidized state, and for elements with significant energy shifts (chemical shifts) due to oxidation, it also enables the evaluation of the presence and proportion of multiple valences. Below are the main metal elements and oxides for which multiple valence evaluations are possible.

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Evaluation of the orientation angle of organic film materials

XAFS: X-ray Absorption Fine Structure

Self-assembled monolayers (SAMs), which are oriented organic films, have their functions and properties, such as surface wettability and adsorption, altered by orientation and orientation angle. Using XAFS with synchrotron radiation, it is possible to evaluate the orientation and orientation angle of organic film materials by analyzing the X-ray incidence angle dependence of peak intensity.

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[Analysis Case] Evaluation of Layer Structure of Organic EL Devices

Preventing oxidation degradation during cutting processing under N2 atmosphere.

Organic EL devices are prone to degradation in the atmosphere, so processing under an N2 atmosphere is necessary. We present the measurement results of Alq3 for organic EL devices that were machined in an N2 atmosphere and left in the atmosphere for 30 minutes, compared to those that were not exposed to the atmosphere. When left in the atmosphere, there is a strong tendency for peaks associated with oxygen to appear in Alq3. In the N2 atmosphere, there is a strong tendency for the parent ions of Alq3 to be observed. By avoiding exposure to the atmosphere, results closer to the true state can be obtained.

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[Analysis Case] Evaluation of the Diffusion Layer of SiCMOSFET Using SCM and SMM

You can evaluate the p/n polarity and carrier concentration distribution of the SiC device's diffusion layer.

A cross-section of the SiC Planer Power MOSFET was fabricated, and the p/n polarity distribution of the diffusion layer was evaluated using SCM (Scanning Capacitance Microscopy), while the carrier concentration distribution was qualitatively assessed using SMM (Scanning Microwave Microscopy). From both sets of data, it was found that a p-type Body layer is formed in a two-layer structure around the n+ type Source layer, and that a Channel Epitaxial layer exists directly beneath the gate. At the edge of the Channel Epitaxial layer, a partial decrease in concentration was observed in the Source layer.

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[Analysis Case] Evaluation of Additives in Polymer Materials

Qualitative analysis of components by LC/MS.

Many additives, including plasticizers, are used in polymer materials such as resin products. We present a case study on the qualitative analysis of additives contained in commercially available PVC resin. The components eluted by immersion in an organic solvent were qualitatively analyzed using LC/MS. As a result, components estimated to be DEHP (DOP) as a plasticizer and epoxy fat (plasticizer/stabilizer) were detected. By using standard samples, it is also possible to quantify each detected additive component.

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Concentration analysis of volatile components using a sample concentration needle.

GC/MS: Gas Chromatography-Mass Spectrometry

The sample concentration needle is a device that concentrates volatile components by sucking them from vials or sampling bags and adsorbing the volatile components passing through the needle onto an adsorbent medium, which is then introduced into GC/MS. There are different adsorbent media available, such as "for organic solvents," "for fatty acids," and "for amines," which are used depending on the target components. In the headspace method used for the analysis of volatile components, it is common to heat the sample to obtain sensitivity; however, in analyses using the sample concentration needle, heating is not necessary, allowing only the volatile components to be supplied for GC/MS analysis at room temperature.

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[Analysis Case] Low-Temperature PL Spectrum of Si After Ion Implantation Annealing Treatment

It is possible to confirm the recovery of crystallinity due to irradiation defects and annealing.

In the fabrication of Si-based semiconductor devices, various processes such as ion implantation and annealing are performed. It is considered important to confirm the degree of irradiation defects and the extent of crystallinity recovery before and after these processes in order to control the manufacturing process. Photoluminescence (PL) measurements at low temperatures are one effective means of investigating these aspects. An example of PL measurements of samples that underwent ion implantation on a Si substrate followed by annealing treatment is presented.

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[Analysis Case] Evaluation of Composition Distribution of Capsule-type Drugs

Imaging evaluation is possible from the overall view to local distribution.

TOF-SIMS allows mass imaging analysis of samples ranging from micrometers to centimeters in size. We conducted mass imaging analysis using TOF-SIMS on the cross-section of a capsule-type drug. We performed cross-section processing and present imaging examples focusing on the entire drug (approximately 7mm x 20mm) and a single granule inside it (approximately 500μm in diameter).

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Evaluation of organic contamination using a wafer analyzer with GC-MS.

GC/MS: Gas Chromatography-Mass Spectrometry

The WA (Wafer Analyzer) is a device that heats wafers with a diameter of φ76 to 300mm to elevate their temperature, gasifying organic contaminants adhered to the wafer surface and trapping them in a collection tube. As a result, it can concentrate compounds such as phthalate esters and cyclic siloxanes, which are considered causes of device characteristic impacts and manufacturing troubles, allowing for high-sensitivity measurement using GC/MS. Quantification using hexadecane is also possible. - Evaluation of organic contaminants on one side of the wafer is possible. - Detection of easily volatile components is possible since vacuum pumping is not required. - Organic components can be detected with high sensitivity (for 300mm wafers, on the order of 0.01ng/cm²). - Quantification using hexadecane conversion is possible.

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[Analysis Case] Image Analysis of Micro Beer

It is possible to evaluate the distribution of micro-regions.

With the miniaturization of circuits, the design and development of micro vias for interlayer connections require an understanding of the quality of filling. TOF-SIMS is an effective method for evaluating the results, as it can simultaneously perform elemental analysis and analyze molecular information of organic and inorganic substances, as well as enable image analysis. This document presents a case study analyzing a sample with Cu filled in vias of approximately 0.5μm in diameter on a Si substrate. The analysis of positive ion results confirmed the distribution of Cu and Si. Measurement method: TOF-SIMS Product fields: LSI, memory, electronic components Analysis objectives: Composition distribution evaluation, failure analysis, defect analysis For more details, please download the document or contact us.

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[Analysis Case] Qualitative Analysis of Organometallic Complexes under Atmosphere Control

Mass spectrometry using TOF-SIMS is possible under conditions that are not affected by oxidation.

Titanium tetraalkoxide is an essential reagent for the Katsuki-Sharpless asymmetric epoxidation and is affected by oxidation in the atmosphere. In this case, we present an investigation using TOF-SIMS on how titanium tetraalkoxide (titanium tetra-isopropoxide) changes under controlled atmosphere and after exposure to air. In MST, the evaluation of the complex can be performed without the influence of atmospheric oxidation due to atmosphere control. Measurement method: TOF-SIMS Product fields: Biotechnology, Pharmaceuticals, Cosmetics, Daily necessities Analysis purpose: Deterioration investigation, Reliability assessment For more details, please download the materials or contact us.

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Evaluation of metal contamination on the Si wafer surface

ICP-MS: Inductively Coupled Plasma Mass Spectrometry

The purpose of evaluating metal contamination on the surface of Si wafers using ICP-MS includes not only the contamination assessment of the Si wafers themselves but also the evaluation of contamination within semiconductor devices and the assessment of the working environment due to Si wafer exposure. Therefore, the analysis of the Si wafer surface is conducted for various purposes. ICP-MS analysis can sensitively obtain the amount of metal contamination on the surface of Si wafers, and it is also possible to specify the evaluation area according to the purpose.

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[Analysis Case] Local Structure Analysis of Aluminum Oxide Thin Films

It is possible to capture changes in the fine structure of the film due to differences in film formation conditions.

Aluminum oxide is used in various industrial machinery and manufacturing equipment parts due to its excellent wear resistance and heat resistance. Additionally, its chemical stability and high insulation properties make its thin films suitable for applications such as catalyst supports and insulating layers in magnetic tunnel junctions. The evaluation of the fine structure of aluminum oxide films, which can take on amorphous structures or various crystalline structures depending on the film formation conditions, is effectively conducted using XAFS. This document presents a case study of the quantitative separation of coordination structures (AlO4, AlO6) in amorphous aluminum oxide thin films.

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[Analysis Case] Evaluation of Nitrogen Substitution Positions in Nitrogen-Doped Carbon Materials

It is possible to identify the substitution position of nitrogen and achieve quantitative separation using chemical shifts.

Carbon materials with nitrogen (N) atoms introduced as substitutes for platinum (Pt), the electrode catalyst in fuel cells, are attracting attention, and the catalytic activity is significantly related to the substitution positions of N within the carbon materials. XPS analysis allows for the evaluation of the N1s spectrum, where chemical shifts occur due to differences in bonding states and substitution positions of N, enabling the identification and quantitative separation of which C positions have been substituted by N.

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[Analysis Case] Evaluation of Si-based IGBT Chip Cross-section by Low-Temperature Micro Photoluminescence Analysis

It is possible to confirm the influence of the lifetime killer from the cross-sectional direction.

IGBT (Insulated Gate Bipolar Transistor) is used in various products as a power semiconductor module, ranging from home appliances to industrial equipment. Lifetime control is implemented for performance improvement in IGBTs, but this control is achieved by creating defects (lifetime killers) in the drift layer. By conducting low-temperature micro-PL analysis from the cross-section, it is possible to gain insights into lifetime killers.

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[Analysis Case] Evaluation of the Skin Permeability of Melbromin

Information about valence bands and intra-gap levels can be obtained by element.

Soft X-ray emission spectroscopy (SXES) using synchrotron radiation is widely used as a method to evaluate the electronic states of materials because it allows for the direct acquisition of the partial density of states (pDOS) near the Fermi level for each element constituting the material. Furthermore, the characteristics of this method include: 1. Information from the bulk can be obtained, 2. It can be evaluated without being affected by charging effects even for insulators, and 3. It has a low detection limit (less than 1 atomic %), making it particularly effective for evaluating materials containing light elements (such as B, C, N, O). In this document, we will introduce the SXES spectrum of a GaN substrate as a measurement example.

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[Analysis Case] Stress Evaluation by Raman Mapping

It is possible to confirm the stress distribution in the sample cross-section.

The peaks in the Raman spectrum of single crystal Si shift to higher wavenumbers when compressive stress is applied to the sample and shift to lower wavenumbers when tensile stress is applied. This allows us to gain insights into the stress in Si. An example is shown where the distribution of stress in the cross-section of an IGBT (Insulated Gate Bipolar Transistor) was confirmed using Raman mapping.

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[Analysis Case] Evaluation of Diffusion Layer Shape of Image Sensors Using SCM

We provide consistent support from sample disassembly to measurement.

This document presents case studies evaluating the diffusion layer of image sensors in smartphones. Using a scanning capacitance microscope (SCM) capable of determining the p/n type of semiconductors, we assessed the distribution of the diffusion layer. By combining the results from cross-sectional and planar SCM, we obtained complementary and extensive information. SCM is one of the effective tools for evaluating the quality of image sensor diffusion layers and for failure analysis.

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[Analysis Case] Observation of Crystal Grains on Cu Surface Using Scanning Ion Microscopy

It is possible to obtain insights into the size and distribution of crystal grains in metallic polycrystals.

The Scanning Ion Microscope (SIM) is a method that irradiates a solid sample with an ion beam and detects the secondary electrons generated. Since secondary electrons produce contrast according to the crystal orientation of each grain, it is possible to easily obtain insights into the size and distribution of crystal grains in polycrystalline metals such as Cu and Al using SIM. This document presents an example of measurements where the surface of Cu was observed using SIM.

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[Analysis Case] Imaging Analysis of Pesticide Active Ingredients in Formulations

You can visualize the distribution of pesticide active ingredients and inorganic components in the formulation.

TOF-SIMS can identify components from the mass of molecular ions, allowing for imaging analysis without the need for labels such as fluorescent substances. Additionally, by measuring not only organic components but also inorganic components, it is possible to image not only the active ingredients of pesticides but also the minerals mixed into the formulations. In this study, we visualized the active ingredients of pesticides and inorganic components in two types of formulations with different mixing ratios. In formulation A (high mixing ratio), the active ingredient was widely distributed throughout the formulation, whereas in formulation B (low mixing ratio), the active ingredient was localized.

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[Analysis Case] Evaluation of Skin Permeability Using Three-Dimensional Cultured Human Skin

It is possible to conduct various evaluations of cultured human skin (morphological observation, distribution assessment of components, quantitative analysis).

■Morphological Observation The morphology of the tissue can be confirmed by staining frozen sections (e.g., HE staining, Nile blue staining). ■Fluorescence Microscopy Observation If the transmitted components have fluorescence, the fluorescent components can also be observed using a fluorescence microscope. ■Mass Microscopy Observation The distribution of components can be evaluated. Temporal changes can also be confirmed with sections taken at different times (TOF-SIMS). ■Quantitative Analysis Temporal changes in the amount of fluorescent components in the skin can also be confirmed (e.g., LC/MS/MS, fluorescence detectors, etc.).

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Analysis of product characteristics of apple juice using LC/MS multivariate analysis.

We evaluate product characteristics and degradation components through inter-sample comparison using multivariate analysis.

As part of quality management, when you want to investigate components characteristic of the origin and variety, as well as components that cause defects between lots, comparisons between multiple samples are necessary. By statistically processing the data obtained from LC/MS measurements using multivariate analysis, it is possible to identify components that are characteristic of the samples among many components. In this case, we will introduce an example of investigating characteristic components among three apple juice products of different apple varieties using principal component analysis (PCA), which is one type of multivariate analysis.

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Surface shape evaluation using a laser microscope.

Laser microscope

This introduces the evaluation of surface shape using a laser microscope.

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High-sensitivity NMR analysis using ultra-low temperature probes

NMR analysis of trace components is possible.

Nuclear Magnetic Resonance Spectroscopy (NMR) is an analytical method that can obtain various information about molecular structure, intermolecular interactions, and molecular mobility, targeting various compounds including organic substances. This document presents examples of measurements conducted with a super low-temperature probe, which achieved higher sensitivity compared to a general-purpose room temperature probe.

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Multiple SNP analyses using mass spectrometry.

The mass array method allows for the simultaneous analysis of multiple SNPs (single nucleotide polymorphisms).

This method is a gene analysis technique that utilizes mass spectrometry with MALDI-TOF-MS, allowing for the analysis of multiple SNP sites in a single measurement. Up to 40 SNPs can be measured simultaneously across 190 samples. The overall analysis follows the flow outlined below. Primers designed to amplify the target SNP regions without overlapping mass peaks, along with primers designed to extend only one base at each SNP site, are used to create mass differences in the DNA fragments, from which the bases are determined based on the detected mass peaks.

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