一般財団法人材料科学技術振興財団　MST Product Lineup

By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. In this case, we present data from high-resolution (HR)-TEM observations of the MTJ: magnetic tunnel junction part, extracted from a commercially available hard disk. Thus, it is possible to clearly observe the structure even in multilayer structures of ultra-thin metal films.

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By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. This case presents data from high-resolution (HR)-TEM observation and EDX elemental distribution analysis of commercially available MPU transistor components. Even for fine multilayer structures like FinFETs, it is possible to clearly observe the structure and elemental distribution of the devices using a Cs-corrected TEM.

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By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. This case presents data from high-resolution (HR)-STEM observation and EDX elemental distribution analysis of the light-absorbing layer of CIGS thin-film solar cells. In CIGS, which has a polycrystalline structure composed of four elements, atomic resolution EDX analysis was performed, visually revealing the distribution of atoms.

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The OPA post-column method is a technique that reacts amino acids with the fluorescent reagent OPA after separation in a column and detects the fluorescence (Figures 1, 2). This method allows for high-sensitivity analysis compared to the ninhydrin method. The fluorescent reagent OPA selectively reacts with primary amines, making it less susceptible to interference from contaminants and enabling highly selective analysis. Proline is a secondary amino acid, but it can be converted into a primary amine by adding sodium hypochlorite to the reaction solution, allowing for measurement. This document presents a case study of simultaneous measurement of 17 amino acid components, including proline (Figure 3).

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This document presents a case study of the quantitative analysis of free amino acids contained in alcoholic beverages using the OPA post-column method. It was found that sake, a brewed alcoholic beverage, contains a rich and well-balanced variety of free amino acids, including alanine and arginine. Furthermore, when comparing three sake products, differences were observed in both the content and balance of free amino acids. Although draft beer is also a brewed beverage like sake, it showed a lower content of free amino acids compared to sake. On the other hand, distilled spirits such as whiskey and awamori contained almost none.

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The vitamin C contained in food refers to the total amount of reduced L-ascorbic acid and oxidized dehydroascorbic acid. Its applications include not only nutritional enhancement but also use as an antioxidant. When measuring vitamin C using HPLC, it is common to convert the oxidized form after noting that dehydroascorbic acid has no UV absorption, and then derivatize it for measurement. By quantifying dehydroascorbic acid using LC/MS/MS, it becomes possible to simplify the pretreatment and analyze with high sensitivity.

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In recent years, with the increase in health consciousness, various health foods have been attracting attention. One of these, Du Zhong tea, is suitable for individuals with high blood pressure and is designated as a Food for Specified Health Uses (Tokubetsu Hōshō). In this case study, Du Zhong tea was analyzed using LC/MS/MS, and five polyphenols were detected: geniposidic acid, chlorogenic acid, asperuloside, p-coumaric acid, and quercetin. Among these components, geniposidic acid, one of the glycosides from Du Zhong leaves, serves as a benchmark for the effective ingredient of Foods for Specified Health Uses.

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Ergothioneine is an amino acid homolog discovered in ergot, known for its strong antioxidant properties and anti-photoaging effects, and research and development are ongoing in the fields of medicine and beauty. Since humans cannot produce ergothioneine in their bodies, they obtain it from sources rich in it, such as certain mushrooms. An analysis of eight types of mushrooms using LC/MS/MS revealed that ergothioneine was detected in all of them. Quantitative analysis was conducted on three types of mushrooms from the Pleurotaceae family, which are said to have high ergothioneine content.

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When conducting elemental analysis, it is possible to establish an efficient evaluation plan by first using XRF analysis to non-destructively examine the elements contained in the target before moving on to detailed analysis. In this case, we present data from XRF analysis conducted on blades for metal cutting. By performing surface analysis over a wide range on the order of millimeters, we roughly examined the distribution of metallic elements in the material and estimated the metal composition by calculating the elemental composition from the XRF point analysis results of characteristic areas. Measurement method: XRF Product field: Manufacturing equipment, parts, daily necessities Analysis purpose: Composition evaluation, identification, composition distribution evaluation, failure analysis, defect analysis For more details, please download the materials or contact us.

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Acrylic resin has superior processability, transmittance, and safety compared to silicate glass, making it widely used as organic glass for windows in aircraft and automobiles, optical instruments such as lenses and prisms, medical materials, daily necessities, and crafts. Mass spectra of representative standard acrylic reagents were obtained using TOF-SIMS. In MST, by comparing the mass spectrum of the analyte with that of the standard reagent, it is possible to estimate the acrylic resin from the detected fragment ions.

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SR measurement involves diagonally polishing the sample and moving two probes in contact with the sample surface while measuring the electrical resistance directly beneath. The depth from the sample surface at a certain measurement point is determined by the product of the value of Sinθ (bevel angle) when the angle of diagonal polishing of the sample is θ and the distance from the bevel edge to that measurement point. The distance from the bevel edge is calculated as [X-step] × [number of measurement points].

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1. Measure the spreading resistance (Ω) directly beneath the surface of the sample that has been polished at an angle by contacting two probes. 2. Create a calibration curve from the measurements of the standard sample and use it to convert the resistance to resistivity (Ω·cm). Additionally, perform distribution corrections as needed through volume correction. *) The calibration curve varies depending on the conductivity type (p-type/n-type) and the surface orientation. 3. Use the relationship between resistivity and carrier concentration*) to calculate the carrier concentration (/cm³).

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Imaging SIMS is effective for obtaining spatial distribution information of hydrogen and impurities at ppm levels. By using a RAE (Resistive Anode Encoder) detector for projection-type imaging SIMS, it is possible to obtain distribution images with a larger diameter and deeper regions compared to the commonly used scanning methods in imaging analysis.

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Nonylphenol ethoxylate (NPnEO) is known to produce nonylphenol (NP) as a degradation product. NP is considered an endocrine disruptor, and due to concerns about its impact on living organisms, it has been added to the environmental standards related to the conservation of aquatic organisms within the environmental standards concerning the preservation of living environments affected by water pollution, with a standard value established (August 22, 2012). To understand the trends of NP, for which a standard value has been set, it is necessary to also monitor the trends of its precursor, NPnEO, leading to an increased demand for analysis.

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As electronic devices are increasingly used in various everyday locations, ensuring the reliability of products has become important. Since it is possible for the copper used in the wiring of printed circuit boards to migrate and cause defects in high temperature and high humidity environments, it is crucial to evaluate the components that promote migration. This case study introduces an example of quantitative analysis of cation components eluted from printed circuit boards using ion chromatography (IC). Thus, IC is an effective method for evaluating the corrosion components on the surface of solid samples.

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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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In controlling properties such as adhesion and wettability of polymer films, it is very important to quantitatively evaluate the polar functional groups (alcohol groups) present on the surface. XPS is optimal for quantitative evaluation; however, it is difficult to separate and quantify the adjacent oxidation state (C-O-C) and hydroxyl state (C-OH). In MST, after selectively reacting only the alcohol groups using a chemical modification method on polyvinyl alcohol (PVA), it is possible to quantify them using XPS. We present a case where the alcohol groups in PVA were chemically modified and evaluated using trifluoroacetic anhydride (TFAA). Measurement method: XPS, chemical modification Product fields: Electronic components, daily necessities Analysis purpose: Composition evaluation, identification, chemical bonding state evaluation For more details, please download the materials or contact us.

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Tetramethylammonium hydroxide (TMAH) is used as a developing solution and etching solution in semiconductors. When measuring the concentration of TMAH solution used in Si etching solutions, the large amount of dissolved Si can become an impurity and affect the measurement results. However, evaluation using the IC (ion chromatography) method allows for quantitative analysis of TMAH concentration without being influenced by Si.

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The state of the water-repellent surface in water-repellent treatment differs based on whether fluorine-based compounds are distributed in an island-like manner or uniformly. Therefore, we conducted observations of the distribution of fluorine-based compounds using TOF-SIMS. As a result, it was found that they are distributed unevenly. Additionally, by performing qualitative analysis in a 1μm square area, it was determined that the fluorine-based film is Krytox. Measurement method: TOF-SIMS Product field: Electronic components and daily necessities Analysis purpose: Composition evaluation, identification, composition distribution evaluation For more details, please download the materials or contact us.

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Organic acids such as citric acid and malic acid are widely used in various fields, including the semiconductor industry as additives in etching and plating solutions, as well as in food as sour agents and emulsifying stabilizers. In particular, the concentration of organic acids in plating solutions changes over time during use, and this balance affects the quality of the plating, making precise control important. Here, we will introduce a case study of organic acid analysis using IC (ion chromatography).

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Among the environmental standards related to the preservation of living environments concerning water quality pollution, 2,4-dichlorophenol has been newly added as a key monitoring item for the environmental standards related to the conservation of aquatic organisms (March 27, 2013). 2,4-dichlorophenol is considered to potentially hinder the habitat or growth of aquatic organisms through environmental pollution, with guideline values set between 0.003 and 0.03 mg/L depending on the water area and type. MST offers a comprehensive service that includes the lending of specialized containers and measurement.

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It has been announced that 4-t-octylphenol will be newly added as a monitoring item in the environmental standards related to the conservation of aquatic organisms, among the environmental standards concerning the preservation of living environments affected by water quality pollution (March 27, 2013). 4-t-octylphenol is considered to potentially hinder the habitat or growth of aquatic organisms through environmental pollution, and the guideline values are set between 0.0004 to 0.004 mg/L depending on the water area and type. MST provides a comprehensive service that includes the lending of specialized containers and measurement.

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In 2002, it was announced that acrylamide, which may have carcinogenic properties, is generated when foods high in carbohydrates are heated at temperatures above 120°C (Figure 1), attracting attention. According to the Ministry of Agriculture, Forestry and Fisheries (MAFF) website, acrylamide is found in many foods, including fried potato snacks, toast, and coffee. At MST, we participate in the proficiency testing FAPAS and confirm that the absolute value of the z-score is 2 or below (satisfactory), allowing us to accurately quantify acrylamide in food using LC/MS/MS.

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Polycarbonate (PC) is a type of thermoplastic that has excellent transparency, impact resistance, and heat resistance, and is widely used as a material for solar panels, eyeglass lenses, CDs, automotive parts, and medical devices. In this study, TOF-SIMS analysis was conducted using GCIB (Ar cluster) with a sputter ion beam to evaluate the degradation layer on the surface of PC. *Note: GCIB stands for Gas Cluster Ion Beam.*

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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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Linear alkylbenzene sulfonic acid and its salts (LAS) are considered substances of concern due to their potential impact on living organisms. Therefore, they have been added to the environmental standards related to the conservation of aquatic organisms within the environmental standards concerning the preservation of living environments affected by water pollution, and a standard value has been established (March 27, 2013). Since approximately 90% of the usage of LAS is for household detergents, measurements were conducted on existing household detergents and household wastewater, and a comparison of the distribution of LAS alkyl chain lengths (C10 to C14) was performed.

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Geosmin and 2-methylisoborneol (2-MIB) are produced by cyanobacteria or actinomycetes and are considered substances that cause odor and taste disturbances in drinking water sourced from surface water such as dams, lakes, and rivers, as well as being known as substances that cause musty odors. This case presents the results of measuring geosmin and 2-MIB contained in water. Detection at ppt (ng/L) levels is possible using GC/MS.

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Water-soluble vitamins can be divided into about 10 types based on their functions in the body. For example, vitamin B1 consists of multiple components (thiamine, hydroxymethylthiazole, and its derivatives) that have the same function, and the total amount of these components determines the content. In this case, a multivitamin supplement was measured using LC/MS/MS, and qualitative analysis was conducted for each component of five types of water-soluble vitamins. By performing simultaneous analysis, it is possible to efficiently confirm the presence or absence of the target components. Analysis of other water-soluble vitamins is also possible, so please feel free to inquire.

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Foods such as pork and eggs are rich in vitamin B1 (thiamine, HET) and vitamin B2 (riboflavin). These are often present as derivatives such as phosphate esters. The content of vitamin B1 and vitamin B2 can be quantified by performing enzymatic treatment as a pretreatment to convert them to their free forms, followed by analysis using HPLC with a fluorescence detector. Although vitamin B1 itself is not fluorescent, it is possible to detect fluorescence by reacting it with a red blood salt alkaline solution in a post-column method, converting it to the oxidized form of thiocrome.

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As exemplified by the separators used in lithium-ion secondary batteries, the microstructure of materials, such as porosity and shape, significantly influences the characteristics and functions of products. When materials have a low softening point, such as resins or polypropylene (PP), they may be damaged by electron beam irradiation during observation, leading to changes in their original structure. We will present a case where ultra-low acceleration SEM observation at an acceleration voltage of 0.1 kV was used to suppress alteration and evaluate the surface morphology of the sample in detail.

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The electrolyte of lithium-ion secondary batteries is known to decompose and gasify due to repeated charging and discharging. By using GC-TCD and GC/MS, the decomposed gas components can be detected with high sensitivity. GC-TCD can analyze the composition ratios of eight components (H2, O2, N2, CO, CH4, CO2, C2H4, C2H6), while GC/MS can qualitatively analyze various decomposition products. We also support gas analysis in not only laminate-type cells but also coin-type and prismatic cells, as well as cells using ionic liquids.

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Organic contamination during the manufacturing process significantly affects product performance. In the analysis of organic substances in liquid samples, such as rinse solutions in the cleaning process, evaluations can be conducted using Total Organic Carbon (TOC) analyzers and Liquid Chromatography-Tandem Mass Spectrometry (LC/MS/MS). Here, we present an example of evaluation using TOC and LC/MS/MS for NPnEO (Nonylphenol Ethoxylate), one of the industrial surfactants.

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When an unusual odor arises from food, it is important to identify the components that cause it. In foods containing various odor components, trace elements can significantly contribute to the overall smell, and the balance of component quantities can lead to substantial differences in odor. Therefore, it is necessary to narrow down the candidate components by comparing the odorous product with a normal product. Here, we present a case study that compares new olive oil and old olive oil using GC/MS to analyze the odor components responsible for the unusual smell.

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Using a two-stage heating method with thermal decomposition GC/MS, we analyzed the material of the sealing agent around the display of commercially available smartphones. By heating the sample at a low temperature (250°C) and measuring the gas components generated using GC/MS, we can detect residual monomers and low molecular weight additives (polymerization initiators, antioxidants). Subsequently, by heating at a high temperature (550°C), we can decompose the polymers and estimate their constituent components. This revealed that the sealing agent is made of a UV-curable material.

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In semiconductor device manufacturing, it is necessary to investigate what causes thin deposits that lead to defects in order to examine contamination processes. An analysis was conducted using TOF-SIMS on the deposits for which carbon was detected by EDX and quantified by XPS. When compared to the gloves used for standard samples in each process, similar trends were observed with gloves A and B. Furthermore, verification was performed by adhering the standard sample gloves to silicon wafers. As a result, it was found that they were similar to glove A. Adhering standard samples to silicon wafers for verification is an effective method.

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The detection sensitivity in SIMS analysis depends on the amount of sputtered sample per unit time. Depending on the element, significantly improved sensitivity can be achieved by limiting the impurities to one element, allowing evaluation down to ppt (parts per trillion) levels of less than 5E13 atoms/cm3, which is effective for assessing low-concentration impurities in IGBT devices and high-purity wafers. This document presents examples of ultra-high sensitivity evaluations of low-concentration impurities in silicon.

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Food wrap films may use additives to ensure stability against thermal exposure during the manufacturing process and to impart plasticity. These additives are required to remain stable under cooking conditions without changing. In this case, we present the results of an investigation using TOF-SIMS to examine whether the state of one of the additives, Irgafos168, changes (bleeds out) before and after heating. *GCIB: Gas Cluster Ion Beam

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Regarding foreign substance analysis, it has traditionally been difficult to analyze using microscopic FT-IR analysis or Raman analysis due to the influence of the substrate. However, with the introduction of micro-sampling tools, it has become possible to reduce that influence. We will introduce examples of analysis for two types of foreign substances.

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Copper (Cu), used as wiring material, forms an oxide film in the air. Here, we present a case study evaluating the differences in film thickness due to variations in storage environments. Copper (Cu) wrapped in aluminum foil and copper (Cu) stored in a plastic bag were each kept for 40 days, and the oxide film thickness was measured using TOF-SIMS. Additionally, a continuous investigation over approximately 20 days confirmed reproducibility. TOF-SIMS allows for depth profiling analysis of inorganic materials such as oxides and metals. Measurement method: TOF-SIMS Product fields: Displays, LSI, Memory, Electronic components Analysis purpose: Evaluation of chemical bonding states For more details, please download the materials or contact us.

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The surface of copper (Cu) metal exposed to the atmosphere is covered with a natural oxide film, and it is known that such copper surfaces can be broadly classified into the states of "Cu," "Cu2O," "CuO," and "Cu(OH)2." By conducting depth profile analysis of commercially available standard powders of "Cu2O," "CuO," and "Cu(OH)2" using TOF-SIMS, it was found that it is possible to obtain characteristic molecular ions corresponding to each state. Using these molecular ions, it became possible to evaluate the depth profile of the natural oxide film on the surface of metallic Cu. Measurement method: TOF-SIMS. Product fields: Display, LSI, Memory, Electronic components. Analysis purpose: Evaluation of chemical bonding states. For more details, please download the materials or contact us.

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By irradiating the surface of polymer materials with ions, changes in surface properties occur. Utilizing these changes, research is being conducted in a wide range of fields, including the development of functional materials. Evaluating the changes that occur in the surface state after ion irradiation is important for efficient research and development. In TOF-SIMS analysis, using a GCIB (Gas Cluster Ion Beam) for the sputtering ion beam makes it possible to evaluate the composition and thickness of the damage layer caused by ion irradiation on the surface of polymer materials.

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The presence of silanol groups (Si-OH) on the surfaces of glass and wafers affects properties such as hydrophobicity and hydrophilicity. Therefore, it is likely to influence subsequent surface treatments, necessitating control. We will introduce a case where the quantification of silanol groups was performed using TOF-SIMS. To conduct the evaluation, calibration curves were created using several types of samples with different concentrations. In the measurement examples, the silanol groups on the surfaces of samples with different materials and conditions were compared. Measurement method: TOF-SIMS Product fields: LSI, memory, electronic components Analysis purpose: Composition evaluation and identification For more details, please download the materials or contact us.

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TOF-SIMS allows for the acquisition of mass spectra in the depth direction, enabling the analysis of components in very thin layers through qualitative assessment of each layer. In this case, we analyzed a hard disk in the depth direction. As a result, it was found that the diamond-like carbon (DLC) layer formed on the surface has a two-layer structure, with a nitrogen-containing C layer on the surface side and a layer consisting solely of C on the deeper side. This method can also be applied to the depth analysis of graphene films. Measurement method: TOF-SIMS Product fields: Electronic components, manufacturing equipment, parts Analysis objectives: Composition evaluation, identification, composition distribution evaluation For more details, please download the materials or contact us.

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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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In AES analysis, it is possible to evaluate the elemental composition of the surface of minute foreign substances, making it useful for foreign substance analysis in small areas. However, due to the effects of damage from electron beams and other sources, there is a possibility that the foreign substances may change or disappear. Particularly when halogen elements are involved, the impact can be significant, and caution is required. An example of a case where a foreign substance disappeared during SEM observation or AES measurement is shown, specifically regarding NaCl particles on a Si wafer, along with the results of the AES analysis.

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