一般財団法人材料科学技術振興財団　MST List of Products and Services

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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In general, to remove dirt, a cotton swab may be dipped in ethanol and used for wiping. When the surface of a Si wafer was wiped with a cotton swab dipped in ethanol, an analysis was conducted using TOF-SIMS to determine what was distributed on the surface. The Si wafer wiped with the cotton swab showed stains that were not visible under an optical microscope, and it was found that these were due to the cotton swab. TOF-SIMS is effective for analyzing stains that are not visible under an optical microscope and for cleaning residues.

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Aluminum foil is produced by rolling two sheets together, where the outer side in contact with the rollers has a glossy surface, while the inner side, where the aluminum sheets touch each other, has a matte surface. We compared the components present on the extreme surfaces of each side. Common organic secondary pollutants such as PDMS (polydimethylsiloxane), BHT (antioxidant), DOP (plasticizer), amines (m/z 182, 242), amides (m/z 256, 284), and carboxylic acids (m/z 255, 283) were not observed. There was a slight tendency for Fe and organic materials (such as hydrocarbons) to be stronger on the glossy side, while substances like SO4 showed a slightly stronger tendency on the matte side.

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Knowledge about the effects of contamination and oxidation during sample transport is important in surface analysis where the detection depth is on the nanometer order. Therefore, we examined the impact of contamination and oxidation due to differences in storage methods on Si wafers. In storage with wrapping paper and aluminum foil, there is a tendency for the peaks of organic materials caused by secondary contamination to be weaker. When samples are wrapped and stored in the matte side of aluminum foil during storage and transport, it can suppress contamination and oxidation compared to other storage methods.

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The concentration of volatile components that humans perceive as odors can be very low, and they may not be detectable using the conventional HS (Headspace) method for GC/MS measurements used for analyzing volatile components. By using Solid-Phase Micro Extraction (SPME), it becomes possible to concentrate the volatile components and introduce them into GC/MS, allowing for the detection of many trace components. This document presents a case study analyzing odor components in trace amounts of essential oils.

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The decomposition behavior of materials when heated in a vacuum or in inert gases such as nitrogen can differ from that when heated in air. Therefore, when conducting gas emission analysis, it is desirable to heat the materials in an environment that closely resembles the actual conditions to which they are exposed. In this case, a comparison of the gases emitted during the pyrolysis of polystyrene at 550°C in helium and in air was conducted. Only hydrocarbon compounds were detected in helium, whereas reaction products with oxygen, such as benzaldehyde, were also detected in air.

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When conducting structural analysis of condensation-type polymers such as polyurethane, information may not be sufficiently obtained using only thermal decomposition GC/MS. In such cases, performing chemical decomposition using methanol can provide more detailed structural information. This case presents the results of decomposing polyurethane-based lightweight aggregate with methanol and conducting GC/MS measurements. Diphenylmethane diisocyanate, dimethyl phthalate, trimethylolpropane, and propylene glycol compounds were detected, leading to the conclusion that this product is composed of polyester urethane made from these materials.

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Conductive paints are used to impart conductivity to insulating materials. Additives are included in the paint to give conductivity to the originally insulating paint itself. This document evaluates two types of conductive paints with different conductivities, focusing on the shape and composition of the additives in the paint, as well as the dispersion state of the additives.

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Coatings are used for various purposes such as coloring, protecting, and imparting functions by applying them to the surface of the target material. In any case, it is required that the coating is applied to the target material without poor adhesion. In this document, we applied conductive paint on two types of substrates: stainless steel and organic film, and observed the state of the paint-substrate interface using cryo-SEM.

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Nitrogen is utilized in various forms across a wide range of fields including chemistry, materials, food, and pharmaceuticals. Nitrogen compounds consist of inorganic nitrogen compounds such as nitrates, nitrites, and ammonia, as well as organic nitrogen compounds like amino acids. In the case of samples in aqueous solution, inorganic nitrogen compounds such as nitrate ions, nitrite ions, and ammonium ions can be evaluated using ion chromatography, while organic nitrogen can be assessed using HPLC or LC/MS. Total nitrogen, which includes both inorganic and organic nitrogen compounds, can be evaluated using spectrophotometry.

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Volatile organic compounds (VOCs) are used during the cleaning of semiconductors and industrial products and may be present in trace amounts in cleaning water, etc. VOCs in water are a concern because even in trace amounts, they can cause odors and health issues. Therefore, environmental standards and discharge standards have been established, and methods capable of measuring low concentrations are required. This case presents an example of detecting trace VOC components (sub-ppb level) in water by introducing components concentrated by P&T (Purge & Trap) into GC/MS.

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At MST, we can accept requests for the consideration and development of analytical methods based on customer needs. In this example, we developed a simultaneous analysis method for pesticide components in water. Traditionally, pesticide analysis has been complicated due to separate pretreatment and measurement methods for each component. If multiple components can be measured at once, it can reduce sample volume and analysis costs, enabling more efficient analysis. In this example, we established a method that allows for easy confirmation of the presence of approximately 70 pesticide components down to low concentration levels by using solid-phase extraction for pretreatment and LC/MS/MS for measurement.

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The electron diffraction method using an electron microscope is classified into three types based on the way the electron beam is incident on the sample. The characteristics of each type and examples of data are presented. It is necessary to choose the appropriate method according to the size of the evaluation object and the analysis purpose.

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XPS can evaluate the chemical bonding state of the sample surface, and further detailed assessments can be made through waveform analysis. Additionally, by using assumed parameters in the waveform analysis results, it is also possible to calculate the thickness of surface oxide films, etc. In this document, we will introduce a case where the composition and state evaluation of the SiC surface was performed, along with the calculation of the oxide film thickness from the obtained peak intensity.

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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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Pole figure measurement is a method that focuses on specific crystal planes and evaluates the distribution of crystal orientations by directing X-rays from various directions onto the sample. The detector is fixed at the diffraction angle (2θ) of the crystal plane of interest, and the two parameters, α (the tilt angle of the sample) and β (the in-plane rotation angle of the sample), are varied to measure crystal planes tilted in all directions. This indicates that the crystal orientations are concentrated in the directions where high diffraction intensity is observed. Additionally, the measurement results are represented in a pole figure as shown in the diagram at the bottom right.

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When measurements are conducted using a two-dimensional detector, information about the diffraction angle (2θ) as well as the tilt direction (χ) can be obtained simultaneously. The observed two-dimensional diffraction pattern can visualize characteristics such as the crystallinity and orientation of the material, making it effective for evaluating materials where orientation affects their properties.

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In lithium-ion secondary batteries, the SEI layer (solid electrolyte interface) is a significant factor affecting the battery's lifespan, and it is important to understand the chemical species of Li contained within it. Li itself has a small chemical shift, making direct evaluation difficult; however, by performing waveform analysis to separate the states of the bonding partner elements (C, O, F, P), it is possible to calculate the presence ratio of Li in different bonding states. An evaluation of the state of Li before and after cycle testing revealed that after the test, the presence ratios of Li2CO3 and Li-POxFy increased compared to before the test.

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ABF-STEM images (scanning transmission annular dark field images) allow for the direct observation of atomic positions of light elements. Simultaneous acquisition with HAADF-STEM images enables more detailed structural analysis. In this case, we present an example of observing atomic columns of strontium titanate (SrTiO3). By combining EDX elemental distribution analysis, we can visually clarify the distribution of atoms. Measurement methods: TEM・EDX Product fields: LSI・Memory Analysis purposes: Shape evaluation・Structural evaluation For more details, please download the materials or contact us.

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The electrodes of fuel cells have a structure in which catalyst particles are supported on a carbon carrier. Evaluating the state of the carrier and catalyst particles is essential for understanding degradation mechanisms and considering design guidelines. XPS analysis is effective for assessing the state of catalyst poisoning (oxidation). Additionally, SEM and TEM observations are effective for evaluating catalyst agglomeration and particle growth. By combining multiple analytical methods, we propose a multifaceted evaluation.

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In this case, we used fabric that had absorbed tobacco odor and measured the differences in odor components with and without the use of deodorant spray using GC/MS. Since tobacco odor is composed of many components, we focused on the peaks that were reduced by the deodorant among the detected peaks for analysis. As a result, a decrease in three odor components characteristic of tobacco odor was confirmed. Additionally, it is possible to verify the effectiveness of deodorants and air purifiers against various other odors beyond this case.

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The electrodes of fuel cells are supported by Pt particles or Pt alloy (such as PtRu) particles as catalysts on carbon. Due to the fine structure of these catalyst particles, which are on the order of a few nanometers, SEM and TEM analyses are used for morphological observation and compositional analysis. In addition to evaluations in the initial state, degradation after current application has been reported, including modulation of alloy composition, leaching of Ru, and an increase in the diameter of catalyst particles; HAADF observation and high-resolution EDX analysis are very effective for these evaluations. Furthermore, multi-field observation and analysis enable the assessment of particle size and compositional distribution.

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The electrodes of fuel cells are supported by Pt particles or Pt alloy (such as PtRu) particles on carbon. Due to the fine structure of these catalyst particles, which are on the order of a few nanometers, SEM and TEM analyses are used for morphological observation and compositional analysis. In addition to evaluations in the initial state, degradation after current application has been reported, including modulation of alloy composition, Ru leaching, and an increase in catalyst particle size; high spatial resolution HAADF observation and EDX analysis are very effective for these evaluations. Furthermore, SEM observation allows for the confirmation of the shape of the carbon support and the state of the catalyst particles.

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XPS and AES are surface-sensitive analytical techniques widely used for evaluating sample surfaces, but by combining them with ion etching, depth profiling analysis becomes possible. When conducting depth profiling analysis, it is important to appropriately differentiate between XPS and AES according to the area to be measured and the material of the sample in order to perform analysis that aligns with the objectives. The characteristics of depth profiling analysis using XPS and AES will be compared using the analysis of SUS passive films as an example.

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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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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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XPS is a surface-sensitive technique, so carbon derived from organic contaminants due to the atmosphere is detected at a significant level. Reducing the influence of this carbon from organic contaminants is important for evaluating the original composition of the film. Typically, Ar ion sputtering is used to remove organic contaminants, but damage caused by sputtering may prevent the evaluation of the film's original composition and bonding states. We present an example where the influence of carbon from organic contaminants was reduced by removing the surface oxide layer using wet etching instead of Ar ion sputtering.

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In semiconductor devices, their performance is greatly influenced by the combination of work functions of various materials that make up the device. Therefore, attempts have been made to control the work function through surface treatments and modifications, and it is important to verify their effects. This document presents an example of evaluating the change in work function of ITO (Sn-doped In2O3), used as an electrode material in organic ELs and solar cells, before and after surface plasma treatment using UPS analysis.

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We compared the states of the Si surface after HF treatment and after ozone treatment. In the positive ion spectrum, the peak intensity of Si was different. The weaker Si intensity after HF treatment is due to Si being metallic, while the stronger Si intensity after UV-ozone cleaning and in the As Received state is due to Si being oxide-based. From the negative ion spectrum, fragment ions reflecting the surface state were detected: SiF, SiH, and Six series after HF treatment, and SiO2 series after UV-ozone cleaning and in the As Received state.

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This text introduces an example of evaluating the composition and bonding states of GaN films used in LEDs and power devices using XPS. Understanding how the composition and bonding states change due to film formation conditions and surface treatments is effective for process management. It is important to appropriately select the X-rays used during the evaluation according to the purpose. Measurement conditions for each focus will also be presented.

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Due to its characteristics such as high hardness and high wear resistance, DLC (diamond-like carbon) films are utilized in a wide range of fields. These films are materials that lie between graphite and diamond, and the separation of sp2 (graphite structure) and sp3 (diamond structure) within the film to obtain the sp2/(sp2+sp3) ratio is one of the important factors that determine the properties of the film. Here, we will introduce an example of evaluating this sp2/(sp2+sp3) ratio by analyzing the C1s spectrum using XPS.

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- 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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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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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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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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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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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 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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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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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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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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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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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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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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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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