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[Analysis Case] Depth Profile Analysis of Impurities in Organic EL Devices Using SIMS

Evaluate organic EL elements with good depth direction resolution.

To extend the lifespan of organic EL devices, it is essential to evaluate the degradation caused by electromigration, making it important to investigate the diffusion state of electrode metal components into the organic layer. However, whether analyzed directly from the cathode side or through the SSDP method from the anode side, the depth resolution decreases, making it difficult to assess the diffusion from the interface into the organic layer. (Note: SSDP method refers to analysis from the backside. For details on the analytical method, see section B0013.) Therefore, by using special processing to expose the cathode/organic layer interface and the organic layer/anode interface, it has become possible to evaluate the organic layer with high depth resolution.

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[Analysis Case] High-Sensitivity Analysis of Light Elements in Semiconductor Substrates Using SIMS

SIMS analysis allows for the evaluation of elements such as H, C, N, O, and F down to levels below 1 ppm.

It is possible to detect H, C, N, and O in semiconductor substrates at concentrations below 1 ppm (approximately 5E16 atoms/cm3) and F at concentrations below 1 ppb (approximately 5E13 atoms/cm3) using this method. Examples of measurements in actual FZ-Si (Figure 1) and the background levels of III-V semiconductors are presented (Table 2). In addition to III-V semiconductors, standard samples have been prepared for various materials such as metal films and insulating films, enabling highly sensitive quantitative analysis. This method is ideal for bulk analysis of various materials, including semiconductor substrates, and for evaluating the contamination of gas components during semiconductor processes.

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[Analysis Case] Discrimination between Anatase and Rutile Types of Titanium Dioxide

TEM-EELS enables elemental identification and chemical state analysis in micro-regions.

Titanium dioxide (TiO2), used in electronic materials, catalytic materials, ultraviolet absorbers, and photocatalysts, exists in two forms with the same composition but different crystal structures: anatase and rutile. We conducted measurements on a polycrystalline TiO2 sample with a thickness of 20 nm, deposited on a Si substrate (Photo 1), using an electron beam probe focused down to approximately 1 nmΦ (FWHM). The EELS spectra obtained from the sample match the standard spectra of anatase TiO2 for both Ti and O (Figures 1 and 2).

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[Analysis Case] Evaluation of Composition and Impurity Distribution of ZnO Films by SIMS

Visualization of in-plane distribution through imaging SIMS analysis.

The uniformity of the film composition and the distribution of impurities, which are one of the elements in device creation, were evaluated using imaging SIMS analysis. Through data processing after measurement, we can obtain planar images (Figure 1), cross-sectional images (Figure 2), depth distribution profiles at arbitrary locations (Figures 3 and 4), and line profiles. From the distribution of constituent materials and impurities, we can gain information that leads to process and film quality improvements.

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Pre-treatment and measurement under high purity atmosphere.

XPS: X-ray photoelectron spectroscopy, etc.

By conducting sample pretreatment, transportation, and measurement under a high-purity inert gas atmosphere, it is possible to evaluate while suppressing surface oxidation and moisture adsorption. ■Examples of Application - Semiconductor electrode materials Evaluation of peeling surfaces can be conducted while minimizing the effects of secondary contamination and oxidation. - Organic EL materials Working in an inert gas atmosphere from the moment of opening prevents material degradation. - Battery materials such as Li If processing in a N2 atmosphere is not possible for materials like Li, treatment can be performed in an Ar atmosphere as an alternative.

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Distortion evaluation using SEM equipment

EBSD: Electron Backscatter Diffraction

Measurements can be performed in bulk state without the need for thinning processes like TEM (NBD: Nano Beam Diffraction). It has the high spatial resolution characteristic of SEM and relatively high strain sensitivity. Additionally, there is a possibility of detecting local lattice strain as tensor data.

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Photoluminescence method

PL：PhotoLuminescence

The photoluminescence method is a technique that involves irradiating a substance with light and observing the light emitted when excited electrons return to their ground state. Various information can be obtained from the resulting emission spectrum. - Samples with a bandgap of about 3.5 eV can be excited. - The mapping function allows for the acquisition of extensive information. - Measurements can be conducted down to approximately 10 K. - Generally, it is a non-destructive measurement that does not require special pretreatment.

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X-ray Absorption Fine Structure (XAFS)

XAFS is a method for analyzing the absorption spectrum obtained by irradiating a substance with X-rays.

- It is possible to evaluate the local structure (interatomic distances, coordination numbers) and chemical state (valence, coordination structure) around the target elements in the sample. - Measurements can be conducted regardless of the environment (high temperature, high pressure, atmosphere). - Measurements can be performed on various sample forms (solid, liquid, gas, thin films, amorphous materials, etc.). - A wide applicable concentration range (from major component elements to trace elements). - Non-destructive measurement. - Depending on the measurement method, it is possible to conduct measurements that are sensitive to the surface as well as bulk measurements.

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[Analysis Case] Evaluation of the Diffusion Layer in Crystalline Si Solar Cells

Quantitative evaluation of dopants and evaluation of carrier distribution.

This is an example of quantitatively evaluating the dopant concentration distribution directly beneath the electrode in back contact type crystalline silicon solar cells. Additionally, by evaluating the carrier distribution, it is possible to determine the polarity of p/n and visualize the depletion layer in the cross-sectional direction.

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[Analysis Case] Evaluation of Carrier Distribution in Crystalline Si Solar Cells

Evaluation of carrier diffusion layer uniformity in samples with surface roughness.

This is an introduction to a case where the carrier diffusion layer distribution of the surface textured part and the back surface field (BSF) part of BSF-type crystalline silicon solar cells was evaluated using SCM. In the textured part, the pn junction is formed along the surface irregularities, while in the BSF part, it can be confirmed that the carrier distribution is interrupted and uneven.

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[Analysis Case] Evaluation of Cleansing Oil's Cleaning Effectiveness

Measurement examples of cleaning residues using TOF-SIMS.

The way makeup is removed varies depending on the type of cleansing oil, even with the same washing method. To investigate the cleansing effect, we evaluated the remaining components after washing lipstick with oil using TOF-SIMS. This report introduces a case where the differences in cleansing effects due to the type of cleansing oil were assessed by conducting relative comparisons of the components of the lipstick (such as pigments and oils) between samples.

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[Analysis Case] Evaluation of SiC Power MOSFET Dopants by SIMS

Imaging SIMS enables the evaluation of localized elements.

We disassembled a commercially available SiC power MOSFET and conducted imaging SIMS measurements to evaluate the concentration distribution of the dopant elements Al, N, and P in a 20 µm square area to a depth of 0.5 µm. We will present a case where we extracted the depth profile concentration distribution of Al, N, and P localized within the sample surface from the data processing after the imaging SIMS measurements.

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[Analysis Case] SiC by SIMS

Imaging SIMS allows for the evaluation of localized elements.

We disassembled a commercially available SiC Schottky diode and conducted imaging SIMS measurements to evaluate the concentration distribution of the dopant element Al in a 40μm square area to a depth of 0.5μm. From the data processing after the imaging SIMS measurements, we extracted the depth-wise concentration distribution of Al localized within the sample surface and present a case study comparing the concentration distributions for each pattern.

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[Analysis Case] SIMS Analysis of Compound Layered Structure Samples

Analysis is possible after selectively removing the compound layer through preprocessing.

In SIMS analysis of layered structure samples, there is a concern that in structures where the layer of interest is located at a deep position from the sample surface, the depth resolution may degrade due to the influence of the concentration distribution of the upper layers. In such cases, it is effective to remove the upper layers through pretreatment before analysis. This document presents an example of selectively and progressively removing layers from InP/InGaAs-based SHBT (Single Heterojunction Bipolar Transistor) samples.

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[Analysis Case] Evaluation of Liquid Crystal Structure and Micelle Size of Emulsifiers by SAXS

Capable of structural analysis at the nanoscale and evaluation of nanoparticle size.

Emulsification technology is a fundamental technology in cosmetic development and is utilized across various cosmetics. Changes in the structure of emulsifiers are closely related to the balance of water and oil in the product, the permeability of encapsulated active ingredients, cleansing power, and changes in user experience, making its analysis very important.

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[Analysis Case] Composite Evaluation of the Active Layer of SiC Power MOSFETs

Evaluate the shape of the active layer and the dopant.

We will introduce a case study evaluating the distribution of the diffusion layer in commercially available SiC power MOSFET devices. In the SiC MOSFET manufacturing process, the channel is formed through ion implantation, activation heat treatment, and epitaxial layer formation. During the active layer formation process, we understood the device structure through TEM observation and evaluated the diffusion layer distribution of the p-type/n-type cross-section and the epitaxial layer from SCM measurements, as well as the depth concentration distribution of dopant elements (N, Al, P) from SIMS measurements. Measurement methods: SIMS, SCM, TEM Product field: Power devices Analysis purpose: Trace concentration evaluation, shape evaluation, product investigation For more details, please download the materials or contact us.

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[Analysis Case] Evaluation of H Concentration in IGZO Film

It is possible to evaluate the depth distribution of H in the IGZO film with high sensitivity.

IGZO films are materials that are being researched and developed as TFT materials for displays. The carrier concentration changes according to the hydrogen concentration in the IGZO film, leading to variations in electrical characteristics. Therefore, it is necessary to accurately measure the hydrogen concentration in the film for evaluating the device characteristics and reliability of devices using IGZO films. We will introduce a case study that evaluated the hydrogen concentration in IGZO films under different heating conditions using SIMS.

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[Analysis Case] Electronic Structure and Local Structure Analysis of LIB Cathode Materials

Evaluation of valence, coordination number, and interatomic distance of cathode materials through XAFS analysis.

In recent years, as hybrid and electric vehicles have been becoming more widespread, there is a growing demand for larger and higher-performance lithium-ion secondary batteries for their power supply. To develop high-capacity positive electrode materials, it is crucial to identify the correlation between composition, structure, and electrochemical properties. By clarifying the electronic states of metal elements and their local structures in positive electrode materials through XAFS analysis using synchrotron radiation, it is possible to gain insights into the correlation between composition, structure, and electrochemical properties.

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[Analysis Case] Simultaneous Analysis of 17 Free Amino Acids

High-sensitivity and selective amino acid analysis is possible using the OPA post-column method.

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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[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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[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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