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Organic EL displays are advancing in practical applications by leveraging advantages such as high brightness, high-resolution color, and thinness due to their self-emissive principle. Organic EL devices are manufactured by stacking organic films, but analyzing the organic films in their stacked state has been challenging. This time, by using the XRR method, it has become possible to measure the film thickness and density of the organic films while maintaining the stacked state. Analysis of the thickness and density of stacked films is possible regardless of whether they are crystalline or amorphous.

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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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It is possible to evaluate the distribution of nitrogen in SiON films in the depth direction, even down to low concentration areas where high-sensitivity SIMS analysis excels, and to assess the amount of nitrogen (unit: atoms/cm²) with high precision (Figure 1). Additionally, nitrogen can be converted to atomic% (Figure 2), and a fitting curve for nitrogen can be calculated, allowing for the determination of nitrogen's peak concentration, depth, and half-width through fitting (Figure 3).

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By conducting SIMS analysis (SSDP-SIMS) from the substrate side, it is possible to obtain measurements that are not affected by the knock-on effects from the high-concentration layer on the surface due to surface roughness and sputtering. We evaluated the amount of boron penetration from the gate electrode (B-doped Poly-Si) into the substrate. Measurements from the substrate side showed no effects from knock-on, indicating that a more accurate evaluation of the penetration amount is possible. Thus, SSDP-SIMS is effective for assessing the barrier properties of barrier metals, the incorporation of metals into Low-k films, and the evaluation just beneath the rough silicide.

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We conducted TOF-SIMS analysis on an organic EL device (Figure 1) estimated to be formed from four layers of different organic compounds (or organometallic complexes) using XPS. For multilayer structural samples, depth profiling analysis using sputtering is also performed; however, in this case, we created a slope surface to expose each layer without breaking the bonds of the constituent components. Molecular weight-related ions and fragment ions presumed to be Alq3, NPD, and CuPc were obtained, confirming that TOF-SIMS analysis of the slope surface is an effective method for component analysis of organic multilayer films.

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The miniaturization of devices has increased the need for evaluating the depth distribution of impurities in extremely shallow regions. To conduct an accurate assessment, SIMS analysis using a primary ion beam with lower energy (below 1 keV) is required. Figure 1 shows examples of measurements of Si wafers implanted with BF2+ 1 keV, P+ 1 keV, and As+ 1 keV, using a primary ion beam energy of 250 eV to 300 eV.

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Due to the miniaturization of devices, it is necessary to evaluate the depth distribution of impurities in extremely shallow regions. To perform an accurate evaluation, SIMS analysis using a primary ion beam with lower energy (below 1 keV) is required. In this study, the relative standard deviation of the surface density of B calculated from six measurements conducted over multiple days using a 1 keV oxygen ion beam on Si wafers implanted with B+ at low energy was found to be less than 3%, demonstrating that high reproducibility can be achieved in the evaluation of extremely shallow impurity distributions, similar to conventional SIMS analysis.

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By using FIB technology that allows for processing at the nanoscale, it is possible to perform planar TEM observations of specific areas. This enables the confirmation of the ONO three-layer structure (silicon oxide film / silicon nitride film / silicon oxide film) of the capacitor insulating film on the sidewall of the hole, which is difficult to verify through cross-sectional observations.

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Silicon dioxide (SiO2) is widely used in semiconductors as an insulating film, in FPD substrate materials, optical materials, and from medical devices to jewelry; however, conducting structural analysis on glass, which is amorphous, is very challenging. Focusing on the cyclic bonding of SiO2 in glass, Raman measurements were conducted. (Figure 1) In single crystal quartz, the spectrum in the glass state is significantly different, and phonon bands due to long-range order are observed. (Figures 2, 3)

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XPS allows for the evaluation of bonding states of oxidized components (components bonded with oxygen) and metallic components (components bonded with metals). Additionally, by using argon ion sputtering, it is also possible to evaluate bonding states in the depth direction. * Regarding the passive film on the surface of stainless steel (with a thickness of several tens of nm to several hundred nm), the results of the above measurements showed that (1) there are many Fe oxidized components on the surface side, (2) Cr oxidized components exist below the Fe oxide layer, and (3) Ni oxidized components are almost nonexistent. * Since it includes changes in bonding states due to sputtering, the evaluation is primarily based on relative comparisons.

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For extremely thin films with a thickness of a few nanometers or less, such as natural oxide films on silicon wafers and silicon nitride thin films, we will measure the Si2p spectrum of the sample's surface. By performing waveform analysis on the obtained spectrum, we will determine the proportion of each bonding state and estimate the film thickness from this result and the average free path of photoelectrons (Equation 1).

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In the method for preparing thin film samples for TEM observation using FIB, high-energy Ga ions (acceleration voltage of 30 kV) are used, resulting in the formation of a damage layer on the processed surface, which causes a deterioration in the image quality of the TEM. By performing processing at a lower acceleration (2 kV) than conventional methods, the damage layer can be reduced, leading to improved image quality. By reducing the damage on the FIB processed surface through low-acceleration FIB processing, high-quality and reliable data can be obtained in TEM image observation and EELS measurements.

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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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In a STEM device equipped with a spherical aberration correction function (Cs corrector), high-resolution observation and high-sensitivity analysis at the atomic level are possible. The resolution is approximately 0.10 nm.

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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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It is possible to directly extract small pieces from the sample (micro-sampling) and perform FIB processing.

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■Measurement Method for Depth Direction Distribution (1) Limitations of Depth Direction Resolution in Oblique Incidence Method The dependence of depth direction resolution on primary ion energy in the oblique incidence method was investigated using δ-doped samples (Figure 1). It was found that in the oblique incidence method, there is a limit to the improvement of depth direction resolution due to the roughness of the crater bottom (Figure 2). (2) Improvement of Depth Direction Resolution by Vertical Incidence Method Figure 3 shows the relationship between the half-width of the B peak (δ-doped sample) and primary ion energy in both vertical and oblique incidence methods. In the region below 1 keV of primary ion energy, where there were limitations in improving resolution with the oblique incidence method, improvements in resolution have been achieved with the vertical incidence method.

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If you have any questions, please feel free to contact us. ◆ Other Notes - Please provide instructions so that the measurement surface is clear. - Please be careful not to touch the sample surface (measurement surface). - If the sample is at risk of deterioration due to exposure to the atmosphere, please consult us separately. - For fragile samples, please ship them in a cardboard box with cushioning material.

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TDS is a mass spectrometry method that allows monitoring of gases generated by vacuum heating/ramping at different temperatures. The TDS spectrum represents temperature on the horizontal axis and ion intensity on the vertical axis. This enables comparison of the amount of gas released and the desorption temperatures. Additionally, due to the vacuum environment, hydrogen and water can be analyzed with high sensitivity. - It is possible to understand the relationship between the gases desorbed from the sample, the pressure, and the temperature at which they are generated. - Since only the sample can be heated, the background is low, allowing for high-sensitivity analysis of low-mass molecules such as hydrogen, water, oxygen, and nitrogen. - It is possible to estimate the composition of the gases generated from the sample and perform quantitative analysis (counting the number of molecules).

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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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