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Applied & Material Science

HORIBA solutions allow you to measure the properties and performance of a material. This involves many factors such as the structure of the atoms and phases fracture through to the material composition ,stress analysis, conductivity, optical, and thermal properties.

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Correlated TERS, TEPL and SPM Measurements of 2D Materials

Correlated TERS, TEPL and SPM Measurements of 2D Materials

This application note reports on nano-characterization with AFM-Raman of 2D transition metal dichalcogenides (TMDCs) materials which are considered of very high potential semiconductors for future nanosized electronic and optoelectronic devices.

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Measurement of Oxygen Deficiency in Lithium Manganate
Spinel-type lithium manganate (LiMn2O4-σ) is said to change its discharge characteristics due to slight differences in composition caused by oxygen deficiency. The differences in the discharge characteristics of lithium manganate batteries are also observed in the particle size and crystal structure, but attention is also paid to the difference in the oxygen bonding ratio, as samples with less oxygen bonding have poorer discharge characteristics.
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Particle Size Distribution of Black Toner
Toner is a primary component of the electrophotographic printing and copying processes. The synthesized toner particles must exhibit some special characteristics such as particle size and shape to obtain high quality and high-resolution printed images. Utilization of smaller particle size toners has been suggested to be effective in achieving high image quality. In this study, the analysis of the particle size distribution of black toner is optimized using HORIBA Partica LA-960V2 laser diffraction particle size distribution analyzer.
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Calcium Carbonate Particle Sizing for Paint and Coating Applications
A pigment obtains, for example, its maximum colour effect only in a narrow particle size range below 1 to 2 microns. Therefore, understanding particle size distribution of calcium carbonates becomes one of the foremost parameters to be examined. In this study, the particle size distribution of the two different grades of calcium carbonate was investigated using HORIBA Partica LA-960V2 Laser Scattering Particle Size Distribution Analyzer.
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Non-destructive failure analysis of a commercial PEMFC using a micro-XRF with a super large chamber
We introduce non-destructive failure analysis on a large membrane electrode assembly (MEA) from a commercial PEMFC stack using a HORIBA XGT-9000SL, a micro-XRF with an extra-large chamber capacity. Thanks to the chamber capacity, we successfully performed non-destructive elemental imaging on a defective area without cutting the sample, and we found unexpected distributions of Fe, Ni, Mn and Cr within the defective area, and that the elements are present in the MEA as a result of possible degradation of the bipolar plate.
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Applications of micro-XRF for PEMFC catalyst research: Pt catalyst uniformity imaging and Pt loading mass determination
The HORIBA micro-XRF system performs two applications for proton exchange membrane fuel cell (PEMFC) catalyst research: One is Pt catalyst uniformity imaging within a catalyst sheet thanks to the imaging capability. The other is Pt catalyst loading mass determination on average, which is a popular application of EDXRF. Through the experiments, we successfully visualized aggregates of Pt catalyst in our samples, and we also got a good linearity of calibration curve for Pt catalyst loading mass determination.
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Magnetron sputtering is a type of Plasma Vapour Deposition that uses magnetic fields to keep the plasma in front of the target, intensifying the bombardment of ions.
GDOES, the Analytical Companion Tool for Magnetron Sputtering Deposition
Pulsed RF GDOES is a companion analytical tool for magnetron sputtering deposition. Magnetron sputtering is a type of Plasma Vapour Deposition. The vacuum chamber of the PVD coating machine is filled with an inert gas, such as argon. By applying a high voltage (RF, HIPIMS etc), a glow discharge is created, resulting in acceleration of ions to the target surface and a plasma coating. The argon-ions will eject sputtering materials from the target surface (sputtering), resulting in a sputtered coating layer on the products in front of the target.
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Multimodal spectroscopy techniques for nanostructured materials characterization
Multimodal spectroscopy techniques for nanostructured materials characterization
In this article, we present the combination of Raman spectroscopy, Photoluminescence and SEM-CL techniques, where the instruments weren’t physically connected. Smart nanostructured materials require a comprehensive understanding of their morphology, elemental and chemical composition. nanoGPS Suite solution allows a colocalized combination of a variety of microscopy techniques, providing a full characterization of nanostructured materials and a precise superimposition of the results obtained.
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Particle Size Analysis of Acid Hydrolyzed Cellulose Nanocrystal
Nanocellulose is a fibrous material derived from wood and is used as composite materials, etc. Cellulose nanocrystals (CNC) are needle-like materials with a width of about 5-20 nm and a length of about 100-250 nm defibrated using chemical treatment. CNC is cheaper and more attractive than other high-performance nanomaterials as an alternative to some other petrochemical products. It is expected to be useable for oil spill cleaning, engineering, pharmaceuticals, container substitutes, biodegradable food packaging, etc. It is important to understand the fiber size and dispersion state. It is necessary to have an analysis method that can quickly evaluate a wide ranges of particle size distribution for separated particles to agglomerates.
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Particle Sizing of Cellulose Nanofiber
Nanocellulose is a fibrous substance derived from wood and is attracting attention as a cutting-edge material. Cellulose nanofibers (CNF) manufactured by TEMPO oxidation are cellulose fibers that have added carboxy groups at high density. This type of CNF is made with high efficiency and is characterized by a very thin and uniform fiber width of about 3 nm. To utilize nanocellulose, it is important to understand the fiber diameter and dispersion state. To do so, it is necessary to have an analytical method that can quickly evaluate a wide ranges of particle size distribution, from well-dispersed particles to agglomerates at high resolution.
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Particle Size Analysis of Fumed Silica
Chemical Mechanical Polishing (CMP) technology is used as an indispensable fundamental technology in the manufacturing process of ultra-large-scale semiconductor integrated circuits (ULSI). CMP is a technique in which the surface of a substrate is softened, removed or flattened by chemical etching and frictional abrasion with a chemical slurry that contains abrasive particles. Fumed silica abrasive particles are synthesized in a gas phase reaction in flame and are dispersed as secondary particles that are aggregates of primary particles. They are known to have thiogenic properties. Although the rate of polishing is high for fumed silica, its polishing precision is inferior to that of colloidal silica.
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Three Dimensional Raman Imaging
Three Dimensional Raman Imaging
Segmented channel waveguides have been fabricated in single crystal KTiOPO4 through a topotactic process of partial cation exchange. The ion-exchanged waveguides maintain the high nonlinear susceptibility of KTiOPO4 to function as frequency doubling laser light sources. We apply three dimensional (3D) Raman imaging to understand and characterize the changes to the chemical bonding and crystalline structure as well as measure the volumetric structure of the waveguide segments.
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A flake of MoS2: the TEPL shift image derived from fitting the PL peak through regression analysis.
Characterization of MoS2 Flakes using TEOS
Both TEPL and TERS images are well correlated with AFM morphological images obtained simultaneously, and all are consistent in revealing the nature (number of layers) of MoS2 flakes. Upon deconvolution, the TEPL signal is even capable of revealing local inhomogeneities within a MoS2 flake of 100 nm size. Kelvin probe measurement supports TEPL and TERS measurements and adds to the power of such tip-enhanced combinative tools. TEOS characterization of 2D materials is likely to contribute to further deployment of these materials into commercial products through a better understanding of their electrical and chemical properties at the nanoscale.
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Combined Raman and Photoluminescence Imaging of 2D WS2
Combined Raman and Photoluminescence Imaging of 2D WS2
Raman and photoluminescence spectroscopy reveal different aspects of the solid state structure of 2D materials. Raman and photoluminescence imaging performed simultaneously with one instrument reveals the spatial variation of the solid state structure and electronic properties of 2D crystals that is not revealed in reflected white light imaging. That ability should allow materials scientists to better design and fabricate electronic and optoelectronic devices based upon 2D crystals.
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A combined (low-frequency and fingerprint) Raman map of MoS2 layers.
Number of Layers of MoS2 Determined Using Raman Spectroscopy
The two methods - Analysis of fingerprint modes (intralayer) and Analysis of low-frequency modes (interlayer) - give complementary results and allow the determination of the number of MoS2 layers. Method 2 (using low frequency modes) gives excellent contrast; however it does not show single layer regions (which is related to the nature of the modes, rising from interaction between at least two layers). Method 1 (using fingerprint modes) shows all the layers, but the contrast is poorer, particularly for higher numbers of layers. The best result can be obtained combining the two methods. All the measurements (low-frequency and fingerprint) were done using ultra-low frequency ULFTM filters which allow a high throughput measurement in a full Raman range, down to <10 cm-1.
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RBM spectrum that represents tubes with at least 3 different properties.
SWNT Quality Control by Raman Spectroscopy
Raman has shown a high potential in characterising the SWCNTs' structure. The correlation between knowledge about structure with physical and chemical properties about the tubes make the technique extremely powerful to control the quality of the SWCNTs for specific applications. Raman spectrometer capabilities like spatial resolution, spectral resolution and excitation wavelength versatility have been examined. Beside Raman, preliminary fluorescence studies are describing the potential of the technique.
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Characterization of diamond layers by SE: crystalline undoped diamond layers on silicon substrate.
Ellipsometric Characterization of Doped and Undoped Crystalline Diamond Structures
In this work, spectroscopic ellipsometry (SE) was successfully applied to characterize the optical properties and the thicknesses of doped and undoped diamond layers. The sensitivity of this technique enables the doped layer to be distinguished from the undoped one in a sample consisting of a stack of these two layers. Moreover, an interface between the two layers has been detected. This work and others reported previously show clearly that ellipsometry is the technique of choice for the characterization of optical and structural properties of layered materials thanks to its sensitivity and the wide range of information it provides.
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A typical spectrum of a hard carbon film.
Derivation of Physical Parameters from Raman Spectra of Hard Carbon Films
The Raman spectra of elemental carbon materials are known to be sensitive to polymorphy. For hard carbon films, the spectra of amorphous and diamond-like carbons can be band-fit to separate the contributions of the "graphitic carbon" (G band) from the "disordered carbon" (D band). The spectral behaviour of carbon films has been empirically correlated with thin film physical properties such as hardness, durability, optical transparency, electrical conductivity, thermal conductivity and corrosion resistance, and can be of use for prediction of these properties without extensive alternative testing. The DiskRam has been designed to automate the collection of Raman spectra from hard carbon coatings on computer hard disk media and the extraction of parameters that are well correlated with the properties of the films. The extracted information is output in spreadsheet format for SPC at a manufacturing facility.

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Evaluation of Diameter (Thickness) and Aggregation/Dissociation State of Carbon Nanotube Dispersions
Carbon nanotubes (CNTs) are thin, light, and flexible string-like materials that are composed entirely of carbon atoms. CNTs easily aggregate, so it is essential to understand and control the state of aggregation in order to achieve the expected performance. For this purpose, an analytical method that can quickly evaluate wide particle size distributions (PSD) from isolated dispersion to aggregation, with high resolution, is necessary.
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PLQY in NIR with Fluorolog-QM and K-Sphere
The Fluorolog-QM fluorescence spectrometer with an integrating sphere option is an excellent choice for PLQY measurements in NIR. The K-Sphere is very convenient and easy to use, as it couples directly to the sample compartment optics and allows a use of external light sources, such as DPSS lasers, which can be attached to the front of the sample compartment. The sphere has holders for cuvettes, slides and powders that can be easily interchanged. The results demonstrate very good reproducibility and precision for NIR PLQY measurements spanning almost two orders of magnitude. Based on multiple measurements, the demonstrated PLQY standard deviations range from 1.3% for high QY value (77%) to 6.4% for the QY below 1%.
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MoS2/Pb nanocomposite coatings for solid lubricants application
Depth profile analysis by GDOES. Pulsed RF Glow Discharge Optical Emission Spectrometry offers ultra-fast elemental depth profiling capability for the investigation of thin and thick films. Thanks to the use of a pulsed RF source, coupled with a high resolution optical spectrometer, the GD Profiler 2 provides an excellent depth resolution, allowing the fast evaluation of the coating quality. In this application note, we focus on a MoS2/Pb composite multilayered sample, used as a solid lubricant. The analysis of such a sample shows the excellent performance of this instrument for the study of nm-thick complex coatings.
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Ellipsometric Characterization and Modeling of Different Types of Nanoparticles
UVISEL ellipsometers have been used for the characterization of several systems of nanoparticles. This ellipsometric characterization involves the development of specific modeling tools available within DeltaPsi2 software. Through this report we illustrate the application of ellipsometry to the characterization of nanoparticle based samples. Our goal is to demonstrate that the technique can apply within a large panel of materials science. The HORIBA ellipsometric product line offers the most versatile hardware of the UVISEL series combined with the DeltaPsi2 software including unique modeling features to get the most of your applied work on this fascinating domain of modern physics.
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Mapping of the nanowire performed by recording step-spectra at every 200 nm with an integration time of 1s.
Raman Imaging of a Single Gallium Nitride Nanowire: Pushing the Limits of Confocal Microscopy
We have performed a complete Raman polarized study of a single GaN nanowire using a confocal microscope together with a high resolution stage. The high spatial resolution of our Raman confocal instrument together with a piezoelectric stage demonstrates unambiguously the possibility to image the optical properties of nano-objects with a resolution better than 200 nm keeping the fill advantage of the polarization control under a confocal microscope.
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Multimodal spectroscopy techniques for nanostructured materials characterization
Multimodal spectroscopy techniques for nanostructured materials characterization
In this article, we present the combination of Raman spectroscopy, Photoluminescence and SEM-CL techniques, where the instruments weren’t physically connected. Smart nanostructured materials require a comprehensive understanding of their morphology, elemental and chemical composition. nanoGPS Suite solution allows a colocalized combination of a variety of microscopy techniques, providing a full characterization of nanostructured materials and a precise superimposition of the results obtained.
open
Particle Size Analysis of Fumed Silica
Chemical Mechanical Polishing (CMP) technology is used as an indispensable fundamental technology in the manufacturing process of ultra-large-scale semiconductor integrated circuits (ULSI). CMP is a technique in which the surface of a substrate is softened, removed or flattened by chemical etching and frictional abrasion with a chemical slurry that contains abrasive particles. Fumed silica abrasive particles are synthesized in a gas phase reaction in flame and are dispersed as secondary particles that are aggregates of primary particles. They are known to have thiogenic properties. Although the rate of polishing is high for fumed silica, its polishing precision is inferior to that of colloidal silica.

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open
A flake of MoS2: the TEPL shift image derived from fitting the PL peak through regression analysis.
Characterization of MoS2 Flakes using TEOS
Both TEPL and TERS images are well correlated with AFM morphological images obtained simultaneously, and all are consistent in revealing the nature (number of layers) of MoS2 flakes. Upon deconvolution, the TEPL signal is even capable of revealing local inhomogeneities within a MoS2 flake of 100 nm size. Kelvin probe measurement supports TEPL and TERS measurements and adds to the power of such tip-enhanced combinative tools. TEOS characterization of 2D materials is likely to contribute to further deployment of these materials into commercial products through a better understanding of their electrical and chemical properties at the nanoscale.
open
Combined Raman and Photoluminescence Imaging of 2D WS2
Combined Raman and Photoluminescence Imaging of 2D WS2
Raman and photoluminescence spectroscopy reveal different aspects of the solid state structure of 2D materials. Raman and photoluminescence imaging performed simultaneously with one instrument reveals the spatial variation of the solid state structure and electronic properties of 2D crystals that is not revealed in reflected white light imaging. That ability should allow materials scientists to better design and fabricate electronic and optoelectronic devices based upon 2D crystals.
open
A combined (low-frequency and fingerprint) Raman map of MoS2 layers.
Number of Layers of MoS2 Determined Using Raman Spectroscopy
The two methods - Analysis of fingerprint modes (intralayer) and Analysis of low-frequency modes (interlayer) - give complementary results and allow the determination of the number of MoS2 layers. Method 2 (using low frequency modes) gives excellent contrast; however it does not show single layer regions (which is related to the nature of the modes, rising from interaction between at least two layers). Method 1 (using fingerprint modes) shows all the layers, but the contrast is poorer, particularly for higher numbers of layers. The best result can be obtained combining the two methods. All the measurements (low-frequency and fingerprint) were done using ultra-low frequency ULFTM filters which allow a high throughput measurement in a full Raman range, down to <10 cm-1.

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