JEOL USA Blog

EDS Spectrum.jpg

How to Decipher an SEM-EDS Spectrum

How to Decipher an SEM-EDS Spectrum

Investigating the chemical composition of materials is important for fully understanding their material properties. Often, chemical heterogeneity at the micro- to nanoscale influences the macroscopic behavior of materials. For these types of samples, SEM-EDS is ideal.

Scanning Electron Microscopy (SEM) can be used in tandem with Energy Dispersive X-ray Spectroscopy (EDS) to better understand material properties. At its core, SEM uses a high-energy electron beam to characterize samples at the micro- to nanoscale, offering higher resolution and depth of field than other microscopy techniques. Secondary and backscattered electrons generated by interactions between the electron beam and sample can be used to characterize surface morphology and composition respectively. Similarly, characteristic X-rays generated by the sample can be analyzed to assess its composition.

Characteristic X-rays are emitted when outer orbital electrons within an atom relax to fill lower-energy vacancies within inner orbitals created by a high-energy source such as an electron beam. Both the energy and wavelength of these X-rays are unique to the element they are generated from. While multiple techniques exist to analyze these X-rays, perhaps the most common to pair with SEM is EDS. At their core, EDS detectors analyze the chemical composition of materials by counting the X-rays being generated and measuring each X-ray’s energy to determine what element it came from.

EDS detectors are prized for their speed, versatility and ease of use. They allow users to quickly assess what elements are present in a sample and estimate the relative abundances, often in near-real time and without destroying the sample. We often visualize EDS data as a spectrum, showing X-ray energy vs. number of X-rays analyzed (intensity). Interpreting this spectrum and how it is transposed into chemical compositions is critical for accurately characterizing materials.

Although technologic advancements such as automatic element identification, peak deconvolution and quantification have vastly simplified interpreting EDS data, it is still important to understand the principles and best practices of SEM-EDS. This basic understanding empowers users to feel confident about their SEM-EDS results and consistently collect the best chemical data possible.

Read on to learn more detail about how to interpret and utilize an SEM-EDS spectrum.

1. Identifying the Elements Present

When irradiated by a high-energy source such as an electron beam, every element emits a set of X-rays with unique energies and wavelengths, hence, “characteristic X-rays”. Modern state-of-the-art SEM-EDS detectors can analyze X-rays ranging in energy from tens of electron volts (eV) to tens of kiloelectron volts (keV), allowing users to characterize nearly every element between Li and U. Most standard EDS systems are optimized for analyzing Be or B through U.

As shown in Figure 1 below, we visualize EDS data as a spectrum, plotting X-ray energy versus intensity. The peak intensity corresponds to the element’s relative abundance in the sample, while the width of each peak corresponds to the energy resolution of the EDS detector, typically 125-132 eV (FWHM at Mn-Kα).

Modern SEM-EDS software is designed to automatically identify X-ray peaks by comparing their shape and energy to a known database. This allows users of all skill levels to readily collect EDS data. However, for minor or trace (~0.1-5 wt%) elements, the software may be unable to distinguish the peak from the background radiation (Bremsstrahlung). In this case, users may need to manually examine the spectrum to confirm the element's presence. Similarly, some X-ray peaks overlap within the uncertainty of the method, requiring software peak deconvolution. While this method is robust for even severe peak overlaps (e.g., Ti-Ba or W-Si), users should be aware of what peak overlaps to expect for their sample to ensure they are adequately accounted for.

2. Quantitative Analysis

    SEM-EDS is used both for providing qualitative information about the elements present and as a semi-quantitative analysis technique. To accurately quantify elemental concentrations, considerations such as the homogeneity, thickness, and surface topography of the sample are essential. These factors influence the accuracy of the quantitative results.

    While there are multiple approaches for calculating the sample composition from an EDS spectrum, the simplest and most widely utilized is standardless quantitative analysis. This method compares the relative intensities of all of the identified peaks, normalizing the results to 100%. A matrix correction (e.g., ZAF, Φρz) is applied to account for variations in X-ray yield efficiency as a function of composition. For an ideal sample, this method is reproducible within ±2% to ±5% for major components.

    Alternatively, some users may choose to calculate quantitative results using standards. In this case, the peak intensity of each element present in the sample is compared to that of a standard. A matrix correction is still applied. While this approach in principle yields more accurate quantitative results, it relies more heavily on ideal sample preparation and is far more susceptible to user error.

    3. Sample Preparation

    The quality of SEM-EDS analysis is highly dependent on sample preparation. The sample should be polished, flat, and homogeneous relative to the interaction volume of the electron beam to ensure accurate chemical analysis. For samples with non-uniform composition, acquiring spectra from multiple areas or acquiring a hyperspectral EDS map can help assess heterogeneity.The quality of SEM-EDS analysis is highly dependent on sample preparation. The sample should be polished, flat, and homogeneous relative to the interaction volume of the electron beam to ensure accurate chemical analysis. For samples with non-uniform composition, acquiring spectra from multiple areas or acquiring a hyperspectral EDS map can help assess heterogeneity.

    4. Consideration of Topography

    The topography of a sample can significantly affect SEM-EDS analysis. Rough or irregular surfaces may preferentially absorb or block X-rays, leading to errors in calculated composition. Positioning the sample to provide a direct line of sight between the region of interest is crucial and can assist in fully characterizing the sample, though quantitative results should be treated with caution.

    5. Accelerating Voltage

    The choice of accelerating voltage is critical for the excitation of X-ray lines of elements in the sample. A voltage 1.5 to 2 times higher than the energy of the X-ray lines from the element(s) of interest is recommended to efficiently excite the element. For unknown samples, using an accelerating voltage between 15 kV and 20 kV ensures that all elements present are identified. However, users might choose to collect EDS data at lower accelerating voltages to minimize interaction volume, especially to aid in characterization of small nano- to micro-scale features.

    6. Hyperspectral EDS Mapping


    ● Complex compositions

    ● Overlapping peaks

    ● Minor/trace elements with low peak/background ratios

    Final Thoughts on the SEM-EDS Spectrum

    With a basic understanding of the principles of SEM-EDS, researchers and analysts can effectively acquire and interpret robust EDS data. This can unlock valuable quantitative and qualitative insights into their samples.

    It is crucial to consider the limitations and challenges associated with SEM-EDS analysis, including sample preparation and the potential for quantitative errors. However, with a careful approach and interpretation, SEM-EDS remains an indispensable tool in materials science and engineering for elemental analysis at the micro- to nano scale.

    JEOL USA’s Tools Incorporate the SEM-EDS Spectrum

    SEM-EDS analyses are fast, effective, and can help interrogate a wide range of material properties and characteristics. Understanding what EDS spectra are and how they can be used to inform qualitative and semi-quantitative chemical analysis of samples is essential for accurately interpreting and gaining the most out of this type of analysis.

    SEM-EDS can provide powerful information about the material properties at the micro- to nanoscale. It is therefore utilized for with a variety of materials such as:

    ● Polymers
    ● Metals
    ● Ceramics
    ● Composites
    ● Batteries
    ● Pharmaceuticals
    ● Rocks and minerals
    ● Forensics
    ● Electronics and semiconductors

    Chemical analysis of these materials by SEM-EDS can be leveraged across industry, government and academic sectors for wide range of applications spanning from investigating the chemical composition of minerals in meteorites to fingerprinting forensic samples to developing next-generation energy storage solutions and beyond.

    If you are looking for an innovative SEM-EDS tool or analytical technique to help you with your research, we, JEOL USA, would recommend browsing our website.


    Ready to learn more about our Gather-X Windowless EDS? This state-of-the-art detector can help you characterize ultra-low energy characteristic X-rays that are under 1 keV, including Li-Kα. When paired with our ultrahigh resolution field emission SEM product line, this ground-breaking technique is transforming the types of materials that we can observe and study.

    For more information on SEM-EDS analysis or the SEM-EDS spectrum, we invite you to browse through our website. Check out our blog page to learn more about elemental analysis with electron microscopes, a guide on energy dispersive spectroscopy and so much more!

    Our technology can help you ensure that your materials have the right characteristics for their future applications. Contact us today to find the best SEM-EDS tool for you.

    PA3 enlarged spectrum on table

    How to Carry Out Particle Analysis with Benchtop SEM

    How to Carry Out Particle Analysis with Benchtop SEM

    PA3 enlarged spectrum on table
    Micro and nanosized particles are found in many types of materials, including food additives, metals, polymers and catalysts. In an effort to formulate novel industrial, medical and scientific applications, researchers seek to characterize the mechanical, thermal and chemical properties of these particles.
    A benchtop scanning electron microscope (or tabletop SEM) is used in industry and academia to characterize particles’ morphological, topographical, and chemical characteristics. They allow a precise determination of these characteristics while rendering stunning images of specimens.

    Sample Preparation for a Benchtop SEM

    Electron microscopy, including transmission electron microscopy (TEM) and scanning electron microscopy (SEM), is recognized as the gold standard for the characterization of particles at nanoscales (orders of 10-9 meters). Electron microscopes are versatile tools providing greater depths of field than optical microscopes, higher resolutions and a capacity to reveal chemical compositions when combined with a range of spectroscopy techniques.
    Sample preparation is an essential part of an efficient workflow when using a benchtop SEM. The sample must typically be dried. For non-conductive materials, the sample may be coated with a nanometer-thick layer of conductive carbon or metal (such as gold) to prevent spurious charging while studying the sample. Once the sample has been prepared, it is placed in the analysis chamber of the benchtop SEM. Typically, analysis is performed in a vacuum, and users may employ cryogenic methods for the preparation of sensitive materials.
    During operation of the benchtop SEM, a high-energy beam of electrons is scanned across the sample. Coaxial magnets focus the electron beam to a point as small as several nanometers in diameter. As the electron beam interacts with the sample’s surface, the signals generated are collected by various imaging and analytical detectors. Thus, high-resolution nanoscale images are formed and precise measurements are obtained.
    Particle diameters and geometries may be studied in great detail. By utilizing several images together with software, the size distribution of particles may be determined and a concentration versus particle diameter may also be calculated. A tabletop SEM enables flexible approaches to the analysis of various types of particulates in semiconductors, powders for additive manufacturing, automotive cleanliness and polymers.

    Particle Analysis Using a Benchtop SEM

    The analysis of particle size is essential to the characterization of materials. This includes the identification of foreign substances, forensic examinations and quality control in additive manufacturing, automotive/aerospace cleanliness and pharmaceuticals.
    In order to elucidate questions surrounding morphology, surface area and porosity, researchers have traditionally turned to light scattering, light obscuration or direct imaging techniques. While characterizing the size distribution of particles is essential, correlating this information with chemical composition offers valuable insights into the characteristics of materials. The combination of a benchtop SEM with energy-dispersive X-ray spectroscopy (EDS) is the ideal solution for integrating particle visualization and chemical composition analysis.
    JEOL’s Particle Analysis Software 3 (PA3) has been integrated into its Benchtop SEM/EDS platform. It enhances the capabilities of a benchtop SEM by automating the detection, chemical analysis and classification of particles, grains and other features found in materials. As part of an efficient workflow, it provides fast, unattended measurements across sizeable areas of a sample or even multiple samples.
    A typical workflow involves taking an optical image with an integrated Stage Navigation System camera. This image is used to quickly navigate regions of interest, simplifying the acquisition of benchtop SEM images and EDS spectra within an automated workflow. User-defined recipes may be utilized for specific use cases. These recipes streamline the setup, allowing less experienced users to execute a run. The software is also preloaded with materials-specific libraries such as the Metal Feature Analysis (MFA) Library, which complies with ISO 4967.
    JEOL’s PA3 software has advanced functionalities for particle characterization, including probe tracking, using shape information to include or exclude particles from EDS analyses and different methods of stopping the run (by count, morphology or element). PA3 facilitates the identification and analysis significantly increasing the throughput of benchtop SEM/EDS-based characterization.

    Learn more:

    Benchtop SEM from JEOL

    The benchtop SEM (and EDS) system from JEOL allows users to set up a compact and user-friendly lab environment without compromising data integrity. This efficient workflow guides the user from sample preparation to imaging, particle analysis and reporting.

    Composite with NeoScope

    How Benchtop SEM can Benefit Energy Storage Applications

    How Benchtop SEM can Benefit Energy Storage Applications

    Composite with NeoScope
    The quest for renewable energy sources is prompting the development of technologies capable of tapping into alternative energy sources such as solar, wind, geothermal and tidal energy. To fully exploit these energy sources, engineers need novel ways of storing and converting these energies.
    Lithium-ion batteries are generally the power source of choice for the booming market in portable electronic devices, including smartphones, smartwatches and laptops. These batteries are complex energy storage devices with unique electrochemical characteristics incorporating high-density metals, low-density polymers and other materials.
    The benchtop scanning electron microscope (benchtop SEM) is a key analytical tool in investigating materials' mechanical, chemical and electrical properties in batteries, fuel cells, supercapacitors, electrolyzers and heterogeneous catalysts.

    Characterization of Energy Storage Devices Using a Benchtop SEM

    In electrochemical systems, the critical properties affecting the quality of energy conversion processes are determined by component surfaces and their microscopic properties. The microscopic properties affecting the bulk behaviors of these components are of particular interest to materials scientists.
    Benchtop SEM anode
    Anode
    The efficiency of batteries and fuel cells is governed by the diffusion of ions, the transport of electrons and the chemical interactions of electrode/electrolyte materials. Using a benchtop SEM, engineers can characterize the structure and properties of components that shed light on their behavior during electrochemical processes. These behaviors may include ion relocation, lattice expansion or contraction, phase transition and surface reconstruction.
    In batteries, the charging and discharging processes involve the transfer of ions through an electrolyte and the interfaces between an electrode and an electrolyte. Improving the performance of batteries requires the design of electrode materials with adequate energy density and efficiently designed electrode and electrolyte configurations.
    Supercapacitors store and release energy through the accumulation and dissipation of charges at solid-liquid interfaces. To improve their performance, engineers need to design efficient interfacial structures that increase charge density (capacity) and enhance the transfer of cations and anions (power density).
    Benchtop SEM cathode
    Cathode
    Fuel cells convert chemical energy into electrical energy by oxidizing fuels such as hydrogen and alcohols. To enhance the kinetics of catalysts, engineers need to optimize their surface composition and structure.
    For heterogeneous thermal catalysts, engineers seek to control the molecular structures of catalysts and enhance support-catalyst interactions.
    These varied applications present unique challenges to materials scientists. Nonetheless, they all depend on efficient transfers and interaction of particles within materials or their interfaces at nanometer scales. The benchtop SEM is an indispensable tool in the characterization of these processes. Using a benchtop SEM, materials scientists can obtain high-resolution images and perform elemental analysis of materials at nanoscales. A benchtop SEM enables:
    • Surface imaging of an electrode
    • Imaging cross-sections of electrodes or battery cells
    • Grain structure and orientation analysis on surfaces
    • Determination of grain boundary losses
    • Defect analysis
    • Elemental analysis of surfaces
    • Chemical phase analysis
    Benchtop SEM EDS map overlay
    EDS map overlay

    Use Cases of a Benchtop SEM in Energy Storage Applications

    Batteries and fuel cells - Lithium-ion batteries are used in portable electronic devices, stationary power sources and electric vehicles. Their performance is determined by energy density, battery capacity, charge and discharge rates and the lifetime of the battery. A benchtop SEM enables the identification of defects and the characterization of nanostructures in lithium-ion batteries. 
    Cathode analysis - Cathodes undergo electrochemical stresses during lithiation and delithiation. This may lead to grain cracking, changes in pore sizes and contact loss of particles, thus reducing the lifetime of the battery. A benchtop SEM may perform particle orientation and structure analysis to track these defects.
    Anode analysis - Similarly to cathodes, anodes undergo electrochemical stresses. However, since they are typically made of graphite, their failure characteristics may be different. A benchtop SEM may help characterize defects in graphite particles that lead to defective ionic transfers, which reduce the lifetime of the battery.
    Photovoltaic solar cells - Photovoltaic solar cells are typically manufactured from crystalline silicon. The bulk behavior of these silicons is determined by their crystallinity and crystal sizes. To improve solar cell technology, materials scientists require a detailed understanding of the nanostructures, compositions and electrical properties of these silicons. Again, a benchtop SEM may help characterize these properties.
    These are a few examples of the applications facilitated by a benchtop SEM. Materials engineers may find other applications for their benchtop SEM that fulfill specific use case scenarios.

    Benchtop SEM from JEOL

    The JCM-7000 benchtop SEM from JEOL incorporates advanced functionalities that make it simple for users at any skill level to obtain outstanding images and elemental analysis results in just minutes. It is equipped with real-time 3D imaging, advanced auto functions and the option to add a fully embedded EDS system for real-time compositional analysis.
    Benchtop SEM particle analysis
    Particle Analysis

    Elemental Analysis with Electron Microscopes

    Electron Microscopy Excels at Elemental Analysis

    Electron microscopes make it possible to see extraordinary details at ultrahigh magnifications, but they also make it possible to determine more details about the material you are investigating. Scanning Electron Microscopes (SEM) and Transmission Electron Microscopes (TEM) are essentially nanolabs when outfitted with multiple analytical detectors. For example, energy dispersive X-ray detectors (EDS or EDX) are used extensively to provide insight for analysis of elements ranging from Be to U. More specialized detectors enable detection of light elements like Li, or, in the case of TEM, fast elemental mapping up to atomic resolution.

    Analytical SEM for EDS and SXES

    EDS in general is considered a semi-quantitative elemental analysis technique. SEM-EDS provides information on the elements present, their relative concentrations and spatial distribution over very small volumes (micron and some instances nanometer scale).
    Gather-X, a new Windowless EDS from JEOL, provides even higher sensitivity and low-energy X-Ray detection, and can collect the entire X-ray range produced from the ultrahigh resolution Field Emission SEM, including low-energy X-rays down to Lithium. Collection provides clear, high count rate EDS maps with high spatial resolution.
    For efficient and parallel collection of very low energy-rays a Soft X-ray Emission Spectrometer (SXES) provides the ultimate high spectral resolution (0.3eV). Ideal for Lithium Ion Battery research, it allows for the Nitrogen Kα and Titanium Lℓ line to be resolved with a separation of only 1.78eV, and also ultra-low energy, low-concentration sensitivity with the capability to detect Li even at low single digit weight percent concentration. An additional, and maybe its strongest asset, is its ability to do chemical state analysis. The spectrometer can detect subtle differences in emitted X-rays from conduction band and valence band which allows the distinction between bonding and crystal structure in samples containing the same elements.

    TEM Analytical Capability at the Atomic Level

    For Transmission Electron Microscopy, JEOL SDD detectors ranging from 60mm 2 to 158mm 2 deliver unparalleled EDX analytical results for a wide range of materials. Utilizing JEOL’s unique, on-the-fly “Lossless Drift Compensation”, large pixel EDX maps can be generated at up to atomic resolution, even for beam sensitive or 2D materials, at various accelerating voltages. In addition, JEOL’s spectrum imaging saves not only the entire spectrum data set but also each individual spectral slice, allowing for the specific summing of any number of frames collected during an experiment, which is useful for in-situ experiments.

    NMR Analysis of Lithium Ion Batteries

    NMR Analysis of Lithium Ion Batteries

    LiB: Next Generation Energy Storage

    Lithium-ion batteries (LIBs) are used to power portable electronics, electric vehicles, and grid storage solutions; they play a crucial role in driving sustainability and are an essential energy storage device. With the demand for electric vehicles and renewable energy sources continuing to rise, there is an increasing need to improve electrochemical storage. The search for new battery materials, alongside the drive to improve performance, and lower the cost of existing and new batteries, comes with its challenges.
    Lithium has one of the highest electrochemical potentials compared to other metals, making it very active. Therefore, it releases the electron from the outer shell much faster than other metals, which makes it a good choice for battery research. 6/7Li are called ‘spin spies’ because they detect changes in structure, state of deterioration, Li-ion mobility, and quantitation during charging and discharging of the battery and have guided the synthesis of new anode, cathode and electrolyte materials.
    A primary concern in finding new forms of electrolytes in secondary batteries is safety because electrolytes can leak in a battery and are very sensitive to temperature change, especially high temperatures.
    LiB: Next Generation Energy Storage

    Leveraging NMR for LiB Analysis

    One method to observe lithium ions is nuclear magnetic resonance (NMR). NMR is one of the few analytical methods to characterize the local structure and ion dynamics of LIB materials. NMR spectroscopy is crucial in studying the electrochemical and physical properties of the LIB components. NMR applications are used for three of the components of LIBs: cathode, anode, and electrolyte. The material that is being analyzed will determine the appropriate NMR technique, such as solid-state NMR, in-situ NMR, and diffusion NMR.
    Characterizing Li-ion cells and batteries can involve a galvanostatic cycle which can study the behavior of batteries being cycled. A current is applied to cause an electrochemical reaction, followed by a reverse reaction, and this is repeated until the battery degrades, usually because of temperature. NMR is used to determine the time this process will take.

    NMR: Non-Destructive Analysis

    The main benefits of NMR spectroscopy over alternative approaches are its non-destructive nature and ability to study a range of operating storage devices in situ. Further research will provide key observations that can lead to the development of more efficient, safer batteries in the future. Magic-angle spinning improves spectral resolution for solid-state samples by physically spinning the sample.
    Ex-situ NMR can uncover the charging and discharging cycle during lithium-ion battery operation. It explored the new cathode material with a multi-layer structure with domains where lithium-ion is contained.
    NMR is a valuable tool for researchers because of its high flexibility and chemical sensitivity whilst remaining non-invasive. NMR spectroscopy is a vital tool for investigating the chemical and physical properties and electrochemical performance of LIBs. It will help advance current research into finding more sustainable and efficient solutions to support the future of our planet. Further applications of NMR in battery research will support battery manufacturing and prevention of battery failures; furthermore, it will improve technologies to meet the demand for high efficiency, longer lifetime and lower costs.
    To learn more about JEOL USA’s air-isolated microscopy workflow proving its value in advanced battery research and production, check our our press release on our Science of Energy theme at Pittcon 2023!

    Designing Better Batteries through Innovative Microscopy Characterization and Analysis

    Designing Better Batteries through Innovative Microscopy Characterization and Analysis

    The drive is on to improve the performance of Lithium-ion batteries, particularly to increase energy density, life cycle, and safety. However, during development and assessment of their performance, lithium-ion batteries can present unique challenges for characterization and analysis using electron microscopy.
    The basic structure of Lithium-ion batteries (LIB) contains as many as 10 different thin films and at least that many solid−solid interfaces. These interfaces consist of thin layers of cathode material, insulating barriers, anode materials, metal current collectors, and the electrolyte. These various components are in the form of powders, sheets, and fluids and require assessment before and after assembly and after repeated charge/discharge operations. Researchers who are correlating electrochemical behavior to what is physically happening within the cell need to study the 3D microstructure of the battery components as well as the interfaces formed between those layers.
    Cross Section of Lithium Ion Battery Layers
    The efficiency of batteries and fuel cells is governed by the diffusion of ions, the transport of electrons and the chemical interactions of electrode/electrolyte materials. Engineers can routinely characterize the structure and properties of components that shed light on their behavior during electrochemical processes, including ion relocation, lattice expansion or contraction, phase transition and surface reconstruction.
    However, since materials containing Li are reactive in ambient environments, being able to prepare, image, and analyze samples without exposing them to the atmosphere becomes vitally important. For that purpose, JEOL has established an air-isolated workflow from sample preparation using ion beam milling, to characterization and elemental analysis in the Scanning Electron Microscope (SEM) or Transmission Electron Microscope (TEM), without exposing the specimen to the atmosphere. JEOL ultrahigh resolution Field Emission SEMs, equipped with our new Gather-X Windowless EDS, detect ultra-low energy elements such as lithium (with Li K line of 54 eV) . Analyzing lithium and other light elements requires low kV imaging and analysis and often high beam current achievable in JEOL’s multipurpose or analytical high resolution SEMs. 
    Learn more about JEOL's air-isolated workflow, pristine sample preparation of sensitive samples, and high resolution imaging and analysis solutions at https://go.jeolusa.com/EM-LIB.

    download6.jpg

    What Analyzers are Used for Polymer Identification?

    What Analyzers are Used for Polymer Identification?

    In the ever-evolving field of polymer science, the accurate identification and analysis of polymers are critical for quality control, research, and development. This blog will delve into the sophisticated analytical techniques used for polymer identification and highlight the principles, applications, and limitations of different polymer analysis techniques.

    Pyrolysis Gas Chromatography-Mass Spectrometry

    A crucial analytical tool that can be used for polymer identification is pyrolysis gas chromatography-mass spectrometry (Py-GC-MS).

    This technique involves the thermal decomposition of the polymer (pyrolysis), followed by the separation and identification of the resulting compounds.

    Frontier lab pyrolyzers are commonly used and paired with JEOL's Q1600GC or GC-Alpha. The msFineAnalysis AI software enhances the process by providing sophisticated data interpretation, leveraging artificial intelligence to analyze complex pyrolysis results. This method is particularly effective for identifying unknown polymers, additives, and fillers, and for understanding their thermal degradation behaviors.

    Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

    Another essential instrument in polymer characterization is matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS).

    JEOL’s SpiralTOF, coupled with msRepeatFinder software, offers high-resolution mass spectra of polymers. This technique excels in determining molecular weights and distribution, end-group analysis, and copolymer composition.

    However, it is crucial to note that as the molecular weight of a polymer increases, the oligomeric resolution declines. Eventually, it will render MALDI-TOF MS unsuitable for identifying the polymer. Only the molecular weight can be determined beyond this threshold, which varies depending on the polymer type.

    Nuclear Magnetic Resonance Spectroscopy

    Nuclear magnetic resonance (NMR) spectroscopy is another versatile tool used for polymer identification. It provides detailed information about the molecular structure, including the arrangement of atoms within the polymer.

    This non-destructive technique can differentiate between crystalline and amorphous regions in polymers and is instrumental in elucidating copolymer composition and sequence distribution. NMR is particularly useful for understanding the chemical structure and physical properties of polymers.

    Meet us at Pittcon

    The field of polymer science relies heavily on advanced analytical techniques for polymer identification. Each method, Py-GC-MS, MALDI-TOF MS, and NMR, offers unique advantages and limitations. Their application is pivotal in ensuring the quality and performance of polymer materials, contributing significantly to advancements in materials science and engineering.

    At JEOL, we are continually inspired by the endless possibilities of polymer science and the critical role of different analysis techniques for driving innovation. These tools are crucial for successfully identifying polymers.
    As we explore the frontiers of material characterization, we invite fellow experts and curious minds to join us at our booth at Pittcon this year. This is an excellent opportunity for you to engage with our team, discover our latest advancements in polymer analysis, and discuss how our cutting-edge technologies can empower your research and development endeavors.

    Together, let's shape the future of polymer science and uncover the next breakthrough in material technology. We look forward to insightful conversations and collaborations with you at Pittcon.

    References

    1. Kusch P. Pyrolysis-Gas Chromatography: Mass Spectrometry Of Polymeric Materials. Singapore: World Scientific Publishing Company; 2018. 
    2. Lattimer R, Montaudo G. Mass Spectrometry of Polymers. USA: CRC Press; 2001. 
    3. Tonelli A. NMR Spectroscopy and Polymer Microstructure: The Conformational Connection. USA: Wiley-VCH; 1989. 
    4. Stuart B. Infrared Spectroscopy: Fundamentals and Applications. USA: Wiley; 2004.

    Fig 4a.png

    Using Cryo-EM for Drug Discovery

    Using Cryo-EM for Drug Discovery

    Cryo-electron microscopy (cryo-EM) is an advanced high-resolution imaging technique that is used to uncover the characteristics of different molecules. Cryo-EM can preserve samples for analysis by maintaining them under cryogenic conditions. This way they can retain their properties as if they were still in their native environments.

    The basics of cryo-EM involve a beam of high-energy electrons used on biological molecules. These electrons help create a three-dimensional (3D) model of a molecule at near atomic resolution. The method also doesn’t require crystallization of biomolecules. Instead, they are preserved through flash-freezing in liquid ethane. This can stop ice crystals from forming and allow high-resolution structural studies of complex biomolecules.

    Thanks to its high-resolution and ability to maintain and analyze molecules, viruses, cells, and proteins, cryo-EM is routinely used to study protein structures and show how they interact with drugs. They can also help us visualize intractable targets so we can learn about how they are formed. Without using tools like x-ray crystallography that require crystallization of biomolecules, it would have been impossible to learn about these targets. But now we can!

    Cryo-EM has already advanced discoveries in structural biology and molecular biology, so much so that it was recognized by the 2017 Nobel Prize in Chemistry. The market for cryo-EM is growing, to the point that when we reach 2028 it will be worth £2.1 billion. It is fueled by the need for innovative imaging tools that utilize high-resolution to study drugs and medications.

    With that said, if you are interested in utilizing the capabilities of cryo-EM for drug discovery, we invite you to read on. In our article, you can learn more about cryo-EM’s enhanced technology. Alongside this, you will see how it is applied to creating and researching different drugs or therapeutics.

    Technological Advancements in Cryo-EM

    Recent advancements in transmission electron microscopes have been crucial in propelling cryo-EM to the forefront of drug discovery. These microscopes utilize a beam of electrons to achieve high-resolution images of biological samples.
    When combined with direct detector cameras and advanced image processing algorithms, they enable scientists to visualize 2D images that can be reconstructed into detailed 3D structures. These images demonstrate cryo-EM’s contribution to the “resolution revolution”. With its high-resolution, it has helped to facilitate the structure determination of nucleic acids, small molecules, and other critical components of molecular biology.

    From 2D Images to 3D Structures: The Power of Cryo-EM in Drug Design

    Cryo-EM has the ability to generate 3D reconstructions from 2D images. These models enable researchers to observe the intricate details of how drugs interact with their biological targets. This technique is invaluable for determining the atomic structure of biomolecules and enhancing targeted drug design. As a result, it can allow for the development of therapeutics with unparalleled specificity and efficacy.

    Unlocking the Secrets of Membrane Proteins

    ViMembrane proteins are vital for numerous biological functions and a primary target in drug development. Studying membrane proteins has always been challenging because of their complex nature. Cryo-EM, with its use of liquid nitrogen for preserving the samples under study, offers a robust solution for visualizing these proteins in their natural lipid environment.

    Confronting Drug Resistance with Structural Insights

    The battle against drug resistance is a major concern in treating various diseases. Cryo-EM provides a window into the molecular changes that lead to resistance. It can offer clues for designing drugs that can bypass or overcome these obstacles.
    Ultimately, cryo-EM can aid in the development of next-generation therapeutics. This is through detailing the structural biology of resistant pathogens or cancer cells.

    Cryo-EM: Shaping the Future of Drug Discovery

    Despite the high costs and specialized expertise required, the potential of cryo-EM in the field of drug discovery and structural biology remains vast. As access to transmission electron microscopes and computational analysis tools improve, cryo-EM's contributions to drug development are expected to grow exponentially.

    Cryo-EM is the Key to Innovation in Drug Discovery

    BatteryPhaseExample (NeoScope).png

    Visualizing Elements Distributions with SEM-EDS Mapping

    Visualizing Elemental Distributions with SEM-EDS Mapping

    Elemental distributions can tell us a lot about the formation of different materials. By understanding the distribution and abundance of the elements found in a material at the microscopic scale, we can better understand its material properties. Essentially, elemental analysis is the key to predicting a material’s macroscopic behavior.

    Pairing Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) can produce maps showing the distribution of the different elements that are present within a material with sub-micrometer resolution. SEM-EDS mapping is fast, high-resolution, non-destructive and can readily be integrated with SEM images and other microanalysis techniques to fully characterize samples.

    Read on to learn more about SEM-EDS mapping and elemental distributions!

    The Principles of SEM-EDS Mapping

    At its core, SEM-EDS mapping utilizes an electron beam to excite and analyze X-rays characteristic of the sample composition. By analyzing the composition at every pixel within an image to create EDS maps, variations in composition can be easily visualized. Recent advancements in EDS detector design and efficiency mean that this method is fast, yielding real-time data in seconds. Integration with complementary SEM imaging detectors provides unmatched insights into how composition relates to morphology and structure, allowing for comprehensive characterization.

    Advancements in SEM-EDS Technology: Automated Solutions

    The advent of advanced AI-powered autofocusing and alignment routines allows users to leverage automated solutions that improve workflow efficiency and reduce the expertise needed to collect SEM-EDS data. Software-integrated automated imaging and EDS mapping solutions such as Simple SEM allow users the flexibility to create and implement custom automation routines within an intuitive user interface. For more advanced applications like automated particle analysis, users can develop custom automation routines in Python or opt for user-friendly solutions like Particle Analysis Software 3 (PA3). PA3 in particular offers rapid particle identification and classification, enabling high through-put analysis of millions of particles. These solutions streamline research and development across various fields, increasing productivity without sacrificing data quality.

    Impact of SEM-EDS Across Industries

    The application of SEM-EDS mapping is vast and varied, including but not limited to:
    • Automotive manufacturing: Assess component cleanliness, identify contamination that may lead to component failure.
    • Additive manufacturing: Optimize materials for better product quality. 
    • Pharmaceutics: Ensure the uniformity of drug formulations and identify contaminants. 
    • Forensics: Identification and examination of trace evidence and gunshot residue. 
    • Electronics: Characterize device structure, identify contaminants and defects.
    • Battery: Characterize battery materials, ensure clean battery manufacturing.

    Navigating the Complexities of SEM-EDS Mapping

    The successful application of SEM-EDS mapping requires a thorough understanding of both its capabilities and limitations. Software solutions including automatic peak identification and deconvolution as well as intuitive data reporting have greatly helped simplify EDS map processing. Utilizing cluster or vertex component analyses using Phase Analysis 2 software enables more advanced processing, including automatic identification and characterization of discrete chemical phases within a sample. However, with all of these solutions proper sample preparation and skilled data interpretation are still essential to fully leverage the technology and derive accurate, meaningful insights. With JEOL’s advanced application training courses, we ensure that every user is empowered to get the most out of their SEM, regardless of prior experience.

    The Future of SEM-EDS Mapping

    As technology continues to advance, the capabilities of SEM-EDS mapping are expected to expand further. This will not only broaden its application range but also deepen our understanding of material properties, reinforcing its indispensable role in the progression of various scientific and industrial sectors.

    SEM-EDS mapping is undeniably a cornerstone technique in modern material science. This method offers a comprehensive view of material structures at the micro and nano levels. Its ongoing development is pivotal for fostering innovation.

    Learn more about Elemental Distributions Through SEM-EDS Mapping

    SEM-EDS mapping is an extremely reliable method of identifying the distributions of elements in different materials. With its versatility comes the ability to apply it to different areas. For instance, SEM-EDS mapping can be used to ensure battery devices are defect-free and then immediately be used to improve the lifespan of an electric vehicle battery.

    To maintain the quality of SEM-EDS mapping, we must keep thinking of ways to improve its capabilities. Right now, there have already been some developments in SEM-EDS mapping. This includes the incorporation of AI-related technologies, like machine learning, and introduction of windowless EDS detectors to expand their sensitivity and detection capabilities.

    Now that you understand SEM-EDS mapping, it is time to find a tool that can be applied to your own research. If you are interested in EDS mapping in particular, we, JEOL, would like to recommend our own EDS detector: Gather-X Windowless EDS.

    The Gather-X Windowless EDS can be utilized for identifying characteristic x-rays. It has been designed to improve the amount of time it takes to receive data and can also decrease the harm that could be done to a beam sensitive material. Its sensitivity at low accelerating voltages and efficiency analyzing ultralow energy X-rays including lithium (Kα) make it uniquely suited for a range of applications including ultrahigh resolution EDS mapping and characterization of Li-ion battery materials.

    To learn more about our Gather-X Windowless EDS, please feel free to contact us at any time. Moreover, you can explore our recent articles to learn about SEM-EDS mapping or related topics. To offer a few examples, we provide more detail about:


    Browse our blogs to expand your knowledge on SEM-EDS mapping. Then you can move onto finding the right SEM-EDS mapping tool that can be used in your own work.

    © Copyright 2024 by JEOL USA, Inc.
    Terms of Use
    |
    Privacy Policy
    |
    Cookie Preferences