JEOL USA Blog

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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

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Why Polymer Identification Matters

Why Polymer Identification Matters

Polymer science is on the frontier of material innovation. It runs the gamut from the every day to the cutting edge. Everything from commodity plastics to life-saving bio-polymers has undergone strenuous analysis and testing.

Polymers are essentially long chains of repeating molecular units. Their intrinsic properties (elasticity, tensile strength, thermal resistance, etc.) differ based on that molecular architecture. The ubiquity of different monomers – the sub-units in a polymeric chain – and their remarkable structural flexibility is what makes polymers so versatile.

This same variety poses challenges. Minor structural differences can dramatically alter polymer properties. Low-density and high-density polyethylene, for instance, are highly distinct from one another despite their similar chemical make-ups. This is due to structural variances. These seemingly minor differences can be make or break in fields like biodegradable plastics, where accurate identification ensures environmental safety. Likewise, in aerospace, material endurance under extreme conditions is non-negotiable.

Advanced polymer identification has deepened our understanding of these essential materials. Let's explore that importance in more depth.

Understanding the Need for Accuracy in Polymer Science

Quality Assurance in Polymer Products

Confirming the composition and identity of polymers is an essential quality check. Qualifying raw materials helps ensure end-product integrity, while minimizing the ethical, financial, and regulatory risks of getting it wrong.

Advanced techniques like Fourier Transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC) are frequently deployed in polymer characterization to screen molecular structures and thermal properties. They are commonly used in packaging, healthcare, and electronics sectors, where polymer properties are fundamental to performance and safety.

For example, FTIR detects contaminants in polymers, ensuring purity, while DSC assesses thermal stability, which is crucial for product safety. Inaccurate polymer identification, especially in healthcare, can lead to device failures, posing serious risks to patient safety.

Verification of Labeling and Specifications

Verification is an essential step in compliance. This is true of any market – although there are higher stakes in tightly regulated markets like the medical sector. Verifying that polymeric materials are correctly labeled is a core part of this process.

Gas chromatography-mass spectrometry (GC-MS) and thermogravimetric analysis (TGA) are critical techniques utilized to ensure product specifications. These methods help to determine polymers' composition and thermal stability. This ensures compliance with regulatory standards and instills consumer confidence in product reliability. GC-MS separates and identifies polymer components, while TGA assesses changes when polymers are heated. Incorrect labeling can lead to regulatory penalties and loss of consumer trust.

For instance, accurate labeling in medical devices is crucial to prevent harmful reactions and ensure patient safety.

Evaluating Material Suitability for a Sustainable Future

Assessing a material’s suitability in a sustainable, circular economy is becoming increasingly important. Understanding the recyclability and biodegradability of polymers is paramount. Techniques like life cycle assessment (LCA) and environmental stress-cracking resistance (ESCR) testing are used to evaluate polymers' environmental impact and longevity in various applications.

Advancements in Polymer Analysis Technologies

Polymer analysis technologies have evolved to provide more detailed and accurate insights into polymer structures and properties. JEOL's solutions in polymer characterization exemplify these advancements:

Field-Emission Scanning Electron Microscopy (FE-SEM)

FE-SEM enables users to observe surface structures with minimal specimen damage. This is ideal for assessing topographic features non-destructively.

Transmission Electron Microscopy (TEM)

TEM is essential for observing the native structure of water-containing specimens, which is crucial in industries like cosmetics and adhesives.

Direct Analysis in Real Time-Mass Spectrometry (DART-MS)

DART-MS is a rapid and effective technique used to determine the chemical composition of nearly any type of sample with little to no sample preparation. It can be used to detect contaminants and additives in polymers. 

Gas Chromatography-Mass Spectrometry (GC-MS)

GC-MS combines gas separation and mass detection, by using quadrupole mass analyzers, to identify and measure the concentration of compounds. It can be leveraged to detect polymer additives and ensure product safety. 

Gas Chromatography-Time of Flight Mass Spectrometry (GC-TOFMS)

GC-TOFMS enables users to separate complex mixtures and detect compounds. It can also be used to quantify known compounds and identify unknown ones. With that said, it is a crucial tool for expanding our understanding of novel polymer blends.

Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (MALDI-TOFMS)

MALDI-TOFMS provides novel insights into molecular weight (MW), copolymerization composition, and structural distribution. Additionally, it can detect synthetic byproducts, impurities, and admixtures. 

Nuclear Magnetic Resonance (NMR)

NMR is a mainstay in the polymer scientists' toolset. It provides detailed information on chemical states, differentiating between crystalline and non-crystalline states.

X-ray Photoelectron Spectroscopy (XPS) and X-ray Fluorescence (XRF)

X-ray analysis is essential for surface composition and non-destructive quantitative additives analysis.

Interested in Polymer Identification?

If you have enjoyed this deep dive into polymer identification and want to learn more, speak to the team. Feel free to contact us directly. Or, if you would like to discuss the topic in person, drop into our booth at Pittcon. We would be happy to discuss the latest trends in polymer analysis and how our solutions can help address your needs in this ever-evolving field.

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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.

High resolution backscattered electron image and corresponding EDS overlay map of a tungsten plug area

Why Use SEM-EDS for Advanced Materials Analysis?

High resolution backscattered electron image and corresponding EDS overlay map of a tungsten plug area
High resolution backscattered electron image and corresponding EDS overlay map of a tungsten plug area with multiple Al and Ti layers on a semiconductor device. The middle Ti layer (purple) is only ~30 nm wide.
Scanning Electron Microscopy with Energy-Dispersive X-ray Spectroscopy (SEM-EDS) has become increasingly pivotal in advanced materials analysis. This combination offers a robust methodology for the microstructural analysis of various materials. SEM-EDS plays a critical role in identifying elemental compositions and understanding the microstructural characteristics of materials, essential in areas such as materials science, metallurgy, and nanotechnology.

Fundamental Principles of SEM-EDS

SEM-EDS integrates two sophisticated techniques: Scanning Electron Microscopy (SEM) and Energy-Dispersive X-ray Spectroscopy (EDS). SEM provides high-resolution images of the material's surface by scanning it with a focused electron beam. The interactions between the electrons and the atoms in the sample generate multiple signals, including secondary electrons, backscattered electrons, and characteristic X-rays. EDS analyzes the X-ray signals, enabling the determination of the sample's elemental composition. The synergy of SEM and EDS furnishes a comprehensive understanding of the surface topography and elemental composition of materials.

Advantages of SEM-EDS in Materials Science

  • High Spatial Resolution: SEM offers exceptional spatial resolution, crucial for analyzing nanostructured materials and microscale features.
  • Elemental Analysis: EDS provides qualitative and quantitative elemental analysis, which is vital for understanding the composition of complex materials.
  • Versatility: SEM-EDS applies to various materials, including metals, ceramics, polymers, and composites.
  • Non-destructive Technique: SEM-EDS is a non-destructive analytical method, preserving the integrity of the sample for future investigations.

Applications of SEM-EDS in Advanced Materials

The applications of SEM-EDS in advanced materials are diverse and significant. In failure analysis, SEM-EDS is a critical tool for diagnosing failure mechanisms in materials. It can identify elemental segregation or impurities at fracture surfaces, providing insights into the causes of material failure. This information is crucial for improving material properties and performance.
In the realm of nanostructured materials, SEM-EDS plays an essential role in characterizing the composition and morphology of these materials. Understanding the intricate details of nanostructures is vital for advancements in nanotechnology and the development of novel materials with enhanced properties.
Additionally, SEM-EDS is widely used in coating analysis. It analyzes the thickness, uniformity, and composition of coatings applied to various substrates. This is particularly important in industries where coatings enhance material properties, such as corrosion resistance or electrical conductivity.

Limitations and Considerations

While SEM-EDS is a powerful tool, it has limitations:
  • Elemental Detection Limit: EDS has a limited detection capability, especially for light elements.
  • Depth limitation: This technique cannot be used to determine elemental concentration of a bulk sample. The volume of interaction depends on the material investigated and the accelerating voltage used, making this technique sensitive to within microns from the surface only. 
  • Quantitative Analysis: Quantitative elemental analysis can be challenging due to various factors like X-ray absorption and fluorescence. Accurate quantitative analysis requires meticulous sample preparation to avoid artifacts.

Future Prospects in SEM-EDS Technology

Ongoing advancements in SEM-EDS technology focus on enhancing resolution, sensitivity, and quantitative capabilities. Developments in detector technology and software algorithms are poised to address current limitations, paving the way for more sophisticated analyses.

Process Flow of AMS7032 Operational Qualification (OQ) Testing

AMS7032: Understanding Aerospace Industry Standards in the Age of Metal Additive Manufacturing

Metal additive manufacturing, also known as 3D printing, has emerged as a transformative force in the manufacturing industry of the 21st Century. It is an innovative technology characterized by its unique layer-by-layer construction. Industries such as automotive, medical devices, and notably, aerospace, are adopting metal 3D printing for its ability to meet high quality, precision, and compliance demands in a cost-effective manner.
The additive manufacturing process, particular with metal powders, poses questions when it comes to aerospace industry standards. Aerospace manufacturers employ this technique not only for its precision in depositing thin layers of material but also for its efficiency in mass production. Ensuring adherence to strict design specifications and user requirements, metal 3D printing utilizes electron beam and energy deposition technologies for equipment qualification and process control.
To reach this rigorous level of precision and compliance, aerospace manufacturers leveraging metal 3D printing adhere to standards set forth by the Society of Automotive Engineers (SAE). These standards are vital in evaluating whether the additive manufacturing technologies can produce materials that meet the rigorous material specification requirements necessary for a production environment.
Standard AMS7032 has been developed to serve this purpose. It is proposed as a foundational guideline for aviation manufacturers, offering a pathway to regulatory compliance and establishing a framework for standardization across the aerospace sector. This standard encapsulates the essentials of the additive manufacturing process, from ensuring the quality of metal powders to defining the serial number tracking for enhanced process control. It underscores the importance of each step in achieving a wide range of high-quality, cost-effective production outcomes, tailored to meet the varied and complex demands of the aerospace industry.

Achieving AMS7032 Operational Qualification

AMS7032 mandates several prerequisites for preparing an aerospace 3D metal printing manufacturer for qualification, including performing an installation qualification, trained operators, compliant facility controls, accredited post processing and testing laboratories, key process variable characterization, and equipment and material setup.
To perform the operational qualification (OQ) per AMS7032, three builds with various test coupons were printed back-to-back and sent to a test lab for radiographic, mechanical, metallurgical, and chemical composition analysis.
Process Flow of AMS7032 Operational Qualification (OQ) Testing
Process Flow of AMS7032 Operational Qualification (OQ) Testing

Assessing JEOL’s Electron Beam Melting Technology

The full details and results of the AMS7032 OQ testing process are too broad to include in a single blog post, so we’ve developed a white paper reviewing that not only showcases the JAM-5200EBM's capabilities but also provides crucial insights for researchers, engineers, and enthusiasts in the field.
This white paper explores:
  • Qualification Process Flow: Learn about the meticulous steps taken in the OQ, including the design of three builds using Ti6Al4V powder, adherence to AMS7032 requirements, and post-processing steps such as Hot Isostatic Pressing (HIP).
  • Testing and Acceptance Criteria: Explore the rigorous testing requirements for tensile properties, chemical composition, radiography, and microstructure analysis. The white paper details adherence to AMS7011 specifications and acceptance criteria for each parameter.
  • Qualification Results: Discover the outcomes of the JAM-5200EBM's operational qualification, including machine operation results, tensile results meeting or exceeding minimum requirements, and compliance with chemical composition and microstructure standards.
While this blog post provides a glimpse into the key points of our white paper, the complete story and detailed data are available in the document itself. We invite you to download the white paper to gain a comprehensive understanding of the JAM-5200EBM's AMS7032 compliance and its potential impact on the future of additive manufacturing.

Advantages of Benchtop Scanning Electron Microscopy

Pharmaceutical Imaging and Analysis: Advantages of Benchtop Scanning Electron Microscopy vs. Optical Microscopy

Optical microscope image (left) vs. Scanning Electron Microscope (SEM) image (right) of pharmaceutical tablet
Throughout the discovery and manufacturing phases of bringing pharmaceuticals to market, scanning electron microscopy (SEM) plays a pivotal role in design and quality control. For visual inspection, the benchtop SEM far surpasses the capabilities of traditional optical or light microscopy with its large depth of field and functionality.

Quality Imaging and Resolution

With the JEOL NeoScope Benchtop SEM it is possible to observe the compositional contrast that cannot be seen on an optical image. Examination of a pharmaceutical tablet or powder sample in the benchtop SEM reveals greater detail and compositional contrast than can be achieved with optical microscopes, even at the same magnification. With magnification up to 100,000X and versatile, automated settings, the SEM makes it possible to easily inspect the microstructure of tablets and powders, textures and coatings, foreign particles, and their chemical composition. Using the benchtop SEM, it is possible to identify the source of contamination from manufacturing processes.

Focus on MXenes, Materials, and Scanning Electron Microscopy

Focus on MXenes, Materials, and Scanning Electron Microscopy

Flower power; Vanadium oxide nano structure synthesized from two-dimensional vanadium carbide MXenes; Yeonjin Baek, Auburn University; JEOL JSM-7000F SEM – November 2023 Contest Winner
MXene Golden Swan; In a moonlight canvas, presenting a multilayered titanium carbide Ti3C2Tx MXene visualized as a golden swan. This MXene is synthesized by the selective etching of the optimized Ti3AlC2 MAX phase. The moon is a digital photo of a MXene film. MXene Swan’s serenade, where beauty and moonlight dance in perfect harmony! Team: Nithin Chandran B S, Dr. Anupma Thakur and Prof. Babak Anasori ; CREDIT: Nithin Chandran B S, IUPUI and Purdue University; METHOD/INSTRUMENT: JEOL JSM-7800F
You might imagine a familiar shape when you look at any SEM image: Polymer “needles” become a field of Christmas trees; a tomato pollen tube resembles a lean Siamese cat. It’s even easier to visualize when the microscopist adds color to define shapes in the image. But one subject in particular seems to suggest likenesses when imaged in the SEM. For this reason MXene images are frequent contestants in the JEOL Image Contest. 
MXenes are a relatively new family of 2D crystalline nanomaterials that are just a few atoms thick and have jagged accordion shapes that when colored, can look like goldfish, bouquets of flowers, dinosaurs, and even sunsets. This November one MXene image “Flower Power” submitted by Yeonjin Baek, Graduate Research Assistant at Auburn University, won the JEOL contest.
Another sci-art “MXene Golden Swan,” submitted by Dr. Anupma Thakur and Nithin Chandran from Indiana University-Purdue University in Indianapolis (IUPUI), won the Science as Art contest during the Materials Research Society (MRS) Fall 2023 conference in Boston.

Synthesizing MXenes

AFM (Atomic Force Microscopy) image of Single layered Niobium carbide MXenes after delamination
We asked Yeonjin Baek about her work at Auburn University, where she focuses on synthesizing and developing different types of MXenes for energy storage applications.
She explained that more than 100 possible MXene compositions have been predicted and more than 30 have been experimentally obtained.
 “They are easy to synthesize in the lab,” says Yeonjin. Her work is helping to create a library of MXene materials to study for their applications with potential use in sensors, water purification membranes, and energy storage, including cathodes in lithium-ion batteries, and supercapacitors.
“The property of MXenes can be tuned by the choice of M,X element and surface terminal groups. Multilayer MXenes are typically imaged in the SEM, but “if you want to look at a single layer of MXene flakes you need to delaminate (or exfoliate) it and then look at it in the AFM. It looks like plate-like sheets.”

The first 2D MXenes were discovered in 2011 at Drexel University, creating an entire family of new materials with a chemical formula of Mn+1XnTx (M covers groups 3 to 6 transition metals, X is carbon or nitrogen, and T represents the surface terminations). (https://link.springer.com/article/10.1007/s41127-022-00053-z)

Yeonjin shared a visual explanation of how MXenes are made:
What is MXenes?
Synthesis of MAX Phase and MXenes

Rise in Populartiy of MXenes Due to Energy Applications

There is no doubt a rise in popularity of MXenes in the world of material science, where all the MXene researchers seem to know one another.
Why are MXenes showing promise for future applications? Yeonjin Baek at Auburn University explains that they have a large surface area, excellent electrical conductivity, hydrophilicity, unique mechanical and thermal properties, an easily accessible structure, and versatile compositions.
Dr. Anupma Thakur, a Postdoctoral Research Associate at IUPU, notes that, “The focus of MXenes at universities is expanding due to its exciting material properties. The field of MXene synthesis is dynamic, with ongoing efforts to explore new precursors, improve scalability, and develop novel functionalization strategies to expand the range of applications for these 2D materials.”
MXene Chronicle; A multilayered titanium carbide. MXene is visualized as a chronicle.
MXene Chronicle; A multilayered titanium carbide. MXene is visualized as a chronicle. The two-dimensional (2D) Ti3C2Tx MXene layers were formed by selective etching of Al layers from the Ti3AlC2 MAX phase using hydrofluoric (HF) acid. Scale:10 micrometers; CREDIT: Nithin Chandran BS, Dr. Anupma Thakur, and Prof. Babak Anasori Indiana University-Purdue University Indianapolis, IUPUI, FE SEM – April 2023 Contest Winner
MXene Nanosaurus; A two-dimensional (2D) multilayered titanium carbide (Ti3C2Tx) MXene is visualized as a nanosaurus dinosaur.

MXene Nanosaurus; A two-dimensional (2D) multilayered titanium carbide (Ti3C2Tx) MXene is visualized as a nanosaurus dinosaur. The Ti3C2Tx MXene was synthesized by selective etching of Al layers from the Ti3C2Tx MAX phase using hydrofluoric acid. With the growing family of MXenes as engineered and tunable 2D ceramics, the future for the field of ceramic engineering is at the nanoscale. Our Team: Anupma Thakur, Nithin Chandran B S, and Prof. Babak Anasori; Anupma Thakur, Purdue University; JEOL FESEM

Dr. Thakur and Nithin Chandran B S sent us an explanation of how MXenes are made and also shared their recent research on the step-by-step guide for the optimized synthesis of Ti3C2Tx MXene:

MXenes are typically synthesized through a process involving the selective etching of MAX phases, which are layered ternary carbide precursors. The most common MAX phase used is titanium aluminum carbide (Ti3AlC2). The synthesis process involves several key steps:
  • MAX Phase Synthesis: The process begins with the synthesis of MAX phases, which are layered compounds with a composition of M(n+1)AXn, where M is a transition metal, A is an A-group element (usually aluminum), and X is either carbon or nitrogen. 
  • Selective Etching: The MAX phase is then subjected to a selective etching process, where the A element (typically aluminum) is removed by using strong acids or other etchants. This leaves behind a layered structure with the transition metal and carbon/nitrogen layers, forming the MXene. 
  • Delamination: After etching, the MXene is often delaminated to increase the interlayer spacing and enhance its properties. Delamination can be achieved through mechanical or chemical methods, such as ultrasonication, intercalation with specific molecules, or other exfoliation techniques. 
  • Surface Functionalization: To tailor the properties of MXenes for specific applications, researchers often perform surface functionalization by introducing different functional groups to the MXene surface. This can enhance stability, improve compatibility with other materials, or modify electronic properties. The choice of precursors, etching agents, and additional processing steps can influence the properties of the resulting MXene, allowing researchers to customize MXenes for various applications, from energy storage to sensing and catalysis. 

Further reading:

An SEM User’s Guide to Energy Dispersive Spectroscopy

An SEM User’s Guide to Energy Dispersive Spectroscopy

EDS innovations for advanced materials characterization

SEM column and typical EDS spectra
SEM column and typical EDS spectra
Scanning electron microscopy (SEM) is a cornerstone of microscopic analysis. It revolutionized the field by enabling researchers to delve deeper into materials than was previously possible. This was primarily due to its unprecedented resolution, courtesy of the innovative electron beam at the heart of any SEM system. But the power of SEM technologies stretches beyond resolution into sheer versatility. Many companion systems have emerged which continue to push that technological letter. One such system is energy dispersive spectroscopy (EDS).
EDS is a method that significantly expands the analytical capabilities of electron microscopy by facilitating elemental analysis and characterization. This article is an overview of the method suitable for beginners.

Understanding SEM: The Foundation

Firstly, you may benefit from a recap of SEM functionality. The principle of SEM operation revolves around using a focused beam of high-energy electrons that interacts with sample surfaces. This interaction generates various signals, each providing unique and valuable data. An electron gun generates the primary electron beam in SEM; typically employing a tungsten filament or a more refined field emission source for sharper imaging.
The diverse types of signals produced in SEM are crucial for different analytical aspects. Secondary electrons, primarily used for imaging, offer detailed insights into the sample's surface topography and morphology. Backscattered electrons indicate atomic number contrast and are invaluable in understanding the composition and phase distribution within the sample. Characteristic X-rays, which are central to EDS techniques, play a pivotal role in elemental analysis. Additionally, cathodoluminescence, another signal type in SEM, can reveal information about the electronic structure of materials.
An SEM's design includes several key components: the electron source for generating the primary electron beam; electron lenses to focus and direct this beam onto the sample; a sample chamber kept under vacuum where the sample is placed and manipulated; and various detectors that capture the different signals such as secondary electrons, backscattered electrons, and X-rays.

Energy Dispersive Spectroscopy: Expanding SEM’s Horizons

EDS data for cross section of lithium-ion battery
EDS data for cross section of lithium-ion battery
Energy dispersive spectroscopy, often integrated into SEM systems, is a qualitative and quantitative analytical technique for elemental analysis. When the electron beam of the SEM interacts with the sample, it displaces inner-shell electrons, causing the atom to emit characteristic X-rays. EDS detects these X-rays, allowing for the determination of the elemental composition of the analyzed volume.

EDS Components and Operation

  1. Detector: The heart of EDS, typically a Silicon Drift Detector (SDD), is responsible for capturing emitted X-rays.
  2. Pulse Processor: Converts the X-ray signals into a digital spectrum.
  3. Data Analysis Software: Interprets the spectrum, identifying peaks corresponding to specific elements.

Advantages of EDS in SEM:

  1. Non-destructive Analysis: EDS is a non-invasive method that maintains the sample's integrity.
  2. Elemental Mapping: Provides spatial distribution of elements, enhancing the understanding of material composition.
  3. Quantitative Data: Offers quantitative information about the elements present in the sample.

Pioneering SEM-EDS Innovation with Gather-X Windowless EDS

At JEOL, we recognize the importance of advanced analytical capabilities in SEM technologies. This is exemplified by our Gather-X Windowless EDS system, a testament to our commitment to pushing the boundaries of scientific exploration. Specifically designed for JEOL SEMs, Gather-X embodies a leap forward in sensitivity and resolution, especially in detecting low-energy X-rays down to Lithium. This capability is not just an incremental improvement but a significant advancement in elemental analysis. It enables researchers to explore new frontiers in materials science, nanotechnology, and beyond.
SEM image and corresponding EDS analysis of lithium in sample
SEM image and corresponding EDS analysis of lithium in sample
The 100mm² windowless EDS of Gather-X, tailored for our IT800 series FE SEMs, offers an expansive X-ray range collection, including those challenging low-energy X-rays. Its novel racetrack design and integrated controls facilitate collection at working distances as short as 1mm, yielding clear, high-count-rate EDS maps with exceptional spatial resolution. This feature is crucial for detailed material characterization and understanding intricate material properties at the nanoscale.
Gather-X's integration into our SEM Center software with Live Analysis enhances user experience, allowing real-time display of EDS spectra or maps concurrently with SEM imaging. This seamless integration underscores our commitment to delivering user-friendly, high-performance analytical tools. The system's flexibility, demonstrated by its compatibility with multiple JEOL EDS detectors, further amplifies its utility across various research and industrial applications.
With features like a large solid angle for higher count rates and fast collection times, Gather-X minimizes potential beam damage to sensitive specimens. The system's unique electron trap design permits EDS data collection under normal analysis conditions without harming the detector, even at high beam voltages up to 30kV. Moreover, the capacity for short working distance/beam deceleration mode analysis ensures safe operation at close quarters, vital for ultrahigh-resolution SEMs.
In essence, JEOL's Gather-X Windowless EDS, an exclusive design for our SEMs, exemplifies our ethos of blending smart, flexible, and powerful technology. This system not only delivers high sensitivity and spatial resolution for both imaging and analysis but also symbolizes JEOL's dedication to advancing the field of electron microscopy with intelligent and versatile solutions.

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Optimizing NMR Processing: Techniques and Best Practices

Optimizing NMR Processing: Techniques and Best Practices

Nuclear Magnetic Resonance (NMR) is a powerful analytical tool used by scientists across various fields. It provides detailed information about the structure, dynamics, reaction state, and chemical environment of molecules. However, the quality of the results obtained from NMR largely depends on the efficiency of NMR processing. This article delves into the techniques and best practices for optimizing NMR data processing.

Understanding the Importance of NMR Processing

NMR processing is a critical step in the analysis of NMR data. It involves the transformation of raw NMR data into a format that can be interpreted and analyzed. This process includes several steps such as Fourier Transform (FT), phase correction, baseline correction, and spectral alignment, among others. The quality of NMR processing can significantly impact the accuracy and reliability of the results obtained from NMR analysis.

Key Techniques for Optimizing NMR Processing

Chemical Shift Referencing

Accurate chemical shift referencing is crucial for reliable NMR data interpretation. Scientists often use a known reference compound, such as TMS (tetramethylsilane), to calibrate the chemical shifts of their NMR spectra.

Phase and Baseline Correction

Phase and baseline distortions in NMR spectra can compromise the quality of the data. These distortions can be corrected manually or using automated algorithms available in NMR processing software.

Spectral Alignment

Spectral alignment is used to correct for small shifts in chemical shifts caused by instrument drift or sample variability. This technique can improve the accuracy of peak identification and quantification.

Spectral Binning

Spectral binning involves dividing NMR spectra into small regions and calculating the area under the curve (AUC) in each bin. This technique can be useful for extracting peak intensities from multiple spectra prior to performing multivariate statistical analysis.

Scaling and Normalization

Appropriate scaling and normalization techniques ensure that NMR spectra are comparable and suitable for further analysis. Different scaling methods, such as Pareto scaling, may be used depending on the specific application.

Scaling and Normalization

Appropriate scaling and normalization techniques ensure that NMR spectra are comparable and suitable for further analysis. Different scaling methods, such as Pareto scaling, may be used depending on the specific application.

Optimizing Data Acquisition Parameters

Adjusting NMR data acquisition parameters, such as relaxation delay, number of scans, and spectral width, can optimize the signal-to-noise ratio and resolution. This can improve the quality of the acquired data and facilitate accurate data processing.

Utilizing Advanced Data Processing Techniques

Advanced data processing techniques, such as Fourier Transform (FT), 2D NMR analysis, and statistical analysis methods like Principal Component Analysis (PCA), can extract more information from your NMR data.

Staying Updated with Best Practices

Keeping up-to-date with the latest research and best practices in NMR data processing is essential. Attend conferences, workshops, and webinars, and engage with the scientific community to learn about new techniques and approaches.

The Role of NMR Processing Software

NMR processing software plays a crucial role in optimizing NMR data processing. For instance, Delta™ NMR Data Processing Software from JEOL is a powerful tool that can help you process and analyze your NMR data more efficiently. It is user-friendly and compatible with our ECZ, ECS, ECA, and ECX series NMR Systems.

The Path to Optimized NMR Processing

By implementing these techniques and best practices, you can optimize your NMR data processing workflow and obtain more accurate and reliable results. We encourage you to explore the capabilities of Delta™ NMR Data Processing Software to enhance your NMR data processing and analysis.

The journey to optimized NMR processing is a continuous one, marked by learning, adapting, and implementing the best practices in the field. Stay engaged with the scientific community, keep abreast of the latest research, and strive for excellence in your NMR data processing endeavors.

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