Experimental methods in nanomaterials

Understanding Nanoparticles & Nanomaterials Through Advanced Characterization Techniques ✍️🔬⚛️ Every nanomaterial tells a story—but no single characterization technique can reveal the complete picture. This note presents a comprehensive roadmap for understanding the structure, morphology, composition, surface chemistry, optical, magnetic, thermal, and electrochemical properties of nanoparticles using advanced characterization techniques. Topics covered: • Why characterization is essential in nanoscience • Structure–property–performance relationship • X-ray Diffraction (XRD) & Rietveld Refinement • Thermogravimetric Analysis (TGA) • Field Emission Scanning Electron Microscopy (FESEM) • Energy Dispersive X-ray Spectroscopy (EDX/EDS) • Transmission Electron Microscopy (TEM) • High-Resolution TEM (HRTEM) • Selected Area Electron Diffraction (SAED) • X-ray Photoelectron Spectroscopy (XPS) • X-ray Fluorescence (XRF) • Atomic Force Microscopy (AFM) • Raman Spectroscopy & FTIR • UV–Visible & Diffuse Reflectance Spectroscopy (DRS) • BET Surface Area Analysis • Vibrating Sample Magnetometry (VSM) • Mössbauer Spectroscopy • Electrochemical Impedance Spectroscopy (EIS) & Impedance Spectroscopy • How these complementary techniques work together to reveal the complete nature of nanomaterials From crystal structure and phase purity to surface chemistry, magnetic behavior, porosity, optical band gap, and electrochemical performance, each technique contributes a unique piece of the puzzle. Together, they enable researchers to design, optimize, and develop high-performance nanomaterials for energy, electronics, catalysis, biomedicine, environmental remediation, and advanced functional devices. "Characterization is not just about measuring materials—it's about understanding the science behind their performance." © Nanoencryption: Removing barriers in the way of science. #Nanoencryption #Nanomaterials #Nanoparticles #Characterization #XRD #RietveldRefinement #FESEM #TEM #HRTEM #SAED #XPS #XRF #AFM #Raman #FTIR #UVVis #DRS #BET #VSM #Mossbauer #EIS #ImpedanceSpectroscopy #MaterialsScience #Nanotechnology #ScienceEducation #Research #STEM

According to the theory, small particles dissolve and redeposit onto the surface of large particles, and the large particles continue to grow until all of the small particles have dissolved. But, Berkeley Lab scientists including Dr. Peter Ercius and Dr. Haimei Zheng revealed that nanoparticle growth is directed not by difference in size, but by defects. Using high-resolution liquid cell transmission electron microscopy (LC-TEM) at the Molecular Foundry,of the Berkeley Lab the researchers captured real-time, atomic-scale LC-TEM videos of Cd-CdCl₂ CSNPs ripening in solution. Researchers conducted the in-situ LC-TEM experiments on the image-corrected Thermo Fisher Scientific ThemIS microscope equipped with a third-order spherical aberration image-corrector which corrects all coherent axial aberrations up to the 3rd order while partially compensating 4th and 5th order aberrations. This phase-contrast TEM image-series visualizes the defect-mediated ripening process of Cd-CdCl₂ core-shell particles at 50 fps. Read the findings published in the journal Nature Communications. https://lnkd.in/dYyY2UWt

🔬 Measuring Nanoparticle Size Using ImageJ – Simplified Guide Accurate nanoparticle size analysis is critical for research in nanotechnology, environmental remediation, and advanced materials. To make this process easier and more reproducible, I’ve created a step-by-step visual guide using ImageJ. 📌 What this guide covers: ✔️ Image calibration using scale bars ✔️ Particle size measurement techniques ✔️ Data recording and statistical analysis ✔️ Common errors & troubleshooting tips ✔️ Advanced options for better accuracy 💡 Why it matters? Reliable particle size determination directly impacts the interpretation of material properties, adsorption efficiency, and catalytic performance. 📊 Best Practice: Always measure at least 50–100 particles and report results as mean ± standard deviation for scientific accuracy. This guide can be especially useful for researchers working with SEM/TEM images, activated carbon materials, and nanostructured systems. #Nanotechnology #ImageJ #ResearchTools #MaterialsScience #SEM #TEM #DataAnalysis #ScientificResearch #Postdoc #Academia

Atom Probe Tomography (APT) is a cutting-edge analytical technique that provides three-dimensional atomic-scale imaging and #chemical composition mapping of #materials with exceptional precision. As a cornerstone of modern microscopy, #APT combines the principles of field ion microscopy with time-of-flight mass spectrometry to enable the spatially resolved identification of individual atoms within a specimen. The technique relies on the controlled evaporation of atoms from a needle-shaped specimen under a high electric field, followed by their detection and chemical identification. The process begins with the preparation of a sharp, needle-like tip with an end radius typically less than 100 nm. Under ultra-high vacuum conditions and cryogenic temperatures, a high voltage or ultrafast laser pulses are applied, inducing field evaporation of surface atoms. These ionized atoms are then projected onto a position-sensitive detector, where their time of flight is measured to determine their mass-to-charge ratio, enabling elemental identification. By reconstructing the impact positions and sequence of detected ions, a three-dimensional atomic map of the material is generated with near-atomic resolution. APT excels in analyzing solute segregation, precipitation phenomena, and interfacial chemistry in metals, semiconductors, and even insulating materials. Its unique ability to provide both spatial and compositional information at the atomic scale makes it indispensable for advancing materials science, metallurgy, and nanotechnology. With ongoing improvements in instrumentation and data analysis, APT continues to push the boundaries of nanoscale characterization, offering unprecedented insights into material properties and processes. #metals #alloys #steels #superalloys

Quantum materials experiments usually mean custom, one-off hardware, a different microwave setup, a different cryostat wiring job, a different sample stage for every lab, every material. We asked: what if a standard chip foundry process could replace all that? We repurposed a commercial 65nm CMOS process into a foundry-fabricated platform that integrates microwave, thermal, and electrical control on a single 1 mm² chip. Three results show what it can do: 1- Cryogenic magnetic susceptibility of Fe₃GeTe₂ at 1.75 K, no sample-specific fabrication 2- NV-center ODMR at 20–25 dB lower microwave power than a commercial antenna, same sensitivity 3- Zero image degradation under live SEM imaging Foundry manufacturing made electronics reproducible at scale. We think it can do the same for quantum materials characterization. Proud to share this work led by co-first authors Sharad Kumar Yadav (Ph.D) and Luca Nessi, with collaborators across KAUST, MIT, and Oak Ridge National Laboratory. Preprint: https://lnkd.in/dZkJAkKD #QuantumSensing #CMOS #QuantumMaterials #2DMaterials #NVCenter #QuantumPhotonics

🌿 From Plants to Particles: A Sustainable Route to Ceramic Nanomaterials This visual summarizes an alternative pathway for producing ceramic nanoparticles by harnessing the chemical potential of natural plant extracts. Instead of relying on harsh reagents, bioactive phytochemicals guide the nucleation and growth of metal oxides in a greener, safer way. The workflow demonstrates how simple laboratory steps can lead to controlled nanoscale structures, including spherical and rod-shaped morphologies, while maintaining alignment with green chemistry principles. 🔍 Why this matters: • Reduces chemical toxicity and environmental impact • Encourages sustainable nanomaterial design • Suitable for advanced applications in materials science, biotechnology, and environmental research Green synthesis is not just an alternative — it’s a step toward responsible innovation in nanotechnology. #SustainableNanotechnology #GreenMaterials #Nanomaterials #EcoFriendlyScience #ResearchVisualization

New publication from our research group in ACS Applied Nano Materials: “AgNiCoCr Nanoparticles: Exploring the Morphological Shift from Elementally Segregated to High Entropy Structures” This work demonstrates the feasibility of atomic-scale mixing of otherwise immiscible elements in nanoscale systems. In this work, we investigate how nanosecond laser-induced dewetting can drive the transformation of multielement AgNiCoCr thin films into nanoparticles with distinctly different elemental distributions and morphologies. A key focus of the study is understanding the transition from elementally segregated nanostructures toward compositionally mixed, high-entropy nanoparticles, highlighting how laser-driven nonequilibrium processing can provide access to complex nanoscale structures that are difficult to achieve through conventional synthesis routes. This work contributes to our broader efforts to understand and control process–structure–composition relationships in multicomponent nanoparticles, with potential implications for catalysis, energy, and other functional nanomaterial applications. Congratulations to the team and collaborators who contributed to this work! #highentropyalloynanoparticles #highentropyalloys #laserprocessing #ACS https://lnkd.in/g3Z_iKQb

🔬 Sol–Gel Method for Nanoparticle Synthesis The Sol–Gel method is one of the most versatile and widely used approaches for synthesizing nanomaterials, especially metal oxide nanoparticles. This method transforms molecular precursors into highly controlled nanostructures through a sequence of: 🧪 Hydrolysis ⚗️ Polymerization / Condensation 💧 Sol formation 🔹 Gel formation 🔥 Drying and calcination The biggest advantage of the sol–gel route is the excellent control it offers over: ✅ Particle size ✅ Purity and composition ✅ Surface area ✅ Morphology ✅ Structural uniformity Because of its simplicity and flexibility, the sol–gel method is extensively used for preparing: 🔬 Metal oxide nanoparticles ⚡ Functional nanocomposites 🧪 Catalytic materials 💧 Membrane additives for separation 🌱 Environmental remediation materials 🔋 Energy storage materials Key benefits include: ✔ Low processing cost ✔ Uniform nanoparticle distribution ✔ High purity products ✔ Better control over nano-scale structure ✔ Scalable for many advanced applications In nanotechnology, controlling synthesis is the first step toward controlling performance. From lab-scale research to industrial applications, the Sol–Gel method continues to play a major role in designing next-generation materials for energy, environment, and membrane technologies. 🔬 Smart Synthesis ⚡ Better Nanomaterials 🌍 Sustainable Future #Nanotechnology #SolGel #Nanomaterials #MaterialsScience #ChemicalEngineering #AdvancedMaterials #Nanoparticles #MembraneTechnology #Catalysis #EnergyStorage #Research #Innovation #Sustainability

Part 1 of this series on nanomaterial characterization reached 50 K + researchers worldwide! Here’s Part 2: “Your Nanomaterial Looks Great. But Does It Work?” Beyond morphology and structure, these advanced techniques uncover chemical states, optical behavior, and real-world performance - X-ray Photoelectron Spectroscopy (XPS): Determines elemental composition and oxidation states, the “chemical fingerprint” of your surface. - Energy-Dispersive X-ray Spectroscopy (EDX/EDS): Confirms elemental mapping and dispersion of fillers in composites. - UV–Vis Spectroscopy: Analyzes electronic transitions, optical band gap, and nanoparticle stability. - Photoluminescence (PL): Reveals defect states, recombination behavior, and semiconductor quality. - Atomic Force Microscopy (AFM): Provides 3-D surface topography and roughness at nanometer scale. - Electrochemical Analysis (CV / EIS): Evaluates redox activity, conductivity, and charge-transfer properties, crucial for energy materials. - Mechanical Testing (Nano-/Micro-indentation): Measures hardness, modulus, and interface strength in nanocomposites. - Thermal & Fouling Behavior (DSC / DTG / Fouling Tests): Assesses thermal transitions, degradation points, and long-term stability. Missed Part 1? Link in the comments

Major Material Characterization Techniques Every Researcher Should Know Understanding a material is just as important as synthesizing it. Material characterization helps us decode structure, composition, morphology, thermal, and surface properties, connecting lab-scale research with real-world applications. 📌 Key Characterization Techniques: 🧪 X-ray Diffraction (XRD) Phase identification Crystal structure & crystallite size 🌈 UV–Visible Spectroscopy (UV–Vis) Optical absorption behavior Band gap estimation ✨ Photoluminescence (PL) Spectroscopy Emission properties Defect states & recombination mechanisms 🧬 Fourier Transform Infrared Spectroscopy (FTIR) Functional group identification Chemical bonding analysis 🔍 Raman Spectroscopy Molecular vibrations Structural disorder & stress analysis 🧫 Scanning Electron Microscopy (SEM) Surface morphology & microstructure ⚛ Transmission Electron Microscopy (TEM) Atomic-scale structural information 📊 X-ray Photoelectron Spectroscopy (XPS) Surface chemistry & oxidation states 🧲 Atomic Force Microscopy (AFM) Surface roughness & topography at the nanoscale 🧊 Brunauer–Emmett–Teller (BET) Analysis Surface area & porosity evaluation 🔥 Thermogravimetric Analysis (TGA) Thermal stability & weight loss behavior 🌡 Differential Scanning Calorimetry (DSC) Phase transitions & heat flow analysis 💡 Why it matters: From physics and chemistry fundamentals to energy devices, semiconductors, polymers, and nanotechnology, characterization is the backbone of materials innovation.