# Materials characterisation techniques: what each one measures and when to use it

> Fifteen materials characterisation techniques explained with sources: XRD, XPS, BET, SEM, TEM, AFM, NMR, FTIR, Raman, TGA, UV–vis, DLS, CV, EIS and ICP-MS.

URL: https://www.labcanvas.com/techniques

Materials characterisation is the set of measurements that tell a chemist what a new material is: its crystal structure (XRD, which identifies phases from Bragg diffraction; Abid et al. 2023), its surface chemistry (XPS, which reads the top 2–10 nm; Baio et al. 2020), its porosity (gas sorption and the BET surface area; Osterrieth et al. 2022), its size and shape (SEM, TEM, AFM and DLS), its bonding (NMR, FTIR and Raman), its stability (TGA and DSC), its optical band gap (UV–vis), its composition (ICP-MS) and its electrochemistry (cyclic voltammetry and EIS). No single technique is enough; each page below explains how one method works, what its data looks like, how to prepare samples and the mistakes to avoid, with every fact cited.

Characterisation techniques Published 27 October 2026 Last updated 27 October 2026 27 references

![Characterisation techniques: How materials chemists measure structure, surface and composition (XRD · XPS · BET · SEM · TEM · NMR)](https://www.labcanvas.com/materials/characterisation-techniques/characterisation-techniques-cover.webp)

**Contents**

**Contents**

- Characterisation techniques at a glance
- Characterisation technique instrument drawing (high-resolution SVG)
- Which characterisation technique do I need?
- Bulk or surface, average or local
- A characterisation workflow for a new MOF
- How to draw characterisation figures in LabCanvas
- Characterisation techniques compared
- Related techniques
- More on LabCanvas
- Frequently asked questions
- References

## Characterisation techniques at a glance

| Crystal structure | XRD: Bragg’s law nλ = 2d sin θ gives peak positions that fingerprint the phase (Wang et al. 2026; Abid et al. 2023) |
| --- | --- |
| Surface composition | XPS: all elements except H and He, from the top 2–10 nm (Baio et al. 2020) |
| Porosity | Gas sorption with N₂ at 77 K; the BET method is the most widely used surface-area metric (Abid et al. 2023; Osterrieth et al. 2022) |
| Morphology | SEM: secondary electrons show topography, backscattered electrons atomic-number contrast (Erlich et al. 2020) |
| Atomic-scale imaging | TEM: samples below about 100 nm thick; HAADF-STEM intensity roughly ∝ Z² (Bijelić et al. 2023) |
| Height and roughness | AFM: 1–10 nm lateral and sub-nanometre vertical resolution, no vacuum (Joo et al. 2025) |
| Local structure and bonding | NMR chemical shifts (Armitage et al. 2013); solid-state MAS NMR for MOFs and zeolites (Brunner & Rauche 2020) |
| Vibrational spectra | FTIR needs a dipole change (Baker et al. 2014); Raman needs a polarisability change (Jones et al. 2019) |
| Thermal stability | TGA records mass against temperature; DSC records heat flow (Abid et al. 2023; Leyva-Porras et al. 2019) |
| Band gap | UV–vis with a Tauc plot; diffuse reflectance for powders (Escobedo-Morales et al. 2019) |
| Size in liquid | DLS gives the hydrodynamic diameter through the Stokes–Einstein equation (Wishard & Gibb 2019) |
| Elemental composition | ICP-MS: more than 65 elements, ng L⁻¹ detection limits for most (Mazarakioti et al. 2022) |
| Electrochemistry | Cyclic voltammetry (Rafiee et al. 2024) and impedance spectroscopy (Lazanas & Prodromidis 2023) |

## Characterisation technique instrument drawing (high-resolution SVG)

![Characterisation techniques instrument drawn as a LabCanvas Library object](https://www.labcanvas.com/materials/characterisation-techniques/characterisation-techniques-drawing.webp)

An X-ray diffractometer, the first instrument most new materials meet, as a LabCanvas Library drawing. Every technique page has its own instrument drawing and an example data plot to edit in the figure editor.

[Edit the drawing in LabCanvas](https://www.labcanvas.com/editor.html?add=ch-xrd-beam)[Download SVG](https://www.labcanvas.com/materials/characterisation-techniques/characterisation-techniques-drawing.svg)[Download PNG (3000 px)](https://www.labcanvas.com/materials/characterisation-techniques/characterisation-techniques-drawing.png)

## Which characterisation technique do I need?

Start from the question, not the instrument. A typical new solid, a MOF, a nanoparticle batch or a battery cathode, goes through several of these in turn:

- **Is it the phase I meant to make?** [X-ray diffraction](https://www.labcanvas.com/techniques/xrd). Peak positions are set by the unit cell, so the pattern is compared with a simulated or published one; it is the first check on a new MOF (Abid et al. 2023).
- **What does it look like?** [SEM](https://www.labcanvas.com/techniques/sem) for particle size, shape and morphology over large areas (Erlich et al. 2020); [TEM](https://www.labcanvas.com/techniques/tem) for lattice fringes, defects and particles a few nanometres across (Bijelić et al. 2023); [AFM](https://www.labcanvas.com/techniques/afm) for true heights, such as the thickness of a 2D flake (Joo et al. 2025).
- **Is it porous, and how much?** [Gas sorption and the BET surface area](https://www.labcanvas.com/techniques/bet), with the pressure range checked against consistency criteria for microporous solids (Gómez-Gualdrón et al. 2016; Osterrieth et al. 2022).
- **What is on the surface, and in what oxidation state?** [XPS](https://www.labcanvas.com/techniques/xps) (Baio et al. 2020).
- **Which bonds and groups are there?** [FTIR](https://www.labcanvas.com/techniques/ftir) and [Raman](https://www.labcanvas.com/techniques/raman), which follow different selection rules and so complement each other (Jones et al. 2019), and [NMR](https://www.labcanvas.com/techniques/nmr) for atom-by-atom local structure (Armitage et al. 2013).
- **How stable is it, and what solvent is still inside?** [TGA and DSC](https://www.labcanvas.com/techniques/tga-dsc) (Abid et al. 2023; Leyva-Porras et al. 2019).
- **What is its band gap or colour?** [UV–vis](https://www.labcanvas.com/techniques/uv-vis) (Escobedo-Morales et al. 2019).
- **How big are the particles in liquid, and will they stay dispersed?** [DLS and zeta potential](https://www.labcanvas.com/techniques/dls-zeta) (Rodriguez-Loya et al. 2023).
- **How much of each element, such as a metal loading?** [ICP-MS or ICP-OES](https://www.labcanvas.com/techniques/icp-ms) after digestion (Mazarakioti et al. 2022).
- **How does it behave in a cell or as a catalyst?** [Cyclic voltammetry](https://www.labcanvas.com/techniques/cyclic-voltammetry) and [impedance spectroscopy](https://www.labcanvas.com/techniques/eis) (Rafiee et al. 2024; Lazanas & Prodromidis 2023).

## Bulk or surface, average or local

The most common mistake is to treat one measurement as the whole story. Techniques differ in **where** they look and **how much** of the sample they average:

- **Surface versus bulk.** XPS sees only the outermost 2–10 nm (Baio et al. 2020), while powder XRD averages over the whole irradiated powder (Abid et al. 2023) and ICP-MS measures the dissolved sample (Mazarakioti et al. 2022). A surface oxide or coating can dominate XPS and be invisible to XRD.
- **Average versus local.** XRD, BET and DLS each report one number for a large population; TEM and AFM look at individual particles, so images need enough of them to be statistically meaningful (Bijelić et al. 2023).
- **Different sizes are different quantities.** A Scherrer size from XRD is a crystallite size, not a particle size (Jeong et al. 2008), and a DLS hydrodynamic diameter is intensity-weighted towards the largest particles (Wishard & Gibb 2019), so DLS and TEM sizes often differ (Filippov et al. 2023).
- **Crystalline versus amorphous.** XRD needs long-range order to give sharp peaks (Abid et al. 2023); solid-state NMR reports local structure whether or not the solid is ordered and complements diffraction (Brunner & Rauche 2020).

## A characterisation workflow for a new MOF

Metal–organic frameworks show how the techniques fit together, because nearly every MOF paper uses the same sequence (Abid et al. 2023):

- **PXRD** to confirm the framework formed and is phase pure.
- **TGA** to see solvent loss and the decomposition temperature, which sets the safe activation temperature: degas below about 75% of it (Abid et al. 2023).
- **Activation and N₂ sorption at 77 K** for the BET area and pore volume, then PXRD again to check the framework survived (Abid et al. 2023).
- **FTIR** to confirm solvent has left the pores (Abid et al. 2023), and digestion **¹H NMR** to count linkers and missing-linker defects (Nerli et al. 2025).
- **SEM** for crystal size and shape, and **low-dose TEM** where atomic detail is needed, since MOFs are damaged by the beam (Zheng et al. 2023).

See it applied on the [UiO-66](https://www.labcanvas.com/mof/uio-66), [HKUST-1](https://www.labcanvas.com/mof/hkust-1) and [MOF-5](https://www.labcanvas.com/mof/mof-5) pages, and the same logic for [battery materials](https://www.labcanvas.com/battery-materials), [2D materials](https://www.labcanvas.com/2d-materials), [perovskites](https://www.labcanvas.com/perovskites) and [zeolites](https://www.labcanvas.com/zeolites).

## How to draw characterisation figures in LabCanvas

Every technique page comes with two editable pictures: a drawing of the instrument (an X-ray diffractometer, an electron microscope column, an AFM cantilever and laser, a potentiostat with a three-electrode cell) and an example data plot, such as a PXRD pattern, an N₂ isotherm, a Raman spectrum or a Nyquist plot. Open either in the [figure editor](https://www.labcanvas.com/apps/figure-editor) to change labels, colours and data, paste in your own measurements, and combine them with structures from the materials pages into a figure or a [graphical abstract](https://www.labcanvas.com/graphical-abstracts) at the exact size your journal asks for.

Free calculators help with the analysis itself: the [Scherrer crystallite size calculator](https://www.labcanvas.com/tools/scherrer-equation-calculator) for XRD peak widths, the [Tauc plot band gap calculator](https://www.labcanvas.com/tools/tauc-plot-band-gap-calculator) for UV–vis, and the [RHE converter](https://www.labcanvas.com/tools/rhe-calculator) and [Tafel slope calculator](https://www.labcanvas.com/tools/tafel-slope-calculator) for electrochemistry.

## Characterisation techniques compared

| Technique | What it tells you | Probe and signal | Sample | Source |
| --- | --- | --- | --- | --- |
| XRD | Phase, purity, lattice parameters, crystallite size | X-rays; diffracted intensity vs 2θ | Powder, film or single crystal | Abid et al. 2023; Wang et al. 2026 |
| XPS | Surface elements and oxidation states | X-rays; photoelectron kinetic energy | Solid in ultra-high vacuum; top 2–10 nm | Baio et al. 2020 |
| Gas sorption / BET | Surface area, pore size and volume | N₂ at 77 K (also Ar, CO₂, Kr); amount adsorbed vs P/P₀ | Degassed powder | Abid et al. 2023; Osterrieth et al. 2022 |
| SEM | Morphology, particle size; composition with EDS | Electron beam; secondary and backscattered electrons, X-rays | Solid, coated if insulating | Erlich et al. 2020; Newbury & Ritchie 2015 |
| TEM / STEM | Atomic structure, defects, diffraction, local composition | Transmitted electrons | Below about 100 nm thick | Bijelić et al. 2023 |
| AFM | 3D topography, step heights, nanoscale properties | Sharp tip on a cantilever; deflection | Flat surface, in air or liquid | Joo et al. 2025 |
| NMR | Local structure, bonding, quantity of each site | Radio-frequency pulses on nuclear spins | Solution, or solid with MAS | Armitage et al. 2013; Brunner & Rauche 2020 |
| FTIR | Functional groups and bonds | Infrared absorption; needs a dipole change | Solid, liquid or film; ATR needs little preparation | Baker et al. 2014 |
| Raman | Bonds, phases; layers and defects in graphene | Laser; inelastically scattered light | Almost any; works in water | Jones et al. 2019; Ferrari et al. 2006 |
| TGA / DSC | Stability, solvent content, transitions | Temperature ramp; mass (TGA) or heat flow (DSC) | Milligrams of solid | Abid et al. 2023; Leyva-Porras et al. 2019 |
| UV–vis | Concentration, band gap, plasmon band | UV and visible light; absorbance or diffuse reflectance | Solution, film or powder | Mayerhöfer et al. 2019; Escobedo-Morales et al. 2019 |
| DLS / zeta | Hydrodynamic size, PDI, colloidal stability | Laser; intensity fluctuations, electrophoretic mobility | Dilute dispersion | Wishard & Gibb 2019; Rodriguez-Loya et al. 2023 |
| ICP-MS / OES | Elemental composition, metal loading, leaching | Argon plasma; ions by m/z or emission lines | Digested solution | Mazarakioti et al. 2022 |
| Cyclic voltammetry | Redox potentials, reversibility, catalytic current | Potential sweep; current | Working electrode in electrolyte | Rafiee et al. 2024 |
| EIS | Resistances, capacitance, diffusion | Small AC signal over frequency; impedance | Electrochemical cell | Lazanas & Prodromidis 2023 |

## Related techniques

[![XRD: Crystal structure, phase and crystallite size (nλ = 2d sin θ)](https://www.labcanvas.com/materials/xrd/xrd-cover.webp) Technique nλ = 2d sin θ X-ray diffraction (XRD) X-ray diffraction explained: Bragg’s law, how to read an XRD pattern, phase identification, Scherrer crystallite size, Rietveld refinement and common mistakes.](https://www.labcanvas.com/techniques/xrd)

[![XPS: Surface elements and chemical states, top ~10 nm (BE = hν − KE)](https://www.labcanvas.com/materials/xps/xps-cover.webp) Technique BE = hν − KE X-ray photoelectron spectroscopy (XPS) XPS explained: binding energy, 2–10 nm surface sensitivity, survey vs high-resolution spectra, chemical shifts, C 1s charge referencing and depth profiling.](https://www.labcanvas.com/techniques/xps)

[![BET: Surface area, pore size and pore volume (N₂ isotherm at 77 K)](https://www.labcanvas.com/materials/bet/bet-cover.webp) Technique N₂ isotherm at 77 K Gas sorption and BET surface area BET surface area explained: N₂ sorption at 77 K, IUPAC isotherm types, the BET range and Rouquerol criteria, pore size, degassing and limits for MOFs.](https://www.labcanvas.com/techniques/bet)

[![SEM: Electron images of surfaces, plus EDS elemental maps (Surface morphology and composition)](https://www.labcanvas.com/materials/sem/sem-cover.webp) Technique Surface morphology and composition Scanning electron microscopy (SEM) How SEM works: secondary vs backscattered electron images, EDS/EDX elemental analysis, resolution, sample coating, low-vacuum mode and common mistakes.](https://www.labcanvas.com/techniques/sem)

[![TEM: Atomic-scale images and diffraction from thin samples (HAADF intensity ∝ Z²)](https://www.labcanvas.com/materials/tem/tem-cover.webp) Technique HAADF intensity ∝ Z² Transmission electron microscopy (TEM) How TEM works: bright field, HRTEM lattice images, SAED diffraction, STEM-HAADF Z-contrast, EDS/EELS, sample thickness and beam damage of MOFs.](https://www.labcanvas.com/techniques/tem)

[![AFM: A sharp tip maps surfaces in 3D, in air or liquid (Height, phase and nanoscale forces)](https://www.labcanvas.com/materials/afm/afm-cover.webp) Technique Height, phase and nanoscale forces Atomic force microscopy (AFM) How AFM works: tip, cantilever and laser deflection, contact vs tapping mode, measuring 2D flake thickness from height profiles, and common AFM artefacts.](https://www.labcanvas.com/techniques/afm)

[![NMR: Atomic-level structure from nuclear spins (Chemical shift δ (ppm))](https://www.labcanvas.com/materials/nmr/nmr-cover.webp) Technique Chemical shift δ (ppm) Nuclear magnetic resonance (NMR) spectroscopy NMR spectroscopy explained: nuclear spins in a magnetic field, chemical shift in ppm, ¹H and ¹³C, coupling, integration, solid-state MAS and MOF digestion NMR.](https://www.labcanvas.com/techniques/nmr)

[![FTIR: Functional groups from infrared absorption (A = log₁₀(I₀/I))](https://www.labcanvas.com/materials/ftir/ftir-cover.webp) Technique A = log₁₀(I₀/I) Fourier-transform infrared (FTIR) spectroscopy FTIR spectroscopy explained: infrared absorption by bond vibrations, the interferometer and Fourier transform, wavenumber regions, ATR and reading bands.](https://www.labcanvas.com/techniques/ftir)

[![Raman: Vibrations from inelastically scattered laser light (Raman shift Δν̃ = ν̃₀ − ν̃ₛ (cm⁻¹))](https://www.labcanvas.com/materials/raman/raman-cover.webp) Technique Raman shift Δν̃ = ν̃₀ − ν̃ₛ (cm⁻¹) Raman spectroscopy Raman spectroscopy explained: inelastic laser scattering, Raman shift, Stokes lines, IR complementarity, graphene D, G and 2D bands, lasers, fluorescence.](https://www.labcanvas.com/techniques/raman)

[![TGA / DSC: Thermal stability, composition and phase transitions (Mass and heat flow vs temperature)](https://www.labcanvas.com/materials/tga-dsc/tga-dsc-cover.webp) Technique Mass and heat flow vs temperature TGA and DSC (thermal analysis) TGA and DSC explained: mass loss and DTG vs temperature, atmosphere, MOF thermal stability, and glass transition, melting and crystallisation in DSC.](https://www.labcanvas.com/techniques/tga-dsc)

[![UV–vis: Absorbance, concentration and optical band gap (A = εcl)](https://www.labcanvas.com/materials/uv-vis/uv-vis-cover.webp) Technique A = εcl UV–vis spectroscopy UV–vis spectroscopy explained: absorbance and the Beer–Lambert law, band gap from a Tauc plot, diffuse reflectance for powders and gold plasmon bands.](https://www.labcanvas.com/techniques/uv-vis)

[![DLS / ζ: Hydrodynamic size and surface charge of particles (D = kT / 6πηr)](https://www.labcanvas.com/materials/dls-zeta/dls-zeta-cover.webp) Technique D = kT / 6πηr DLS and zeta potential DLS and zeta potential explained: Brownian motion, Stokes–Einstein hydrodynamic size, intensity vs number distributions, PDI and colloidal stability.](https://www.labcanvas.com/techniques/dls-zeta)

[![CV: Current vs potential: redox peaks and kinetics (ΔEp ≈ 59/n mV (reversible))](https://www.labcanvas.com/materials/cyclic-voltammetry/cyclic-voltammetry-cover.webp) Technique ΔEp ≈ 59/n mV (reversible) Cyclic voltammetry (CV) Cyclic voltammetry explained: three-electrode cell, scan rate, redox peaks, 59/n mV reversibility, Randles–Ševčík, RHE conversion, ECSA and Tafel pitfalls.](https://www.labcanvas.com/techniques/cyclic-voltammetry)

[![EIS: Resistances, capacitances and diffusion vs frequency (Z(ω) = Z′ + jZ″)](https://www.labcanvas.com/materials/eis/eis-cover.webp) Technique Z(ω) = Z′ + jZ″ Electrochemical impedance spectroscopy (EIS) EIS explained: small AC perturbation, Nyquist and Bode plots, Randles circuit, charge-transfer resistance, Warburg diffusion, batteries and catalysts.](https://www.labcanvas.com/techniques/eis)

[![ICP-MS: Argon plasma elemental and isotopic analysis (Elemental content down to ng L⁻¹)](https://www.labcanvas.com/materials/icp-ms/icp-ms-cover.webp) Technique Elemental content down to ng L⁻¹ ICP-MS and ICP-OES ICP-MS and ICP-OES explained: argon plasma, detection limits, acid digestion, interferences, single-particle ICP-MS and metal content of MOFs.](https://www.labcanvas.com/techniques/icp-ms)

## More on LabCanvas

- [All characterisation techniques](https://www.labcanvas.com/techniques): XRD, XPS, BET, SEM, TEM, NMR, FTIR, Raman and more, explained with cited sources
- [Graphical abstract sizes and templates](https://www.labcanvas.com/graphical-abstracts): ACS, Wiley, Angewandte, RSC, Elsevier and Cell Press, with templates at the right size
- [Materials explained](https://www.labcanvas.com/blog/materials): MOFs, COFs, 2D materials, perovskites, batteries and zeolites, with cited facts
- [Journal figure size guide](https://www.labcanvas.com/blog/journal-figure-size-guide): Column widths and resolutions for 38 journals

## Frequently asked questions

### What are the main materials characterisation techniques?

The core set is X-ray diffraction for crystal structure, electron microscopy (SEM and TEM) and AFM for morphology, XPS for surface chemistry, gas sorption (BET) for porosity, NMR, FTIR and Raman for bonding, TGA and DSC for thermal behaviour, UV–vis for optical properties, DLS for particle size in liquid, ICP-MS for composition, and cyclic voltammetry and EIS for electrochemistry. Each has its own page here with sources.

### Which technique tells me if I made the right crystalline phase?

Powder X-ray diffraction: peak positions are set by the size and shape of the unit cell, so the measured pattern is compared with a simulated or published one to identify the phase and check purity (Abid et al. 2023).

### What is the difference between SEM and TEM?

SEM scans a focused beam over the surface of a bulk sample and images topography and atomic-number contrast (Erlich et al. 2020); TEM sends electrons through a sample thinner than about 100 nm and resolves lattices, defects and diffraction (Bijelić et al. 2023).

### What is the difference between XRD and XPS?

XRD measures long-range crystal structure averaged over the sample (Abid et al. 2023); XPS measures elements and their oxidation states in only the top 2–10 nm of the surface (Baio et al. 2020).

### What is the difference between FTIR and Raman?

FTIR detects vibrations that change the dipole moment (Baker et al. 2014); Raman detects vibrations that change the polarisability, so the two are complementary; in centrosymmetric systems no mode is active in both (Jones et al. 2019).

### Why do my DLS and TEM particle sizes not match?

DLS gives an intensity-weighted hydrodynamic diameter in liquid, which strongly favours large particles because scattering scales with d⁶ (Wishard & Gibb 2019); TEM measures dry cores. Differences of 200–300% are common (Filippov et al. 2023).

### Which characterisation techniques are used for MOFs?

PXRD for phase, TGA for stability and the activation temperature, N₂ sorption at 77 K for the BET area, FTIR to check activation (Abid et al. 2023), digestion NMR for linker defects (Nerli et al. 2025) and low-dose TEM for atomic detail (Zheng et al. 2023).

### How do I make a figure of characterisation data?

Each technique page has an editable instrument drawing and an example plot in LabCanvas; open them in the figure editor, replace the data with your own and export at journal resolution.

## References

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## Draw Characterisation techniques figures for your paper

LabCanvas is a browser workspace for scientific figures: instruments with their beam and light paths, editable data plots, crystal structures, graphs and graphical abstracts at journal sizes.

[Draw Characterisation techniques in LabCanvas](https://www.labcanvas.com/editor.html?add=ch-xrd-beam)

**Contents**

- Characterisation techniques at a glance
- Characterisation technique instrument drawing (high-resolution SVG)
- Which characterisation technique do I need?
- Bulk or surface, average or local
- A characterisation workflow for a new MOF
- How to draw characterisation figures in LabCanvas
- Characterisation techniques compared
- Related techniques
- More on LabCanvas
- Frequently asked questions
- References
