Past exam of the frontiers of experimental condensed matter physics course of the University of Cambridge / 2013 / Paper 1 / 3

Atomic force microscopy senses tip–sample interactions through a compliant cantilever. Contact deflection, oscillation amplitude, phase or resonance frequency can be converted into a feedback signal. Chemical bonding and short-range repulsion, van der Waals forces, electrostatic forces and, where relevant, magnetic or capillary interactions produce contrast. Apparent height at a fixed force or frequency setpoint can therefore contain interaction contrast as well as geometry. Lateral resolution depends on the effective tip apex and interaction range; finite tip radius broadens features. Vertical sensitivity also depends on thermal and detector noise, cantilever calibration, vibration, drift and feedback bandwidth. Strongly localized short-range forces favor atomic resolution, whereas extended interactions average over more of the tip and surface.

For small oscillations about equilibrium separation $z_0$, write $z=z_0+x$ and linearize $F(z)=F(z_0)+F^{\prime }(z_0)x$. The constant force is absorbed into the equilibrium displacement. The cantilever equation becomesConsequently the small-amplitude AFM frequency shift isThe linear expression is the small-force-gradient approximation, $|F^{\prime }|\ll c$, in addition to the small-oscillation assumption. For an attractive force $F=-C/z^2$, $F^{\prime }>0$ and the resonance softens. A finite oscillation amplitude samples a weighted range of forces rather than only the gradient at one separation, and $F^{\prime }\ge c$ destroys local stability in this simple static model.

In a scanning electron microscope, a focused electron beam scans the surface and a detector records an emitted signal at each beam position. Low-energy secondary electrons escape from near the surface; changes in local slope, edges and detector-facing geometry give strong secondary-electron topographic contrast. Backscattered electrons result from elastic deflection of primary electrons and generally have a larger yield for higher atomic number. Their backscattered-electron atomic-number contrast therefore helps separate compositional regions. Detector geometry, crystal orientation and topography can also affect this signal, so brightness is not a unique elemental identification.

An environmental scanning electron microscope admits gas around the specimen while pressure-limiting apertures and differential pumping preserve the electron-optical column's vacuum. Electron collisions ionize the gas. Positive ions can neutralize negative charging of a poorly conducting specimen, enabling observation without a conductive coating. A gaseous secondary electron detector uses gas amplification to collect secondary-electron signals under these conditions. Gas pressure, path length and scattering must be controlled because they also affect the probe and background.^[ref]

Finally, acquire an energy-dispersive X-ray spectroscopy spectrum at each pixel to add elemental specificity. The beam creates inner-shell vacancies, and characteristic X-rays emitted as they fill identify chemical elements. Selecting fitted characteristic-line intensities yields elemental maps that can be compared with the electron image. Peak overlap, detector response, absorption and the X-ray-generating interaction volume limit identification, quantification and spatial resolution. This gives chemical-element contrast; resolving different bonds or oxidation states generally needs more detailed spectral information than one broad elemental map.