X-ray fluorescence spectroscopy (XRF) is one of the most common techniques used for studying the elemental composition of different materials. In this materials characterization method the sample is irradiated with x-ray radiation, which knocks out electrons from atoms, leaving them in an excited state. During the relaxation of these atoms the excess energy is released in the form of x-ray radiation. The energy and intensity of this radiation however depends directly on the composition of the material. Therefore it is possible to study a materials composition by detecting the x-rays that come out of the sample. Watch our video to learn more!
Low-energy ion scattering spectroscopy (LEIS) is an exciting technique that allows to study the structure and chemical composition of a materials surface.
In this materials characterization method the sample is bombarded with a stream of ions and the positions, velocities and energies of the scattered ions are observed. The energy of scattered ions depends on the mass of the target, so there are distinct peaks in the energy spectrum of the scattered ions. These peaks give information about the samples elemental composition. The uniqueness of this technique lies in its sensitivity to the very first atomic layer on a sample and with forward scattering setup it is even capable of directly observing hydrogen atoms.
One of the main components of the system is the ion gun, that shoots ions at the studied substrate. The most widely used ions for that purpose are ionized noble gas or alkali atoms. Noble gas such as helium, neon or argon is ionized with electrons, giving them a positive charge. Alkali ion beams can be created by heating alkali wafers. In low-energy ion scattering spectroscopy the ions usually have an energy from 500 eV to 10 000 eV. The precise desired energy of the ions is obtained by applying a suitable accelerating voltage.
Before interacting with the substrate, the ions first need to pass through the ion beam manipulator, that narrows the beam and also filters the ions based on mass and velocity. For some experiments the ion beam is also chopped with an unipolar electrical chopper – a pulsed-wave generator, that lets through ions only when no voltage is applied. As a result the ion beam leaves the ion beam manipulator in pulses. By using short ion pulses, one can separate backscattered primary ions, for example He, from sputtered ions of different masses by time gating. This makes it possible to detect signals that would otherwise be buried in the background that is caused by ions sputtered from the sample surface.
The sample itself is attached to a special holder that allows the operator to adjust the position and angle of the sample for different experiments. When the ions hit the substrate, different interactions take place. Some ions are scattered at a certain angle and also their energy will be different after the impact. Some ions however become neutral as they pick up electrons from the substrate. The ions may also be implanted into the material or deposited on the substrate surface. The primary beam ions may also kick out electrons or atoms from the substrate and the atoms may even be ionized in the process. Radiation may also be emitted from the substrate as the excited atoms undergo a relaxation process.
The electrostatic analyzer is commonly used to detect the velocities and energies of the scattered ions. In this hemispheric device an electrical potential is applied between the inner and outer wall. The outer wall with positive potential repels the positive ions and the inner wall with negative potential attracts the positive ions. Neutral particles are unaffected by the field and hit the wall and thus never reach the detector. Positive ions with too low energy are pulled to the inner wall and also don’t reach the detector. If the cations energy is too high however then it simply hits the outer wall. Only if the ions energy is just right, it can pass through the analyzer and create a signal by interacting with the detector. By changing the potential between the walls, the operator can scan through a wide energy range in order to find out the energy of the emitted particles. In newer systems however a double toroidal analyzer is preferred as it integrates the signal over the scattering azimuth, so the intensity is some orders of magnitude higher compared to a hemispherical analyzer. The drift tube is used in TOF experiments in order to detect the energies and velocities of the scattered ionic and also neutral particles. Neutrals can easily be seperated from ions with the accelerator. There are two types of detectors that are commonly used – channel electron multipliers and microchannel plates. If the ion or a neutral particle with sufficient energy hits the detector then a cascade of secondary electrons is created and the signal significantly amplified. Microchannel plates also give information about the particles position but that comes at the cost of sensitivity.
Measurements with low-energy ion scattering spectroscopy are performed in ultra-high vacuum in order to avoid interactions with the surrounding gas. Having a good vacuum also ensures that the studied substrate and system parts are clean. Ultra-high vacuum is achieved with turbomolecular and ion pumps with the help of rough vacuum pumps.
Samples that have been exposed to open air are always contaminated for this type of surface sensitive characterization method and therefore they need to be cleaned inside the system in vacuum with appropriate equipment. Common ways to remove the contaminated top layer are sputtering, annealing or exposing to atomic oxygen.
There are of course few other surface sensitive materials characterization techniques such as XPS, AFM and SEM but each of them has distinct advantages and disadvantages. Therefore they are often used together when studying novel nanomaterials as they compensate each others weaknesses and allow to get a better overview.
The quadrupole mass spectrometer (QMS) is used to detect and measure the abundance of gas phase ions. These ions have to pass between electrically connected rods in order to reach the detector. By combining alternating and direct voltage on these rods, it is possible to ensure that only ions with specific mass-to-charge ratio are capable of reaching the detector.