Tag Archives: vacuum system

Low-Energy Ion Scattering Spectroscopy (LEIS)

 

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.

 

Leak Finder For Vacuum Systems

 

Leak finder for vacuum systems is explained and demonstrated in this short video. All you need is a spectrometer tuned for helium and a tank of helium. In order to find the leak, you need to expose the vacuum system locally to helium. If a leak is present then the gas is sucked inside and pumped out into the mass spectrometer. The beeping noise immediately alerts the user if helium has reached the spectrometer and the leak is found. The most common places for leaks are usually at the connections of the vacuum systems parts.

Quadrupole Mass Spectrometer

 

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.

Hot Filament Ionization Gauge

 

The hot-filament ionization gauge is widely used for measuring the level of vacuum. The electrons are emitted from a hot cathode and accelerated towards the anode. In that process the electron may ionize a gas molecule. That gas molecule is pulled towards the collector and ion current is measured with an ammeter.

Penning Ionization Gauge

 

The Penning Ionization Gauge, also known as cold cathode gauge is used to measure the level of vacuum. High voltage between the anode and the cathode causes gas discharge and the resulting ionic current is measured with an ammeter. The measured amperes are then converted into pressure units such as Pascals or Torrs.

Thermocouple Gauge

 

The thermocouple gauge is a device used to measure low vacuum. A filament is heated up by passing a current through it. When gas molecules interact with the filament, heat is carried away. Therefore higher pressure in the chamber means that more heat is taken away. The temperature of the filament can be measured with a thermocouple where the generated voltage depends on the temperature. Therefore in this system the voltage of the thermocouple is measured and converted into pressure units like millibars or pascals.

Pirani Gauge

 

The Pirani Gauge is used to measure low vacuum. In the system tungsten filaments are heated up by passing current through them. As gas molecules interact with the filament, heat is carried away and electrical resistance changes. Therefore if the measured current or voltage can be converted into pressure units.

Diaphragm Pump

 

Diaphragm pump (membrane pump) is an oil-free vacuum pump that is used for obtaining ‪#‎prevacuum‬ of about 0.5 mbar. The pumping in this device is based on the movement of the membrane. As the membrane is pulled down, the volume of the chamber increases, causing a drop of pressure and gas enters the chamber through the inlet. Next, the inlet is closed, outlet opened and the membrane pushed up. This causes the volume of the chamber to decrease and pressure to increase. So the gas is forced to leave the system through the outlet.

Sorption Pump

 

The sorption pump is an oil-free ‪#‎prevacuum‬ pump that is based on the adsorption of gases on cold surfaces. The colder the surface, the more efficient the pumping is! Therefore liquid nitrogen with a temperature less than 77 degrees Kelvin is used for cooling the adsorber. The adsorber is a porous zeolite with a very large surface area as the pores have a diameter in the range of a few nanometers (or less). If the pump is full, then it needs to be renewed by degassing, which is basically heating the adsorber so that the gas can remove the pump through the outlet.

Rotary Vane Pump

 

Rotary Vane Pump is an oil-based vacuum pump, that can be used to obtain ‪#‎prevacuum‬ or even medium vacuum (depending on the system). In this device the rotor and vane(s) are in the housing, that is filled with oil. When the gas enters the chamber through the inlet, it gets trapped in the oil and is transported through the working chamber with the help of the rotor and vane(s) to the outlet, where the gas exits the system. The oil acts as a lubricant and also allows the pumping of some corrosive gases, as it protects the metal to some degree. Although this pump is quite fast and efficient for obtaining pre vacuum, it also may contaminate the vacuum system with oil. Therefore the use of oil traps is highly recommended.