Investigation of field electron microscope tips bombarded with microparticles at limited field emission currents

Mo, Ta, W, and Re field electron microscope (FEM) tips, bombarded with microparticles at limited field emission currents (400 MΩ resistor in series with the FEM tip) were investigated by means of FEM, transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Two groups of tips could be distinguished: One group had a slight tip radius increase to a maximum of 2.5 μm and microcraters were formed along the tip shank. The other group had no detectable tip radius change; however, there was microcrater formation near the tip apex area. FEM patterns showed surface contamination clearly. Heating such contaminated tips and tips where phosphorescent material (Zn:Cd)S had been deposited in less than monolayer concentration by evaporation from a heating coil, resulted in similar sequences of FEM patterns. A new type of microcrater with smooth crater lips could be detected in both groups. These results support the combined microparticle-field emission mechanism [1], which was proposed earlier to be responsible for melting cap and microcrater formation. Excerpts were presented at the 19th Field Emission Symposium, Urbana, Illinois (USA), August 1972.     

Processus simultane d'évaporation libre et de diffusion de surface

If a conical metal tip is annealed in vacuum, the radius at the apex increases with time by surface diffusion. This was calculated by Nichols and Mullins and recently verified by the authors. This phenomenon is now calculated in case of a simultaneous action of evaporation and surface diffusion. By evaporation the blunting rate should be lowered until it becomes zero for a critical value of the curvature radius. Numerical data for different temperatures and cone angles are calculated for some metals (W, Mo, Pt, Ni, Cu). Measured are profile changes of Mo tips during annealing. The lowering of the blunting rate and the existence of a limit radius are confirmed. An evaporation can also occur as a consequence of a surface reaction. The measured radius changes of tungsten tips annealled in 1.5 × 10^?5 torr and 2.5 × 10^?5 torr of oxygen agree fairly well with the predictions. Surface self-diffusion measurements at high temperatures may be erroneous if evaporation is not considered, an example for Mo at 2150°K is given.     

3D atom probe assisted by femtosecond laser pulses

The 3DAP allows to image a material in 3D on a nearly atomic scale. It is based on the field evaporation occurring at the surface of a biased tip like shape specimen with an end radius of 50 nm. Surface atoms are removed one by one from the tip by means of fs laser pulses so that the physical process involved in this laser enhanced field evaporation might correspond to the very early stages of the ablation process. This technique makes possible to distinguish between different regimes of material removal such as thermal evaporation or in the case of metals or semiconductors an evaporation assisted by the rectification of the optical field at the surface. In this paper the principle of the 3DAP is presented and the underlying physics involved in the field evaporation assisted by femtosecond laser pulses is discussed.     

The properties of the nonequilibrium LaB6 surface resulting from field evaporation

The nonequilibrium surface of single-crystal lanthanum hexaboride needles and its modifications are studied with a time-of-flight atomic probe. The surface is obtained by room-temperature field evaporation. The mass spectra of field evaporation shed light on the surface composition at the needle tip immediately after tip etching, corrosion in residual gases, intense cleaning by field evaporation, and the relaxation of the nonequilibrium surface by heating to 1250 K. Conditions for the breakdown of an oxide film on the tip surface and for obtaining the mass spectra of field evaporation for stoichiometric or lanthanum-enriched pure LaB₆ single crystals are discussed.     

Signature of tip electronic states on tunneling spectra

The influence of STM tip electronic states on the electron transport through an atomic object on a surface is studied both experimentally and theoretically. We present scanning tunnelling spectroscopy (STS) experimental results on Ag islands with two, blunt and sharp, STM tips. The data taken with the sharp tip have an additional peak at positive bias which corresponds to the tip apex atom state. We show that sudden tip sharpness variation and corresponding I(V) characteristic change may help to differentiate between electronic states of the tip and the sample. The experimental data are discussed and compared with theoretical calculations performed for two different tips. The current and differential conductance calculations are carried out by means of the Green's function technique and a tight-binding Hamiltonian.     

Confinement of the field electron emission to atomic sites on ultra sharp tips

The spatially controlled field assisted etching method for sharpening metallic tips, in a field ion microscope (FIM), is used to study the evolution of the field emission when the tip apex radius is decreased below 1 nm. Unlike the conventional image formation in a field emission microscope (FEM), we demonstrate that at this scale the field emission is rather confined to atomic sites. A single atom apex fabricated at the end of such tips exhibits an outstanding brightness compared to other atomic tips. The measurements have been repeated for two double atom tips, with different atom-atom separations, and images of atomic field emission localization have also been obtained. We have found that the field emission intensity alternates between adjacent atoms when the applied voltage is gradually increased beyond a threshold value.     

Ultrafast emission of ions during laser ablation of metal for 3D atom probe

The 3D atom probe(3DAP) is an imaging instrument based on the controlled field evaporation of single atoms from a sample having a tip shape with an end radius of 50 nm. In the fs laser assisted 3DAP the evaporation is induced by the laser pulses so that the physical process involved in this 3DAP analysis might correspond to the very early stages of the ablation process. In this paper we present the principle of the 3DAP and we discuss the existing models of the fs assisted evaporation. At last, we test the relevance of these models with pump-probe experiments on tungsten tips in the tomographic atom probe.     

Nanolithography with an atomic force microscope

A lithographic technique, employing the vibrating tip of an atomic force microscope to mechanically pattern various materials such as photoresist, metals or semiconductors in the nanometre regime has been developed. We use this technique for the fabrication of etch masks as well as for the patterning of evaporation shadow masks.The tip quality has been found to be a crucial factor in the lithographic resolution. We therefore use ultra hard, amorphous carbon tips, which are prepared by electron beam deposition in an electron microscope. With these tips, additionally sharpened in an oxygen plasma, we now succeed in fabricating hole arrays with periods in the 10 nm regime. These hole arrays are transferred to the electron system of a GaAs–AlGaAs heterostructure, and the magneto resistance of such fabricated antidot arrays is discussed.     

Field desorption microscopy of the 〈111〉 trihedral angle of a reconstructed tungsten tip

The surface structure near the 〈111〉 trihedral angle, which forms in an electric-field-heated tungsten tip, is studied by field electron microscopy, continuous-mode field desorption microscopy, and high-temperature field evaporation microscopy. The shape and structure of the surface depend on the temperature, field, and time. The angle is formed by three {011} planes, with the (111) plane at its vertex being retained in the form of a triangle or a hexagon with randomly arranged atomic clusters. The edges between {011} faces represent long and narrow {112} planes having longitudinal or transverse steps. In the absence of field evaporation, the edges and angle sharpen, becoming monoatomic. Field evaporation from the angle or microprotrusions on the edges extends these edges and causes transverse steps to appear on them. The explanation of the changes in the shape and structure of the surface is based on considering the competition of surface diffusion, crystal growth in an electric field, and field evaporation.     

Silver whiskers and epitaxial layers on tungsten tips as fem specimens; Their growth and behaviour on annealing and oxidation

In order to investigate whether field-emission microscopy (FEM) can be applied to the examination of adsorption on low-melting metals, a study has been made of the preparation and the stabilization of silver surfaces that are suitable as field electron emitters. Single silver whiskers, showing negligibly distorted FEM patterns, could be grown at 873 K by in-situ deposition of silver vapour onto the apex of thermally cleaned blunt tungsten tips. Single-crystal silver layers could be grown at 296 K by the same technique on field-evaporated sharp tungsten tips. The nucleation and growth of the layers take place more uniformly on these crystallographically perfect surfaces than on thermally cleaned tips. At elevated temperatures (673 K) considerable diffusion of silver from the apex of the tip to the shank was noticed when the latter had been thoroughly cleaned by previous heating. The occurrence of this effect was avoided by applying the field-evaporation step in the tip-preparation procedure after the tip had been strongly oxidized ; thus, the oxidized tungsten bordering the cleaned apex acts as a silver diffusion barrier. The silver surfaces obtained have a high degree of cleanliness. Adsorbed oxygen can easily be removed by heating to 673 K ; hardly any blunting results from this treatment. However, when a silver layer has been strongly oxidized, complete field desorption of silver reveals oxidation also of the tungsten at the tungsten-silver interface. Application of positive voltages to a crystalline silver layer on a tungsten tip at 77 K in ultra-high vacuum deforms the layer extensively before actual field evaporation of silver is achieved.     

Field-desorption microscopy study of the deformation of a tungsten tip subjected to thermal treatment in an electric field

Deformation of a tungsten tip 500 to 1000 nm in radius subjected to heating in an electric field is studied using field-emission microscopy and continuous-mode field-desorption microscopy. Measurements are performed immediately after the thermal field treatment without any smoothing of the tip by either heating or field evaporation. The edges of the tip (which is shaped into a polyhedron) are found to consist of monatomic steps about 1 nm wide and about 100 nm long. Microscopic protrusions about 10 nm in size are shaped like pyramids or wedges with single-atom apexes or monatomic edges and facets that are a continuation of the facets of the reconstructed tip or an outgrowth on which the protrusions are situated. The outgrowths are shaped like stepped truncated pyramids with monatomic edges. The observed phenomena are explained in terms of competing processes of surface diffusion, crystal growth in an electric field, and field evaporation.     

Localized multiphoton emission of femtosecond electron pulses from metal nanotips

Intense multiphoton electron emission is observed from sharp (approximately 20 nm radius) metallic tips illuminated with weak 100-pJ, 7-fs light pulses. Local field enhancement, evidenced by concurrent nonlinear light generation, confines the emission to the tip apex. Electrons are emitted from a highly excited nonequilibrium carrier distribution, resulting in a marked change of the absolute electron flux and its dependence on optical power with the tip bias voltage. The strong optical nonlinearity of the electron emission allows us to image the local optical field near a metallic nanostructure with a spatial resolution of a few tens of nanometers in a novel tip-enhanced electron emission microscope.     

Heat-field treatment of tips made of tungsten-hafnium alloy

The combined effect of a high electric field and a high temperature on the morphology of W-Hf field-emission tips is studied. It is shown that, while the tip reconfiguration stages for this alloy are basically the same as for pure tungsten, they have a number of specific features due to the surface segregation of hafnium. The heat-field treatment of these emitters narrows the solid angle of emission significantly, improves the emissivity of the tips, and is accompanied by the high-temperature evaporation primarily of Hf atoms.     

A measurement of the local electric field on field emitter crystals using T-F emission

A method is introduced to measure in situ the absolute value of the local field strength on the surface of a field emitter tip by using T?F emission. The method is based on the unified theory of electron emission (Christov) which is now experimentally well confirmed. The method is tested on several single crystal faces of tungsten tips. The absolute value of the local field can be determined within an error of about 5%. Relative field strengths at different points on one single crystal face can be measured with an error of 2%. Once the absolute value of the field strength is thus measured, the absolute value of the work function can be obtained additionally, but so far only with a fairly great error.     

Fabrication of 15 nm curvature radius polymer tip probe on an optical fiber via two-photon polymerization and O2-plasma ashing

Polymer tips with 15 nm curvature radius apexes that are capable of scanning the surface of a sample have been fabricated on the surface of an optical fiber using two-photon photopolymerization (TPP) and O₂-plasma ashing with a SCR500 resin. First, the parent conical polymer tip with a 125 nm curvature radius apex was fabricated via TPP using a continuous scanning method and the accumulation of circular layers. Next, the tip was sharpened using an O₂-plasma ashing process with high reproducibility. As a result, the apex radius of curvature had a maximum reduction to 15 nm. In order to evaluate the performance of the 15 nm curvature radius polymer tip, a 30 nm thick gold layer with holes of 250 nm radius and a single layer of polystyrene beads with a 350 nm radius were imaged using a tuning-fork-based atomic force microscope. The topographic images obtained by the 15 nm polymer tip were improved in width and depth compared with those obtained by the 125 nm polymer tip due to the reduction of the imaging artifacts. This method can also be commonly used to reduce the radius of curvature of the polymer tip in order to achieve more accurate imaging.     

An examination of field evaporation theory

Contrary to opinions expressed by earlier investigators, thorough examination of the existing models for field evaporation indicates that they are capable of predicting changes in the relative abundance of ionic species as temperature is changed and evaporation rate is held constant, without assuming atomic tunneling or slowness of electronic transition. However, this need not imply that atomic tunneling and slowness of electronic transition do not exist. Furthermore, the inclusion of energy level shifts in field evaporation theory results in the prediction of higher charge states than would be otherwise expected. This is in agreement with the observations of various investigators on copper and other metals. The examination further reveals that very significant differences in the predicted variation of evaporation rate with field exist between the image-hump and intersection models. This suggests a means by which one can attempt to determine experimentally the “correct” model to apply in a given situation. Furthermore, rigorous interpretation of the intersection model in conjunction with the experimental data of Tsong and Müller can result in significantly different values for the distance of the equilibrium position of the surface atom from the metal surface and the polarizability of the surface atom, than obtained using linear approximations.     

Numerical investigation of temperature effects in materials irradiated by high-energy heavy ions in the framework of heat conduction equation for electrons and lattice

A system of equations for electron gas and lattice around and along the trajectory of a heavy uranium ion with an energy of 700 MeV in nickel at constant heat capacity and heat conduction taken at room temperature is solved numerically in an axially symmetric cylindrical coordinate system. On the basis of the lattice temperature obtained as a function of radius around the ion trajectory and depth, a conclusion is made that the ionization energy losses of a uranium ion in nickel are sufficient for melting and evaporating the material from the surface. The maximum radius and depth of the region in which melting and evaporation take place are estimated.     

Miniature electron bombardment evaporation source: evaporation rate measurement

Miniature electron beam evaporation sources which operate on the principle of vaporization of source material, in the form of a tip, by electron bombardment are produced by several companies specialised in UHV equipment. These sources are used primarily for materials that are normally difficult to deposit due to their high evaporation temperature. They are appropriate for special applications, like heteroepitaxial thin films growth that require very low and well controlled deposition rate. We propose a simple and easily applicable method of evaporation rate control. The method is based on the measurement of ion current produced by electron bombardment of evaporated atoms. In order to be able to determine the ion current – evaporation flux calibration curves we measured the absolute values of evaporation flux by means of Bayard-Alpert ion gauge.     

Influence of the accommodation coefficient on the water drop evaporation process in a radiation field

The process of water drop evaporation in a field of intense laser radiation is examined on the basis of the hydro-thermodynamics equations under the assumption of quasistationarity in the conditions in the surrounding medium and in the radius. The influence of the accommodation coefficient on heating of the drops on the magnitude of the surface jump in water vapor density and on the position of the upper bound of the convective evaporation region is analyzed. It is shown that the surface jump in the vapor does not alter the rate of convective evaporation of the drop in practice, but can result in substantially different time dependences of the radius of a diffusely evaporating drop as compared with those found without it. The solution obtained is compared with the solution of the problem of evaporation in a Stefan approximation.     

Scanning tunneling microscopy with spin-polarized electrons

We present a short outline of the first STM experiments with spin-polarized electrons performed in ultrahigh vacuum by using ferromagnetic CrO₂ tips and a Cr(001) single crystal surface. A clear distinction can be made between topographic STM line scans obtained with a non-magnetic tungsten tip and those obtained with a ferromagnetic CrO₂ tip, which are modified due to an additional contribution from spin-dependent vacuum tunneling. STM therefore has the potential to measure the local electron spin polarization of the free surface as well as the spatial distribution of spins on the atomic scale.