Microstructure and tribological performance of self-lubricating diamond/tetrahedral amorphous carbon composite film

In order to smooth the rough surface and further improve the wear-resistance of coarse chemical vapor deposition diamond films, diamond/tetrahedral amorphous carbon composite films were synthesized by a two-step preparation technique including hot-filament chemical vapor deposition for polycrystalline diamond (PCD) and subsequent filtered cathodic vacuum arc growth for tetrahedral amorphous carbon (ta-C). The microstructure and tribological performance of the composite films were investigated by means of various characterization techniques. The results indicated that the composite films consisted of a thick well-grained diamond base layer with a thickness up to 150 μm and a thin covering ta-C layer with a thickness of about 0.3 μm, and sp³-C fraction up to 73.93%. Deposition of a smooth ta-C film on coarse polycrystalline diamond films was proved to be an effective tool to lower the surface roughness of the polycrystalline diamond film. The wear-resistance of the diamond film was also enhanced by the self-lubricating effect of the covering ta-C film due to graphitic phase transformation. Under dry pin-on-disk wear test against Si₃N₄ ball, the friction coefficients of the composite films were much lower than that of the single PCD film. An extremely low friction coefficient (∼0.05) was achieved for the PCD/ta-C composite film. Moreover, the addition of Ti interlayer between the ta-C and the PCD layers can further reduce the surface roughness of the composite film. The main wear mechanism of the composite films was abrasive wear.     

Optimized FIB silicon samples suitable for lattice parameters measurements by convergent beam electron diffraction

The aim of this paper is to check the effect of artefacts introduced by focused ion beam (FIB) milling on the strain measurement by convergent beam electron diffraction (CBED). We show that on optimized silicon FIB samples, the strain measurement can be performed with a sensitivity of about 2.5 × 10⁻⁴ which is very close to the theoretical one and we conclude that FIB preparation can be suitable for such measurements in microelectronic devices.

To achieve this, we first used CBED and electron energy loss spectroscopy (EELS) which provide a procedure permitting an exact knowledge of the sample geometry, i.e. the thickness of both amorphous and crystalline layers. This procedure was used in order to measure the FIB-amorphized sidewall layer. It was found that if the FIB preparation is optimized one can reduce this amorphous layer down to around 7 nm on each side. Secondly different preparation techniques (cleavage, Tripod™ and FIB) permit to check if the surface damaged layer introduced by FIB influences the strain state of the sample. Finally, it was found that the damaged layer does not introduce measurable strain in pure silicon but reduces appreciably the quality of the CBED patterns.     

Investigation of physical properties of quartz after focused ion beam bombardment

Optical properties (transmission and refractive index) and phase change (from amorphous to crystal) of a commonly used glass, quartz, were investigated before and after focused ion beam (FIB) bombardment with ion energy from 30 to 50 keV. We found different influences of FIB bombardment on the optical properties and chemical structure of the quartz in the wavelength region of visible and near infrared, respectively. The quartz still can be used in the infrared wavelength for conventional optical applications. As an application example, an array of diffractive optical elements (DOEs) was directly fabricated on the quartz by the FIB milling. The measured diffraction efficiency of the DOEs is 83.5%, which is acceptable for practical use.This revised version was published online in March 2005. In the previous version, the published online date was missing     

Imaging characterization of carbon nanotube tips modified using a focused ion beam

A carbon nanotube (CNT) tip, which assembled on the sharp end of a Si tip by dielectrophoresis, was structurally modified using focused ion beam (FIB). We described the imaging characterization of the FIB-modified CNT tip in noncontact AFM mode in terms of wear, deep trench accessibility, and imaging resolution. Compared to a conventional Si tip, the FIB-modified CNT tip was superior, especially for prolonged scanning over 10 h. We conclude that modified CNT tips have the potential to obtain high-quality images of nanoscale structures.     

Self-organized amorphous material in silicon (0 0 1) by focused ion beam (FIB) system

A method using a focused ion beam (FIB) to prepare a silicon amorphous material is presented. The method involves the redeposition of sputtered material generated during the interaction of the Ga⁺ ion beam with a silicon substrate material. The shape and dimensions of this amorphous material are self-organized and reproducible. The stability of this amorphous material under electron irradiation was investigated in the transmission electron microscopy (TEM). Electron irradiation can induce recrystallization of the amorphous material, resulting in the lateral and vertical growth, starting at an amorphous-crystalline interface, of polysilicon containing defects.     

TEM and HREM of diamond crystals grown on Si tips: structure and results of ion-beam-treatment

Diamond single crystals were grown on the silicon whiskers by a hot filament chemical vapor deposition technique at the filament temperature about 2100 degrees C and the temperature of support 800 degrees C. Specimens were examined by SEM, TEM, HRTEM and SAED. When the filament temperature was about 1900 degrees C globular polycrystalline diamond particles were grown. At a support temperature more then 800 degrees C SiC nanoparticles were formed. To investigate the ion etching process of the silicon tip/diamond system, tips were treated with an Ar(+) beam with energy up to 30 kV. The results depend on fluence: at 4 x 10(18)ion/cm(2) diamonds and partially Si tips were destroyed, amorphous layer was formed (sometimes with nanometric size fragments of diamond); at 1 x 10(18)ion/cm(2) sharpened diamonds (radius of curvature about 20 nm) covered with amorphous layer (radius about 80 nm) probably with nanoclusters of diamond were observed; at 4.4 x 10(17) ion/cm(2) there was no visible tip sharpening but formation of amorphous thick layer occurred. The emission characteristics of Si tips covered with diamond were improved due to ion treatment. Since such tips in our case were covered with amorphous layer containing nanometric size fragments of diamond, we suppose this layer is responsible for electron emission improvement.     

Crystallographically-dependent ripple formation on Sn surface irradiated with focused ion beam

The metallographically polished polycrystalline Sn surface was sputtered by 30 kV focused Ga⁺ ions at room temperature. The experiment was carried out using various FIB incidence angles (0°, 15°, 30°, and 45°) over a wide range of doses (10¹⁶–10¹⁸ ions/cm²). The surface morphology was carefully characterized under the optical microscope, scanning electron microscope (SEM) and atomic force microscope (AFM). Ripples were observed on the irradiated areas even at the normal FIB incidence angle, which is not consistent with the Bradley–Harper (BH) rippling model. The orientation of ripples relies on crystallographic orientation rather than projected ion beam direction as predicted by BH model. The ripple wavelength is independent of ion dose, while ripple amplitude increases with ion dose. It is found that the ripples are formed by self-organization due to anisotropic surface diffusion in the low melting point metal.     

Redeposition effects in transmission electron microscope specimens of FeAl-WC composites prepared using a focused ion beam

Artifacts associated with transmission electron microscope (TEM) specimens prepared using a focused ion beam (FIB) are not well understood, especially those in non-semiconductor materials. In this paper the extent and origins of artifacts associated with redeposition of milled material in TEM specimens of a FeAl--WC metal matrix composite prepared by FIB were investigated. Cross-sections were prepared normal to an initial FIB cut that allowed direct observation of any damage layers, which are believed to be associated with both redeposition of sputtered material and amorphisation of the surface of the specimen by the ion beam. Techniques for the minimisation of redeposition using either final cleaning mills at low accelerating voltages or plasma cleaning were also investigated and found to be ineffective in removing or reducing these damaged layers. TEM cross-sections of specimens treated using low energy mills and plasma cleaning, further confirmed that these techniques did little to reduce any redeposited or amorphous material.     

Occurrence of particle debris field during focused Ga ion beam milling of glassy carbon

To explore the machining characteristics of glassy carbon by focused ion beam (FIB), particles induced by FIB milling on glassy carbon have been studied in the current work. Nano-sized particles in the range of tens of nanometers up to 400 nm can often be found around the area subject to FIB milling. Two ion beam scanning modes - slow single scan and fast repetitive scan - have been tested. Fewer particles are found in single patterns milled in fast repetitive scan mode. For a group of test patterns milled in a sequence, it was found that a greater number of particles were deposited around sites machined early in the sequence. In situ EDX analysis of the particles showed that they were composed of C and Ga. The formation of particles is related to the debris generated at the surrounding areas, the low melting point of gallium used as FIB ion source and the high contact angle of gallium on glassy carbon induces de-wetting of Ga and the subsequent formation of Ga particles. Ultrasonic cleaning can remove over 98% of visible particles. The surface roughness (R_a) of FIB milled areas after cleaning is less than 2 nm.     

质量分离低能离子束沉积碳膜及离子轰击效应

用质量分离的低能离子束沉积技术得到了非晶碳薄膜,X射线衍射、Raman谱以及俄歇深度谱的线形表明,此种非晶碳膜中镶嵌着金刚石颗粒.碳离子的浅注入是该碳膜SP³形成的主要机理.从一个侧面说明了化学气相沉积法中偏压预处理增加金刚石成核的主要原因是因为离子轰击效应. 关键词： 非晶碳 离子轰击 质量分离低能离子束     

Focused ion beam Moiré method

A focused ion beam (FIB) Moiré method is proposed to measure the in-plane deformation of object in a micrometer scale. The FIB Moiré is generated by the interference between a prepared specimen grating and FIB raster scan lines. The principle of the FIB Moiré is described. The sensitivity and accuracy of deformation measurement are discussed in detail. Several specimen gratings with 0.14 and 0.20 μm spacing are used to generate FIB Moiré patterns. The FIB Moiré method is successfully used to measure the residual deformation in a micro-electro-mechanical system structure after removing the SiO₂ sacrificial layer with a 5000 lines/mm grating. The results demonstrate the feasibility of this method.     

Etched facet and semiconductor/air DBR facet of a AlGaInP laser diode prepared by focused ion beam milling

The study of focused ion beam (FIB) milling for making etched facet and semiconductor/air distributed Bragg reflector (DBR) facets of AlGaInP-based red laser diodes (LD) is presented in this letter. For the Ga ion beam current of 100 pA at fixed accelerated voltage 30 kV, FIB milling rate of GaAs was found to be 0.46 μm³/nC. As a trade-off between high reflectivity and enough technical tolerance, the combination of third Bragg orders of semiconductor wall and air gap was chosen. The deeply etched mirror and distributed Bragg reflector facet consisting of pairs of semiconductor wall/air gap on laser diodes (LD) cavity facets with vertical sidewall on AlGaInP LDs were fabricated by focused Ga ion beam milling. Comparison of the AlGaInP LD with the mirrors between cleaved and FIB made facet was given and discussed.     

Investigating the mechanisms of diamond polishing using Raman spectroscopy

Recent research has shown that a phase transformation of diamond to a different form of carbon is involved when diamonds are polished in the traditional fashion. The question as to how this phase transformation is activated and maintained to produce high wear rates is of great technological interest since it may radically change the way we view the processing of diamond. This paper describes the use of Raman spectroscopy to examine debris produced on the diamond polishing wheel, both during its preparation and during polishing. In addition, polished diamond surfaces were examined for the possible existence of non-diamond surface layers in an attempt to identify material removal mechanisms. Raman spectroscopy proves ideal for these analyses because its relatively high spatial resolution is well suited to the analysis of small wear features and debris particles, and because of the wealth of information it reveals about chemical structure. This level of structural information has been lacking in previous analyses of diamond polishing debris. In addition to the non-diamond carbon found in the wear debris, significant quantities of two iron oxides, magnetite (Fe₃O₄) and haematite (α-Fe₂O₃), were also found. An interesting observation was that a transformation from magnetite to haematite could be induced either by using high power laser excitation or by frictional heating during polishing. It is suggested that some of the Raman peaks previously attributed to lonsdaleite might better be explained by the presence of these oxides.     

Self-assembled film thickness determination by focused ion beam

The thickness evolution of multilayer film is investigated by focused ion beam (FIB) in the domain of polymer multilayers. This method, currently used in the modification and the characterization of integrated circuits, proves it is possible to determine the polymer film thickness. Sample cutting and its observation of the cross-section are performed in the FIB without leaving the vacuum chamber. Two main conclusions can be drawn: (1) the roughness of the film increases with the number of layer deposit, (2) the film growth changes from nonlinear (called exponential) to linear beyond 300 nm (70 layers).     

Electrical and piezoresistive properties of ion beam deposited DLC films

In present study diamond like carbon (DLC) films were deposited by closed drift ion source from the acetylene gas. The electrical and piezoresistive properties of ion beam synthesized DLC films were investigated. Diode-like current–voltage characteristics were observed both for DLC/nSi and DLC/pSi heterostructures. This fact was explained by high density of the irradiation-induced defects at the DLC/Si interface. Ohmic conductivity was observed for DLC/nSi heterostructure and metal/DLC/metal structure at low electric fields. At higher electric fields forward current transport was explained by Schottky emission and Poole–Frenkel emission for the DLC/nSi heterostructures and by Schottky emission and/or space charge limited currents for the DLC/pSi heterostructures. Strong dependence of the diamond like carbon film resistivity on temperature has been observed. Variable range hopping current transport mechanism at low electric field was revealed. Diamond like carbon piezoresistive elements with a gauge factor in 12–19 range were fabricated.     

Focused ion beam milling and ultramicrotomy of mineralised ivory dentine for analytical transmission electron microscopy

The use of focused ion beam (FIB) milling for preparation of sections of mineralised ivory dentine for transmission electron microscopy (TEM) is investigated. Ivory dentine is essentially composed of fibrillar type-I collagen and apatite crystals. The aim of this project is to gain a clearer understanding of the relationship between the organic and inorganic components of ivory dentine using analytical TEM, in order to utilise these analytical techniques in the context of common skeletal diseases such as osteoporosis and arthritis. TEM sections were prepared in both single and dual beam FIB instruments, using two standard lift-out techniques, in situ and ex situ. The FIB sections were systematically compared with sections prepared by ultramicrotomy, the traditional preparation route in biological systems, in terms of structural and chemical differences. A clear advantage of FIB milling over ultramicrotomy is that dehydration, embedding and section flotation can be eliminated, so that partial mineral loss due to dissolution is avoided. The characteristic banding of collagen fibrils was clearly seen in FIB milled sections without the need for any chemical staining, as is commonly employed in ultramicrotomy. The FIB milling technique was able to produce high-quality TEM sections of ivory dentine, which are suitable for further investigation using electron energy-loss spectroscopy (EELS) and energy-filtering TEM (EFTEM) to probe the collagen/apatite interface.     

氧回旋离子束刻蚀化学气相沉积金刚石膜

利用非对称磁镜场电子回旋共振等离子体产生的氧回旋离子束刻蚀了化学气相沉积金刚石膜,研究了工作气压和磁电加热电压对金刚石样品附近的离子温度和密度的影响,并分析了金刚石膜的刻蚀和机械抛光效果。结果表明:当工作气压为0.03 Pa,磁电加热电压为200 V时,离子温度和密度最大,分别为7.38 eV和 23.81010 cm-3 。在此优化条件下刻蚀金刚石膜4 h后,其表面粗糙度由刻蚀前的3.525 m降为2.512 m,机械抛光15 min后,表面粗糙度降低为0.517 m,即金刚石膜经离子束刻蚀后可显著提高机械抛光效率。     

Focused ion beam based sputtering yield measurements on ZnO and Mo thin films

In order to facilitate the lateral structuring of solar cell multilayer structures, the ion beam sputtering behaviour of Mo and ZnO thin films deposited onto soda-lime glass and single crystalline Si substrates was studied. Prior to ion beam processing the layers were analyzed by Energy Dispersive X-Ray Spectrometry (EDS), X-Ray Diffractometry (XRD) and Rutherford Backscattering (RBS). In order to characterize the ion beam sputtering of the investigated layers, 2×2 μm² fractions of the thin films were removed by a scanned 30 keV focused Ga⁺ ion beam (FIB) in a dual beam system. SEM images taken during the milling process allowed continuous monitoring of the process without breaking the vacuum. The depth of the groove after removal of the layers was measured by Atomic Force Microscopy (AFM) and was plotted as a function of the ion dose. The sputtering depth has a dependence on the ion dose that is close to linear. The deviation from linearity is produced by heating effects at high beam currents. Sputtering yield values calculated from the experiments and simulations showed good agreement in the case of Mo but deviation was found in the case of ZnO.     

Irradiation effect of yttria-stabilized zirconia by high dose dual ion beam irradiation

Yttria-stabilized zirconia （YSZ） is irradiated with 2.0-MeV Au2＋ ions and 30-keV He＋ ions. Three types of He, Au, Au ＋ He （successively） ion irradiation are performed. The maximum damage level of a sequential dual ion beam implanted sample is smaller than single Au ion implanted sample. A comparable volume swelling is found in a sequential dual ion beam irradiated sample and it is also found in a single Au ion implanted sample. Both effects can be explained by the partial reorganization of the dislocation network into weakly damaged regions in the dual ion beam implanted YSZ. A vacancy-assisted helium trapping/diffusion mechanism in the dual ion beam irradiated condition is discussed. No phase transformation or amorphization behavior happens in all types of ion irradiated YSZ.     

Sample preparation by focused ion beam micromachining for transmission electron microscopy imaging in front-view

This article deals with the development of an original sample preparation method for transmission electron microscopy (TEM) using focused ion beam (FIB) micromachining. The described method rests on the use of a removable protective shield to prevent the damaging of the sample surface during the FIB lamellae micromachining. It enables the production of thin TEM specimens that are suitable for plan view TEM imaging and analysis of the sample surface, without the deposition of a capping layer. This method is applied to an indented silicon carbide sample for which TEM analyses are presented to illustrate the potentiality of this sample preparation method.