Analysis of the Focusing Ion Beam Microscope Ion Mirror Method for Studying Influence of the Measuring Chamber

The growth of Ag films deposited on various substrate materials such as MoS2, mica, graphite, and MgO has been investigated extensively using the in situ electron microscopy technique. The three stages of film growth, namely, the nucleation, growth of islands followed by liquid-like coalescence have been observed in both the vacuum vapor deposited and ion beam sputtered thin films. The mechanisms of nucleation and growth of silver films formed by ion beam sputtering on the (111) plane of silicon comprise the subject of this paper. A novel mode of epitaxial growth is observed to that seen previously.The experimental arrangement for the present study is the same as previous experiments, and the preparation procedure for obtaining thin silicon substrate is presented in a separate paper.

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Effects of Ion Beam Milling on Surface Topography

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100070862 ◽

1973 ◽

Vol 31 ◽

pp. 84-85

Author(s):

P.G. Pawar ◽

P. Duhamel ◽

G.W. Monk

Keyword(s):

Surface Topography ◽

Ion Beam ◽

Solid Material ◽

Beam Current ◽

Atomic Mass ◽

Micro Milling ◽

Ion Milling ◽

Controlled Atmospheres ◽

Milling Operations ◽

Sufficient Energy

A beam of ions of mass greater than a few atomic mass units and with sufficient energy can remove atoms from the surface of a solid material at a useful rate. A system used to achieve this purpose under controlled atmospheres is called an ion miliing machine. An ion milling apparatus presently available as IMMI-III with a IMMIAC was used in this investigation. Unless otherwise stated, all the micro milling operations were done with Ar+ at 6kv using a beam current of 100 μA for each of the two guns, with a specimen tilt of 15° from the horizontal plane.It is fairly well established that ion bombardment of the surface of homogeneous materials can produce surface topography which resembles geological erosional features.

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Nucleation and Early Growth of Sputtered thin Films

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100069570 ◽

1970 ◽

Vol 28 ◽

pp. 516-517

Author(s):

Dudley M. Sherman ◽

Thos. E. Hutchinson

Keyword(s):

Thin Films ◽

Electron Beam ◽

Ion Beam ◽

Ion Source ◽

Water Cooling ◽

Stages Of Growth ◽

Lens Assembly ◽

Microscope Technique ◽

Ion Beam Sputter Deposition

The in situ electron microscope technique has been shown to be a powerful method for investigating the nucleation and growth of thin films formed by vacuum vapor deposition. The nucleation and early stages of growth of metal deposits formed by ion beam sputter-deposition are now being studied by the in situ technique.A duoplasmatron ion source and lens assembly has been attached to one side of the universal chamber of an RCA EMU-4 microscope and a sputtering target inserted into the chamber from the opposite side. The material to be deposited, in disc form, is bonded to the end of an electrically isolated copper rod that has provisions for target water cooling. The ion beam is normal to the microscope electron beam and the target is placed adjacent to the electron beam above the specimen hot stage, as shown in Figure 1.

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SEM analysis of DC magnetron sputtered beryllium films

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100106867 ◽

1988 ◽

Vol 46 ◽

pp. 960-961

Author(s):

E. F. Lindsey ◽

C. W. Price ◽

E. L. Pierce ◽

E. J. Hsieh

Keyword(s):

Fine Structure ◽

Electron Emission ◽

Secondary Electron ◽

Low Voltage ◽

Ion Beam ◽

Secondary Electron Emission ◽

Sem Analysis ◽

Fused Silica ◽

Grain Structure ◽

Silica Substrate

Columnar structures produced by DC magnetron sputtering can be altered by using RF biased sputtering or by exposing the film to nitrogen pulses during sputtering, and these techniques are being evaluated to refine the grain structure in sputtered beryllium films deposited on fused silica substrates. Beryllium is brittle, and fractures in sputtered beryllium films tend to be intergranular; therefore, a convenient technique to analyze grain structure in these films is to fracture the coated specimens and examine them in an SEM. However, fine structure in sputtered deposits is difficult to image in an SEM, and both the low density and the low secondary electron emission coefficient of beryllium seriously compound this problem. Secondary electron emission can be improved by coating beryllium with Au or Au-Pd, and coating also was required to overcome severe charging of the fused silica substrate even at low voltage. The coating structure can obliterate much of the fine structure in beryllium films, but reasonable results were obtained by using the high-resolution capability of an Hitachi S-800 SEM and either ion-beam coating with Au-Pd or carbon coating by thermal evaporation.

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Ion Beam Induced Interfacial Reactions in Molybdenum Thin Films on Silicon

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100097466 ◽

1981 ◽

Vol 39 ◽

pp. 162-163

Author(s):

L. J. Chen ◽

L. S. Hung ◽

J. W. Mayer

Keyword(s):

Ion Beam ◽

Chemical Vapor ◽

Interfacial Reactions ◽

Practical Applications ◽

Microelectronic Devices ◽

Recent Emergence ◽

Chemical Vapor Deposited ◽

Atomic Mixing ◽

Silicon Interface ◽

Kinetics Of

When an energetic ion penetrates through an interface between a thin film (of species A) and a substrate (of species B), ion induced atomic mixing may result in an intermixed region (which contains A and B) near the interface. Most ion beam mixing experiments have been directed toward metal-silicon systems, silicide phases are generally obtained, and they are the same as those formed by thermal treatment.Recent emergence of silicide compound as contact material in silicon microelectronic devices is mainly due to the superiority of the silicide-silicon interface in terms of uniformity and thermal stability. It is of great interest to understand the kinetics of the interfacial reactions to provide insights into the nature of ion beam-solid interactions as well as to explore its practical applications in device technology.About 500 Å thick molybdenum was chemical vapor deposited in hydrogen ambient on (001) n-type silicon wafer with substrate temperature maintained at 650-700°C. Samples were supplied by D. M. Brown of General Electric Research & Development Laboratory, Schenectady, NY.

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The Microstructure of Nickel Oxide Scales

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100097144 ◽

1981 ◽

Vol 39 ◽

pp. 86-87

Author(s):

M. T. Tinker ◽

L. W. Hobbs

Keyword(s):

Electron Microscopy ◽

Nickel Oxide ◽

Ion Beam ◽

Oxide Scales ◽

Nickel Substrate ◽

Outward Diffusion ◽

Transmission Electron ◽

Nickel Substrates ◽

Nickel Base ◽

Technological Interest

There is considerable technological interest in oxidation of nickel because of the importance of nickel-base superalloys in high-temperature oxidizing environments. NiO scales on nickel grow classically, by outward diffusion of nickel through the scale, and are among the most studied of oxidation systems. We report here the first extensive characterization by transmission electron microscopy of nickel oxide scales formed on bulk nickel substrates and sectioned both parallel and transversely to the Ni/NiO interface.Electrochemically-polished nickel sheet of 99.995% purity was oxidized at 1273 K in 0.1 MPa oxygen partial pressure for times between 5 s and 25 h. Parallel sections were produced using a combination of electropolishing of the nickel substrate and ion-beam thinning of the scale to any desired depth in the scale. Transverse sections were prepared by encasing stacked strips of oxidized nickel sheet in epoxy resin, sectioning transversely and ion-beam thinning until thin area spanning one or more interfaces was obtained.

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Lorentz electron microscopy of magnetic domains in rapidly solidified and annealed Pt-Co-B alloys

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100088233 ◽

1991 ◽

Vol 49 ◽

pp. 784-785

Author(s):

N. Qiu ◽

J. E. Wittig

Keyword(s):

Rapid Solidification ◽

Ion Beam ◽

Magnetic Behavior ◽

High Coercivity ◽

Magnetic Domains ◽

Beam Angle ◽

Tem Analysis ◽

Intrinsic Coercivity ◽

Hard Magnets ◽

Rapidly Solidified

PtCo hard magnets have specialized applications owing to their relatively high coercivity combined with corrosion resistance and ductility. Increased intrinsic coercivity has been recently obtained by rapid solidification processing of PtCo alloys containing boron. After rapid solidification by double anvil splat quenching and subsequent annealing for 30 minutes at 650°C, an alloy with composition Pt42Co45B13 (at.%) exhibited intrinsic coercivity up to 14kOe. This represents a significant improvement compared to the average coercivities in conventional binary PtCo alloys of 5 to 8 kOe.Rapidly solidified specimens of Pt42Co45B13 (at.%) were annealed at 650°C and 800°C for 30 minutes. The magnetic behavior was characterized by measuring the coercive force (Hc). Samples for TEM analysis were mechanically thinned to 100 μm, dimpled to about 30 nm, and ion milled to electron transparency in a Gatan Duomill at 5 kV and 1 mA gun current. The incident ion beam angle was set at 15° and the samples were liquid nitrogen cooled during milling. These samples were analyzed with a Philips CM20T TEM/STEM operated at 200 kV.

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AEM investigation of ZrO2 solid solution formation in ZrO2/mullite composites

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100112087 ◽

1984 ◽

Vol 42 ◽

pp. 408-409

Author(s):

T. R. Dinger

Keyword(s):

Solid Solution ◽

Ion Beam ◽

Analytical Electron Microscopy ◽

Transformation Toughening ◽

Solid Solution Formation ◽

Solution Formation ◽

Propagating Crack ◽

Analytical Electron ◽

Microcrack Toughening ◽

Made In

Zirconia (ZrO2) is often added to ceramic compacts to increase their toughness. The mechanisms by which this toughness increase occurs are generally accepted to be those of transformation toughening and microcracking. The mechanism of transformation toughening is based on the presence of metastable tetragonal ZrO2 which transforms to the monoclinic allotrope when stressed by a propagating crack. The decrease in volume which accompanies this transformation effectively relieves the applied stress at the crack tip and toughens the material; microcrack toughening arises from the deflection of a propagating crack around sharply angular inclusions.These mechanisms, however, do not explain the toughness increases associated with the class of composites investigated here. Analytical electron microscopy (AEM) has been used to determine whether solid solution effects could be the cause of this increased toughness. Specimens of a mullite (3Al2O3·2SiO2) + 15 vol. % ZrO2 were prepared by the usual technique of mechanical thinning followed by ion beam milling. All observations were made in a Philips EM400 TEM/STEM microscope fitted with EDXS and EELS spectrometers.

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Preparation of TEM samples by focused ion beams

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100138968 ◽

1995 ◽

Vol 53 ◽

pp. 518-519

Author(s):

John F. Walker ◽

J C Reiner ◽

C Solenthaler

Keyword(s):

Integrated Circuit ◽

Polycrystalline Silicon ◽

Field Effect Transistor ◽

High Spatial Resolution ◽

Ion Beam ◽

Ion Beams ◽

Focused Ion Beams ◽

Precise Location ◽

Effect Transistor ◽

Circuit Technology

The high spatial resolution available from TEM can be used with great advantage in the field of microelectronics to identify problems associated with the continually shrinking geometries of integrated circuit technology. In many cases the location of the problem can be the most problematic element of sample preparation. Focused ion beams (FIB) have previously been used to prepare TEM specimens, but not including using the ion beam imaging capabilities to locate a buried feature of interest. Here we describe how a defect has been located using the ability of a FIB to both mill a section and to search for a defect whose precise location is unknown. The defect is known from electrical leakage measurements to be a break in the gate oxide of a field effect transistor. The gate is a square of polycrystalline silicon, approximately 1μm×1μm, on a silicon dioxide barrier which is about 17nm thick. The break in the oxide can occur anywhere within that square and is expected to be less than 100nm in diameter.

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Atomic force microscopy (AFM) of the topography of silicon surfaces exposed to ion beams

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100130298 ◽

1992 ◽

Vol 50 (2) ◽

pp. 1132-1133

Author(s):

Mark Denker ◽

Jennifer Wall ◽

Mark Ray ◽

Richard Linton

Keyword(s):

Secondary Ion Mass Spectrometry ◽

Incidence Angle ◽

Ion Beam ◽

Depth Profiling ◽

Depth Resolution ◽

Ion Beams ◽

Scanning Tunneling ◽

Tunneling Microscopy ◽

Trace Impurities ◽

Energy Dose

Reactive ion beams such as O2+ and Cs+ are used in Secondary Ion Mass Spectrometry (SIMS) to analyze solids for trace impurities. Primary beam properties such as energy, dose, and incidence angle can be systematically varied to optimize depth resolution versus sensitivity tradeoffs for a given SIMS depth profiling application. However, it is generally observed that the sputtering process causes surface roughening, typically represented by nanometer-sized features such as cones, pits, pyramids, and ripples. A roughened surface will degrade the depth resolution of the SIMS data. The purpose of this study is to examine the relationship of the roughness of the surface to the primary ion beam energy, dose, and incidence angle. AFM offers the ability to quantitatively probe this surface roughness. For the initial investigations, the sample chosen was <100> silicon, and the ion beam was O2+.Work to date by other researchers typically employed Scanning Tunneling Microscopy (STM) to probe the surface topography.

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