Chemically Assisted Ion Beam Etching (CAIBE)- a New Technique for TEM Specimen Preparation of Materials

1990 ◽  
Vol 199 ◽  
Author(s):  
Reza Alani ◽  
Joseph Jones ◽  
Peter Swann
Keyword(s):  
Ion Beam ◽  
Semiconductor Industry ◽  
Active Species ◽  
Inert Gas ◽  
New Technique ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Ion Beam Etching ◽  
Specimen Holder ◽  
Argon Ion

ABSTRACTChemically assisted ion beam etching (CAIBE) is widely practiced in the semiconductor industry. In the electron microscopy field, the CAIBE technique offers a new method for preparing specimens that are difficult to make by conventional inert gas milling techniques, e.g. indium containing type III-V compound semiconductors. CAIBE employs a collimated, molecular beam of a reactive species, e.g. iodine in combination with a conventional inert gas fast atom beam for thinning TEM specimens. CAIBE should not be confused with reactive ion beam etching (RIBE) which takes a chemically active species (e.g. iodine) and converts it into a beam of fast ions directed at the sample. CAIBE has three major advantages over (RIBE): i) corrosion of the ion gun components does not occur, ii) much smaller quantities of reactive gas are required and hence pump maintenance and pollution problems are minimized, iii) a wider range of chemicals may be used. Superior results are obtained if CAIBE is done on only one side of the specimen at a time. This is achieved using a new type of specimen holder post which enables very low angle milling and minimizes specimen contamination by sputtering from the holder. This new technique is described and results from iodine CAIBE milling, iodine RIBE milling and argon ion milling are compared for InP, InSb and GaAs as well as metals like tungsten. Also, the beneficial effects of very low angle (∼1°) argon ion milling in preparing specimens of silicide containing Si based IC wafers is reported.

Narrow-Beam Argon Ion Milling of Ex Situ Lift-Out FIB Specimens Mounted on Various Carbon-Supported Grids

2018 ◽  
Author(s):  
M. J. Campin ◽  
C. S. Bonifacio ◽  
P. Nowakowski ◽  
P. E. Fischione ◽  
L. A. Giannuzzi
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Carbon Support ◽  
Ex Situ ◽  
Specimen Preparation ◽  
Narrow Beam ◽  
Ion Milling ◽  
Preparation Methods ◽  
Argon Ion

Abstract The semiconductor industry recently has been investigating new specimen preparation methods that can improve throughput while maintaining quality. The result has been a combination of focused ion beam (FIB) preparation and ex situ lift-out (EXLO) techniques. Unfortunately, the carbon support on the EXLO grid presents problems if the lamella needs to be thinned once it is on the grid. In this paper, we show how low-energy (< 1 keV), narrow-beam (< 1 μm diameter) Ar ion milling can be used to thin specimens and remove gallium from EXLO FIB specimens mounted on various support grids.

Recent Advances in Broad Ion Beam Based Techniques/Instrumentation for SEM Specimen Preparation of Semiconductors

1999 ◽  
Author(s):  
R. Alani ◽  
R. J. Mitro ◽  
W. Hauffe
Keyword(s):  
Cross Sections ◽  
Chemical Etching ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Inert Gas ◽  
Specimen Preparation ◽  
Ion Beam Etching ◽  
Wet Chemical ◽  
Wet Chemical Etching

Abstract The semiconductor industry routinely prepares crosssectional SEM specimens using several traditional techniques. Included in these are cleaving, mechanical polishing, wet chemical etching and focused ion beam (FIB) milling. This presentation deals with a new alternate method for preparation of SEM semiconductor specimens based upon a dedicated broad ion beam instrument. Offered initially as an alternative to wet chemical etching, the instrument was designed to etch and coat SEM and metallographic specimens in one vacuum chamber using inert gas (Ar) ion beams. The system has recently undergone further enhancement by introducing iodine Reactive Ion Beam Etching (RIBE) producing much improved etching/cleaning capabilities compared with inert gas ion beam etching. Further results indicate Ar broad ion beam etching can offer a rapid, simple, more affordable alternative (to FIB machines) for precision cross sections and for “slope cutting,” a technique producing large cross-sections within a short time frame. The overall effectiveness of this system for iodine RIBE etching, for precision cross sectioning and “slope cutting” will be shown for a number of traditional and advanced semiconductor devices.

Chemically assisted ion-beam etching in a low-angle ion mill

1993 ◽  
Vol 51 ◽  
pp. 718-719
Author(s):  
R. Alani ◽  
P.R. Swann
Keyword(s):  
Nitrous Oxide ◽  
Ion Beam ◽  
Diamond Films ◽  
Compound Semiconductors ◽  
Inert Gas ◽  
Specimen Preparation ◽  
Ion Beam Etching ◽  
Preferential Sputtering ◽  
Argon Ion ◽  
Reactive Gas

In conventional ion mills, chemically assisted ion beam etching (CAIBE) has become an establish method for TEM specimen preparation of certain materials. CAIBE employs a reactive gas which brought in contact with the specimen through a jet assembly, while an inert gas ion beam is directed on the same area. Therefore, thinning occurs by the combination of chemical reaction and physic sputtering, which leads to enhanced thinning rates. The reactive gas used in the CAIBE technique can generated from a solid source which sublimes e.g. iodine or it can be injected directly from a pressuriz gas bottle e.g. nitrous oxide. Nitrous oxide in combination with a xenon ion beam has been used from cross sectioning TEM specimens of diamond films on silicon.It is well known that indium-containing compound semiconductors develop indium islands on the surface when thinned with an argon ion beam. It is believed that preferential sputtering enriches the surface with indium and that heating by the ion beam melts the indium which then agglomerates to for small globules on the surface.

Low Energy Ar Ion Milling of FIB TEM Specimens from 14 nm and Future FinFET Technologies

2018 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
M.L. Ray ◽  
P.E. Fischione
Keyword(s):  
Field Effect Transistor ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
High Resolution Tem ◽  
Effect Transistor ◽  
20 Nm ◽  
Argon Ion

Abstract Transmission electron microscopy (TEM) specimens are typically prepared using the focused ion beam (FIB) due to its site specificity, and fast and accurate thinning capabilities. However, TEM and high-resolution TEM (HRTEM) analysis may be limited due to the resulting FIB-induced artifacts. This work identifies FIB artifacts and presents the use of argon ion milling for the removal of FIB-induced damage for reproducible TEM specimen preparation of current and future fin field effect transistor (FinFET) technologies. Subsequently, high-quality and electron-transparent TEM specimens of less than 20 nm are obtained.

Transmission Electron Microscopy of Semiconductor Based Products

1998 ◽  
Vol 523 ◽  
Author(s):  
John Mardinly ◽  
David W. Susnitzky
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Size Reduction ◽  
Specimen Preparation ◽  
Specimen Thickness ◽  
Ion Milling ◽  
Feature Size ◽  
Transmission Electron

AbstractThe demand for increasingly higher performance semiconductor products has stimulated the semiconductor industry to respond by producing devices with increasingly complex circuitry, more transistors in less space, more layers of metal, dielectric and interconnects, more interfaces, and a manufacturing process with nearly 1,000 steps. As all device features are shrunk in the quest for higher performance, the role of Transmission Electron Microscopy as a characterization tool takes on a continually increasing importance over older, lower-resolution characterization tools, such as SEM. The Ångstrom scale imaging resolution and nanometer scale chemical analysis and diffraction resolution provided by modem TEM's are particularly well suited for solving materials problems encountered during research, development, production engineering, reliability testing, and failure analysis. A critical enabling technology for the application of TEM to semiconductor based products as the feature size shrinks below a quarter micron is advances in specimen preparation. The traditional 1,000Å thick specimen will be unsatisfactory in a growing number of applications. It can be shown using a simple geometrical model, that the thickness of TEM specimens must shrink as the square root of the feature size reduction. Moreover, the center-targeting of these specimens must improve so that the centertargeting error shrinks linearly with the feature size reduction. To meet these challenges, control of the specimen preparation process will require a new generation of polishing and ion milling tools that make use of high resolution imaging to control the ion milling process. In addition, as the TEM specimen thickness shrinks, the thickness of surface amorphization produced must also be reduced. Gallium focused ion beam systems can produce hundreds of Ångstroms of amorphised surface silicon, an amount which can consume an entire thin specimen. This limitation to FIB milling requires a method of removal of amorphised material that leaves no artifact in the remaining material.

Ion-Beam Milling Materials with Applications to TEM Specimen Preparation

1996 ◽  
Vol 54 ◽  
pp. 266-267
Author(s):  
Ron Anderson
Keyword(s):  
Glow Discharge ◽  
Ion Beam ◽  
Reactive Ion Etching ◽  
Dry Etching ◽  
Surface Cleaning ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Physical Sciences ◽  
Ion Etching ◽  
Ion Beam Etching

For the last thirty years, ion milling has been an indispensable part of preparing TEM specimens in the physical sciences. While great improvements have been made in our ability to thin most materials to the point where ion milling may not be a requirement, there will still be a need to utilize ion milling to clean and polish specimens and to provide small amounts of incremental thinning as needed. Thanks mainly to the work of Bama we now understand a great deal about the physics of ion milling. We also benefit from the works of a number of investigators who have studied the artifacts produced by ion milling (see Barber for a review).Ion milling is a subset of the topic “dry etching,” which consists of two major categories: glow discharge methods and ion beam methods. Glow discharge methods include plasma etching, reactive ion etching, and glow discharge sputter etching. These techniques have little application in TEM specimen preparation aside from surface cleaning. The reactive ion etching literature is a source for suggesting gas/specimen combinations to perform chemically-assisted ion beam etching (CAIBE), to be discussed below. The other major dry etching category, ion beam methods, includes ion milling, reactive ion beam etching, and CAIBE.

Automated End-Point Detection and Targeted Ar+ Milling of Advanced Integrated Circuit FIB TEM Specimens

2017 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
J.T. Harbaugh ◽  
M. Boccabella ◽  
...  
Keyword(s):  
Integrated Circuits ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
End Point Detection ◽  
Point Detection ◽  
Argon Ion

Abstract The sub-nanometer resolution that transmission electron microscopy (TEM) provides is critical to the development and fabrication of advanced integrated circuits. TEM specimens are usually prepared using the focused ion beam, which can cause gallium-induced artifacts and amorphization. This work presents the use of a concentrated argon ion beam for reproducible TEM specimen preparation using automatic milling termination and targeted ion milling of device features; the result is high-quality and electron-transparent specimens of less than 30 nm. Such work is relevant for semiconductor product development and failure analysis.

Focused Ion Beam Sample Preparation of Non-Semiconductor Materials

1997 ◽  
Vol 480 ◽  
Author(s):  
M. W. Phaneuf ◽  
N. Rowlands ◽  
G. J. C. Carpenter ◽  
G. Sundaram
Keyword(s):  
Cross Sections ◽  
Automobile Industry ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Semiconductor Materials ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Cross Sectional ◽  
Galvannealed Steel

AbstractFocused Ion Beam (FIB) systems have been steadily gaining acceptance as specimen preparation tools in the semiconductor industry. This is largely due to the fact that such instruments are relatively commonplace as failure analysis tools in semiconductor houses, and are commonly used in the preparation of cross-sections for imaging under the ion beam or using an electron beam in an SEM. Additionally, the ease with which cross-sectional TEM specimens of semiconductor devices can be prepared using FIB systems has been well demonstrated. However, this technology is largely unknown outside the semiconductor industry. Relatively few references exist in the literature on the preparation of cross-sectional TEM specimens of non-semiconductor materials by FIB. This paper discusses a specific use of FIB technology in the preparation of cross-sectional TEM specimens of non-semiconductor samples that are difficult to prepare by conventional means. One example of such materials is commercial galvannealed steel sheet that is used to form corrosion resistant auto-bodies for the automobile industry. Cross-sectional TEM specimens of this material have proved difficult and time-intensive to prepare by standard polishing and ion milling techniques due to galvanneal's inherent flaking and powdering difficulties, as well as the different sputtering rates of the various Fe-Zn intermetallic phases present in the galvannealed coatings. TEM results from cross-sectional samples of commercial galvannealed steel coatings prepared by conventional ion milling and FIB techniques are compared to assess image quality, the size of the electron-transparent thin regions that can be readily prepared and the quality of samples produced by both techniques. Specimen preparation times for both techniques are reported.

Reactive Ion Beam Etching (RIBE) Technique and Instrumentation for SEM Specimen Preparation of Semiconductors

1999 ◽  
Vol 5 (S2) ◽  
pp. 912-913
Author(s):  
R. Alani ◽  
R.J. Mitro ◽  
K. Ogura
Keyword(s):  
Ion Beam ◽  
Original System ◽  
Surface Cleaning ◽  
Specimen Preparation ◽  
Cross Sectional ◽  
Ion Beam Etching ◽  
Semiconductor Structures ◽  
Wet Chemical ◽  
Wafer Processing ◽  
Argon Ion

Argon ion beam etching has established itself as an alternative technique to “wet chemical” etching for the preparation of cross sectional SEM specimens of semiconductors [1]. Complementing this technique, we are reporting the results of an iodine RIBE method for improved etching/cleaning capabilities with a measurable increase in etching rates as compared to argon ion beam etching. RIBE systems have been used for decades in the semiconductor research/industry for wafer processing, patterning and surface cleaning. This same technique has also been used for high quality TEM specimen preparation of certain semiconductor materials [2,3]. The beneficial aspects of the iodide RIBE technique for surface etching for a variety of semiconductor structures along with the related instrumentation will be discussed. The semiconductor specimens include traditional ICs and more advanced copper technology devices.The design and construction of the original system used in this work has already been reported [4].

Precision Ion Polishing System -A New Instrument for TEM Specimen Preparation of Materials

1991 ◽  
Vol 254 ◽  
Author(s):  
Reza Alani ◽  
Peter R. Swann
Keyword(s):  
High Speed ◽  
Ion Beam ◽  
Type Specimen ◽  
Vacuum System ◽  
Specimen Preparation ◽  
Ion Milling ◽  
High Voltage Power Supply ◽  
Specimen Holder ◽  
New Instrument ◽  
Work Chamber

AbstractThe article describes the design, construction and performance of a new bench top instrument for high speed ion beam thinning and polishing of materials. In this system, the combination of very low angle ion milling and powerful ion guns has led to the rapid production of high quality TEM specimens. The main subassemblies are (1) a work chamber (2) gas control system (3) vacuum system and (4) electrical system. The work chamber consists of a pair of newly designed Penning type ion guns and Faraday cups to measure ion currents. The Whisperlok™ mechanism provides specimen rotation, pneumatically driven airlock for very fast specimen exchange and transmission/reflection illumination for specimen viewing. The ion guns are mounted to deliver a nominal, 4° milling angle on the specimen surface with precision alignment of ±2° about horizontal and vertical axes. The actual thinning is undertaken from one side using a single, post-type specimen holder which minimizes the specimen heating and contamination. The ion beam current of each gun can be individually optimized by varying the flow rate of the ionizing gas. The main chamber is evacuated by diaphragm and molecular drag pumps to produce a clean, dry vacuum in the 10−6 Torr range. The discharge and accelerating voltages required for the operation of each gun are provided by a dual high voltage power supply capable of delivering ion energies in the range; 1 keV to 6keV. TEM micrographs of typical ion polished specimens of semiconductors, metals, ceramics and composites are included to illustrate the performance of the instrument.

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