Comparison TEM specimen preparation of perovskite thin films by conventional Ar ion milling and tripod polishing

AbstractThin films of YAG and YAG/alumina mixtures were prepared by gelling a sol across a TEM grid. The grids were heat-treated to temperatures as high as 1550°C. The resulting ceramic thin films were observed by standard and high resolution TEM techniques. Ion-milling, carbon coating, or other specimen preparation was not necessary. The phase and microstructure evolution, as well as pore structure evolution and spheroidization of film edges could be easily observed. Abnormal grain growth was observed in yttrium-aluminum garnet (YAG) films. Lattice images were taken of the matrix, abnormal grains, and structures that evolved from the abnormal rains at higher temperatures. The grain size preceding abnormal grain growth was 20–50 nm. The abnormal grains were composed of 20–50 nm subgrains with up to several degrees of misorientation. High resolution observations were also made of small (< 0.2 μm) YAG inclusions in alumina. An orientation relationship of (111)[011]alumina//(112)[021]YAGwas observed. This orientation relationship was not observed in large inclusions.

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Comparison of TEM specimen preparation of perovskite thin films by tripod polishing and conventional ion milling

Journal of Electron Microscopy ◽

10.1093/jmicro/dfn018 ◽

2008 ◽

Vol 57 (6) ◽

pp. 175-179 ◽

Cited By ~ 22

Author(s):

E. Eberg ◽

A. F. Monsen ◽

T. Tybell ◽

A. T. J. van Helvoort ◽

R. Holmestad

Keyword(s):

Thin Films ◽

Specimen Preparation ◽

Ion Milling

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Direct Observation by Transmission Electron Microscopy of the Early Stages of Growth of Superconducting Thin Films

MRS Proceedings ◽

10.1557/proc-169-509 ◽

1989 ◽

Vol 169 ◽

Cited By ~ 3

Author(s):

M. Grant Norton ◽

Lisa A. Tietz ◽

Scott R. Summerfelt ◽

C. Barry Carter

Keyword(s):

Electron Microscopy ◽

Thin Films ◽

Transmission Electron Microscopy ◽

Substrate Surface ◽

Critical Role ◽

Specimen Preparation ◽

Superconducting Thin Films ◽

Ion Milling ◽

Early Stages ◽

Transmission Electron

AbstractThe fabrication of high quality thin films often depends on the early stages of the growth process during which epitaxy is established. The substrate surface structure generally plays a critical role at this stage. Many observations of the high‐Tc superconductor film‐substrate interface structure and chemistry have been made by transmission electron microscopy (TEM) of cross‐section samples. Ion‐milling induced damage, however, can be severe in these specimens. In the present study, the early stages of the growth of high Tc superconducting thin films of YBa2Cu3O7&#X03B4; have been studied by TEM using a technique which requires no post‐deposition specimen preparation.

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Imaging Thin Films of Nanoporous Low-k Dielectrics: Comparison between Ultramicrotomy and Focused Ion Beam Preparations for Transmission Electron Microscopy

Microscopy and Microanalysis ◽

10.1017/s1431927606060041 ◽

2005 ◽

Vol 12 (2) ◽

pp. 156-159 ◽

Cited By ~ 11

Author(s):

Leslie E. Thompson ◽

Philip M. Rice ◽

Eugene Delenia ◽

Victor Y. Lee ◽

Phillip J. Brock ◽

...

Keyword(s):

Thin Films ◽

Cross Section ◽

Focused Ion Beam ◽

Preparation Method ◽

Ion Beam ◽

Specimen Preparation ◽

Ion Milling ◽

Transmission Electron ◽

Low K ◽

Diamond Knife

Ultramicrotomy, the technique of cutting nanometers-thin slices of material using a diamond knife, was applied to prepare transmission electron microscope (TEM) specimens of nanoporous poly(methylsilsesquioxane) (PMSSQ) thin films. This technique was compared to focused ion beam (FIB) cross-section preparation to address possible artifacts resulting from deformation of nanoporous microstructure during the sample preparation. It was found that ultramicrotomy is a successful TEM specimen preparation method for nanoporous PMSSQ thin films when combined with low-energy ion milling as a final step. A thick, sacrificial carbon coating was identified as a method of reducing defects from the FIB process which included film shrinkage and pore deformation.

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Microstructural characterization of YBa2Cu3O7-x thin films formed by metalorganic CVD

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100089718 ◽

1991 ◽

Vol 49 ◽

pp. 1080-1081

Author(s):

P. Lu ◽

W. Huang ◽

C.S. Chern ◽

Y.Q. Li ◽

J. Zhao ◽

...

Keyword(s):

Thin Film ◽

Thin Films ◽

Critical Current Density ◽

Critical Current ◽

Current Density ◽

Film Growth ◽

Chemical Vapor ◽

Microstructural Characterization ◽

Ion Milling ◽

Conventional Grinding

The YBa2Cu3O7-x thin films formed by metalorganic chemical vapor deposition(MOCVD) have been reported to have excellent superconducting properties including a sharp zero resistance transition temperature (Tc) of 89 K and a high critical current density of 2.3x106 A/cm2 or higher. The origin of the high critical current in the thin film compared to bulk materials is attributed to its structural properties such as orientation, grain boundaries and defects on the scale of the coherent length. In this report, we present microstructural aspects of the thin films deposited on the (100) LaAlO3 substrate, which process the highest critical current density.Details of the thin film growth process have been reported elsewhere. The thin films were examined in both planar and cross-section view by electron microscopy. TEM sample preparation was carried out using conventional grinding, dimpling and ion milling techniques. Special care was taken to avoid exposure of the thin films to water during the preparation processes.

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Corrections for surface films in microanalysis by EDS and EELS

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010013078x ◽

1992 ◽

Vol 50 (2) ◽

pp. 1230-1231

Author(s):

J. Bentley ◽

E. A. Kenik

Keyword(s):

Hydrocarbon Contamination ◽

Specimen Preparation ◽

Surface Films ◽

Ion Milling ◽

Preferential Sputtering ◽

Electron Energy Loss Spectrometry ◽

Composition Determination ◽

Analytical Electron ◽

First Order Correction ◽

Electron Energy Loss

Common artifacts on analytical electron microscope (AEM) specimens prepared from bulk materials are surface films with altered structure and composition that result from electropolishing, oxidation, hydrocarbon contamination, or ion milling (preferential sputtering or deposition of sputtered specimen or support material). Of course, the best solution for surface films is to avoid them by improved specimen preparation and handling procedures or to remove them by low energy ion sputter cleaning, a capability that already exists on some specialized AEMs and one that is likely to become increasingly common. However, the problem remains and it is surprising that surface films have not received more attention with respect to composition determination by energy dispersive X-ray spectrometry (EDS) and electron energy loss spectrometry (EELS).For EDS, an effective first-order correction to remove the contribution of surface films on wedge shaped specimens is to subtract from the spectrum of interest a spectrum obtained under identical conditions (probe current, diffracting conditions, acquisition live time) from a thinner region of the specimen.

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Microscopy of porous ceramics

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100154160 ◽

1989 ◽

Vol 47 ◽

pp. 438-439

Author(s):

H. M. Kerch ◽

R. A. Gerhardt

Keyword(s):

Porous Ceramics ◽

Specimen Preparation ◽

High Porosity ◽

Ion Milling ◽

Forming Process ◽

Preparation Methods ◽

Pore Texture ◽

Proper Design ◽

And Function ◽

Function Information

Highly porous ceramics are employed in a variety of engineering applications due to their unique mechanical, optical, and electrical characteristics. In order to achieve proper design and function, information about the pore structure must be obtained. Parameters of importance include pore size, pore volume, and size distribution, as well as pore texture and geometry. A quantitative determination of these features for high porosity materials by a microscopic technique is usually not done because artifacts introduced by either the sample preparation method or the image forming process of the microscope make interpretation difficult.Scanning electron microscopy for both fractured and polished surfaces has been utilized extensively for examining pore structures. However, there is uncertainty in distinguishing between topography and pores for the fractured specimen and sample pullout obscures the true morphology for samples that are polished. In addition, very small pores (nm range) cannot be resolved in the S.E.M. On the other hand, T.E.M. has better resolution but the specimen preparation methods involved such as powder dispersion, ion milling, and chemical etching may incur problems ranging from preferential widening of pores to partial or complete destruction of the pore network.

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A procedure for cross-sectioning materials for TEM analysis without ion milling

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100176848 ◽

1990 ◽

Vol 48 (4) ◽

pp. 742-743

Author(s):

J.P. Benedict ◽

Ron Anderson ◽

S. J. Klepeis

Keyword(s):

Surface Topography ◽

Milling Time ◽

Specimen Preparation ◽

Ion Milling ◽

Cleaning Operation ◽

Tem Analysis ◽

Platinum Silicide ◽

Surface Alteration ◽

Polishing Damage ◽

Tools And Methods

Traditional specimen preparation procedures for non-biological samples, especially cross section preparation procedures, involves subjecting the specimen to ion milling for times ranging from minutes to tens of hours. Long ion milling time produces surface alteration, atomic number and rough-surface topography artifacts, and high temperatures. The introduction of new tools and methods in this laboratory improved our ability to mechanically thin specimens to a point where ion milling time was reduced to one to ten minutes. Very short ion milling times meant that ion milling was more of a cleaning operation than a thinning operation. The preferential thinning and the surface topography that still existed in briefly ion milled samples made the study of interfaces between materials such as platinum silicide and silicon difficult. These two problems can be eliminated by completely eliminating the ion milling step and mechanically polishing the sample to TEM transparency with the procedure outlined in this communication. Previous successful efforts leading to mechanically thinned specimens have shown that problems center on tool tilt control, removal of polishing damage, and specimen cleanliness.

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

10.31399/asm.cp.istfa2018p0241 ◽

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.

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Transmission Electron Microscopy of Semiconductor Based Products

MRS Proceedings ◽

10.1557/proc-523-03 ◽

1998 ◽

Vol 523 ◽

Cited By ~ 9

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.

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