Recent Developments in the use of the Tripod Polisher for TEM Specimen Preparation

1991 ◽  
Vol 254 ◽  
Author(s):  
John Benedict ◽  
Ron Anderson ◽  
Stanley J. Klepeis
Keyword(s):  
Cross Sections ◽  
Colloidal Silica ◽  
Mechanical Stability ◽  
Semiconductor Industry ◽  
Polished Surface ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Thin Specimen ◽  
Tem Analysis ◽  
Area Of Interest

AbstractCross sections of material specimens for TEM analysis must be produced in the shortest time possible, contain few, if any, artifacts and have a large area available for analysis. The analyst must also be able to prepare these cross sections from specified areas of complex, heterogeneous structures on a routine, reproducible basis to meet the growing needs of the semiconductor industry for TEM analysis. The specimen preparation spatial resolution required for preparing precision cross sections is substantially less than one micron. Cross sections meeting these requirements can be prepared by mounting a specimen to the Tripod Polisher and mechanically polishing on one side of the specimen, using a sequence of progressively finer grit diamond lapping films, until the area of interest is reached. This polished surface is then very briefly polished on a cloth wheel with colloidal silica to attain the final polish on that side. The specimen is then flipped over on the Tripod Polisher and polished from the other side, using same sequence of diamond lapping films to reach the predefined area of interest. The Tripod Polisher is set at a slight angle, to produce a tapered, wedge-shaped specimen, which has the area of interest at the thinnest edge of the taper. The specimen is polished with the diamond lapping films and the colloidal silica until it is 1000 Angstroms or less in thickness. The specimen is removed from the polisher and mounted on a 2 × 1mm slotted grid with M-Bond 610 epoxy. After the epoxy is cured the specimen can be taken directly to the microscope for analysis. The need for ion milling has been eliminated or reduced to a few minutes in most of our work because of the thinness of the final specimen. The total specimen preparation time is between 2.5 and 4 hours, depending on the specimen and the size of the specified area. The area available for analysis ranges from 0.5mm up to the full size of the mounting grid opening. The wedge shape of the specimen provides the mechanical stability needed for a long thin specimen.

A technique for preparing semiconductor cross sections for both TEM and SEM analysis

1989 ◽  
Vol 47 ◽  
pp. 712-713
Author(s):  
Stanley J. Klepeis ◽  
J.P. Benedict ◽  
R.M Anderson
Keyword(s):  
Sample Preparation ◽  
Cross Section ◽  
Cross Sections ◽  
Sem Analysis ◽  
Preparation Technique ◽  
Ion Milling ◽  
Tem Analysis ◽  
Polished Cross Section ◽  
Area Of Interest ◽  
Polished Side

The ability to prepare a cross-section of a specific semiconductor structure for both SEM and TEM analysis is vital in characterizing the smaller, more complex devices that are now being designed and manufactured. In the past, a unique sample was prepared for either SEM or TEM analysis of a structure. In choosing to do SEM, valuable and unique information was lost to TEM analysis. An alternative, the SEM examination of thinned TEM samples, was frequently made difficult by topographical artifacts introduced by mechanical polishing and lengthy ion-milling. Thus, the need to produce a TEM sample from a unique,cross-sectioned SEM sample has produced this sample preparation technique.The technique is divided into an SEM and a TEM sample preparation phase. The first four steps in the SEM phase: bulk reduction, cleaning, gluing and trimming produces a reinforced sample with the area of interest in the center of the sample. This sample is then mounted on a special SEM stud. The stud is inserted into an L-shaped holder and this holder is attached to the Klepeis polisher (see figs. 1 and 2). An SEM cross-section of the sample is then prepared by mechanically polishing the sample to the area of interest using the Klepeis polisher. The polished cross-section is cleaned and the SEM stud with the attached sample, is removed from the L-shaped holder. The stud is then inserted into the ion-miller and the sample is briefly milled (less than 2 minutes) on the polished side. The sample on the stud may then be carbon coated and placed in the SEM for analysis.

Precision Ion Milling of Layered, Multi-Element TEM Specimens with High Specimen Preparation Spatial Resolution

1991 ◽  
Vol 254 ◽  
Author(s):  
Ron Anderson ◽  
John Benedict
Keyword(s):  
Composite Material ◽  
Failure Analysis ◽  
Spatial Resolution ◽  
Ceramic Composite ◽  
Semiconductor Industry ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Tem Analysis ◽  
Ceramic Composite Material ◽  
Resolution Requirements

It is now a requirement in the semiconductor industry to prepare TEM specimens of pre-specified regions with a specimen preparation resolution exceeding 100nm. In other words, given the coordinates x, y, z of the location desired for TEM analysis, the TEM specimen preparation procedure must yield a thin TEM specimen containing the point x, y, z plus or minus 100nm. Preparation of failure analysis specimens in other fields of endeavor, such as: metallurgical, ceramic, composite material laboratories etc., have specimen preparation spatial resolution requirements below one micron in some cases with the likelihood that greater precision will be required in the future.

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.

A Tutorial of the Fib Lift-Out Technique for TEM Specimen Preparation

1999 ◽  
Vol 5 (S2) ◽  
pp. 516-517
Author(s):  
Lucille A. Giannuzzi
Keyword(s):  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Subsequent Development ◽  
Bulk Sample ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Plan View ◽  
Area Of Interest ◽  
Wide Range

The focused ion beam (FIB) instrument has been developed and exploited by the microelectronics arena for specimen preparation for both scanning and transmission electron microscopy (TEM). The inception [1] and subsequent development [2] of the FIB TEM lift-out (LO) technique has enabled electron transparent membranes of generally uniform thickness to be produced for TEM analysis. The primary advantage of the FIB technique is that site specific cross sections (or plan view sections [3]) may be fabricated quickly and reproducibly. The FIB LO technique has been used extensively in our laboratory for a wide range of materials [4] and biological applications [5] which are summarized in figure 1.The FIB LO method consists of milling a series of trenches around an area of interest. Then the bulk sample is tilted up to ∼60 degrees to allow the beam to impinge on the lower portion of the specimen surface so that cuts can be made along the bottom edge and the lower 2/3 of the distance up one side of the specimen.

Rapid preparation of semiconductor cross sections for TEM analysis

1993 ◽  
Vol 51 ◽  
pp. 708-709
Author(s):  
John Benedict ◽  
Ron Anderson ◽  
Stanley J. Klepeis
Keyword(s):  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specific Area ◽  
Specimen Preparation ◽  
Preparation Time ◽  
Rapid Preparation ◽  
Tem Analysis ◽  
Short Sample ◽  
Area Of Interest

Semiconductor manufacturers examine cross sections of their semiconductor devices to check the quality and integrity of their product. The growing complexity and diminishing size of these devices has caused manufacturers to increasingly rely on the resolving and analytical capabilities of TEM. The manufacturers' requirements for TEM analysis are: high specimen preparation spatial resolution (preparation of a specific area, usually less than 0.5 microns in size), a large sample area (at least 0.5 mm) available for examination, and a short sample preparation time (e.g. several hours). To meet these needs we have developed a technique for rapid preparation of cross sections for TEM analysis.The specific area to be cross sectioned on the sample is identified by marking it with a laser or Focused Ion Beam (FIB) tool. The sample is then cut down to a 3 x 6 mm rectangle with the area of interest in the center. This rectangle is mounted using wax onto a Tripod polisher with the area of interest protruding over the edge of the polisher.

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

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.

Sample Preparation and Preservation for TEM Analysis of Copper Interconnect Integrated Circuit

2004 ◽  
Author(s):  
Qiang Gao ◽  
Mark Zhang ◽  
Ming Li ◽  
Chorng Niou ◽  
W.T. Kary Chien
Keyword(s):  
Integrated Circuit ◽  
Thermal Exposure ◽  
Ambient Atmosphere ◽  
Ion Milling ◽  
Tem Analysis ◽  
Single Beam ◽  
Copper Interconnect ◽  
Beam Modulation ◽  
Area Of Interest ◽  
Transmission Electron

Abstract This paper examines copper-interconnect integrated circuit transmission electron microscope (TEM) sample contamination. It investigates the deterioration of the sample during ion milling and storage and introduces prevention techniques. The paper discusses copper grain agglomeration issues barrier/seed step coverage checking. The high temperature needed for epoxy solidifying was found to be harmful to sidewall coverage checking of seed. Single beam modulation using a glass dummy can efficiently prevent contamination of the area of interest in a TEM sample during ion milling. Adoption of special low-temperature cure epoxy resin can greatly reduce thermal exposure of the sample and prevent severe agglomeration of copper seed on via sidewall. TEM samples containing copper will deteriorate when stored in ordinary driers and sulphur contamination was found at the deteriorated point on the sample. Isolation of the sample from the ambient atmosphere has been verified to be very effective in protecting the TEM sample from deterioration.

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.

Tem Specimen Preparation by Mechanical Microthinning

1987 ◽  
Vol 115 ◽  
Author(s):  
H. K. Plummer ◽  
S. Shinozaki
Keyword(s):  
Soft Materials ◽  
Diamond Powder ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Thin Specimen ◽  
Basic Premise ◽  
Mechanical Abrasion ◽  
Hard Materials ◽  
Transmission Electron ◽  
Lathe Tool

ABSTRACTMechanical abrasion has been used by the authors to prepare a variety of materials, mainly ceramics, which have been thinned to electron transparency. The basic premise of this technique is the rotation of a spherically shaped wood tool at right angles to a rotating 3mm specimen disk (∼100 μm thick). A slurry of 1/2 μm diamond powder in a glycerin vehicle thins the specimen and carries away the abraded matter. In addition to the wood tool other materials such as brass, teflon and polyethylene have been tried without success. Abrasion “marks” left on the thin specimen surface can be ignored in some situations or removed by a touch up ion milling at 3 keV for ∼1/2 hr. Recently, attempts to thin N+ implanted Al from the un-implanted side using a wood tool were found to be extremely time consuming, i.e. 60 hr or more. It was found that a spherical stainless steel tool produced a suitably thin transmission electron microscopy (TEM) specimen using glycerin as the vehicle and no diamond powder. Depending upon the pressure applied to the tool these specimens could be thinned in as little as 3 hr. The turning marks left by the lathe tool proved to be sufficient to thin the soft aluminum. From this result It appears that soft tools will thin hard materials and hard tools can be used to thin soft materials efficiently. A number of other specimens recently prepared using mechanical microthinning will also be presented.

Focused Ion Beam Study of Ni5Al Single Splat Microstructure

2006 ◽  
Vol 983 ◽  
Author(s):  
Yuhong Wu ◽  
Meng Qu ◽  
Lucille A Giannuzzi ◽  
Sanjay Sampath ◽  
Andrew Gouldstone
Keyword(s):  
Cross Sections ◽  
Focused Ion Beam ◽  
Surface Engineering ◽  
Ion Beam ◽  
Deposition Process ◽  
Rapid Quenching ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Columnar Grains ◽  
Lift Off

AbstractThermally sprayed (TS) coatings are widely used for surface engineering across a range of industries, including aerospace, infrastructure and biomedical. TS materials are formed via the successive impingement, rapid quenching and build-up of molten powder particles on a substrate. The impacted ‘splats’ are thus the fundamental microstructural constituents of the coatings, and their intrinsic properties, as well as intersplat bonding and morphology, dictate coating behavior. Beyond the obvious practical considerations, from a scientific standpoint, splats represent a fascinating template for study, due to the highly non-equilibrium processing conditions (rapid deceleration from sub-sonic velocities, million-degree/sec cooling rates). In the literature, many studies of isolated splats on substrates have been carried out, but these have focused on overall morphology (disc-shape vs fragmented). Direct observations of microstructure, in particular cross-section, are limited in the specimen preparation stage due to splat size (tens of microns in diameter, 1-2 microns in thickness). However, Focused Ion Beam (FIB) techniques have allowed this problem to be addressed in a robust manner; in this paper we will discuss such approaches to observe Ni5Al splats on stainless steel substrates. Cross-sections through the splat and the substrate were created by recourse to ion milling and the ion beam itself provided good channeling contrast for grain imaging. The typical splat microstructure with sub-micron Ni(Al) columnar grains, a chill zone at the bottom and a lift off area is observed in high detail. In addition, an amorphous aluminum oxide top layer of 100-200 nm is partially present on top of the Ni(Al) columnar grains. At the splat/substrate interface, defects such as micro- and nano-scale pores were characterized for the first time and will be discussed. These observations provide insights into splat and interface formation during the deposition process and may drastically improve our current understanding of Ni5Al splat properties.

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