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.

TEM Studies of Low Energy Argon and Iodine Ion Milling Phenomena in Compound Semiconductors

1985 ◽  
Vol 62 ◽  
Author(s):  
A. G. Cullis ◽  
N. G. Chew ◽  
J. L. Hutchison
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Compound Semiconductors ◽  
Low Energy ◽  
Specimen Preparation ◽  
Dislocation Loops ◽  
Ion Milling ◽  
Thin Specimen ◽  
Transmission Electron ◽  
Dense Arrays

ABSTRACTThe nature of disorder produced by low energy Ar+ and I+ ions (and atoms) in the III–V compound semiconductors InP and InSb, and in the II–VI semiconductors CdTe, ZnS and ZnSe has been studied in detail by conventional and high resolution transmission electron microscopy. It is demonstrated that for Ar+ ion bombardment the disorder in the III–V compounds comprises segregated indium islands which accumulate on the machined surfaces, while for the II–VI compounds the disorder consists of dense arrays (∼1011 cm−2) of small dislocation loops near to each bombarded surface. When Ar+ ions or Ar atoms are used for thin specimen preparation by milling prior to electron microscopy, the disorder produced gives contrast which seriously obscures images and so complicates their interpretation. This problem concerning the presence of artifactual defects can be greatly reduced or even eliminated by the use of reactive I+ ion milling for the final thinning of specimens.

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.

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.

scholarly journals Mechanical and Compositional Implications of Gallium Ion Milling on Epoxy Resin

Polymers ◽  
2021 ◽  
Vol 13 (16) ◽  
pp. 2640
Author(s):  
Raz Samira ◽  
Atzmon Vakahi ◽  
Rami Eliasy ◽  
Dov Sherman ◽  
Noa Lachman
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Soft Materials ◽  
Morphological Data ◽  
Ion Milling ◽  
Element Analysis ◽  
Transmission Electron ◽  
Direct Measurements ◽  
Quantitative Results

Focused Ion Beam (FIB) is one of the most common methods for nanodevice fabrication. However, its implications on mechanical properties of polymers have only been speculated. In the current study, we demonstrated flexural bending of FIB-milled epoxy nanobeam, examined in situ under a transmission electron microscope (TEM). Controllable displacement was applied, while real-time TEM videos were gathered to produce morphological data. EDS and EELS were used to characterize the compositions of the resultant structure, and a computational model was used, together with the quantitative results of the in situ bending, to mechanically characterize the effect of Ga+ ions irradiation. The damaged layer was measured at 30 nm, with high content of gallium (40%). Examination of the fracture revealed crack propagation within the elastic region and rapid crack growth up to fracture, attesting to enhanced brittleness. Importantly, the nanoscale epoxy exhibited a robust increase in flexural strength, associated with chemical tempering and ion-induced peening effects, stiffening the outer surface. Young’s modulus of the stiffened layer was calculated via the finite element analysis (FEA) simulation, according to the measurement of 30 nm thickness in the STEM and resulted in a modulus range of 30–100 GPa. The current findings, now established in direct measurements, pave the way to improved applications of polymers in nanoscale devices to include soft materials, such as polymer-based composites and biological samples.

Mechanical Microthinning For TEM Specimen Preparation

1985 ◽  
Vol 43 ◽  
pp. 178-179
Author(s):  
H. K. Plummer ◽  
S.S. Shinozaki
Keyword(s):  
Mechanical Damage ◽  
Diamond Powder ◽  
Specimen Preparation ◽  
Mechanical Abrasion ◽  
Grooved Surface ◽  
Short Time

In two previous papers the technique of TEM specimen preparation using only the mechanical abrasion of boxwood tool and a dispersion of diamond powder in glycerin to thin the specimen has been presented with a number of examples shown. It is the intent of this paper to discuss additional details of the technique and to exihibit further examples where mechanical microthinning has been advantageous in obtaining useful information even in the presence of obvious mechanical damage.A.C.Faberge reported the use of teflon as a fine polishing lap. The grooved surface similar to that shown in Fig.1a, polished exceptionally well but after a short time in use the pocked surface, as seen in Fig.1b, was formed. in Fig.1a, polished exceptionally well but after a short time in use the pocked surface, as seen in Fig.1b, was formed.

Ultra-high-vacuum, high-resolution Transmission Electron Microscopy at 400 kV

1986 ◽  
Vol 44 ◽  
pp. 606-609
Author(s):  
F. A. Ponce ◽  
S. Suzuki ◽  
H. Kobayashi ◽  
Y. Ishibashi ◽  
Y. Ishida ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
High Vacuum ◽  
Milling Process ◽  
Electron Bombardment ◽  
Ultra High Vacuum ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
Preparation Stage ◽  
Resolution Imaging

Electron microscopy in an ultra high vacuum (UHV) environment is a very desirable capability for the study of surfaces and for near-atomic-resolution imaging. The existence of amorphous layers on the surface of the sample generally prevents the direct observation of the free surface structure and limits the degree of resolution in the transmission electron microscope (TEM). In conventional TEM, these amorphous layers are often of organic nature originating from the electron bombardment of hydrocarbons in the vicinity of the sample. They can in part also be contaminants which develop during the specimen preparation and transport stages. In the specimen preparation stage, contamination can occur due to backsputtering during the ion milling process. In addition, oxide layers develop from contact to air during transport to the TEM. In order to avoid these amorphous overlayers it is necessary: i) to improve the vacuum of the instrument, thus the need for ultra high vacuum; and ii) to be able to clean the sample and transfer it to the column of the instrument without breaking the vacuum around the sample.

A temperature-jump technique for time-resolved cryo-transmission Electron Microscopy

1989 ◽  
Vol 47 ◽  
pp. 742-743
Author(s):  
H. Chestnut ◽  
D. P. Siegel ◽  
J. L. Burns ◽  
Y. Talmon
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Liquid Crystalline ◽  
Temperature Jump ◽  
Specimen Preparation ◽  
Thin Specimen ◽  
Time Resolved ◽  
Sequence Of Events ◽  
Transmission Electron ◽  
Focused Beam

Transmission electron microscopy of rapidly-frozen, hydrated specimens (cryo-TEM) is a powerful way of examining labile microstructures. This technique avoids some artifacts associated with conventional preparative methods. Use of a controlled environment vitrification system (CEVS) for specimen preparation reduces the risk of unwanted sample changes due to evaporation, and permits the examination of specimens vitrified from a defined temperature. Studies of dynamic processes with time resolution on the order of seconds, in which the process was initiated by changes in sample pH, have been conducted. We now report the development of an optical method for increasing specimen temperature immediately before vitrification. Using our method, processes that are regulated by temperature can be initiated in less than 500 msec on the specimen grid. The ensuing events can then be captured by plunge-freezing within an additional 200 msec.Dimyristoylphosphatidylcholine (DMPC) liposomes, produced by extrusion, were used as test specimens. DMPC undergoes a gel/liquid crystalline transition at 24°C, inducing a change in liposome morphology from polyhedral to spherical. Five-μl aliquots of DMPC dispersions were placed on holey-carbon-filmed copper grids mounted in the CEVS environmental chamber, and maintained at 6-8°C and 80% relative humidity. Immediately before the temperature jump most of the sample was blotted away with filter paper, leaving a thin specimen film on the grid. Upon pressing the trigger, an electronic control circuit generated this timed sequence of events. First, a solenoid-activated shutter was opened to heat the specimen by exposing it for a variable time to the focused beam of a 75W Xenon arc lamp. Simultaneously, a solenoid-activated cryogen shutter in the bottom of the CEVS was opened. Next, the lamp shutter was closed after the desired heating interval. Finally, a solenoid-activated cable release was used to trigger a spring-loaded plunger in the CEVS, propelling the sample into a reservoir of liquid ethane. Vitrified samples were subsequently transferred to a Zeiss EM902 TEM, operated in zero-loss brightfield mode, for examination at −163°C.

Preparation of Electropolished Transverse Sections of Thin Aluminum Sheet for Transmission Electron Microscopy

1987 ◽  
Vol 115 ◽  
Author(s):  
Steve Smith
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Transverse Section ◽  
Aluminum Sheet ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
Thin Aluminum ◽  
Time Required

ABSTRACTThe preparation of transverse section TEM foils from thin (0.2 mm to 1.5 mm) aluminum sheet would usually be accomplished by a combination of dimpling and ion milling. Both of these techniques are time consuming. A technique has been developed which allows these transverse section foils to be prepared by electropolishing, which greatly reduces the time required for specimen preparation. This technique also produces far more thin area for examination than a comparable foil which has been dimpled and ion milled, and eliminates artifacts produced by ion milling.

Sign in / Sign up

Export Citation Format

Share Document