A Freeze Shadow Technique for the Preparation of Soft Paint Latexes for Electron Microscopy

Author(s):  
Earl R. Walter ◽  
Glen H. Bryant

With the development of soft, film forming latexes for use in paints and other coatings applications, it became desirable to develop new methods of sample preparation for latex particle size distribution studies with the electron microscope. Conventional latex sample preparation techniques were inadequate due to the pronounced tendency of these new soft latex particles to distort, flatten and fuse on the substrate when they dried. In order to avoid these complications and obtain electron micrographs of undistorted latex particles of soft resins, a freeze-dry, cold shadowing technique was developed. The method has now been used in our laboratory on a routine basis for several years.The cold shadowing is done in a specially constructed vacuum system, having a conventional mechanical fore pump and oil diffusion pump supplying vacuum. The system incorporates bellows type high vacuum valves to permit a prepump cycle and opening of the shadowing chamber without shutting down the oil diffusion pump. A baffeled sorption trap isolates the shadowing chamber from the pumps.

Author(s):  
S. Basu ◽  
D. F. Parsons

We are approaching the invasiveness of cancer cells from the studies of their wet surface morphology which should distinguish them from their normal counterparts. In this report attempts have been made to provide physical basis and background work to a wet replication method with a differentially pumped hydration chamber (Fig. 1) (1,2), to apply this knowledge for obtaining replica of some specimens of known features (e.g. polystyrene latex) and finally to realize more specific problems and to improvize new methods and instrumentation for their rectification. In principle, the evaporant molecules penetrate through a pair of apertures (250, 350μ), through water vapors and is, then, deposited on the specimen. An intermediate chamber between the apertures is pumped independently of the high vacuum system. The size of the apertures is sufficiently small so that full saturated water vapor pressure is maintained near the specimen.


Author(s):  
N. Yoshimura ◽  
K. Shirota ◽  
T. Etoh

One of the most important requirements for a high-performance EM, especially an analytical EM using a fine beam probe, is to prevent specimen contamination by providing a clean high vacuum in the vicinity of the specimen. However, in almost all commercial EMs, the pressure in the vicinity of the specimen under observation is usually more than ten times higher than the pressure measured at the punping line. The EM column inevitably requires the use of greased Viton O-rings for fine movement, and specimens and films need to be exchanged frequently and several attachments may also be exchanged. For these reasons, a high speed pumping system, as well as a clean vacuum system, is now required. A newly developed electron microscope, the JEM-100CX features clean high vacuum in the vicinity of the specimen, realized by the use of a CASCADE type diffusion pump system which has been essentially improved over its predeces- sorD employed on the JEM-100C.


Shinku ◽  
1962 ◽  
Vol 5 (7) ◽  
pp. 279-285
Author(s):  
Yukio ISHIBE ◽  
Hideo YAMADA

Author(s):  
W. C. Bigelow ◽  
F. B. Drogosz ◽  
S. Nitschke

High vacuum systems with oil diffusion pumps usually have a pressure switch to protect against Insufficient cooling water; however, If left unattended for long periods of time, failure of the mechanical fore pump can occur with equally serious results. The device shown schematically in Fig. 1 has been found to give effective protection against both these failures, yet it is inexpensive and relatively simple to build and operate.With this system, pressure in the fore pump line is measured by thermocouple vacuum gage TVG (CVC G.TC-004) whose output is monitored by meter relay MRy (Weston 1092 Sensitrol) which is set to close if the pressure rises above about 0.2 torr. This energizes control relay CRy (Potter & Brumfield KA5Y 120VAC SPDT) cutting off power to solenoid-operated fore line valve Vf (Cenco 94280-4 Norm. Closed) which closes to prevent further leakage of air into the diffusion pump


Author(s):  
P. B. Basham ◽  
H. L. Tsai

The use of transmission electron microscopy (TEM) to support process development of advanced microelectronic devices is often challenged by a large amount of samples submitted from wafer fabrication areas and specific-spot analysis. Improving the TEM sample preparation techniques for a fast turnaround time is critical in order to provide a timely support for customers and improve the utilization of TEM. For the specific-area sample preparation, a technique which can be easily prepared with the least amount of effort is preferred. For these reasons, we have developed several techniques which have greatly facilitated the TEM sample preparation.For specific-area analysis, the use of a copper grid with a small hole is found to be very useful. With this small-hole grid technique, TEM sample preparation can be proceeded by well-established conventional methods. The sample is first polished to the area of interest, which is then carefully positioned inside the hole. This polished side is placed against the grid by epoxy Fig. 1 is an optical image of a TEM cross-section after dimpling to light transmission.


Author(s):  
Pamela F. Lloyd ◽  
Scott D. Walck

Pulsed laser deposition (PLD) is a novel technique for the deposition of tribological thin films. MoS2 is the archetypical solid lubricant material for aerospace applications. It provides a low coefficient of friction from cryogenic temperatures to about 350°C and can be used in ultra high vacuum environments. The TEM is ideally suited for studying the microstructural and tribo-chemical changes that occur during wear. The normal cross sectional TEM sample preparation method does not work well because the material’s lubricity causes the sandwich to separate. Walck et al. deposited MoS2 through a mesh mask which gave suitable results for as-deposited films, but the discontinuous nature of the film is unsuitable for wear-testing. To investigate wear-tested, room temperature (RT) PLD MoS2 films, the sample preparation technique of Heuer and Howitt was adapted.Two 300 run thick films were deposited on single crystal NaCl substrates. One was wear-tested on a ball-on-disk tribometer using a 30 gm load at 150 rpm for one minute, and subsequently coated with a heavy layer of evaporated gold.


Author(s):  
Ng Sea Chooi ◽  
Chor Theam Hock ◽  
Ma Choo Thye ◽  
Khoo Poh Tshin ◽  
Dan Bockelman

Abstract Trends in the packaging of semiconductors are towards miniaturization and high functionality. The package-on-package(PoP) with increasing demands is beneficial in cost and space saving. The main failure mechanisms associated with PoP technology, including open joints and warpage, have created a lot of challenges for Assembly and Failure Analysis (FA). This paper outlines the sample preparation process steps to overcome the challenges to enable successful failure analysis and optical probing.


Author(s):  
Jason H. Lagar ◽  
Rudolf A. Sia

Abstract Most Wafer Level Chip Scale Package (WLCSP) units returned by customers for failure analysis are mounted on PCB modules with an epoxy underfill coating. The biggest challenge in failure analysis is the sample preparation to remove the WLCSP device from the PCB without inducing any mechanical defect. This includes the removal of the underfill material to enable further electrical verification and fault isolation analysis. This paper discusses the evaluations conducted in establishing the WLCSP demounting process and removal of the epoxy underfill coating. Combinations of different sample preparation techniques and physical failure analysis steps were evaluated. The established process enabled the electrical verification, fault isolation and further destructive analysis of WLCSP customer returns mounted on PCB and with an epoxy underfill coating material. This paper will also showcase some actual full failure analysis of WLCSP customer returns where the established process played a vital role in finding the failure mechanism.


Author(s):  
Hyoung H. Kang ◽  
Michael A. Gribelyuk ◽  
Oliver D. Patterson ◽  
Steven B. Herschbein ◽  
Corey Senowitz

Abstract Cross-sectional style transmission electron microscopy (TEM) sample preparation techniques by DualBeam (SEM/FIB) systems are widely used in both laboratory and manufacturing lines with either in-situ or ex-situ lift out methods. By contrast, however, the plan view TEM sample has only been prepared in the laboratory environment, and only after breaking the wafer. This paper introduces a novel methodology for in-line, plan view TEM sample preparation at the 300mm wafer level that does not require breaking the wafer. It also presents the benefit of the technique on electrically short defects. The methodology of thin lamella TEM sample preparation for plan view work in two different tool configurations is also presented. The detailed procedure of thin lamella sample preparation is also described. In-line, full wafer plan view (S)TEM provides a quick turn around solution for defect analysis in the manufacturing line.


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