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Ten Different Ways to Measure Thickness
Dear Tom,
 
Time for more helpful information from your colleagues at Rocky Mountain Labs.  We would like to share a number of data images with you, that were selected by our staff.  They all involve the measurement of material structures: whether surface coatings, buried structures, or multi-film stacks.  Please let us know if you find this newsletter useful or if there is any topic that you would like us to discuss in a future issue.  Comments can be sent to info@rockymountainlabs.com.
 
Sincerely,
 
Rocky Mountain Labs' Stafftop
Applications
Generic Three-film System
Passivation on Stainless Steel
Color Coded Pedicle Screws
Thin Fluorocarbon Lubricant Coating
Multilayer Antireflective Coating
Infrared Detector Diode
Polished Cross Sections
Drug-eluting Arterial Stent
Organic Coating on Micro-wire
UV Mirror
Aluminum Wire to Gold Film Bond
Fiber/Adhesive Interface
Polyimide Coating on Display Chip


We are often asked to measure the thickness of thin-films, bonds, and other material structures.  Rocky Mountain Labs has a variety of methods for accomplishing this, depending on the situation.  Films from 1 Å to 1 mm (107 dynamic range) can be measured by our methods.






The analysis thicknesses of our various analytical techniques affect the ultimate film thickness that can be measured by that technique.  Field Emission Scanning Electron Microscopy (FESEM) and Atomic Force Microscopy (AFM) can measure the thinnest films.

Generic Three-film System

Auger sputter depth profiling offers a rapid method of characterizing thin film structures.  This example is of a multilayer system employed in the past for a hard disk for data storage.  The structure is:

C/Cr oxide/CoNi/NiP



Passivation on Stainless Steel



The measurement of the chromium oxide film on a properly-passivated stainless steel surface is easily accomplished with Auger Sputter Depth Profiling (AES-SDP).





Color Coded Pedicle Screws

Screws of various lengths are used in back surgery.  These titanium screws are color coded for easy identification of their length in the operating room.  Different colors are achieved by manufacturing different thicknesses of titanium oxide on the surface.






Auger profile of titanium oxide thickness on pedicle (back) screw.
 









Optical photo of an actual titanium oxide coating on titanium.  The color gradient, which correlates to the oxide thickness, was revealed by ion etching the sample at a shallow angle.  The color of a thin film is the result of optical interference between light reflected from the surface and light reflected from the oxide/metal interface.



Thin Fluorocarbon Lubricant Coating


Films in the range of 1-100 Å can be measured by X-ray Photoelectron Spectroscopy (XPS/ESCA).  The technique makes use of the short, finite escape depth of the electrons that are measured.  Electrons cannot escape through more than a ~100 Å thick surface layer.  For layers < 100 Å thick, electrons from the substrate begin to be detected.  The smaller the substrate signal, the thicker the overlayer film.  The thickness of the fluorocarbon film in this example is 3.5 nm.






Multilayer Antireflective Coating


Optical components such as these in our FTIR instrument are designed, e.g., to reflect or transmit a specific wavelength of light; in this case infrared.  The optical response is designed by depositing various sequences of films with a multitude of chemical compositions, on a thick substrate.
 
 



Devices can be reverse engineered to reveal their thin film composition.  Insulating materials such as these are profiled by XPS.

Infrared Detector Diode

This thickness measurement was accomplished by scanning an electron beam across a cross-section of an infrared detector diode and monitoring Auger electron signals for each element of interest. 


Easy, except that the sample was held at typical operating cryogenic temperatures, cleaved in ultra-high vacuum just prior to analysis, and was electrically wired to simultaneously provide the Electron Beam Induced Current (EBIC) to correlate with the compositional data.
 


Polished Cross Sections





Polished cross sections are prepared by mounting samples in epoxy and grinding and polishing them to a mirror-like finish.
 
 









Rocky Mountain Labs has in-house capabilities for preparing cross-sections of a broad range of materials.
 






Drug-eluting Arterial Stent




An estimated $24 billion in stents have been sold in the U.S. over the past fifteen years.









This sample of a stent, which is manufactured with a very soft organic coating on a metal substrate, was prepared as a polished cross section.  The exterior and interior surfaces of the drug-eluting film are highlighted by proprietary RML techniques.







Organic Coating on Micro-wire







The thickness and uniformity of this organic coating on a wire is depicted by SEM observation of a polished cross section.  The interfaces are accentuated by RML proprietary techniques.





UV Mirror




Field Emission Scanning Electron Microscopy (FESEM) is required for observation of very thin layers.  This image is of a polished cross section of a multilayer optical component.  Original magnification equal to 40,000X.






Aluminum Wire to Gold-film Bond



This optical image shows the cross section of an aluminum wire bond to a gold-coated substrate.  The thickness of the gold coating can be measured.  Original magnification 1,000X.
 









EDS mapping of an expanded view of the wire bond depicts thin-film thickness by the elemental image of the metal stack in cross section.







Fiber/Adhesive Interface






RML is experienced in preparing cross-sections by many methods; including this Instant PrepSM of a fabric/adhesive system.









Polyimide Coating on Display Chip

Atomic Force Microscopy (AFM) is used to accurately measure film thicknesses in the
0-5µm range.  We sometimes calibrate our instrument by observing the 4 Å lattice steps in cleaved GaAs.

 



3-D imaging and thickness calculations can characterize films with various surface morphologies.






 







This polyimide coating on a silicon substrate is measured to be 55 nm in thickness.








All data presented in this newsletter are actual data obtained from our instruments and modified with presentation tools.
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About Rocky Mountain Laboratories, Inc.

Rocky Mountain Labs has provided surface and micro-analysis services to the international community since 1983.  We proudly provide analysis to manufacturing, medical device, pharmaceutical, photovoltaic, academic, aerospace, defense, research, and other industries around the world.

Rocky Mountain Laboratories, Inc.
602 Park Point Dr., Suite 101
Golden, CO 80401 USA

800-PRO-LABS (800-776-5227)

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