Example - Diamond coatings

Analysis of a DLC coating follows; a different coating, SampleA, is analyzed here.  Return to Texas Diamond analysis.

      Over 100 commercial sources produce various types of DLC
  This is an analysis of a sample from one of them deposited upon 304 stainless steel.

SampleB

  SampleB

Notable is that the debris from deposition of the coating not yet impacted into DLC could be burnished away with light pressure. A play of interference colors appeared on the cleaned surface. A section was cut from the sample for analysis.

The first essential to determine is the thickness of the DLC

 

   

 

 


  A bore hole can be "dug" with ions and the elements streaming back out of the hole can be identified and recorded for each depth into the coating as the hole is dug. The concentration  of one element, hydrogen in this case, can be calibrated in terms of atoms/ cm3 at the different depths into the coating of DLC. 

 

The DLC coating is seen to be 1.0 mm thick.

 

Secondary Ion Mass Spectroscopy (SIMS) Analysis

 

If the sample coating were pure diamond with density of 3.5 g/ cm3 there would be 17.6 (x1022 ) carbon atoms/ cm3 . The amount of hydrogen shown by the calibrated part of the SIMS measurement would be a fraction of 2.2/17.6 or 12.5%. However, the sample is not pure diamond with a density of 3.5 g/ cm3 . While the amount of hydrogen is known absolutely the fraction that represents depends upon the actual density of the DLC.  
The next concern is for the fractional abundance of hydrogen in the DLC.

 

   


From the measured value of H atom density the H atom fraction can be determined from formulas if the mass density of the coating is separately measured.



The issue is that the mass density tells how much carbon is in the coating with the measured amount of H. Carbon is heavier; the more the carbon, the greater the mass density.
 
 

Possible fractions of hydrogen for different possible densities

PossibleHfractions

For different possible values of coating (mass) density, the colored zones show the ranges for possible fractions of hydrogen where the zones cross the vertical line marking the measured value of H atom density.
 An independent measurement of mass density can be made with Laser-excited Surface Acoustic Waves (SAW)
 

Accurate measurment of the mass density of the film "fixes" the fractional content of hydrogen diluent in the DLC.   

            Density of the coating on the same sample was measured by technical experts at the Fraunhofer-IWS Institute in Dresden by laser-acoustics excitation of surface acoustic waves (SAW). It is the technique best suited for thicker coatings where there might be surface layers of unrepresentative residue from the deposition process. Using the value determined from the SIMS measurement of coating thickness, a density of 2.25 g cm-3 was reported to us. The corresponding value of hydrogen content is:

 

                        Fractional hydrogen content = 16.6 %

 To completely locate the type of DLC the fraction of sp3 must be discovered.  Direct measurement is difficult.

 
The same SAW measurements give the Young's Modulus of Elasticity (YME) of the film.


Standards relate the value of YME to the sp3 %.


For SampleB YME was found to be 210 in metric units of GPa.
  AcceptedStandard
Figure reproduced from Fig. 5b in Shi Xu, et al., Phil. Mag. 76, 351 (1997). Results for Sample B are shown.
Having the fractional contents of hydrogen diluent and fraction of the conversion of graphite to diamond give the precise type of DLC
 

 

The type of DLC is definitively located.   TypeDLC

This type of DLC is good and has useful functionality, but it could be made much stronger if the amounts of diluents of hydrogen and of unconverted carbon were reduced.