Microporous Magnesium Fluoride Nanomembrane Becomes Stronger as the Film Thickness Increases

The title really says it all. I have been attempting to make a better cell culture substrate with the Magnesium Fluoride Films. Previous posts have shown the overall structure of the film, and now I am trying to quantify the strength with a burst pressure measurement. In order to make a direct comparison, I needed to utilize the same window/pore geometry, and only vary the film’s thickness. I used wafer PFI02 (120 nm silicon nitride, 0.4 micropores, 1:1 pitch, five 0.1×3 mm slots).

 

Fully etched MgF2. Some infilling is apparent as the pyramidal rim structures exist below the bottom plane of the holes.
Fully etched MgF2. Some infilling is apparent as the pyramidal rim structures exist below the bottom plane of the holes.

 

Here, I’m comparing a 50 nm thin film process (actually came out about 45 nm) to a 200 nm thin film process.

50 nm Process

  • Evaporate MgF2 onto 0.4 micron pore, 12o nm thick Si3N4 substrates
    • 250 C
    • 2-3 Angstroms/sec
    • Platen Rotation
  • Etch with RIE, backside to remove Si3N4
    • CHF3:O2 (90%:10%)
    • 100 W Net Power
    • 100 mTorr etch pressure
    • Etch for 120 sec

200 nm Process

  • Evaporate MgF2 onto 0.4 micron pore, 12o nm thick Si3N4 substrates
    • 150 C
      • The different temperature is to mitigate the larger overall amount of film stress generated by the thicker film
    • 2-3 Angstroms/sec
    • Platen Rotation
  • Etch with RIE, backside to remove Si3N4
    • CHF3:O2 (90%:10%)
    • 100 W Net Power
    • 100 mTorr etch pressure
    • Etch for 120 sec

The burst pressures then are (slowly ramping up with N2 gas, ~1 PSI every 5 sec):

50 nm Process 200 nm Process
1.12 6.98
0.73 6.92
0.82 9.43
Average [PSI] 0.89 7.78
Std. Dev [PSI] 0.20 1.43

 

Increasing the thickness 4-5x improved the burst pressure strength by ~8x. There are yield improvements too; many of the broken chips for the 200 nm process had more windows than that of the 50 nm process. Here I only got 3 chips for each treatment, but I processed 9 chips for the 200 nm process and about 20 chips for the 50 nm process. This data suggests that I am on the right path to make more robust cell culture membranes.

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2 Comments

  1. Greg: Can you directly pattern the micropores into MgF2 with photolithography and RIE?

    BTW – We use Si-rich, non-stoichiometric SiN (so not Si3N4).

    1. Thanks for the reminder that the film is non-stoichiometric – SiN, not Si3N4. Will update post to reflect this fact.

      You could pattern the micropores, but I have yet to find an effective RIE that attacks the MgF2. I’m sure it exists somewhere, but my own experiments show very little etching of the film with CHF3-based chemistry. Maybe we could wear it away with an Ar plasma over a long time? It will all come down to the selectivity – what sort of photoresist thicknesses are we working with nowadays (1-3 um)?

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