Things I have learned from Failed Aerogels

  • Every experiment is exactly that.
  • Research can only account for so much. Most of the important crap is left out of the research papers and online info is worth what you pay for it.
  • Use the proper reagents.
    • Ethyl and TEOS mix better without contaminants.
    • Ammonia, Ammonium Fluoride, H2o, CO2, Ethyl, Isopropyl, Hexane, TEOS, and TMCS are to be handled with respect.  Forget at your own peril.
    • Alcogels take at least a 60F ambient temperature to gel.
    • Water Purity is critical. Don’t drink the distilled water, unless you have a cup.
    • Clay dissolves in Hexane. Natural lasts longer, but every time seal is broken to wash the Monoliths, it needs replacing
    • Plastic, Rubber and Silicone swell when exposed to hexane, and melt in the presence of TMCS
    • Hexane is extremely flammable.
  • Use, or if necessary, improvise or create the proper tools for the task.
    • Alcogels are FRAGILE.
    • Rigid Molds are easier to create Monoliths within, but can be a bitch to remove from whole. Failed attempts have used glass, plastic, metal, ceramics, grout, and clay.
      • The most promising is my new idea to use 1/2 of a mason jar. the first problem i have is cutting the glass. Any suggestions?
    • Flexible molds are easier to remove the monoliths from, but can be a bitch to handle while decanting, as crushing or breaking the Monolith is easy.
      • I have another idea for this one, using a more semi-rigid pre-made muffin pan I ran across. The last time I used one of these, I learned how Silicon reacts to sulfuric acid. Not pretty.
    • The issues we experienced with the old Autoclave were numerous. The most critical, and the one I couldn’t do anything about at the time, was the Oil-Well casing the Autoclave was created from was rough, to the point of cutting my hands multiple times per interaction.  Ethyl would be trapped in the wall, and we would lose the batch every time we used it.
      • Epoxy resin is ethyl soluble
      • Rubberized tool dip is ethyl soluble
      • Wax is Ethyl + CO2 soluble. It also reacts badly to Hexane and TMCS
      • The potential usability of this autoclave depends on how difficult it would be to either grind the interior smooth, or if a ceramic, glass, or powder coating would prove insoluble in carbonated ethyl.
    • Handling.
      • Alcogels are FRAGILE
      • Changing the wash ethyl requires a container that is easy to store, remove, and replace the Monoliths in, or a system for removing and replacing the ethyl in place.
      • Thin and broad tools are best for scooping the Gels.
      • H2o, Ethyl, Isopropyl, Hexane, TEOS, and TMCS have different needs in containers. Respect them.
    • Every component of the process is necessary to the process. Treat your tools correctly, or remake them.
    • Pressure in the Autoclave shall not fall below 600 PSI during the Ethyl to CO2 transfer, and shall remain there for the duration of the boiling.
    • Autoclave boiling is not to take place until the exhaust has NO Ethyl. Trace Ethyl indicates residual Aerogel destroying solvent within the Autoclave.
  • There is more than one way to do any task I have mastered. Other ways may be superior or inferior to my methods.
    • In the three years this project has consumed, patience is the key to everything. Also, setbacks, while expected, are still surprising.
    • High Pressure CO2 escaping onto a vertical surface that overhangs H2O results in CO2 sublimation into a solid, that falls into the H2O, re-sublimates into Gas, and boils the water vigorously. This understatement brought to you by the letters C, H, O & the Number 2.
    • There is more, but I have already exceeded 600 words, so L8r.
  • Suggestions and comments are welcome.

About Rey d`Tutto

Hey, Y'all, I've been rather ill recently, and that has kinda deprived me of the ability to post regularly. I may or may not ever post regularly again. Thank you for playing.
This entry was posted in Aerogel, For Science!, random thoughts.. Bookmark the permalink.

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