Cold-Formed Ceramics

It was twenty years ago that I was witness to a chemical change during an experiment with ceramics. I was involved in the process as a tech. I was taught how to make liquid ceramic ‘resin’ with no organic materials, that consists of an acid and a base mixed together. Once the ‘resin’ was made, and cool, it was stored in large glass containers. Later the resin was used to make samples. All of the samples that were made, when tested for mechanical properties, did not meet the specs of the customer. They were trying to make light weight architectural panels, that needed a minimum bend strength needed to be able to handle a 2′ x 4′ panel made from the materials.  During the mixing of the last composite mixture, I had outside help in handing me asked for ingredients.  As I added the first one handed to me, I had started to add it in to the liquid resin before I had noticed that it was marked differently than the one for which I had asked.  It was the same colored and type of dispensing container in either case so it was an easy mistake.  So I continued to add the remainder of the contents, and watched closely the mixing as it took place.  Previously, the mixing containers had been small, and it wasn’t easy to see what if any reactions were taking place.  Now, this time during the making of a larger panel, the mixing surface was easier to view, and so was the reaction.  Nothing had changed during the addition of what then was thought to be the proprietary blend of materials.  So I got a container of the other dry ingredient and started to add it into the mix, continuing to watch the mixing surface closely as I added in the material.  During the addition of the second material, and not a lot of it, the mixing surface changed in appearance.  I had seen the error of their ways, and did make an attempt to indicate a need for a formula change, however I was told to continue with the planned formula, so I did. 
Fast forward to 2006.  I get re-inspired with the concept of cold-formed ceramics / ceramic composites.  I do patent research, material research via the Internet to see what is current, I make calls to individuals and organizations, about cold-formed ceramic composites, etc., trying to do diligence before I put my money down to buy similar materials and try it for myself.  I find that what I had wanted to accomplish, hadn’t been done so already, nor had the process of formulation of the resin, nor composites made from the liquid ceramic resin, been patented.  So I decided to look for grant money.  Please note here that the first attempt at this was through an outside ‘help-you-do-it’ agency.  They took money up front and did little or nothing for it.  Definitely not the way to go.  I then found, the main portal to any grant program the US government has put into action.  I went through the motions, filled out the forms, then filed to early and had to withdraw my submission.  After rereading what I had written, based upon for what I had thought that they were looking, I am glad I had withdrawn it.  I had hurried the effort and the results, in the much later rereading, were not pretty.  Then I rewrote parts and sent emails to the respective reviewers to see if my concepts had any merit in their eyes.  I got the impression that they were somewhat prejudiced against me for lack of an academic support institution, no scholarship, and in no position to be asking for a grant for research into cold-formed ceramic composites.  I felt challenged.
So I made the decision to do it on my own.  During 2008, I took what extra money I had left to my name, and bought the materials and equipment that I could, and then borrowed and asked for the rest.  I needed a laboratory and some acids, for which I didn’t have the money, but managed to get them anyway. 
Once I had everything I thought I needed in place, I went to work.  I didn’t have the same oven, original materials, mixer and cook pot, but close equivalents.  I measured and weighed the ingredients that make up the liquid ceramic resin, based upon what I had remembered from twenty years past, and mixed and cooked them together.  Something was wrong, as the liquid was too thick, and not clearing up as it boiled.  Then I went over again, in my mind’s eye, what I had done physically, to make the liquid resin, then and now, and realized that I had used too much of the dry ingredient this time.  OOPS.
So I tried to recover from the material that I had just made, a thick gooey sticky sludge, and tried to ‘thin’ it out with the liquid ingredient, with some success, but it wasn’t the right mixture.  I hemmed and hawed for a little while before making a second go at making the liquid ceramic resin.  I was much more careful and used the correctly remembered amounts, and followed the mixing schedule closer.  I still had managed to leaveout one of the liquid ingredients, but remembered it and added it last, knowing it would still do its work.  I had transfered the final mix into a ‘stainless steel’ cookpot, to keep until I came back the next day.  The liquid ceramic resin is somewhat acidic, however I though the cookpot was actually stainless steel, and would be OK for the time that I would be away.  Time and the tides, and nine days go by before I get back to it.
When I did get back to it, the first thing that came in to my mind was the line Scotty said in a Star Trek episode: "I don’t know what it is, but it’s Green…" and then the following rhyme:
Pease porridge hot, pease porridge cold, Pease porridge in the pot, nine days old;
Some like it hot, some like it cold, Some like it in the pot, nine days old.
It was a nice transparent emerald green color.  The cookpot hadn’t been made from stainless steel as advertised.  It had been made from steel plated with Nickel, and Murphy strikes again.  So I bottled each into separate empty plastic gallon jugs and closed them up tightly with caps and put them into a refrigerator for keeping as the process of mixing the composite involved using cold liquid ceramic resin.  Two different batches, two different results, one clear, one green, neither the same as the very first batch I made for the professor.
My first attempt was with the clear recovery batch.  I cooled and mixed and cooled some more, all the while looking at the mixing surface.  I tasted, added, cooled and mixed more of my dry reactant into the liquid.  It never got cold enough to get lumpy like I had seen twenty years earlier, which had changed to smooth, and then back to lumpy, which I had witnessed twenty years prior.  It just stayed smooth.  So I checking for the right point, by taste.  I had gotten it to a certain point, but it had remained smooth and I was running out of cold, and was getting blistered hands and frustrated, and was running out time for that day so I stopped the mixing.  I had waited five minutes that it had taken the samples twenty years ago to solidify, yet nothing seemed to be happening.  Time had run out for the day.  So I left the cold mixture in the bucket, looking like milk, with bits of plastic that the mixer blades had carved off from the plastic bucket that I had used to mix the composite, to solidify. 
Time and the tides, and several days go by before I get back to it.  Interestig, but not what I was after.  I guessed that I needed a filler like I had surmized that one of the original ingredients actually had been, insted of it being the secret reactant they had led on it to be.
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