Sonication & Hydrogenation of Nano Nickel (video)

Sonication & Hydrogenation of Nano Nickel (video)

 

LENR Fuel Preparation 

During this fuel preparation experiment we subjected 20 micron nickel powder to 12 hours of ultrasound bombardment at low temperature. During the course of the sonication, the flask containing the nickel was alternately vacuumed and flushed with pure hydrogen.  The purpose of this experiment was to remove surface oxides from the nickel and adsorb hydrogen into the metal matrix.  The nickel also contained two additives, both of which are used as ‘spillover’ catalysts to promote hydrogen absorption.

The complete recipe was:

  • 5 grams 20 micron nickel
  • 0,5 grams 100 micron copper
  • 0.5 grams acetylene derived micron-size carbon black
  • Heptane 

At the conclusion of the sonication treatment, the Heptane carrier fluid was replaced by Hexane, which is more volatile at room temperature. The hexane was then evaporated by bubbling pure Hydrogen through it until it evaporated entirely. The finished fuel is now ready for testing in our New Differential Calorimetric Reactor.

 

  • Alan Smith

    Hi Again Simon.

    I noticed your comment about buying quicklime. Not too difficult in France- I replastered the inside of my house in France with lime plaster. purchased from the lime-burner just up the road. Little lime kilns are dotted all over central France- which is limestone country- you may have some near you..

  • Alan Smith

    Current thinking –

    I have some very nice Ni Foil strips. Pondering co-deposition of Hydrogen and More Ni (from another Ni electrode) via electrolysis in de-gassed distilled water.

    What do you rhink?

    • Simon Derricutt

      Alan – sorry for delay (Happy New Year!). Some Nickel-plating solutions are not used commercially because the Nickel deposited is brittle and can flake off. This is because there is too much Hydrogen co-deposited and the internal pressure/stress is too high. I found a list of them a while back, and if wanted I’ll see if I can find it again. Still, you actually want that co-deposition, so using the “bad” plating solutions such as pure Nickel Sulphate is probably what you want. May be useful using a somewhat higher voltage than normal to get more Hydrogen evolved, though making the voltage too high gives a powdery dark grey deposit that wipes off (but that deposit may also be what you want if it’s dried out). Experimentation needed, but it may be a way to get very fine Ni powder that is pre-loaded – just the problem with some hydroxide possible as a surface layer, but hydrogenation at >400°C will fix that.

      Maybe worth noting that you can start with the plating solution as just the acid, and build up the Ni in solution by plating current. Pure degassed distilled water won’t conduct that well, so may need high voltage (20-30V) anyway and produce nanoparticles of Ni that are hydrogen-rich and have a coating of Ni(OH)2 on them. The deposits would be blown off the cathode by the evolved Hydrogen, so never get big. There’s maybe a possibility of using LiOH as the electrolyte, and putting the voltage high-enough to get Li co-deposited as well, but I haven’t worked out the voltage needed for that – the idea is that though normally any deposited Li would immediately go back into solution, if it’s got a few atoms of Ni protecting it it may get incorporated in the nanoparticles of Ni that are produced. Experimentation needed…. Here I’m thinking of doing all the things that electroplaters tell us give a bad result, since you actually want those “faults” here. Using a weak acid (such as vinegar or Boric acid) gives a better deposit, and using a strong acid (such as Sulphuric or Hydrochloric) gives more Hydrogen in the plate.

      I got 4N Nickel foil from China pretty cheaply on eBay, and you can get 3N Nickel wire from http://www.wireandstuff.co.uk/ (Crazy Wire – they stock vaping stuff). They also stock Kanthal and other stuff you may find useful.

      I have a few bags of chalk left over from the build here. Mostly CaCO3 by now, but with firing I can get quicklime from it. Here in the SW I haven’t seen local lime-burners, but it’s easy to make. I can also buy pure CaCO3 from the winemaking suppliers – it’s used for reducing acidity of wines. Higher-quality than the building supplies.

  • Alan Smith

    Hi Simon. Good to hear from you.

    You suggestion (below) seems like a really good idea. I currently use Hydrogen alternating with Vacuum at 300C, 2 hours of each four times each- finishing up with Hydrogen. The Vacuum pulls off the water vapour pretty well.
    But I do have my doubts about the effectiveness of this method – after all, if it was this easy why did they develop the Mond process?

    I had a chat with Roland Pettersen recently- he is also studying this problem and finding it difficult to come up with a good system. As a Forensic Analytical Chemist with access to some amazing hardware and decades of working to 7 decimal places at times he is better equpped than most of us to find a way.

    I have a concern about using Alkanes in general – Butane partially oxidised at best may well produce CO, which in turn could (perhaps) produce Carbonyl Nickel which is pretty deadly stuff. I must confess I have not read up the reaction dynamics for Carbonyl Nickel to see if that really could happen, but it would not be a desirable outcome.

    C’est la vie pseudo-scientific!

    • Simon Derricutt

      Alan – one of the things I was thinking about was that the Hydrogen you’re using won’t be totally dry, so may give hydroxides that won’t give you a clean surface. It seem unlikely that vacuum would change the hydroxides.

      Exposing the clean Nickel to air gives an almost-immediate oxide coating that is temperature-dependent. At room temperature seems to be 3 atomic layers, but at 300°C the depth just keeps increasing, so handling the powder afterwards would be pretty critical if you want it to stay oxide-free.

      For Carbonyl Nickel, see http://blogs.sciencemag.org/pipeline/archives/2004/03/28/thing_i_wont_work_with_2_nickel_carbonyl which is a little worrying. High vapour pressure and boils off easily, so apart from the poisoning danger you could separate it from the powdered clean Nickel by heating above 44°C under Argon. Something I hadn’t considered, though, so thanks for that. I didn’t see any liquids formed when I tested it out, but then I also set light to the stream of Butane coming out and that would have destroyed it too (leaving fine NiO in the gas, maybe). The Mond process uses the volatility of Carbonyl Nickel to purify it from other metals, but starting with pure (ish) Nickel it’s more of a nuisance. To start the process they simply use Hydrogen, though, to produce Nickel (with impurities) from the ore. Looks like Ni combines with CO at 50-60°C, so I probably made some.

      Easy ways of getting Hydrogen seem to all produce moist Hydrogen. Burns just as well but maybe not ideal for what you want to use it for. It may be possible to crack Ammonia to get a mixture of H2 with N2 that would be better, but then I’ve only seen Ammonia for sale in solution – back to square 1. The only reasonable way I can think of to get dry Hydrogen is to pass it through quicklime, which of course can be easily made. Seems I can only buy slaked lime here, but heating it up to orange heat quickens it. I think that having dry Hydrogen may help in getting the Nickel squeaky-clean on the surface.

      Sorry for delay in answering. Lots happening at the moment and the system didn’t alert me to a reply.

  • Simon Derricutt

    Just for interest, Alan, you can turn the surface oxides on Nickel back into metal by using Butane (or of course Hydrogen, though I haven’t tried that yet) at a bit over 400°C and at atmospheric pressure. This would probably be easier than sonic treatments to remove the oxide, as well as being a lot faster. At 410°C, the reaction happens in a few seconds. Butane has the advantage that it’s a bit safer and will be completely dry, thus leaving the Nickel surface as just metal with no hydroxides. It’s also quite a bit cheaper than lab-quality Hexane or Heptane. No other catalysts required, so unless you need the Copper and Carbon in there you’ll have just clean Nickel.

    By using alternate butane and air/Oxygen flowing through at 410°C or so (with something like Argon sweeping out the last gas used between them), you would probably produce a very disturbed surface on the Nickel particles with a higher effective surface area. May be helpful. I don’t however have an SEM to check the results, and this is just a logical inference that needs testing.

  • Alan Smith

    Thank you Paul. If you are anywhere near London UK, btw, you are very welcome to visit the lab sometime.

  • Paul Maher

    I can’t begin to tll you how happy I am to see a venture such as yours. I will do all I can to spread the word.
    @pmaher_art