MFMP: Automated experiment with Ni-LiAlH

  • Could the wetted Li boiling actually cause a "precipitation" of the H- onto the Ni surface?


    After giving a bit more thought to this: boiling can generally remove a large fraction of gases dissolved in liquids. This should occur with metals too, although their behavior with gas solubility is different than liquids like water.


    I've found the graph below which shows the solubility of hydrogen in Al over a wide temperature range at atmospheric pressure. It increases until somewhere below the boiling point, then it markedly drops. Li may behave similarly assuming that some H remains in solution after all the LiH is decomposed, but I don't know if it would precipitate out directly as H-.




  • can

    That curve is an interesting find. Thanks for posting.


    Presently working on prep for the next experiment. Next reactor tube will be epoxied today. Ni is being prepared - powder will be ultrasonically HCL etched and freeze fractured; then mixed with LiAlH4. I am working on code to do the automatic file mirroring - prototype is working. I am contemplating running another calibration while I am working on the fuel.

  • I am preparing the framework for the next experiment. The data will be found in this Google Drive folder: https://drive.google.com/drive…B0NkRqSDhkWDg?usp=sharing


    There is not much there yet, but I have just started a calibration run using the reactor tube that I will soon fill with fuel for the fueled run. It is a useful activity while I am preparing the fuel for the next experiment. As data for the calibration comes out of the automation, I will add it to the Google Drive folder. This will be the same 32 hour calibration script as before and should produce the same calibration data.


    The next experiment should be ready to begin on 5/3 or 5/4. I am experimenting with the fuel preparation now. The plan is to etch the Hunter AH50 Ni powder in 15% concentrated HCl (by mass, about 10°Baume') at 50°C in ultrasound. Then the powder will be rinsed (multiple times) in degassed H2O, drained, and frozen in an attempt to fracture the particles. Following that, the powder will be heated and vacuum dried. It will be mixed with 10% LiAlH4 as the fuel. The protocol will include heating to 1200°C and at some point reducing the pressure to see if Li boiling can be stimulated.

  • Can ---- may I ask you something directly? I follow you and your thoughtful/posts you are very helpful. I find it amazing that you are on point always. If you care to respond do you have an idea (not a theory nor hypothesis) on what to look for? and how to look for it? Just something that you think will be able to break the C barrier. I am sorry if I put you on the spot, but I am hoping you are willing to share what you think. But I always appreciate your posts. And Bob H goes without saying....(cough hero cough cough)

  • I also think (and even Andrea Rossi expressed it), that at the case of LiAlH4 systems the fusion reaction actually runs at the thin surface film of lithium covering the nickel. It would also correspond the Lipinski experiments, where only (semicrystalline) surface layer of molten lithium has been involved. At the case of future deuterium plasma experiments in Me356 style such only an arrangement would have some meaning (you wouldn't want to cover the nickel surface against corona with crust of Li hydrides).

  • Can ---- may I ask you something directly? I follow you and your thoughtful/posts you are very helpful. I find it amazing that you are on point always. If you care to respond do you have an idea (not a theory nor hypothesis) on what to look for? and how to look for it? Just something that you think will be able to break the C barrier. I am sorry if I put you on the spot, but I am hoping you are willing to share what you think. But I always appreciate your posts. And Bob H goes without saying....(cough hero cough cough)


    In short

    For what can reasonably be done with these experiments using the usual powders, either try to repeatedly and continuously "ride" the reversible hydride reactions of LiAlH4/Li (as apparently successfully done during GS5.2 and GS5.3) or have a non-wetted, solid high surface area transition metal environment in an atmosphere of hydrogen and Li vapors and attempt to trigger a reaction by sudden temperature changes/impulses.

    A bit longer

    Recently I've exchanged a couple emails with an Italian gentleman who has notably been involved in various LENR experimentation in the past 28 years or so. To my surprise - or perhaps not so much - it seems that LiAlH4 on its own can show excess energy, but only if the proper triggering protocol is respected (which I haven't read about yet from this person - he takes his time to reply - but I've had a quick overview from another (**)). It seems that the observation of anomalous energy revolves around the reversible hydride reactions of this compound, as I previously suspected.


    According to his recount, one of his associates, who didn't know the full details of the process, at some point tried to replicate the effect in his own laboratory but never managed to due to failure to comply with the triggering protocol, as he found later on.


    Not many details yet but I think it's possible to make some observations here:


    - The MFMP GlowStick 5.2 and 5.3 which had rapid and frequent temperature/pressure variations where the LiH would decompose and release hydrogen might have been on the right track;

    - Apparently without a proper triggering process nothing will happen in either case.

    - Li boiling might end up being a different method for doing what the decomposition of the ionic hydride achieves (or perhaps as I'm thinking it's also a matter of surface coverage).

    - Parkhomov reports of reaching temperatures of 1200-1300°C where excess heat may arise. I'm assuming this is externally measured, which means that internal ones will possibly be above 1350°C => Li evaporating at 1 atm.


    (**) Apparently a successful triggering protocol involves taking the LiAlH4 to 500°C at a rate of 2°C/min or less, then switching off the heating allowing the system to cool to 300°C. At that point temperature is quickly ramped to 700°C or above. Excess heat lasting a few hours might follow.

  • can ,

    Nice to know you are still out there watching and contributing!


    I ran a test yesterday of the etch rate of the AH50 powder in a 15% mass concentration of HCl. I was afraid that the reaction could be so fast that the powder would just be gone in a short time. So I put 1g of the AH50 powder in 50ml of the HCl etchant and watched it for an hour. There were fine bubbles coming from the powder continuously, but the etching was fairly slow. At the end of 1 hour, the powder mass did not appear to be noticeably diminished and the bubbling continued. The bubbles are believed to be hydrogen of course. Today I am going to process the actual fuel Ni. 100ml of HCl etchant will be used, 5-10g of powder, and the etch will proceed at 50°C in ultrasound. I have already degassed 200ml of distilled water for rinsing; and while still wet, but drained, I am going to freeze it overnight. Tomorrow I will heat it in a vacuum to dry it.


    I wish I had an SEM to see how the morphology of the test etched Ni has changed. [One of these days.] I will be saving a portion of the fuel powder (as I do for each experiment). If the experiment shows any activity, I will have SEM and EDS analysis done on the fuel and the ash by an outside lab.

  • BobHiggins

    Further increasing the temperature of the HCl bath - if possible - may increase the reaction rate non-linearly in an advantageous manner:


    http://www.mikeblaber.org/oldw…ics/Temprate/Temprate.htm


    Image12.gif


    As far as I am aware of, hydrogen loading may occur to some extent with this process, by the way.

    EDIT: e.g. https://www.corrosionpedia.com…ion/32/acid-embrittlement

  • Calibration graph made with the last data point in before the descending steps phase. It looks like the current calibration almost perfectly matches the previous one until the last two steps. I think a third degree fit works better here.




    Here is the data. The power and temperature data points here are the average of the 100 samples preceding the indicated timestamps, except for the first one.


    Time Stamp Heater Power (W) Tube (C-k)

    2017-05-01 21:38:07.183550+00:00 1.7220428332672002e-05 17.942339999999998

    2017-05-01 22:35:00.442770+00:00 7.664807786896651 100.0839074

    2017-05-01 23:34:59.973660+00:00 12.644998846405777 150.01106800000002

    2017-05-02 00:34:59.600540+00:00 18.133817051990818 200.39287689999995

    2017-05-02 01:34:59.139421+00:00 23.896451427578167 250.0262765999999

    2017-05-02 02:34:58.766310+00:00 30.18091099963513 300.00385389999985

    2017-05-02 03:34:58.289190+00:00 36.64975614044998 349.97075779999983

    2017-05-02 04:34:57.924080+00:00 43.37305085003351 399.99852180000016

    2017-05-02 05:34:57.454960+00:00 50.315560292769334 449.9978108000001

    2017-05-02 06:34:57.089850+00:00 57.39183947735066 499.9888697

    2017-05-02 07:34:56.612730+00:00 64.87330223265138 549.9905457999998

    2017-05-02 08:34:56.247620+00:00 72.47135871071728 600.0379964000005

    2017-05-02 09:34:55.770500+00:00 80.6033403371504 649.9752067000002

    2017-05-02 10:34:55.413390+00:00 88.5913023331697 700.480553399999

    2017-05-02 11:34:54.936270+00:00 97.4853823143232 749.9825112999985

    2017-05-02 12:34:54.571150+00:00 106.15427356512576 799.9729999999972

    2017-05-02 13:34:54.142040+00:00 115.333362565592 849.957331099999

    2017-05-02 14:34:53.688920+00:00 124.60688635248215 899.9522664999982

    2017-05-02 15:34:53.307810+00:00 135.2208374344002 950.159078399998

    2017-05-02 16:34:52.846690+00:00 144.98418170356058 999.9508285999997

    2017-05-02 17:34:52.467570+00:00 155.74080537269398 1049.9104676999998

    2017-05-02 18:34:52.012460+00:00 166.98754319927102 1099.973550000001

    2017-05-02 19:34:51.631340+00:00 178.78322825757604 1149.1512001000003

    2017-05-02 20:34:51.170230+00:00 190.72940516887724 1199.9968420000018

  • I have added a Photos folder to the main experiment folder. It shows some snaps from processing the Ni powder. ( https://drive.google.com/drive…B0NkRqSDhkWDg?usp=sharing )


    The 15% HCl etchant was first heated to 50°C in a water bath in the ultrasonic tank. The photos show the use of a Kodak process control thermometer for measuring water temperature because the setpoint by the ultrasonic cleaner is highly inaccurate. After 1 hour coming to temperature, 7g of AH50 Ni powder was slowly added to the etchant and the ultrasound was turned on for 10 minutes (120W). At the end of this 10 minutes, the flask was removed and the etchant was leaf green. The flask was placed in a fixture having a magnet at the bottom of the flask to hold the Ni powder and the etchant was drained into a bucket of water (ALWAYS add acid to water - NEVER add water to acid!). 25ml of degassed water was added, the flask swirled, placed in fixture, and drained again - this was repeated twice. Next, 25ml of the degassed water was added and the flask was put back in the ultrasound bath for 2 minutes, and then drained as before - this was done 5 times. Finally, the flask was wiped dry, stoppered and placed in a ziplok bag and put in my freezer. Tomorrow I will dry the powder and hopefully be ready to load it into the reactor tube that is now performing a calibration.


    @Alan, I suspect that quick freezing will not make any difference. The reason is that in ordinary freezing the water expands to ice and doesn't leak away. In the case of trying to steam fracture, it must be done quickly because otherwise the steam escapes before it has done any fracturing. But, I have never done it before on the AH50 powder, so a comparison has yet to be tried. Now where was my SEM?

  • can ,

    The steam fracturing has [apparently, because I haven't read what he had] been described in Rossi's patent application for fracturing the Ni particles. I like the idea you suggest of superheating the wet Ni at high pressure and then suddenly dropping the pressure as a means to have accelerated boiling. Great input.

  • BobHiggins


    EDIT (reworded): what Rossi writes in his patent on the process is poorly described. I had a short list of patents describing the fragmentation process of porous particles by rapidly expanding gases, but I can't seem to find it anymore. Here's one which in addition to the general process (surely applicable to water/steam) uses preferably liquids that are gases at normal temperature and pressure: https://www.google.com/patents/US6929199


    EDIT2: according to section 2.3 here, depressurization of water below a certain temperature might not necessarily occur explosively, so my suggestion from the previous comment might also not necessarily be useful: http://onlinelibrary.wiley.com…2/full#jgrb15754-fig-0003

  • The 'BarG' way to do the explosive decompression might be to boil the water/nickel in a borosilicate flask and then stopper it and plunge it into an ice water cooling bath. that will boil continuously due to steam condensation.

  • Alan Smith

    I'm not sure I understand the process there. There's a risk the flask could shatter instead, even if it's made of borosilicate glass.


    But more in general, in retrospect I think that perhaps since Bob Higgins is going the oxide-free way it might not be so useful to attempt to fragment the Ni particles by steam fracturing at this stage. If the aim is obtaining smaller particles, wouldn't letting them digesting longer in the HCl and/or at higher temperatures eventually accomplish the same anyway?


    It seems to me that the treatment ordering could be different. For example something like:


    1) Oxidize particles completely or almost completely

    2) Flash reduce particles in hydrogen at high temperature (will cause a porous structure)

    3) Steam fracture

    4) Final cleaning and etching in ultrasonic acid bath (will remove all oxides)


    It's not clear if doing all this would actually be useful, though.