Freethinker's replication attempts

    Possibly the Nickel could form oxides during the baking process however it seems that Nickel apparently only starts oxidizing at about 400 deg C. Baking Nickel oxide in a hydrogen environment apparently reduces it back to Nickel anyway according to Wikipedia.

    Quote from Ecco

    I remember discussing about this. I also remember that they attributed the weight loss during the low temperature baking process to:




    So, not really due to loss of oxides. I could be misinterpreting this, though.


    Or maybe it is ... :


    ". As discussed before, it corresponds to the removal of organic
    matter as well as absorbed water and gases. The dwell period at
    250 C shows a very slightly weight variation after the aforementioned
    loss, keeping the total weight unchanged after the whole cycle.
    In the case of the sample treated at 300 C after the start of the
    heating period, a light weight gain can be observed, confirming
    that oxidation starts to be detectable between 250 and 300 C."

    Quote from FreethinkerLenr2

    @Ecco @BlowFish


    The rational is that the Ni infact, in the regime 100-350C does not oxidize but actually shedding oxide. I will look into the ref for this, But it is something I picked up in discussing this with Bob G and some other guys replicating. There is a paper showing this clearly. I will look for it.


    IN EDIT: http://goo.gl/Zclfx8 p174 fig 2.



    Probably worth recalling that ogfusionist / OEL has long and repeatedly indicated here at the Forum that the green color of nickel monoxide / a.k.a. nickelous oxide, remains undiminished in his "reactor" even after its hydrogen meltdown above 830 degrees C. He indicates that his matrix was surely Al2O3 perhaps with some SiO2, but in any case the the high temerature version of FiberFrax of 40 to 50 years back. His protocol seems likely to have resulted in nickel in a variable but low oxidation number because of its intimate bonding to the refractory fibers. Also, of course, the surface area and the areal exposure of such redox ambivalent nickel was surely very high.


    A further feature that has only been mentioned once here, to my knowledge, is that running an LENR within such a strong thermal insulator can make an even modestly over unity reaction rapidly go into positive feedback and lead to catastrophic breakdown-- assuming the reaction itself has some positive temperature coefficient (most, if not all do, if Dr. Mitchell Swartz is right).


    And I see that is a very good reference FreethinkerLenr2 gives [Cabanas-Polo in Corrosion Science 2012] with respect to intermediates of Ni and NiO.

    @Ecco


    I will not push the envelope on this discussion ;) I am by no means an expert, just that it did make sense to me that way.


    At any rate, it does seem to have a good effect on trapped water and CO2, and in the end, it should have created a more rugged and cavity rich environment. What I hear from other replicators, is that those who have been baking 2-4 h have seen clear indications on anomalous heat. As I of late have had a tough time getting anything good going - Longview may be right - I though the baking might help. And help it might have done, after all. Not just the way I wanted. But still, the elevated radiation seem not to be from normal inorganic chemistry mixing Ni and LAH and Al2O3 and heat it. It is still a special observation, regardless if the Ni is oxidized or not.


    Many thanks for the input.


    @Longview


    I wouldn't mind the destructiveness, if it could only be led in evidence that it was and indication of LENR.

    "Probably worth recalling that ogfusionist / OEL has long and repeatedly indicated here at the Forum that the green color of nickel monoxide / a.k.a. nickelous oxide, remains undiminished in his "reactor" even after its hydrogen meltdown above 830 degrees C. He indicates that his matrix was surely Al2O3 perhaps with some SiO2, but in any case the the high temerature version of FiberFrax of 40 to 50 years back. His protocol seems likely to have resulted in nickel in a variable but low oxidation number because of its intimate bonding to the refractory fibers. Also, of course, the surface area and the areal exposure of such redox ambivalent nickel was surely very high."


    Thanks Longview for the recollection, maybe someday when economically acceptable this method for fusing hydrogen will be exploited. It's impact on burning oil would be enormous.


    It's your contributions to this forum that make posting of experimental results worthwhile. You have made me feel a little less worthless.

    Should have included in the previous post that the NiO residing on the Al2O3 substrate presents the optimum spacing of the -Ni-O-Ni- proton interaction sites to allow -p-p- fusion when exposed hydrogen reaches dissociation temperature. The ragoel protocol is a method for producing the catalyst.

    The scientific process seems to be that a reaction has to be observed to register on the conscious mind and then the unconscious/conscious combine to offer an explanation at the conscious level. A NiO array on an Al2O3 support will cause hydrogen to fuse in a simple reaction if preliminary temperature increases are controlled to maintain the correct oxidation level of nickel. I've observed this reaction and explain it as another example of stellar fusion. Of course it's simple, it involves the simplest of atoms undergoing the simplest reaction and is the reason why hydrogen and helium are the most abundant atoms in the universe.
    No, it's not all imaginary.

    Radiation measured with a GMC during a hydrogen fusion experiment:
    This was done during a controlled run with hydrogen flow over a NiO reactor. The Geiger counter was held at room temperature of ~70 F. while monitoring the count rate. There was no increase over the normal 30 cpm for this location. The GMC is not sensitive to alpha, betas. This radiation would not escape the reactor housing. The gamma wave length is predominantly in the IR region from the LENR indicating that there is no safety concern with this reaction.

    Hi Freethinker.


    Was both the LiAlH4 fuel and Ni baked in your experiment or just the Ni powder?


    Im no Chemist but I am curious about a couple of points and if Oxygen in the LiAlH4 rather than the Ni could actually be a problem. (Thats not to say it would not still be useful in the Ni)


    I notice in the MFMP SEM/EDX analysis of their powder that the one sample that looks like fuel #46 tends to have more Oxygen associated with the Aluminium (and by implication the LiAlH4) than the Nickel. Also the SEM/EDX of the source material shows similar ratios. The LiAlH4 seems to have quite high Oxygen content compared to the Aluminium about 9 or 8 times. I'm not sure where the oxygen would be stored in this sample as if it s unlikely the be H2O since the sample is dry to prevent reactions. I'm also not sure if MFMP baked the Ni in this cases.


    I suppose that if LiALH4 was baked it would need a much lower temperature if it is baked or during grinding since it normally melts at about 150 deg C (about the same time it starts to desorb Hydrogen to form Li3AlH6). Interesting the melting can be inhibited when ground with Nickel powder of the right type apparently. Note pure Lithium also melts at about 180 deg .


    Is there an advantage to bake the LiAlH4 at below 150 deg C in dry nitrogen to remove the Oxygen?


    Note if Hydrogen reacts with Oxygen it will produce water which will itself react with the LiAlH4.


    There is also this analysis by Sangho Bok recently performed as part of the current analysis:


    https://drive.google.com/file/…kED9Wa1dqb2c5eWI0U0k/view


    It is reported and discussed a bit on the MFMP Facebook page on 27th August this year. But I don't think it was discussed much else where at the time as some interesting experiment were going on.


    Is the Oxygen Aluminium ratio in these SEM/EDX analysis from the surface only as opposed to the bulk?


    I suppose once the LiAlH4 is broken down any water present is not a problem providing there is sufficient Hydrogen available for the LENR.

    @Ecco
    @StephenC


    Thank you for your excellent input.


    I have only baked the Ni powder. When ready to fill the core tube, I have moved the miniature crucible, capped with a piece of aluminum foil, (actually an end stump of a COE Alumina tube) while still warm into the N2 rich glove box with a relative humidity of maximum 30% (instrument is a cheap one and not reliable at the low end, minimum is allegedly 20%). The warm powder, not warm for long is weighed in again and put into a mortar where iy is allowed to cool a few moments while LAH and Al2O3 is weighed in. Then all is ground together for a couple of minutes. The Sum of the fuel is again brushed down on the scale tray and weighed again, after which the power is put into the core tube using a funnel.


    The baking serve the purpose of removing the water as such but also in breaking up the surface of the particles to make them more rugged and potentially create more NAE's.


    Ecco: No I have not had the plan earlier to bake both the Ni and the Al2O3 together. But I will consider it. It is a question now of priorities, as I have my argon kit delivered, and the Li is inbound, expected Wednesday, while still having an interesting payload in my reactor.... We'll see. When the Li comes, I will no doubt put my focus on that immediately.


    StephenC: To bake the LiAlH4 either by itself or with Ni... well, I guess it may throw out some humidity, but so far I have had no problems with getting the H2 out , to the contrary. On the other hand if water is detrimental to the possibility of achieving LENR, it may be a good idea. It is not something I plan at the moment. I have a, perhaps over exaggerated, respect for LAH. Messing with it inside the glove box is way enough for me.

    @Ecco


    Yes, I have seen those pictures before. I believe your first part there is exactly what I am looking for, while the non-oxidization in alumina matrix is of less importance. As the powder is in the crucible, the largest part of the volume will not be in contact with alumina, but rater to other Ni particles. The pictures and other information is the basis for the 200 C argument. The main reason is to make the surface rugged and create cavities that can hold H- and Li, basically create NAEs. The main thing is to get rid of H20, but I was under the assumption from the previous reference we discussed that there was also a redox effect while heating to 200C. I may be wrong, but CO and water and possible other compounds or elements may be removed. This is one of the things that MFMP presented after discussions with Parkhomov (as I recall). Heat the Ni to 200 degrees for 2h. The reason would be the one you mention (albeit related to oxidation, but also from "blowing up" water molecules to condition the particles for LENR.


    I have never seen any radiation in my experiments before. I think the baking may be a good thing. I just need to come to terms how it changes the game for me in my test bed and how I go about heating my reactor.

    Quote from Ecco

    @FreethinkerLenr2: the reason why I'm sort of pressing about oxidation is that when I tried to find information about the low-temperature oxidation behavior of nickle powder some time ago, I stumbled upon an open access paper mentioning that cavities can form (on nanoparticles, at least) at the interface between the oxide layer and the bulk of the particles.


    EDIT: on the other hand, if you want to prevent oxidation, it appears that heating Ni particles in air in an oxide matrix (ie alumina) will reduce their rate of oxidation: http://www.sciencedirect.com/s…cle/pii/S0038092X00000256


    Your reference seems clear that the rate constant is lower for particles in the aluminum oxide matrix. While I only see the abstract, it appears likely that the oxide matrix is protecting the nickel from ambient air or oxygen. This may or may not be what you get, or exactly what you want, when you heat nickel powder and/or LiAlH4 and/or Al2O3 powders together. In my mind anyway, it would be important to control (that is systematically study) the redox environment when preparing your reactor, and when running it as well. An important role for alumina powder may be that it greatly increases the surface area that can be potentially wetted by the metals... nearly all heterogeneous catalysts rely on surfaces for their activity, so the more surface the greater the rate of reaction. Surface catalysis can be understood in several ways. One phenomenon at surfaces is the presence of "frustrated" orbitals that are often, for example, in partial or fractional oxidation states due to the ambiguous stoichiometry at surfaces. Also, having a solid refractory substrate can allow a metallic surface catalyst to be far above its melting point, allowing rapid shifts in bond character as well--- good catalysts can form transient bonding to one or more reactants, then release the product rapidly-- No reason to doubt that nuclear catalysis, while mechanistically quite different, in regards to surface rate enhancement may very likely be similar.


    If you really want to prevent "unwanted" oxidation, then inert gas such as argon is likely a good choice-- keeping in mind that at high enough temperature some sort of nickel oxide / intermetallic may form by sharing an oxygen with the alumina. That may be a good thing... experiments may tell.

    Thanks Longview for the interesting information.


    Surface, I would then surmise, is important. As almost every run has been showing up something odd and interesting, using Al2O3, I will continue using it.


    Today, I made a new run with the radiating reactor, but it seem it has now lost it spunk.It was a weird day, starting with a unusual high baseline on the GMC, more like 35+ on average. Soon after I started there was a thunder storm, and after that the values were lower, as though the electrostatic buildup played a role. Also, while during the run there's a buildup in the GMC, values increasing, there was an amazing thunderclap just overhead, and the GMC count dropped like a rock. Those were the top weird things.


    Otherwise I managed to sort out that just a aluminum plate and a couple of copperplated pertinax boards were not enough to block the elevated count, but putting a 25mm thick lead brick infront of the GMC did bring it down to normal level. This then suggests that the radiation is either X-ray or gamma, not beta. No directional test was done, as it was hard enough to trigger levels to test shielding.


    Basically, the spunk has left the reactor, it was not possible to coax it to any higher value than into the 60s of cpm.
    There were another interesting phenomenon though, that will be investigated Monday. At about 1000C, where I could previously pull the power, put it back, and I would get a boost in radiation of 46/47 cpm, the same maneuver would only give a slight increase in cpm, but a weird increase in temperature, directly connected to an increase in power. So after turning on/off like so, when the temperature would be restored, it would then increase some more, and typically the cpm would meander to lower values, after a while of this weird Power/temperature increase, there would come a rapid increase in cpm, being coupled with a similar downfall in temp and power. My interpretation is that the radiation somehow interact with the coil/reactor tube/shell such that the impedance of the load get varied. It looks as the temperature is rising, but it is not a free ride, you pay by pumping more power.


    A weird day in the lab.

    Hi Freethinker. I wish you could get hold of a gamma spectrometer. Any chance anyone near you could loan you one? The signature could be very significant about the type of processes going on for example 511 keV would imply beta + production and annihilation which might be indicative of proton absorption rather than neutrons for example, other values may indicate good signatures of other processes.


    the following book seems relevant


    https://books.google.nl/books?id=FmH7-Yw7K1sC&pg=PT602&lpg=PT602&dq=li3alh6+and+ni&source=bl&ots=p0gp6S5OZY&sig=uez4esZRPWHKycS8Dh7DX2F53rA&hl=en&sa=X&ved=0CCMQ6AEwA2oVChMI0vyT-9TbxwIVpb1yCh3TlAbT#v=onepage&q=li3alh6 and ni&f=false


    It mentions ball milling liAlH4 with Ni intrestingingly it points out that including Ni in the fuel prevents the LiAlH4 melting near 150 deg C about the temperature it starts to desorb Hydrogen.


    I suppose that if ball milling is performed care should be taken that the temperature does not increase significantly.


    and great care that the liAlH4 does not react violently with moisture.

    @Ecco


    Well, Ecco, you are right about the baking time, that Parkhomov talked about longer duration. I keep and deploy my powders (except at baking) in a N2 rich environment at very low humidity. Parkhomov just keep his chemicals in the kitchen (or so it seem) and does not worry about humidity or air, except that to note that one should check the potency of the LAH. If it is 2 minutes, 5 minutes or similar in hours, let us all agree, that no one really knows for how long I need to bake to have similar compound status as Parkhomov. There is a matter of practicality, as I am sure also many times governed Parkhomov. I have heard about other successful replicators (in third person) that they have baked for 4 hours, and have had interesting runs after that.


    For now, two hours baking will suffice, as it is a reasonable amount of time for me so I can directly run hydrogenation during a reasonable working day. I do not live in my lab, like Parkhomov. Like I said, a matter of practicality. I cannot bake over night due to the make shift nature of my oven contraption - I don't trust it to not start a fire when I am not there, nor am I completely sure at what temperature it would land on after such long baking.


    As far as the grinding goes I will keep my current mortar and pestle. Had it been that I made run upon run never seeing anything interesting, I would perhaps look into details like that, but for now, I have no problem filling my time, without parameterize also the grinding of the powder.


    With that said, I thank you for the link showing the freethinker page in your database. I am honored that my work would seem worth while tracking like so. I also agree with your suggestions. I don't find it to be a stretch to bake both alumina and Ni at the same time, increase the amount of Al2O3 or for that matter grind for a couple of more minutes.


    @StephenC


    Regarding "loaning" such equipment.... First of all I really need to be anonymous, for the time being. Secondly, in my circles, the only place to borrow such equipment would be from the university, and that would mean involving - likely - physicists at that university. They are well known skeptics, and would not lend me anything, nor giving a the time of day to explain my hobby research. Further, the current reactor has lost its spunk. There was no really extreme values during the run yesterday and if you check over the three days of running this thing, it seems as though it has diminished in "perkiness" over time. There is no telling if I can get it going again, either with this payload or a new one. Also, I expect Li mid week coming week, and I will for sure prioritize a Ni-Li-LAH run before trying to get a new reactor that radiates. Ofcourse, that said, maybe the Rossi-Patent like run will give up all kind of subtle radiation.


    But you are right that one driving force could be positron-electron annihilation yielding two 511keV gamma photons. It would have been very interesting to get the spectrum, I remember doing such an experiment a long long time ago...




    I thank you both for your links and encouragement. :thumbup:

    Freethinker: Regarding loaning equipment from organisations I fully understand about your concerns. By the way I love the image of you quietly performing the test in a thunderstorm and getting interesting results. Tesla would have been proud to see that I think.


    Ecco: thanks a lot for that link of the whole analysis, it looks great.

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