jeff: E-Cat Replication Attempt

    Hi Jeff:


    Because of the reaction issues (amongst other reasons), MFMP has gone to a rather thicker steel metallic capsule to contain the solid part of the fuel (see the GlowStick 5 Run). The higher temp reaction/breakdowns of LAH[:Li] can get rather complicated, and I am sure that others will comment about this in further detail. It is believed that Rossi has/had used a metallic containment system for the fuel, and Parkhomov used a Stainless Steel Sleeve to facilitate transferring fuel to the heating tubes, but it may have also aided in protecting the tube for a period of time.


    I think you are probably aware of most of this, but I thought I would hash over it as a starting point in this discussion. MFMP hasn't loaded additional Li yet, but that may happen soon. This is when the thicker metallic capsule will really be tested against additional Li. Since Gas Exchange is promoted via the MFMP capsule design, there is really nothing preventing liquid phase fuel from escaping the capsule, just slowing that eventual process down.


    ... If you have some better design ideas on a containment system, I am sure all of us would like to hear!

    Clearly alumina does not work as a containment material when molten Li is present. See the attached photo. Based on a URL that I posted earlier today, the results were not unexpected. I'm just amazed by how reactive molten Li really is. I'll need to line the cell with a metal that is compatible. The previously mentioned article suggests pure Fe, ferritic stainless or Mo, Ta, W. Ferritic stainless is probably the easiest to get.

    As I mentioned in an earlier thread, and from personal experience, alumina is not compatible with molten Li. That got me doing some research. Several references I tracked down state that Alumina + molten Li involves an exothermic reaction yielding oxide complexes of Al and Li, essentially destroying the alumina. My question is: whether the thermal decomposition of LAlH produces the same reactive effects on alumina as molten Li. It would seem that the effects must be attenuated; otherwise how was Rossi able to get his E-cat operating for any length of time. Is it possible that the metallic Li reacts immediately with the Ni and therefore was not available to attack the alumina. I don't know.


    Another reference (dealing with conventional fusion reactor design) compared the compatibility of refractory metals and alloys with molten Li and concluded that Ni essentially dissolves in Li, making the traditional corrosion resistant Ni alloys unsuitable. This is an interesting observation and may explain the formation of the NAE environment due to morphological changes in the Ni in the presence of Li.


    Getting back to compatible materials, among those identified as compatible with molten Li were the low carbon stainless steels (including 316L and 304L), pure iron, and refractory metals such as Mo, Ta and W. I have ordered some 316L tube which will fit inside the alumina tube and will contain the Li and Ni. Unlike the first run, I will not include any Al2O3 powder with the Ni. Sintering may occur, but it is my belief that the Al2O3 reacted with all the Li leaving none available to react with the Ni.


    One more question: does any one know whether the Al from decomposed LiAlH plays any role in the E-Cat reaction?


    Jeff

    I suspect that this paper has been referenced before, but it contains such a wealth of information that I'm posting it again. http://www.scribd.com/doc/2703…lysis-of-the-Lugano-E-Cat


    The paper indirectly addresses a conundrum that has been bugging me for quite a while. Most Ecat experiments are run at temperatures well in excess of the sintering temperature of Ni. So why doesn't the Ni undergo sintering and stop the heat generation process? I believe the answer lies in the presence of metallic Li (and possibly Al) which wets the Ni and prevents diffusion of the Ni across particle boundaries. Ni is highly soluble in Li, which accounts for the poor performance of Ni and its alloys as molten Li containment materials. So at elevated temperatures the Ni would tend to diffuse into the Li rather than across Ni grains.


    It is also interesting to conjecture how Rossi hit upon Li in the first place. The use of molten Na or Li as a heat transfer medium in nuclear reactors and plasma fusion devices is well known, and Rossi would have likely considered an alkali metal for its thermodynamic characteristics. Li is less reactive than Na, and has a higher heat capacity. So Rossi may have chosen Li, and by chance, it possessed other atomic properties that make it an effective LENR catalyst.


    Jeff

    Quote from jeff

    Ni is highly soluble in Li


    Compared to other metals it is. Nickel is very susceptible to corrosion by Li:
    https://books.google.com/books?id=tfDwOe7xWeQC&pg=PA427&lpg=PA427&redir_esc=y#v=onepage&q&f=false





    (The above graph in a linear scale for Nickel and Chromium)




    But apparently Li and Ni don't alloy together:



    (and neither Fe and Cr do with Li - in their pure/metallic form at least)



    I've been wondering lately if these properties could have something to do with the reported excess heat effects by Rossi and others.



    Quote from jeff

    Getting back to compatible materials, among those identified as compatible with molten Li were the low carbon stainless steels (including 316L and 304L)


    At high temperature on the long term stainless steel will also eventually get affected by molten lithium. C and N impurities in Li can also increase SS316 corrosion:


    [1] http://www.sciencedirect.com/s…icle/pii/0022311582904226
    [2] http://www.sciencedirect.com/s…icle/pii/0022311591901609


    Interestingly, it turns out that prolonged high temperature exposure of austenitic steels to liquid lithium causes primarily Ni and Cr corrosion, eventually leaving a brittle porous ferrite (magnetic Fe) layer on the affected surface. Nitrogen content in lithium (not much needed at all: 200 ppm by weight - 0.02%) enhances this selectivity.


    This also implies that it's what would probably happen over time with the stainless steel layers in the "wafers" used in Rossi's Fluid Heater patent, or Parkhomov's stainless steel container. Temperature should accelerate this process. At 1200°C or above it should occur very much faster than observed in the papers linked above.



    Hopefully these findings will ring some bells.

    А And if you try to lithium oxide and unclean Li? At the moment, I spend without experience, for comparison (NiO + Tio2 + Al2O2 + C in equal proportions by volume flow + H2). And then I will be with hydroxide (if there is no appreciable effect).

    The 100 micron fuel particle studied in the Lugano test results was sintered from 5 micron COTS nickel particles. Rossi's patent says that his fuel preprocess explodes the 5 micron particles to create additional cavities on the surface of the nickel particles by heat initiated steam explosions.


    The source of the many exotic heavy elements including rare earths found on the Lugano fuel particle #1 may have come from the pretreatment of the fuel using an electric arc between electrodes made of heavy refractory elements like molybdenum or tungsten. The wide array of heavy elements look like a list of transmutation products rather than an additive of separate chemicals.


    There has been many LENR experiments where electric arc driven transmutation have produced an array of dozens of heavy element byproducts. This process may be how Rossi seeds his fuel with Exotic neutral particles(ENP) produced through the action of an electric arc heating process. Rossi does not describe the nature of the heating process that he uses to preprocess his fuel in his patent. Fuel preprocessing is the key component in LENR engineering reaction designs.


    There is experimental evidence derived from exploding foil experiments that ENP can remain active for up to three days after ENP creation.


    Holmlid must preprocess his fuel for weeks using laser irradiation before his fuel becomes LENR active. The ENP must store a huge amount of EMF energy before it can become active and mobile in order to catalyze a LENR reaction.

    316L SS tubing received earlier this week was machined to fit into alumina outer tube. Initial test material consists of ~1g Hunter Chemical AH50 Ni powder and 35 mg metallic Li. Quartz wool plugs in both ends of the SS tube permits evacuation of atmosphere from and introduction of H2 into capsule. Cell reassembled and evacuated to < 1mT while temperature was slowly raised to ~350C, which is high enough to melt the Li and evaporate water vapor and any other volatiles.


    Heater power switched off and cell allowed to cool while maintaining vacuum pumping. Then vacuum was turned off and cell pressurized to ~20 PSI of H2.Testing consisted of applying power to heater winding, starting at 4V and going up to a max of 24V in 2V increments. Surface temperature of heater monitored with a Thermosense IR thermometer that was previously calibrated against type K thermocouple. Pressure was monitored with a 0-100 psi Baratron and Vacuum General controller. Pressure changes as small as 0.1% can be resolved. At temperatures in the 700-800C range the H2 pressure dropped, indicating that it was taken up, either by the heater filament or, more likely, by the Ni/Li. No pressure change was observed when apparatus was powered off for 24 hours, indicating that H2 leakage is not occurring.


    Unfortunately, no excess heat was measured. The good news is that the 316L SS capsule tolerated molten Li for 10+ hours with no signs of degradation. By contrast, molten Li attacked and penetrated alumina almost immediately. Next step will be to include aluminum in the mixture. This will, at least, replicate the elemental species and proportions used in the Parkhomov experiment. Beyond that, I suspect that I’ll be in the position of most replicators: trying to understand how to create an NAE environment without a good theoretical model on which to base rational design.

    @jeff: what was the maximum internal reactor temperature in your case? Do you have more data, or can you produce experiment graphs?


    316L SS can tolerate well molten Li for a prolonged amount of time (compared to alumina or other ceramics). However surface pitting and selective leaching of Ni and Cr will slowly occur over time at an exponential rate with temperature according to the information I found.

    HI Jeff, All interestng stuff and you seem to have proper equipment. Maybe you have said it above somewhere, but can you tell what coil material you use and what type of power controller? Besides that, I think it can be important that at temperatures above 1000C the Aluminia starts to conduct electricity, which than will also partly run through the fuel. For that reason a three phase system can make a huge difference, because there is a lot of voltage difference between the three heating coils, that should be wound in between each other (see Lugano test).

    @jeff
    Use Martensitic grade or Ferritic grade stainless steel for the reactor shell because those grades are magnetic. Select the grade with high chromium and/or molybdenum content for resistance to lithium corrosion but yet highly magnetic.



    Martensitic Grades -
    Martensitic grades were developed in order to provide a group of stainless alloys that would be corrosion resistant and hardenable by heat treating. The martensitic grades are straight chromium steels containing no nickel. They are magnetic and can be hardened by heat treating. The martensitic grades are mainly used where hardness, strength, and wear resistance are required.


    Type 410


    Basic martensitic grade, containing the lowest alloy content of the three basic stainless steels (304, 430, and 410). Low cost, general purpose, heat treatable stainless steel. Used widely where corrosion is not severe (air, water, some chemicals, and food acids. Typical applications include highly stressed parts needing the combination of strength and corrosion resistance such as fasteners.


    Type 410S


    Contains lower carbon than Type 410, offers improved weldability but lower hardenability. Type 410S is a general purpose corrosion and heat resisting chromium steel recommended for corrosion resisting applications.


    Type 414


    Has nickel added (2%) for improved corrosion resistance. Typical applications include springs and cutlery.


    Type 416


    Contains added phosphorus and sulphur for improved machinability. Typical applications include screw machine parts.


    Type 420


    Contains increased carbon to improve mechanical properties. Typical applications include surgical instruments.


    Type 431


    Contains increased chromium for greater corrosion resistance and good mechanical properties. Typical applications include high strength parts such as valves and pumps.


    Type 440


    Further increases chromium and carbon to improve toughness and corrosion resistance. Typical applications include instruments.






    Ferritic Grades -
    Ferritic grades have been developed to provide a group of stainless steel to resist corrosion and oxidation, while being highly resistant to stress corrosion cracking. These steels are magnetic but cannot be hardened or strengthened by heat treatment. They can be cold worked and softened by annealing. As a group, they are more corrosive resistant than the martensitic grades, but generally inferior to the austenitic grades. Like martensitic grades, these are straight chromium steels with no nickel. They are used for decorative trim, sinks, and automotive applications, particularly exhaust systems.



    Type 430


    The basic ferritic grade, with a little less corrosion resistance than Type 304. This type combines high resistance to such corrosives as nitric acid, sulfur gases, and many organic and food acids.


    Type 405


    Has lower chromium and added aluminum to prevent hardening when cooled from high temperatures. Typical applications include heat exchangers.


    Type 409


    Contains the lowest chromium content of all stainless steels and is also the least expensive. Originally designed for muffler stock and also used for exterior parts in non-critical corrosive environments.


    Type 434


    Has molybdenum added for improved corrosion resistance. Typical applications include automotive trim and fasteners.


    Type 436


    Type 436 has columbium added for corrosion and heat resistance. Typical applications include deep-drawn parts.


    Type 442


    Has increased chromium to improve scaling resistance. Typical applications include furnace and heater parts.


    Type 446


    Contains even more chromium added to further improve corrosion and scaling resistance at high temperatures. Especially good for oxidation resistance in sulfuric atmospheres.


    Use the stainless steel shell as the last layer in the reactor shell. Keep the temperature of the stainless steel layer under 700C(Curie point of iron) to preserve its magnetic properties by using radiative cooling(ie water or air).

    @jeff


    Why Parkhomov's reactor works and the reactors of his replicators don't as follows:


    Parkhomov was lucky in that he used a Russian built power triac lamp dimmer that produced square waves with the proper higher frequency harmonics wavelengths that stimulate the LENR reaction.


    To duplicate this condition, use a second coil for RF stimulation whose length is in the citizen band wavelength range (35 to 37 feet) and drive it with a CB radio.


    If you elect to use a triac, how do you know that you are using a good one that is producing the proper harmonics. You can test your triac for the proper harmonic frequency by listening for interference coming from a CB receiver when the triac cycles through your heater coil. The length of the coil should be between 35 to 37 feet of wire to match CB wavelengths or some fraction of that length (1/2, 1/4, 1/8, etc.)

    My reading of Parkhomov's work has convinced me the secret sauce is the pretreatment of the Ni powder. His powder was 30 years old and when it ran out he started having problems getting excess heat. Also the Ni powder in the US is passivated so it's essentially coated in an oxide. I think the wetting and rapid heating that Rossi included in the patent may be a good idea. I would also try adding some carbon to get a good wet gas (hydrogen and carbon monoxide mix) that will really eat up the oxide on the nickel as well as possibly creating some nice nanostructures for the reactions to take place in. Good luck!

    My reading of the fuel used in the Lugano demo is that it was pretreated in a way that the treatment method generated extensive transmutation on the surface of the fuel particles. The nickel fuel particle was covered with all kinds of heavy Z elements including a full range of rare earths. It is doubtful that Rossi salted the fuel with heavy elements because these elements were not detected in the bulk element analysis of the fuel load. My guess is that this pretreatment process involved spark discharge into the nickel particles in the same way that Mizuno activates his nickel surfaces. This pretreatment was energetic enough to produce sintered particles where many 5 micron nickel particles combine into some numbers of 100 micron particles. Yes, pretreatment of the nickel is the key to a successful LENR reaction.


    It takes a long time to load energy into the Exotic Neutral Particles (ENP) as shown by the weeks of laser irradiation that Holmlid uses to make his iron powder LENR active. Rossi may be producing ENPs into hs fuel through the use of electrical arcing treatment.. The half life of these ENPs are measured in days.

    Ecco,


    Max temperature has been maintained at <1000C. The apparatus could go higher (probably to 1200C) without sustaining any damage. However, it is my understanding that some LENR effects are observed at or below 1000C when COP >>1 occurs at higher temperatures. Since the calorimeter is capable of resolving to 1 watt, even small LENR effects should be observable.


    Jeff

    I would agree that Rossi is doing some type of pretreatment, and that is his trade secret. The Ni I'm using is likely to have an oxide layer, but nickel oxide should reduce in a Hydrogen atmosphere at high temperatures. If you Google "Ellingham Diagram" you will find some diagrams that include NiO reduction under Hydrogen and can confirm the necessary minimum temperature to make the reaction proceed at a rapid rate.


    Jeff

    @jeff: I see, thanks for answering. It makes sense that with a more accurate calorimeter lower temperatures could be used. My impression was that excess heat onset in Parkhomov's case was somehow abruptly occurring with temperature, though.


    If you're out of ideas and you're interested in an easily accessible and cheap method for producing porous particles ranging from the nano to the subnanometric range as suggested in Rossi's Fluid Heater patent, have a look at this paper I found the other day. It requires NiCl2 hydrate, tannic acid powder and a microwave oven:


    Novel Microwave-Assisted Synthesis of Nickel/Carbon (Ni/C) Nanocomposite with Tannin as the Carbon Source


    My understanding is that heating the product of this reaction in air at 500°C will burn most of the carbon. The resulting porous nickel nano/submicro powder could be then further processed/mixed with fillers, lithium, LiAlH4, etc.

    Well...


    Rationally, you could consider the P experiments and the Lugano experiment and in each case reckon what is the likelihood that they achieved an NAE envt? Then the (limited but real) info in each case about conditions etc can be weighed by whether relevant.


    And you should use the best guess temperatures for Lugano, which are, for active tests, approx 700C-800C.

    @Thomas Clarke: I tried graphing data from Parkhomov's presentation here: link


    And this was the result. The curve appears to start increasing sort of abruptly after a certain temperature (EDIT: and even eventually resulting in a better COP than Lugano's)



    Did it really occur? I can't say, but since people are so bent on attempting to replicate Parkhomov's claims, then I say let's embrace them fully and do as he suggests, including heating the reactor tube "no less than 1200°C". Source for this: starting from minute 3:55 in the following video:


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    Quote from David Fojt

    Corrosion by "sting " creates some deep holes helped by HCl ..


    What do you mean by "sting" ?

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