Reducing Ni Powder and Inspecting It

Welcome, BTE-Dan.

Quote from BTE-Dan

1) Should the Ni powder sample really turn shiny? (Ihave a feeling that it won’t even when fully deoxidized. Particles may be sosmall and irregular in shape that they always look a dull gray.)

2) Is there a reliable way to test or inspect the Ni powderto see if it’s really deoxidized?

3) Any ideas on how to improve my approach?

None of the hobbyists willing to provide rigorous verification has reported reliable excess heat; hopefully we'll learn something about me356's results before too long. Your guess as to the answer to these questions is as good as anyone's, fortunately or unfortunately. Perhaps Alan Smith , BobHiggins , magicsound or Brian Albiston will have an opinion.

BTE-Dan

Maybe you could try placing a larger piece of metal of the same material together with the powder to see more clearly if the treatment has an effect.

For what it's worth, from what I've seen chemical cleaning (acid bath) is very effective in making at least the larger pieces shiny in a matter of seconds even at room temperature, but especially with small powders it evolves hydrogen gas in the process which you will have to vent away safely.

Quote from Alan Smith

Also, a final idea. Ni is ferromagnetic, but oxides are not. Magnetic separation is a possibility.

If the oxides only form a thin layer on the surface wouldn't the ferromagnetic grains still retain their magnetic properties?

Anyway, I just did a test with powder composed of mostly micrometric iron in a water suspension. Nothing rigorous but I thought it could be interesting to note this here. To my eyes the smaller deoxidized particles appear even darker under diffuse light than the starting oxidized particles, but under strong direct lighting (especially when stirring the mixture) they do seem to reflect light better/differently, or almost shine.

However, if I remember correctly me356 was writing about wires, not powders, when referring to the shining quality of the treated surface.

I would also consider whether putting a lot of effort into a given procedure such as reducing nickel is warranted:

1. Is removing oxygen from nickel something that is worthwhile? It might be; but what if oxidation is beneficial?
2. Is using nickel nanopowder something that is worthwhile? It might be; but what if micron-sized particles are better? Piantelli even successfully used a metal bar, if I recall.
3. Is using only nickel something that is worthwhile? It might be; but what if an impurity of some kind is critical to getting NiH LENR to work? Piantelli's patents mention many possible additives.

Best to question every little tidbit of presumed wisdom about NiH LENR. Rossi, me356, Parkhomov, Songsheng Jiang, Celani — none of them have rigorously established that they have anything, so what they say is apocryphal, or even possibly misdirection in specific cases, and if one is to copy one of their suggestions or choices, one should do so noncommittally. By contrast, Piantelli has gone about things rigorously, as I understand it, which perhaps makes his observations worth paying special attention to.

First, regarding the appearance of the Ni powder... Alan is mostly right that due to the high surface flowery nature of the carbonyl Ni powders, that you would not expect to see "shiny" powder. "Shiny" implies specular reflection and that will not be seen with these powders. If there was a very low degree of optical attenuation in the surface reflection, the powder would appear white with a completely diffused reflection of most of the incoming light intensity. However, optical reflectivity of clean Ni is not that good - what is not reflected is absorbed in every reflection. In a carbonyl particle, there could be many reflections before a photon makes its way back to the direction of your eye, so the powder will appear gray. If there are lots of reflections, the powder will appear darker and darker. It is not evident that surface albedo for this kind of powder is a measure of oxidation. With any of the chemical and thermo-chemical processing I have done, I have never seen the carbonyl Ni powders come out shiny, white, or even light gray - they come out dark.

We have heard Me356 describe using Ni wires. Wires have simple surfaces and are much more likely to have near specular reflections, making them look shiny. Piantelli uses a rod with a simple surface in his reported Ni-H experiments. Shiny surfaces look clean, but are a poor metric for being oxide free. Shiny surfaces are also going to have small surface area for a given mass of Ni.

Don't even consider using Ni nanopowder without a great deal of controls to handle the material (beyond even what many good laboratories have). People have gotten seriously ill from handling nano-Ni. It will readily penetrate gloves and skin; and then organs, including the big one in your top knot. It is one thing to handle nanomaterials of a noble (non-reactive) metal (Au, Pd, Pt) and quite another to handle nanopowders of a reactive metal like Ni.

I cannot presently account for the apparent success of Parkhomov, Jiang, or sometimes Zhang Hang with the Ni - LiAlH₄ system. Parkhomov claims that he does not use special Ni powder (we have examined his powder under the SEM and found nothing special), or a special preparation to make his reactors active; and from MFMP interactions, he seems honest and genuine. Jiang apparently does use some pre-processing of the Ni, but it is undisclosed. Even still, Jiang's results are not entirely repeatable in his own experiments.

I think Me356 claims that stimulus is important, and we are hearing the same from George Egely, and from Suhas for his 1 MHz electric discharge reactor. Parkhomov's apparatus had some degree of magnetic stimulus from his heater coil and his step switching of the heater's AC current. There are plenty of ways to add low frequency magnetic stimulus and RF stimulus - it is perhaps the last unexplored (or at least unreported) variable. Could that be because when RF stimulus is used, it works, causing the authors to go quiet?

I believe Piantelli uses a unique means of stimulus in his Ni-H LENR that is not directly extensible to powders: the use of actively generated thermal waves, combined with "right sized" surface metal grains, producing transient condensate behavior. It appears to be a low frequency thermal wave resonant stimulus. I think it is teachable in many ways, but hard to imagine how it could be applied to powders.

BobHiggins

Piantelli et al.'s expired 1995 patent and some of the papers published in the 90's suggest that their bars were acid-etched and electroplated, not simply plain bars.

can

Yes, but that was done to produce a surface Ni film that had grains the "right size". Piantelli examines the surface with SEM and micro-XRD to understand what surface grain structure he is creating. This is tied to his means for LENR stimulation based upon (my interpretation) an actively resonant thermal wave stimulation.

It's possible the process of electroplating deposited an impurity element such as platinum.

Let me just throw in for encouragement that Parkhomov sees excess heat without any pre-processing of the Ni powder, and without SEM analysis. MFMP's analysis of Parkhomov's powder (actually by Ed Storms) shows it to be ordinary carbonyl Ni powder with a range of particle sizes of 3-10 microns with no unusual chemistry. What I have not seen reported is someone replicating Parkhomov's magnetic field stimulus that he provides with his stepped AC drive of his solenoid heater coil.

The less encouraging is the fact, that even Parkhomov himself wasn't able to replicate his first experiment (probably rather measurement error than lucky accident). The LiAlH4 is extremely reactive substance, the probability of their keeping in air-tight reactor at high temperatures is literally zero in amateur conditions. With compare to it, the hydrogen plasma will clean the nickel surface and saturate it with hydrogen continuously - so no special preprocessing of nickel may be actually necessary.

Zephir_AWT

In Parkhomov's first experiments with sealed tubes, the ones that sealed well exploded (cracked open) and failed. The ones that leaked with a small leak were the ones that worked. When MFMP got Parkhomov to measure his pressure, it was found that in the region of XH, the H₂ pressure was below atmospheric (less than 1 bar absolute) - primarily by leak. If there is no leak, when the LiAlH₄ decomposes, the pressure can go to >100 bar.

I had good results in surface cleaning of Ni foam in FeCl3 (PC etching solution). See the images at:

Ni Foam hacking II

Compare that surface morphology to the First image at Substrate Micro Structure, to see the effect of surface etching.

BobH has also used acid etch (HCl) on Ni micro particles. My impression is that Ferric Chloride is pretty aggressive, and low concentration dilute solution would be needed to avoid Carbonyl Ni dissolving completely.

magicsound

The FeCl₂ etch is interesting. Did you use PCB etchant or did you make up your own FeCl₂ solution? Normally HCl is added to PCB FeCl₂ etchants. Also, the result ends up with NiCl₂ and iron in the solution. If you are working with Ni powder and use a magnet to drain the solution from the powder, you will be left with iron and maybe NiCl₂ in the mix with the Ni powder. Hopefully the NiCl2 remains dissolved in the water and is washed away even if a magnet is used to retain the powder. Sounds interesting, not sure what the iron will bring to the reaction, but it was reported in Rossi's low temperature fuel.