MFMP: Automated experiment with Ni-LiAlH

I am starting a new automated experiment - beginning now. There was a little bit of a false start as pressure began increasing, but was programmed to be low. Found that I had unplugged the pressure control solenoid. Now plugged in and the pressure is headed to its control point. Hopefully smooth sailing from here.

The first DAQ data file hasn't completed yet, but when it does, it will be copied to the Data_DAQ folder in the following Google drive master folder for this experiment:

https://drive.google.com/drive…1ONmdOdEFIX0k?usp=sharing

The experiment is a high temperature experiment, but it is not with a Parkhomov-like fuel. The fuel is about 0.35g of Ni foam that has been electroplated with Pd. The plated foam was supplied by Dennis Cravens. Separated from this foam in the end with a zirconia felt plug is about 0.05g of LiAlD₄ which was supplied by Mathieu Valat. So, the predominant hydrogen isotope will be D₂, though there will be some H₂ from the OH that is attached to the LiAlD₄. There are some clean-up heating and vacuum cycles, and then the experiment will be run in comparatively (to Parkhomov's experiments) at high pressure - as much as the LiAlD₄ can generate in decomposition up to 90 PSIA. The temperature will top out at 1100°C and will last about 36 hours. This experiment also has a few cycles between 190°C and 350°C which Dennis identified as critical loading temperatures for the Pd. From a setup standpoint, the reactor looks just the same as it did in the previous experiment. Only the fuel, hydrogen isotope species, and the heat/pressure protocol have changed.

Other notables... the vacuum system has its leak repaired (I used Rectorseal #5 instead of Teflon tape on the joints) and a timer has been setup to run the vacuum pump once per hour for 5 minutes. This should keep the vacuum reservoir below 10 Torr. The bug in the DAQ Labview code that caused the .csv files to be missing a character has been fixed. The gamma spectrometer software has been modified to produce a true 24 hour time stamp and include the offset from UT in the stamp.

I've been busy with completely different things lately and I haven't had enough time and dedication to improve the previously used graphing system or make it automated. I tried plugging in the new .csv data files and calibration values into the old script and so far it seems to work. I'll try to post updates regularly but this time I cannot guarantee that I will always be able to.

Here's the last three hours of data or so.

can,

I cannot adequately thank you for the plotting you do. I am grateful for whatever you can supply!

Next I need to figure out how to get the graphing reported automatically and the file transfer to Google as well. I may try to work on automatic file transfer tonight.

BobHiggins

If you don't want to transfer files while they're still being modified, perhaps additional commands could be added to your script so that when a new file gets created the old one gets moved/copied in the synced Google folder.

Here's the latest composite graph showing about 7 hours of data.

Quote from BobHiggins

This experiment also has a few cycles between 190°C and 350°C which Dennis identified as critical loading temperatures for the Pd

Here are pressure vs atomic ratio isotherms for Pd-H, from http://dx.doi.org/10.1007/BF02667685. From this graph it appears that at 1 bar (red line) best loading would be achieved roughly below 150°C. Above this temperature at this pressure the H/Pd ratio becomes very low. I guess you could verify this by monitoring hydrogen pressure in the chamber. However, to be fair, this is for bulk samples and doesn't account for the increased pressure in pores and lattice defects.

Good morning all,

Sorry for the delay in posting the data - that part is not automated yet and I was asleep. The latest files are now posted.

A couple of observations ... The pressure spike at 120°C was likely steam and it was all pumped out. The later pressure spike at 160°C was unexpected. At 160°C, the script was still evacuating the system as part of the cleaning and de-gassing of the Ni foam. However, in this case the LiAlD₄ was at the far closed end of the reactor tube which is apparently a little hotter than the middle. At 160°C in the center it apparently reached the decomposition temperature of the LiAlD₄ and the pressure spike at 160°C was D₂. Unfortunately in this first time script protocol, the system was still in vacuum mode and all of that D2 was lost. This was not all of the D₂ in the deuteride, but it was D₂ gas I didn't intend to vent. At 350°C now, the D₂ pressure has climbed back to 18.5 PSIA and there will be no more vacuum cycles - the pressure will be limited to whatever is evolved as long as it doesn't exceed 90 PSIA. So there is D₂ still present.

At the moment, the experiment is holding at 350°C, and in a little over an hour it will begin a monotonic march to 1100°C over the course ~ 8 hours.

can,

Thanks for the cited graph of Pd loading. Dennis tells me that loading with D is different than H because its de Broglie wavelength is half that of H. However, that type of analysis presumes a bulk Pd lattice. He also noted that this is thin Pd on top of Ni. While this experiment is run in D₂ (from the LiAlD₄), it would also be interesting to run in H₂. The Pd could act like a monatomic filter to present the hydrogen species to the Ni.

Attached is a graph of the last 14 hours of data, from the newly uploaded csv files. I've temporarily limited the pressure range in the chart to 16-20 psiA.

I find the long term decrease in maximum pressure following the fixed up-down temperature steps interesting. Unfortunately the rigid nature of these experiments doesn't allow to look more into it right away.

BobHiggins

I think one possible benefit of this thin Pd layer is that the pressure of hydrogen trapped defects and pores at the interface between Pd and Ni can be very high, if hydrogen permeates through the Pd layer. It's not exactly 100% related but I'm aware that hollow thin palladium cathodes can achieve very large internal pressures when they're made to absorb hydrogen, so I'm thinking that perhaps a similar effect (on a micro/nano scale) could be achieved in gas experiments.

Gas "pressure" in condensed matter is an interesting quantity. While the gas is monatomic and interstitial, it is more of an alloy and there is not any real gas pressure. When a vacancy in the lattice is filled with more than one atom of hydrogen, then there is "gas" and gas "pressure". The pressure is related to how tightly the orbitals of the molecular form of the gas have been compressed to fit into the vacancy. Historically this was related to explosions of steam boilers. The cast iron boiler would have large bubble-like vacancies in the metal. Some monatomic H would enter from the steam into the iron lattice and would dissolve into the metal. When the monatomic H found a physical vacancy in the iron, it would stay there and accumulate with other H atoms forming H2 molecules. The pressure inside these vacancies in the iron could become >100k PSI and would eventually cause so much internal stress that the boiler would just explode under the combined stress of the internal vacancies and the pressure from the applied steam.

It appears like there is some loading of the D₂. I checked the calibration, and at the moment there does not appear to be any excess heat. We'll see what happens at higher temperature.

I know this might sound rather naïve, but could a sort of water hammer effect occur if hydrogen was to impulsively flow through these vacancies? Pressure transients could potentially be much larger than steady state pressure.

Attached is the 14-hour graph updated with the latest hour of data.

can,

I am familiar with the water hammer effect in plumbing but I don't see how it applies in this case. Once the molecular gas forms in a vacancy, it is stuck there - it is too big to traverse the lattice. There may be sonic impulses when a second atom enters a vacancy and forms a molecule. The only way out for a molecule from a vacancy is for a crack to form or for LENR to occur to change the molecule into something else.

In defects slightly bigger than lattice vacancies that perhaps could be more properly defined as nanopores, wouldn't adsorption and dissociation of the hydrogen molecules on the internal surfaces still be able to occur, allowing the atoms to eventually leave the environment?

The latest data shows a pressure drop occurring during the 500 °C temperature step. It appears that pressure would have continued decreasing more before the next power increase.

If a vacancy is big enough to admit 2 atoms, then a molecule forms because the reaction is endothermic, and hence thermodynamically favored. For one of the hydrogen atoms to leave, enough energy must be supplied from the lattice to break the molecular bond of the H2 which is less likely from an entropy standpoint.

BobHiggins

To clarify, I wasn't implying that the dissociation of the hydrogen molecules on the internal surfaces and subsequent diffusion would be exothermic or that it occurs spontaneously.

On an unrelated note, below is attached (.pdf) the latest graph with the most recent data from the current experiment. Pressure didn't increase very much for the latest (900°C) power step. Is deuterium being bled off?

can,

As usual, thank you for the excellent graphing!

I was just pointing out that the molecular-ization is exothermic and is favored, while the de-molecular-ization is endothermic and not favored. So, once the molecule forms, it wants to stay as a molecule and not re-enter the lattice. Of course, it could cause such forces that the lattice will crack and the molecule can escape as a whole. Escape by diatomic flux is not believed to be associated with LENR, but "breathing" (flux in either direction) of monatomic D is believed to be important for Pd-D LENR (but not necessarily for Ni-H LENR).

No, I haven't allowed any of the D₂ to be vented. It is either being absorbed or leaking at a slow rate (not impossible).

1000°C step and pressure still decreasing, albeit slowly at the moment:

I believe that the LiD (and LiH) will undergo periods of rapid release of hydrogen and then at some higher temperature take back in some of the hydrogen. Just because the LiD is segregated from the Pd-on-Ni foam, doesn't mean that the LiD cannot re-absorb hydrogen as the solubility of hydrogen varies with temperature.

Update:

So far (and the experiment will soon be coming to a close), there is no excess heat. The calibration and repeatability seem spot on. The COPs are coming out within about 0.2% of 1.000. This is about the residual in the calibration curve. I believe that when there is excess heat, we will see it.