Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

I tested the fusor with the deuterium from the metal hydride cartridge and found equivalent performance to the deuterium from the lecture bottle. Due to some arcing from a damaged grid insulator, voltage was limited to 30kV. A run with a deuterium lecture bottle was followed by a run with the metal hydride cartridge, which was followed by another run with the lecture bottle. Purging of the fuel lines brought the core up to a few torr of air, followed by a few torr of D2 between each run.

Run parameters for both runs were:
30kV, 17.4mA, 10mTorr, ~200k n/s

So that's a confirmation that it will work.

Lecture bottle and metal hydride cartridge
IMG_20200311_223453589.jpg
lose up of metal hydride cartridge, regulator, and connection to piezo valve
IMG_20200311_223505220.jpg
Star mode with metal hydride cartridge
IMG_20200311_223733286.jpg
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Rich Feldman »

That is really cool, Andrew. Hip, hip, hooray!

Might well be a "first time in the world" demonstration, without needing many words of qualification.

Confirms that gas dry enough to put into hydride cartridges is dry enough for fusing.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

I recently dismantled one of the used metal hydride cartidges that would no longer take a charge.

The top screws on, though I was unable to find a way to unscrew it, it may be epoxied in place
IMG_20200312_223728291.jpg
There are threads on the ID of the cylinder
hydrostick1.jpg
Cutting the cylinder with a tube cutter removed the top. It is filled with loose powder
IMG_20200313_114639214.jpg
The casing is pretty thick, about 1/8"
IMG_20200313_114724975.jpg
The cap contains a filter assembly to prevent powder from getting out, and a valve that is opened by depressing the pin
IMG_20200313_114643311.jpg
XRF analysis on the powder indicated it's composition by mass is
70.9% Ni
21.1% La
6.92% Ce
0.42% Cr
0.68% Mn

The powder is almost certainly Lanthanum pentanickel (LaNi5), a common AB5 metal hydride for hydrogen storage. The other elements are likely impurities, probably reflecting the low cost compared to commercial reagent grade LaNi5, though it obviously doesn't seem to affect storage.
https://www.sigmaaldrich.com/catalog/pr ... &region=US
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Rex Allers »

Great stuff Andrew. Thanks for taking it all the way to fusion and sharing the results.

Good info (with resources not available to many) on what is inside too.
You said, "one of the used metal hydride cartidges that would no longer take a charge."

Any idea why it wouldn't take a charge?
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

It was a used one that I got on ebay with a Brunton Reactor fuel cell. It was left screwed into the fuel cell for probably long after it was empty and air with moisture likely got in (by permeating through the fuel cell membrane after there was no flow of hydrogen out of the cartridge) and destroyed the metal hydride.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Rich Feldman »

Fascinating. Probably not good stuff to eat or get in your eye! Nice that you identified it as a standard formulation. Online searches for charge/discharge pressure curves etc. need not be limited to Hydrostik brand.

Andrew, would you be interested in helping to answer an old question, by doing one more "assay by fusor"?

Right here is one Brunton core that was bought new, a few years ago, and run to shut-down in a fuel cell while ampere hours were logged. Then immediately disconnected, and stored clean and dry with whatever residual hydrogen is left in it.
If you have no such thing on hand, you can have mine as a gift. Hope you can then repeat your fill-and-fuse exercise, with no special effort to purge the regular H2.
Neutron yields in a stable system are easier to measure than H2/D2 ratios (and more relevant), for those of us without mass spectrometers.

p.s. Harold Urey's discovery of deuterium used a high-resolution optical spectrometer. But he had to do a lot of enriching, by letting LH2 boil down, before there was enough D to detect that way. First trial failed because the H2 was prepared by electrolysis, and was deuterium-depleted to begin with!
Mass spectrometry had been developed, and had already measured the stable isotopes of all other light elements. But deuterium was hiding behind molecular ion H2+ in the mass 2 channel. Soon after Urey's report, deuterium in enriched samples was confirmed in the mass 3 channel, as HD+. There ought to be no such problem using a mass spec. to measure H contamination in D.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

No special method to purge the residual hydrogen was used on my metal hydride cartridges. They were emptied of H2 down to atmospheric pressure then filled with D2. The H2 to D2 ratio would probably be a few ml H2 per 11L D2.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by ian_krase »

Beware -- hydrogen storage material is sometimes pyrophoric!
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Rich Feldman »

Andrew, thanks for response about the residual hydrogen question. Back in 2016, technical sales told us that unlike the Brunton cores, new Hydrostiks came evacuated. That suggested no extractable hydrogen, or even argon/nitrogen from the factory atmosphere, and that a new cartridge would weigh more after filling and then emptying to 0 psig. Have you heard or found otherwise?

Am still having trouble making sense of this chart, from a European maker (or seller) of hydrogen storage cartridges:
https://www.pragma-industries.com/broch ... -V2019.pdf
hydrides2.png
hydrides2.png (138.88 KiB) Viewed 54459 times
Perhaps very generic, and old, but it seems to show most of the hydrogen locked up at 1 bar! Maybe something was lost in translation.
For material comparisons, one would think the capacity at some stated (or conventional) absolute P_min is just as important as the capacity at P_max.

Andrew, it was insightful to show us the Sigma Aldrich unit prices for hydrogen storage media,
which (in 10g quantities) are many times the retail price of whole Hydrostiks or Hydrocores.

Online documentation taught me some things about Hydrostik and Hydrostik Pro.
The latter supports faster charging and discharging, "for educational applications", using a different storage medium.
The former uses a TiMn2 formula according to one document, and an "AB5" according to another. https://www.horizonfuelcell.com/minipak

Did the non-Pro Hydrostik and Hydrofill get discontinued, or just re-named and labeled?
Hard to find non-Pro stuff online today, except that minipak brochure and this old Hydrofill manual (version 13 :
resources.arcolaenergy.com/docs/Manuals/HYDROFILL_Manual_V13.pdf

One paper lists a bunch of LaNi5 variants, with other elements replacing some of the nickel. They don't show the ceriated flavor that you found.
hydrides.png
from fcto_h2_storage_summit_motyka.pdf

Can't find the documentation from an instrument maker whose hydrogen storage medium is/was depleted uranium powder.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

I think the non pro versions were discontinued.
The one I took apart was the brunton hydrocore (a rebranded hydrostick pro).
Both the Brunton hydrocore, and the hydrostik pro version come full with hydrogen.

Depleated uranium is usually only used for storing tritium. It has to be heated to several hundred C to release the tritium which gives a level of protection against accidental release if the canister is damaged since it will not desorb unless heated.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

I think one benefit of electrolysis at home is no hazmat or freight shipping issues.
Same can apply to using deuterostiks at home, if some enthusiast starts a filling service.
Can items be listed on ebay with a price that includes refundable core fee? - Rich Feldman
Would anyone be interested in purchasing D2 filled cartridges for the following cost + shipping
Filled Brunton Hydrocore / Horizon Hydrostik PRO cartridge containing ~2g (~11L) of D2 = $115
Cartridge refill for ~2g (~11L) of D2 = $65
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Rich Feldman »

I would go for that.
But promised myself not to work on deuterium before I have an operating vacuum chamber again.

Cartridge connectors and pressure regulators are easy to get on ebay, but I would first look into hacking the Brunton fuel cell unit on hand.
viewtopic.php?f=10&t=11147&p=73509&hili ... ted#p73509
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

Recently did some more development on the proportional valve pressure controller. I have the proportional solenoid valve working open loop with both air and hydrogen with very promising results. The drift is less than the piezo valves I was using previously, and they don't require a high voltage source. The end goal is to have an arduino controller query the presser over an rs-485 connection to the vacuum gauge and run a digital PID control loop to stabilize pressure.

This was using the clippard ET-PM-10-0925-V proportional valve $67 ea from http://www.gocfa.com
https://www.clippard.com/part/ET-PM-10-0925-V
and the EVPD-2 valve controller $276 from clippard, however any current driver will work (or voltage source if you are willing to accept a slightly non-linear response)
https://clippard.com/part/EVPD-2

Ion source testbed mounted on dry turbo station
testbed.png
MKS 901p piezo/pirani gauge
vacuum gauge.png
Clippard valve mounted on 1.33CF flange
valve.png
valve controller, taking a 0-5v analog input signal
controller.png
pressure when stepping input voltage to controller
pressure.png
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Richard Hull »

Andrew, a plus-ultra setup! Very nice indeed. Nice plot on pressure as well. Were those wide ranging pressure regimes under you new control setup? We look forward to future posts on this system.

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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

plots are for open loop control of the valve stepping through different input voltages on the driver.

latest tests using a Recom RCD-24-0.30/W/VREF LED constant current driver ($18) to run the valve instead of the more expensive Clippard EVPD-2 driver.
https://www.digikey.com/en/products/det ... EF/2612667
you can also get them as free samples:
https://recom-power.com/en/rec-s-RCD-24.html?0

The LED driver does not have the scaling functions that the clippard driver has so the programming voltage to the driver to command pressured between 1-10mtorr is only a several hundredths of a volt wide, id does work as a valve driver though, at much lower cost. The clippard driver does work better out of the box, but the led driver certainly could have an op-amp or resistor scaling network put before the input.
recom-led-driver.png
recom led.png
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

Latest tests:

Charging pressure from hydrofill pro is about 270psi for steady state operation, this is just the output pressure from the fuel cell, no compressor is used.
Over a 1h run blanked off against a pressure gauge: for the first ~10min no D2 is produced, then pressure climbed rapidly to 300psi over 2min, then slowly to 335psi over the next two min, then slowly dropped to 270psi over the next 10min and held that pressure until it was turned off. I know it has a pressure sensor inside, possibly a digital pressure gauge though it may also be a pressure switch. It says the rated output pressure is 435psi and it never reached this level, it's possibly the microcontroller has some intelligent gas pressure regulator to determine the best output though.
chraging presure.png
Metal hydride cartridges have an outlet pressure of ~250psi
metal hydride pressure.png
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Richard Hull »

Amazing! Your own little tank of D2 at a pressure that will allow for many runs of a stock fusor. A very nice and for sure a rather costly little system that you have reported on before. While I have a larger tanked system and two PEM cells, if needed in future, your system is sort of a middle ground that in many ways is ideal.

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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

More tests on the Hydrofill PRO.

The circuit boards have a KA7500 switchmode controller chip running a buck converter connected to the fuel cell. and an Holtek HTT46R066B microcontroller. The The pressure switch is digital and is connected to pin 16 of the microcontroller (a digital i/o line). The switch pulls the i/o pin high to 5v when closed. Measurements on the fuel cell indicate a voltage between 3.06V-3.2V and current between 7.9A-8.75A. Connecting the switch i/o pin to 5v through a 2k resistor turns off fuel cell current. Doing this a few times shuts down the fill cycle on the cartridge (turns the status light solid green, shuts down fuel cell current). I believe the purge cycle on the molecular sieve hydrogen purifying column is triggered through a timer and not a pressure sensor. The cartridge connector on the Hydrofill has a check valve on it so venting the water trap / molecular sieve column does not empty any deuterium from the cartridge. There is no pin on the fitting to open the cartridge valve so it is opened by pressure alone.

Circuit Board front/back
circuit front.png
curcuit rear.png
Current measurement on cell
current cell.png
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Matt_Gibson »

Thought I would revive this thread now that I see deuterium lecture bottles have doubled in price ($800 plus shipping hazmat).

Has anymore work been done with these? Any chance someone with one of these might be willing to fill a hydrostik if we supply the hydrostik and the heavy water?

I can’t see myself paying $1k for a lecture bottle once mine runs out…

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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Emma Black »

I've been using these for a while now and so far have been working great, much easier than messing around with the syringe and pem arrangement. Each one lasted many months and the refill station has worked well. I got a ridiculous quote of £1300 + shipping for a normal gas bottle here.

Pretty sure Andrew is still able to supply filled cartridges - although the powers that be didn't seem to like these being shipped internationally. I'm also happy to supply these at cost for any UK folks, they work out about £100 each.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Matt_Gibson »

Hi Emma,

What are you using for a regulator on the hydrostik?

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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Emma Black »

I'm using the Horizon one, it screws onto the cartridge and it drops the pressure right down:
https://www.h2planet.eu/en/detail/one_s ... egulator_1

Same one as in the photo at the top of the thread.

Each recharge using the refill station about 30g of D2O.
IMG_4451.jpg
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

The purge solenoid on my Hydrofill unit failed, fortunately it's pretty easy to find on ebay. I have 2 backup electrolyzers so not an issue for deuterium generation, but hopefully I'll have this one fixed
It's a 3v, 10ohm coil, with a normaly closed config
https://www.ebay.com/itm/262673367726
$_57.JPG
s-l1600.jpg
While I had the unit apart I decided to replace the silicone hoses which were degrading and examine the other components inside. All the hose connections are o-ring sealed with a washers compressing a rectangular o-ring against the stainless tube and the seat of a threaded fitting. They are pretty east to remove.
PXL_20231209_015012324.jpg
PXL_20231209_015016560.jpg
PXL_20231209_015026283.jpg
PXL_20231209_015158882.jpg
This unit turned out to be a combination of a reservoir to collect water that made it through the electrolysis, and a pressure regulator to limit the pressure the purge solenoid must handle. The output is over 300psi, but the solenoid is probably limited to about 10-20psi. When the solenoid opens any water in the reservoir is forced out.
PXL_20231209_014837528.jpg
PXL_20231209_014829545.jpg
PXL_20231209_014623774.jpg
PXL_20231209_014611795.jpg
PXL_20231209_014607816.jpg
PXL_20231209_014558854.jpg
PXL_20231209_014537952.MP.jpg
PXL_20231209_014529587.jpg
PXL_20231209_014515784.jpg
The other cylinder as expected appears to be some manner of molecular sieve for purifying the hydrogen/deuterium.
PXL_20231209_015206836.jpg
Appears to have some sort of relief valve on the bottom
PXL_20231209_015219690.jpg
x-rays show some powder inside and you can hear something granular when you shake it
Image__2023-12-08__21-20-17.png
Last edited by Andrew Seltzman on Sat Dec 09, 2023 8:12 pm, edited 1 time in total.
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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Richard Hull »

I noted earlier last year, I think, that the price of heavy water has definitely more than doubled in the last decade. Are production costs increased? There is a limitless supply on earth of raw material (water). I might imagine labor costs, regulations and the electricity demanded in production have increased. I would hate to think someone, entity, nation state, etc. is building up a stockpile of D2 gas or heavy water and bidding the price upwards as it comes on the market. Supply and demand. Same goes for tanked gas as D2 gas isn't found in nature and must come from electrolysis in the end.

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Re: Mark III Advanced Pressure Control / Deuterium Generation from D2O / Metal Hydride Storage

Post by Andrew Seltzman »

Unfortunately it seems this electrolyzer has died (fortunately I have 2 more). The replacement solenoid valve did fix the problem, but it stall wasn't producing deuterium at anywhere near the rate it should. It was producing 0.3l/h and should be producing 3l/h. Blanked off against a pressure gauge, the cell would still produce about 400psi output but at very low supply rate. Cell voltage was at the maximum 5v the board could supply and it was only drawing a few hundred mA. Connecting the cell directly to a power supply required 12-13V across the cell (normal voltage should be 2-3v) to drive the required ~8A. At this current the cell would produce the required 3l/h but would rapidly overheat due to the increased power dissipation. This effect points to PEM membrane degradation (see fig 2) in following paper.
https://h2tools.org/sites/default/files ... er_194.pdf
I decided to dismantle this unit for exploration an possibly future repair.
PXL_20240211_023915089.jpg
The fitting the hydride cartridge screws into also has a pressure relief valve on the back that was not previously visible.
The PEM cell has an M5 output thread, which will also fit a 10-32 face seal pneumatic fitting rather than the internal o-ring they designed. The bolts holding the steel plates (1/4" thick on the water side, 1/2" thick on the deuterium side) were torqued to about 16 in-Lbs as assembled.
PXL_20240211_031528643.jpg
Halves are sealed with a silicone o-ring
PXL_20240211_031922798.jpg
There is an array of channels to allow water access to the cell electrodes and membrane.
PXL_20240211_031927850.jpg
The electrode feed throughs are sealed with RTV
PXL_20240211_031932720.jpg
PXL_20240211_032007009.jpg
The output fitting is stainless and has a fiberglass backup washer
PXL_20240211_032144944.jpg
The metal mesh electrode is spot welded to another finer metal mesh and lays on top on another fine metal mesh. These electrodes have some oxidation (rust?) on them and the water in the electrolyser was starting to get a very fine rust particulate material in it when the electrolyser was run. The good ones don't have this issue.
PXL_20240211_032647374.jpg
Under this electrode is the polymer PEM membrane
PXL_20240211_033212572.jpg
The OEM membrane is bonded to a graphite cloth presumably impregnated with a catalyst. The membrane surface abuts an o-ring that steels it against the opposing electrode to trap the deuterium, a hole drilled through the stack to the other end allows deuterium to diffuse to the center and exit the electrolyzer
PXL_20240211_033320659.jpg
A rigid graphite plate contacts the graphite cloth on the membrane
PXL_20240211_033547315.jpg
The sealing o-ring is removed
PXL_20240211_033711022.jpg
The negative electrode is bonded to a graphite cloth that contacts the graphite plate
PXL_20240211_033916680.jpg
The hole through the electrode allows the deuterium to exit
PXL_20240211_033957863.jpg
and is sealed to the output fitting with an o-ring
PXL_20240211_034016776.jpg
Resistance measurements are as follows
PXL_20240211_033439662.jpg
PXL_20240211_033451638.jpg
PXL_20240211_033519657.jpg
PXL_20240211_033933633.jpg
Does anyone have a guess on the exact type of membrane?
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