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General Powder Update [UPDATE #2 - Loading Cells]

Geschrieben von Wes Baish am .

To start: our sincerest apologies for the delaying data. A lightning storm Monday wreaked havoc on our internal network in addition to a large scheduled upgrade to our servers/network - making the already arduous repairs even more laborious for our IT department. Things are quite chaotic, even losing a measly internet connection for minutes at a time! Please be patient as we look forward to a more conducive network that affords us much more room for expansion. 

In the meantime, Malachi and I have focused on various tasks that require no internet connection, including the parallel updates below.

Status of the R3 Pressure Anomalies

I thought we singled out the instrumentation responsible for these little dips in R3's pressure when switching the P_Resistance and Pressure sensor circuits on the HUGnet endpoint (mentioned in update #2 here), however the next day proved the anomalous data more evasive. I was left with no choice but to plumb in a second transducer, the results of which can more or less be interpreted as devastating to their objective. 

The last of these drops was certainly just as interesting as its predecessors, even yielding two phases in its entirety. The implications of this slope being a real effect would be extremely exciting. The last pressure displayed is low 135 psi at ~0900 local time.

Later that day (1530) I learned a lesson about the unity between a valve head and its seat. Particles that may enter the valve chamber can prevent a flush seating and thus hinder the valve's ability to close, the result displayed above. The equilibrium between the hydrogen line and the cell across the valve was disrupted upon its separation, and the cell lost ~25 psi when the second transducer was added (quarter turn valve open). NOTE that this occurred before the bellows valve was opened to the addition.

Odder still, when I did open the bellows valve, pressure in the second transducer (supposed pressure sink) actually reduced while the cell pressure (supposed source) increased. How is it possible that a plumbing addition at atmospheric pressure gained more pressure than the ~100 psi cell? 

The plumbed addition. 

With the blast shield it's quite a tight squeeze. 

And the result of the second transducer? It mostly agrees with the original sensor, tracking just slightly above pressure. Currently they're both hovering at ~91 psi, however the pressure dips have not occurred since the 25 psi loss from the second transducer's addition. Either there is a pressure threshold that causes the drops to occur in the first transducer, or I stamped out a beautiful and mysterious physical effect. Next week I'll plumb the hydrogen source to the setup and re-pressurize it to test for the former. Otherwise we're out of fingers to point at the instrumentation, and the effect passes as a physical phenomenon. Hopefully we can get it to come back. This joke is not funny.

The straight decline from 2200 to 1430 is a gap where the computer was not communicating with the board (due to the thunderstorm). 

Introducing R4: R5's Replacement

 R5's media was an unfortunate flop, but the idea behind doing a standard no-nonsense hydrogen and nickel nanopowder experiment is still well and alive and (in my opinion) should not be set aside. Therefore I'm breathing life into its fellow juggernaut cell: R4. 

The two cells are virtually identical, as is their protocol, so there's not much to say about it other than we have a new baseline test! The cell is talking with a HUGnet board (as pictured) and is proving stable. I'll soon be moving to step 2 of the protocol, putting the cell on the vacuum and doing a thorough bakeout. 


UPDATE #1 - General Update

Sounds like I work for the department of redundancy department, eh? Wink

As most of the team will be gone for the majority of next week on a business trip, I thought I'd relay the status in powder research. 

Reactor 3: 

The pressure debacle pervades us still, however we have a pretty nice pressure drop. After several attempts, I cannot find any leaks and am left to the assumption that we're finally seeing continuous loading! I promised an increase in pressure to sniff for those interesting cliffs, but as luck would have it we've run out of swagelok ferrules to plumb in the line. The parts are on order, but until then R3 is treading water.

Reactor 4: 

R4 sits comfortably on the turbomolecular drag pump baking out. As of 5 minutes ago the vacuum transducer read 3.5 X10-8 Torr - very close to the 2.8 X10-8 Torr mark we're looking to hit. I HOPE this time we'll see good loading, and am hesitant to move it until I have sufficient time to be near the cell. Time on the vacuum only makes things better, so we'll wait to pull it off the vacuum until the swagelok shipment arrives. This matters because. . .

Reactor 5:

R5's re-recommissioning took a turn for the worst in the argon box as I was confronted with hoards of sintered particles, the largest of which refused to break up and remains in the bottom of the cell. Looking to load new powder into the cell, this massive blemish put the brakes on that idea and R5's pressure transducer and bellows valve were scrapped to ease the transition into a new powder cell. Of course, the assembly couldn't be completed without a key component: the 1/4" swage ferrule. 

That's it for now. Look forward to the unveiling of R7, a brand new powder cell. 

Thanks for reading!


UPDATE #2 - Loading Cells

Though typically no one wants to be wrong, I'm happy to report that the aforementioned necessary parts arrived a week earlier than expected. I'm ahead of schedule; Dreams do come true. 

The word of the weekend is loading, and I hope to see more of it come Monday. 

R3 repressurized and with a decent rate of loading, to boot. P_Resistance following suit which is always a good sign. There are no leaks in any part of the reef hydrogen plumbing. I've checked, checked, and quadruple checked; the hydrogen is going into something other than the atmosphere. 

Still no pressure drops. Were the previous anomalies a real physical effect? We will have to see what the weekend brings.

R4's initial loading curve which (to me) is pretty pleasing. The noise in the latter half of the slope is a bit of a mystery to us. It's present  in all 4 thermocouples as well as H_Resistance. Puzzling. R4's cell temps share an ADC on its sense board, T_amb is on R3's sense board, and H_Resistance is way down below on the reef power supply control board. The noise doesn't show up in any other R3 sensors. We're still sorting this one out, but it very well could be real. Thoughts?

R7 is on it's way, holding a preliminary vacuum at 2.8 X10-8 Torr. I'll be inserting powder media and vacuuming again this afternoon. Hopefully we'll get it baking out by Monday. 

Lastly, R7 NEEDS a protocol before we get too serious. We could easily do another straight-laced Ni-H interaction study, differing only by the duration of exposure to a hydrogen atmosphere and the 70nm particle size. However we could also do carbon deposition for hydrogen storage, particle dispersants to ensure no sintering occurs, or something else. I would love to hear some suggestions Wink 

Thanks for the read!

 

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0 #6 Wes Baish 2013-09-05 16:08
@All looks like we're gonna go ahead and pull R4 off the TMD because it's pressure surpassed the mark at 1.7e-8 Torr. Check the powder experiment log for updates on its progress as it'll need some time to cool down before it gets moved back onto the reef and R4 data stream. Bring on the loading.
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0 #5 Edwin Pell 2013-09-01 20:57
Wes, sintering BAD. It reduces the exposed Ni surface area. Putting some inert material between the Ni particles stops them from touching and bonding together. I think some people use Al2O3 and some SiO2 and various ceramics. Some use zeolites but one person who had used them said they turn to mush and stop working so I would avoid zeolites.

If you have no inert material my prediction is you end up with one big block of Ni foam, I did. Exact how much surface area is lost? I do not know. You might be able to tell by measuring the initial H2 load on baked un-loaded Ni and repeating after sintering.

But do not worry it is a good start pure Ni powder. Just open it up and look at it after a month or so.
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0 #4 Robert Greenyer 2013-08-31 07:47
@Charlie

It has not been forgotten, I just had to put it on hold whist I focussed a little on my business to earn some income and my family who were starting to think they had become MFMP orphans. It has been interesting to see several of the points discussed in other forums.

I am working on the beta for my first iOS app and after release, should have much more time to devote to closing that discussion piece out.
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0 #3 charlie tapp 2013-08-30 14:38
@robert greenyer still waiting and wondering about that big blog we were going to see after iccf. it hinted at new info on makeing this thing work any idea how long till we can know what you guys learned? i wish someone from defkalion would send you there secrets it would certanly speed up things for them they would probably even pass up rossi in the race to sell these things.
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0 #2 Wes Baish 2013-08-30 14:26
R4's powder is 40nm, nothing else. Do you find any advantage to sintering, Ed? I can't think of anything other than a more stable electrical path to drive off oxides.
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0 #1 Edwin Pell 2013-08-30 05:12
The plain nickel powder what size powder? Any anti-sinter agent?
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