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Solid States Devices => solid state devices => Topic started by: Jimboot on December 24, 2019, 05:29:23 PM

Title: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 24, 2019, 05:29:23 PM
hi all I'd mad some intercalated graphite recently using fecl3 and some plant material. I used Robert Murray smith method of soaking in fecl3 then into the kiln slowly ramped up to 750c . The device on my bench measures just over a volt and is dry. Not a chemical reaction. Can post scope shots and videos if anyone wants to take a look. It does not seem like normal behavior though. MERRY CHRISTMAS!
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 24, 2019, 11:11:32 PM
Hook a bunch of them in series and parallel
See what happens


By the way, is your ground reference the earth?
Or is your scope isolated?


During the Cold War ionic carbon was thought to be a
potential source of a room temperature superconductor.
Many governments enlisted the scientists of the world to
try and make one.
They are still trying today......
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 25, 2019, 04:01:35 AM
I've tried both more interesting results with the house ground https://youtu.be/mfo_ITGSjh8 (https://youtu.be/mfo_ITGSjh8) you may recognise the material given your handle. Check your pm at our.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 25, 2019, 06:49:42 AM
Here's a quick and dirty conductivity test https://www.youtube.com/watch?v=mGU5Aw7hKKE
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 25, 2019, 08:17:09 AM
If you have your meter connected between anode and cathode you are seeing galvanic voltage. You won't be able to discharge it like a capacitor. I am also working on a rechargeable aluminum ion battery. I've only been at it a few weeks so I've still much to learn. Looking forward to seeing your further progress. Ps: The oxide layer that forms on aluminum is a killer. Saltwater will not readily strip it away.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 25, 2019, 10:36:19 AM
Try an analog meter
some of those dmm's can send V in reverse
because of the way the internal resistance circuits are designed.


The voltage climbing when you connect the meter may be a clue.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 25, 2019, 10:54:24 AM
Nice work making it conductive.
In theory, it is possible for Cl Ions to have been trapped
inside the carbon lattice
however it is a higher probability that some iron was not
able to fully oxidize, and therefore would also be trapped
inside the carbon structure.
This will of course depend on the cell structure of your carbon source
and how it is contained during the thermal processing.


I have not yet had that much success, but was on a similar path about a year ago.


I got distracted into reactive nanocarbons because they act like they're alive.

Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 25, 2019, 11:02:25 AM
Acetates were a little easier for me to work with
my goal was entrapping ionic metallic acetates in the lattice.


Equally as hazardous but lower working temps.
in a hot liquid crystallization process, it is possible to
bond a metallic salt directly to the carbon while it is forming
allowing the growth of a complex crystalline interface


Most of my experiments failed because I was using the wrong
type of crystal and the carbon wasn't able to out gas properly
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 25, 2019, 03:46:52 PM
Quote from: kajunbee on December 25, 2019, 08:17:09 AM
If you have your meter connected between anode and cathode you are seeing galvanic voltage. You won't be able to discharge it like a capacitor. I am also working on a rechargeable aluminum ion battery. I've only been at it a few weeks so I've still much to learn. Looking forward to seeing your further progress. Ps: The oxide layer that forms on aluminum is a killer. Saltwater will not readily strip it away.
there is no corrosion. There is no chemical reaction, the cell is dry
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 25, 2019, 08:16:55 PM
I saturated a paper towel in saltwater and then dried it in microwave. I placed it between a 2"x2" piece of copper and aluminum. The voltage I measured was near about the same as with wet separator. As a control I used a dry towel that had not been soaked in saltwater and still measured a voltage. Now for the stick in the spokes. I removed the copper and touched one probe to aluminum and the other to wet separator and also measured voltage. Lay the probe tip on its side so as not to penetrate the towel. The readings varied between.5 volts and .7 volts on all test. Maybe you can try this to see if you get similar results. i have suspicions of what's going on, but can't be certain.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 26, 2019, 12:34:36 AM
Graphite electrodes could help resolve that type of conjecture

Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 03:04:15 AM
Smoky2, I can only guess that your suggestion to use graphite is to point out something I'm overlooking. But instead of the teacher giving the answer, your going to make me work for it. Since I'm at work I can only test with aluminum and copper. I did not mention that I had ran across this before. I can't remember if I had the separator only on aluminum or a graphite electrode. Given that I measured around 1.62 volts I believe the separator was on aluminum. What I did not realize at first was that my hand was touching the bench top. When I lifted my hand I could not read a voltage. Now the test I did previously I was still able to measure voltage even though no other part of my body was grounded.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 26, 2019, 07:22:27 AM
One probe on the graphite one on the al. I thought at first the same as you. I wanted to find evidence of it so I could dismiss it and move on to th grapene process. Intercalated graphite is weird, smoky comment about these thing behaving like their alive rings true with this material
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 07:28:14 AM
I haven't made it to the level that your at with processing the material. But I have to say that this thread has made me realize many of my mistakes and clear up some misconceptions that I had. Hopefully smoky can shed some more light on things.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 26, 2019, 07:43:26 AM
Quote from: kajunbee on December 25, 2019, 08:16:55 PM
I saturated a paper towel in saltwater and then dried it in microwave. I placed it between a 2"x2" piece of copper and aluminum. The voltage I measured was near about the same as with wet separator. As a control I used a dry towel that had not been soaked in saltwater and still measured a voltage. Now for the stick in the spokes. I removed the copper and touched one probe to aluminum and the other to wet separator and also measured voltage. Lay the probe tip on its side so as not to penetrate the towel. The readings varied between.5 volts and .7 volts on all test. Maybe you can try this to see if you get similar results. i have suspicions of what's going on, but can't be certain.
did you try it with a dry separator? I'd be be interested in the results. Might help explain it away so I could get on with my life 🙄 so everything is dry for a couple of weeks now,in the shed in an Aussie summer. I was then thinking it was the meter doing something but tested it on the scope and the opposite was true. The dmm was attenuating the voltage. It's doing my head in. I'm trying to find the gremlin. So all feedback appreciated

Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 07:45:10 AM
A couple things you might keep track of is temp and humidity. It is socked in fog where I'm at so moisture in the air may have some effect.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 07:50:17 AM
I tried everything I could think of.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 26, 2019, 08:49:24 AM
Quote from: kajunbee on December 26, 2019, 07:45:10 AM
A couple things you might keep track of is temp and humidity. It is socked in fog where I'm at so moisture in the air may have some effect.
I have a barometer in the shed so that's a very good test. Thanks. I should get some good transients of the next couple of days. It has felt more humid but I have not measured it. I should add though if I hit with a torch voltage will increase.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 11:53:39 AM
I had to find out for myself how much moisture content effects the measurements. These are the results from 3 runs. I started each run with saturated separator of salt solution. I then popped the separator in microwave in ten second intervals and recorded voltage of assembled cell.
Quote


Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 12:16:52 PM
I just realized that I'm not taking into account the contact when the separator drys. It becomes rigid and wrinkled and is effecting the readings. I'll try to clamp it someway before taking measurements.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 26, 2019, 01:52:28 PM
Quote from: kajunbee on December 26, 2019, 03:04:15 AM
Smoky2, I can only guess that your suggestion to use graphite is to point out something I'm overlooking.


It was for Jimboot , to eliminate galvanism as a possible explanation.
it is standard battery practice to use inert electrodes.
this also prevents corrosion and extends the lifetime of the cell.


You can connect Al or Cu or any suitable conductor to a graphite rod
and not worry about erroneous readings.


Analog meters don't usually cause the same problem that the DMM's do.
Because internally they are built to respond to the circuit,
Where as a DMM alters the circuit then analyzes the results.


Also DMM's can be susceptible to static charges and be inaccurate at times.
(sometimes shorting the terminals or removing the battery can 'fix them')




On the uneven paper electrode surface:: the paper towel might not be the best way to go.
You may need coffee filter or something that will stay flat

Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 02:01:40 PM
Thanks for the info, I have a roll of celgard 2400 seperator material on order. What I need badly is some ideas for a non aqueous electrolyte that would be suitable for aluminum ion battery.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 26, 2019, 02:12:57 PM
I will repeat the test tomorrow using filter as you suggested. I'm on night shift so I'm getting a little cross eyed from no sleep.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 26, 2019, 11:54:23 PM
At 65% humidity 1.125 at 60% 1.140 . Btw this started at 300mv . I surprised it's risen over time. My analogue meter is busted but that will be a good test.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 27, 2019, 12:03:55 AM
Also these are screen shots I took on the 21st. I'm using the house ground which is adding by the looks of it a harmonic set of spikes. The zoom is of the final spike in the sequence.[/size]

[/size]

[/size]
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 27, 2019, 01:04:13 AM
What I noticed in my test was the voltage was lower when I first formed the cell. After the first 10 second warming period the voltage increased. Now I'm not sure which way I should look at this. Did the warming lower its ionic resistance. Or did removing some of the water raise the salt concentration which lowered the resistance. Or a combination of the two. https://en.m.wikipedia.org/wiki/Aluminium–air_battery (https://en.m.wikipedia.org/wiki/Aluminium%E2%80%93air_battery)
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 27, 2019, 08:01:01 PM
Still at 1.18 this morning I built it two weeks ago.  I think I need to go and buy an analogue meter. It will be interesting to see the effect as when I remove the dmm the voltage rises.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 27, 2019, 08:28:03 PM
Earth ground will always introduce those low-amplitude feedback signals
Partially telluric currents, partially underground television cables
(and yes with an Amp and filters you can watch tv from an earth battery signal)


But, 0 will always be 0 unless your other reference is a different part of earth.


With an ungrounded scope, 0 is the scope case, and what you are measuring could
be at any potential until you try to measure it.
At which point it is referenced to the scope.
Why does this matter?
Normally it doesn't.
The scope shielded case has a high inductance.
but if it's sitting on a metal desk and the cooling fan is blowing charged air onto it
the scope takes on a charge (and the desk oppositely)
Which makes 0 not 0.
(in which case everything would take on a voltage when you try to measure it)


There are many ways in which we can measure a potential.
When my PC is on, my desk measures +4.3v  with respect to earth fairly consistently.
(fatal flaw in electronics, ground everything to the case but the PSU to earth)


Once you eliminate every other possibility, and are still unable to discharge the material
Feel free to classify it as
an Electret
Category: 1n









Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 28, 2019, 12:17:04 AM
.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 28, 2019, 12:20:23 AM
Thanks Smoky.

I bought a passive analogue meter. Over the 3k resistor I get around 100mv. Leaves me scratching my head.
Every time I measure seems to get less and less so what ever it is looks like I'm dissipating heat? 
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 28, 2019, 01:58:49 AM
Made a new cell of ground up material. Wrapped in tissue a few drops of salt water. Then clampep. 800mv over the 3k resistor same waveform but the scope voltage is 10x whereas the dmm is still 1.1? Wtf also the earth spikes have phase shifted
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 28, 2019, 03:50:03 AM
In all my battery experiments at home I use graphite cathode and aluminum anode. Depending on the electrolyte and its strength will effect its performance. The highest voltage I was able to get was 2.8 volts. This was by replicating a YouTuber named Cayrex2. The video I believe was "bi-functional hydrogel aluminum battery".
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 28, 2019, 04:14:25 AM
When you wrap the tin foil do you put shiny or dull side facing out. If you put shiny side facing out does it start to dull over time. Or should I say faster than it normally would.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 28, 2019, 04:51:53 AM
Smokys comments have forced me to rethink everything I have done up too this point.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 28, 2019, 09:45:44 AM
Kaj,


Important thing to know about aluminum foil
(or any pressed oxidizing metal foil /thin sheet)


The machines that do this run dual-layers of material
against each other then press them.
the shiny side was facing the roller and has a very thick oxide layer
the dull side was al-al through the press and the oxide layer is very thin


Always put the dull side in the battery. This surface can make a much
better contact with the electrolyte.








Jim,
you see from that circuit now what I was talking about?
The 1MOhm resistor in the DMM can feed that V back the other way
I'm pretty sure the 1V is the drop from 5v to 4v internally
the resistors are set up for multiple pathways and the IC can bleed
so while you are measuring outside, the inside sends the V through
the lead loop, and picks it up as a measurement.


With the analog meter it has to actually BE there to move the needle.


The scope shot is interesting.
Seems like it is able to pick up the signals better when it's smaller pieces?
I know this isn't about earth currents, but your "antenna" got an upgrade

Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 28, 2019, 11:44:29 AM
Next question:


Is the ground wire a true earth ground?
Or tied to your house ground which then goes to earth?
On the house ground you can get a signal from each appliance
on the line with all the tv channels and the telluric


Not the current the device is using, that all goes back to the line
But a mirrored feedback of much lower intensity will appear to ground.
By turning on/off stuff in your house you can isolate individual spikes
The house currents don't normally spike like that. They hang out near
the 0 line as "fuzz". Cable signals can be the largest of those because
of so many underground lines pushing a lot of power from the tv station.
But if you wanted to isolate your house (and any airborne signals )
you can run a piece of coax straight to a rod in the earth and make an
independent ground for the experiment.


Then you will only have the feedback signals from the earth.


I'm wondering if the (avg) particle size is acting like a receiver to certain
of those spikes, amplifying them somehow?
You should run many tests and collect a lot of comparable data.
Maybe multiple identical cells side by side
narrow down what changes cause what effects etc.


Wishing I had a kiln right now.....
Highest I can go is about 700F....
You're pushing 1300 degrees!!


Fire pits don't work cause you can't really control the temp
so I can only sit back and observe atm
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 28, 2019, 12:22:59 PM
I have a cheap POS meter and thought maybe I was getting false readings also. I borrowed a Simpson 260 from the port captain so I could do a comparison , and these are some measurements I took. I'll have to investigate further with graphite once I get home. I have several new materials on order and I'm chomping at the bit to get started. In a couple weeks maybe I'll have something worthwhile to report.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 28, 2019, 12:31:17 PM
Smoky , do all DMM have that issue or is it just the cheaper grades.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: sm0ky2 on December 28, 2019, 03:02:49 PM
More expensive ones have better circuits so the problem may be
less of a hassle. Some even have a button that "zero's" it out.
But yes, in short, the method of measuring voltage with a DMM
can put a charge on the circuit unintentionally.
Sometimes they will charge a capacitor while you're trying to measure it.


Yours looks pretty accurate looking at your log.
0.1v is about as accurate as you can expect a DMM to be.

Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 28, 2019, 07:44:30 PM
Quote from: sm0ky2 on December 28, 2019, 11:44:29 AM
Next question:


Is the ground wire a true earth ground?
Or tied to your house ground which then goes to earth?
On the house ground you can get a signal from each appliance
on the line with all the tv channels and the telluric


Not the current the device is using, that all goes back to the line
But a mirrored feedback of much lower intensity will appear to ground.
By turning on/off stuff in your house you can isolate individual spikes
The house currents don't normally spike like that. They hang out near
the 0 line as "fuzz". Cable signals can be the largest of those because
of so many underground lines pushing a lot of power from the tv station.
But if you wanted to isolate your house (and any airborne signals )
you can run a piece of coax straight to a rod in the earth and make an
independent ground for the experiment.


Then you will only have the feedback signals from the earth.


I'm wondering if the (avg) particle size is acting like a receiver to certain
of those spikes, amplifying them somehow?
You should run many tests and collect a lot of comparable data.
Maybe multiple identical cells side by side
narrow down what changes cause what effects etc.


Wishing I had a kiln right now.....
Highest I can go is about 700F....
You're pushing 1300 degrees!!


Fire pits don't work cause you can't really control the temp
so I can only sit back and observe atm
Thanks Smoky, I'll put my own ground in. Been meaning to do it for a while for these sorts of tests. The Kiln is my wifes that she uses for silversmithing. Robert Murray Smith read and others papers recommend this method. I think simpler identical cells and comparison is a good idea. I'll get back to you :) I started this thread at overunityresearch. 
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 29, 2019, 04:58:07 AM
ignore dmm & scope shots. They're rubbish. So Im just using the Analogue meter. Still get 500mv, working to get it higher or build cell in series. I'm also making a toroid from the material to run some tests with.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: kajunbee on December 29, 2019, 08:32:55 AM
Jimboot, I didn't think to ask what you are trying to make. Is it a capacitor or a rechargeable battery. In my experiments I have been attempting to make a battery. I realize now that it's impossible with and aqueous electrolyte. All I will get is water electrolysis because as you already know it only requires a potential difference of 1.23 volts. Much lower than it would be for aluminum. But something else I've been missing is how I've been charging the cell. With electrolytic capacitors the insulation is a hard anodized layer. So if I understand the process correctly when I'm charging the cell I'm forming that oxide layer. But the electrolytes I've been using (naoh, koh) rapidly dissolve that oxide layer. This might explain why I can store charge with some electrolytes and not others. I'll have to do some more research to know for sure.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 29, 2019, 07:05:41 PM
Hey Kajunbee, I'm in the middle of creating graphene from the intercalated graphite when I noticed a resting voltage without charging it. At the moment I'm trying to isolate the source of it. I made 2 cells last night for testing 500mv resting voltage 1v in series.
Title: Re: Intercalated graphite carries a resting voltage without giving a charge.
Post by: Jimboot on December 31, 2019, 07:04:52 AM
RMS got back to me. He tends to think it's an electrostatic or ambient temp changes etc. I tend to agree. I'll move on from this now. Thank you Kanjunbee & Smoky both for your help. A cell with around 450mv no load. Attached a 10k resistive load drops to 150 and bounces around.