Making Graphite Substrate Lead Dioxide Anodes
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- Опубліковано 11 кві 2018
- Creating these anodes was not too hard once it was all worked out correctly. after a few failures i found the key seems to be the Pre treatment. getting a nice erosion layer is the difference between having the plating flake off or hold tight. the other parameters are important too but having a good substrate is key.
I am still yet to test them in the very harsh environment of an electrolytic perchlorate cell so hopefully they last OK. i don't see why not though.
Other people seem to have had mixed success making decent anodes this way but i'm confident that these will be up to the task. The plating is quite hard, solid and very well adhering to the graphite. If they only last a short while that is fine too. the starting materials are cheap and it's not hard to do.
I also came across some old MMO anodes which i will be plating onto as well, under ultrasonic vibration.
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One from best video, tutorial on PbO2 electroplanting theme. Great work. Hat down.....Dr.
Laboratory of Liptakov thanks. They should work well.
Now i can make tones of chlorate and perchlorate 😀
Great video! I just can't wait to see it in action in a chlorate cell.
Tiltrode I use MMO for the chlorate first and these will be used for Perchlorates. I think they may suffer erosion in a chlorate cell and You can’t use dichromates with them so that cuts efficiently a lot.
impressive job mate
The motor is awesome. I wish I could use something similar in my copper plating bath.
I have some cobalt nitrate and i am going to make cobalt dioxide anode but i cant get any titanium base. Can i coat graphite rods cobalt dioxide whit this method
how much RPM gives your motor? I have failed one with 3000 rpm
does this work for coating metals like steel?
i suppose you could place a spinning rod in the beaker and then keep the actual electrodes apart from that, the spinning effect in the water should fix the bubble issue, may be possible to mess up the geometry of the spinning rod a bit to get greater stirring effect
Can this process also be used for lead substrate
Just wow, this is with out a doubt the best tutorial on a graphite lead dioxide anode I have found after 3 hours of searching. I am looking to make a titanium substrate lead dioxide anode for a larger perchlorate cell. Are you familiar with making these? Any help would be greatly appreciated
Ark Survivor Titanium as substrate can be used only if you cover titanium with thin layer of platinum powder or ruthenium or iridium oxide,and then coat PbO2.
Just what I needed to learn!!! Have always wanted to know how I can do away with those heavy Lead grids for the positive and negative electrodes. So I think I will electroplate some graphite plates and then oxidize one in H2SO4 into PbO2 positive plate! Can't wait to try this!
Super!
How much graphite rod that can be plated with the single batch of electrolyte (I mean that lead&copper salt solution)? Do I need to replace and make new electrolyte when no more PbO2 formed or just simply top-up more lead salt?
dominique rennz the bath should be kept constant and not allowed to deplete lead salt. I made essentials twice as much liquid than required and it was enough. Not sure exactly how much but it is sufficient for at least 3mm thick coat on one rod.
Very nice procedure.
Hello,
I would like to try this, do you know what rpm that motor was spinning at?
Close to the camera framerate, i'd say 30rps * 60s/min = 1800rpm
Great job allchemistry but i wonder if the bottom of the electrode was rounded off there would not be a sharp edge for the plating to build up to much.
Maybe it can be prevented by making sure, that some of the cathode wire sits beneath the graphite rod (e.g by bending it to an L at the end).
For the first successful attempt I did not round off the bottom and there was dendritic growth of the dioxide plating. the round nodules were actually stuck pretty fast and one that did come off was very hard and solid. The next attempts I did round the bottoms and this seemed to stop the extra growth. I guess it will help with conductivity of the anode.
Can i use copper sulfate/lead nitrate ?..
No, this will trigger a double displacement reaction since lead sulfate is insoluble in water. I'd suggest using copper acetate if anything since lead acetate is highly soluble in water as well
Couldn't you just use a stir bar?
why u add Cu2+ to the plating soln? arent u plating PbO2?
IRC you do this so the copper plates out on the cathode so the lead wont plate out and make a mess
Tobinator thx
I'm so confused... How do the metals get attached to the anode? They are normally attracted to the cathode. Is it because they are turned to oxides first... and then being conductive metal oxides... are attracted to the anode?
Or are you calling them anodes because they will be used as anodes in the future... but in this coating process they are cathodes. lol.
This is a serious question. lol. Not all people properly color code their polarity in their videos. But seeing how your using an oscilloscope I assume the color/polarity of your wires is correct.
Excuse me , I have a problem. I have made this type of anode and the result is looking good, but when i ran it for a while in NaCl cell to make NaClO3 , the solution's color change to yellow and some orange precipitate began to appear. After a drop of HCl has been added to the solution some white PbCl2 precipitate appear. So i guess the orange precipitate is PbO. did my Anode reduce itself from PbO2 to PbO? and is there a way to fix this?
ณัฏฐ์คณิน พลพินิจ ideal use of this anode is to convert NaClO3 >NaClO4. Too much NaCl will erode anode. There’s not really any way to fix this on a homemade Anode. Best just start again.
@@AllChemystery ok Thanks
PbO2 can make NaClO3 but not without excess errosion also on graphite it has so many issues including its porosity and overall your best bet is using Ti electrode then painting on a PbO2-Polymer composite substrate and plating in strong oxidizing acid plating bath like Pb(NO3)2 , Pb(ClO3)2 or Pb(ClO4)2 and the latter 2 are far more soluble than lead nitrate and can run at room temperature during plating with zero consequence to the final product.
Plating needs to be done using the copper salts when using Pb(NO3)2 but never dare make copper chlorate or perchlorate!! they are unstable and its best to use a membrane seperated plating cell with Pb(ClO4)2 and adding in some Pb(OH)2 as feed to keep lead ion concentrations up.
@@AllChemystery I somewhat solved that errosion problem with doping it while plating and refining the layered composite PbO2 anode where now it can run at 70 Celsius without flaking and go from chloride to perchlorate.
some errosion is there but its no more terrible than starting from chlorate and will dissapear once it reaches completion to perchlorate stage as the loose lead dioxide particles redissolve dissolves and plates on both the electrodes respectively.
BTW have these graphite substrate ones worked so far because I have long given up on graphite due to shit like thermal expansion.
I cant run 250ma/cm^2 without em getting hot unless I really cool the solution and thats not feasible as the GSLD has a lower operating temp of 35 Celsius max unlike TSLD which if made correctly can run up to 70 Celsius and my process no longer starts with MMO but bare Ti and HF yea thats needed or it wont adhere and resistance will go up as plating happens.
@@CatboyChemicalSociety Running Voltages/Amps & Temperature are one thing.
Extensive Running times are what will really test them.
Ideally if you have the time then maybe a thermostat to kill the power intermittently to allow cooling? That may extend the lives.
How u think
Would this work for Perchlorate/Chlorate cells??? Also could any other substrate work such as stainless steel strips, if so.. would the procedure work the same?? I bought Platinum electrodes and well the chloride concentration dropped EXTREMELY low in the cell and I saw my anodes eroding away :/ i'm discouraged to purchase another anode, still works fine but i'm sure it'll be done for soon.. love the content! Thanks
ive made working perchlorate anodes using Ti electrode and superglue + PbO2 serious!! and ofc other stuff includes membrane cell 1 for plating and other for ion exchange for Pb(ClO3)2 plating solution.
@@CatboyChemicalSociety You got some interesting stuff over on your channel!
That's actually really funny, superglue anode! Amazing!!!
Left a sub.. thanks for the response
@@reformlabs8742 I actually discovered it when superglue spilled on my MMO mesh and I thought chlorate run will remove it but to this day its still stuck to the mesh!!
@@reformlabs8742 holy shit guess what 1 thing I found just now
www.researchgate.net/publication/274890045_Novel_Lead_dioxide-Graphite-Polymer_composite_anode_for_electrochemical_chlorine_generation
THESE GUYS ALSO MADE A SUPERGLUE PbO2 anode!!
Congrats! By chance would lead plate onto steel or titanium??
why would you do that neither of those are good electrode materials
@@simonlinser8286 titanium is the best material for anode although it has some nuance with coating
I was going to try this years ago but just ended up buying platinum electrodes. Steven Hayes did a video o this like 2 or 3 years back but never did a video using them. So please let me know how well they hold up in chlorate/perchlorate cells.
Darian, im using acetates they do pretty very well, they depend on the thickness of the coating, mine was way very thick and is less conductive but still gives me some good yeild, they really stand on making chlorate but not perchlorates, they just felt of about a straight use in a week but not so bad, love using acetates,tht are way cheal and easy to make compair to nitrates :)
how the fck PbO2 beta cant stand perchlorate.You get something wrong at proces or you have some cracks at dioxide layer
you are talking about perchlorate, you thought pbo2 can run a perchporate cell? go google it my friend, as of my experience it cannot make perchlorates and may start to fell off in a straight use for a week. could you upload some video so that i can see you using pbo2 in your perchlorate cell
Am so busy last days and far away from home.I will upload video soon and try to explain where you getting wrong.Its not so simple to avoid micro cracks and lead dioxide layer,but be sure when you do that it stand up to 2000 hours in sodium perchlorate solution at 2,2-4volts and and 20-400 amps depend on anode size.Solution temperature must be btw 40-55 celsius.Some serbian factories use dioxide anodes in 1980-1990 for ammonium perchlorate production,actually in sodium perchlorate production then just doing double displacement with ammonium salt,and go so with killing chlorates with sodium metabisulphide.I have bounch of text because i have man from factory that giving me infos.Right now they use pure platinum plates,not a supstrate coated with platinum.Just be sure once ago they didnt have platinum at all but we had such a great rockets with AP propellant.And they didnt avoid electrolise for production.Just dont give up..try to find way where you get wrong.
Lead dioxide was investigated as an anode substitute for platinum in the production of sodium perchlorate. Rod shaped deposits were prepared on nickel and platinum clad tantalum wires. The plate was dense, heavy, metallic‐like in appearance and not too fragile for ordinary handling. The first phase of experimentation was performed in small laboratory cells to determine approximate electrolyses data. Larger bench‐scale production cells were also run simulating plant operating conditions. Lead dioxide anodes produce sodium perchlorate at high cumulative current efficiencies. One lead dioxide anode was used in cell operation for 3,000 hr. Cumulative current efficiency for a given anodic current density is a function of the cathode material, cathodic current density, and the additive used. Perchlorate can be produced using nickel, copper, stainless steel, and carbon steel cathodes. Energy requirements, under identical experimental conditions, indicate that stainless steel and nickel are the best cathode materials. A current efficiency of 91.5% was obtained with a stainless cathode at anodic and cathodic current densities of 15.5 amp/dm2 and of 7.25 amp/dm2, respectively. No unusual metallic contamination could be detected in the ammonium perchlorate prepared from the sodium perchlorate.
nice work man, thank for the video !, this is a tiny anode...
can i do that on a flat graphite plate? the problem seems to be turning the anode.... are you sure that just stirring the electrolite is not suffiscient?
I have some remarks, i have read some article about lead dioxide plating:
they say that PbO2 had two form, alpha and beta.
it depend on how much you using A (ampereage):
The amount of Beta or Alpha that is plated can be controlled by current density on the Anode according to one source I have communicated with. High current density (70mA per square cm) giving mainly the Alpha, 40mA per square cm and below giving mainly the Beta. This has been confirmed by X ray studies. See Electrochimica Acta 52 (2006)
Sometimes a large current density is used at the start of plating in order to create a large density of PbO2 nucleation sights to improve adhesion of the PbO2 to the substrate.
Generally lower plating currents give smoother coats of Lead Dioxide and about 20mA/cm^2 is good.
This current density will give Beta Lead Dioxide.
current density on Cathodes should be at 2X to 3X Anode current density.
they don't speek about a absolutely nessesary turning anode...
Maybe you should decrease ampereage after few minutes??
Possibly but a decrease just means longer exposure to the current and warm plating bath. The spinning is to essentially stop build ups of weak plating in one spot closest to cathode.
reducing temperature of the electrolite ..? I do not understand why it is necessary to rise to this temperature ... why not try at 40-50 ° C?
Or literally ambient temp ???
as you can see 70c seems to be too much if it destroys the plating ...
It is best to use a weak emperage, and beta-LB plating is more resistant than alpha LD plating, particulary in perchlorate cells.
I think this minimizes the formation of weak plating near the cathode because less current density means less agitation.
Maybe the agitation of the electrolite with Magnetic stirrer is enough to divide the electron flow.
if my theory is true, it mean that possible to plating graphite plates without spinning her, with just a moderate-energy of magneting stirring.
what you think about a circulare cathode in the bottom of the cell?
Stirring cathode?? lol i'm joking
spinning graphite plate at low speed can be do the job?
thank for interest
forget about graphite its trash as substrate!!
use Ti coated in conductive cobalt or manganese oxide as substrate and plate first with lead acetate for a nice alpha PbO2 precoat which is more nonporous then adding a beta coat in a plating bath consisting of either hit lead nitrate or room temp lead perchlorate/chlorate with excess lead carbonate/hydroxide for the beta coat.
then plate alpha to remove the porosity of the beta PbO2 layer and plate beta ontop of that again then just rinse and repeat!!
Is the copper nitrate must be 10g/200 ml ratio with water?
Yeah. All examples that had any degree of success used this ratio.
@@AllChemystery tfi. want to ask again, how much voltage that you use to run the dynamo?
Chemist Kid the motor? It was a 12 volt motor.
@@AllChemystery yes, so you use 12v for that?
Chemist Kid that’s what I said... but it doesn’t have to be exactly copied to work . It just needs to spin fast.to shed off the gas bubbles that are generated
I tink on graphite or on carbon are a bad idea , cause it will crack and fall off and fail with thime.
ive made 34pcs of this by means of using acetates, they are very cheap and super easy to make most of mine, they do pretty very well and just yeild about 300g og this, i actually have a video of making graphite substrated lead dioxide for the first time but its quite bad in coating so i just delete it :(
im using 2 plating solutions for my GSLD since I saw papers saying that beta PbO2 alone is very porous without careful control of conditions and that most commercial PbO2 electrodes have alpha + beta PbO2 in layers and hence I have 1 lead acetate + HCl to force black Beta PbO2 and another containing sodium acetate and lead acetate to create alpha PbO2 which is dark brownish in color and forms a more even compact coat.
can you try it on ceramic plates ?
lead azid ceramic doesnt conduct el.power so coating cant be done
i heard that ceramic adsorbs Pb(NO3)2 solution , and releases PbO2 crystalls on heating , in the ceramic structure . After this ceramic become electro conductive .
lead azid Good info,let give a try.I will upload video of my gsld home made anode.After a two year of fails i found method to produce hard beta layer without pin holes of bubles.And it stand in sodium perchlorate cell more than chinese PbO2 mesh grid anode.My final point was ammonium perchlorate.
@@accipiternisus649 what was that method ?
2 ампера для такого електрода багато, покриття буде нерівномірне, а головне - з високою внутрішньою напруженістю, що гарантовано призведе до розтріскування.