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dann2
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All you need is Iron (my foot)
Hello Quest,
New to this thread eh!!
My take on LD Anode is that amateurs have been having a hard time producing a long lasting anode.
Substrates tried have been Graphite, ceramic, plastic, cloth,
none! (massive anode) and Ti.
I am getting around to trying Ti. It needs a precoat to stop Ti oxide from forming and electrically isolating LD from Ti.
Some reading here>
http://www.geocities.com/CapeCanaveral/Campus/5361/basechem....
Iron has been mentioned in the patents and scientific literature usually to make a massive anode. I seen an anode once that used an iron wire as the
substrate to make the anode but the iron wire was then ignored when anode was put into service.
(ie. it was a ,so called, massive anode)
Massive anodes are very very likely to crack and break.
Dann2
[Edited on 3-10-2007 by dann2]
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quest
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first try at alpha-LD making:
* I used 2 iron electrodes, 3*1 c"m in dimension.
* distance between electrodes = 4 c"m
* electrolyte = 700 m"l water, 5N NaOH, 27 gr' PbO. (not all PbO was dissolved)
* 2 Volts, 0.08 A.
* 30 degree celsius.
run this cell for two and a half hours with constant stirring.
result:
1) alot of metalic Pb on the cathode and on the bottom of the vessel.
2) a thin coat of black substance on the anode. this substance was very easy removed when scraped with my hand (I wore gloves of course).
when smudged on my glove the substance looked brown.
So why am I getting so much metalic Pb? is there any way to stop this lose of Pb ion?
And do you think the black substance was alpha-LD or just some iron salt?
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chloric1
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Quest the first problem I notice right away is your lack of tartarate. This complex might keep lead from plating on the cathode.
About iron, even the alpha coating is going to oxidize the iron once placed in a chloride or chlorate solution. Did you etch your iron prior to
plating. I would dip the iron in a dilute acid such as HCl or H2SO4 prior to plating to give the LD a rough surface to "grab" . Better than that,
concentrated HNO3 will give black iron oxide on steel passivating it. I wonder what would happen if you plated that?
Fellow molecular manipulator
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hashashan
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| Quote: | Originally posted by dann2
| Quote: | Originally posted by hashashan
Hi, did some alpha lead plating, weired thing... i only got a thin brown plating, couldnt get the thick black deposition. Anyone tried to plate alpha?
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Hello Hashashan,
Never plated Alpha myself. I used to communicate with a guy who did lots of plating from a Lead Acetate bath, (made from vinegar and Lead metal). It
plated OK but anodes were falling apart. The substate was ceramic.
You cannot plate Alpha onto Graphite for some reason or other.
What is your substrate and bath type.
Dann2 |
The substrate was Ti with some silver spots impregnated into it. The bath was a sodium plumbate bath just like quest used. The deposit was dark gray
very thin but it caught thee substrate pretty well. Ill try some beta over it as soon as ill get home.
quest: you don't need any alpha for your anode, just plate beta over your iron. I know someone who did it.
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dann2
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| Quote: | Originally posted by hashashan
The substrate was Ti with some silver spots impregnated into it. The bath was a sodium plumbate bath just like quest used. The deposit was dark gray
very thin but it caught thee substrate pretty well. Ill try some beta over it as soon as ill get home.
quest: you don't need any alpha for your anode, just plate beta over your iron. I know someone who did it. |
Hello Hashashan,
Did the Iron Substrate anode work for long when it went into a (Per)Chlorate cell?
Dann2
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hashashan
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The iron wasn't a substrate, It was later removed exposing a massive 5-7mm anode.
The cell was PH and temperature controlled for 6 days of slow deposition
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hashashan
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Well guys I think i've hit the jackpot. Still not sure though.
I took a piece of Ti, made some pitts in it with a hammer, plated with silver untill the holes were full, sanded the Ti untill the silver was only in
the pits, plated with alpha PbO2 after that with beta PbO2.
I tested it for 40 minutes in a NaCl solution with 4 amps, the current dropped a bit but i believe that it was because of bad contacts and
evaporation.
Ill check it in a full NaCl to NaClO4 cell and then ill post the results, Ill check one mole.
I belive that this concept of mine will work 
Sorry for no images .. they will come if the anode will be proved to produce perchlorate
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hashashan
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Update : Installed the anode in a NaClO3 cell. It works, but it seems like most of my silver pits were lost. The current isn't high only 4.5 amps for
a 20cm^2 anode ... which is really not enough.
Ill keep the electrolysis, the current is rising a bit hopefully it will hit the 5amps and last.
I guess the next update will be tomorrow.
5 minutes passed : too soon to be happy, a large chunk of the anode just cracked off. It still runs though.
I guess ill have to make holes through the Ti on the next try.
[Edited on 12-10-2007 by hashashan]
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dann2
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Silver (Per)Chlorate
Hello,
I would be inclined to keep away from Silver in the (Per)Chlorate cell.
Would there not be some risk or danger from Silver Chlorates and Perchlorates when products are being sued for Pyrotechnique purposes.
Actually I discussed this before and you said that since Ag
Chloride is insoluble all Ag ions will be ppt out of solution which was a good point.
Is there a risk from Ag with Chlorate and Perchlorate compounds in this situation do any of you guys know?
Still have not got back to the Anode stuff.
Cheers,
Dann2
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12AX7
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Copper isn't a hazard as near as I can tell. Sodium and potassium chlorate seem to be less soluble than those sorts of things, so it's difficult for
them to even form.
Tim
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hashashan
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I already discussed the silver issue with dann and explained to him that because both silver chlorate and perchlorate are soluble and the chloride is
not soluble there si no risk at all.
anode update: thje lead dioxide coating wasnt adherent enough and it passed away  ./
the dioxide just peeled off. I belive that next time ill have to make holes through the Ti this is very important.
question: what can i use as a surfacant to avoid bubles? I have never seen those matters that dann explains in his site, maybe there is a more common
name to those surfacants? where can I get them?
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dann2
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| Quote: | Originally posted by hashashan
question: what can i use as a surfacant to avoid bubles? I have never seen those matters that dann explains in his site, maybe there is a more common
name to those surfacants? where can I get them? |
If you cannot obtain surfactants you might try using mechanical movement to help eliminate bubbles.
Dann2
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hashashan
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I may obtain them but i have no idea where do you get them guys. Ant chance that they will be in a chem shop?
tried mechanical ... I used a magnettic stirrer but it just didnt knock off the bubbles
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Twospoons
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1: Photographic wetting agent, from a photographic darkroom supplier, used to prevent waterspots on film.
2: "Spray Stick" or similar wetting agent from garden shops, used to improve adhesion and wetting of plant sprays.
I'm sure I've mentioned these before.
You will probably still need some mechanical agitation for best results.
Helicopter: "helico" -> spiral, "pter" -> with wings
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hashashan
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Ill try to find those where I live.
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Twospoons
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Don't forget that if you add a surfactant you will have to deal with some foaming.
Helicopter: "helico" -> spiral, "pter" -> with wings
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hashashan
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So if there will be foaming, whats wrong with just soap?
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dann2
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Hello,
There will also be decomposition products from use of surfactants. I have no idea what theses products will be or how quickly they will form or what
effect they will have (or not have).
The original GSLD Anode patent discussed washing these's products out of tank efffluent using amyl (as far as I can remember) alcohol. This
complicated things.
Dann2
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Twospoons
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Soap will form insoluble crud with lead ions - the lead salt of the fatty acid. The surfactant is supposed to be a non-ionic surfactant, probably so
it wont react with the lead and drop out of solution!
Basically you are going to have to experiment with whatever you can lay hands on - mad science at its best!
Helicopter: "helico" -> spiral, "pter" -> with wings
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12AX7
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What of long alkyl quaternary amines?
Tim
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hashashan
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Experimentation is nice and all, but only untill it is getting close to lead salt spills.
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dann2
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Hello,
Total hair brained idea:
If you could connect a vacuum source to the plating tank and pull a vacuum every 5 minutes approx. this would get rid of bubbles. Far far too much
trouble and 'hassle' I would think.
If adding a Lead Compound to neutralize acid and replenish Lead ions that releases CO2, the tank contents are very much more inclined to foam up all
over the place if surfactant is used. A toxic foaming tide flows all over you bench if not controlled. Not a pretty sight.
Perhaps you can ignore bubbles forming on anode and let the Ti do its 'self healing trick' for any part of metal not covered with Lead Dioxide.
Another stunt that was spoke of in a patent was to add a quantity of glass beads to the plating tank and use stirring. The beads mechanically removed
bubbles forming.
US 4,026,786 (1977) I think was the patent.
also US 4,159,231
Dann2
[Edited on 17-10-2007 by dann2]
[Edited on 17-10-2007 by dann2]
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hashashan
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Glass what? what are those?
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Phosphor-ing
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http://cgi.ebay.com/PERFORATED-GLASS-SODA-LIME-BEADS-6-mm-CO...
These things or something similar.
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hashashan
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But wont such beads flying around in the solution with enough speed to knock off the bubbles hurt my anode?
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