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Author Topic:   Anodizing palladium ingot failure
malaci
Hive Bee
posted 11-18-1999 01:20 PM     Click Here to See the Profile for malaci      Reply w/Quote

What are some problems anodizing?
Has anyone had problems with
getting their palladium
blackened.The electrolyte is 100ml
dh20 and 5ml of 96% reagent
sulfuric acid.It seems like the
edges of the palladium get
blackened pretty good but the face
has a rainbow looking color to
it.Is the whole palladium ingot
suppose to turn dark black or just
the edges and a lighter
discoloration on the face?

Wizard X
PimpBee
posted 11-18-1999 08:09 PM     Click Here to See the Profile for Wizard X      Reply w/Quote
Don't be overly concerned if all the Pd ingot isn't black. Pd-H2 surface saturation is required.

malaci
Hive Bee
posted 11-19-1999 05:48 AM     Click Here to See the Profile for malaci      Reply w/Quote
Doesn't pd hold hydrogen without anodizing and putting the palladium black oxide on it's face?I heard pd holds 900x it's weight with hydrogen is this correct.

aquaticZX
Hive Bee
posted 11-19-1999 11:48 AM     Click Here to See the Profile for aquaticZX      Reply w/Quote
Just the edges should be black in that part of the procedure. It's a surface-area related phenomenon. The edges are the easiliest(or more prominantly) attacked surfaces. It shouldn't affect the reaction at all.

readyeddie
Hive Bee
posted 11-20-1999 08:28 AM     Click Here to See the Profile for readyeddie      Reply w/Quote
Malaci take a torch to your pd ingot for about ten seconds on each side this will burn the poisons out of the metal.It should be done once in a while you know.For the anodizing it does not have to be very black the edges will but the face no.Fester says that the anodizing increases the palladiums ability to absorb hydrogen you understand and get something on your eyes you hear.

FreeFlow
Hive Bee
posted 11-20-1999 01:40 PM     Click Here to See the Profile for FreeFlow      Reply w/Quote
I would not even consider this meterial if I was you.......leave it for industry

Does only one thing last a while sucks up electrons, when dried out these ellectrons can attract hydrogen in the air and also oxygen then as a result explosion....

Um it could even consider this the umm worst meterial to choose from really

DickWad
Hive Bee
posted 11-20-1999 03:08 PM     Click Here to See the Profile for DickWad      Reply w/Quote
Whoops, is that U freeflow?

OU812
Hive Bee
posted 11-26-1999 08:12 PM     Click Here to See the Profile for OU812      Reply w/Quote

I have a problem with the palladium getting black also the corners do but that is it.I turn up the volt to about 3amps to try to get a better black surface and i'll be damned if all the black comes off and turns the electrolyte a dark color.Why couldn't you just flame the damn ingot with a torch to get it black then charge and so on.

Uncle Fester
Hive Bee
posted 11-28-1999 04:06 PM     Click Here to See the Profile for Uncle Fester      Reply w/Quote
Here's what I've seen. The acid solution can dissolve off the blackened surface if it isn't anodized hard enough. It will dissolve off,turning first brown, then dissappearing. It can be gone in the length of time required to switch around the wiring. I prefer to anodize nice and hard, seven volts drawing around 3 amps. This gives a surface more intensely black around the edges of the ingot, but noticably and definitely black on the forward face as well. Then I pull the ingot out of the acid while switching around the wires. Then I come at it with around an amp with the Pd as cathode for a minute or so before dropping down the current, and adding ester mixture. Then the blackening won't dissolve. Pd in solution isn't a problem anyway, but I thought I'd pass it along. You know, if one wishes to scale up, that ingot dissolves nicely to PdCl2 in HCl at a current of one half to one amp. Condom cell divider is required because H2 will sludge out PdCl2.

OU812
Hive Bee
posted 12-18-1999 10:56 AM     Click Here to See the Profile for OU812      Reply w/Quote
What the fuck???Fester i took your advice on anodizing harder at 7 volts around three amps still no luck.The palladium metal i have is around 6 1/2 square cm and 1mm thickness.When i first got it it anodized pretty good.Could it be possible that the metal is poisoned and no longer any good or could their be some kind of plaque plating on the suface keeping it from anodizing?I tried to anodize it and then charged it took it out of the beaker and dried it off and took a lighter to it and it did burn like hydrogen was present.The H2SO4 is ACS 95-98%.The anode is lead it's 4 inches long and about a quarter inch wide and 2mm thick.

Uncle Fester
Hive Bee
posted 12-19-1999 02:58 PM     Click Here to See the Profile for Uncle Fester      Reply w/Quote
You say it used to anodize well, but now it gets nothing on the surface. That's really interesting. If I had that ingot, I would sandblast the surface lightly to expose some fresh metal, or dip into nitric for a couple of minutes then rinse to expose a fresh layer of metal.

readyeddie
Hive Bee
posted 12-19-1999 03:38 PM     Click Here to See the Profile for readyeddie      Reply w/Quote
OU812,I know someone that had this problem and the answer was the condom did not have enough electrolyte.Add more electrolyte to the condom to really get things flowing.You may also want to add a few drops more of H2SO4 to it as well.Are you using lead or a battery carbon rod for the anode?

Huffalump
Hive Bee
posted 12-19-1999 04:34 PM     Click Here to See the Profile for Huffalump      Reply w/Quote
If you don't have a sandblaster or nitric acid, you might want to try a bit of emery paper.

Electro_Dreamer2
Hive Bee
posted 12-20-1999 10:57 AM     Click Here to See the Profile for Electro_Dreamer2      Reply w/Quote
Some palladium is different than others.Check your sulfuric acid solution in the condom to make sure it is of the right level.Sand off the face to a fresh layer then soak in HCl solution for 30 min.Now take a torch and flame it for a few seconds on each side.If you still have problems getting it to anodize let it run until it does get black but keep you voltage down.You don't want your sulfuric acid solution getting hot.

------------------

You can't play the game if you don't know the rules!!!


OU812
Hive Bee
posted 12-20-1999 07:54 PM     Click Here to See the Profile for OU812      Reply w/Quote
Thanks readyeddie & Electrodreamer2
between both of your replies i got it
to anodize.One of the problems was
not enough solution in the condom.The
ingot turned all different colors but
mostly brown when wiring was turned
around all the colors came off but a
black surface.So i guess this is what
i'm looking for right?

Dextracyclins
Hive Bee
posted 12-20-1999 08:10 PM     Click Here to See the Profile for Dextracyclins      Reply w/Quote
Did ya come to cause problems or look to soulution to problems????? I have now learned that um the most obvious failure is in fact failure to conduct electricity See that acedic acid is a very weak electrolyte it does not conduct electricity it therfor could be related to the fact tht the acid the sulpheric acid is goofing it up, ya off course need this acid to conduct any electricity, this might ya might simply start however with a more available counter acid such as thiosulph this will infact produce your desired end result in the acid sulpheric acid that is but umm well adding some carbon should help at least some humm not a bad idea however it the co levels in the solution as the result of an incompleat consideration such as to the basic necessity of order in such a reaction has not been dealt with I do not belive in santa cluase neither though it is a ???

Zion
Hive Bee
posted 03-23-2000 10:49 PM     Click Here to See the Profile for Zion      Reply w/Quote
Very interesting. Is the strength of the electrlyte related to the sIze of the metal
surface or the amount of amps needed, or both?

malaci
Hive Bee
posted 03-23-2000 11:32 PM     Click Here to See the Profile for malaci      Reply w/Quote
No the electrolyte should be just right electrolyte to week will have week current flow.Electrolyte to strong will cause the palladium black oxide to come off or dissolve off your ingot when the wires or turned around.You want to keep the electrolyte around 3-5%.

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