IrC
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Palladium on Carbon
I was wondering if anyone knows of a good method to plate Palladium onto a carbon rod. I am looking for an electrochemical method hopefully involving
Palladium Chloride and Palladium foil and/or Palladium metal pieces (as this I have). Other methods are of interest as well from an informational
standpoint. I want to use a method that is not too expensive (I do not have the equipment to accelerate ions in a vacuum), and preferably a method
that is not too chemically hazardous as well. Also I would like to have a fairly thick Palladium layer, as I am not interested in a catalyst but
rather absorbing Deuterium from D2O.
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chemoleo
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Here is a prep I have found (from the Hive for palladium-activated charcoal, I imagine one can use it (possibly less efficiently) on a carbon rod as
well. If it is an absorption experiment, wouldn't powder be preferred?
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18gr of Palladium on Carbon were prepared using following methode:
- 1,7 gr PdCl2 in 2 ml 31% HCl and 20 ml dH2O are heated for 15 min at 80°
- 20 gr activated carbon are heated with 450ml H2O and 15ml 31% HCl for 2h; the carbon is filtered off.
- the PdCl2 solution is added to 30 gr sodium acetat trihydrate in 200ml dH2O in a 500ml Flask
- the washed carbon is added to this solution
- hydrogenate the mixture for 3 hours, using a hydrogen generator producing 1mol of H2; don't forget to stir vigorously
- when the hydrogenation is complete and the carbon settles down you should have a colorless mixture with the catalyst at the bottom
- filter the carbon , wash it with 4-5*100ml dH2O; dry the catalyst at 50°
- I got 18gr (my filter methode wasn't good, use only glass no plastic, easier to clean) of 5% Palladium on Carbon. |
This however comes from unverfied sources, although people seem to have (successfully) used this very method. I am thinking that this could be adapted
to for your purpose.
Alternatively, of course you can do it electrochemically. The PdCl2 would have to be dissolved witith NaCl to form the soluble Na2[PdCl4] (i.e. 1.6 g
PdCl2, 1.1 g NaCl in 25 ml water, according to Brauer). Then electrolyse at low current (densities), using the carbon rod as a cathode. The Pd should
deposit. Low current because you want the plating to be slow and good.
This should be an easy experiment, because if it doesn't work as you wish, one can always redissolve the Pd with aqua regia, and recycle it.
However, Brauer also mentions the ability of Pd to take up hydrogen: On page 1727 it suggests to reduce the Na2PdCl4 with hydrazine or sodium
formate, a reaction that commences slowly at RT, and occurs rapidly at 50 deg C. By varying temperature, pH and concentrations, the Pd product can
have strongly differing surface characteristics.
When dry, the powder can take up 870-fold its volume of H2, when in aqueous suspension, it can take up 12000 times its volume in hydrogen!!
Anyway, as a result I am not sure whether this absorptive ability is present when electrochemically deposited onto a carbon rod. I think this ability
is the result of a massive surface area... which is hard to produce by plating.
Also, I'd suggest a literature search on the subject, for instance this article may give you some ideas.
[Edited on 8-3-2005 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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IrC
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Thanks, very helpful and interesting. I do have a bottle of 30% Pd on C so I would not need to make any that's for sure, but your ideas of
adapting have merit. You are right, revisiting cold fusion is what I am after. With Pd wires, the bulk of the mass is useless as the deuterium does
not migrate that far into the crystal structure. As expensive as this metal is it seems to me that gaining a large surface area while reducing the
metal mass makes sense, and the top of the carbon electrode is good for the connection, while carbon is fairly unreactive to most chemicals, in my
mind making this method a good choice. As far as I understand it is the crystalline structure, capturing a deuterium atom within a lattice cell, that
allows the deuterium to be soaked up within the metal. This makes what you mentioned of paramount importance, i.e., do you get a good crystalline
structure when plating electrically. Another avenue I am going to need to investigate further.
I also have another unrelated problem. How does one appear "well adjusted happy", as opposed to "mad scientist happy"? So far all
I am capable of is looking "mad scientist happy". (I am referring to a link I found on this site to the people in Oregon with a website on
chemistry)
[Edited on 9-3-2005 by IrC]
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HNO3
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HNO3 scratches head...EUUUUUUUUUUUUUUreka! Don't be a chemist!  Other than
that, I suppose you could alllllllways cut out the *I'm George Sorros, and I'm here to take over the world* type grin, and No don't
wear your facesheild and chemical resistant gloves in the store, even when your 100% nitric acid just corroded your homemade distillation apparatus
and released itself to wreak havok on your house, and you just found out that any base, salt, and your water was turned off because you didn't
pay your bills (because you were so busy with your experiments) during your
experiment, so it won't work. [/rant]
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