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dann2
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| Quote: | Originally posted by Rosco Bodine
| Quote: | Originally posted by dann2
Why bother with a Co Spinel when the DTO will do on its own under LD?
Dann2 |
Because Co spinel appears to be a superior interface which gets past difficulties involved with ATO at the interface . It seems like you would be the
first person to understand this usefulness for all the problems that you have encountered with ATO as an interface material .
And why bother with catalytic baked coatings or PbO2
if all it takes to make perchlorate is ATO ?
@dann2 , please edit that attachment down to 550-600 pixels width so it doesn't foul up the page formatting .
X number of electrons flowing through Y amount of
resistance are going to dissipate the same net IR loss
no matter how you work the geometry you think applies ,
sideways, lengthwise , or through the thickness .
[Edited on 15-12-2007 by Rosco Bodine] |
Most of the problems I have had regarding DTO coatings were in relation to attempting to use Stannate (available to me, or variations using H202 to
get 'Stannic'), as opposed to Stannic from a jar. They are quite easy to do. My enitial failure with Stannic was using far far too much Sb (up in the
20's%) I think.
All attempts at using Stannate for me failed. I shall leave it to some one else more skilled in the art....
If it's an OTC argument then Cobalt wins no dought.
The DTO on it's own may be a good enough anode for Pechlorate. One successful run of a Perchlorate cell does not prove the anode is reliable.
It appears not to make Chlorate so well though as I cannot get a ppt from a Chlorate cell that I ran. Need to run longer I guess.
Will come back about the bulk resistance stuff........
Dann2
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Rosco Bodine
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It never hurts to have some backup options ,
alternatives , as a bit of insurance against becoming
one of these :
http://www.youtube.com/watch?v=7I2k3tITHzc
Here's some possibly interesting items ,
but I haven't read them yet
http://dx.doi.org/10.1016/S0378-7753(01)00620-6
http://dx.doi.org/10.1016/j.tsf.2007.01.042
[Edited on 16-12-2007 by Rosco Bodine]
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dann2
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Hello,
Can't watch video, too slow connection. Hope it's not something dogy.
The DTO is not difficult IMHO. All (as I said) of the 'messing' around is now over for me......I hope.
The resistance of DTO films on glass as shown in US 2564707 ( DTO on glass patent) are not relevent to making anodes IMHO.
The resistance look high when read from the graph, ohms, tens of ohms etc. This gives the impression that if a low Sb content
for the DTO is not chosen then there will be too much voltage drop/ power dissipation in the DTO coating on an anode.
The films in the patent are very very thin. Most of the measured resistances are from films of a unit square by 3870 Angstroms thick.
Thats 0.000387 micrometer thick coat!! A rather puny conductor.
The resistence is measure from one of the unit square end to the other end. This is like measuring gold leaf end to end only gold
leaf is far far thicker that theses films.
The resistance of the DTO coat 'seen' by the current leaving an anode is microscopic compared to the resistances in graph.
The bulk resistance was calculated for some of the examples. Thickness of film examples below are 3870 Angstroms.
Example 2: 1.5 % Sb-------> 17 ohms measured--------------> Resistivity of DTO = 6.58 x 10^-6 ohm Meters---> very small
Example7: 42.3% Sb----->104K ohms mesured----------->Resistivity of DTO = 0.04025 ohm Meters---->very small
Taking a one square cm on the anode (unit square) and assuming the anode DTO coat is 0.001 meters thick (a HUGH thick coat)
The resistance of this square from the point of view of the anode is
Example 2: 6.58 x 10^-9 ohms or 0.00000000658 ohms
Example7: 4.025 x 10^-5 ohms or 0.00004025 ohms.
Assuming a current densiy on anode of 0.2 amps per cm squared this will not represent a measurable volt drop or Power loss.
The Sb content of DTO should not be influenced on the notion of achieving 'minimum resistence' when making anodes.
The above is calculated from Resistence = Resistivity x Length/Area
As an illustration, the resistivity of DTO at approx. 2% Sb content is comparable to graphite but remember the current only has to travel though the
thin coating.
A 20% Sb DTO is comparable to, well, 20% Sb DTO, it will not 'drop' voltage.
Hope above is correct
Dann2
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Xenoid
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@ Rosco - I imagine you as the hirsutely challenged person on bass.... 
I recall being devastated when Simon & Garfunkel split up.... 
How old am I...?
[Edited on 16-12-2007 by Xenoid]
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dann2
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Hello,
and regarding the old well proven Lead Dioxide coat that will always work????????
That's the problem, ye old LD coat in *Amateur* circles has been a total failure IMHO. Sweet dam all people that I know of have got it to work on a
long term basis. Hopefully the DTO on Ti will change that.
Hope I am not insulting anyone here but LD up to this point has been a washout and I am talking about the last 10 years, not the last 6 months.
How old is THAT.
Dann2
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Rosco Bodine
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@Xenoid
I felt the need to have a cool breeze blow through and leave some extra cool across this page before I blow my own  Paul Simon seemed appropriate to the moment .
@dann2 , I get the impression there's nothing I can say here to get you to put together other information that
is well established , from sources beyond the few patents you seem to favor investing confidence as some singular truth , to see the larger picture
and draw your own conclusions . You are on a bandwagon there and along for the ride to wherever that confidence (bias) takes you .
There's different ways I have tried to cover this topic and provided references , but none of it registers with you as relevant , so you want to argue
the relevance . I don't . It distracts me from working the problems I recognize which you are certain don't exist , because we aren't even on the same
page concerning ATO , how it works , proportions , precursors , interpreting measurements ,
expected color indicators, ect . And when I give a valid
explanation which will withstand scrutiny you dispute it
not because you have different information but because
you believe having a different opinion somehow trumps
the data that tells a different story . This really becomes
tiring and frustrating and distracting .
I have no particular preference or bias and simply want
to go where the data leads in indicating higher art .
You act like there is some personal investment you have
which makes that somehow threatening , and that could only be because you have closed your mind and zeroed in on one possible solution you think is
*it* like there is
only one way to do this .
And just because your own experience with PbO2 has not been good doesn't mean that PbO2 isn't still the best
and most technically simple solution even if it requires
precisely controlled conditions to do right . If you will
get off this little ATO crusade and let the experiments
proceed in peace , then maybe a solution can be worked out that is more user friendly if not truly idiot proof .
A plausible process was worked out for massive PbO2
and that was no good , too complicated ....so what's
your solution, Titanium substrate , yeah boy that's it .
Just didn't notice that Ti is an exotic material and making use of it requires higher tech than what was causing failure and problems for the PbO2 ?
And now you still
likely have the PbO2 to deal with , only now it has a
high tech prosthesis for a backbone . Well damn if
folks just can't hack the massive PbO2 on iron in the
garage , lets fix that technical handicap by adding
complexity two magnitudes greater , and then bitch and whine incessantly about why it should be more difficult .
Let me ask you , are you enjoying playing a troll here
and continually shitting on good data ?
Why don't you go buy yourself a pound of platinum
instead of staying at me for a pound of flesh , because
in the world of technology I am an apex predator .
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dann2
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Hello,
| Quote: | Originally posted by Rosco Bodine
@Xenoid
I felt the need to have a cool breeze blow through and leave some extra cool across this page before I blow my own Paul Simon seemed appropriate to the moment .
|
Try the pills and Absolute ethanol, always works for me
You'll be looking for them after listening to that shit, .................(ONLY JOKING).
| Quote: | Originally posted by Rosco Bodine
@dann2 , [snip]
you are certain don't exist , because we aren't even on the same page concerning ATO , how it works , proportions , precursors , interpreting
measurements ,
|
My bottom line on the information for DTO for anodes is that I am much, much, much more inclined to follow DTO information that is presented in Anode
patents, as opposed to DTO information regarding applications for making resistors/conductors on glass and other non conductive substrates and other
time consuming speculation. I have deviated from known solutions in an attempt to use OTC stuff.
I cannot get Stannates to work. No anode guru has either, that I am aware of.
| Quote: | Originally posted by Rosco Bodine
And just because your own experience with PbO2 has not been good doesn't mean that PbO2 isn't still the best
and most technically simple solution even if it requires
precisely controlled conditions to do right .
|
Thats EXACTLY what I am trying to get away from.
Perhaps I will fail.
I am well aware of how to make Lead Dioxide anodes under well controlled more expensive conditions etc
(large tanks, lab chems. pumps, surfactants, bla bla bla).
Even managed to get a ceramic substrate anode to work for three months continous 24/7 (My claim to fame).
Ceramic substrate anodes are shit, far too fickle and too much trouble to make IMHO.
| Quote: | Originally posted by Rosco Bodine
A plausible process was worked out for massive PbO2
and that was no good , too complicated ....so what's
your solution,
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Cloth substrate anode
It is illuminating to note that no major manufacturer have touched massive LD Anodes for the past 40/50/60 years with a forty foot bargpole.
| Quote: | Originally posted by Rosco Bodine
Titanium substrate , yeah boy that's it .
Just didn't notice that Ti is an exotic material and making use of it requires higher tech than what was causing failure and problems for the PbO2 ?
And now you still
likely have the PbO2 to deal with , only now it has a
high tech prosthesis for a backbone . Well damn if
folks just can't hack the massive PbO2 on iron in the
garage , lets fix that technical handicap by adding
complexity two magnitudes greater , and then bitch and whine incessantly about why it should be more difficult .
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I shall purchase my Ti, not make it myself
The idea (as pointed out to you a long, long, long time ago here
http://www.sciencemadness.org/talk/viewthread.php?tid=2465&a... ) is that Ti is self healing/ self sealing. Hopefully (that's hopefullly. It may
not work) less demanding Lead Dixode plating conditions will produce workable, repeatable anode(s), it may not. Your opinion is that they will not
work (the Ti substrate ones). I intend to try.
| Quote: | Originally posted by Rosco Bodine
Let me ask you , are you enjoying playing a troll here
and continually shitting on good data ?
|
::Incert Simon and Carabunkle here, as a cooler::
The only reason for my last post was to give a blow by blow worked example in order to illuminate the (non) resistance problem.
| Quote: | Originally posted by Rosco Bodine
Why don't you go buy yourself a pound of platinum
instead of staying at me for a pound of flesh ,
|
| Quote: | Originally posted by Rosco Bodine
because in the world of technology I am an apex predator . |
.............or have I just been ravished by a dead sheep!
Dann2
P.S.
Please disregard all insults towards Simon or/and Garfunkle.
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Rosco Bodine
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| Quote: | Originally posted by dann2
Hello,
| Quote: | Originally posted by Rosco Bodine
@Xenoid
I felt the need to have a cool breeze blow through and leave some extra cool across this page before I blow my own Paul Simon seemed appropriate to the moment .
|
Try the pills and Absolute ethanol, always works for me
You'll be looking for them after listening to that shit, .................(ONLY JOKING).
| Quote: | Originally posted by Rosco Bodine
@dann2 , [snip]
you are certain don't exist , because we aren't even on the same page concerning ATO , how it works , proportions , precursors , interpreting
measurements ,
|
My bottom line on the information for DTO for anodes is that I am much, much, much more inclined to follow DTO information that is presented in Anode
patents, as opposed to DTO information regarding applications for making resistors/conductors on glass and other non conductive substrates and other
time consuming speculation. |
Yeah but the point here is that your inclination is *not*
science , but you keep arguing it as if it was . The amount of dopant which can be held within solution in the SnO2 ,
doesn't generally have one thing to do with the substrate ,
unless a significant amount of the substrate has itself mingled with the SnO2 to form a ternary system having enhanced cosolvent properties towards
the dopant .
Unlikely that this would happen with Ti , and indeed the
Ti and its oxides are known fillers for SnO2 . You are betting that SnO2 does the same thing to Ti oxides as does Ruthenium , and it doesn't work
that way . There's no
place for so much Sb dopant to go except to drop out as a separate phase , rupturing the lattice of the SnO2 , and in the process compromising greatly
both its physical integrity
mechanically and chemically and reducing its electrical conductivity . You miss the significance of the electrical
resistance measurements and what they indicate , where the values suddenly jump much higher is an indication where
the lattice is ruptured and you no longer have an intact
film . You think that data can just be ignored since the tests
weren't performed on a titanium substrate . You have a
microscope and an ohm meter , and it would be a real surprise if that data doesn't track parallel for the same film
on any substrates which have low solubility in the SnO2 .
| Quote: |
I have deviated from known solutions in an attempt to use OTC stuff. |
Did you quantify your components and keep careful notes of
tare weights for flasks , materials added , weights of residues , making the quantitative survey of the reactions needed to be able to predict what
you have as a result ?
Making your own reagents is not a matter of guesswork
when it is solutions that are being prepared , as opposed
to isolating solid end products .
| Quote: | | I cannot get Stannates to work. |
What stannates ? Are you speaking of the ammonium derivatives . And are you saying that the problem was in making them or that you made them okay but
in trying them they would not work ? Anyway many of the dopants in
the SnO2 are believed to exist in the form of stannates .
There is some basis in chemistry for that belief , so the the
extent that some of your Sb is in solid solution with SnO2
you may have to that extent actually made *that* stannate work , even if the other two from an ammonia solution were a problem
| Quote: |
No anode guru has either, that I am aware of. |
Your awareness is more anecdotal than analytical ,
and it takes a mix to do any fact checking . There are
other *anode specific* patents that put the Sb figure lower
and yet you seem to insist the more unsupported figure
has the greater probability of being correct . That's bias .
| Quote: |
| Quote: | Originally posted by Rosco Bodine
And just because your own experience with PbO2 has not been good doesn't mean that PbO2 isn't still the best
and most technically simple solution even if it requires
precisely controlled conditions to do right .
|
Thats EXACTLY what I am trying to get away from.
Perhaps I will fail. |
The same patent as was the basis for Alembics Ti substrate PbO2 anode used a DTO interface , and if the DTO interface
was "good enough" for a perchlorate cell as is , then why
bother to apply a PbO2 wearing coating ? And there's a whole slew of other patents that do the same thing , use a DTO on Ti substrate , and then a
jacket of PbO2 for the
operating anode coating . Did all of those inventors likely
miss the whole point that the PbO2 wasn't really needed ?
Do you think they were just going to a lot of extra needless work ?
| Quote: |
I am well aware of how to make Lead Dioxide anodes under well controlled more expensive conditions etc
(large tanks, lab chems. pumps, surfactants, bla bla bla). |
Being aware and delivering on performing the task correctly
are two different matters . Exacting work is just that .
| Quote: |
Even managed to get a ceramic substrate anode to work for three months continous 24/7 (My claim to fame).
Ceramic substrate anodes are shit, far too fickle and too much trouble to make IMHO. |
There you go again . Suppose someone else using a different ceramic and a different technique had good results ,
then what ? There may just be a niche set of conditions and materials that will work fine , and everything else is shit ,
and your tests were not in the same range of conditions .
| Quote: |
| Quote: | Originally posted by Rosco Bodine
A plausible process was worked out for massive PbO2
and that was no good , too complicated ....so what's
your solution,
|
Cloth substrate anode
It is illuminating to note that no major manufacturer have touched massive LD Anodes for the past 40/50/60 years with a forty foot bargpole.
|
Assuming that's correct , does it mean that the thousands of tons of perchlorates made by the earlier methods involves
a less attainable technology , than the more modern commercial methods using more modern materials .
Often the latest greatest commercial method is the worst thing to try to duplicate as a small scale or improvised method . Newer is not necessarily
better , for a more primitive environment .
| Quote: |
| Quote: | Originally posted by Rosco Bodine
Titanium substrate , yeah boy that's it .
Just didn't notice that Ti is an exotic material and making use of it requires higher tech than what was causing failure and problems for the PbO2 ?
And now you still
likely have the PbO2 to deal with , only now it has a
high tech prosthesis for a backbone . Well damn if
folks just can't hack the massive PbO2 on iron in the
garage , lets fix that technical handicap by adding
complexity two magnitudes greater , and then bitch and whine incessantly about why it should be more difficult .
|
I shall purchase my Ti, not make it myself
The idea (as pointed out to you a long, long, long time ago here
http://www.sciencemadness.org/talk/viewthread.php?tid=2465&a... ) is that Ti is self healing/ self sealing. Hopefully (that's hopefullly. It may
not work) less demanding Lead Dixode plating conditions will produce workable, repeatable anode(s), it may not. Your opinion is that they will not
work (the Ti substrate ones). I intend to try. |
No it isn't my opinion at all that the Ti substrate anode won't work . In fact it is my opinion that not ony Ti but other substrates are also operable
. And I am fully aware of what
valve metals are , as well as why they are deemed to be necessary as substrates for anodes .....it is all about
*Porosity* . If the substrate could be 100% effectively sealed , hermetically sealed beneath the anode working coatings .....then ANY conductive
substrate could be used ,
and no valve metal would be required , for passivation
to seal off the defects , the pores , through which corrosive
electrolyte makes it way down to the substrate .
It is *precisely* my understanding of this parameter which
accounts for my emphasis upon the critical importance of
the integrity of the films of SnO2 , and causes me to cast a
discerning eye at the composition of those SnO2 films ,
for *optimizing* the imperviousness of those SnO2 layers
which are nearest to the substrate and serve as its protection from chemical attack . It only makes *good sense*
to optimize the film strength and chemical and electrical properties of the near substrate SnO2 layers . The outer
layers where the catalytic materials are tasked differently ,
can be more porous , indeed may even have greater catalytic effect and be better at their specialized task when made porous deliberately . But for
the near substrate lower layers that porosity is an anode killer . I don't know why you can't seem to understand that this is true . Isn't it
somewhere in the patents , explained how these composite layered anodes are supposed to work , and doesn't what I am describing fit that explanation ?
So why would you think
an SnO2 interface layer having a ruptured lattice from excessive doping would be desirable ? It doesn't make sense .
One thing that does makes sense is that thinner catalytic coatings , and thinner layers of PbO2 can be used on a
conductive ceramic seal coated metal substrate , since the substrate provides strength . And as I have said , some of the patents have said also ,
*if* the integrity of the sealing
coatings can be made perfect , then any metal can be used for a substrate , copper and aluminum , even iron . The
technology necessary is in the coatings and the interface ,
for both the requirements of what substrate can be used ,
as well as for what wearing coatings go on the outside
and have good efficiency at producing perchlorate .
| Quote: |
| Quote: | Originally posted by Rosco Bodine
Let me ask you , are you enjoying playing a troll here
and continually shitting on good data ?
|
::Incert Simon and Carabunkle here, as a cooler::
The only reason for my last post was to give a blow by blow worked example in order to illuminate the (non) resistance problem.
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It is not a resistance problem per se , it is what the sudden increase in resistance at a certain composition indicates
is occuring , a rupturing of the SnO2 lattice from oversaturation of the SnO2 solid solution , compromising the
physical and chemical , structural integrity of the layer .
The sudden jump in resistance is a marker that something
else bad has happened , worse than just the electrical degradation which is only the tip of the iceberg .
| Quote: |
| Quote: | Originally posted by Rosco Bodine
Why don't you go buy yourself a pound of platinum
instead of staying at me for a pound of flesh ,
|
| Quote: | Originally posted by Rosco Bodine
because in the world of technology I am an apex predator . |
.............or have I just been ravished by a dead sheep!
Dann2
P.S.
Please disregard all insults towards Simon or/and Garfunkle. |
Beware of the jaws . I like trolls cause they are crunchy. Hopefully we are on the same page now . Please don't come back with more of the ATO is
magic at 16% stuff ....
as an interface . Prove it first , because the bulk of the references indicate that is simply not likely at all to be true .
[Edited on 17-12-2007 by Rosco Bodine]
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dann2
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Hello,
| Quote: | Originally posted by Rosco Bodine
Beware of the jaws . I like trolls cause they are crunchy. Hopefully we are on the same page now . Please don't come back with more of the ATO is
magic at 16% stuff ....
as an interface . Prove it first , because the bulk of the references indicate that is simply not likely at all to be true .
[Edited on 16-12-2007 by Rosco Bodine] |
Certainly not, the 16%'s a bit low!
When I say Stannates I meant SnCl2 as opposed SnCl4.
Where are the anode patents that extol the virtues of low Sb content? (no conductive/resistive coats on glass patents, or battery or capacitor etc
pats)
There are no sharp changes in the resistance curve in the patent we are discussing above. A smooth curve all the way.
Did you read col. 6 line 0 regarding thick coats of DTO.
Regarding LD on top of the DTO. If DTO proves to be a reliable 'holy grail' anode I will not be going near Lead Nitrate. I have me doughts.
Sorry about this but that's all I have time for.
Cheers,
Dann2
Long live the Diamond Shamrock patents.
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Rosco Bodine
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| Quote: | Originally posted by dann2
(snip)
When I say Stannates I meant SnCl2 as opposed SnCl4. |
That is Stann(ous) for the +II valency and
Stann(ic) for the +IV valency .
Stannates are generally substituted bimetal oxides of the
+IV stannic oxide ....a whole different thing .
Like zinc stannate for example .
| Quote: |
Where are the anode patents that extol the virtues of low Sb content? (no conductive/resistive coats on glass patents, or battery or capacitor etc
pats) |
I don't recall the numbers right now but I have posted them
before and cited them in response to this exact same discussion about three iterations back and that's precisely why I am losing patience with this
argument . It was studied
in the early ruthenium doping related patents where Sb
was being investigated , and there were several references
where the maximum solubility of Sb was identified as ~8%
and the optimum was somewhat less IIRC , and those references were exactly why several of us said that 95/5 solder was good enough , as it was sort of
intermediate
in the useful range for Sb to Sn . It's not going to change
if you keep repeating the same old stuff .
| Quote: |
There are no sharp changes in the resistance curve in the patent we are discussing above. A smooth curve all the way. |
Evidently we aren't looking at the same graph .
Col. 5 line 25 is where you need to read .
| Quote: |
Did you read col. 6 line 0 regarding thick coats of DTO.
|
Yes I did and I already answered this too when you brought it up before , You are beating a dead horse .
| Quote: |
Regarding LD on top of the DTO. If DTO proves to be a reliable 'holy grail' anode I will not be going near Lead Nitrate. I have me doughts.
|
Your doubts that the intermediate layer will be a satisfactory working anode are well founded doubts , because if the
DTO was a satisfactory working layer then there would have been no need for additional coatings as working coatings ,
which have some acceptable efficiency as producers of perchlorate .
| Quote: |
Sorry about this but that's all I have time for.
Cheers,
Dann2
Long live the Diamond Shamrock patents. |
There's some useful information spread out among them ,
and some others too . Lets do good science here
and stop this opinionated unscientific rant . This subject
has been *covered* now for a third time in different threads .
Until there are some intelligent projections based on reported solubilities , oxygen overvoltage for certain dopants , catalytic information , good
experimental data or more specific references , can we please give this worn out subject of ATO dopant percentages a rest ?
[Edited on 17-12-2007 by Rosco Bodine]
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dann2
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Hello,
The patents that extol the virtues of low Sb content as on interface of LD and Ti, do not exist (unless something else is being use along with the Sb
+ SnO2).
All the Sn02 + Sb that I have seen use high Sb amounts. I have no plans to use Ru or other Nobles.
Regarding the 95/5 being 'good enough', it may well be.
Elecetic was using 95/5 because he can get that OTC. Perhaps (perhaps not) if he could get 90/10 or (dare I say) 82/18 he would use that. I do not
know exactly why he made the decision use 95/5, if it was science alone (and not the OTC argument) then, I guess, he agrees with you.
There is no Sb containing solder in my neck of the woods.
Regarding resistance of DTO. Col 5 line 25 says that the resistance changes rapidly so they need to use a log scale. They do not state that the reason
the resistance changes rapidly is that the DTO is going through phase changes. The DTO is I am sure going through phase changes. This info cannot be
gleaned from a resistance graph alone.
Are you saying that the resistance curve (smooth) tracks phase changes that occur as we change Sb content? I do not believe it does.
| Quote: |
Your doubts that the intermediate layer will be a satisfactory working anode are well founded doubts , because if the
DTO was a satisfactory working layer then there would have been no need for additional coatings as working coatings ,
which have some acceptable efficiency as producers of perchlorate .
|
What is acceptable to me and what is acceptable to industry is two very different things. DOT may (may not) suit the back yard brigade.
Magnetite suited the Japanese when graphite was scarce, it was not touched by others.
If a high Sb content for a DTO interface is good enough for the Diamond Shamrock people (assuming their examples are not downright lies) then it is
good enough for me to try, and I shall be doing so. You are going to have to grin and bare, clinch you teeth, think of England, etc, etc, while I
preform the operation.
I do not belive there is a 'best' percentage of Sb.
It is a compromise. I intend to follow the examples in the Diamond Shamrock pat's (the one's 'cobbled together to extract more money out of the
writers employers').
You do not think they will work. You may be right.
Dann2
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Xenoid
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@ Dann2
@ Rosco
This is the Co oxide (spinel) thread!
How about continuing this discussion (hopefully non-acrimoniously) in the Antimony/Tin Oxide thread;
http://www.sciencemadness.org/talk/viewthread.php?tid=8253
Or had you all forgotten about it?
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DerAlte
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Gentlemen, I have been following this and other similar threads on coated metal anodes. What exactly is your purpose in all this mainly fruitless
activity? To make a single purpose anode for chlorate production? A chlorate factory? I am sure you all know perfectly well that this can be done with
straight carbon anodes. Read 12AX7’s posts and see his neat and innovative high current cell and note his production numbers. Well, done, 12AX7,
though I cannot imagine why anyone wants that much! Even for pyrotechnics.
Like a good engineer he also has calculated his cost of production. Sure it uses up carbon. Carbon is cheap! The pyrotechnics boys have been doing
this for over 30 years, possibly longer. Certainly since the birth of the internet.
Although I very much admire the industry of Xenoid (where do you find the time and energy, X?) and it looks like he is close to some sort of success,
is it really worth all this effort? The efforts of Dann2 and jpsmith are also noteworthy.
I have given up reading Rosco’s verbose and repetitive posts in this thread. Apart from being difficult to follow and with endless references to
(probably) useless patents, he has a fixation with spinels, to me merely a class of minerals. Lord help us if he gets on to perskovites… Call them
mixed metals oxides, MMOs. A monometal spinel? That one got me until I realized he meant Co3O4 (I think – it’s difficult to follow his acrobatic
mind).. Magnetite is classed as a spinel mineral, IIRC. But are these MMO coatings really spinels?
I realize that the holy grail of all this is probably perchlorate, and agree that is a horse of a different color. But even perchlorate can be made
with carbon anodes. Do not imagine that the same cell structure and conditions work for both. I have made both using carbon, some ten years ago being
the last time. I still have a few ounces of both but haven’t made any since, but feel tempted to try again – using naked carbon anodes... I am a
heretic. I see I am in danger of going OT here, so enough. If anyone is interested in good old carbon, I’ll post my thoughts somewhere more
appropriate.
Rosco, if you kept your posts shorter and with less repetition, maybe you could impart something useful to the experimenters. I am no judge but it is
easy to be a critic.
Regards, Der Alte.
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Xenoid
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@ DerAlte
This is true SCIENCE MADNESS...
Personally speaking, I am finding this quite an interesting endeavour, and thoroughly enjoying myself.
Here in NZ I have to import genuine graphite anodes from the US, the postage, etc, etc costs 5 times the price of the graphite. Gouging rods work, but
they disintegrate fairly quickley, and introduce all sorts of colloidal contaminants.
The dream of going directly from salt to perchlorate with a perfectly clear solution, and anodes that only need replacing say once per year is highly
desirable. After experiencing the simplistic beauty of a perchlorate cell using a platinised Ti anode and Ti cathode, there is no going back (well,
with the exception of my 10 litre bucket cell, that is) for me!
DerAlte, I touched on this in an earlier post (and someone please correct me if I am wrong) but industry does not particularly need a anode (even a
fairly efficient one) that goes from salt to perchlorate. They have ultra efficient - long lived chlorate anodes, and the same for perchlorate. The
chlor-alkali industry is huge, the perchlorate small, they can use cheap chlorate for feedstock.
It seems to me that there is a lot of scope here for the amateur to try all sorts of things and even if a "holy grail" anode is half as efficient and
has 1/10 the longevity of an industrial process it doesn't really matter.
Remember high temperature superconductors - who would have thought that, mix a witches brew of oxides together and bake in an oven.
If it proves possible to develop an anode that can be made simply, by baking a few coats of easily obtained materials on to it, why would any one want
to go back to gouging rods or even graphite!
If we were to follow your line of reasoning we would still be listening to the radio using a cat's whisker and a galena crystal, it works, but not
particulary well....
Oh, I thought of another, people were using candles to make light for centuries and they thought it was a really great way, until along came the
incandescent, then the fluorescent and now the white LED. I know which process I prefer when trying to drill a hole in titanium, and it isn't a
candle!
[Edited on 17-12-2007 by Xenoid]
[Edited on 17-12-2007 by Xenoid]
[Edited on 17-12-2007 by Xenoid]
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chloric1
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@Der Alt-I have read your post before making perchlorate via carbon. If thats working to your satisfaction then great. This August/September was my
first time making chlorate electrolytically. As much as I derived satifaction from it, I could not stand all the gunk and debris. I managed to
obtain pure white chlorate after performing a number of filtering and purification parlor tricks but knew there was something better so I quit
temporarily with my 700 or 800 grams of sodium chlorate. I feel Xenoid is on the same boat with me by hating the ridiculous crud. He is nothing less
than inspiring especially considering Rosco's knowledge and perspective. Strangely, Roso spends so much time bashing dann2 yet I cannot remember
seeing any actual working anode from him. It is not easy to experiment when one has so many obligations but I digress, some just talk alot.
@Xenoid-well got the heat gun now just need to prepare the precursor cobalt nitrate, nicke nitrate, and manganese nitrate. I have some bismuth metal
if I can find it. Would like to make some bismuth nitrate soup So how is
Gerty doing? Do you still have some lithium perchorate thing running?
[Edited on 12/17/2007 by chloric1]
[Edited on 12/17/2007 by chloric1]
Fellow molecular manipulator
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Xenoid
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| Quote: | Originally posted by chloric1
@Xenoid-well got the heat gun now just need to prepare the precursor cobalt nitrate, nicke nitrate, and manganese nitrate. I have some bismuth metal
if I can find it. Would like to make some bismuth nitrate soup So how is
Gerty doing? Do you still have some lithium perchorate thing running?
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Chloric - I have had to take a break (at the risk of divorce).
1) The 4-coat Co-spinel anode has finally passivated after 11 days in a chlorate cell.
2) Li (per)chlorate cell is still bubbling away, I added some more water this morning. I don't have a clue what it's doing or how long it will last!
3) "Gerty" is sitting on a bench, still awaiting a perchlorate catalytic outer coating! I plan to add several coats of Sb doped beta MnO2. I am about
to make, hopefully some Sb nitrate (dissolve Sb2O3 in excess cold, conc. nitric acid).
4) I have obtained some iso-propyl alcohol to improve coating technique.
5) I have made some Pb nitrate which is crystallising at the moment.
6) I have sourced some 99.99% Bismuth here in NZ. I first checked Bi shot at sports shops, minimum purchase was 3Kg for a couple of hundred $$$s..
I have now found some for about NZ$40 per Kg but the company has closed down for Christmas and will not open again until January 7th... (Hey, this is
NZ).
7) I am making another Chlorate cell using two of my MMO (RuO2/TiO2) chlorinator cell electrodes just to try them out!
8) I am stll not divorced...
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chloric1
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Amen- Can't live without my wife and 2 year old but experiementing is definately frowned on here. I need to sell some of my anodes just to keep
things in check. Told her I would use the heat gun to remove the death gray ugly paint off the kitchen cabinets. Need to buy the scraper though. I
did prove to her how useful this gun is. Yesterday, the back gate lock was encased in ice and not only did I defrost it but heated bone dry! The
relentess snow and ice has hampered my efforts immensely. I forgot my barium nitrate on my bench and it is covered in 12 centimeters of snow. It
might be 2 degrees Celsius tommorrow. That is when I will reclaim my barium and at least react some cobalt sulfate with baking soda to get the
carbonate. If I have enough beakers available I will try some soda with some nickel sulfate. I will be about 15% where I need to be but at least it
is a start. I like summer better for comfort but winter is nice because the air is cold and dry. Great for crystalizing things!
Fellow molecular manipulator
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dann2
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Hello,
@DerAlt
Thanks for the compliment.
You have "given up reading Rosco’s verbose and repetitive posts"
I presume you are still reading my verbose and repetitive posts, eh
Regarding the Perchlorate with Graphite. I am a 100% 'doubting Thomas' when I hear of Perchlorate made with Graphite. Did you ever try a conc.
sulphuric acid test on a 50/50 mixture of your Perk. + sugar. Use eye protection. Perhaps I asked you this before.
There are lots of accounts on the net showing great yields of Perchlorate from Graphite. The vast majority of them all stem from the one source 8/9
years written by a guy who has since admitted it was bullshit. I have not been able to make it in any sensible fashion or yield with C.
Roscoe posted a patent some time ago showing a cell with C and a diaphram. It would be a very interesting project IMHO.
http://www.sciencemadness.org/talk/viewthread.php?tid=8592&a...
Since this is a Co Oxide thread...................
My Co Oxide anodes are still going OK. Only two days so they have only started.
The DTO in Lithium Cell still OK, need to check for Perk. I need to see if the Perk. is forming yet (easily) as per the patent.
The DTO in Na Perk. cell has run now for 14? days. 'Run Time' of cell is 10 days.
I want to titrate the Chlorate to see if DTO can reduce the Chlorate level down to where it is sensible to simply take the liquid from cell and
destroy all residual Chlorate to get pure Perk.
@Roscoe Perhaps a wee bit of indulgence was engaged in but I have to confess I did enjoy it!!!
Dann2
Totally, absolutely and completely relaxed communication with his fellow communicators in the Co Oxide thread.
http://i168.photobucket.com/albums/u200/anodes_2007/smash2vu...
p.s. Though shalt not speak ill of the Diamond Shamrock patents.
[Edited on 18-12-2007 by dann2]
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Rosco Bodine
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| Quote: | Originally posted by DerAlte
I have given up reading Rosco’s verbose and repetitive posts in this thread. Apart from being difficult to follow and with endless references to
(probably) useless patents, he has a fixation with spinels, to me merely a class of minerals. |
It's way more than patents that are the basis for my studies of this subject . It isn't me who is FIXATED on one ambiguous reference and trying to
redefine science using that dubious information as a guide .
Merely a class of minerals ? If you read the patents and journal references you think are useless you wouldn't have that oversimplification
as your confusion . It is the notable electrical and chemical properties of certain ones which makes those particular ones interesting , along with
the fact that they can be readily made at relatively low temperatures from fairly common materials . All of that
makes these materials pertinent to experiments concerning
the making of a durable and efficient perchlorate anode .
| Quote: |
Lord help us if he gets on to perskovites… Call them mixed metals oxides, MMOs. A monometal spinel? That one got me until I realized he meant Co3O4
(I think – it’s difficult to follow his acrobatic mind).. |
Oh yes I'm really turning somersaults trying to hijack a focused thread with meaningless anecdotal bullshit
masquerading as science , whilst at the same time trying to
sort out the mystery of valency hierarchy indicated by
3rd grade science class suffixes like "ic" and "ous" .
Yeah I'm really the one that's lost here and out of my element huh .
A debate and discussion is an exchange of information .
An argument is generally just an exchange of ignorance
and a waste of time .
| Quote: |
Magnetite is classed as a spinel mineral, IIRC. But are these MMO coatings really spinels? |
Not the entire composite no , just the interface and
some other components .
| Quote: |
I realize that the holy grail of all this is probably perchlorate, and agree that is a horse of a different color. But even perchlorate can be made
with carbon anodes. Do not imagine that the same cell structure and conditions work for both. I have made both using carbon, some ten years ago being
the last time. I still have a few ounces of both but haven’t made any since, but feel tempted to try again – using naked carbon anodes... I am a
heretic. I see I am in danger of going OT here, so enough. If anyone is interested in good old carbon, I’ll post my thoughts somewhere more
appropriate.
Rosco, if you kept your posts shorter and with less repetition, maybe you could impart something useful to the experimenters. I am no judge but it is
easy to be a critic.
Regards, Der Alte. |
I was *very focused* on the subject of this thread until
it was hijacked for the satisfaction of someones ego
who wants to make this thread about something else .
It would please me to resume that focused task on which I was working , if left to that task instead of being distracted with the breach of decorum by
someone who seems intent on diverting this thread .
I want to do science here , not arguments about off topic
nonsense involving the percentage content of Sb in ATO .
This *is* indeed the cobalt oxide anode thread , and I would much prefer the topic had never changed . I was the person to first post concerning the
possible usefulness of cobalt in this endeavor as an alternative interface material , and possibly having greater value as well . For several months
I have been thinking about ways to make use of the material .
If you have something constructive to add in this thread or
any other I am always happy for the sharing of information .
And I promise , we won't have to cover the same thing in
different threads , several different ways for either of us
to "get it" . If you tell me something I don't understand ,
I'll do more reading till I do understand , instead of arguing with you pretending to know something I don't .
[Edited on 17-12-2007 by Rosco Bodine]
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chemoleo
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Ok let's stop it right there and get back to the topic of this discussion - cobalt oxide anodes!
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Rosco Bodine
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Bismuth Oxide catalytic anode coating
Okay , back on topic , resuming with prior business
of interest before the unfortunate detour occurred ....
think *bismuth* is a possible catalytic oxide coating ,
which seems "most likely" among those three possibles
listed in the MnO2 patent which claimed such unusual
efficiency in perchlorate production .
Bismuth has been mentioned in several perchlorate anode related patents as useful , specifically as a coating catalyst for perchlorate anodes . If
had to put money
on the most likely one of the three As , Sb , and Bi ,
my money is on the Bi .
Curiously , bismuth nitrate also undergoes pyrolytic
decomposition to form an adherent film , similarly
as does SnO2 , and at a lower temperature it can even
be applied by spraycoat pyrolysis or by other methods .
It may possibly serve as working anode outer layer
alone . I am accumulating references and trying to
formulate a plan . Will post anything pertinent that
I find .
Here's something interesting as a possible filler
and final coating component
50nm microcrystalline Bi2O3 at 100C
http://dx.doi.org/10.1016/j.matlet.2005.03.037
[Edited on 17-12-2007 by Rosco Bodine]
Attachment: Bismuth Nitrate spray pyrolysis film.pdf (101kB)
This file has been downloaded 1148 times
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Xenoid
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@ Rosco, I will have to try Sb for the moment and even that is proving difficult. I wont have any Bi till the new year!
Regarding the 4 - coat Co spinel anode chlorate cell. It appears to have produced a considerable amount of chlorate. I put a few mls of solution in a
test tube and added a little saturated KCl, there was immediate fine crystalline precipitation. I put it in the fridge and the solution is now about
half crystals...
I've also checked this for perchlorate, but as might be expected it is absent!
[Edited on 18-12-2007 by Xenoid]
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DerAlte
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Apologies for butting in above.
@Xenoid – I understand –it’s like climbing mountains – because they’re there. Go to it! The filth the C anode produces is about as bad as
manganese dioxide– but you know all about that too.
@Dann2 – you’ve got me worried. I am going to check the old bottle with white powder in it to see whether it is perchlorate or bullshit.
@Rosco – no offense, just a small dig. You do tend to get a bit verbose, though!
Butting out, but reading with interest,
Der Alte
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The_Davster
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I wonder if bismuth subnitrate in a nitric acid solution could suffice in that paper you posted Rosco? Bismuth subnitrate is common and decently
priced at pottery stores, I have a half pound of it that I ordered a while ago.
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Xenoid
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| Quote: | Originally posted by The_Davster
Bismuth subnitrate is common and decently priced at pottery stores, I have a half pound of it that I ordered a while ago. |
Yes! I inquired about this a while ago at my local pottery place. My tame pottery supplier said it was now listed as a hazardous substance (OMG - it
has NITRATE in the name). I should make further inquiries I suppose. He said there was someone around here who was using it. It produces spectacular
glaze effects!
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