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plante1999
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Tutorial:the poor man MMO anode
The poor man MMO anode
Material :
Aluminium rod ,I us 3/8 inch, can be found in any hardware store.
Beaker:approx 150-250ml
Tin solder,can contain pb or sb,can be fond in any hardware store
Distilled water
Sulphuric acid 10%
Aluminium paper
Hydrochloric acid 30%
Power supply 1.5v 0.3amp
Steel wool
Piece of clothe
drill
acetone
torch
Chloride
Aluminium
Take 10ml of HCl and ad 30ml of distilled watter and drop aluminium in and wait.
Tin:
Take 50ml of HCl and ad an exess of tin metal , wait.
When your tin chloride is maked ad around 150ml of 10% sulphuric acid , a large amount of tin dioxide will be produce.
Take your aluminium rod and rub it with steel wool then rub it with acetone.
Mix 10ml of your al solution and 10ml of your tin sulphate solution and pour it on a piece of cloth.
Take your al rod and rub it with your cloth, than take your drill and insert the rod.
Take your drill lite your torch and turn the drill to on , and spin it over the flame with linary movment. Make this 10 or 11 time.
Then for protect your substrat take it in 10% sulphuric acid as an anode and apply 1.5 volt for 1-24hours.
Your poor man MMO anode is complete!
for who want to know this is about 2 mont of search about anode, specialy with otc equipement.for this anode the spining of the drill and the heating
uniformaly make a hard coat of Al + SnO2 when we make the electrolisis of sulfuric acid the Al oxidise to Al2O3.
Devlopement: find a way to better corode the al rod for better adherence, I am working on this, other devlopement will be a better ratio of AlCl3 and
SnSO4 , pulverising the mix with a pulverisator like windex, because we use a clothe, some of the coat, decape when the friction is to high, later I
will test all this think for a better coat , and a better price!
After 24hour in sulphuric acid solution the anode is dark gray,after this I made chlorate for abouth 2week without visible deterioration.the test
result show that this anode could work in all conssentration of nitric acid, all consentration of hydrochloric acid, just at 5% hydrofluric acid and
finaly all conssentration of sulphuric acid.in future I will test for hydrobromic , iodic acid.
[Edited on 22-1-2011 by plante1999]
[Edited on 22-1-2011 by plante1999]
[Edited on 22-1-2011 by plante1999]
[Edited on 22-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
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plante1999
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this is a picture of the first anode i made after2week of intense use in very corrosive media.
i dont know why it is black because tin dioxide and aluminium oxide is very white.I think a intermetalic compound have been formed, but this layer is
vey very very hard and chemical resistan.
[Edited on 23-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
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plante1999
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after some search i find it can be this: http://en.wikipedia.org/wiki/Aluminium_antimonide
because in my solder i ave 50% antimony. wath do you think.
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Xenoid
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Noooooooo...... . Surely it can't be as simple as this 
I can see how your coating is analogous to Beer's co-deposited, mixed crystal oxide coatings, RuO2/TiO2 on Ti (MMO).
You have SnO2/Al2O3 on Al. I believe the Beer system works, in part, because both RuO2 and TiO2 both have a tetragonal "rutile" structure. SnO2 also
has a "rutile" structure, but Al2O3 on the other hand has a trigonal "corundum" structure. Difficult to see how they would form a "solid solution".
I can also see how it might work in an oxidising environment, but I am amazed that it would last 2 weeks in a chlorate cell. Did it actually produce
any chlorate in this period. What voltage/ current were you using.
The grey/black colour may be due to the extremely small grain size of the coating material absorbing light rather than an antimony compound.
What is the flame temperature of your "torch", I assume you were heating the coated rod to about 500 - 600 oC.
Congratulations - this is an interesting development 
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plante1999
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Quote: Originally posted by Xenoid  |
I can also see how it might work in an oxidising environment, but I am amazed that it would last 2 weeks in a chlorate cell. Did it actually produce
any chlorate in this period. What voltage/ current were you using.
What is the flame temperature of your "torch", I assume you were heating the coated rod to about 500 - 600 oC.
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I run it at 3 volt 1amps.
I coated it at 600-800(my torch heat at 600to 1100degree c)
it producted arround 100 gram of potassium chlorate without degradation.
[Edited on 23-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
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plante1999
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so my first anode is a 15 day in chlorate cell. I make a TiO2 ,SnO2 anode with titanium trichloride and this anode show this apect:
anode: alumina/titania
conductivity:good/medium
chemical resistan:good/very good
hardness of the coat:epic/good
solubility:epic/good
so this is the test result i made with same conssentration of coating.
edit: I wanted to see ow much voltage the anode take a 3amps and at 8volt it deterior rapidili at 12 volt the coating flake of and lets appear
aluminium crystal.So dont do this with more than 5 volt.
[Edited on 23-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
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dann2
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Hello,
That's one for the patents no doubt.
Any chance of a clear picture of the Anode?
Dann2
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plante1999
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here a re-dimentioned picture.
later i will re-retake some picture of the 2 anode,titania and aluminia for demonstrating the variance of the 2 anode,some picture of the processe ,
more explanation and some improvement.
[Edited on 23-1-2011 by plante1999]
[Edited on 23-1-2011 by plante1999]
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plante1999
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Tutorial: the Poor man MMO anode V 2.0
This is the version 2 of the guide
there is the material:
Material :
Aluminium rod ,I us 3/8 inch, can be found in any hardware store.
Beaker:approx 150-250ml and 50ml
Tin solder,can contain pb or sb,can be fond in any hardware store
Distilled water
Sulphuric acid 98%
Aluminium paper
Hydrochloric acid 30%
Power supply 1.5v 0.3amp
sand paper corundum
Piece of clothe
drill
acetone
torch
First you need to pour 30ml of 30%HCl and ad tin solder.
than take 25ml of water and 25ml of HCl and ad an essess of aluminium to it.
Cut your alu rod to the heigth desired.
than run your drill and use a sand paper to corod it:
Optional:rub the alu rod with HCl , this step help to harden the coat.
than rub it with acetone.
ad per small amont 10ml of sulfuric acid 98% to the tin solution, it will boil very readily.
than soak your cloth with 50/50solution.
than rub your rod with it,heat it re rub it re heat it ect, here is a picture but you cannot see the flame.
repeat this until you think you have a hard layer.
ther is it!
to harden the coat electrolise as an anode a 10%sulfuric acid solution .
[Edited on 24-1-2011 by plante1999]
[Edited on 24-1-2011 by plante1999]
[Edited on 24-1-2011 by plante1999]
[Edited on 24-1-2011 by plante1999]
[Edited on 24-1-2011 by plante1999]
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Xenoid
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Well, this is all so easy, I have to give it a go....
The reactions;
Aluminium chloride hexahydrate decomposes above 300 oC. to give HCl, water and Al2O3
AlCl3.6H2O --> 3HCl + 4.5H2O + Al2O3
Tin (II) sulphate decomposes somewhere above it's melting point of 378 oC. to give SnO2 and SO2. How come this procedure was not mentioned in the SnO2
anode and SnO2 doping threads!
SnSO4 --> SnO2 + SO2
I have prepared AlCl3 solution by dissolving scrap Al in concentrated HCl. Careful the reaction is quite vigorous and gets very hot! The solution was
filtered hot and allowed to cool. The solubility of AlCl3 at 20 oC. is 45.8 g/100mls.
The tin (II) sulphate solution was prepared by reacting pure tin granules with hot copper (II) sulphate solution until the solution is colourless. The
solution was filtered and allowed to cool.
Sn + CuSO4 --> Cu + SnSO4
The solubility of tin (II) sulphate at 20 oC. is 18.9g/100mls.
I gather the coating process puts a conducting mixed metal oxide layer of Al2O3/SnO2 on the bare Al. The low voltage "annealing" process in the dilute
sulphuric acid then fills any cracks or weak spots in the coating with a layer of non-conducting Al2O3.
Well, I have had two attempts at this so far, both were total, unmitigated disasters.
Attempt 1. The Al rod was abraded with 150 sandpaper and etched with NaOH for 10 - 20 seconds, washed with water and wiped with acetone. The 50:50
coating solution was sprayed on using a small perfume sprayer, this produces too much coating, and after about 3 spray coats I had a thick, crusty,
crumbly coating that was a grey/cream/whitish colour. I removed some of the excess material by rubbing with a cloth, and proceeded to the "annealing".
Applying 1.5 Volts produced a current in excess of 1.8 Amps and increasing (the electrodes were close together, and the acid was not as dilute as I
thought it was). I reduced the voltage to 1.0 Volts and the current stabilised at about 1.5 Amps. The anode was bubbling away, producing copious
oxygen. Since it seemed stable, I left it for an hour or two, when I came back the container was filled with grey crud and the anode had been partly
eroded away!
Attempt2. This anode was pre-treated as above, but the 50:50 solution was applied by wet cloth, any excess was wiped off. At least 12 coats were
applied, with the rod allowed to cool between coats. This produced a coating of the purest, glistening, sapphire .... no, no, I digress. This produced
a silky looking coating, which was a clear/grey/creamy colour. I gave it a bit of a polish and with high hopes put it in the (now more dilute)
sulphuric acid for "annealing". This resulted in no current flow, right up to about 13 or 14 Volts. The coating was a very good insulator. This was
confirmed out of the cell with a multimeter.
The obvious difference in my procedure is the use of "pure" tin (II) sulphate, made from CP tin granules rather than solder, so perhaps the presence
of antimony plays a part here.
I used an old small wholly metal drill chuck, mounted in the "plasticky" chuck of my cordless drill. This avoids the possibility of melting the
plastic on modern chucks, as it gets pretty hot.
I await input from others, before proceeding!
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plante1999
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after your test , it show that antimony is probably the missing thing.
i will buy some pur tin and i will test tanks for the test i show to me that i need to change mi recipe.
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plante1999
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| Quote: Originally posted by Xenoid | Well, this is all
I have prepared AlCl3 solution by dissolving scrap Al in concentrated HCl. Careful the reaction is quite vigorous and gets very hot! The solution was
filtered hot and allowed to cool. The solubility of AlCl3 at 20 oC. is 45.8 g/100mls.
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wath is the conssentration of your acid mine is 30% dilued in half so it is 15%.
does antimony react with copper sulfate?
Can you post some picture of the 2 anode please it will help me a lot.
[Edited on 25-1-2011 by plante1999]
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dann2
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Hello,
It's 2008 all over again??
Regading Tin Oxide from Tin Sulphate see US 4028215, example 13 (below)
EXAMPLE 13
A strip of porous titanium having a surface area of approximately 7 square inches (45 square centimeters) was coated with a solution of tin and
antimony compounds by use of a vacuum to suck the solution through the porous material. The solution consisted of 5.27 grams of stannous sulfate, 2.63
grams of antimony trichloride, 10 milliliters of hydrochloric acid, and 20 milliliters of butyl alcohol. This was done four times with the baking of
one-half hour at approximately 500.degree. C. between each pass through the porous titanium material. A 50 percent aqueous solution of manganese
nitrate was passed through the material in the same fashion with a baking between each pass of 45 to 60 minutes at approximately 200 degrees
centigrade until a weight gain in the range of 3.36 to 3.56 grams of manganese dioxide is contained therein.
[SNIP]
Tin Sulphate cropped up from time to time in patents but they always used porous Ti (whatever exactly that is) as the substrate, never smooth plate.
Just about all Tin compounds decompose to SnO2 when heated. Some give 'usable' SnO2 (for an Anode application) in certain situations, some don't.
(IMO)
@Plante1999
You used the Anode for two weeks at one amp and got 100 grams of Chlorate (say K Chlorate).?
That gives (by my calculations using Swede's formula) 39% CE.
(131.22 * (100 GRAMS))/(336 AMPER HOURS) = 39
Dann2
[Edited on 25-1-2011 by dann2]
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Xenoid
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| Quote: Originally posted by dann2 | Hello,
It's 2008 all over again??
Regading Tin Oxide from Tin Sulphate see US 4028215, example 13 (below)
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Good grief, dann2 - do you have all those patents committed to memory. It even has aluminium listed as one of the "valve" metals
I presume the porous Ti is sintered Ti powder, very high surface area.
I have that patent in my collection, it makes interesting reading. I'm not sure why I never bothered with it though, probably because it mentions
electro-winning rather than chlorate/perchlorate anodes.
I thought you were in West Africa, with a bag of salt, looking for a wife
@plante 1999 - I am surprised the SnO2 alone is not able to make the Al2O3 conducting. I have some pure antimony metal, and it would probably react
with copper sulphate, however it is insoluble so that's not much use. I will investigate antimony trichloride.
Edit: Re-reading your post; I would have thought that antimony sulphate would have been precipitated when you added the sulphuric acid to the solder
dissolved in HCl. Thus, your tin sulphate would be antimony free!
[Edited on 25-1-2011 by Xenoid]
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Zaratukhshthra
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wow! seems too good to be true!
maybe you've made some kind of Al-Sb doped SnO2
aluminum doped SnO2 is known. For example US3901067 gives some info on making semiconducting Al doped SnO2 for H2S sensing. They use a solution of
Al(NO3)3.9H2O and SnCl2 in glycerol to coat the electrode and heat from 25 to 430^C over 30 minutes. The resistance of a film with 4000A thickness is
reported to be 1.7x10^5 to 2.2x10^4 ohm/square at 130^C (it was measured along the film).
No Al2O3+Sb2O3 can't be reduced to AlSb by flame! in your link it's actually mentioned that AlSb burns to produce aluminum oxide and antimony
trioxide.
Edit:
I dont have access to the fulltext of this articleBut in the abstract it's claimed that: The room temperature electrical conductivities of the films are obtained in the range of 0.21 S
cm−1 to 1.36 S cm−1 for variation of Al doping in the films 2.31–18.56% (which is a satisfactory conductivity range in my opinion)
[Edited on 25-1-2011 by Zaratukhshthra]
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dann2
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Hello,
| Quote: Originally posted by Xenoid | Good grief, dann2 - do you have all those patents committed to memory. It even has aluminium listed as one of the "valve" metals
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Yes. Chapter, paragraph and line No's. in my head :-|
Al is not very 'Valve' though. I tested it some time ago together with Ti, Nb and W. It could only withstand about a Volt or two before it started to
corrode/conduct when used as an Anode. According to Wouters site it corrodes when used as a Cathode!
If it works as an Anode substrate it would be great.
Perhaps if people are getting it hard to get this Anode to work they could try the idea using Ti (you will get no corrosing if coating is a bit iffy).
Get that to work and then migrate to Al. Then again perhaps it only works using Al at the starting substrate?
Just home. Wife secured. I am not 100% pleased as see is a bit old for me. Hard to have it all your own way. Her father is very very pleased (he got
his 28 pounds of salt), and of course my (new)wife is very very pleased (she got ME). My older wife......... not so pleased.
I decided to include a picture of her (new wife). It depicts her happily keeping an eye and jotting down some pH readings from my latest Chlorate
cell. This cell uses a MetaStanic derived poly Mono Metal Spinal combined with a Perskovite doped inverse Spinel containing strategic quantities of
Zn, Bi, As, Co, Ni etc etc etc.
Dann2
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tnphysics
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Maybe Sb-doped SnO2 appears, and the Al2O3 is just for adhesion.
I LOVE science!
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pyromaniac
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Can you substitute lead metal from fishing weights for the tin solder?
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plante1999
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no but you can buy tin solder at 5dollars search for 50/50 tin antimony and fallow this guide and you will have great anode for making , with your
naame i think you will made chlorate or perchlorate.
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tnphysics
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AlSb may form by 3AlSbO4+8Al->3AlSb+8Al2O3. It would be doped with Sn and likely conductive.
I LOVE science!
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plante1999
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yes i was thinking the same.
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pyromaniac
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nahh, I like electrochemistry mostly. I bought some Roebic drain cleaner for the sulfuric acid and I do not know to concentration. I tried pouring a
pouring a little into a container and added about 3 times as much (by mass) sugar. It started soaking up the sulfuric acid and the sugar at the center
turned dark brown gradually getting light brown as it went outwards. I guess that I added too much sugar to make the carbon and the drain cleaner is
brown. I am guessing that it's not that pure but I am planning on boiling the sulfuric acid to 100% purity (untill white fumes appear) and then using
that stuff. Will that work or will it not be pure enough?
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pyromaniac
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BTW this anode can make perchlorate? Is it basically a lead dioxide anode?
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plante1999
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the acid after boiled will be good if you ad some hydrogen peroxide end boile it , basicaly this anode is a aluminium oxide doped with aluminium
antimonyde and tin dioxide anode.
[Edited on 6-2-2011 by plante1999]
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otonel
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I try to make MMO anod but I failed to make tin sulfate using hydrochloric acid, what is the trick.
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