Some observations from the experiment.
That's my ffnding too- the HCl plated items rust pretty quickly.
I need to clarify. There is very little rust on the acid WE plates after one week. Slight discolorations only in small spots. Most of the coating is still shiny. They look the same today as in my post #981. The Steel Anode forms rust when removed from the solution very quickly but not the CE. I am not sure why my WEs do not seem to rust as yours and Stevenson's did?
Ken, what about rusting of your samples?
My active WEs rusted in a very short time (less than one day, with first visible signs just after few hours). Inactive or "less active" ones took longer (few days).
Also rusting was not uniform in active WEs, it started soon in few points then spread more slowly to the entire part. I think other described something similar.
Oddly I have seen very little rusting of my plates, some are 2 weeks old and they still all look ~97% rust free. The samples coated with the acid electrolyte have a bit of of rust in spots more of a discoloration, the Alkaline ones have no rust at all. The Steel anodes rust quickly when removed from the solution. Pure Iron as opposed to steel is known to be less prone to rust. The relative humidity has been between 35-45% lately which may have some impact on the amount of rust..
Thanks for the update Ken. In my opinion I think you should dilute your electrolyte by 50% and go again with a target voltage od 2.5-3.0V so that you can see the hydrogen bubbles flowing freely off the surface of your plate. I am still up to my neck with lab rebuild ( and rewire, repaint, re-calibrate everything) but hope to do a few more tests next month.
Alan.
Hi Alan,
I have found with low dilutions and .4 Amps fixed I can see tiny bubbles start to show at .7 Volts with the intensity increasing as Voltage is increased. At Currents in the 1-2 Amp range and Volts over ~1.84 I can see what looks like smoke (micro bubbles) in the solution at the top of the CE streaming toward the Anode vigorously. At 4 Amps and 2 Volts plating forms in minutes.
Two more attempts at plating with Acid.
These attempts used higher voltage than previous attempts and weaker acid solutions. Power supply was set to maintain a fixed voltage rather than current.
#1
- Set volts to ~ 1.84 Volts and added acid to bring current to 2 Amps
- Current dropped to .92 Amps in 5 hours. Gray coating just starting to form
- dried with paper towel and it read 10-20 mV but dropped to 000.0mV when dried with a 60 watt lamp for ~ one minute
- back in tank, moved anode closer to maintain 2 Amps
- after 7 hours total time, very shiny but coarse, dried and LEC read 000.0 mV
#2
- fresh solution ~ 80mL acid in 1.5 L water
- brass plate ~ 2 inched from heavy iron plate Anode
- 1.37 Volts @ 2 Amps
- no coating after 1.5 hours increased volts to 1.5
- no coating after 6 hours so upped Voltage to 1.64
- no coating after 12 hours so upped voltage to 1.84V
- left over night, very heavy coating with coarse particles ~ .5mm in size(colour very shiny, chrome like) some clumps could be rubbed off with fingers.
- dried with towel and lamp and LEC read 000.0 mV
Some observations
- All trials so far will read some low voltage 2-20 mV or so if the WE is damp. Condensation can often be seen on the CE plate when this occurs.
- When dry no attempt so far has read any voltage at all.
- lower currents and voltage ~ .2 Amps, 400-600 mV yield smoother gray to dark gray plating with magnatite
- higher current and voltage over >1.84 Volts plate very fast with a coarse bright shiny coat, no obvious sign of magnetite
Left: ~ 500 mV 200 mA Right: 1.84 Volts 2 Amps
Today I discovered something interesting.
I placed a small tube (6 mm OD, 13 cm long) of copper, close to a similar tube of aluminium (the gap was about 1 mm). The tubes were connected to a multimeter with a 10 MOhm impedance (copper to positive probe, aluminium to negative probe). As expected the resulting voltage was 0.0 mV.
Hi Stevenson
You could try the Am241 pellet from a smoke detector. 1 µCurie, 60 keV
Display MoreHi Ken.
In order to raise the voltage while keeping the current at a reasonable level you will need to increase the resistance of your electrolyte. This means reducing its concentration so as to reduce the number of free ions. This paper from Spzack and Pam Boss gives the essentials for Palladium in Heavy Water, but basically there is little difference if you are using Iron in light water.
https://www.lenr-canr.org/acrobat/SzpakSreliablepr.pdf
They say in this extract :-
.
Hi Alan Smith
I have been trying less HCI concentration but will reduce it more it my next trial.
the three vertical dots in the right of every post header)
Display MoreUse the “quote” function instead, you can quote entire posts by selecting the quote option in the drop down menu (the three vertical dots in the right of every post header)
Or, alternatively, You can select a text and the options of “save quote” “insert quote” should appear in your screen if you are on a mobile.
If you choose insert quote, The text will be added to your reply, in quote format.
Hope this is nearly clear enough for being of use for you.
Hi Curbina
I do not see the three vertical dots in the right of every post header.
Example of what my Fire fox browser shows me:
If I use the quote symbol at the bottom right and I paste text from another application I get a code box
Hi Ken! Good to hear that you got a plating with HCl. It looks quite similar to the one that I got (it is less shining compared to the sulfate solution). Also in my experiments I got a kind of magnetite mixed with the plating: this made the electrode magnetic (i.e. capable of attracting iron wires). I suspect that it was this kind of nano-magnetite that triggered the effect. It's a pity that you still don't get any voltage...
If you want to try another plating solution, the most easy is the original one used and suggested by Frank Gordon: FeCl2. Don't use FeCl3: apparently it doesn't give good results.
Hi Stevenson
I found a couple of other recipes.
One uses Ferrous Chloride and Calcium Chloride supposed to produce soft and thick deposits, the other uses Ferrous Chloride and Potassium Chloride for Hard deposits According to Blum,G.;Hogaboom,W. Principles of electroplating and electroforming, New York 1949. (I have ordered this book)
I noticed that the copious black sludge that accumulates in the bottom of the tank using Ferrous Sulfate when dried it turns an army green color and is slightly attracted to a magnetic. My plates themselves do not seems to be magnetized.
On another note when I try to cut paste text into my reply a box named "Code" comes up with the text. Appears to think I am entering computer code. How do I paste without this box?
Well, I think Alan Smith provided a very important advice as the LEC doesn’t require a good plating, but a suitable co deposition of hydrogen with the metal layer. Now you can begin focusing in codepositing instead of plating.
I appreciate the advice, my background is in electronics and radiation measurement, I am weak in chemistry. Clear description of how to go about the co deposition\plating process is helpful.
Hi Ken
Are you running at above the voltage required to split water? Anything under 2V and you are unlikely to be doing co-deposition.
Max voltage was 600mV or so. Current would increase to over 2 Amps above ~ 700mV. Plating only seemed to start occurring when the Voltage dropped on its own to about 400 mV.
A programmable rig that monitors and controls plating regimes flashed into a recent dream of mine.
Designing an Arduino to control a TO3 package regulator chip that would allow programming current, voltage and time would not be particularly hard or expensive. At the moment though I need to find a reliable and fast coating protocol and I need to see voltage from a working LEC before looking at making a programmable power supply.
I finally managed to get a coating using HCI. It took almost 2 days before the coating started to form. I used a tray with 800 mL solution and twisted wire anodes that had to be replaced 3 times. The coating looked very smooth, well adhered but very thin compared to what the Ferrous Sulphate recipe produced. I dried it and tried in on the brass CE but no Voltage, 000.0 mV. After 1\2 hour I put it back in the tray for a few hours but the coating did not seem to increase. I then added 100 mL Ferrous Chloride and ran it overnight. It was covered with black (magnetite?) which I removed with a scotch brite. The iron coating underneath looked no thicker than the day before. Still no voltage was produced.
I have found a couple of other recipes for iron plating on Brass that I will try.
Display MoreA recently completed masterpiece I'll title
Turmoil at Sea
It is indeed a masterpiece, frame it and spray it with lacquer!
Really I don't know... The recipe, currents and times are ok. The only variables left are the anode and the total volume of the solution. The actual plating starts only when the HCl is completely "decomposed". Probably this may require more time if the volume of solution is bigger than the one I used (essentially a test tube). If you keep the voltage at about 300-400 mV, you will notice that at some point the current and the bubbling decreases a lot. This is the moment when you have to increase the voltage > 500 mV to get the desired current, and the plating starts. Probably in order to work with this voltages you need to keep the anode relatively close to the cathode (< 0.5-1 cm) and the anode have to surround well the cathode (it can be made from multiple wires or just one wire wrapped around the cathode, the wires being of 1 mm diameter or less).
I have changed anodes to 2 twisted pair of "mechanics wire" of 18 gauge in 4 groups about 1 inch from the cathode. (Probably steel as I could not locate pure Iron wire). I reduced the HCl to 200 mL (to reduce the smell). My container is the same size 1.6 L, if this does not work I will reduce the container volume. Right now its drawing 350 mA @ 300 mV ~ 2 hours from start.
Great!
Flat plates should work well, just as tubes, and in addition they make easier to do a number of interesting experiments.
BTW, I made some experiments months ago to specifically check out if a partially wet or moist electrode can produce the effect. The result was that twofold: a) no effect can be induced just by wetting a plated (but inactive) electrode, b) since a wet electrode may generate a voltage if set in galvanic contact with the counter-electrode, it was possible to verify that the isolation I used was very effective, even with a much greater level of moisture of usual active electrodes. Moreover the electric characteristics provided by a galvanic contacts are very different from the one seen on a genuine LEC (for example the current is much higher, the internal resistance is much lower and when an external voltage is applied the V/I curve is modified due to heating).
I have found that my inactive CEs will produce a voltage if I soak them in tap water for a few minutes then place them on a brass plate at .5 mm spacing. The output persists for an hour or so until the water evaporates. The voltage is usually less than 25 mV.
One thing to watch is that checking the LEC with an ohmmeter will charge the cell as an ohmmeter functions by applying a voltage and then reading current and scaling the readout as ohms. If the cell is functioning as an electro chemical cell it will take on a charge from the ohmmeter. Also the cell capacitance will acquire an electrostatic charge. The cell capacitance though is very small and my load resistance of 1 megOhm will discharge the capacitance within micro\milli seconds and the electro chemical charge in seconds.
Great!
Flat plates should work well, just as tubes, and in addition they make easier to do a number of interesting experiments.
I attempted to plate with HCl and no coating formed.
400 mL of 31% HCl in 1.6 L tap water, 25 deg C
.9 mm thick brass plate 88 cM^2 per side, 240 grit sanding,
heavy steel plate anode
1 hour at 17 mA
1 hour at 35 mA ~200mV
2 hours at 350 mA ~ 300mV
3 hours at 700 mA ~ 520 mV
At this point no coating had formed, I watched for 3 more hours and no coating, lots of bubbles. I tried for 3 more hours and boosted the current to 2 amps for a 1\2 hour without result. I left it over night at reduced current of 200 mA and no coating other than at the top area above the water line. The solution remained clear with a gram or so of iron particles around the base of the anode. Any ideas what went wrong?
Display MoreAmazing work Ken!
Your protocol seems ok, the only variable is the plating process. Frank and Harper used chloride salts (either for Pd or Fe), I used Fe + HCl, J.P. Biberian used also chlorides and bromides. I suspect that a lower pH is needed in order to either increase the H+ concentration and codeposition, and also to modify the plating structure at micro/nano level (increasing the number of defects).
All pictures I saw from successful replications had a coating that looked quite "ugly". In my first successful replication I was very disappointed with the plating result!
I recap my protocol, in case you would to try it out:
- start with a clean and finely sanded brass electrode as cathode
- use as electrolyte tap water with about 5% of HCl (I used 1/4 in volume of 20% HCl)
- use a number of 1 mm iron wires evenly spaced around the cathode, at a short distance (< 1 cm)
- start with a current density of about 100 uA/cm^2 for one hour then about 200 uA/cm^2 for another hour (resulting voltage should be around 200 mV)
- increase the current at about 2 mA/cm^2 for about 3 or 4 hour (voltage will be around 300 mV)
- you have to gradually increase the voltage in order to keep the desired current, within the above mentined limits
- In this first part of the process you should note a sensible evolution of hydrogen at the cathode and almost no plating forming
- After about 4 or 5 hours, you should note that the gas evolution stops or reduces a lot, the current will also decrease: this is the start of the second part of the process
- Increase the voltage so that the current will be about 3-5 mA/cm^2. The resulting voltage will be about 500 mV (do not exceed 600 mV). Keep this setting for about 4 hour
- You should note that from that moment the cathode starts to plate with a black coating, the hydrogen evolution is small and the current will maintain quite stable
- After these last 4 hours, take out the cathode, that will look kind of carbon black, not shining at all. Rinse and dry very well with a towel. Do not use an oven and do not take too much time, because it will rust very rapidly! However take all the measures so to avoid unwanted wet contacts.
Assemble a LEC with a brass, copper or aluminium counter-electrode, and measure the voltage: after a few minutes it will rise to some 100s mV (hopefully!
).
Thanks Stevenson for the detail, I will follow this plating method with HCI and report my result. Ill likely use flat plates again rather than tubes as they are a bit easier to manage with my set up at the moment.
Ken thanks for your efforts, I guess you conclude the effect is not real. Can you post a detailed procedure of the electroplating protocol for letting Frank Gordon , Stevenson , Alan Smith and jean-paul biberian see what might be the problem?
I don't conclude anything yet. I am still trying variations. I have described the electro plating in my posts. 1.3 volts at 150-200 MA was used in the flat plate LEC and chemistry as described. Solution at 21 deg C. The coatings are well adhered, they do not remove with moderate scrubbing with a scotch bright and they are magnetic. The brass plates are .9 mm thick. I see only a very small area of rust forming after 5 days. The humidity is around 40%.
Another several attempts at replication using Iron plated copper pipes as a WE and CE pipes of Steel, Zinc coated steel and Brass with air gaps of approximately .2, .5, 1 and 2.5 mm have produced no voltage +- .1 mV. Plating method as per my previous post #924
I then switched to brass plates for electrodes and plated in Ferrous Sulphate 30 gr, Sodium Citrate 30 gr, household ammonia cleaner 150 gr, 1.5 litre of tap water, heavy steel plate Anode with mill scale ground of. The WE plated on both sides. A magnet is attracted to the plating. The LEC read 150 pF capacitance at .5 mm spacing.
The WE was rinsed with tap water and dried with a paper towel but still showed signs of dampness so it was gently heated with a 60 watt Halogen bulb for about 2 minutes until it looked dry.
I stacked the WE .5 mm above the CE with vinyl electrical tap as a spacer at each end of the cell. A 1 megohm load resistor was connected across the cell. The cell was checked for shorts and it read 1.03 megohm. The voltage read 000.0 mV initially then climbed slowly to about 20 mV. I removed the WE and noticed that the CE had small areas of condensation (tiny bubbles). Apparently though the WE looked dry it still held moisture in the porous iron coating. I heated it again under the bulb for a few minutes and by then the CE condensation had evaporated. I placed the WE on the CE and the voltage read 000.0 mV and did not climb at all. I placed the WE back in the plating tank to continue plating and after 4 hours I removed it repeated the same drying protocol and assembled the LEC. The result was the same, incomplete drying of the iron surface caused condensation to form between the plates that is the likely cause of an electro chemical based voltage. With the WE placed back in the plating tank for 4-10 hours and then dried thoroughly with heat and tested again I get 000.0 mV. Tests with various plate spacing of .5 – 2 mm also showed 000.0 mV
