48g initial anode
Small Cu riser wire lead soldered to large Cu anode wire, insulated with electrical tape
500ml tap water in spaghetti sauce jar
Cathode is multi-stranded 8AWG copper wire
Filtered once to remove insoluble whitish gunk, some remained
Started 5:30pm 12-19-2015
Using a constant current power supply
Around two hours after start, small crystals visible on wire
Switched to 20mA, ~1.05V
21:30 12-21-2015 Noted clear top layer of solution, black coloration and polyp-like growths with black layer, voltage at 1.113V, current at 20mA
Stirred solution to get Cu2+ ions mixed around again, key is to use copper or plastic for stirring, not iron -single displacement rxn
Cloudy precipitate stirred up, black stuff flaked off of anode to reveal shiny surface underneath, much of the black gunk and some of extensions of the crystal fell off during stirring as well, didn't look very solid-copper-like
Voltage now at .860v
Shiny copper dendrite structure look is back after removal of black gunk
0.9V after all of this, going to bed
8:00 12-22-2015 Stirred solution, no more black gunk on cathode
Voltage now at 0.812V
22:00 12-22-2015 Voltage at .830V, no solution separation or black gunk
Stirred again, voltage now .798V
10:00 12-23-2015 voltage at 0.851V, copper nodule looks good
Stirred again, voltage now at .791V, quite vigorous stirring, some solids agitated
22:00 12-23-2015 voltage 0.848V, still looking shiny
Stirred, voltage now at 0.751V
Scraped some dark flaky layers off of anode
Stirring most mornings and evenings
12-27-2015 looking really good, stirred again
12-28-2015 morning: noted no visible mixing of solutions when stirred, saw that positive clip was unconnected; reconnected with 0.697V
Stirring thrice daily
Removed 11:30 1-4-2016, dipped and swirled twice in clean water
Use single, thicker (12AWG) Cu cathode, have it protrude less into solution. Shorter (from 13cm) distance between electrodes to facilitate ion diffusion. Constant voltage, use LM317 circuit powered by a fanless power source. Don't let current exceed 10mA. Try adding 0.06g/L Cl- to inhibit dendrites, and coat washed crystal with clean mineral oil to keep shine. Let crystal grow for longer, and possibly add Cu metal to anode to enable larger crystals.
Experimental Run #2
Initial anode weight (includes wire, tape, smashed Cu pipe): 56g
Electrode spacing: 7cm
Voltage: 0.575 to 0.610
4-3-2016, 9:00pm: Start of experiment, running at about 5mA, noticed that current seemed to be slowly rising. Also observed a voltage decrease when ammeter was taken off-line and a direct connection was used instead. No visible growth. Forgot to add chloride.
4-4-16, 7:30am: Noticed very slight growth (mainly on tip of downward-protruding wire). Voltage at 0.510V, current at 5.78mA. Voltage still varies when ammeter is connected vs. disconnected.
4-4-16, 4:30pm: added chloride
4-4-16, 10:53m: 0.484V, current at around 6.6mA. Growth visible. Solution appears uniform. LM317 is "room temperature."
4-5-16, 9:30pm: 0.484V, 6.4mA. Same observations as before.
4-10-16, 4:00pm: 0.610V, ~4mA. Noticed that the solution had a clear layer on top. Crystal growth had polyp-like black growths on it with fragile, tiny crystals. Turned off and aborted experiment.
4-10-16, 5:00pm: Added another ~10.5g CuSO4 to electrolyte bath and stirred to dissolve. No insolubles were visible, so the bath was immediately put back in action with a fresh cathode. Less than a gram had been removed from the anode, so it was left, as well. Everything was taped and covered again. The voltage is (with ammeter reading) 0.331V at 4.97mA. Without ammeter in line, 0.306V. Nothing to do now but wait and pray deposition doesn't exceed diffusion again!
4-10-16, 7:20pm: 0.322V at 5.06mA with ammeter, 0.296V without.
4-11-16, 10:30pm: 0.295V at 5.45mA or 0.270V. Swirled solution a bit, current went up a bit. A connection may be a bit sketchy; check again. No certain growth visible.
4-12-16: 0.290V at 5.5mA or 0.260V. Adjusted so voltage without ammeter measured 0.270V. Removed cathode for a moment and saw definite crystals encasing wire.
4-14-16, 2:45pm: 0.308V at 6.46mA or 0.275V. Upon swirling voltage dropped by 0.006V and current increased by 0.24mA. Beautiful small crystals now surround wire cathode, no solution separation visible. Leaving VWA (voltage without ammeter) at 0.268.
4-16-16, 10:20pm: 0.281VWA, 0.317V at 7.4mA. No visible solution color gradient. Swirling jar for 15s dropped voltage to 0.303V at 8mA. Noticeable growth now. Left VWA at 0.262.
4-18-16, 7:30am: 0.305V at 7.65mA, 0.261VWA. No noticeable solution color gradient. Did not swirl solution.
4-19-16, 10:45pm: 0.299V at 7.11mA or 0.261VWA. Did not swirl solution. Did not observe color gradient indicative of a Cu2++ depleted solution.
4-20-16, 9:40pm: Heard multiple jokes related to the cannabis plant. 0.264VWA, 0.300V at 6.91mA. No solution depletion noticed. After swirling with medium intensity current topped out at 7.79mA at 2.79V. Noticed some black flakes, presumably anode material, swirling in currents. Moved experiment to a safer spot and left VWA at 0.242.
4-21-16, 10:00am: 0.260VWA. Solution still shows no separation.
4-23-16, 9:30pm: 0.242VWA. Adjusted to 0.271VWA.
4-25-16, 8:45pm: Measured 0.275VWA. Moved experiment back into open. Now at 0.291VWA. No concentration gradient visible. Swirled solution. VWA now at 0.269. Added some water to cover crystal. Briefly removed crystal and observed medium-sized, medium-sharpness-of-definition bright pink crystals! Left experiment at 0.305V at 8.06mA, or 0.263VWA.
4-26-16, 9:15pm: 0.263VWA. Adjusted current to 8.4mA at 0.283V. Looks good still!
5-2-16, 6pm: Noticed slight solution gradient, darker blue on bottom and thinner blue at top. Not clear, though. 0.318VWA. 0.356V at 7.97mA. Swirled thoroughly, now 0.326V at 9.32mA. Added small amount of water forcefully through syringe and noticed effervescence in solution. Momentarily removed growth and saw nice pink crystals of good size. Adjusted down to 0.310V at 8.8mA, or 0.263VWA.
5-5-16, 3:30pm: 0.271VWW. Swirled a bit. Now 0.261VWA, or 0.305V at 8.5mA.
5-6-16, 8:30pm: 0.290VWA. 0.340V at 9.83mA. Adjusted down to 0.305V at 8.78mA. No visible gradient. 0.259VWA.
5-11-16, 5pm: 0.251VWA. Swirled a bit. Things are looking good. Added water to top up electrolyte bath. Now 0.235V at 7.8mA.
5-14-16, 5pm: 0.231VWA. 0.270V at 6.76V. Swirled some. Now at 0.264V at 7mA. Adjusted up to 0.3V at 8.07mA. Left at 0.259VWA.
5-17-16, 2pm: 0.277VWA. Solution is perhaps slightly less blue farther up. 0.321V at 8.44mA. After moderate swirling, 0.310V at 8.85mA, or 0.268VWA.
5-22-16, 8:15pm: 0.335VWA or 0.370V at 8.80mA. Solution appeared to have lighter layer on top; it was fairly light blue. After thorough swirling, 0.356V at 9.38mA. 0.293VWA.
5-24-16, 8pm: 0.310VWA
5-25-16, 3:40pm: 0.300VWA or 0.386V at 8.10mA. Solution does not look separated.
End anode weight (wire, tape, and pipe): 42g
Extra solids weight: negligible
Thoughts: I noticed that the anode wire that hooked it up to voltage had been corroded through in one place. It broke when I picked it up. There was a lot of dark red powdery stuff at the bottom of the cell, and it looked like some copper had flaked off. The smashed copper pipe placed atop the anode had been etched to show a neat grain, but it hadn't been eaten away much. The copper crystal itself was positively stunning, with beautiful large pink crystal faces everywhere.