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Nixie
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Plated platinum black with some lead oxide in the chloroplatinate and then sent to someone bake in inert atmosphere to diffuse the plating into the
substrate as per a patent that was posted here a while back.
\"Good is a product of the ethical and spiritual artistry of individuals; it cannot be mass-produced.\" --Aldous Huxley
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jpsmith123
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Electrodeposition Of Diamond-Like Films
I found an interesting abstract of a thesis (couldn't get the paper though):
Diamond-Like Carbon (DLC) films were successfully deposited on the ITO substrate by electrodeposition technique. This method has several advantages in
terms of low cost, rapid growth rates and simple setup. Electrodeposition of DLC thin film was carried out at low DC potential by using a mixture of
acetic acid and DI water as electrolyte. The Raman spectra showed two peaks located at 1350cm-1 and 1580cm-1, which were the characterized peaks for
DLC films deposited on ITO substrates. By varying the experimental parameters such as the deposited DC potential, distance of electrodes, and the
concentrations of solution, the growth mechanism of deposition process was investigated, and the best quality of DLC films was also achieved. Scanning
electron microscopy (SEM) and atomic force microscopy (AFM) were used to make insight into accurately the surface morphology of DLC films related to
deposited parameters
In addition, according to the experimental results, it indicates that the quality of the DLC film was improved as deposited at higher DC voltage.
Finally, to demonstrate the effect of annealing on the interfacial characteristics the C-V and G-V curves of MIS structures are the further works.
http://etd.lib.nsysu.edu.tw/ETD-db/ETD-search/view_etd?URN=e...
So, all you need is some distilled vinegar and a low voltage power supply? That sounds like my kind of experiment. Too bad I couldn't download the
full paper.
And here's another interesting abstract:
doi:10.1016/S0009-2614(01)01040-5
Electrodeposition of diamond-like carbon films in organic solvents using a thin wire anode
Hao Wang, 1 and Masahiro Yoshimura,
Materials and Structures Laboratory, Tokyo Institute of Technology, Nagatsuta, Midoriku, Yokohama 226-8503, Japan
Diamond-like carbon films (DLC) have been electrodeposited on silicon substrates in organic solvents using a thin tungsten wire anode under high
potential. During the deposition, if the applied potential is sufficient enough, the spark could be observed even by the naked eye. It has been
manifested that this method could produce an extreme environment which is favorable to form much more sp3 bonded carbon atoms compared with
conventional electrolysis.
#####################################
And here's yet another, apparently related, thesis:
In the early years, DLC films was deposited at high voltage applied by electrochemical method. In this study, DLC film was deposited alternatively at
low voltage applied using electrodeposition. The ITO glass substrate was used as the cathode, and graphite sheet was the anode. The electrolyte is a
mixture of acetic acid with DI water. The applied voltage was mere 2.1 volt during the electrochemical process.
For investigating the structure of deposited films, the deposited DLC layers were characterized by Fourier transform infrared (FTIR), Scanning
electron microscope (SEM) and Raman spectrometer. The SEM results show that the DLC films have a rough surface and their roughness increased with
longer in deposition time as well as raise applied voltage. The Raman spectra shows distinct broad characteristic peaks at ~ 1336 cm-1 (D-peak) and ~
1601 cm-1 (G-peak), which indicate the disordered graphite-like structure and the graphite structure, respectively. While the bond angles occur to
bend or the increase the content of sp3 bonds in DLC film, both the G-peak and the D-peak shift to the lower wave numbers. Peaks at ~ 2956 and ~ 2917
cm-1 found in FTIR measurement were used to recognize the existence of sp3 and sp2 combined carbon atoms in the films. Based on above results, it
could conclude that the DLC film could be prepared by electrodeposition under low applied voltage.
http://etd.lib.nsysu.edu.tw/ETD-db/ETD-search/view_etd?URN=e...
Once again unfortunately it seems the full paper is not available for download.
[Edited on by jpsmith123]
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dann2
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Hello,
The Vinegar and battery sounds good!!
If you put in a request in the reference section someone may be able to get it for you.
One wild idea I was thinking today was this. (It is off topic in a Diamond Anode thread though ).
If you were to use a solvent other that water, an alcohol perhaps, would this give any advantages when making (Per)Chlorates. There would be no
problems with O2 evolution, perhaps less anode corrosion, hugh yields of (Per)Chlorate  etc etc. I presume the solutions would be conductive or would they?
Cost and inflamability comes to mine for disadvantages.
Think it's time for another drag from by pipe...............
Dann2
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jpsmith123
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Hmmm, well the oxygen for the perchlorate comes from the water so I don't know what would happen with alcohol.
As far as bizarre new ideas are concerned, I don't think it would be practical, but it would be academically interesting to me to see what would
happen if you flow NaClO3 solution over a piece of anodized Ti out in the sun. I wonder if you could photocatalytically oxidize the chlorate to
perchlorate that way? Given that you'd be depending on wavelength content less than 400 nm (you'd only have a useful solar flux of a few tens of
watts/m^2 or something like that), and given that the process isn't very efficient in the first place, you'd probably wait a long time for a few
ounces of ClO4.
BTW someone uploaded the paper I requested (DLC films from electrolysis of DMSO) in the reference section and it's an interesting read. It's seems
clear that these DLC films can be made at home. I'm also trying to get the theses I referenced. It seems our problem may be trying to dope the films
to make them conductive.
######################################
Edit:
It seems DLC films have been electrodeposited from many different things. I wonder, what about trimethylglycine (TMG) dissolved in distilled water or
alcohol? I'm going to have to start experimenting here pretty soon.
[Edited on by jpsmith123]
######################################
Edit:
Just for the hell of it I took a piece of Ti that I had previously hydrided and stuck it in a stainless steel cup filled with about 300 ml of
distilled water. With the Ti as cathode and the cup as anode and the power supply maxed out at 30 VDC, I was reading about 150 uA.
Then I took about 30 grams of trimethylglycine and dissolved it in the distilled water, and the current increased to about 4.5 mA.
I'll let it sit there all night and see if the current changes at all. If it's depositing a poorly conducting DLC layer, I suppose I should expect the
current to decrease.
I'll have to get some distilled vinegar tomorrow and try that too. Too bad the theses involving vinegar aren't available.
[Edited on by jpsmith123]
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jpsmith123
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The vinegar might actually be making a DLC.
Using vinegar as electrolyte, I noticed an effect that makes me think it could be working.
I started at 2 vdc and increased the voltage incrementally while watching the current.
Every time I increased the voltage somewhat, the current would also increase, but then it would fall off a little bit. For example, if the current
initially went up by 50 uA, then, over the course of a minute or so, it would fall off by 10 to 20 uA.
As I took the voltage higher and higher, this effect was no longer noticeable as I had to switch from a uA to a mA meter, and I think the "hydrogen
current" was swamping the "diamond current" at this point.
I didn't notice this subtle effect when I used the trimethylglycine solution. I'm guessing that 30 volts isn't enough for this electrolyte.
What I want to know, is, how can I easily tell if the "grey discoloration" now on the Ti is a DLC or is it TiH2?
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JohnWW
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Besides doped diamond-like carbon thin films being a suitable coating for electrodes to prevent corrosion in electrolysis, another use for diamond (or
diamond-like boron nitride) films, although not necessarily doped, would be as an extra-hard coating or cladding for metal-cutting power tools, such
as drill bits and saw blades and the bits used in lathes and milling machines. Some of them are already plated or clad with titanium, but even this,
along with tungsten carbide chips, may not be hard enough to cut some materials.
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jpsmith123
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The other day while looking to see if boron-doped-diamond (BDD) powder was available for sale anywhere, I came across an interesting paper showing
that BDD was actually a better coating for cutting tools than straight diamond. If I can find it again I'll upload it.
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jpsmith123
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Well I tried to duplicate the DLC synthesis by way of low voltage electrolysis of dilute acetic acid, as per the paper by Gupta et al., to no avail.
(At least I don't think anything happened). The only difference was that I used titanium as a substrate rather than silicon, as I had no silicon
available.
Some papers on the subject reported fairly decent DLC growth, not over bare Ti, but over a native TiO2 layer on Ti...which is what I thought I
had...yet still no results.
Before giving up I intend to try the HV electrolysis of methanol as soon as I get set up for it.
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not_important
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If the paper you are talking about is titled Low voltage electrodeposition of diamond-like carbon films, they used conductive SnO2 on glass,
not silicon.
The films were thin, no more than a micrometer in thickness. How were you testing to see if a film had formed? Did the set-up have a similar I-V
curve to theirs?
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jpsmith123
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Sorry my mistake, you're correct, Gupta et al. used SnO2 on glass; the experiments with methanol used silicon substrates. (I've been looking at so
many papers lately, my head is spinning).
If I had to guess, what I think went wrong in my experiment is that my drug store distilled water was too conductive. At an applied voltage of 4.1
volts, my current density was much higher than theirs, and it didn't fall off with time, as it apparently should have.
They reported 0.1 mA/cm^2 (@4.1 V), whereas I was seeing almost 1 mA/cm^2. Thus I probably had way too much hydrogen, which etched the substrate
clean.
For purposes of analysis, I started with two lengths of Ti, cut from the same piece; unfortunately all I could do was compare them visually, and
compare the electrical resistance with a DMM. Doing this, I saw no difference whatsoever.
Edit:
I wonder where can I get some ultrapure deionized water cheaply?
[Edited on by jpsmith123]
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dann2
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Hello,
Used to work (some say Dann2 would'nt work on a F*C&%^G battery) in a factory where they made water for injections. THAT stuff was clean. Way
beyond deionized.
You can probably purchase it from a chemist or vetinary source.
One place you can get it for free (don't laugh) is in a needle exchange (or addicts). They dole it out in small 'one shot' bottles.
The procedure is this:
Throw on a pair of what this guy has on  .
Enter exchange.
In a very strained voice you say "What's the story man, what's the story man" etc etc.
May help to take a handful of second hand syringes.
      (that could
cover all persuasions/points of view)
Dann2
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jpsmith123
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Hmmm you seem to be very familiar with that method, Dann2...verrry familiar .
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Xenoid
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@ jp
I believe the "usual" way to produce ultrapure water is to distill it using a low temperature (non-boiling) quartz glass still. I helped set up an
isotope lab many years ago and that was part of the "equipment". The still is heated with a ?100W light bulb, and charged with normally distilled and
deionised water. The important thing is that droplets of water from boiling are not carried over. An ordinary glass still operated at low temp would
probably work.
How about a bowl of purified water, with a sheet of gladwrap on it and a weight in the centre to drip the condensation into a small container, also in
the bowl. Put it out in the sun!
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jpsmith123
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Those sound like some good ideas, Xenoid, but for right now I would like to just buy some somewhere, if possible.
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JohnWW
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I have just received the following periodic email, on solid-state physics and materials science, from Japan, to which I am subscribed. Some articles
linked in it, which can be viewed for free, are highly relevant to growing diamond films, and diamond semiconductors (doped with B or N):
From: ipapAlert@ipap.jp
To: johnww@...........
Subject: APEX/JJAP E-mail Alert; March 4, 2008
Date: Tue, 4 Mar 2008 12:14:05 +0900
APEX/JJAP E-mail Alert; March 4, 2008 by Institute of Pure and Applied Physics
http://www.ipap.jp
Dear APEX/JJAP Readers:
We are very glad to inform you that the first issue of the Applied Physics Express (APEX) has been partially available online. We look forward to
your access to APEX Online.
* New Issues Applied Physics Express Online (http://apex.ipap.jp/)
Vol. 1 No. 3 (Feb. 29, 2008)
http://apex.ipap.jp/journal/APEX-1-3.html
* JJAP Highlights
JJAP Highlights present a selection of the most important and influential papers featured in JJAP on the current developments in applied physics.
The selection was made by the JJAP Editorial Board. All articles listed on the JJAP Highlights can be viewed by everyone free of charge.
http://www.ipap.jp/highlights/jjap.html
* JJAP Invited Review Paper
http://www.ipap.jp/jjap/current/showEditorChoice.cgi?ip+47
* Pioneering Contributions to Applied Physics in the Last Half Century: Vertical-Cavity Surface-Emitting Laser: Its Conception and Evolution, by
Kenichi Iga. URL: http://jjap.ipap.jp/link?JJAP/47/1/
Development of Electron Holography and Its Applications to Fundamental Problems in Physics, by Akira Tonomura. URL: http://jjap.ipap.jp/link?JJAP/47/11/
* Top 20 Most Downloaded Articles: http://www.ipap.jp/jjap/mostDL/most_downloaded.cgi?year=2008...
* Selected Topics in Applied Physics: http://www.ipap.jp/jjap/section/stap.html
* ------ APEX New Articles published 29 February 2008 ------
Appl. Phys. Express Vol. 1 No. 3
http://apex.ipap.jp/journal/APEX-1-3.html
Ferroelectric Polarization Reversal by a Magnetic Field in Multiferroic Y-type Hexaferrite Ba2Mg2Fe12O22
by Kouji Taniguchi, Nobuyuki Abe, Shintaro Ohtani, Hiroshi Umetsu, and Taka-hisa Arima
URL: http://apex.ipap.jp/link?APEX/1/031301/
Lowering Threshold by Energy Transfer between Two Dyes in Cholesteric Liquid Crystal Distributed Feedback Lasers, by Koji Sonoyama, Yoichi
Takanishi, Ken Ishikawa, and Hideo Takezoe
URL: http://apex.ipap.jp/link?APEX/1/032002/
Optical and Conductive Characteristics of Metallic Single-Wall Carbon Nanotubes with Three Basic Colors; Cyan, Magenta, and Yellow by Kazuhiro
Yanagi, Yasumitsu Miyata, and Hiromichi Kataura
URL: http://apex.ipap.jp/link?APEX/1/034003/
Influence of Substrates on Initial Growth of Diamond-Like Carbon Films by Nobuto Yasui, Hiroshi Inaba, and Naoto Ohtake
URL: http://apex.ipap.jp/link?APEX/1/035002/
Near-Surface Defects in Boron-Doped Diamond Schottky Diodes Studied From Capacitance Transients
by Pierre Muret, Julien Pernot, Tokuyuki Teraji, and Toshimichi Ito
URL: http://apex.ipap.jp/link?APEX/1/035003/
Nitrogen Gas Flow Driven Unintentional Incorporation of Al during the Growth of Dilute Nitride Semiconductor by Plasma-Assisted Molecular Beam
Epitaxy, by Shudong Wu, Masakazu Kato, Masayuki Uchiyama, Kotaro Higashi, Fumitaro Ishikawa, and Masahiko Kondow
URL: http://apex.ipap.jp/link?APEX/1/035004/
Correlation Imaging of Magnetic Recorded Patterns and Grain Structures of Perpendicular Magnetic-Recording Media, by Yoshio Takahashi
URL: http://apex.ipap.jp/link?APEX/1/037001/
Enhanced Transfection Efficiency in Laser-Induced Stress Wave-Assisted Gene Transfer at Low Laser Fluence by Increasing Pressure Impulse, by Shinta
Takano, Shunichi Sato, Mitsuhiro Terakawa, Hiroshi Asida,
Hideyuki Okano, and Minoru Obara
URL: http://apex.ipap.jp/link?APEX/1/038001/
* Do not directly reply to this e-mail address as you will not receive a response.
* If you have any questions or comments, please contact us by sending an e-mail to the following address.
online-support@ipap.jp
[Edited on 4-3-08 by JohnWW]
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dann2
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Hello,
And another.
Hope they have not been uploaded before.
Dann2
Attachment: doped diamonds2.pdf (2MB)
This file has been downloaded 1043 times
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jpsmith123
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Look at this!
Apparently you can now buy, online, from their "CVD diamond eshop" (LOL!) a piece of polycrystalline "electrochemistry grade" CVD diamond.
Maybe this is the perchlorate "Holy Grail"? I think I might have to order some to find out...
http://www.e6cvd.com/cvd/page.jsp?pageid=161
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dann2
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Hello JP,
That's an interesting find and it would be an even more interesting purchase....
There is some reading under the 'Education' link on the page too.
I have attached an article from the link.
Must do some reading up on these Diamonds.
Dann2
Attachment: History of CVD diamond.pdf (17kB)
This file has been downloaded 1393 times
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Xenoid
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Interesting find jp.....
.....but it's bloody expensive, more than I paid for my Pt coated electrode and it's only 1 cm square. How will it be possible to make an electrical
connection? I suppose it could be bonded onto a Ti strap somehow. Why don't they coat some inert metal with this stuff, to make it more practical?
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jpsmith123
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It's too bad they don't have a bigger size available "off the shelf".
Anyway, I too am wondering how you would mount it and/or make electrical contact with it.
Maybe it could be mounted as a "window" somehow, sealed against the wall of the cell with a viton o-ring, with a piece of wire epoxied to it?
Let's say its resistivity is 0.1 ohm-cm, then with a thickness of 0.06 cm and 1 cm^2 area, its resistance would be about 0.006 ohms...so it should be
able to handle a few amps I would say.
I'm still trying to find type "IIb" conductive diamond grit somewhere...that's the stuff I would like to experiment with. I can't believe that nobody
is selling it yet.
Edit:
I bet if you had a piece of this stuff to start with you could add to it with electrodeposition from methanol or DMSO or something.
[Edited on by jpsmith123]
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chief
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What about plain old silicon: Does it dissolve in an perchlorate-cell ? Does it form an isolating SiO2-Layer ?
As long as Si has the same structure as Diamond (which it has), it might be useful for the purpose ? Someone might slaughter an old Diode or
something, and try out ...
If it works: Standard solar-cells might be abused (also coated with SnO2); question only would be, if it wouldn't exhibit nonconducting
Diode-Properties in the wrong direction: Then the SnO2 would have to be coated with some metal (for contacting), and the back of the solar cell would
have to be used ... ; There would be a Power-consuming voltage-drop, but this could be come by usind the Si-electrode for rectification directly ...
[Edited on 29-1-2009 by chief]
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chief
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Next post, different idea: Electrodeless electrolysis can be applied using a high voltage, and corona-discharging onto the electrolyte: The current
flows, but the electrode isn't immersed in the electrolyte, and therefore not subject to the agressive chemistry therin.
A long time ago I electrolyzed a solid CuSO4*xH2O-crystal like that, using the anode-voltage from a small TV, limiting the current by a 5
MOhm-resistor to maybe 5 mA. After a while it could, under the microscope, clearly be seen, that elementary copper was made.
This might maybe useful for the diamond-deposition-elecrolysis ; also maybe an electron-beam-chamber might be used ... .
[Edited on 29-1-2009 by chief]
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jpsmith123
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Electrolytic DLC over SnO2
Here's an interesting paper re DLC on stainless steel with an intermediate layer of SnO2.
Attachment: 01.10_m._roy_a.k._dua_a._english.pdf (805kB)
This file has been downloaded 803 times
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dann2
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Hello,
As far as I can see, DLC is a nonconducting coating and not the same as diamond. (see page 63 below graphs seems to suggest this too.) Could be wrong
though.
I worked in a place where they deposited DLC films and they were totally Nonconducting.
Dann2
[Edited on 8-2-2009 by dann2]
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Xenoid
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| Quote: | Originally posted by dann2
I worked in a place where they deposited DLC films and they were totally conconducting.
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LOL, "conconducting" is that a new type of conduction Dann2? Or is it actually nonconducting but you have managed to convince others that conduction
is occurring!
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