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4hv.org :: Forums :: Chemistry
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Inert metals? / PVD process

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Daedronus
Wed Sept 19 2012, 12:35PM
Daedronus Registered Member #2329 Joined: Tue Sept 01 2009, 08:25AM
Location:
Posts: 370
Apparently titanium is used as getter in vacuum systems....interesting, titanium is relatively cheap.

and, I managed to finally deposit "something"
actually deposit, with good adhesion, but 0 electrical conductance.

but not with evaporation, just plain DC sputtering, with 2 copper electrodes and a glass piece next to them.
it looked rather nice, goldish...shiny, far from opaque, probably because of the short deposition time.
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Ash Small
Wed Sept 19 2012, 01:09PM
Ash Small Registered Member #3414 Joined: Sun Nov 14 2010, 05:05PM
Location: UK
Posts: 4245
Daedronus wrote ...

Apparently titanium is used as getter in vacuum systems....interesting, titanium is relatively cheap.


Titanium is used in 'ion pumps' for removing 'hard to pump' gases like helium.

Ion pumps have two charged plates, which ionise any gas molecules that 'happen' to drift in between them, the +ve ion (He2+ or alphas) are attracted to the cathode, where they become implanted, eventually resulting in 'helium embrittlement', and the electrons are attracted to the anode plate. Ion pumps therefore have a limited lifespan and are only used for ultra high vacuums.
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Daedronus
Wed Sept 19 2012, 01:37PM
Daedronus Registered Member #2329 Joined: Tue Sept 01 2009, 08:25AM
Location:
Posts: 370
That's different from a titanium sublimation pump:
Link2

This kind has a pure getter style operation, and it will remove reactive gasses (good for what i want).

Also limited lifespan, but titanium wire seems to be cheap....
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Ash Small
Wed Sept 19 2012, 03:45PM
Ash Small Registered Member #3414 Joined: Sun Nov 14 2010, 05:05PM
Location: UK
Posts: 4245
Interesting article, but again, TSP's operate at ultra high vacuums, not the low vacuum levels you'll get without a turbo or diff pump.

Your best bet is to look on ebay, etc. for a small diffusion pump. They are often a lot cheaper than you might expect.

EDIT: Your Welch will make an ideal roughing/backing pump for a diff. pump.
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Daedronus
Wed Sept 19 2012, 04:59PM
Daedronus Registered Member #2329 Joined: Tue Sept 01 2009, 08:25AM
Location:
Posts: 370
right now I see 3 options...

1. deposit gold, should work with just the mechanical pump, but, it's expensive, I will have problems to etch it (did I mention I also need to etch the metalization? :)

2. deposit copper in argon gas but I don't have a argon bottle and it's quite a bit of a initial investment...but it will also come in handy when I get a tig welder...I do want one...someday.

3. get a diffusion pump, should be fun for more then just the metalisation, simple enough to operate...but I kinda hate the water cooling, but I should be able to do any metalisation process with any materials.
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Ash Small
Wed Sept 19 2012, 06:26PM
Ash Small Registered Member #3414 Joined: Sun Nov 14 2010, 05:05PM
Location: UK
Posts: 4245
Daedronus wrote ...

right now I see 3 options...

1. deposit gold, should work with just the mechanical pump, but, it's expensive, I will have problems to etch it (did I mention I also need to etch the metalization? :)

2. deposit copper in argon gas but I don't have a argon bottle and it's quite a bit of a initial investment...but it will also come in handy when I get a tig welder...I do want one...someday.

3. get a diffusion pump, should be fun for more then just the metalisation, simple enough to operate...but I kinda hate the water cooling, but I should be able to do any metalisation process with any materials.

You can get small bottles of argon for around £10: Link2

You can get air cooled diff. pumps, just rig up a cooling fan Link2

They come up on Eay quite regularly.
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Daedronus
Wed Oct 10 2012, 10:18PM
Daedronus Registered Member #2329 Joined: Tue Sept 01 2009, 08:25AM
Location:
Posts: 370
Here is a try with copper:
Link2

Didn't work at all.

But, I tried again today with silver, and it works very nice. it's almost a perfect mirror.
Silver seems to be inert enough.

I will also have a micron pressure gauge later this week so I will see the actual working vacuum level.

Also, probably next week I will have some viton material, to replace the silicon seals.

The problem with silver however is that it seems to have really bad adherence, I can clean it off with a finger. Is silver that soft or maybe it's my coating?

And, what do you guys think will serve me better? a diffusion pump or argon gas?

I have a chance to get a seemingly nice diffusion pump:
Link2

But this will cut my funds for a while
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Carbon_Rod
Thu Oct 11 2012, 08:05AM
Carbon_Rod Registered Member #65 Joined: Thu Feb 09 2006, 06:43AM
Location:
Posts: 1155
Typically an inert gas like pure Argon (not the welding gas mix with CO2) will allow this to occur at higher pressures and KV.

The effect can be nuisance issue that can erode Nickel plates in electronic tubes, or completely cook the shells off of neon tubes during "burn-in".

Note at one time optical coating for mirrors used temporary Gallium based amalgams, tin based chemical coating processes, and Silver based toxic plating processes.

Zirconium based coatings tend to keep things "shiny" these days.
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Daedronus
Wed Oct 24 2012, 12:32AM
Daedronus Registered Member #2329 Joined: Tue Sept 01 2009, 08:25AM
Location:
Posts: 370
OK, so, my obsession continues, I got both a diffusion pump and argon (in the small bottles, it turns out some locals stores do sell them, they had like 2 bottles, too bad if someone else needs some...and oh...they don't have the regulators, doh! but I got one never the less).

I don't have the diffusion pump ... yet (or the oil, cooling and connections, for that matter) so this will have to wait for a while

but I did try the argon, and it makes a BIG difference for copper.

In argon the copper sputtering is starting to look right, I got the oh so nice distinct green glow of copper ions (copper self sputtering, free copper atoms ionize and eject more copper atoms, or decay and make the nice green glow):

Link2

And since I now have a pressure gauge, I can tell you it was at about 100 microns in flowing argon.

And yes, controlling the flow from 2bars to 100 microns is a pain, I'm using a restriction (pinched hypodermic needle) a vacuum line regulator for a intermediate pressure and the bottle regulator, that basically I can just open a little and close back.

I also tried silver again, in argon, and it pretty much is a perfect mirror, it was pretty good without argon to begin with...
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Daedronus
Tue Nov 20 2012, 10:39AM
Daedronus Registered Member #2329 Joined: Tue Sept 01 2009, 08:25AM
Location:
Posts: 370
Copper deposition seems like a tough nut to crack. Ether I don't have a clean enough vacuum or I need 5N oxygen free copper.

Right now I have only viton seals, and i can get down to 1 or 2 microns, maybe even lower, I zero out my pressure gauge.
The pressure is so low my high voltage flyback transformer has problems igniting a plasma.
I don't play too much in this regime as I probably get x-rays.

Aluminium doesn't seem to deposit anything at all, or maybe it's Al2O3 that is transparent...
On the aluminium sputter target I got some white power, that's definitely Al2O3.

Titanium works, after it gets hot enough/bright enough plasma, the color of the plasma changes drastically and the pressure takes a nose dive.
The deposition is quite shiny and conductive, so it's not titanium oxide (white) or nitride (gold).

For fun I will try to run titanium with plain air instead of argon, and see if I get the oxide or the nitride.

I will try to get a titanium filament as a getter.
Tungsten doesn't work, there is actually a water cycle that just moves tungsten from the filament to everything else.
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