Evaporating Metal in a High Vacuum to Coat Glass and PLA - PVD
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- Опубліковано 16 чер 2024
- In today's video, I'll be using my vacuum chamber to vaporize metals like copper and silver, applying them to glass surfaces and 3D-printed parts. This coating process is known as thermal evaporation and falls under the umbrella of Physical Vapor Deposition (PVD).
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Huygens Optics: / @huygensoptics
AGS-Braunschweig: www.ags.tu-bs.de/
Sources fort he pictures:
en.wikipedia.org/wiki/Physica...
voc-vacuum.com/en/virtual-leaks/ - Наука та технологія
Some might say 20mm copper is overkill. But can you even call it a high amperage pass through if it can't handle currents in the kA range?
Not only that but you would need lot thicker conductors in vaccum.
Any conductor has losses and in a vaccum it would be able to overheat.
I didn't research this I'm just going off from vaccum being thermal insulator
@@blackturbine I calculated the max current with the assumption that the water cooling is used. But even without it the heat will conduct through the walls of the pass through and it should be fine.
@@MaxWithTheSax i commented before I realized he was using water cooling but yeah with copper being so thick it would conduct enough heat away passively.
Thank you for responding :]
Watching metal get deposited on those glass slides in real time was amazing.
I think some of the surface finish issues you encountered at the start might also be due to boiling the material too quick, which ends up flinging some tiny drops of metal at your target as well. I encountered something similar during my master's thesis with a commercial evaporator in a cleanroom.
You are definitely right! When evaporating the silver for the first time, I raised the temperature too fast and I could see the metal spatter a bit.
When using the copper, I raised the temperature slower and and coating was a lot better. But you could still see some of the contaminations that came from the glass.
I wonder if you acid etch (or sandblast) the glass a small amount if the metal would hold on better, less likely to scratch or peal off.
I think I will try that.
Yup, you want it hot but not actively boiling the metals. Are you planning on using your chamber to sputter coat as well as thermal evaporation? Maybe even try your hand at building an E beam evaporator. Then you could do nonmetallic coatings of stuff that would react with the boats. Happy tinkering.
Yes, electron beam evaporation is also planned. But I would have to do a lot lore research about the design.
Nice! This is well into Applied Science territory in terms of coolness.
Thank you! I'm a great fan of him so that's a huge compliment!
We use Polyimide (Kapton) tape all the time with our PVD setups. Additionally, certain materials tend to "spit" when you ramp the power at too high of a rate. The shutter should be effective in reducing that issue, but I would try and ramp up the power slowly initially to avoid those spots you see on some of your depositions.
Yes, I definitely ramped up the temperature too fast when evaporating the silver. I could see it "spit". When evaporating the copper I raised the temperature slowly and did not get those spots on the glass surface.
How do you prepare the glass surface before coating it? And which metals do adhere best to glass surfaces in your experience?
Thanks a lot for the information!
@@AdvancedTinkering Ideally, we follow an RCA clean procedure. Though you can usually get away with Acetone/IPA/DI w/ ultrasonication. Cr and Ti both work really well as adhesion layers for SiO2. Generally, we find that Ti is best for Si and Cr for SiO2
Nice video. You did a great job on the build. And what a clever thermal evaporation source design!😊
I'm very glad you liked the video! Even though it wasn't nearly as detailed as yours.
Yes, I got the design for the thermal evaporation source from a brilliant video about PVD ;)
To get the metal to stick to glass first bake it dry, then deposit a thin layer of titanium on it, then apply the desired metal. ❤
Thanks for the advice! I will try that!
Huygens optics is awesome, he does a lot of PVD for his first surface mirrors
It's always a special treat to "see" a metal as a gas especially transition metals like copper, silver and gold considering that metals don't typically become gases (at normal atmospheric pressure) unless we reach nearly impossibly high temperatures of well over 2 kilokelvin!
Definitely. I thought about creating a plasma to excite the metal in the gas phase. Or maybe just build a sputtering system.
@@AdvancedTinkering I'm down with that! I'm curious to know what colors metals like say gold and silver are as plasma!
@@AdvancedTinkering I would love to see your experiments with this!
When i was using thermal evaporation at university, we used glass wool over the evaporated sample in combination with shutter to reduce sample contamination. It is amazing what you can do in a home lab :)
I used to do this for work as a teenager. We used to coat the reflectors for maglight flashlights and the old school Nokia phones .
That’s a massive high vacuum chamber. Also, Applied Science has video on cleaning glass already, but I guess another one won’t hurt.
Yes, his videos are great. I have seen the one about the cleaning process. I doubt mine will be nearly as detailed as his.
While that's definitely a really large vacuum chamber for someone to have at home, the semiconductor industry utilizes significantly larger chambers (we're talking 60 cubic feet or more) that hold roughly the same pressures. Buuuut the pumps are, of course, much bigger as well.
As a new silversmith and enamel artist this is like magic to me. I had no idea this was possible until this week
This is absolutely amazing! Really inspiring!!!!
One tip. Do not EVER use brass inside vacuum chamber. Zinc inside brass has tendency to get out and ruin your Vacuum, also in this kind of application it will get inside your layer.
Vielleicht kannst du auch so versuchen Blattgold herzustellen. Cooles Experiment!
Puh, Gold wäre dann doch etwas zu teuer für mich ;) Aber es gibt ja noch genug andere Metalle, die man testen kann.
Good work! Very cool.
Love that feedthrough design, awesome stuff!
Thanks! I'm very interested to see how the feedthrough holds up over time.
Amazing stuff at a home DIY workshop... Hats off, and keep up the good work!
You can take a low power incandescent lamp and ramp up the voltage to the point where the lamp runs too bright but doesn't melt. after a while, lamp will slowly turn opaque due to tungsten deposition.
Very nice! I had fun evaporating titanium, and you can modulate the color of the deposits by varying the pressure of the chamber-- I got some very beautiful gold-colored layers this way. If you're not too concerned with coating things around your chamber, you might try the much cheaper stranded tungsten wire heaters, wrapping a bit of the desired metal around the tungsten, where it will melt and wick onto the heater wire before evaporating. Another cool experiment I tried was evaporating silver onto paper, and it doesn't take much to become quite conductive. You'd think the rough surface of the paper would prevent this, but it works very well.
Very cool! I also wanted to evaporate titanium to see if I can get some pretty interference colors. Do you remember at which pressures you evaporated the titanium to get the golden colored layers?
This is pretty cool. I use to run a very large PVD coating machine via sputtering for coating automotive windshields to reflect sunlight and uv radiation.
Those are realy nice results.
Thank you!
This is one of the most interesting demonstrations I have seen
Thank you! I'm glad you found it interesting.
It's content like this that makes YT great, keep up the great work! That MOT is hot...:)
Thank you! I appreciate hearing that you like the videos!
That's a sweet chamber
Trade secrets.
Very nice👏
that copper coating looks beautiful
Neat setup. I have a smaller chamber with a smaller Varian diffusion pump I used to use to coat Mylar with about 150 angstroms of gold to make condenser microphones. I haven’t made them for quite a while though.
Love your build! Going to try some of your design improvements to my basic thermal evap setup (no cooling, just copper bolts in aluminum base to hold tungsten boat and chamber as ground); love your large chamber!
This is a fantastic video, and a really interesting topic.
Back in the 90s I briefly worked for a company that coated glass using the sputtering process. Mostly I worked in color filters, but spent a couple of weeks testing glass that would act as a light filter for solar panels in satellites. (blocking most of the sun's full spectrum light, except for a narrow band, preventing the solar cell from burning up) That glass was only 0.004" thick, and really easy to break. We also put coating on that would reduce the amount of light reflected from the glass. My job was running the glass pieces through a spectraphotometer to make sure the coating was the exact color, according to customer specifications, cut the glass to shape and discard the pieces that were out of spec. Then environmental testing, which consisted of rubbing the coating with an eraser to make sure the coating didn't peel off.
I must admit, I very much envy your high-vacuum setup man, everything looks so refined and professional! I had a basic vacuum setup a while back that could get down below 100 microns, but it was very finicky, and the pump died some time ago. Keep up the good work, can't wait to see what you use this for in the future!
I use a lot of the same fittings and components at work, can confirm this setup looks like a scaled down & simplified version of an industry equivalent PVD chamber, just a lot more manual and less automated.
This turbomolecular is sick 😮
With this power supply it is possible to setup a rather primative DC cathodic arcs deposition system, I think that'll be rather entertaining!
In fact, you can easily add 3rd crucible as well, nice design :)
You are right! I didn't think about that possibility.
Super! Thank you very much!
Amazing i really enjoy learning what you do much appreciated
Thank you! I’m glad you enjoyed the video and learned something.
Huygens was an OG
Wave Theory of Light: Huygens proposed that light was a wave phenomenon, countering Newton's particle theory. This was a fundamental shift in understanding light and laid the groundwork for later wave theories.
Huygens' Principle: He formulated this principle to explain how wavefronts propagate. It states that every point on a wavefront acts as a source of new waves. This principle is fundamental in understanding wave optics.
Pendulum Clock: Huygens invented the pendulum clock, which was a major advancement in timekeeping and greatly improved the accuracy of clocks.
Titan Discovery: He discovered Titan, Saturn's largest moon, and studied Saturn's ring system, making significant contributions to astronomy.
Huygens-Fresnel Principle: Together with Augustin-Jean Fresnel, he helped develop the wave theory of light, which was a crucial step in the field of optics.
Mathematical Contributions: Huygens made notable contributions to the field of probability and dynamics, including work on the theory of evolutes and the centrifugal force in circular motion.
Nice work.
Thank you!
Many thanks for opening an enterely new and fascinating topic. The field of applications is just endless. For example, I believe the coated goggles can be used for direct sun observations or welding purposes. Further, you could build your own reflecting telescope. Last but not least, if you try to evaporate graphite you should be able to deposit tiny diamonds.
Yes, there are many interesting possibilities. I think the hard part about making optics would be the the precisely ground/shaped glass surface. And I think channels like Huygens Optics are way more capable in that area.
I don't think it will be possible to evaporate graphite. Or do you have any information about that? I would be very interested because I'm thinking about making diamonds via CVD for a long time but it's a pretty involved process.
@@AdvancedTinkering "I don't think it will be possible to evaporate graphite"
Really hard to do if you want to stick to just a crucible. One option would be to use a laser for that: Heat up the carbon with electricity and use a laser for the last push to evaporation. But certainly that is not easy as now you have to deal with all the problems of having high-powered laser-pulses on an evaporating material. Can lead to some nasty splattering.
Love it! I used similar (Hysol 1C) 2-component epoxy to make some custom holders for weird shaped samples for a e-beam/thermal evaporator. Super low outgassing. Nice video overall.
Great video! Gut Gemacht!
Danke!
Good job
Thank you!
Greetings from Hildesheim, great vid!
Greetings back! Thank you!
this would be so cool for DIY parabolic reflectors, especially since you could probably resin 3d print the reflector shape and then coat it after, youd have so much creative freedom
Wow much much greatful thank you 👍👍👏👏🙌🙌✨👑🔥🔥
It requires a little more attention to safety but you might try piranha solution for cleaning glass. Just make sure that you don't try with anything organic!
Awesome results and video! Thanks for taking the time to also share this with us.
That is nice dude
Great video, thank you. A video including a piezoelectric sensor that measures the layer thickness would be awesome, I like that idea
Hello. You could try to use a special formulation of transfer tape using low outgassing acrylic compound like 3M 9703.
We use it on spacecrafts all the time and it works really well for lightweight components which needs to be electrically conducive.
I recently found a Leybold TurboVac 350i unit which had been discarded. I was wondering what it was so started researching and came across your channel. Cool stuff!
There were actually 2 such units but not knowing what it was at the time I only acquired 1 of them for a mere $20. 😀
Now to start seeing if I can get it in use...
Great video! The Huygens optics guy's channel is awesome too, was happy to find it mentioned here. Huygens I think should be pronounced Dutch, as the physicist Huygens, and would read roughly as 'hau-kchens' as a German reader, with the kch sound being a typical Dutch throaty g sound as the 'ch' in the German 'auch' :D
Thank you!
Ah, that's good to know :D thanks!
Very cool to see you work on pvd! Im going to grad school to work on a few pvd techniques (molecular beam epitaxy and sputtering) since im currently a senior undergrad. Impressive setup for sure! Id love to build a setup like this one day. What are some of the future projects that you are thinking of with this system?
make glass circuit boards with it. glass circuits would be so fancy and cool wouldn't it?
I’m definitely going to try that. If you have any ideas for a circuit, let me know.
Since the vinyl tape was able to survice the process, you can probably simply use thin slices of viny tape to fix leaks in the coating container to safeguard your vacuum chamber.
Awesome
Wow! 20mm copper rod! I managed to fit two rods in single KF25 flange :) You have very nice setup!
Thank you!
Soo good
Thank you!
Ground glass surfaces would hold the metal better, perhaps? Also structural colours would be interesting, if you can peel off the metal foil with the surface structure that causes different colours.
Nice.
Well done they look amazing how are you doing
Cooles Video
Danke!
your vaccuum chamber looks like the apparatus from Flubber
One thing that might be interesting to try is indium tin oxide. In thin layers, it's completely transparent yet quite a good electrical conductor (think touch screen). I'm not sure if it needs a sputtering setup, though.
You could combine this with simple electroplating to do some cool things.
For example you could coat plastic 3D prints with some cheap but conductive copper, and then nickel plate them.
Then you can buff out the nickel plating to get that perfect shine you want.
Nice to see your setup working this well. Really amazing that you can get nice mirror finishes.
If you take a second cruible, make a tiny hole in it and put it onto the first crucible upside down, you might be able to get a nice pencil beam.
Did you consider using ellipsometry to measure the thickness of your deposit?
Interesting idea to use a crucible with a hole inside. I will try that out.
I haven't thought about ellipsometry to measure the thickness. I honestly never heard of it. But I will take a look into it.
@@AdvancedTinkeringif you are near a university with their own characterization facility (and with X-ray diffraction capability) you might be able to ask them if they could perform x-ray reflectivity on your samples to see thickness and determine growth rate. If that's something important to any future projects!
@@ianmercer1291 You can also measure the thickness of metals if they are thin enough with spectroscopic reflectometry, which is a bit easier and cheaper.
Very High Vacuum = "Danger." +Very High amp Electricity = "MORE Danger".. Very Hot Molten metal vapor = "Even More Danger" ..
I like where this is going ....
Good thing you have your Shiny Safty Squints.
Safety squints are always engaged ;)
10:50 To use vinyl cut lettering, you should cut the lettering with the backing paper still attached, remove the unneeded parts while the cut letting is still on the backing paper and only then use transfer tape to transfer it to final surface. Even then the "remove the unneeded parts" is a bit tedious but with a flexible surface and much less stickiness, it's still much easier.
Congratulations for the experiment! Not many companies can do PVD but you managed to do it at home. How do you plan to use the piezoelectric sensor to measure the thickness ?
If you heat your object the coatings hold a lot better. A way to clean is to coat the object with a thin oil film and evaporate it in heat and vacuum.
Awesome, you could help people with classic cars, motor cycles to recoat their headlights.
: )
Tip, use mixture of little bit battery h2so4 and alume Aqueous solution on aluminum or ceramic pot and heat it untill broken steel bit desolved in the copper without doing anything to Aluminium brass or copper metals.
5:07 You could actually power up to three different crucibles. Running power trough connectors A-B, A-C or B-C
Hab mich schon die ganze Zeit gefragt was du mit der Vakuum Pumpe anfangen willst😂.....aber das ist richtig geiler scheiß😁👍
Very cool! I wonder if the foil peeled off due to different thermal properties.
The silver safety glasses should be perfect for observing nuclear tests!
wonderful experiment you run there! but i was thinking does the copper and silver piece generate a millivoltage like a thermocouple?
Thanks! Very interesting question. I will try and see if I can measure some voltage when I heat a similar piece.
Metal becomes transparent if you make it thin enough, iridium enhances light. Gold enhances color.
You can also try applying a shielding layer of Silicon Monoxide, as they do for optical front surface mirrors.
(Came here from Huygens Optics)
You didn’t mention any current control for the heater, adding either current or temperature control could be a good idea to help get more consistent results.
As for your piezo sensor to allow you to measure the thickness of the metal, that sounds really interesting, can you share any details about that?
Love that you designed an extremely complex extra water cooling step that, because you didn't actually test if was necessary to begin with, just.. was a whole part of this video that was unnecessary lmao
Haha! Yeah, I did spend way too much time building the water cooling system. I even had to order the thick-walled copper pipes from China. Well, at least now the design is future-proof in case I ever need a lot more current.
use a base bath with isopropyl alcohol and sodium hidroxide to clean the glass
I have developed this instrument for scientific use.For a dense coating, the substrate may have to be cooling.This takes into account the melting point of the material and the thickness of the coating.
I have done a great deal of electroplating, which has resulted in a wide range of quality of plate jobs. I'd be very curious to compare conventional electroplating to these types of PVD based plate jobs.
I think the real use for this should be gold-plated astronaut ice cream. 😏
Since you're basically making mirrors - why not use a mirror to monitor the deposition process while providing shielding for the rest of the chamber / line of sight?
Accidentally turning a mirror into a mirror wouldn't be too bad
Very impressive. I got an idea that i wish to see: why you don't try printing a circuit board on 3D printed part, or even on glass, and by uaing very thin glass (telescope glass) then you might end with multiple layers circuit board by stacking the predesigned circuit 😍
@AdvancedTinkering can you please us tell me why you were pulling vaccum in the cesium vedio after 1st distillation where you can just seal all the openings including the vaccum pump and maintain inert atmosphere in your apparatus
What if you covered the inside of the safety glasses with the vinyl and only coated one side, would it make a difference in being able to see through them??
No, the glasses are actually only coated on one side. But it's completely reflective on both sides.
I would have to make the coating a lot thinner to be able to make it see-through.
The amount of material used to coat a small glass surface so it will be opaque is so small that it will be measured in milligrams or even that.
Have you considered giving the glass a light sanding before deposition? It's to make it adhere to it.
mega geil! ich hab auf Arbeit auch eine ungenutzte Vakuumkammer und viele der benötigten anderen komponenten. Ich hoffe das ich das in zukunft auch mal bauen kann! Wie lange hat es so gedauert um das Glas zu beschichten? Im video sieht es so aus als ob wirklich ein paar sekunden gereicht haben? Und hast du deine Vakuummessröhre irgendwie besonders abgeschirmt? Wäre glaube ich ungeil wenn das Pirani Element mit zusätzlichem Metall beschichtet wird (?) xD
Danke! Das Beschichten hat wirklich nur ein paar Sekunden gedauert. Das Video wurde an der Stelle nicht beschleunigt.
Meine Vakuummessröhre (in dem Fall ein Ionisationsvakuummeter, da Pirani Sonden bei dem Druck nicht mehr funktionieren) ist am Boden angebracht und liegt nochmal ca 2.5 cm in einem KF25 Flansch. Da sehe ich keine Gefahr, dass es mit beschichtet wird. Wenn die Sonde in direkter Linie zum Wolframschiffchen steht, würde ich sie definitiv abschirmen.
@@AdvancedTinkering alles klaro super zu wissen! Vielleicht komme ich in Zukunft ja mal dazu das zu bauen. Vielen Dank für den Content und weiter so! ;)
Can the stencil be dissolved in an HF acid bath or would that also remove the PVD metal (such as silver)?
Since you used JB weld in a dielectric for your first DIY passthough, Ill head off the inevitable "OMG JB weld has metal in it!!1!" comments. Bulk JB weld is an insulator, as there isnt enough metal loading for JB weld to be conductive, unless you compress the bondline during curing, to the point its thin enough both of your parts are crushing the iron fill.
Haha, I actually expected a comment like that. But you are right, JB weld is non conductive.
I still wouldn't use it for high voltage stuff though. I would imagine the breakdown voltage is a lot lower due to the metal.
At the extremely low voltage, about 2V or so its not gonna be an issue❤
You should plasma treat the surface of the glass to stick the metal way better
That's the plan.
Is there a way to attract the metal vapor in a precise manner instead of the scattering?
You could use some kind of aperture to let the metal only come out there. Or you can use a stencil (like I did when I applied my channel name to the glass). For very intricate structures, photoresist is the best option.
Lots of questions and fun experiments, I'd especially love to see the results of depositing bismuth metal.
Pure metals are interesting, but I've always wondered how this process works with alloys? Would something like aluminum bronze work? or maybe you could use the process to make alloys via deposition by running more than one crucible at a time, or in short bursts back and forth? Could you deposit tungsten itself by using a thin filament as the conductor so it will evaporate from the current? Is this a way to make novel tungsten alloys? Is it possible to deposit non-metallic elements such as graphite? could the process be slowed down to encourage crystallization? Makes my imagination go wild lol.
Looking forward to more videos about it.
The copp3r is soooo pretty
Don't limit yourself to metals! Ceramics are perfectly suited to being used in thermal vapor deposition. I've even seen plain glass (SiO2) used.
pretty cool! I love playing with modified MOTs :) How do you control the power? with a variac?
You could probably make PCB's using a mask for the tracks no? That would be a cool project.
Yes, I used a variac. Yes using photoresist or detailed stencils I should be able to make pcbs.
@@AdvancedTinkeringooh, you could use ceramic as a substrate!
Yes, I want to try that. It may even be possible to solder or braze metal to the coated ceramics and make vacuum tight connections this way.
Or I could integrate circuits into 3D printed parts.
Would the copper-coated silver now be a thermocouple?