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    Default Suppliers for high vacuum components?

    Hey all,
    I am working on a process which will have to be conducted under a vacuum of at least 10^-4 Torr. I have sourced a few components already but I would like suggestions for good suppliers of vacuum system parts if you guys know any. Mainly looking for rotary/power feedthroughs, KF flanges and hardware, thermocouple gages, valves, etc...

    So far I know of Lesker and IdealVac, seems like McMaster has a small selection of flanges and pipes as well. Looking for other sites that have online pricing and purchasing if you guys have any suggestions?

    If there are other forums where this kind of thing is discussed more regularly I would love to hear about them as well!

    Also if anyone has experience brazing ceramic and copper/stainless for power feedthroughs I would love to hear about it! I will probably be buying pre-made feedthrough pins and TIG them to blank KF flanges to get what I need but the more options I have the better!

    Thanks guys,
    Aaron

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    Make sure any bolts inside the chamber have vent holes. These can be purchased or drill your own.
    Bil lD

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    Quote Originally Posted by Bill D View Post
    Make sure any bolts inside the chamber have vent holes. These can be purchased or drill your own.
    Bil lD
    Yes sir, will do! I saw McMaster has vented stainless cap screws as a standard item which is great.

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    I just happen to have the June 2020 edition of the periodical "vacuum technology & coating" . Lots of component vedors advertiase or are featured.

    check out vtcmag.com

    accuglassproducts.com has a full page spread on the 5th page ;-)

    at -4 torr, don't worry about screws and trivial virtual leaks. Water vapor on the chamber walls and furniture will be yoiur pumping devil.

    Oh! contemporary epoxy potting is the way to "roll your own" feed throughs. Unless heat over 100C is anticipated.

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    Quote Originally Posted by CalG View Post
    I just happen to have the June 2020 edition of the periodical "vacuum technology & coating" . Lots of component vedors advertiase or are featured.

    check out vtcmag.com

    accuglassproducts.com has a full page spread on the 5th page ;-)

    at -4 torr, don't worry about screws and trivial virtual leaks. Water vapor on the chamber walls and furniture will be yoiur pumping devil.

    Oh! contemporary epoxy potting is the way to "roll your own" feed throughs. Unless heat over 100C is anticipated.
    I knew there would be at least a couple of people on here with relevant experience, I appreciate you chiming in!

    I will check out the vendors mentioned, thank you.

    I was wondering about epoxy sealing for power feedthroughs. For 10-4 torr would I need to use a low outgassing epoxy like 'Torr Seal' or would a more generic adhesive be fine? My process temperature *must* stay below 200ºC max at the substrate but I am not sure what actual process temperature will be yet, depends how much power I need to pump in to get what I need I guess! The chamber and baseplate around the feedthroughs can be cooled fairly easily so I don't think temps around the feedthroughs will be very high.

    What are the best ways to reduce water vapor load? High polish on inside of chamber and on furniture? Likely my chamber will be aluminum and most furniture will be ceramic (for insulating standoffs) or stainless for the actual process furniture.

    I'm real new on this stuff but reading a lot and hopefully learning fast. Throwing myself in at the deep end This was something that started as a skunkworks project and has become much higher priority because of a vendor issue unfortunately...

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    Another supplier:

    Mass-Vac: Vacuum Inlet Traps, Filters and Accessories

    Lesker is very good.

    1 e-4 torr is easily achieved. You could do this with nothing but a mechanical pump and an LN2 trap, or with cryopumps - which are canisters of zeolite that
    are immersed in LN2.

    Depending on how large the chamber is, a small turbopump works very well.

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    Anything with a conflat fitting is usually good to 250C for bakeout purposes.

    I would look at MDC/Insulator Seal. Once you get past the prices cross reference on ebay.

    MDC Vacuum Products | Vacuum Components, uhv Chambers, valve flanges, Flanges & Fittings

    I've never worked with a real aluminium vac chamber only stainless but practice good cleanliness, avoid smears grease etc.

    10-4 isnt a very hard vacuum as far as these things go, a light bakeout will solve your problems.

    Anything in particular you are trying to accomplish? Vacuum science is a very mature technology

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    If you are not in a hurry, time is an effective way to deal with evolution from interior surfaces. A 2 1/2 hour pump can be useful for most vacuum processes at the levels you mention. (Chamber size dependent, Do the math, volume pumps in moments, surface area?.... not so fast there)
    If time is money, a dry nitrogen purge maintaining around 100 microns is Very Effective at moving stuck water molecules down the hole.
    Oil sealed mechanical pumps appreciate the dry pass through.

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    Quote Originally Posted by Maxim View Post
    Anything in particular you are trying to accomplish? Vacuum science is a very mature technology
    The ultimate goal is to get setup to apply DLC coatings myself, definitely not inventing anything new. I understand that it's going to be a bumpy road to get there but I've been having so many vendor issues that I think it's necessary at this point. It's something I've always wanted to do anyway, so now's a good chance!

    I would like to get setup for resistive evaporation coating of Nickel as well if I can, hence trying to shoot for 10^-4 Torr (maybe I need better?), my understanding is that magnetron sputtering doesn't need pressures that low as you'll be flowing argon constantly anyway...

    Smallest chamber I've found with the right dimensions (mainly height) is 10 gallons...

    I don't have much need for 'quick' in this case, happy to just run one cycle a day. Just need to get this process running without the constant mishandling and re-work that I'm enduring now. My current coater scrapped the entire last batch of blades I sent them, and the previous batches haven't been much better unfortunately there aren't many other vendor options around here.

    First go round I'll be running everything manually, but once I get the process parameters worked out I want to rebuild the system so it can run unattended if possible...

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    Quote Originally Posted by aarongough View Post
    The ultimate goal is to get setup to apply DLC coatings myself, definitely not inventing anything new. I understand that it's going to be a bumpy road to get there but I've been having so many vendor issues that I think it's necessary at this point. It's something I've always wanted to do anyway, so now's a good chance!

    I would like to get setup for resistive evaporation coating of Nickel as well if I can, hence trying to shoot for 10^-4 Torr (maybe I need better?), my understanding is that magnetron sputtering doesn't need pressures that low as you'll be flowing argon constantly anyway...

    Smallest chamber I've found with the right dimensions (mainly height) is 10 gallons...

    I don't have much need for 'quick' in this case, happy to just run one cycle a day. Just need to get this process running without the constant mishandling and re-work that I'm enduring now. My current coater scrapped the entire last batch of blades I sent them, and the previous batches haven't been much better unfortunately there aren't many other vendor options around here.

    First go round I'll be running everything manually, but once I get the process parameters worked out I want to rebuild the system so it can run unattended if possible...
    When you get ready for full automation, I have a Denton Discovery unit that is no longer important to me.
    16inch box , dual thermal sources, HV-DC bias rotational substrate holder, PLC automated, fully configurable to any process. Dual gas Mass Flow controls, Turbo pumped. RGA included! ;-)

    Too bad you are not just a bit closer....S.Vt is an entirely different country ;-)

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    Quote Originally Posted by CalG View Post
    When you get ready for full automation, I have a Denton Discovery unit that is no longer important to me.
    16inch box , dual thermal sources, HV-DC bias rotational substrate holder, PLC automated, fully configurable to any process. Dual gas Mass Flow controls, Turbo pumped. RGA included! ;-)

    Too bad you are not just a bit closer....S.Vt is an entirely different country ;-)
    Just looked that system up, looks pretty awesome! Part of me wishes I had the money just to buy an off-the-shelf system, but then I feel like I'd also be missing out on the fun (and frustration) of rolling my own

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    Quote Originally Posted by aarongough View Post
    Just looked that system up, looks pretty awesome! Part of me wishes I had the money just to buy an off-the-shelf system, but then I feel like I'd also be missing out on the fun (and frustration) of rolling my own
    Vacuum systems are just fancy plumbing....

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    Quote Originally Posted by CalG View Post
    Vacuum systems are just fancy *expensive* plumbing....
    Fixed that for you!

    I have been having good luck on ebay so far sourcing components. On average it seems like I've been able to find used components in good condition for about 1/10th of what they are listed for new, but I don't have everything yet... I plan to build the sputter and resistive power sources myself. Building the resistive source will be simple as I'm only aiming it at a single filament type so I don't need to go too crazy on the specs.

    I'm planning to go very simple for the DC sputtering source as well, basically a Variac driving a high voltage transformer, high voltage bridge rectifier, some caps and that's pretty much it. Seems like the basic manual commercial ones are pretty similar. All pretty familiar from my time building tube amps...

    My biggest concern in the short term is just safety with the sputtering power source. I plan to build everything into rackmount enclosures to keep everything locked away from my own stupidity. I will interlock the power source with the vacuum chamber access door and make sure rough vacuum is achieved before it's enabled.

    I have seen some guys mucking about with microwave oven transformers and glass jars doing small-scale sputtering, with bare high voltage wires just running everywhere and that stuff gives me nightmares (as it should!).

    Regarding pump down times and getting water vapor out of the chamber:
    I found an interesting tech document from Lesker regarding the impact of a polished chamber, apparently the reduction in pumpdown time is significant!

    They also talk about igniting a plasma at rough vacuum as a way to speed up the pump-down times which is interesting! Shouldn't be too hard to make the sputter supply do double duty for that purpose.

    Here's the link to the paper, it's short: https://www.lesker.com/leskertech/ar...ougo_part6.pdf

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    Quote Originally Posted by aarongough View Post
    I'm planning to go very simple for the DC sputtering source as well, basically a Variac driving a high voltage transformer, high voltage bridge rectifier, some caps and that's pretty much it. Seems like the basic manual commercial ones are pretty similar. All pretty familiar from my time building tube amps...
    A sputtering power supply built in the 1970's consisted of a 3 phase SCR fed 240 volt to 1000 volt transformer with optional output taps at 750 volts and 500 volts. The transformer output was fed to a 3 phase rectifier, a small capacitor and then through a large inductor. There was also a set of metal oxide varistors connected to the output.

    The inductor was required to limit the current to the sputter source target during the frequent arcing events. The SCR controller ran at line frequency to regulate output voltage and was useless for limiting the arc current. The varistors limited the damage to the power supply when the inductor voltage peaked during a arc. These early power supplies were used because nothing else was available at the time. A arcing event would frequently destroy the substrate being coated. The power supplies can be found at junk yards and are priced based on their copper content.

    By the late 1980's the SCR power supplies had been replaced with compact light weight switching power supplies with milli second arc shutoff response times , very low stored energy, and control logic for delays in turning the power back on.

    By 1995, these supplies were replaced by mosfet based power supplies with micro second shutoff times and even lower stored energy.

    Around 2000, the power supplies were replaced by switchers which allowed the user to program a positive voltage pulse running at a duty cycle to prevent a arcing event from occurring. This last improvement has allowed significantly faster sputter deposition times.

    The current generation of power supplies introduced in 2015 has increased reliability and additional control of the voltage pulsing.

    Making your own power supply is a waste of time. You can buy a 1990 vintage 5 kw Advanced Energy sputter switching power supply for $300 on EBAY. The faster response time early ENI power supplies are also available. at low cost.

    These supplies are obsolete by current standards and the price reflects that status. The switching power supplies are a consumable in industry. The earlier models used transistors rather than mosfets and were very complicated and difficult to repair. The newer supplies have fewer and more durable components.


    The design of DC sputtering sources has also undergone several generations of design improvements. The improvements are driven by the need for better deposition rates, better substrate film uniformity, better target utilization, fast turn on time and optimum film growth. Some sources have modified magnetic fields to direct ionized as well as electrically neutral particles to the substrate to control the film growth.

    The sputter sources may look simple and easy to make. They are not.. A afternoon spent reviewing the online patents will give you a better idea as to what is involved.

    Modern DLC coatings are produced using cathodic arc sources rather than sputter sources. In the past these films have been made using ion beam sources or by plasma enhanced chemical vapor deposition. The basic requirement is a source of ionized carbon. Sputter sources produce primarily electrically neutral particles. Their use is limited to depositing carbon films. An example of this application is the carbon film applied to disc surfaces in magnetic storage. The thin film prevents damage to the read head when there is unintended contact with the disc.

    There have been major improvements in DLC film quality in the last few years. Kyocera, among others, now offers a DLC coating service in the US. A large batch arc deposition coater is about 3 feet in diameter and four feet tall. The interior contains several vertical rotary planetary substrate holders. One of these machines can process a batch of several thousand inserts. You will find that the cost of the coating service is modest compared to what you are about to spend in an attempt to recreate a DLC coating that was obsolete 30 years ago.

    Balzers made the transition from sputter systems to arc deposition systems about 5 years ago. The coating time for a multilayer tool coating went from 12 hours to 6 hours with improved film properties.

    Coating - KYOCERA UNIMERCO


    One more comment:
    The base pressure of a sputtering system is in the 1.0 E-6 torr range or lower. The low base pressure is required to remove reactive gases such as oxygen from the chamber before sputtering can begin

    The base pressure can be achieved more rapidly with heat , UV light, or a glow discharge dislodging the oxygen or water vapor stuck to the chamber walls, fixtures, and substrates.

    Oil contaminated substrates can be cleaned prior to coating in a oxygen glow discharge.

    Sputtering gas pressures are in the 1 to 5 E-3 torr range. Sputtering is done with a continuous Argon supply in the 10 to 100 sccm range depending on chamber size with the high vacuum pump running continuously to flush out the reactive gasses in the chamber.

    My knowledge on this subject is from the 1990's. Things may have changed in the last 20 years.
    Last edited by Robert R; 06-27-2020 at 09:27 AM.

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    Quote Originally Posted by aarongough View Post
    The ultimate goal is to get setup to apply DLC coatings myself, definitely not inventing anything new. I understand that it's going to be a bumpy road to get there but I've been having so many vendor issues that I think it's necessary at this point. It's something I've always wanted to do anyway, so now's a good chance!

    I would like to get setup for resistive evaporation coating of Nickel as well if I can, hence trying to shoot for 10^-4 Torr (maybe I need better?), my understanding is that magnetron sputtering doesn't need pressures that low as you'll be flowing argon constantly anyway...
    ...
    Look at the melting point of nickel. It's pretty high. You basically need an E-beam setup to do evaporative Ni. Sputtering maybe a better choice? Another point to ponder: There's a general rule in vacuum systems - at about 1e-6 pressure, you are depositing one atomic layer of stuff on your substrate per second. If you are not actually putting down your material, that stuff is junk. Water vapor, other outgassing from your chamber and pumps. Even though the argon flow raises the pressure in the chamber, the base pressure still counts.

    Back in the day we used to use an LN2 shroud around the e-beam gun, and then deliberately evaporate niobium before putting down our real evaporant. The niobium would "getter" the atmosphere in the chamber, that is, adsorb any residual gasses. We could cheat and get a factor of ten lower base pressure that way. This was a chamber pumped with an 18 inch diameter cryopump.

    You plan is ambitious - compare the tradeoffs in your time, money, space and effort, with the costs of having your material coated by an outside vendor.

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    Aside from the vendors you mentioned there is also Agilent, ThorLabs, and Newport that I have some experience with. There are many others.
    If you don't already have it then I would also recommend https://www.amazon.com/Building-Scie.../dp/0521878586 which has a pretty good discussion of high vacuum technique and the construction of high vacuum apparatus. Stuff that is difficult to get from vendor sources because... they are interested in selling you their stuff and services not in telling you how to build your own.

    -DU-

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    Quote Originally Posted by Robert R View Post
    You will find that the cost of the coating service is modest compared to what you are about to spend in an attempt to recreate a DLC coating that was obsolete 30 years ago.
    Quote Originally Posted by jim rozen View Post
    You plan is ambitious - compare the tradeoffs in your time, money, space and effort, with the costs of having your material coated by an outside vendor.
    Hey guys!
    Really appreciate all the info in your responses, thank-you for taking the time! Lots of great info there that I will unpack with further reading!

    Just so you guys know: this is not really a project that I am taking on lightly... I would prefer to have an outside vendor that I can simply trust to do the job, but that has proven to be elusive.

    I have a local vendor that I have been dealing with for more than 5 years for DLC coating. They were a bit difficult right from the start as their owner & staff do not have the best communications skills. That gap was bridged by their sales guy who was great, but the sales guy was either fired or left in frustration about 6 months ago, I have been unable to get the full story. Since the sales guy left their already inconsistent quality has gotten much much worse...

    The last batch I sent them was 60 blades and every single one came back with handling & smudge marks. There were even obvious fingerprints on some of them, which are now incorporated nicely into the DLC and impossible to remove except by blasting the coating off. When I contacted the owner to try to straighten things out I asked him to confirm that they had been ultrasonically cleaned before processing as that has been an issue in the past. He said they had not as they 'looked clean enough' so they didn't bother. When I suggested that perhaps the lack of strict adherence to a consistent process was an issue he said 'its not the problem'.

    Never mind that 'all parts must be ultrasonically cleaned' is the first item on the spec sheet that I send them with every batch... If I can't trust them to follow a simple instruction like that, what about my other requirements? Are they sticking to the max process temperature that I specify??

    If I can't trust a vendor then I have no use for them.

    There are only 3 vendors in the province where I live that do DLC. One of them is so bad at communication that I have only ever gotten a single email back from them. One is the company I have dealt with already. The third company I am currently in talks with and they have some sample blades to process. I can't say I'm overly hopeful though as their facility was dirty when I visited and they had employees wearing shorts and soft shoes moving heavy items and so on...

    I have considered shipping the blades further away for coating either in the US or in another province here in Canada, but I'm concerned that I would have similar issues and not even have the recourse of visiting to talk them through. Sending valuable nearly finished product back and forth across the border also promises to be a nightmare of duties misunderstandings and lost packages as well I think.

    If you guys have recommendations for a coater who does fantastic work, communicates well and is happy to do relatively low volume work then I would certainly love to hear about them!

    The main driver for wanting to bring this in-house is that I have learned the hard way that no company's management or employees are going to care about my product as much as I do.

    If I had the capital I would take CalG up on his offer of buying a machine ready to go, but since I'm relatively capital poor and time rich I need to take the other option instead I think!

    There are a couple of other factors: 1) I find projects like this extremely interesting, and I'm fine with spending a couple of grand simply to learn far more about a process that I rely on so much. 2) My customers love seeing me take on projects like this, and I will be documenting the process for Youtube so there is 'marketing' value in the project as well as process value.

    I completely agree that an outside vendor would be the far simpler and more cost effective option overall!
    -Aaron

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    Quote Originally Posted by aarongough View Post
    There are a couple of other factors: 1) I find projects like this extremely interesting, and I'm fine with spending a couple of grand simply to learn far more about a process ...
    -Aaron
    I'm going out on a limb here and am going to say to do this so it actually works reliably ever time, you should be considering spending between $10K and $100K. You can
    purchased used stuff and fix it up of course. What's your time worth.

    Lesker will sell you a custom, turn key vacuum system like that. Many years ago we bought one off-the-shelf more or less. Two sputter guns, mutiple pocket e-beam gun,
    supply for the e-gun, two sputter sources and a plasma gun, a couple of rate monitors. System was pumped with a dry scroll pump backing a turbo and then a large cryopump for the main chamber. Basically just plug in the power, cooling water, process gas, and go. That was around $200K or so about 10 years ago, and we considered it money very well spent.

    You don't have very extensive requirement I know, but you need to worry about vacuum gages, rate monitors, and a way to translate or rotate your item you are coating inside the chamber so it gets fully coated.

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    The DLC coating process is more complicated than it first appears. It is a multilayer film. It consists of a chrome adhesion layer followed by a chrome-carbide thermal transition layer and finally the DLC film. Chrome is the universal glue for attaching films to glass or metals. The transition layer is required to prevent film cracking from the thermal expansion mismatch between the substrate and the DLC layer.

    The development of the process recipe is very time consuming. The patent applications do provide the recipes. One could copy an existing successful process. If you were determined to do this kind of work your best option would be to wait for one of the obsolete Balzers DLC coating systems built in 2001 to show up on the surplus market. These were combined chrome sputter and e-beam assisted chemical vapor deposition systems using acetylene as the feed gas for the carbon source.

    If you read German the international patent number for this older process is WO 01/79585.

    There are a number of Balzers coating centers in the US. They will do exactly what you want at a competitive price. The Kyocera coating center is another option. The large coating centers run 24 hours/day and offer quick turn around for standard tool shapes. For some geometries the major coating centers may reject the work if it requires non standard fixtures. If that is the case you are stuck with the smaller high cost low volume coating companies.

    If you would like to know more about the current generation of DLC coatings, fixture layout or how modern deposition systems are constructed spend a few minutes on the Balzers website.

    http://www.oerlikon.com/balzers/com/...linit-dlc-star

    Your time is better spent studying the online DLC patents than it is looking through the vacuum chamber components catalogs.

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