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  1. #21
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    Quote Originally Posted by jim rozen View Post
    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.
    Buying used and fixing things up is how I operate pretty much all the time anyway so no issue there. I hate being in debt and like to keep my fixed costs low so I have pretty much operated my business that way from the start. I actually quite enjoy that kind of work, and I have definitely gotten my money's worth that way! My most recent VMC purchase was $4,900 plus about $5k in parts and a month or so of part-time working on it in between 'real' work, it is up and running now 8 hrs a day and making good parts! I'm not too worried about that side of things.

    I am working on finalizing the purchase on a large lot of plumbing/valves/etc from a custom PVD line that was built and then never put into operation and they are basically scrapping the whole thing out. Seems like I should get a lot of stuff I need from that for very reasonable prices.

    I have also bought a Leybold Trivac oil-sealed rotary vane that should do the bulk of my pumping, if I need more pump than that then I have a line on options for a turbo pump or a diffusion pump...

    I think I will start smaller than I was originally planning: just a resistive source inside a ~1L chamber made from glass. I will make the chamber disposable and have it do double duty as the test substrate while I figure out the early steps.

    That way I can get my feet wet without too much investment, and move toward the stage of knowing how much I don't know, as opposed to where I am now where I have no idea how much I don't know At least that makes it easier to be confident about tackling the problem

    One thing I was thinking in regards to Robert's comments earlier regarding sputter power sources:

    I think that with a lot of things the tech is pushed by the needs at the cutting edge, most likely semiconductor thin film coatings in this case. In that application it totally makes sense that a 1% improvement in uniformity or cleanliness would have a huge impact as just a couple of atoms in the wrong place can probably scrap a die or wafer... I guess for me that system would be equivalent to a Kern 5 axis machine, with the pallet changer and all that. I just want the 3 axis Fadal or maybe even the Tormach (gasp) of thin film coating systems, no fancy options just the bare minimum needed to run a particular process reliably. If I can apply a DLC film with a 10% reject rate then I'll still be doing better than my current vendor has been at least

  2. #22
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    Quote Originally Posted by David Utidjian View Post
    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-
    Thanks David! I have heard others mention that book a few times but hadn't yet picked up a copy, I will get that today!

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    Quote Originally Posted by Robert R View Post
    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 60 page international patent number 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 constructed spend a few minutes on the Balzers website.

    //www.oerlikon.com/balzers/com/en/portfolio/balzers-surface-solutions/pvd-and-pacvd-based-coatings/balinit/carbon-dlc-based/balinit-dlc-star/
    Thanks for the links Robert! I remember speaking with my vendor about how the coating actually had a couple of layers in it, but hadn't heard about anything beyond a Chromium Nitride adhesion coat and the Carbon top-coat, I believe they 'dope' their carbon with Tungsten and some other stuff but of course the are circumspect about the exact recipe.

    Unfortunately the blades that I refer to as the substrate in my case are actually hunting/camping knives, so very much a non-standard geometry! When I first started working with my current vendor they had me pay $1k or so for a custom stainless christmas tree fixture, which they later abandoned anyway in favor of simple stainless wire hangers attaching the blades to a circular stand which goes on the central carousel. They do not independently rotate each blade around it's axis though, which has caused some uniformity issues in the past during the plasma cleaning stage...

    You can see my work (and what I'll be coating) here: Resolute MkIII - DLC - Black w/ Green Liners – Gough Custom

    The substrate is A2 tool steel, grit blasted to achieve the matte finish. I soon hope to swap out the grit blasting process for a process which uses zirconia ceramic beads as the media to get a matte finish with lower overall roughness.

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    What kind of conditions do you need to achieve, how do you plan to crack the gas and what is your carbon source?

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    Quote Originally Posted by aarongough View Post
    You can see my work (and what I'll be coating) here: Resolute MkIII - DLC - Black w/ Green Liners – Gough Custom
    .
    The knife blade will fit within a cylinder 1.5 inches in diameter by 10 inches long. There will be a planetary fixture in inventory that will handle that. You just need to supply the knife blade with a temporary 1. inch diameter by 1.5 inch long pin that is clamped to the knife handle with set screws. The pin will fit the coater planetary tool socket in the same way that a large end mill does. The blade will be coated on the fixture used for the large diameter gear hobs and broaches. Balzers may want different pin dimensions but the idea will be the same.

    I realize that you are still determined to make your own deposition system. However you still need to make knife blades until that happens. Spend a few minutes talking with a Balzers engineer and have a drawing ready to email showing a blade with attached pin for a price quote. It would be best to supply the blades in a batch size that will fill one planetary fixture..

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    Cathodic arc= TIG in a vacuum

    Call it Tungsten in Vacuum = TIV ? ;-)

    Your choice of filler rod ;-)

    More simply, carbon arc "burning". ;-))

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    The knife blade will fit within a cylinder 1.5 inches in diameter by 10 inches long.

    A tube furnace with a quartz tube and QC oring fittings is a standard way to do a vacuum chamber like this and will work up to 1200C and maybe -6 torr or 7 torr with viton fittings and a small turbo pump.

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    Quote Originally Posted by aarongough View Post
    I have also bought a Leybold Trivac oil-sealed rotary vane that should do the bulk of my pumping, ....
    Consider that if you leave that pump on the chamber for any length of time, once the pressure goes below about 20 microns (more or less the lower limit acheived by that pump) then oil will backstream into your chamber. Investigate 'mean free path length' for vacuum systems.

    Another good book is by O'hanlon:

    https://www.amazon.com/Users-Guide-V...s=books&sr=1-2

    This is a very practical book.

    Another one, handbook of PVD:

    https://www.amazon.com/Handbook-Phys...s=books&sr=1-1

    I know this is available in paperback, I've got it.

    Those two books alone will get you most of the way there.

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    I have given the project some more thought and am now of the opinion that Aarongough has a workable idea.

    Some background: The latest generation of cathodic arc batch coaters for cutting tools have process times of about 6 hours. The long process time is a result of the 2000 1/4 inch diameter end mills loaded in the chamber all sharing the same deposition source. If you had a very small chamber and processed one end mill at a time the process time would only be about 40 minutes with the right deposition source design. This would not be practical for the end mills but would be practical for a custom made blade.

    The out of pocket cost of coating the single end mill on a home built machine would, for example, be $50 rather than the $3 dollars that the batch coater charges.

    The economics of coating the knife blade are more favorable. The batch coating fee may be in the $30 dollar range and closer to the out of pocket expense of doing it yourself. I am assuming that a home built machine can be assembled for under $5000 and will process at least one hundred parts over its design life. (I left out a few details)

    Is a $5000 dollar home built machine possible? Yes it is if you know what to look for in the surplus market.

    My home built would consist of 3 process chambers and maybe a load lock.
    Each process chamber is a box 8 inches wide , two inches deep and 10 inches tall. Each box has a centered front and back face 6 inch diameter port. There is a bottom slot for loading the knife blade. There is a narrow side pumping port and a few smaller ports for gas feeds and electrical connections. The 3 process stations are mounted on a larger lower chamber which has a mechanism for transferring the blade between stations.

    The first station does a sputter etch and heating operation which cleans the blade and raises its temperature to 220 deg C. The blade must be heated to insure that the deposited films will be in compression when the blade returns to room temperature. The process will take less than 5 minutes.

    The second station has a pair of 4 inch diameter chrome sputter sources facing each other. The source targets are about a inch apart and the blade sits in the gap. The chrome glue layer can be deposited in 5 seconds. The chrome/carbide or chrome/nitride transition layer will take about 10 minutes to deposit. These are both done in the same chamber.

    The third chamber does the DLC coating. This can be either a RF glow discharge process confined with a pair of magnetic coils (Helmholtz coils) , a hot filament discharge process, or a ion source direct deposition. The DLC coating is 20 microns thick and is deposited at 1 micron/minute with either the RF or hot filament method . Thicker coatings will crack from the thermal expansion mismatch with the substrate,

    The feed gas is either acetylene or methane. The vacuum pump for this station is sized for the hydrogen by product of the DLC process.

    The reason for the separate chambers is to avoid depositing the diamond electrically insulating layer on the sputter sources. The sputter sources need to cleaned once this happens or there will be extensive arcing. The large batch coaters are equipped with shutters to allow a cleaning operation without damaging the loaded substrates. This setup is not practical in a small chamber.

    The 4 inch chrome sputter sources are chosen because the sources are or were available on the surplus market.

    Up until 2005 some of the hard disk magnetic media companies were running rotary transfer coating machines. Each machine had 12 process stations and a load and unload lock mounted on a 8 foot diameter transfer chamber. The process stations were equipped with a front and back face source as described above and had roughly the same station geometry as described above. The process stations included heating, chrome deposition, magnetic layer deposition, and carbon deposition. In the 2000 and later years, their were attempts made to replace the carbon process stations with DLC stations. .

    These machines became obsolete with the higher density discs that required more film layers than the rotary machines could produce.

    The obsolete process stations do show up on E-bay. In spite of the asking prices shown they have little market value. They would be a ready made source for the knife coating project.

    The sputter sources have a motor driven rotating magnetic field assembly behind the target that insures high film uniformity and high target material utilization. The target thickness was sufficient to coat about 70,000 discs. That was a one week production run.

    Other comments:

    Aaron mentioned his blades were coated with a tungsten carbon DLC film The metal addition is done to reduce the internal stress in the DLC film and to prevent it from peeling off the substrate.The film has a hardness of about 50% of that of a pure carbon DLC film. (Reference Thin Solid Films Journal vol 355-356 pages 174-178, 1999)

    The Thin Solid Films Journal and the Vacuum Science and Technology Journal are good sources for process recipes and equipment design. The recipes are for lab sized coating work.

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    Awesome feedback and responses guys, thank you very much for taking the time!

    I am planning to forge ahead with a very simple resistive thermal evaporation system as the 'first step'. As I said earlier I think it will be a really good way to get my feet wet without a lot of capital investment, and most of the equipment needed will have utility later for other things as well as potentially in a larger/more complex system. I have been reading a lot, and will read further with the books listed above!

    I have done the rough calculations for building a resistive power supply, albeit a small one. Initial design will be very simple/crude: a variac driving a 6V/40A toroidal transformer. I will change the fuse in the variac to a lower rating to protect the 6V transformer against over-current. Power measurement will be with a simple AC power meter before the variac. The filament will be both the heater and source to keep things simple, though I know this is not the preferred way in industry as melting the filament is all too likely. I do not plan to measure filament temperature directly, instead I will measure the power needed to melt the filament at the target pressure, then simply using that as the upper power bound for subsequent runs with identical filaments.

    Chamber will be a very small (~1L) glass vacuum jar, with a polycarbonate outer container at atmosphere for safety.

    I am completely aware this is a very (very) 'mickey mouse' setup and will likely not end up being terribly useful, but I think I need to move toward getting my hands dirty ASAP as that definitely helps me learn faster and helps to keep me motivated!

    I read an amazing article last night that covered the history of thin film vacuum coating: https://avs.scitation.org/doi/10.1116/1.4998940

    Apparently the first deliberate vacuum coating was done in the early 1800s, using hand pumped piston vacuum pumps... If they can do it and I can't I'm going to feel very inadequate

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    Quote Originally Posted by CalG View Post
    Cathodic arc= TIG in a vacuum

    Call it Tungsten in Vacuum = TIV ? ;-)

    Your choice of filler rod ;-)

    More simply, carbon arc "burning". ;-))
    I really appreciate this comment! For some reason I had not looked at arc sources much, instead I had mainly been focusing on planar magnetron sources, but after your comment I did a fair bit of reading on them. The principle seems very simple which I like, of course the devil is in details I'm sure. It sounds like arc sources are used a lot for DLC too which is great!

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    Quote Originally Posted by aarongough View Post
    I really appreciate this comment! For some reason I had not looked at arc sources much, instead I had mainly been focusing on planar magnetron sources, but after your comment I did a fair bit of reading on them. The principle seems very simple which I like, of course the devil is in details I'm sure. It sounds like arc sources are used a lot for DLC too which is great!
    For defect free (reduced) films Filtered Cathodic Arc is a method to get a lot of material applied quickly.

    Check out Strong's "Procedures in Experimental Physics" for an easy read that includes practice.

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    Chamber will be a very small (~1L) glass vacuum jar, with a polycarbonate outer container at atmosphere for safety.


    If you poke around ebay you can find a conflat vac chamber or a nipple with about those same sizes for maybe 15% of new. They are good to 200C-250C

    Check out Strong's "Procedures in Experimental Physics" for an easy read that includes practice.





    this is a great and wonderful book

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    DLC films do not have a high hardness relative to the metal nitrides. . They are used because they are inert and have a low coefficient of friction.
    They are a good choice when there is metal to metal contact. Examples of this application are end mills cutting non ferrous metals or piston rings sliding in a cylinder.

    MICRO HARDNESS OF THIN FILMS
    With the exception of diamond these numbers are all ranges and will vary significantly
    with deposition method and substrate preparation

    GPa= giga pascals

    Diamond __________________________________100 GPa

    Titanium- Silicon -Boron nitride multi layer ______40 to 80 GPa
    Boron nitride multi layer _________________________40 GPa
    Silicon carbide ________________________________ 25 GPa

    DLC films (varies with hydrogen content) _______20 to 30 GPa
    Aluminum oxide _______________________________ 20 GPa
    Titanium nitride ________________________________20 GPa
    Chromium Nitride______________________________ 11 GPa
    tungsten doped DLC ___________________________ 10 GPa
    Hardened Steel ________________________________ 8 Gpa


    One major correction to my earlier post: The deposition rate given for a DLC film was the highest number that appeared in the references. It may not be accurate or it may represent current best practice. Other references, from 20 years ago, show deposition rates in the 1 micron/hour range.

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    DLC are tribological films

    For a sheath knife application, it is entirely marketing. But that is no small point.

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    Quote Originally Posted by aarongough View Post
    I have done the rough calculations for building a resistive power supply, albeit a small one. Initial design will be very simple/crude: a variac driving a 6V/40A toroidal transformer. I will change the fuse in the variac to a lower rating to protect the 6V transformer against over-current. Power measurement will be with a simple AC power meter before the variac. The filament will be both the heater and source to keep things simple, though I know this is not the preferred way in industry as melting the filament is all too likely. I do not plan to measure filament temperature directly, instead I will measure the power needed to melt the filament at the target pressure, then simply using that as the upper power bound for subsequent runs with identical filaments.

    Chamber will be a very small (~1L) glass vacuum jar, with a polycarbonate outer container at atmosphere for safety.
    Often metal mesh covers are a good idea. The bell jar needs to have a spherical top, NOT a flat top. You do not want to see what happens when one of those implodes.

    Not sure exactly what the evaporant will be inside the fillament, or what size the fillament is going to be. For a relatively thin tungsten basket that has maybe three inches of wire length overall, that needed about 50 amps to run. If your fillament is heavier or shorter than that you will need upwards of 100 amps, the voltage will be very low, probably below a volt. You are looking for a high current, low voltage transformer. It will weigh about 30 pounds and you can measure the current with a lead through a multi-turn torroid where the secondary goes to a meter.

    If you are trying to put some evaporant in your source, one issue to note is that the evaporant will coat the inside the basket or boat when it melts, and will short out the turns if it is multi-turn. Vendors sell ceramic coated sources to insulate the heater from the evaporant if this winds up being a problem for you.

    Another issue is the evaporant will immediately coat the inside of your bell jar, rendering it opaque. You won't be able to see what is going on after a few runs. One cheat is to put a clear glass container (I used one liter glass beakers) as a screen. Large microscope slides clipped on to various supports also worked as sheilds. Paper binder clips work well to hold things in place. They're basically vacuum clean out of the box. Likewise the glass microscope slides. Things will get HOT inside the chamber so stay away from anything that will melt or outgass. No polymers.

    When the glass slide near the target goes opaque, that's about 1000 angstroms of thickness. Count how long that takes. If you want more,
    keep counting.

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    Quote Originally Posted by CalG View Post
    DLC are tribological films

    For a sheath knife application, it is entirely marketing. But that is no small point.
    No so much marketing as simply appearance. I had a lot of customers who wanted a non-reflective black blade... Previously I delivered that with a firearms spray coating called Cerakote, which had excellent corrosion resistance, but the wear characteristics are not that great on a knife blade.

    DLC has much better wear characteristics and overall looks much better! The corrosion resistance is not as good though unfortunately... I have been sending out knives with the DLC coating for quite a few years now and overall it has been great! I would like to add an anti-corrosion layer if possible. The 'possible new vendor' also does electroless nickel in house so I am getting some samples of blades treated that way for testing.

    EDIT: I should note that I think TiCN would work just as well in my application, but I haven't found a local company that can apply it below 400ºF...

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    One of my favorite suppliers- Catalog | DUNIWAY

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    Just found another really interesting supplier: Fil-Tech (Quality Quartz Crystals & Thin Film Hardware Manufacturer | Fil-Tech)

    They have vacuum gauges, rate monitors/controllers, sensor heads and crystals for same as well as a magnetron source and e-beam parts... Their pricing on rate monitors/crystals/heads and vacuum gauges are by far the best I have seen for new parts so far. Haven't dealt with them yet though so I'm curious if anyone else has?

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    Quote Originally Posted by aarongough View Post
    should note that I think TiCN would work just as well in my application, but I haven't found a local company that can apply it below 400ºF...
    Annealed M2 steel has about the same machining and grinding characteristics as A2. Once heat treated, it will maintain a hardness of Rockwell 65 up to 1000 deg F. This is the material to use If you intend to use thin film coatings on your knives.
    Last edited by Robert R; 07-01-2020 at 02:23 PM.


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