Atomic Layer Deposition of copper - If you like sputtering, you'll love this!

[@kasparroosalu]

You are accidentally still doing CVD. There's huge amount of reactants still in your lines after you close the fow meters and instead of 30s cycle time you probably need 30min. To truly stop reactant flow in those lines you need inert gas barriers on each source. Hydrogen is simple with two solenoid valves and two needle valves. Put two T junctions on the line. First (closer to flow meter) goes trough solenoid and needle valve straight to your vacuum pump. Second (closer to reactor) goes trough solenoid and needle valve to your carrier gas supply. Now when you open both solenoids hydrogen has straight path to pump and leftovers in the line will be purged by reverse carrier gas flow. Close the solenoids during hydrogen pulse. For copper source it's the same principle. Just imagine that the second T-junction is inside the reactor hot zone and and reactant is just before it. You'll need one extra feed trough into your reactor for the blocking gas. This apparatus is usually made out of quartz but you can probably get away with glass or even stainless steel. Source: I operated and modified experimental lab-made tubular ALD reactors in uni for many years.

[@UnitSe7en]

This feels correct.

[@call_me_stan5887]

Still thumbs up for the effort, aye? :)

[@kmit9191]

I'd rather use Argon or Nitrogen

[@kasparroosalu]

@@call_me_stan5887 For sure! In principle the ALD procsess is quite simple but in reality nailing the procsess window with all the temperatures, flows and pulse timings is not trivial even with commercial machines. What Ben has achieved is impressive. I hope he'll pursue this further because ALD capability would be handy considering the stuff he does in hes projects.

[@call_me_stan5887]

​@@kasparroosalu Thank you for your insightful discussion :) I'm sure Ben will surprise us with many, many projects. I know he reads comments and sometimes indeed modifies methodology accordingly.

[@fredo514]

The flow controllers probably use a proportional valve which are notoriously leaky when off. The usual way to deal with that is just to put a regular solenoid valve (which are not leaky) in front.

[@zacharysamenfeld2487]

This

[@bob505470]

this^^^ even the highest end MFC's are leaky. CVD systems ive built always have a pneumatic high vacuum valves before and after the flow controllers.

[@johnalt4792]

I have that same controller but in the equilibar brand. You are absolutely right.

[@jeffmorris9893]

Yup. Valves that control flow don't control no-flow very well. Vice versa as well. In gas measurement on larger scales you're exactly right -- both types of valves are used in-line.

[@billdlv]

Alicat makes controllers with that option. We ordered one for work, still have not received it though.

[@sparqqling]

The comment section of this channel is pure gold, so many useful comments.

[@theoldbigmoose]

The folks assembled here are the brightest in the world. Amazing capability!

[@dogodogo5891]

ben's topic probably are miniscule percent compared to all youtuber, maybe we'd reached the star if there any 50% ben😃

[@miss-astronomikal-mcmxcvii]

Pure gold. No pun intended lol

[@IstasPumaNevada]

Other channels: "Check it out, I made plasma!" This channel: "I tried two different ways of plasma-cleaning as a prep step for my actual project but neither was sufficient so I had to try something else." *shows 20 second clip of _really rad looking plasma flow_ *

[@rkirke1]

For Ben's channel _really rad looking plasma flow_ is so 7 years ago :D Link to the plasma cleaning video if you haven't seen it yet: kzbin.info/www/bejne/l6W5hKusl86DnZI

[@broekspijp41]

I want to plasma clean my dishes now.

[@nitehawk86]

Applied Science is the science youtuber's favorite youtube channel.

[@F0tr]

For creating plasma, you only need a microwave, anything with IQ of washmaschine can put a spoon in bowl a put it on .... than screem on Tik Tok.....

[@It-b-Blair]

@@broekspijp41 once we get the energy grid sorted environmentally, it’d be so cool to have plasma based dishwashers! What a light show that would be! Being the restaurant dishwasher wouldn’t be the begrudged kitchen job it currently is 😜😸👍👍

[@Sam_596]

I am unimaginably jealous of the time and money you are spending on these projects. This is the kind of thing I wish i could do for a living

[@robertschnobert9090]

You can. Do it! I believe in you! 🌈

[@johndawson6057]

Do you code in java?

[@Sam_596]

@@johndawson6057 Mostly c++ nowadays, but I do still have some tasks in java

[@dankaxman7312]

HMMMM I design and and build custom electric musical instruments.I also construct mostly all components for them.This ''process'' could be helpful in bringing a unique ''steam-punk-look and feel to the various proto-types I have ''waiting in the wing'' to apply that ''motif'' to.

[@cannaroe1213]

@@dankaxman7312 no ur a motif

[@failforwardresearch3127]

I picked up an evaporation type apparatus, it was someones project... I goofed up the roughing pump, because I didn't know there was a valve to close, by the time i realized that, there was oil all over the floor. When i refilled the pump with oil, i realized there was now oil at the bottom of the diffusion pump. When i ran the diffusion pump, nothing seemed to happen except it got hot. I managed to get what i thought was a decent vacuum, and tried plating something... I ended up with soot all over the inside and the heater bowl was cracked. I clearly don't know what the hell i am doing LOL. I can only imagine how much fiddling this must have taken you. Great job.

[@chrissscottt]

This is a good demonstration of why chip manufacture is so tricky and requires such contaminant free environments.

[@eclectichoosier5474]

If I recall correctly, chip manufacturing is the only industry that commonly uses chlorine trifluoride for surface cleaning. Guaranteed to remove anything (except, perhaps, teflon.)

[@SeanBZA]

@@eclectichoosier5474 Removes PTFE as well, just slowly. Also will remove all surfaces an atom at a time, which is why the inside of the cleaning machinery is classed as a disposable part.

[@SuperAWaC]

@@eclectichoosier5474 Also when reprocessing uranium to make uranium hexafluoride which is then enriched.

[@praetorianstride5948]

The chips are sensitive to damage from static electricity as well, so they are frail in many ways.

[@vanhetgoor]

It is very nice to hear a man speak about a subject that he knows a lot of, and then trough experiments he learns even more. There is no end to gaining knowledge! I would never dare to put an atomic layer deposition of copper on glass. But it is beautiful. It would look nice on an old fashioned candescent lightbulb, like it has burned for more then a century continuously.

[@__-nd4hf]

26:00 bottles were probably made in a way that cools them unevenly, like rolling on the conveyor belt after forming. This would shift the lattice structure of the glass touching the belt, creating the line. Try annealing the glass in the furnace and cool it down slowly. Also a comment about mass-flow controllers - they are not used this way on an industrial ALD we have. Our system has one flow controller and electically controlled valves for pulsing the precursors. Flow controller is used to provide a constant flow of a purge gas and nothing else. Ammount of the precursor delivered in each pulse is controlled by the time of the e-valve being open, while carry gas is supplied at constant pressure to the precursor vessel.

[@ericblenner-hassett3945]

Depends on the bottle maker. Some are still hot glob spun moulds then excess cut off prior to release and cooling. The bottle at the beginning does look like a 2 step where after the spun mould, it has the neck heated and rolled like you say and definitly changing the latice. I have not tryed personally, however, wouldn't getting the whole bottle back up to almost molten state then cooling realign them?

[@ColonelSandersLite]

Yeah, I agree that this is almost certainly from some kind of rolling press that shapes the top and/or trims the excess after forming. I suspect that annealing it would help but probably can't mitigate the problem entirely. Not without heating the bottle to the point where it loses it's shape anyways. I wonder what the results would be if you abrade the surface as well or instead?

[@Macieyevsky]

Normal youtuber: DO NOT TRY THIS AT HOME!!! Applied Science: If you want to try this, you will need another couple of thousands of dollars in parts and a couple weeks of free time. I really appreciate your channel for such approach to the topic. Good job, keep going.

[@burtpanzer]

DO NOT TRY THIS AT HOME means WARNING! A level of knowledge and experience is required for safety! Not, if you've got the time and money, go for it!

[@sriracha3049]

The pattern on those glass pieces is most likely due to the amorphous structure being aligned differently when the glass was necked down

[@mackensteff]

I use similar vials and silver them using Tollen’s reagent. If I don’t clean them I see the same pattern. I end up lightly chemically etching them with a hydroxide solution and then get a nice even mirror. I agree it has something to do with how they are manufactured.

[@codygoldhahn2680]

Is there a guess as to the vials being blow molded(looks like a beer bottle with a noticeable seam, with a bubble of glass inflated into a two part mold)? Or spin cast (usually no seam but a molten ingot spun into a radial mold)? I'm interested in the physics of the manufacturing that may lead to the materials properties...

[@mduckernz]

Yeah, had the same thought; you reckon if annealing the glass and cooling it down very slowly might help?

[@bobweiram6321]

Glass can hold a charge. Could it be those areas are slightly charged? Could grounding it help?

[@BRUXXUS]

That would make sense to me. Also super fascinating! I never considered how molted glass is formed could create different structures, but yeah, makes sense. I wonder if there's any other ways to detect these variations.

[@izzie9526]

I remember sophomore year of high school, I asked my chemistry teacher if was possible to physically measure the size of a single atom. She told me about copper atomic layer deposition and I found it fascinating. Great video :)

[@Dr.Sortospino]

I'm a PhD candidate in Materials Science at CU, my thesis is on ALD. One of the issues that you are also running into is the nucleation delay of ALD metals. It's well known in our lab that if you wanna deposit a metal, it's better to deposit a Al2O3 ALD layer in order to create a small layer that allows a better nucleation. We deposit tungsten, and you need ~20 cycles before you see a film growth. The other is probably a not-perfect ALD process. As other people mentioned you probably need a very long purge and better dosimeters. for experience, leaks make very weird ALD films.

[@rustalisin8950]

Emanuele, stochiometric surface reaction is the only way to ALD, true ? CVD may deposit amorphous or nanosheet layers if precursor not strict ( as Crashy, above comment) substrate needs to be hotter (local heat) than gas flow temp, with nucleation pretreatment ( TiCl4 ) only how to guarantee 1 layer for TiCl4 ? what is best commercial polished substrate (Si ?) Have u found Si nitride isolates phonon / electron / hole puddles that form on Si02 / Si ?

[@Dr.Sortospino]

@@rustalisin8950 oh yeah. If you remove the SiO2 from a wafer you see that H-terminated sites gives islands, not monolayers. Basically, If there are not enough nucleation sites you'll have islands. Then yes, on ALD you are mostly limited to stechiometry, you can't go far from it.. while CVD you can add basically all. SiO2 with dopands? Adding NH3 to precursor and you have SiON or better SixOyNz.. If you have leaks, like here, you definitely doing CVD =D plus the metal nucleation issues.

[@piduguDileep]

I have a doubt if we can to remove layer by layer of an material using laser ablation method

[@Dr.Sortospino]

@@piduguDileep you can do with Atomic layer etching. You can remove Al2O3 with alternate pulse of HF and TMA Very layer by layer according the QCM

[@JlerchTampa]

You gave me flashbacks to cleaning my 400mm telescope primaries so I could coat them in my home brew chamber. I spent weeks in circular cleaning -> coating -> cussing -> stripping the Al coating -> start over hell. Fortunately I didn't have to resort to your more extreme cleaning measures, a simple but vigorous CaCO3 + H2O wash followed by water rinse and then original Windex applied to a Kim-wipe and used as a vapor worked in the end. 10 years later the mirrors still look pretty good (dusty sadly).

[@TheFlyingScotsmanTV]

good analogy with the op-amp. I remember the same feeling when I first learned about them - amazement, then disappointment

[@Nono-hk3is]

You are doing a tremendous service by validating academic results. Even presuming good faith on the part of article writers, the thoroughness by which they document the entirety of their procedures leaves much to be desired.

[@Zohar-Modifier]

Wonderful channel ... he does everything for weeks ... while we gain his doings in minutes ...

[@bensthingsthoughts]

To be honest, I have an engineering degree, and still, I admire more than I gain...

[@bettinaneumeyer6760]

I know nothing about this stuff. However I am so glad that there are people out there in this country that does. Thank goodness and let progress continue to flourish.

[@pcfreak1992]

Seeing Applied Science upload a video instantly makes my day!

[@pattonpending7390]

This brings me back to when I was young, dumb, and worked 3rd shift in the sputtering department of a wafer fab. It got boring after a while, so I would experiment with coating anything I had available. After a while, I had titanium coated sunglasses and platinum and gold coated car keys. The coatings never lasted long, but it was fun.

[@DanielSMatthews]

You can test the bottle surface difference hypothesis by trying to coat a broken one, just a (flattish) section in the area of most variability should make it clear if the bottle geometry is relevant, or if as I suspect there is some diffusion of some element into or out of the glass from the mechanical characteristics of the process line where they are made. This could actually be useful, hint at a pretreatment step to enhance the effect, if it is boosts the deposition probability.

[@edengoodwin1399]

ALD chemist here: Evap/sputtering are directional, CVD is diffusion limited, ALD is reaction limited. A lot of ALD precursors can be CVD precursors under different operating conditions, or even have some CVD components. Flow rate, system pressure, pulse/purge times all affect the growth rate, con-formality, and surface structures of a film.

[@mikeydude750]

Fantastic video! My thesis is all ALD work (actually running a 16 hour deposition right now lol) and watching someone do it all home-made is pretty cool. Now try a selective process :) EDIT: Just made it to the end - the surface condition being key can be a pain for a blanket film but you can do some really interesting things by exploiting this for selective deposition.

[@harolddavies1984]

This channel always impresses me with someone taking on a hard project, and succeeding. This is one of 2 channels I recommend/require of my students.

[@JonS]

This is great. My father would of got a kick out of this. He was a process engineer who built the first plasma etcher (while at STL in Harlow in the UK), and later a CVD coater for aluminium. Now, I deal with optics where ALD is starting become commercial viable and should offer substantial benefits over the traditional evaporative and sputter coating methods.

[@Spit823]

Ben I would kill to be 1/10 as smart as you. Your knowledge of so many topics is so awesome. You’re a legend and definitely one of my heroes.

[@4.0.4]

I love how you make stuff that's way over my head kinda understandable to the best of my abilities.

[@Polite_Cat]

You are the scientist I wished I could be in pre-school (and now, too). Messing around in your garage with lots of fun tech and chemicals on really advanced projects sounds fantastically fun and rewarding.

[@NightmareQueenJune]

I felt that OpAmp analogy deep in my heart.

[@theterribleanimator1793]

I felt it in my bum, should i seek medical attention?

[@NightmareQueenJune]

@@theterribleanimator1793 Nah, just pull that eight legged spikey thing out of there and you should be fine. Although you could face amplification issues after that.

[@joek81981]

My entire computer chassis looks like the thumbnail. Shiny, beautiful copper.

[@hawaii8857]

I did my PhD in ALD, designed and built reactors. In terms of aspect ratio, ALD can achieve an aspect ratio of 10^5. In ALD, it is all about timing, temperature and pressure. The reactor needs to have really good seal too depending on what is being deposited. The most interesting thing is that the seals become fragile over time because layers also grow inside the rubber seal when exposed to the precursors. Fun fact: ALD was invented by the Soviets but they only published it in their own journals in the 60s. The Fins took the technology from then and exported it to the world and got all the credit.

[@jrshaul]

Running a thermocouple through a spark plug to create a pressure seal is some serious creativity.

[@PIESISSYSTEMS]

Great job! The patterns of deposition that you get on those vials, is indeed due to the way they are manufactured. They start as a glass tube, where the edge is torch heated in a lathe untill it softens and then the neck and lip are formed. The same goes for the bottom. So, the reheating that takes place in these two areas, is changing the chemical composition (i.e. taking away Na atoms) and the surface morphology (i.e. sealing nano-cracks). Submerging the vials for a short time in hydrofluoric acid before the ALD, will most likely give a more uniform deposition! Also, refluxing organic solvent over your substrate will help removing organic contaminants. I hope that helped!

[@Marcelcas]

I think a piranha solution would be better to remove organic, followed by RCA clean.

[@viesic]

i don't understand, why this channel does not have a 100 million subscribers?

[@waynecribbs8853]

I really enjoyed your analysis, especially where you elaborate on what went wrong and your guess as to why. More of these!

[@Forensic1Man]

I really appreciate all the time and money you have contributed to this KZbin video. It is so interesting to see real-world work on high technology concepts. I am still trying to make liquid crystal glass circuit panels. Possibly, some day I will make a LCD displays that looks good. You should now try to make a display that says "Applied Science"!

[@DIYBiotech]

3:13 "In the beginning, there was evaporation" *Thunder Rumbles*

[@helpabrothawithasubisaiah5316]

Then God spoke and said "there will be light" and so there was, and it was good

[@worldscar6422]

This comment and this reply are golden.

[@redapproves1330]

Don't think I'll ever get to play with these experiments but it's fun to learn about the process.

[@katelights]

On the subject of cleaning, I want to see how you clean that tube furnace.

[@AppliedScience]

I forgot to include the video clip of that! I used a shop towel dipped in a small amount of ferric chloride, then wrapped around the end of a broom handle. Then I just hose it off outside, then spray some distilled water to rinse. It works surprisingly well.

[@pharmdiesel]

Yes please, I was just about to ask if your tube becomes contaminated

[@mduckernz]

@@AppliedScience Hopefully you plasma clean the tube after that as this is likely introducing quite a few contaminants!

[@TheRainHarvester]

When you open the vacuum, are there metal dust particles that you could breathe?

[@rehoboth_farm]

@@AppliedScience did you try doing a quick HF etch of the target surface? It would seem that would clean it better than anything else and give you better adhesion.

[@IXSigmaXI]

I appreciate your use of the term adsorption. hadn't heard that one in a while!

[@dimitar4y]

When you get down to the atoms, you find a lot of things you never knew and would have never guessed, but was always there.

[@riturajborah382]

Wow Ben! Content like this worth more than many books! I am only thankful. Keep enjoying your work !

[@HuygensOptics]

I once did experiments on monolayers of Cu phthalocyanine.The surfaces had to be cleaned using boiling sulfuric acid and then triple rinsing with very (very very) pure water. I think it's called Type1. Any other grade of water contained too much contamination for producing a good monolayer after rinsing. I'm not sure how you rinsed after the pirhana, but that might be a possible cause for the pattern in the vials.

[@captainmidnite93]

Timely video, went thru grandpa's stuff last night and found a pirani meter with box of various detector tubes, 2 oil diffusion pumps & oil, yards of vacuum glass, various silvering compounds, plasma/electron guns, etc, yikes I see a project consuming my workbench in the future.

[@whatshappenedhere1784]

If you ever want to add a filter in to one of these systems, I recommend using a 1/4 inch flare filter-drier. They are easy to find since they are used in refrigeration systems to absorb water and other contaminants. And they will also screw directly on to your 1/4 inch flare hoses, they have their limitations but will be useful for a lot of applications.

[@capnthepeafarmer]

This is why I love your videos, your absolute determination to get an academic paper to work is inspiring!

[@rexdalit3504]

Hi AS, to clean glass for spectroscopy we used to: clean ultrasonically with dd H2O rinse, hydrofluoric acid wash (carefully) with spectroscopically pure H2O rinse, spectroscopically pure acetone rinse. Do not let the final acetone rinse "pool" in any way on your glassware. Your lab looks messy, which is ok, but you need to have functional "very clean" areas of your lab for spectroscopically clean work.

[@theinternaut1991]

The name of this channel is just so accurate and I just love it

[@TechGorilla1987]

As if my Saturday evening couldn't get any better...

[@odczynnik]

Sunday morning here 🙃🇵🇱

[@SonofTheMorningStar666]

@@odczynnik Same here. 🇸🇪

[@SoulDelSol]

@@SonofTheMorningStar666 here too 🇺🇸

[@fukpoeslaw3613]

Sunday evening here (19:17)

[@fukpoeslaw3613]

...and one month later...

[@lukedowneslukedownes5900]

I’m brand new to your channel. They you for explaining and not being overly excited for dumb shit like the majority of KZbin scientists. I really love your realistic explanation

[@jasonk8311]

I've been wanting to develop this in my lab for several years. I'm really stoked to see you take it on! I can't convince my coworkers to abandon our thermal ALD to commit it to Cu as they still process PV Si from time to time. A custom system would be perfect for what we need. Thank you for the video Ben. My engineer friend and I are big fans of your work.

[@helpabrothawithasubisaiah5316]

I'm curious what you do for work

[@jasonk8311]

I'm a chemist/physicist studying photovoltaics and chemical catalysts

[@helpabrothawithasubisaiah5316]

@@jasonk8311 ah, I wish I had a job like that... I don't have the schooling so I'm stuck atm, I need to get in school so bad

[@helpabrothawithasubisaiah5316]

@@jasonk8311 i personally have an interest in nanotechnology, I've seen some articles showing alot of promise when mixed with photovoltaics

[@initialb123]

fantastic amount of work and research, compressed into a 27minute video. Huge thank you for uploading your experiments and findings for us to digest!

[@SarahKchannel]

i think your gas flow is quit turbulent due to the high reactor diameter, you would most likely benefit from making it more laminar by passing it trough some glass wool or something within the reactor tube.

[@TheVirtualFoundry]

I love your willingness to fail! I've made a living by inventing things for the last decade or so. I NEVER start a new process with the expectation that I'll succeed. It's all about the incremental improvement. Sometimes I get no where for days, then wham, progress! So, thank you for sharing your fails. I don't think you can have success without first failing. I've watched many of your videos. In most cases I didn't think these things could be done in a home lab. If someone just told me they did these things I'd be very skeptical, but watching you do them removes all doubt.

[@MrMonkeykiller1996]

be careful at using a spark plug as a connector some have built in resistors that will throw off your measurements

[@SeanBZA]

True, but simple enough to check, as the resistor is typically around 30k, and the solid slug is just a steel rod. For the plasma cleaning the resistor type is preferred, as it acts to limit current in the plasma, which has a negative resistance, and having the resistor close reduces capacitance. You really need to use long reach plugs though, and use a lathe to cut the the thread back to the minimum that will fit the feedthrough. Thankfully long reach plugs are common now, Ford Triton uses them, and you can just buy the cheapest ones to use, just use torr seal on the ceramic to metal base of each plug, because they are likely to leak there.

[@captaintoyota3171]

Usually ngk plugs have R in their code to show resistor plugs. U can get non resistor plugs ez thats what i run on my old motorcycle

[@SF-fb6lv]

Geez man - I sure wish my EE education was like this. We never talked about ANY of this. FanTASTic videos, thanks!

[@surplusdriller1]

The only channel on youtube that i will pause an great movie for half an hour, watch, then read about the subject for an hour then realize i was watching an movie and not really caring about what it was anyways. Great work as always Ben.

[@umageddon]

"Great"

[@surplusdriller1]

@@umageddon Thanks internet grammarnazi, if it was not for ppl like you taking time out of there busy day i would never have known what an "grate" grammatical error i did. Thanks

[@brunonikodemski2420]

I designed OpAmps. You are totally correct, in that when you get beyond the electronic design, and down to the actual processing and buildup, you get completely different results. In OpAmps, and electrometers, and similar devices, even a few hundred atoms of contaminant will make huge differences in leakages, and any electronic migration effects will cause surfaces to change dramatically.

[@erezra]

By far the most interesting channel on YT

[@Sam_596]

So far, Ben has made (among many other things): * A homemade SEM * A homemade sputter coater * A homemade waterjet cutter * A homemade oscilloscope (or at least crt) * A homemade high-power ruby laser * A homemade tube furnace * A homemade ALD process And many more things. What's next? A linac? (Can you imagine him renting a big hanger and building a collider?)

[@davidbroadway3012]

Impressive stuff!

[@nicktohzyu]

To see if the glass bottle geometry is affecting the coating process, perhaps try cutting a glass bottle in half vertically, then attempt the same process.

[@sczygiel]

I really love your comment about the overhype debunking. Today world is filled with unsupported or partially correct statements/propaganda and its really hard to tell how much of it reaches us. Its really eye opening that it also happens in scientific areas and you can be sure about the statement only if enough of people actually check the facts, try themselves and share the results. This is somewhat related to replication crisis. And lastly, reading some comments below even your attempt was not flawless as your setup could be rearranged or more heavily monitored. Like setting up mass spectrometer to see how pure is the deposition area and not have to rely on the assumption that the flow will do its thing. I love your videos as you are open and share the experience! Keep up your good work!

[@ChrisB-ms3cw]

Wow, really impressive, you are such a thorough thinker it's a pleasure to hear the stream of consciousness commentary

[@kylechin8706]

I watched 3 mins of this before i subbed, you are amazing.

[@electronicsNmore]

Great video! Always learn something new.

[@Venturestarx]

Learning academic papers aren't perfect by any means is priceless.

[@Capslacka]

As for the glass vials with strange patterns, in my experience, the glass will be formed into those shapes using graphite paddles or cast iron tools coated in carbon. Maybe those particles contaminated the glass in the areas they touched and mixed with the glass while it was soft.

[@memberHD]

Still the most underrated channel on the internet

[@vk2zay]

Looks like those glass vials have been altered chemically by the forming process for the bottom and neck, maybe something has diffused into the surface from the tooling, likely cast iron or graphite. You might try passivating the glass with phosphoric acid, that has worked for me in reducing the effects of the glass surface on the decay rate of active nitrogen plasma afterglows. A little HF-based glass cleaner might refunctionalise the surface too.

[@bgdwiepp]

I was thinking this too, i think when the bottom and neck are manufactured some form of die is pressed against the glass with some form of "lubricant" to stop the glass sticking, probably graphite, the center section is possibly made out of some massive mandrel drawn/spun/blow molded section of glass that is then cut to length attached between the top and bottom sections. Or maybe even more likely is there is an external die used to form the bottom section of the glass, then an internal die to form the middle section and then an external die used to form the neck, and the die and its "lubricants" are what allows it to stick better. who knows... Definitely on the train for annealing, passivating or a quick HF/slow NaOH etch/clean

[@DanielSmith-gv4fu]

Fascinating video and great presentation! My masters research degree involved closed-field unbalanced magnetron ion sputter plating (a type of physical vapour deposition) to produce amorphous ternary alloys. The beauty of this technique is that you can control alloy composition by optimising the current applied to each of the metal targets (and various other parameters). I would deposit the alloys onto microscope slides and sometimes single-crystal silicon wafers. As you suggest, I also imagine using pure quartz or single-crystal silicon would result in a more even Cu deposition. Although, the purported advantage of ALD is the uniform coating of complex shapes, which tend not to be so readily available made out of pure quartz.

[@spokehedz]

"The Devil is in the details." has never been more applicable.

[@MacksCurley]

Wow, wow,wow, you always amaze me with you knowledge and tenacity. It is like electroplating but in gas.

[@Killermyr]

I wonder if there's something about the chemistry of the glass at the surface that differs between the contrasting levels of coating on those bottles. I know that lab-grade glassware is usually made from torch-heated tube stock which is then shaped as needed, and that the localized heating will strip certain atoms (Sodium, I think) from the glass.

[@JustinMayfield]

I love your channel! I love that experts are weighing in on every video too. Giving you shit and providing insights. This is a show of respect. You are doing great, interesting and ego-less work. I really hope you keep this channel alive for a long time!

[@TheNicolaivlog]

Havent seen the video yet, I just know it will be a great one already!

[@beautifulsmall]

Youve got to love the rigs and methodology more than the results, thats where the learning is. Teensy 4.1 ? dynamite dressed as a party popper. Tried and failed to clean metals for bonding in the lab, had to call the experts. So when a fruit fly lands in my wine and I pick it out, the wine isn't clean. Helpful MFC flow controller comments, Great work, Fascinating.

[@curtisbeef]

Maybe it has something to do with how the neck is formed? Maybe that changes how the glass is in those regions and makes it harder for it to be accepted there.

[@Spit823]

Idk... my girlfriends neck is formed weird but it doesn’t have any trouble accepting anything

[@snozzmcberry2366]

@@Spit823 A key component of maturity is learning to infer & understand propriety as a function of context & situation. This is not the place for comments like yours.

[@Spit823]

@@snozzmcberry2366 oh ok sorry mom

[@scottcortus9590]

I like the high-level wisdom you’ve been sharing more lately like at the end of this video. Good stuff. Thanks!

[@harperwillis5447]

The sputtering vid is one of my most watched so big promises ben I trust you

[@wires99]

Fascinating video, great detail. This is very similar to the process for making the preform for drawing optical fiber. The preforms I worked with were about 5 feet long and 1.5" in diameter. They were drawn through an induction furnace like drawing taffy. One preform would result in over 70 kilometers of fiber. The preform was made by CVD of silicon chloride, germainium chloride, and phosphor chloride, resulting in the respective layers of glass inside the tube. The machine was much like a lathe, but instead of a cutting tool, it had a semi-circular hydrogen/oxygen torch heating the rotating tube and slowly traversing from one end to the other. The gas was introduced at one end and sucked out the other, and it would form a haze inside the tube on the cold side of the torch. As the torch passed, the haze would be fused to the inside surface and become transparent. There were many passes of this to build up the layers. At the end, the torch would traverse much more slowly from one end of the tube to the other, causing the tube to collapse into a solid rod. When the rod was drawn down to very thin optical fiber, the different glass layers became waveguides for different wavelengths of light, since they had different diffraction indexes. It was a neat process for so many years ago.

[@LanceThumping]

This reminds me of a paper I read awhile back that indicated they could make graphene on a copper substrate in a way that sounded like CVD, they claimed that it could easily be varied for different quality graphene and was designed in a way that would allow reel-to-reel manufacture of sheets. However, I haven't heard of anything coming from it despite it sounding amazing. I wonder if you could try duplicating it because it'd be really interesting for someone to manufacturer uniform sheets of graphene in a home lab.

[@JakeWitmer]

I assume you've watched James Tour's technical videos on copper sheet CVD graphene but, if not, they're good

[@Listeningtomuzak]

In my lab’s sputter and vacuum coating, we use a nitrogen gas gun fitted with a deionizer to finish cleaning our substrate. Make sure you are also baking your substrate at 50C for at least an hour to remove any residual water condensate.

[@daveb3910]

You need the acid wash on the glass, remember silica glass absorbs oxygen. Also try researching the optical cleaning process prior to coatings

[@rdizzy1]

He did say he did an acid wash on some of the glass. Didn't work. 24:50 onwards.

[@mwilson14]

I've got a couple test tubes that I had coated with metallic copper a couple years ago by passing copper ions over with carbon monoxide while heating the target test tube with a blow torch. I don't imagine I've anything remotely close to what you have accomplished, but now I'm wanting to revisit the experiments I had performed. I'm also going to have to check my spam folder because I don't recall getting a Patreon notice for anything lately. Your attention to detail is always amazing. Take care!

[@Amasarac]

my first assumption as a glassblower is that the heating of the tube neck when forming the threads is causing it to lose fluxand change its chemical properties, another possibility is that thermal stresses are at play here; the neck area is heated much more than any other part of the bottle when being machine blown and improper annealing could also be causing some sort of effect

[@helpabrothawithasubisaiah5316]

Could you blow me a mercury arc valve, just the case and electrodes... I have my own mercury and I would buy a vacuum pump and seal it off

[@EthanReesor]

If annealing is the issue, is that something he could try fixing himself? Could he reuse one of his kilns for that, or do you need specialized equipment?

[@Amasarac]

@@helpabrothawithasubisaiah5316 i do not have the equipment for making and testing glass to metal seals

[@Amasarac]

@@EthanReesor yes if its an annealing issue Ben could absolutely try fine annealing the glass himself in a kiln

[@outputcoupler7819]

Very cool stuff! I anodize aluminum at home, which I used to think required pretty ridiculous cleaning. But all I have to do is drop my parts in a concentrated solution of ethanol and potassium hydroxide for a few hours and rinse with distilled water. By comparison, the level of cleaning needed for ALD is absolutely off the charts.

[@twin1q]

As an EE guy. I approve of this message.

[@peterfuchs7822]

Clean the glass with HF acid or stick it in the kiln at about 500 C. Rinse with alcohol. Great video thanks

[@beliasphyre3497]

That is exactly my thoughts on cleaning dishes.

[@ChrisBigBad]

ya. I have become creeped out by dishes being washed manually with a stinkin cloth. Evenly distributing the dirt and calling it "clean". A dish-washer is probably similar, but at least it does not use the bacterial reservoir - erm - cloth.

[@beliasphyre3497]

@@ChrisBigBad Oh, I'm not creeped out. I find cleaning dishes a futile act, so I don't bother. I just dilute the reactive substances and biological agents to a *minimum* safe level.

[@appa609]

@@ChrisBigBad why is there dirt on your dishes? I only put food on them...

[@ChrisBigBad]

@@appa609 ah! The thing is that food quickly turns to dirt if left alone

[@goodi2k7]

He was like: "As it turns out it's pretty easy, you just .....". And I was like: "What? What? What? I don't understand anything." Great video as always!

[@KSPilo]

Would it be possible to direct the evaporated or sputtered plasma, ions, atoms or molecules through a high voltage electric or magnetic field, similar to a cathode-ray tube? Would it help, if you would etch the surfaces of the glass bottles with hydrofluoric acid?

[@bUwUmer1260]

I would call that "particle beam deposition" I wonder if that's a thing?

[@ethanmye-rs]

The evaporated or sputtered particles are neutral particles, so no force if your apply a magnetic/electric field. You could, however, shape the plasma in sputtering and so could selectively sputter part of the target. You’re just going to lose resolution at distance because the path will spread out like a cone from the source, but it could work for big features

[@bUwUmer1260]

@@ethanmye-rs I did some googling and apparently they do this at a micrometer level with scanning electron microscope beams!

[@BRUXXUS]

I had the same thought! How cool it would be to "print" with a focused beam of molecules/atoms. Would be sort of the opposite photolithography.

[@TheBackyardChemist]

@@bUwUmer1260 You can do something similar in a FIB (focused ion beam) machine, you can dig into an IC from the backside and form a probe to a single transistor.

[@powertripco]

Absolutely amazing work! A few comments. I would not call ALD a true atomic layer deposition process but it is close. The name is a bit elusive, in practice islands of material are formed during each cycle. As others mentioned that is probably a CVD process there. A way to ensure the precursors are not in at the same time is through a manifold with a carrier gas and precursors connected to it and controlled by fast acting valves. The precursors need to be in heated jackets or in bubblers to control the vapour pressure. A pump is required down stream. When you are within the ALD window you should be able to increase both the precursors' exposure/purge time by, for example, 50% and the growth rate should remain the same. Regarding cleaning ultrasonics and FNA works well. RCA is excellent though as it also chemically terminates the surface which facilitates the adsorption of many metal-organic precursors. Happy to provide references if needed.

[@hunter00047]

Very interesting. Do you think this could be focused to a specific area using a magnetic field like a CRT? I have always enjoyed your work well done

[@satchitnagpal7859]

No

[@SickEntertaining]

Nah but NASA is working on a CVD laser 3d printer. data.nasa.gov/dataset/Laser-Directed-CVD-3D-Printing-System-for-Refracto/c64h-y7vc

[@joshdeval9545]

Incredible content as always! Love hearing you explain technical stuff in your videos and seeing your process

[@vlogerhood]

I appreciate at 16:40 when the channel briefly becomes NileRed.

[@SlamminGraham]

Fantastic video!

[@HebaruSan]

Now I can say I watched this before somebody needed it for an Apollo mission recreation, lol

[@kylejacobs1247]

RCA-1 clean is the best. If you're getting excessive bubbling your temperature is too high. 60-70C is ideal, but above 80C the bubbling gets unnecessarily vigorous. It's all down to how easily the H2O2 reacts. Generally I heat the water/ammonium hydroxide first then add the H2O2 at the end so it doesn't decompose too much while warming. I would also make sure the glass is pretty clean to start with, some glass slides have a residue on them that I have to mechanically scrub off with soapy water before the RCA-1 clean would get them clean enough for coating.

[@rowdy420cat]

can you make Dichroic glass? I would love to see a video on that tech!

[@helpabrothawithasubisaiah5316]

I think he already has a video on that

[@rowdy420cat]

@@helpabrothawithasubisaiah5316 do you have a link, I can't find it 😫

[@helpabrothawithasubisaiah5316]

@@rowdy420cat no I don't, but I'm pretty dang sure I've seen a video on it. Hopefully someone else will see this comment and point you to it

[@rowdy420cat]

@@helpabrothawithasubisaiah5316 I can't find it at all

[@helpabrothawithasubisaiah5316]

@@rowdy420cat this may or may not be it? kzbin.info/www/bejne/o4bGhqxtiNaXiZI

[@matthewrossilini5808]

Awesome video. I work in manufacturing and almost all cutting tools come in coated and uncoated variants. You could spend a lifetime studying different coatings, but its good to broadly know the different application methods