Live Stream from the Hiden Plasma User Meeting 2023, co-hosted with the Fraunhofer IWS, Dresden, Germany. View the lectures from the day here.
Morning everybody Welcome to frown Hofer welcome to the plasma user meeting from hi analytical for 2023 um it’s great to see so many people here um so all thank you for coming your attendance is is very much appreciated and before I get started um a couple of notes on the
Agenda so we have we have the you can you’ve got a copy of the agenda on your desks and we have some transport problems from the guys from leig so Dr bunders man’s presentation will be now after lunch and we can cross our fingers that that that he attends by by
Lunchtime so the other presenters are going to shift upwards by one so after Sam we have Amir abas and um then we have Dr Kos after after I’m here uh so yeah good news wise lunch is at 12: and midday um and please don’t pay for your lunch that’s that’s on us from
Hidden okay so please enjoy your lunch and refreshments so I I’m Dr D Walker I’m the marketing manager from hi analytical um and my colleague here is uh sort as well as um Andre Kaiser um and and I’m sure you’ve met Andre before as most of you have met Sam before as
Well so I’m going to do a little introduction to hi analytical um as uh I’m sure a lot of you have have come into contact with us before um I’ll give you an insight into what other applications other than plasma that we that we address as well
As a bit about about what we do so heyen has been in business for more than 40 years so so last year we had our 40y year anniversary um and since that time we’ve been privately owned we’re based in Warrington in the UK uh we have the factory there in the
Sunshine with around 100 100 staff and were privately owned um we’ve been in business like I say in the UK for around 40 years we’ve got a US subsidiary based in Michigan which addresses the the whole of the US um and we have since 2019 we have hide in Europe based in
Dorf um which Andre Kaiser is the sales manager for um and we provide a local presence all around the world so we have offices all around the world with uh with with many staff and agents all around the world um one thing that we do pride ourselves on is our customer
Support um so we have lifetime email telephone support with with all of our systems so we’re still um we’re still providing support for systems that are up in excess of 30 years old so our main um our main business is mass spectrometers that’s probably 99% of
What of what of what we what we manufacture so our ranges can contain gas analysis um dissolved species analyzers catalyst catalys and thermal analysis instruments we have systems for thin films and surface engineering as well as plasma surface analysis and and RGA systems as well all based around Quadra form
Spectrometers so for gas analysis we we we’re looking at measurement of reactions from gas streams so our new system here we can see the qga 2.0 and that was released two months ago here in here in Germany um and that’s our next Generation gas analyzer that’s a real time um capillary sampling gas
Analyzer we have dissolved species analyzers for um looking at dissolved species in in liquids and for electrochemistry so we can look at real time electrochemical reactions as well um and we also have up to the the the huge hbr 60 system which has an integral eqp plasma analyzer which is a
System for analysis of neutrals radicals and ions which you may have come into contact with so we have a wide range of applications for gas analysis um as as you can see there and we’re really driven by the applications that we address so for electrochemistry uh and Battery
Development we have Dem systems so differential electrochemical Mass spectrometers which look at the dissolved species in real time electrochemical cells for battery development and things like that uh we can also look at environmental um applications where we measure radical voccs in seawater um for mud logging as well we
We have systems uh for oil and gas um we look at catalyst we look at fuel cell reactions as well all the way to realtime human breath analysis where we’re looking at lowlevel voc’s in in breath analysis as well for surface analysis we have the tpd workstation which is temperature um
Controlled dsorption temperature program dsorption while we’re looking at samples such as uh dissolved hydrogen in steels or dyum in Steels um so we heat up sample and then measure the species coming off with our with our quadri Mass spectrometers we have Sims so we have secondary iron master electron
Systems um with integral iron iron beams to locally analyzed surfaces um we work with ionb matching systems so we have iron Milling probes as well and we we can look at we have custom softwares for Elemental Imaging and surface mapping for plasma Diagnostics as you know we have the
Ekp and we also have the hbr 60 um which is the molecular bass spectrometer system which is the atmospheric sampling or round atmospheric sampling um plasma system um and we can analyze neutrals and radical species using our um plasma sampling my spectron we have more simple um vacuum Diagnostics with residual gas analyzers
So these are bolted into process Chambers um we can look at um low levels of contaminants we can look at quality of um the species inside the process chamber um we can we can um do real time monitoring um we also have more high performance systems
For um Fusion systems such as the dls20 which is a 20 mil quadripole um which can separate for example helium and detarium so again there’s some more application areas of Industry that we that we address so we have biotechnology oil and gas semiconductor Aerospace nuclear solar industry for The Sims um
And obviously plasma Coating in research we have very very similar again we we address a lot of different um research Avenues so we have electrochemistry is a a huge one at the moment we have materials analysis space research um nuclear fusion and then biotechnology so what our key to our our
Success as as a company and how we like to work is that we we address the application we work with the end user um and and we really we have application Specialists that are specialists in um in in their Avenues of research um so we we do we do try and understand the
Application uh as well as we can to provide the the correct solution for the the end user um so we we are quite flexible in that we have a full design team we have a full software team so we can customize our products to to address um address
The end users requirements and we do that quite a lot um some recent customers of ours so we again worldwide customers for semiconductors Aerospace uh and government research labs um and and then universities as well so we we we’re proud of proud to work with all these with all these
Customers um and and we see that um we we’re we’re working very closely with them so this is US based in this is our HQ in the UK um with our contact details and then I’ll say a little bit about the team with hiding analytical Europe so we have Andre Kaiser here we
Have sashin and Jurgen and also and also Wolf Gang and now my colleague Luke Wells um so that’s our team based in Germany um so between them they they address the whole of Germany um and Austria so I’d like to over to Sam and if there’s any questions um please raise
Your hand while Sam gets gets sorted so Sam is one of our application Specialists for plasma and a lot of you will know Sam from installations and trainings okay thanks Dan hello everyone so yeah as the title says I’d just like to talk briefly about some recent advancements that we’ve been making to
The product line I know some of you are probably already aware but I just want to make sure everybody um is up to speed so yeah so the three things I want to talk about is multi chn scaler mode the eq20 and Dual Zone operation so before we start I thought
I’d show you one of our test Chambers uh back of the factory so a lot of the data that I’m going to show you today was done uh using this um it’s also used for testing all the new instruments that we ship out and if you return any for
Maintenance this is how it’ll be tested before we uh ship it back to you so it’s a Capac itively coupled um plasma The View through the window um you can see in the top corner so the electrodes on the left the eqp is on the right
Typically keep it about 5 to 10 uh centimeters away so 13.56 megahertz plasma so we have the matching Network um and we can also pulse the plasma using the function generator so we can do time resolved um studies as well so the time resolve measurements this is way you a repeating event
Happening usually multiple times per second and what people want to measure is yeah the time evolution of the different plasma properties and so I just got an example from the literature there showing the three different plasma species and how they evolve over the course of a
Pulse so the the standard gating um that all instruments are supplied with it’s a box car averaging technique so we Supply the instrument with a synchronization signal at the plasma frequency and then we choose um a window of time within the pulse where we can acquire
The data and we can change the position and the width of the pulse with the two parameters it works really well but it does have a weakness in that the narrower you make the acquisition window the the lower the effective duty cycle of the measurement is so the
Instrument ends up scanning for a much shorter time and it’s just waiting uh for much longer so to get around this we developed multi- Channel Scala mode so it’s works in the same way with the synchronization signal but instead of just a single acquisition window we now
Have many uh up to around 6,000 we call them bins because we’re emulating a multi Channel scaler card so the main advantage of this is just the speed the instruments acquiring data for much big larger proportion of the time do that so what this looks like is this a
Comparison between the two so this was done on that chamber um 1.7 KZ pulse frequency 150 microc seconds pulse duration you can see the data’s roughly the same uh but it’s the acquisition time so 8 minutes versus 9 seconds and that’s at quite a high U
Pulse frequency if that was say 170 HZ more like a high pins or something then you know 8 minutes versus 90 seconds suddenly a lot more things become possible so this is looking at a single energy uh but it’s also possible to do the same scan but for multiple energies
And then plot them in uh three dimensions so if we do that that’s what we get here so we’ve got um Iron energy uh down here and time going up there and if we take slices in this direction after the because it acquires the data this way if we take the slices
Horizontally through here we’ve acquired all of the iron energy distributions at the different points in time so I think this one was a one microsc resolution and then after you’ve acquired the data you can then um extract the iron energies um after the fact so I just
Chose some where they look a little bit different that so the the advantage is you can just get all the data shut down the process and then get the iron energies um afterwards so the next thing I want to talk about is the eqp 20 so it’s called
The eqp 20 because it’s got 20 mimet quadrio rods so the three um eqp members of the family are shown so we’ve got the eqp 6 the eqp 9 and now the eqp 20 so the advantage of going larger with the quadripole is it improves the transmission through it so that gives us
Yeah higher sensitivity so in the table um the important one is the ratio so at the low masses it could be up to 16 times as sensitive as a 9 millimeter um and that Advantage does drop off at higher masses but it’s up to five times the sensitive
And because it’s larger and it’s harder to drive the mass range is slightly limited compared to the other one so it’s only a maximum of a th there’s a picture of one so it’s the same mounting Arrangement um all the same um everything uh down here is the
Same so we can still do magnetic shielding water cooling driven electrodes they’re all the same the only difference is the quadrio section here which is much larger so it sort of linked in with the eq20 is the Dual Zone operation so all of our other quadrupoles run in what we call Zone one
Um so this is a stability diagram so normally would be um when you’re sweeping the mass you’re increasing the RF and DC volts and hopefully just skimming the top of these stability regions to do that but there is another stability region uh which we call Zone H
Which is at much higher uh RF and DC volts so the advantage of operating here is just greater resolving power um but due to the very high voltage that does limit the mash range so it’s only available to 0 to 20 AMU so for that reason we make it
Usable user switchable in software so you can still do Zone one 0 to two 100 but then you get this high resolution mode 0 to 20 uh we originally developed it for Fusion research U looking at sort of around Mass 4 the helium and dyum and
That’s some example um data that I got from the sales stuff here so the the red line is Zone one where there is some separation but it’s not fantastic but then green as soon as we switch to Zone H it’s much improved and then it mostly replicates the same
On the right hand side but the um this one here which is the helium 3 isotope with HD Plus that shows the maximum uh resolving power we can get which is 0.0 five so as you go up in Mass um it’s not possible to do 0.005 but we can do this
So this was again done on that chamber just using the residual water in the chamber and the Argon in the Argon plasma so there we can separate 0.0 28 AMU so these will both be a nominal mass of of 18 so then because it’s an eqp you can
Also do the iron energy distributions on those if you’re expecting them to be different um I chose to do the MCS on it um so there is a difference there so the two the two irons do behave differently when it’s a pulsed plasma and without that resolving power you wouldn’t be
Able to separate those it would be an average sort of of the two so yeah I think that covers it I don’t want to say much more every time so can answer any questions now or if you want to come and find me over lunch or whenever
Yeah y thanks for your presentation okay my question is for the resol measurement the distance from to the plasma matters a lot you have get the um yeah so it’s not something I’ve tried but yeah as you move further away you would expect them to smear out slightly yeah um
Yeah Ops to to adjust the system to VAR the distance um we could if that was a so we have a standard test routine so we try and position the eqp when we’re testing it uh to send out to a customer in the same position so that we can use VAR
Ious measurements that we take as benchmarks to make sure it’s performing properly so that’s the main function of that uh chamber but if say we had a special request um to do that as part of the testing process then yeah we could fit a a z as that translator to it and
Position it differently we are still in our case are limited we have our our chamers they have large size and then you have some one meter difference between the me and this is a lot so you have time effects and this is your sure yeah so that’s why you
Would yeah was also a question did you cover some temperature problems during this me um no no so it’s it’s running at quite a low power this would be sort of 20 watts 20 to 60 watts um I know what do and then when we’re pulsing it the duty cycle is quite low
So anybody else yeah okay which yes so it’s a a sort of a stability region so um yeah so it’s at a certain ratio of RF to DC volts and magnitude that will allow ions of a certain Mass um to pass through so this is for both uh both of
The yellow and the red are both for Mass 20 I believe yeah um so you’ll get transmission both in the Red Zone and uh the yellow for that it’s just the magnitude of the RF and the DC that matters it’s not like is dep onity um yes to compare between if you wanted
To do some measurements in zone H and some in zone one you would have to calibrate between the two so perhaps do an RGA measurement with the internalization source or perhaps with the plasma just in a steady state make one measurement with uh Zone one and
Then one with Zone H and then you can work out the the sort of the correction ratio in but you meas Z although there is no difference sity to yeah so you get the mass uh Mass dependent transmission so the the transmission does fall off um at the
Higher masses so that’s a wellknown um thing you can usually get a I think we publish a a rough table of that there’s a relationship there for that um well that would be something you would do um afterwards yeah yeah it only matters if you’re doing sort of quantitative measurements if
You’re doing relative measurements you know the mass is sort of independent you know the the signal level doubled when we did this uh you don’t have to take it into account yeah else yeah can you just talk a little bit more about the the test plasma that you
That you used why that’s maybe a little bit different to what customers would use in a when you go on site um well we’re just it’s designed for testing instruments so we just want it to be um stable reliable the same every time we put it on uh we don’t want to be
Sputtering anything or coating anything um because it has to be sent out clean to the to the customer so we we try and limit what gases we put in that’s why for that zone H stuff it was just water in the Argan I don’t want to go put in
Ammonia in or something like that yeah any more questions no worse I’ll let you do that feel better at driving all right so now we have me change yeah please this just place this microphone your sh yes okay oh go okay hello everyone uh I’m Amir I’m doing my master expertises in
Fon Hare ipms uh Matias rodolf abishek Batel and Jennifer Canon Help me in this regard and uh uh the title of this presentation is plasma diagnostic of uh radio frequency exitation on Industrial Door frequency capacity of couple plus matching tool using quadruple Mass spectrometry uh here you can see the
Outline of this presentation I start with motivation experimental setup I speak about the tool and the plasma diagnostic tool I go to methods ID of summation measurements error and conclusion let’s start with motivation okay to8 the development of process uh for back end of line and interlayer
Dialectric uh and due to the increase in material limitation and technical difficulties due to device miniaturization uh we Face problems such as uh Edge uniformity critical Dimension control Edge selectivity edge profile expansion charge accumulation H damage and pattern Distortion here you can see a photo and illustration showing the uh interlayer
Dialectric here is the copper line and this is the dialectric and here is the front of front and off line uh yeah and this is a trade of triangle showing that the ion flu radical FL ion energy R uh uh radical flu and byproducts effect on uh profile selectivity and aspect ratio dependence
H so it’s good to be able to control the radical flux and ion energy so here there are two ways that uh can help in this regard dual frequency CCP and pulse plasma and because the lack of knowledge about the plasma condition I did plasma diagnostic I start with argon plas
Because it’s simple and it doesn’t degrate the tool itself and uh I did some higher frequency and lower frequency uh variations and I uh did experiments on pulse plus M and the advantages is it’s Institute methods nondestructive and real time methods and it gives us Insight on ION
Per radical ratio and control over ion flx and ion energy so now the experimental setup so here is the schematic of the Dual frequency CCP a chamber with plasma diagnostic systems I use a tvus lk3 chamber it has two radio frequency generator one in lower frequency and the other is higher frequency at
12.88 MHz and 1468 so I call this one LF from now on and this one HF the qms from hien analytical eqp 500 is connected to the chamber wall in the wafer level and other diagnostic tool uh higher resolution OES and Sears from plus Matrix is also available
So here I speak about the highden eqp 500 plasma diagnostic tool uh highden eqp 500 Mass spectrometer with energy analyzer it can go to Mass from range of 0 to 500 AMU Mass Spectra of neutral and ions energy Spectra of ions RGA mode for NE and seams mode for ions yes
So I mostly work with idfs for in Sims Plus mode uh IDF shows how energetic active ions in plasma are snapshot of ion B bombardments Energy being transferred to surface uh ion flag generated inside plasma is product of the the integral intensity under the plot so this is the
IDF and the integral intensity under this plat is Ion flx the IDF is mainly influenced by uh the transit time an ion uh take to cross the sheet and by collisions the ion experience in the sheet region and IDF depends on the following param RF power RF frequency and chamber
Pressure so here you can see a mass scan and an energy scan using the qms tool now we go to methods dual frequency CCP it can generate cont continuous wave plasma and pulse plasma this is a chamber LF power and HF power different Decay time constant for uh ions radicals and uh
Electrons is different when the plasma is off so uh this helps us with uh Hing profile so in continuous fave you will you see the Hing profile is different because uh of the opening here but in pulse mode because of the control over the ion periodical ratio you will see this etching
Profile so this is a design of experiment for continuous faave plasma I did pressure variation in the in this pressures 30 m to 100 m power variation for HF power 0 to 300 and LF power from from 0 to 300 and I did a spotter rates for all these
Experiments here is a snapshot of argon plasma Mass scan we will focus on Argon plus and argon argon plus argon argon plus uh gives us the ion energy because if uh inter goes into any Collision inside the uh its way to the uh orifice it uh disappears so if we see argon
2+ it’s uh shows us the ion energy and here is the process power variation so I start with hf0 and LF variation and and other poers okay here is the spotter rat for all continuous wave uh here you you see the effect of LF power HF power at pressure 30
Millor how is the spotter rate different at different pressure so I start with pressure why at different pressure the Spates are different this is the idea for Argon plus 300 HF 300 LF you see when the pressure is increasing the IDF integral intensity and Peak energy decreases so in LF
Case when the pressure increasing the inter integral intensity at higher ion energy decreases and the inte integral intensity at lower ion energy increases and in HF case the integral intensity decreases and the peak shifted to the lower energies so as the pressure is increasing the average energy and the integral intensity
Decreases so pressure mainly influence the ion collisions in the sheet region and that’s why we see this spatter rates but when I check the VPP from The Tool uh I noticed uh this two plots so what is VPP the amplitude of the radio frequency voltage applied to the plasma so when we
Change the power this is the amplitude and the difference in voltage between the maximum positive and maximum negative PS Within one cycle of the wave from so when we change the pressure for RF power at higher frequency we don’t see any change in Upper VPP but when we change the pressure
For uh lower RF power we saw differences in VPP so it is a tool adjust itself when we change the pressure so to see the real pressure effect we run an exp ment with constant VPP so this is the B4 constant power 300 and here is constant VPP so here you see
The real pressure effect just decreasing in integral intensity and the energies are constant now I speak about the power effect the LF power effect and HF power effect here is uh the effect of LF power only so the HF power is off here when we go from LF power from 100
Watt to 300 watt we see an increase in ion energies so the ion energies increase in higher range and also the Argon 2 plus shows the increase in ion energies this is the HF only so the LF power is off and we only increase the power for HF frequency
And you see the increase in integral intensity and also uh uh increase in ion energies and this is the effect of both LF power and HF power so you see an increase in this artion why we see two peaks in our idfs so the lower energy Peak correspond
To the influence of the minimum sheet voltage whereas the higher higher energy Peak is caused by the maximum sheet voltage and why we see this differences in the BD of the Peaks at lower frequency the ion Transit time is almost uh equal to RF cycle so we see more separated
Peak and at higher frequency the ion Transit time is much higher than RF cycle so the Peaks are more unified and ion respond to average sheet potential and this is the influence of power on VPP so when we change the HF power and LF power the upper VPP just uh U
Influenced by HF power and the lower VPP is influenced by both of the HF power and LF power and this is the conclusion for continuous wave you see the uh HF power and LF power influence on ION flux so ion flux is mostly influenced by HF power and you see the HF
BPP which is the product of HF power and you see it only correspond to higher frequency and the lower frequency uh cause having higher ion energies so when the LF power is increasing the ion energy is increasing and you see this effect better in LF
VPP and here is the ion flux ion energy and spatter rate so you see the spotter rate is depend on Ion energy and ion flux both of them together and by combining the idfs with uh spatter rates we see the spatter threshold this is my experiments and these are the
Literatures so for the case of both LF power and HF power on we get 25 EV as a spotter threshold and it’s almost close to the literatures and in the case of LF only and HF only this is the spotter threshold so far I speak about uh
Continuous wave plasma now I’m going to talk about the pulse plasma so the tool can generate uh pulsing mode for LF power and or HF power or pulsing both the RF at synchronized way and with different frequency and duty cycle so in pulsing mode I speak about pulsing mode
Versus pressure frequency duty cycle ion energy and ion flx comparisons and spotter rate comparisons the RF power for continuous wave kept at 300 HF and LF 300 BT I did pressure variation at frequency and duty cycle so here is the influence of pressure on pulsing
Mode in case of LF pulse HF pulse and syn pulse for all of them when we increase the pressure the intensity at higher ion energy range decreases and the intensity in the lowerer energy range increases for all of the pulsing mode this is the same this is the influence of frequency
On different pulsing modes so in case of LF pulse as the frequency increases from .1 khz to 10 khz the integral intensity almost remain constant in case of HF pulsing the frequency increasing impact on Lower integral intensity and in case of syn pulsing the the frequency increasing impact on
Higher integral intensity so the idfs are here and this is the influence of duty cycle on pulsing modes as the duty cycle increases in LF f the higher energy range integral intensity increases and in the lower energy range it decreases but in case of HF pulsing the integral intensity of the
Whole IDF increases and in case of syn pulsing the integral intensity increases and the lower energy range is not available so here is different pulsing modes ion flux ion energy of different pulsing modes for different duty cycle so as we increase the duty cycle to The Continuous wave we see HF
Pulsing has decreases in ion energy LF puling ion energy increases when we go to higher Duty Cycles and the syn Sy decreases and this is for different pressures and this is the effect of duty cycle on ION flux so the LF pulse has decreas in ion
Flux HF pulse increase and sink BS also increase this is the effect of frequency on ION energy and ion flux for HF pulse and LF pulse as the frequency increases the ion energy almost remain constant and ion flux almost remain constant so the frequency doesn’t have
So much effect on the ion energy and ion flux in different pulsing modes for Argon plasma and this is the duty Cal effect on spotter rate so when the duty cycle increases the spotter rate increases for different pressure for HF pulse LF pulse and SN pulse and this is the uh frequency
Effect on spotter rat so you see also the frequency doesn’t have so much effect on the spoty this is the spatter threshold for for different pulsing modes so you see the spotter threshold in pulsing modes is a mix of uh different Beauty cycle and pulsing modes with both power on
Thus we see so much difference and so much spread here and this is the comparisons with continuous wave so in LF FSE you see is this energy for spatter threshold for HF fulse and S pulse and this is versus continuous wave so now we go to ID of
Summation this is idea for LF pulsing 300 HF 300 LF at duty cycle 50 DC and these two are the two continuous wave plasmas one is HF only and the other is both powers on and this is the resulting IDF with duty cycle 50 which is almost the same IDF as LF
Pulsing so the summation of two IDF two continuous fa experiments can be simulated with single pulse plar Ron keeping the desired IDF shape from both and it help on recipe selection so in case of summing both IDF and pulsing modes this is the shape of the
P and this is here I speak about measurement errors so the starting time of the ID of measurement after 4 minute after 10 minutes and 15 minutes gave me different idfs so I always start the measurement at uh same time and this is the IDF versus qms position so qms is uh located
Uh on the chamber wall but it’s not always connected to the chamber and it’s located on a z shift so whenever we want to use the qms we connect the qms so here you see when it’s 2 mm more inside or 2 mm outside this is the resulting
IDF and always the qms position kept the same and here is the chamber environment so we always run a same recipe and whenever we see any changes in the IDF we do chamber cleaning and chamber environment clean yeah and reach the conclusion so pressure has major influence in ion collisions in the sheet
Region for continuous wave and continuous wave mainly in continuous wave higher frequency governs ion flx and ion energy influenced by lower frequency so this is the main conclusion for continuous wave mode in the pulse mode pressure increase causes shift to intensity from higher to lower ion energy in pulsing mode and
Frequency has only a slight influence on duty and duty cycle has the major influence in pulsing mode and from the spatter rates I came to this conclusion that the spatter rates highly dependent on pressure and LF power and weekly dependent on HF power also is spotter rate is
Codependent on ION flux and ion energy a spotter threshold slightly varies between each position each pulsing mode a spotter rates is high highest when both RF poers on and with increasing duty cycle the spotter rate increases and this increase is ch sharper at lower pressure thank you for your
Attention Okay so we have time for questions if you have any questionss yes with time yeah uh it can be uh because of the tool itself so the plasma condition can uh change over time or it can be because of the qms itself it can be problem with uh like
Um the extraction of PL like capacitor and the it doesn’t give the voltage that we set exactly in a time so the IDF might varies over the time that’s why we kept the uh measurement start time the same thank you for ni presentation thank you was very interesting and one
Question I have how do you measure the eding rate your uh so I run a test for 1 minute itching uh uh silicon oxide thermal oxide and and after one minute I used ellipso meter to uh see theat and the question adding to this is do you also measure the Silicon you have
Some neutal silic in the plasma I assume you should measure it or me and have some direct measuring of the maybe I I didn’t understand the question have you me theas maybe but NE in Mass scans you mean uh yeah we saw traces of silicons
Uh in uh when we started the process for M scan there was some traces of silicon also after itching yes relate the amount uh no I didn’t do that is there any more questions okay well thank [Applause] you next we have Frank here so then hello also from from my side we
Are from FR of for iws this is where you are right now we are hosting this event or together with with Heiden they came to us I think it was last year already and then we talked about or we asked are there some some meetings to discuss with
Other applicants of the devices how they measure what the what new developments are and measuring strategy I think this is the most important if you start measuring with the eqp as we did and so we have to discuss a lot and so the the lifetime support by email phone calls
And so on is very important then first you have to get this running and then the measuring is done within a few days but get it running then you need for years maybe but if you have some help and know the people you can talk to then this is of course a great
Thing just want to click on I also want to introduce you to to frover and the frover society I think this is the the name Giver of our of our institution we have some very many employees right now I think that’s are above 30,000 in Europe and or Germany and and Europe
Also and we have some branches in in the US in US and other countries of the world too and the concept of roundover is important not only here it’s some role model also for other countries they they visit us and want to do something like this also in in their
Countries and why is this this is the combination of the the research we do anyway the the invention of new things and the very important point is as thrown over itself did he was also had a factory and has had to earn money with his ideas so we want to combine all of
It all of it and do some applied research and directly for the industry or very near to Industry needs and so they can make money out of our ideas or the things we develop together if they they ask us for Doo this is what we are
Doing this is the number I came up with earlier what the last slide many many peoples the staff is including students also and full-time employees maybe there are 22,000 or so and some many people and we do we don’t are allowed to give Doctorate Degrees Of course but we are connected this strong
To universities all over Germany so that we always have professors working at The Institute as a head of the Institute or or leading some technology units and so we are strongly connected and so this is something we we do typically all the time this are I think 76 institutes and
Research units right now maybe since the presentation was made it’s it’s changed a little but this is is the range and uh three billion EUR Financial volume this is a lot of course and what we what you see on the right side it’s the the basic funding we get anyway the
30% and the other things we have to do inustrial contracts or do public funded projects for for this money so we have to to write proposals of course uh develop new ideas find Partners to develop it h discuss with the industry discuss also in in this uh meetings as
We do today find new ideas what do we have to develop next what’s the next big thing and of course we have to be ahead of new topics that we are or we can involve ourselves in the development of this so the FR of iws is also is not a large
Institute within frover but we have some 320 people here and this are only full-time employees and 450 with students and and part-time uh also assistants name it like this and we are doing it’s front of ips it’s named for material and beam technology with beam this is mean laser
We don’t develop lasers but we do all kind of laser processing Technologies all around what you have a test uh for for cutting for for joining and for structuring surfaces it’s important for for many many applications and of course we also do this is what I do we do also
Codings also different kind of codings we do some we have the generative technology we are using also do 3D printing of ultra large scale devices for some space applications and also this is a whole range we are working in and the material is one of our base component understand what the material
Does what it can how it can improveed this is our topic here at the iws so what do we have next now we have the outline of of my talk I changed the name a little it’s now only industrial scale carbon codings with Laser Technology we don’t have to
Look at at the applications because we are a user seminar and we are want to look at what can we do with plasma measurements what are the the problems we have to to achieve that and so I put this more in the focus and also to
Prepare you for our lapor later than at at 2m so you already know how it’s working so we can then focus on the on the measuring technique and the results we see the okay as the Laser Technology is our base technology for doing carbon codings then I tell you something about ECP
Measurement requirements in our case and the results to it and of course a summary at the end so if you hear carbon and carbon codings a name maybe you have heard a lot is DLC it’s some overall name describing all kinds of carbon codings
And they can range in a in a really wide range from graphi to Diamond and describes nearly everything when it’s a coding because they see in it’s clear than it’s a coding but it’s the it’s very different what it can mean in our case we can’t do diamonds we still have
An our coding Technique we are generating morphos codings and so we are out of the the right side with diamond and nanoc crystallin Diamond but we can achieve the the codings here named AC and and Tac now the the picture is missing and it’s in range sp3 content
From 20 up to to 80 this is one advantage of our technology we can can get these kind of of hard codings this is special about technology and also in very high rates and of course we are hydrogen free or nearly hydrogen free so we we don’t have it in the chamber maybe
If there is some leage or then we have some very small amounts in it but no hydrogen in the codings at all and so at the end we got very hard codings maybe now you it’s back again the AC and Tac you see the different bonding types the
That the darker ones are are the sp3 ones and the Bri ones are SP2 the graphite like bondings uh carbon is a very great material in this case also for doing Coatings but what we did in the last time we add additional elements we we doped our carbon and so we can
Change anything there just one L too much now there can add additional functions and modify the electr chemical and mechanical properties of the FMS by adding small amount of of other elements in it in the low percentage range and of course in this case we have a plasma containing carbon and additional
Elements and so it’s more difficult to measure this instead of only measuring carbon we have to also look at other elements and the heavier they are the different the difficult it gets to measure it so now let me introduce you to the Laser Technology it’s called L lamb for the and m stands
For modulus this was an additional idea an initial idea to make it uh adaptable to any coding chamber or at nearly any coding chamber this is what you see on the left we have some graphi cathod material and this is what we want to evaporate and we are working with some
Pulse laser this is the the first picture in the left for the ignition it’s some some short pulse laser 100 NS to generate some initial plasma and then we start our an an arc an arc discharge with some high current for in this case here 1.6 kiloamps is some some usual
Number we are using and then we have some spot splitting as also it’s described the literature a lot and it’s more difficult on on carbon because we don’t have a a fast movement of the C spots on the on the surface of the graphite so we have to stop this process
After some some milliseconds or some micros seconds in this case wait wait a little or there is some time in between and then we reignite it at another at a different position and if we scan very fast we have some linear carbon Source after all what are the advantages of our
Technology we don’t need magnetic fields for control of the arpot otherwise if you use DCR you have some magnetic field generator or some magnets on the back side maybe adjustable also to get a good utilization of your of your cathode and in our case we don’t need this anymore
And as you see on the right side we have some new and some end of life graphite cathode and we can utilize nearly all of the material because we can scan and we do use all in in areas of the of the cathod is this the same and this high volume targets also
Leads us to longer coding processes and very thick codings we can do 20 30 micrometer thick hard codings for for several application where it’s needed and of course you can use thinner ones also then d targets you you need is only then in this case one for week or so
Depending on on the how much you use your Cod and how thick the films are okay the combination with other PVD uh PVD equipment is is possible without a problem but mostly people come to us and asks for a a designated bch coder and then we work with Partners together
To to make this working for them and what we also have which is important as you know always if you have Arc Coatings then you have the problem with the droplets in case of metal films or nitrides oxides and so on and in our case we have no there is no solid
Graphite it’s then in this case in are particles and so we have particles in our films and if we do filtering if you have plasma anyway we can use magnetic fields to bend the plasma as you see on the right picture in the bottom then we can do plasma filtering and get smoother
Codings thing this is how it looks like the two types of of our coding machines and plasma modules on the left side you have some high deposition rate variant uh up to 2 micrometers an hour mostly we are limited then by the temperature we put in in the chamber
If you want to grow carbon you need to stay at lower temperatures below 100° C and the higher you get in temperature the the software your films get that means at 180°c you don’t get any sp3 codings anymore and then you have to cool your sample holder or have to
Reduce the deposition rate so we are could be limited also by by this we have some trets or particles of course in the films this is what we expect and so it’s mostly necessary to do some post treatment of the surfaces if there are like like
Piston rings they are very easy to to process and also easy to to grind afterwards so that some standard process and of course there are applications when you are not able to grind anything or or adjust the surface after coating anymore if you think about gears then
You need initial smooth coatings to make this working and on the right side we have some scheme of such a particle filter and as you see the plasma is generated at a graphite then the particles are flying straight in some some structure and only the pure plasma
Is going to the deposition chamber and so we get smoother Coatings but also of course if you have a filter then you always have some reduction interposition rate and so we have 50% which is good but we still have particles in there and in this case then up to 1 micrometers
Per hour for a full loaded chamber this is our our equipment we have one of our machines and then you can also see our problem we have some basic plant put in in this case the it’s the schematic is not in the right scale of course then we have on the left side
One mod module with filtering on the right side one module without filtering and so we can combine our codings but what we can’t do anymore in this case as you see we can’t adjust or adapt our our plasma monitor anymore because all the flanges are adapted with some plasma
Sources already and so in this case we can’t measure at all this is one problem we we had and we had to overcome this and how we did this I’ll show you later and of course uh special dop codings we can also put in through the filter we
Can evaporate and see also differences by the filtering because our filter is usually iron energy selective and so there are also effects if we evaporate duped cathodes in the system and on the other hand we can do all on the right side all kind of codings and what we
Also did is mos2 codings which are working very well and we got a much better adition at the spot films they are available on the market and maybe there are an option for applications but it’s a complicated process for this and I don’t know if someone in Industry
Wants to do this except there is this advantage of these kind of films that it’s making the the cost sry valuable m okay this is some presentation some some video of our process of our principle this was the the larm modulus attached to the to the
Cathode to the to the chamber then you here now see the the scanning laser and the arc spots on the cathode surface this process is very fast is uh 300 Herz no 150 Hertz each each uh cathode and so at all you got Some you get some some linear carbon source so now we can also put to spe and here you see now the plasma and of course pbd or laser Arc as PVD technique it’s line of site that means we always have to rotate our our samples to make it Cod it all
Around okay the eqp measurement requirements as I told you before we have to look straight in our plasma source and we did some some changes anyway we developed some new some new filter with some 90 Dey uh deflection and so we had a chance in this case here
You see our this is this the standard laser AR module as I showed you before and now we want to bend our plasma to the to the main chamber which is shown here and but now we have all the options to look inside the plasma straight from
The other side we adjusted flanges to the side in the in the beginning because we know we want to measure it but we can also do measuring from this side there are also flinches attached in this so we can measure the plasma straight and also the bended plasma by 90 degrees
But we haven’t done the this measuring already we only adapted the the device in here and so we can do all the developments need for that and here this is is the scale how it looks like and our thinking is bend the plasma and avoid particles being reflected and
Coming back to the or coming inside the main chamber we are very flexible by our Arc discharge and we heard about some some low power spattering processes before and of course we have some much higher Powers we have some one 1,600 M for example at at 80 volts or so that means
We got a lot of power in the system and so also if we do the measure measurements later with the eqp we have to reduce the frequency otherwise we we heat it up and so we can’t measure only for for short time this is something we have to think about always it’s many
Different aspects we have to think about if you want to get some decent measurements out of it different kind of of pulse forms we can adjust also to think about we want to adjust the plasma exactly as we want and of course then we expect differences between some short PS with some high
Current as you see here this is our more or less our standard it’s now rectangle named but it’s scene shaped also a little and the other one is U the thinking about this was uh reduce the current by the half and then make it twice as
Long but in our case I only showed the results of of this what we have as a plasma properties out of this pulse form we have as I showed you short paes here the 300 microc also but long braks in between and if you want to tune the
Device you have to to gate the measurements every as always otherwise you don’t get signal the system can’t work with some some time where no ions coming in then it’s for some reason maybe it’s the old software maybe it’s a principle it’s not possible to tune you always have to gate this is
Something we we put in and we use some some gating with some delay and then some measur measuring window and we also look what do we expect in what uh window this is also some very important thing for us but after all it’s it’s essential for us to to gate the
Measurements this is one measurement of the of the current itself inside the chamber this is the exact Arc current I showed you before on the slide it’s starting with time zero and then we have some sample holder here in the in the in the chamber after bending of the plasma
Of course 90 degree and then we have some some iron current you see the different scale over here and so we have some some time of light effect of course some at least uh 50 micros seconds the plasma needs from the starting point to the to the substrate and of course the
Substrate is always uh put in with some 100 volts bius voltage to avoid electrons coming in and here this is some effect you always see first are the electrons and then you have some some small Peak also but the shape is is nearly the same and so this is what what we
Expect so now let’s come to the eqp results to remember this is our plasma Source here our our base chamber and this is the place we are starting the measuring and we did some no plasma redirection measurements in the beginning and this is the the cph of it
Here in the energy in electron volts this is always easy possible if it’s some some single charged ions then you have to not uh think about voltage or electron WTS the count rates are good of course and we I added this at 100% or put this
To 100% And then we did the plasma redirection active and so we have some reduction of the of the surface under the the plasma flux then itself and then we have some 55 uh 35% rest of of plasma or plasma flux to the to the aqp and we also measure this one that
Total different process at a different time the the dep rate at one sample here and one sample here same more or less same distance and we see some I name it similar it’s maybe it’s 55 and 65.3 it it’s not this accurate of course we don’t expect this but we have the
Same range we have .9 micrometer film thickness in the sample here and 1.4 in the at the sample here that means we got a a plasma transmission over 50% with our 90° filter which is better than the 60° one I showed you before and I think there are additional options to to increase
This in the in the future also the next thing I want to show you I started this in the beginning is the multimaterial evaporation and so we put in different materials in this case we we used some some metals and nonmetals in forms from Boron and Mum they are two two two
Examples Boron as a nonmetal very light element and Mum as a very heavy metal for for different kind of applications we had some thinking about in the beginning why use Boron Boron doesn’t affect the sp3 SP2 ratio this much because it wants to form sp3 bondings
Anyway so it stabilizes and in mum the thinking behind this was to make it um or to adapt it to Applications where you need lubricants with some mum in it and it forms some some dry sliding components m d sulfide in the on the on the surface and this
Was one of the thinking why we use the mum and the differences between you can see here in the cross seis in the beginning we have Tac with really rough codings and we have defect structures in the in the tsse codings in this case there are thick five micrometers and if
You do some break then you see this structure and if you go to TB we have the same hotness meain seem same s sp3 ratio and here we have some very smooth film without any defects anymore and if you look to the mum one then you see also a
Smooth surface and you see nothing as defects in it anymore and two differences at the at the selected area reflection you see up here in this pictures you stay amorphous as a carbon TSC is amorphous always the TSB stays amorphous and at AC mum it’s some some
Graphitic Nano structure we see in there and this also we can also use this kind of structure for several applications but I come to this later but here we have of at all some effect of the heavy mum and some results of this I show you at the next slide
Now first we did some initial measurements of our graphi electrode cathode which we evaporated with the process the pulse form I showed you before the 1,600 M and rectangle puls and here we have now the the ion energy in electron volts this is correct and
For the C+ and C2 plus and of course you we know we have many many uh parts of it in in C+ and only a little c2+ and there are also effects as the thermal effects of our graphite cathode that means if the cathode is very cold in the beginning we got some
Some large larger amount of of C2 plus but it’s get if it’s getting hotter and hotter then it’s get less and less and so we always did some initial running in of the cathode so that they gained temperature and measured after this always and the average ion energies this
Is some value we know from the literature also and it’s around the 30 EV for the single charged ions now this scale is now changed to voltage and if you want to go to the electron Vols you have to multiply this with with the with the ion State this is
Uh two times ionized so it’s moving to the right side of course and for both Boron it’s the same and if we compare this now to each other the the Boron and the carbon we see it’s it’s very similar and it’s also in der ranged for the two
Times charges and the and the single charged ions and so we this something we we see also if you use a plasma filter we have the same concentration of or the same relation between carbon and boron in the film independent or also if you do filtering or no filtering it’s always
The same because they are in a similar energy range and so it’s they are filtered the same now if you go to the mum one it’s only five Atomic per in it which is is not much but it has a huge effect and here we see some movement to the right
Side and some very large area or iron flux in the in the carbon plus here it’s voltage that means you have to scale this of course multiply by two and if we go to the to the left side then we of course you have do some measurement at each
Uh chart state of each element then you have to do the scan or set up one scan where you do all this at a at a time and here if you have the voltage this you have to multiply this by by the charge time the blue one stays the same and the
Other ones going far and Far to the higher ion energies and if we are now at the the four plus we are maybe at 200 electron volts which is some very high energy of the mum and of course it’s also heavy and this has some large effect of on our carbon codings of
Course what we see also what we expect from the literature we have some two times charge three times charge this is the the dominant species as we expected also from from other scientists okay now I put it together also always the the C+ for the three different cathodes all the other process
Is the same and we see now the reference in carbon and then we see some movement to to higher ion energies or some higher ion energies if you put boron in it and if you put MO in it and it moves straight to the to the right side and of
Course we affect our our properties of our fims with it how we do this I haven’t brought you here I think this would be too much but we can use this device very well for our measurements and of course if you go then to time resolution then there are other other
Questions we have and it’s still difficult to measure but we are doing it or we I I like to do it it very much and this brings me to the summary laser Arc at all is a technique for industrial scale carbon codings and the machines are sold or running in Industry at several
Several sites and the new customized tsse codings allow new applications or many new applications we have some interests in this already and we want to understand or better understand the evaporation of these kind of materials and utilize this knowledge also in preparing the codings for all kind of
Applications so this brings me to the end thank you and I’m happy to answer questions I think I used the time very well so we can do seven minutes talking and then any questions I don’t know if this is a question or I I can
Answer I I know okay yeah so we we we can um have a specialized version which can be up to 1,100 electron volts um so if we have a high high current there then then then where it biases the whole instrument up to up to the higher
Voltage so it can deal with higher higher high Curr as well so the energy filter is um is able to be driven externally as well as that as well as internally up to so generally that’s okay for higher energy but the thing you you it’s your question answered I think
I know what you mean you have electrons also coming to the to the nozzle of the device also electrons and ions and then of course you heat up the the whole system with the electrons changing temperature and reducing accuracy of the of the device and maybe doing some some
Setup where we extract the electrons before and you have some some plate with some hole in it to reduce the the electron rate to the to your system so so we can the system can be supplied with actively cooled an actively cooled shroud so on the front end of the system
It can be actively Co so it can be kept at a constant temperature um also we can have um we can have some deflection there as well to deflect preferentially the electrons so inside we have we have lenses at the front which can be set to repel electrons as
They come to the front of the system as well so the the structure of the lenses is all is all tunable so you can deflect the species before they even get further down into the system um and by by the time they’ve gone through the extraction system um and through the energy sector
Analyzer um then then yeah they can be or be repelled or they interact with any of the species either internally or externally on the system yeah there’s A’s there’s a few options few options and and does the device have to operate it grounded or can you also put it on some little
Negative potential I think we only need some some 10 wats or so yeah so it can be it can be floated externally the whole device can be can be floated so normally it’s grounded it can be it can be Flo and isolated externally as well so
Um some users are floting to maybe three or four Kilts to to mat their CL condition so this that’s also that’s also possible yeah it is it is low it’s only 1% not 10% as we expect it’s it’s low yes and we know we have to do some
Adjustments to increase the the the the coding rate also for the sample standing in front that means also in this case the the current is very low it’s by the way we operate with the two circuit system and using only the the anode for the for the AR current not the chamber
Anymore and so we have this bad effect and we s also some years ago when we tested it this setup once it’s it’s really bad and we have to adjust this where we have the the the electron sync in in the chamber this is the thing we want to look at
Next but yes it’s too low and of course I can say something about the angle we are using and we have some small sample but it’s it’s still low I’m curious how do you with some some coil magnetically youing already the co the the coil is is covered so there
Are no codings on the on the coil what like some kind of of no it’s it’s purely magnetical bended then you have some high flux in the middle of your coil and this is bended by 90° it’s some aov principal filter type which is well developed and used
For for at several codings nanofilms they are building machines with some double 90° filters to achieve very smooth Coatings and we want to to scale this for for industrial applications for our linear Source how do you de with like the addition of Caron on different on on hours so in the in the
Chamber no we we know Carbon sticks very well to Plastics and we have some some cold coating anyway so we can coat Plastics very well but if you have Metals then you have to use some some addition layer in between something which have some good connection to the
To the steel for example which is chromium and also carbon and chromium are work very well together because they are forming nitrides and so chromium is a very good interlayer for this and we got very good adhesion and no problem at all in this case also have question regarding Ed but
No in the me System since you have Caron issues we we don’t have looked at the inside we sent it back to the to the colleagues and they send it back to us and said there’s no problem at all everything is still conductive but yes if you have high ionized carbon then you
Have some non-conductive films generating and you need only a few and then you have no connection anymore but this was not a problem what we see we have our orice we use a small one at least I assume 50 micrometers if it’s small or not this is something you know
Better and we have to grind this all the time because we get thick coating on on the nozzle and the orifice also at Short measuring times we only measuring for for two three hours or so between cleaning experence you have and you see that the signal is going
Down and you have to do some initial measurement then do your real measurements and then you have to uh repeat the one you did in the beginning and see if it’s still the same if you have still the same transmission through the orice through the the
Device no we we we do it by by some adhesive tape only clean up afterwards this is working fine using a mechan shutter just and then we can just turn it into the so then we when we know okay we would like to to make some initial evaporation process dark then it’s not
Necessary to make a tuning process or something like that use shutter and then after several minutes 30 minutes we open the shut and so we prevent the welcome yes now we we know it of course what we have in the in the cathod initially which is five atomic
And then in the codings for Boron we have exactly the same independent if it’s filtered or nonfiltered and for mum we have some some changing in ratio mostly we have some more mum in the coding than it was originally in the cathode but up to 10% maybe 7 to 10 it’s the
Highest it does yes of course you have the heavy mum you expect some changes if you shoot the mum deep inside the carbon then you have some some SP2 Rich traces or graphenic traces inside the material which makes totally different properties we did edx measurements a it it’s working
Good then it’s it’s getting more difficult of course we also did or not we another front of Institute in the project did XPS measurements of it do some some spot deep scan and seeing what’s the contribution or distribution of the single elements within the coding
Depth and so we see also we have not the highest amount of M on the surface it’s 20 30 nanometers below the surface it’s not it’s it’s this small it’s very difficult to measure of course with exd we don’t see anything that’s what we expect of course no we haven’t looked in
It this much to see exactly what we have some nanoc Crystal of this materials it’s maybe it’s possible by fancy techniques but we don’t have it and so we don’t do it and if we don’t get it by selected a reflection then we don’t want to look any deeper in
It okay thank you thanks