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I am working on the sputtering of Tungsten. For that I wish to ball mill Tungsten and make a compact using hydraulic press. I have doubt with the duration of ball milling and after making the pellet at which temperature the pellet should be annealed in order to remove PVA.
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Thanga Bharathi Tamilmani Depends on what the chemistry is of the balls in your ball mill (for example if ceramic, they they will mill and not the hard W) and their size. It may not be possible - Google 'comminution limit.' You may only get plastic deformation with tungsten and not comminution...
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I am trying to make a Tungsten sputter target compact. First I am going to dry mill the Tungsten powder in a planetary ball and after milling addition of binder PVA and making a compact and annealing the compact in a tube furnace. But I have a doubt with the temperature at which the compact has to be annealed.
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I don't have an exact graph for that, but in order to change anything about the homogeneity in your sample, the atoms have to move around. At which point this movement becomes significant enough in order to make a difference, depends on the energy required to remove an atom from its old position - and the macroscopic properties that are associated with this process are the melting point and the melting enthalpy.
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I am trying to prepare to Lanthanum-Tungsten alloy target. For that, I am in need of proper procedure to carry out that step. Please give me some general instructions for the preparation of alloy sputter targets.
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You can purchase La doped Tungsten (La-W) alloy sheets which can be 2 to 3 mm thick, and make a target out of it to make thin films. Well machining them to a circular shape can be difficult, and you may consult the manufacturer and he can probably provide you with circular discs. You can google, and find the following company Edgetech industries LLC, and check if they can help you out. Try to google and find out the availability of such a thing.
Make such a target yourself by pressing powders is not an easy task to make an alloy target, because you need sufficient expertise in powder pressing techniques, and the specialised equipment to do the pressing at high pressures and temperature, and preferably n vacuum, to prevent oxidation.
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How to make an alloy sputter target (La-W)?
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If you want to mix metals, you can indeed use a hydraulic press, but that would not be a fully alloyed target, it would just be granular enough for decent results in many cases. As I said, the bottleneck for your particular system would pobably be not so much the boiling point but rather the oxygen load since you would have a constant source of oxygen within the target. In the works that my former colleauges at KIT did that wasn't important because they used preparative mass spectrometry and could easily deselect oxidized clusters; in a magnetron sputtering epitaxy setup like the one I'm using in my current job that would be deadly which is why we don't do that here.
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I am trying to sputter ITO film with RF at room temperature on the flexible substrate, but my lowest resistivity can only be 2.5Ω ·cm. My sputtering condition :30min/0.3~1.5pa/120w/Ar/room temperature. I have referred to many papers, but my experimental results have been unsatisfactory. What can I do to get the resistivity down
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Dear Li,
the resistivity depends on the material which are using for sputtering. So firstly confirm about the material resistivity. Again you can try with another Ar flow rate and RF power.
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I have prepared zinc oxide sputter target by using PVA as the binder. But in case of Tungsten target whether PVA is suitable and will it react with tungsten?
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PVA cannot react with tungsten, but if you do not completely remove it during firing (for example, by heating the compact too quickly above 400°C), then the carbon that remains from the thermal decomposition of PVA will be able to react with tungsten when further heated above 800°C As a result, your tungsten target will have a small amount of tungsten carbides. I believe that even in this case there should be no problems with the work of the target.
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I am not able to understand the reason behind non-stoichiometric behavior shown by the thin films deposited with reactive sputter deposition technique.
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Again, have you verified with a TixNy standard of defined stoichiometry that your XPS values are accurate? At this point of the discussion it's still not settled that your compounds are non-stoichiometric in the first place.
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How can we mathematically calculate the critical thickness of polycrystalline(Sputtering) grown thin?
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Thank you, Dr. Len
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Please explain what difference in principle makes them unfit for an interchange. Also TMP works max at 10^-6 practically. However many companies claim that they can attain a vacuum of 10^-10. WHy is this not possible practically?
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Following up: a scroll pump is a rough-vacuum pump used to pump down from atmospheric pressure. A turbopump cannot be started directly at atmospheric pressure, you need another pump (a backing pump, for example a scroll pump) to get the inlet pressure down to typically <<1 mbar before you can start the TMP.
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I have to analyse my Chitosan Cu nanocomposite sample through XPS. I need an idea about the energy of Ar+ ion and the time of sputtering if etching is done prior to XPS analysis.
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Dear Dr. Elbright Dillu ,
I suggest you to have a look at the following, interesting paper:
-Towards reliable X-ray photoelectron spectroscopy: Sputter-damage effects in transition metal borides, carbides, nitrides, and oxides
G.Greczynski,. L.Hultman
Applied Surface Science, Vol. 542, 148599 (2021)
My best regards, Pierluigi Traverso.
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Hi all, I am depositing thin films onto quartz glass substrates, but due to supply problems the only adhesion metal available to me is chromium. My 2nd layer is silver to provide good conduction. Does anyone have experience with chromium-silver films? Does silver adhere well to chromium?
Done the usual googling and came up with nothing - maybe I'm not googling correctly.
Thanks in advance,
Nick
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In the past I have Cr and Al thin films (<5 nm) onto SiO2 substrates, followed by a much thicker Cu layer. With evaporation I managed to create a robust Cu layer to about 200 nm. Moving to a sputtering process allowed Cu layers up to 1 um. In both cases my process was very similar to K. Sreenivas' outlined above.
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When using the  Kurt J. Lesker Co (R301/MC2)  for Sputter deposition of AZO, at the process pressure of 2 mTorr, Forward power of 146 W, Reflected power- 5 W and RF power of 150W, the normal DC bias is around 100 V. Recently it has started to change and keeps on increasing. The same process recipe is now resulting in AZO films with sheet resistance 5x higher. I want to know possible causes and remedies for this.
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I have simillar problem, but in my case the bias decreased from 190 V to 5 V. I checked for magnetic properties of magnets and they are all working well. I am using 400 W for a tungsten target (Kurt J Lecker) and the target is new and it is working on other magnetrons. What can be the possible reason that the magnetron is not working properly?
Thank you
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I deposited the thin films of MgTiO3 using RF sputtering onto quartz substrate. After XRD analysis of thin films and sputtering target (home made), it is observed that the lattice parameters of films are smaller than the Sputtering target. Please help me to find the reason.
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Enough time has passed since you asked the question, but if the question is still at all relevant. All answers imply that you grow an epitaxial film of MgTiO3 on a monocrystalline substrate. Is this really your case? And one more point - to what extent the lattice constant of the sputtering target corresponded to the tabulated values? Maybe the problem was in the target, for example there were impurity atoms that caused an increase in the lattice constant.
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how to hold powdered nano particles as substrate in sputtering system
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In another way, you can make target (pellets) as per your sputtering unit requirement by solid state reaction method. Then anneal (sinter) the pellet more than 900oC, your target will ready for sputtering.
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What mean by the ionization degree of the plasma injected into the vacuum chamber for sputtering process? What's the relation between this degree and the number of gas ions?
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The relationship you are looking for is this one:
So, it's just the percentage of atoms/molecules in the gas phase which are ionized.
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I have Al2O3 and AlN insulators with graphite & SiC sputtered deposit which needs to be cleaned off. I've tried HF (currently limited to spot cleaning due to safety restrictions), HNO3 and Aqua Regia (40-50 Celcuis, 1h). Currently none of these methods seem to touch it. Can you suggest some chemical methods to clean these ceramic components?
Perhaps H2SO4 or H2O2? Could an alkaline solution work?
Thanks.
NB: These insulators are used as part of a GD-MS source, and in use will build up a deposit of sample. This is what must be removed.
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Cleaning alundum is as easy as shelling pears - you need to heat it in air to 500 - 600 C - carbon will simply oxidize, and SiC will be removed mechanically (in order for it to oxidize and silicon enter the structure of alundum, significantly higher temperatures are needed). By the way - aqua regia and acids in general are a very bad idea. After two or three treatments, alundum crumbles along the grain boundaries (it will very brittle) ... I have never worked with aluminum nitride - I don’t know.
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For NbN,
The mol. weight = 106.91 g/mol
The volume = 87.65 cm^3
Density = 8.102 g/cm^3
The time of deposition = 90 min
The mean thickness = 1118.1 nm
The deposition rate = 12.4 nm/min
For VN,
The mol. weight = 64.95 g/mol
The volume = 70.95 cm^3
Density = 6.080 g/cm^3
The time of deposition = 125.15 min
The mean thickness = 1461.8 nm
The deposition rate = 11.7 nm/min
The two targets are :
1- Radio Frequency (RF). The power is 180 W
2- DC Pulse. The current is 0.5 A
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The question you have on energy transfer in binary conditions in sputtering is given by the formula:
Et/Ei = 4(mi*mt)/(mi+mt)2 * (cos)2 angle (a)
The fractional energy transfer Et/Ei (transfer vs incoming) from mass mi (Ar impinging on target) and mass mt (NbN or VN) is determined by the above formula. Normally, the indicent angle a is 0 degree to the normal and the sputter yield is given by:
S = 3a/4pi2 * (mi*mt)/mi+mt)2 * E/Uo, where E is the nuclear stopping power of the material and a is monotonic increasing function of mi/mt, which has value 0.17 for mt/mi =0.1 increasing up to 1.4 for mt/mi = 1.0. Uo is the surface binding energy of the material.
In practise, mol weight of VN is closer to mol weight of Ar sputter gas compared to mol weights of NbN to Ar. The fractional energies are 0.93 (VN) versus 0.23 (NbN) using above formula
Assuming similar DC-bias (kin energy) on the two targets would mean the VN sputters ~4 times faster than NbN. This might deviate a bit because also the spatial distribution from fragments coming from the target is wider for VN tan for for NbN.
regards,
Peter
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What are the factors affecting the peak intensity for a sputter deposited epitaxial thin film and how to control these in order to get a highly crystalline film ?
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By increase x-ray path length
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I'd like to have a metallic film with porouses inside by using dc sputtering method. In this way, what parameters of sputtering should be higher or lower ?
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Lower Substrate temperatures (room temperatures to upto 100 degree Celcius) and Low sputter power gives thin films more porous thin films
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Hello everyone,
I want to study the change in oxygen vacancies in gallium oxide using AES. I looked for papers, but couldn't find any. If you have any references please let me know.
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Aman Baunthiyal oxygen vacancies are mainly studied by theoretical methods, as you can see in the article below. To obtain some experimental insights about it I recommend you perform X-Ray Photoelectron Spectroscopy (XPS) analysis.
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Hello all,
What are the opinions of the following three companies for sputer coating and carbon evaporators?  Denton, Cressington or Quoram.
Thanks for your replies,
Michael Delannoy
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Hard to compare, we have Quorum coaters - those are fine and easy to maintain. I believe any of those will do the job, the question is only money you have and space to place it :)
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hello.
I want to obtain a plot of the sputtering rate according to the angle of the sample with the incident angle of the ion beam fixed.
In this case, I think that should calculate using "Ions with specific energy/angle/depth (full cascade) using TRIM".
To do that, I need to create a TRIM.DAT.
However, a TRIM file can only contain information about the location and orientation of ions, not the sample.
Please advise on how to obtain the sputtering rate according to the angle of the sample.
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It is very easy to get phonon.txt file. You just run with detailed calculation with full damage cascade then you will find the option of phonons. On the left side of phonons there is a option of file which you can save to your computer and you get text file data phonons by ion and phonons by recoils with the depth. Hope you will able to do.
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One cycle Argon ions reach and sputter sample, the next one electrons neutralize the surface keeping the process going on.
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Hi Fernando, 60Hz is just too slow a frequency to have any real sputtering effect on an insulator. You are correct in how the process would occur but the target behaves as a very small capacitor, so there is only a very small amount of charge transferred with each cycle, at 60Hz this would be so tiny as to have no noticeable sputtering. Even at the normal MHz RF sputtering frequency the sputtering rate is very slow, so actually insulator sputtering is always the very last resort, if reactive sputtering or some other technique cannot be used.
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I am looking for a cheap and simple sputter unit that can sputter metals like Au, Ni, Cr, Al onto a substrate through a shadow mask for pattering (20 mm x 15 mm mask area, 30 micron resolution, for film thickness in the order 100 nm). One target at a time is enough.
I am on a budget so I am looking for researchers with personal experience of a simple machine, not for marketing broadcasts from manufacturers.
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Hi Martin, a simple system such as those made for SEM / TEM sample coating might meet your needs. (Have a look for "SEM coater".) You can probably find one at a microscopy department to have a "play" with to see if it does the job.
You might be able to find a second hand one for sale on the internet.
Many use a simple "diode" magnetron, which lacks a magnet, this will actually give you much better target usage, (particularly helpful with expensive materials like gold) but does reduce the sputter rate though this should not be a big issue.
Materials like Ni, Cr and especially Aluminium, can be difficult to start sputtering however as they get a tough oxide coating on the target that is difficult to sputter off, so may need a more complicated system.
You could consider a thermal deposition system which would be very quick and simple. A "bell jar thermal coater". Typically if you used a liquid nitrogen cold trap, to improve the pressure Aluminium etc. will coat very easily and cleanly.
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We generally sputter SiO2 using low power (~25 watts) RF sputtering.
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To avoid the pinholes of SiO2 from sputtering, the minimum thickness should be more than 100 nm.
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Hello
I have a couple of sputter targets that are not working anymore because they have holes burned in the middle - the Ar plasma arc is burning out almost only around the middle region of the target (see picture).
Since there is clearly some 90% material left can I somehow reuse/recycle the target?
Is there a possibility to recast it to be thinner but still working?
I use pure gold and Au/Pd: 80/20 targets.
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Melting and reshaping requires controlled environment, which may be more difficult task ...and if contamination occurs that will affect your results...hence better option is to give it to supplier and get discount...
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Looking for recommendations for sputter coaters. All the ones I've looked at seem to be, by and large, the same. Looking to sputter, C, Au and Au/Pd. Any important differences I should be aware of? Thanks!
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Dear Garrett, we've bought two different systems in the past - the main difference was the size and shape of the sputter target. One system had a ring-shaped target, which is difficult to exchange, so that you have to rely on the support of the supplier company, that you'll be able to get suited targets in, say the next 5 or 10 years. The other system simply has a circular-shaped target, where you can easily replace the target material to whatever you want. We have now used that system not only for standard coatings like the ones you've mentioned (such as Carbon, Au, Cu, Pd), but also for much more "exotic" materials like W, Ta, Ti, Al, ... and even a high-TC superconductor YBa2Cu3O7 and other compound materials. So I would strongly recommend a system with an easy exchange of targets and the possibility of using self-made targets. Best regards, Dirk
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How can I know all these?? Are there any references of ionic crystal's sputtering annealing time and temperatures? Thanks.
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The sputtering happens in a low vacuum chamber, P >= 10^-3 Torr
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Dear all,
I was trying to use DC sputtering to coat around 50 nm silver on both side of a casted PVDF film (thickness around 25 micron). I used a 3d printed ABS mask during the sputtering. I checked the surface morphology under SEM and found no pinholes and severe porosity. I wonder is there other reasons this short circuiting could occur, and potentially how to avoid it.
Thank you very much.
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Jignesh G. Hirpara Thank you very much for your answer. May I know the reason of using the metal as mask? I thought you explain it in the first thread but I fail to understand. Thank you.
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Does ZnO (for instance by sputter deposition) deposited on glass reduce the wettability of glass?
I have come across a few references that say ZnO is hydrophilic, other that it is hydrophobic. Under what circumstances does it become hydrophobic?
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Switching between hydrophobicity and hydrophilicity has been observed on ZnO and TiO2 surfaces by interrupted UV illumination. In addition to surface energy considerations (orientation of crystallographic planes) and roughness factors (increased proportion of air/water interface increases the hydrophobicity), surface defect sites play a crucial role. Oxygen terminated surface will be hydrophobic while oxygen vacancy sites will easily bind with water.
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The ring type occurs after some time when coating get started. It will goes away when we reduce the RF power of system. It also make a ring track on AZO target.
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For sputtering AZO (Al-doped ZnO), because of its relatively high conductivity, you can use DC. You don't need RF at all. I agree with Dr. Weippert that you have a rotating magnet array below the planar target, there must be some form of interference with the RF frequency. My experience is that such technology (RF) gives rise to all kinds of aberrant effects during processing.
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Does anyone know of a good reactive sputter recipe for yielding TiO2 optical thin films with low extinction coefficient, small grain size and low surface roughness? I have some papers but most of them use a biased substrate (something I can't do in my tool).
I've been using RF sputtering at room temp, 540W and a 3"Ø x 0.25" thick pure Ti target which I pre-condition with Argon to sputter off any native oxide. I keep finding that even with low O2 flows, I get target poisoning no matter what. The target clearly comes out oxidized and my deposition rate gets choked to about 2nm/min. My throw distance is restricted to about 5 inches.
I've not yet tried DC sputtering but most of what I'm seeing online is pointing me in that direction. Again I'd like to stress that I need low optical loss above anything else.
Any advice is welcome, thanks!
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2nm/min is actually not that bad, by the way. It's normal that oxide sputtering can be a bit slower.
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I need to figure out a way to depoison a cerium target that was poisoned during reactive sputtering with O2. Any experience or advice is very much appreciated.
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Sure you can, this process is referred to as "pasting". It means you introduce a dummy substrate and perform just metallic sputtering in order to blast off the poisoned top layer.
However, this is not always straightforward and may require some development time since a too harsh pasting may cause the coatings on your chamber shields to become unstable while, of course, a too soft pasting simply doesn't do the job.
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I want to create a hard etch mask for etching Si anisotropically using KOH. The etched structures need to be quite deep, several 100 um.
I understand that the two common hard etch mask materials are Si3N4 and SiO2. Currently I have access to RIE, but only Ar and O2 gas tanks, so I can't dry etch the silicon nitride, which seems to be the most common method. We've tried sputtered Cr as a mask, but the adhesion to Si is less than ideal. The best success we've had is a complicated process: sputter Cr onto Si3N4 coated Si, create a photoresist mask, etch the Cr, strip the resist, etch the Si3N4 with BOE, strip the Cr and finally etch the Si with KOH. I'm looking for something simpler ideally.
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Thank you both very much, I really appreciate it. I will investigate the possibility of acquiring SF6 or CF4, although I am not sure the exhaust system is set up to handle the byproducts. We do have a Ti target, so that is certainly an option.
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Like to know If I take without doing sample preparation Shall I get clearly images or not? Where I can do sample preparation in Tamil Nadu for taking TEM images with EDX?
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Dear Dinesh Babu, I taken TEM images of polystyrene-Silica nanocomposite without coating. I got good images.
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I made evaporated Cr/Au patterns through lift-off process on silica on Si.
Then, I sputtered Cr on the wafer and pattered the Cr layer for SiO2 dry etch mask formation.
Cr/Au was for heater on silica waveguide, and etched trench was for thermal isolation between waveguides.
After SiO2 etch process, Cr etchant did not remove completely the Cr hard mask on Au layer.
On the other hand, Cr on SiO2 was removed without problem.
The residual Cr was confirmed by measuring the surface profile, showing ~100nm thickness.
Has anyone experienced something similar?
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Hi, there are two types of chromium etchant, what you observe happens quite frequently using the mixture of perchloric acid and ceric ammonium nitrate on heterostructures which have undergone certain processes. Instead the Cr etchant based on sodium hydroxide and potassium permanganate does not have such issues. You can find different commercial solutions CR etch 100, 200, 210... tailored for different material selectivity but i do not expect particular problems for gold.
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Hi,
I would like to know if there are special issues when sputtering PTFE with shared cleanroom infrastructure. Would there be cross contamination, out-gassing during later depositions, etc? I have trouble finding much info in the literature, and generally polymers are kept away from the vacuum systems.
Thanks!
Michael
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Sputtering fluoropolymers will give you very persistent fluorocarbon/ fluoride contaminations in your vacuum system. It will be a source of fluorine for a long time! The cleaning would be rather difficult: sand paper.
Nobody published about such a mess!
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Hi, I want to deposit a metallic film (~800nm, sputtering, evaporation...) on top of a FTO glass to improve the conductivity of the substrate. The substrate will face temperatures of 500 ºC for 2h in air environments. I'd need a metal which does not oxidize or just the superficial nanometers, thus a significant part of it is still metallic
do you know any metals which can be deposited and stand these conditions? better if we can avoid Pt/Au/Ag and other expensive/rare materials
thanks a lot!
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If you really want to avoid noble metals, you're going to have a hard time achieving your goal.
There are of course non-noble metals which form a passivating layer such as Al, Ti or Cr which will form thin oxide layers. You could check out if the passivation effect on these is sufficient up to your process temperature.
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So we receieved multiple sputtering targets. First we tried chromium and it sputtered well with high deposition rate at pressure 1.68e-02 Torr and argon flow 30-50 SCCM. After we tried to make series of cobalt films. When cobalt filme were sputtered, we tried to sputter chromium again, but plasma just blinking even with high pressure (5.5e-02 Torr) and maximum voltage (1200 V) and old sputtering parameter do not work either. Only after reducing argon flow ( and as a result pressure) to it's possible minimum, plasma has stabilized, but brightness of plasma is very low and deposition rate is almost zero. So i can't find an answer why it happens and how to make chrome sputtering as good as it was before cobalt sputtering.
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Hi Nikita, It sounds a bit like your Cr target has developed an oxide / contamination layer. You should be able to clean this off running at the lower pressure for some time (but it can take a while!). Or you can take the target out and polish the surface to clean off the oxide contamination.
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I am depositing Silicon using RF magnetron sputtering onto glass/CaF2 substrates for my research.
My standard process parameters are:
Power: 400W
Pressure: 0.24Pa
Base pressure: 3.35e-4 Pa
Target to substrate distance is about 6cm
Reflected power: 9W
Vbias: 360V
I have ran this process in the past and it has worked fine to produce a film of about 1µm thickness for about 100 minutes deposition time. But since last week when I try to run this process, there is no material on the substrates at all and there is also some amount of dust accumulated on top of the target after the process.
I thought this issue could be from the dark shield being placed incorrectly but I checked different position and it did not change anything. My other thought is that the substrate holder is somehow not grounded properly anymore and the material atoms are no longer being accelerated towards the substrate. I have no checked this as I am not sure how to check the bias between the target/magnetron source and the substrate holder safely.
Any advice/suggestions on what the issue could be or how to fix this would be appreciated. Thanks.
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Hi Philip. Did you, in the past record the bias voltage of your RF supply? This can be a useful guide as to if something had changed.
It actually sounds like the surface of your silicon target might have developed a tough oxide coating on it. (the DC bias voltage would been seen to have increased).
I recommend abrading the target surface to break through the layer.
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How the backing plate can effect sputtering during process?
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Babak answered the problem concisely. Targets without backing plates are generally clamped down, so if the material is likely to object to this, and crack a backing plate is used.
However I would absolutely recommend NOT using RF for metal targets! RF is a very last resort when sputtering is it is very hard to get a good sputtering efficiency and deposition rate, so really only used for ceramic and insulating materials. The preference is DC... then pulsed DC, then Mid RF.. then (last resort) RF..
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In my research I am using sputtered electrically contacted gold electrodes for voltammeric measurements on a glass slide.
To prevent the adhesive layer from detaching at the anode, I use titanium as an adhesive layer. Cr is dissolving at the anode resulting in a detached gold-electrode.
Since I have very limited access to a high-vacuum dual-target sputter, I was wondering if there is a way to create a voltage-stable adhesive layer with a cheap single-target sputter.
Thank you in Advance!
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Hi Maxamillian. You should be able to get gold to stick reasonably well to your glass substrate, but it must be very well cleaned. As the other reply suggested you can RF bias the substrate. If you have limited options, you could simply use a magnetron with a target that does not sputter well, and make sure the substrate is bathed in the plasma for some time, a little oxygen in the plasma would also help if this is an option, the gold should then be deposited whilst the substrate is still under vacuum to prevent re-contamination (water vapour is the most likely form). If you run a finger over a "cleaned" substrate you should find your finger sticks to the surface and if it moves, "squeaks" - like a plate cleaned with hot soapy water. (An finger on an uncleaned substrate will more "smear").
You could use reactivity sputtered aluminium (with a little oxygen). The aluminium oxide makes a good adhesive layer, but it can be very hard to get a good sputtering rate, so you can utilise the plasma itself for the cleaning. Or if you don't have the option of oxygen even Aluminium itself, as again it can be hard to sputter this material to begin with.
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For Sn and Fe sputtering targets bending of plasma occur; we need nearly focused plasma of these targets. Even after increasing power, results remain the same.
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I agree with Babak Bakhit.
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for sb2se3 thin-film solar cell. I had deposited ito/sb2se3 next step is to deposit Cds . what is the best method to deposit it for solar cell fabrication? except than sputtering also discuss efficiency behavior.
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you can use chemical deposition
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To obtain the same amount of plasma at the same pressure:
Is RF power needed for (copper bonded sputtering target) is greater or equal to RF Power needed for (unbonded sputtering targets)?
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As some of the previous replies emphasised, there should be no difference in the plasma. Cu backing plate, and Cu bonding to target is basically used for efficient cooling purposes. Without bonding some target materials will simply crack at higher powers. Cu is preferred because of its high thermal conductivity, and will efficiently remove the heat generated during the sputtering process
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As stated in the question, we want to deposit thin film using an iron target by magnetosputtering under argon atmosphere with a DC current source. But we couldn't even start the arc. The sputtering machine we used has a face-to-face geometry of target and substrate, where the substate is at top while the target at bottom. The target-substrate distance maintains ~92 mm. The parameter we've tried are sputtering power of 150 W and 300 W at an Argon pressure of 4 Pa, 6 Pa, 7 Pa, 8 Pa and 9 Pa, respectively.
We would like to ask for your knowledge on magnetosputtering and suggest a way to resolve this issue. Thank you.
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I also have some experience growing magnetic thin films. As Paul Lippens mentioned, the key point to ignite plasma is having correct magnetron configuration. That is why such films cannot be grown in most deposition system as their magnetron powers, polarities, etc. are not suitable for these types of depositions. Indeed, the target should be as thin as possible, but the challenge is that lower than some critical thicknesses, you get deformation in the target. You may be able to ignite plasma by applying very high pressure, go for almost the maximum ones of your system, and try to ramp up power. It may be a good idea if you have a supporting target as well (co-sputtering), like Ti, to see if it helps or not. All these 3 helped us to ignite Fe and Co plasmas.
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I coat Ge over Al using sputtering for wafer bonding without breaking the vacuum between the two layers. I started having a dull color on the top surface after a target change. I tried diltue HF cleaning but it didn't affect the dullness. The layers seem fine when they are coated separately. What might be the reason for this?
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Hello Gürel,
may be , you have an optical effect. Then, the reflectivity must depend on the thickness of the upper layer.
Aluminium has a high reflectivity(metallic). Germanium is a dielectric layer (conductive, if doped, but in this respect (reflectivity) dielectric). We can apply Fresnel's laws. Furthermore we must take into account the gap of Ge (nearly 0,7 eV). That means a high absorption for visible radiation.
If the layer compares to the wavelength of light (what is fulfilled at sputter deposition, then the light can penetrate the Ge-layer and is reflected at least one time from the Al-surface. The light is reflected and transmits the Ge-layer but is almost strong absorbed. Therefore, the intensity is damped what gives a grey effect. Besides this you have an interference effect (like the UV-protection layer on photo objectives (there you have a blue-dark vision). This erases the outcoming light and gives a dark effect (must depend on incident angle).
For thick layers only the reflectivity determines the optical appearance. Furthermore, the surface quality determines the surface scattering. For rough surfaces (structure elements comparable with wavelength) you don't have bright (directed light) but dull (scattered light) surfaces.
With Regard
R. Mitdank
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In the case of magnetron sputtering, we have to fix the sputtering chamber pressure to a particular value. But after the formation of plasma, the chamber's pressure will increase. So, my query is that we have to consider the working pressure in the presence of plasma or the absence of plasma?
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During the RF process, the meaningful parameter is the pressure during the deposition process - with the presence of the plasma.
See i.e.
"Prior to the experiment, the sputtering chamber was evacuated to be less than 1 × 10−6 Torr. For sputtering, RF power was kept at 160 W and Ar gas was used for plasma generation. Pressure was varied from 20 to 80 mTorr. The parameters chosen in this study are those commonly used in the RF sputtering process".
This process affects the quality and morphology of the coating, so during the characterization of the process, the pressure is one of the optimization parameters.
"The purpose of this study is to confirm how the generation of charged NPs depends on pressure and affects the film deposition during RF sputtering using a Ti target". Hope this helps.
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Hi, everyone. How can I to reduce the cracks when a Au film(the thickness is 100 nm and the width is 150 um )is deposited on PDMS with sputter coating. In addition, how to improve the conducity of sputtered Au film. Thanks a lot
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Dear Liu Peng,
The PDMS is soft and flexible. To avoid the cracks of Au films on the PDMS, you may need to have an adhension layer between Au and PDMS such as organic self monolayers. Alternatively you could try 5nm Cr or Ti thin films.
You are right the gold films can't be thicker than 300nm. Ideally 200nm is enough for a good conductivity of Au films.
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Suppose gold sputtering layer thickness is thicker than the thin film thickness of my sample. What type of error shows for the morphology of my thin film.?. Is there any chance of only gold morphology?.
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If Au layer is smooth and uniform then you can get signatures of morphology of underlaying thin film.
You can also try X-ray reflectivity to determine the roughness.
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If you had to protect a thin metallic layer by depositing (sputtering?) a capping layer, what would you use if you had the additional problems that
1) you dont want it to be a metal,
and
2) you dont want it to be an oxyde
???
thanks for any input...
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There are many thin, hard coatings on metals that consist of nitrides. The best known are functional coatings based on titanium, aluminum, chromium and zirconium nitrides on cutting tools. The thickness of current coatings applied by PVD methods is usually in the range of 1-5 microns. The thinnest functional carbon based coatings (DLC) are about 0.5 mm thick. In principle, coatings several tens of nanometers thick cannot be either protective or functional.
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Hello everybody
I'm looking for the experimental parameters used in sputtering process as:
1~ vacuum chamber energy, gas pressures and temperatures range
2~ distance between target and substrate
.....etc
Thanks a lot
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I suggest you to have a look at the following, interesting papers:
-The Effect of Sputtering Parameters on the Film Properties of Molybdenum Back Contact for CIGS Solar Cells
Peng-cheng Huang, Chia-ho Huang, Mao-yong Lin, Chia-ying Chou, Chun-yao Hsu, and Chin-guo Kuo
International Journal of Photoenergy, Article ID 390824 (2013)
- Influence of sputtering parameters on microstructure and morphology of TiO 2 thin films
Seon-Hwa Kim, Yong-Lak Choi, Yo-Seung Song, Deukyong Lee, Se-Jong Lee
Materials Letters, 57(2), 343-348 (2002)
Available, as full texs on RG, at: Influence of sputtering parameters on microstructure and morphology of TiO 2 thin films
- Effect of sputter deposition parameters on the characteristics of PZT ferroelectric thin films
Zhenxing Bi, Zhisheng Zhang and Panfeng Fan
Journal of Physics: Conference Series 61 ,115–119 (2007)
- The Effect of Sputtering Parameters and Doping of Copper on Surface Free Energy and Magnetic Pr operties of Iron and Iron Nitride Nano Thin Films on Polymer Substrate
Waheed Khan, Qun Wang, Xin Jin, and Tangfeng Feng
Materials (Basel), 10(2): 217 (2017)
…..and a previous similar RG question, available at:
Good luck and my best regards, Pierluigi Traverso.
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Dear all,
I am trying to deposit Al over bonding layer on Glass to get Al mirror using RF sputtering. What should be the exact thickness of Al layer to get the stable Al mirror. Also, what should be the RF power and estimated time accordingly.
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Dear Shashi Kant , thanks for sharing this question with the RG community.
Let us assume that you want a mirror which blocks completely the pass of light (visible light). In my own experience you would need a film thicker than 150 nm, otherwise the mirror will be a partial mirror (some light will pass through). For security you can deposit a thicker layer, say 200 or 300 nm thick.
In my experiments I never used a bonding layer. Aluminum is fairly attached to the glass surface (soda-lime glass, BK7) and also to several polymers (PET, PDMS, PMMA, etc). Of course the substrate must be cleanead following the common cleaning processes.
The RF sputtering parameters do not just depend on the RF power, several other aspects are important as well, such as base pressure (chamber vacuum), the sort of sputtering atoms used, their presure while sputtering is also important, the deposition rate, RF power and temperature are also variables to take into account.
This aspect has been already clearly explained previosly here, please, see for example:
For more detailed descriptions you might be interested in reading some classic publication, such as:
Apart from direct internet searches you could give a try to the RG´s searching option, it will provide useful informations in most cases.
One last note, that could be or not important for your work. Aluminum surface will be readily oxidised when exposed to the air, in few hours it will be completely covered by a thin layer of Al2O3, but as the oxide layer get thicker it becomes more and more impermeable to O2 and when it reaches a thickness of around 4 nm it stops growing.
Hope this helps. Good luck with your work and my best wishes!
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my group has a small vacuum chamber built for thin film co sputtering, the two guns were initially coupling but we solved that issue by spacing the guns farther apart. However, the issue with the plasma is still there. When we fire both guns, the plasma starts flickering on and off at a high frequency. We are fairly sure that it’s not due to contaminants in the chamber.
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In addition to the comment by Valentin Bogatu , how does the matching for your RF source work? Is it automatic or manually?
If it's manually, it could make sense to check if the flickering can be decreased by retuning, if it's automatic, check if the capacitors don't come to rest, maybe their positions might be correlatable to the flickering frequency.
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Hi,
I wonder if anyhow is familiar with the lift-off process of sputtered SiO2 layer with the thickness of ~200nm?
I would be really appreciate if you could recommend the suitable photoresist and stripper (if acetone does not work) that could do that. I understand that sometime sputtered materials are difficult to lift-off with acetone.
Many thanks!
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Hi,
I also wanted to ask the same question as Chun Hong Kang.
Is that possible to do a lift-off process for PECVD deposited SiO2?
Thanks and best,
Huijie
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I am doing ferroeectric loop tracer on ferroelectric thick polymer films, but my sample always get puncher well before the coercive filed. Why such thing is happening?
1. Porosity in sample?
2. Electrode (sputtered and silver pasted?)
3. Other parameter (frequency, ramp, thickness or anything)
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The thickness of polymer film can be 30 to 60 micron (we can tune it) with 100 nm EBeam sputtered electrodes. We are also using silver pasted electrodes to measure the PE loop (also reported in literature).
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I am planning to buy LNO powder but not sure on how can I make the LNO target with 3 inch diameter and 0.125 inch thickness by using this LNO powder.
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Dear Md. Abu Sayeed thanks for posting this interesting technical question on RG. In this context, please have a look at the following relevant article which might help you in your analysis:
Structural and electrical characterisation of lanthanum nickelate reactively sputter-deposited thin films
The paper is unfortunately not accessible as public full text on RG, but two of the authors have RG profiles. Thus it should be easily possible to request the full text of the article directly from one of them via RG.
There are various commercial sources of LNO sputtering targets, e.g. https://www.sputtertargets.net/oxide-ceramic/lanthanum-nickel-oxide-sputter-target.html
and
Good luck with your work!
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I want to validate these results which are showing in pictures. I am using SRIM software. I do not know about the hydrogen ratio in this combination. I read many research articles but do not find right solution. I mention below the paper link..
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Waheed, please reformulate your question, because it is unclear.
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It is required to calculate the sputtering yield of the material (for example, graphite), taking into account its additional heating to a high temperature of about 1500K. Ion sputtering of the material occurs at a fixed ion energy (Ar+ at energy 500eV).
How can the temperature of the sputtered target (for example 1500R) be set in SRIM/TRIM?
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Anna,
SRIM let you possibility to calculate the sputter yield. At high enough temperature you can estimate evaporation in addition to sputtering. But these two processes are different. So, as Mustafa Kamel Jassim said already SRIM does no include evaporation.
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why does sputtering have better step coverage compared to thermal 
evaporation? 
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The sputtering pressure is higher than that of thermal evaporation, there are many particle collisions, and the sputtering has a magnetic field, so the particle trajectories are different. In addition, the incident energy of sputtered particles is tens to hundreds of times greater than that of thermal evaporation. The sputtering has diffraction phenomenon, the shadow effect at the step is not obvious, while the thermally evaporated particles move almost in a straight line and can not reach the step. The film quality is poor. In addition, it is also related to the incident energy of particles
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If I deposit TiO2 on a FTO/perovskite substrate by RF sputtering, is there any chance that the sputtered TiO2 particles damage the perovskite layer.
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Dear Anurag, thank you for asking this very interesting technical question. My personal suggestion would be to just try out this experiment instead of speculating. For more information about RF sputtering of TiO2 on FTO/perovskite substrates please have a look at the following potentially useful article:
Radio Frequency Magnetron Sputtering Deposition of TiO2 Thin Films and Their Perovskite Solar Cell Applications
This article has been published Open Access and can be freely downloaded from the internet (please see attached pdf file).
I assume that only an experiment can give you a definite answer to your question.
Good luck with your work and best wishes, Frank Edelmann
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I am currently working on some magnetic multilayer stacks. I am thinking if it could be possible to grow magnetic layers on top of a TiN seed layer. Usually I use TaPt as my seed layer.
I can do room temperature sputtering deposition and directly deposit TiN (non-reactive) on to thermally oxidized silicon wafer. Could someone give some insight into this?
Thanks!
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We tried to compare quality of magnetron sputtered Cr layer on polycrystalline diamond surface compared to magnetron sputtered Cr layer on Zr surface. The quality of Cr layer sputtered on polycrystalline diamond surface was worse.
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Yes, corrosion protectivity of coatings/resistance of protected nuclear fuel rods against hot steam corrosion are our performance parameters. On ZIRLO nuclear fuel rods surface even before the hot steam treatment is 1-2 microns thick ZrO2 layer. Diamond layer we are working with is 500 nm thick so, in fact on both samples surfaces there are dielectric layers but the el. conductivity of diamond surface is lower. According to your estimation could be worse adhesion/quality of Cr coating on diamond surface caused by the different bare ZIRLO/diamond coated ZIRLO conductivities?
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There are some AFM raw data and analyzed images of some sputtered thin films.
Now it is required to find the grain size.
What will be the accurate method to measure the grain size?
Thanks in advance.
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One aspect to bear in mind is that the finite size of the AFM tip can matter if your grains are relatively small. That is, in the measured images the grains will appear wider than they actually are if the radius of the tip apex is similar to the grain diameter, or even bigger. In the opposite case of a tip radius much smaller than the grain diameter (eg, 5nm tip radius vs 150nm grain size), this dilation effect should be negligible. To get an idea of the tip size, you might like to image nanoparticles with a narrow and well-known size distribution. To check for potential tip wear, such reference measurements could be run before and after the actual imaging of the grains. Good luck!
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Actually, I am using Aluminium as my substrate and coating Copper using Magnetron Sputtering. But once sputtered Copper will not adhere it permanently. How to make it permanent, as I need to make connections on it through soldering? Also, the copper layer can be pulled off by normal transparent adhesive tape or by other tapes too.
This creates problem and copper removed from the aluminium substrate. Can anyone suggest me the solution to this problem, I want to use copper as an electrode over which piezo material to be coated with another copper layer with same aluminium substrate!
Sorry if my question confuses you but I need to form following layers over one another:
Aluminium-Copper-ZnO-Copper
Please suggest a solution to this problem!
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I also agree with Andrey V. Blednov. The oxide layer might be the issue. There are two ways to overcome this. First you can reverse bias the magnetron and substrate so that ions will bombard with the substrate surface and the oxide layer can be removed significantly. Second one is depositing some aluminium alloy which consist copper content (Al 3000 series) in it prior to copper deposition. Chromium also good choice but aluminium alloy is cost effective. Note one thing that, Al alloys consist other elements also like Cr and Ti etc.
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Dear all,
I have a question about the operation of an RF Ion source with 3 Molybdenum grids used as sputter source In DIBS (dual ion beam sputtering) system. During the deposition of metals and especially Platinum, the Ion beam current decrease. To compensate this, the software of the DIBS system has to increases the generator power until saturation at 1000W. After saturation, the current continue to decrease along the process. Moreover, this effect is irreversible. Indeed, for a second process the source is already saturated from the beginning. I think that this problem come from the into the sputter source.
I tried to:
- Increase the flow of Ar --> it help but not as required.
- Decrease the process ion beam current --> power saturation occurs after more time.
Many thanks in advance for your assistance
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Typically RF sources are not recommended for metal processes. The plasma is formed by the RF coil around a quartz chamber, and when that quartz chamber gets coated with metal, it blocks the RF signal from reaching the plasma. Increasing the power allows it to penetrate the metal, but you've already reached the limit of your power supply.
This effect is technically reversible; you just need to pull out the quartz chamber and remove the metal from it. This can be done by etching (liquid or ion), or with mechanical means. For cleaning our in-house sources, we use a sand blaster with fine grit media and only turn the pressure up high enough to remove the coating. If you're too aggressive, you can shatter the quartz chamber, and then it must be replaced. (if you want advice on this, contact me: rice at ionsources.com and I can try to help)
Are you sputtering oxides in addition to your metals? Are you using oxygen as a process gas? If not, you might consider switching to a DC-type source, which has a metal chamber that doesn't mind being coated in metals. Oxygen and oxides will reduce the filament lifetime, and you'll end up trying to remove glass from metal instead of the other way around. However, if you're sputtering both metals and oxides, I think the RF is the right type of source for that.
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I have an old 5cm Ion Tech hollow cathode ion source that is installed in a sputter system. The goal is to do ion beam assisted deposition. However the source I inherited comes with everything except the manual. I've been in contact with their company which is now "Veeco" however I have had no luck. I have several of their filament sources and manuals but I'm in the dark on this one. All I have is a schematic of the gun and neutralizer. Any help is greatly appreciated.
Thanks!
-SM
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Stephen McCoy Did you ever get help with this? Was your question about installation, operation, or maintenance?
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Hello!
I'm ph.d student in Seoul Nat' University.
Our group is right after bought 2-gun RF magentron sputter for deposition IGZO thin film with another ZnO(or AlO) target.
We are mainly using IGZO target, however, after several depostions, we found out that our rarely-using target (ZnO) is contaminated by IGZO.
Is there any way to prevent this contamination?
We are now considering to place partition to isolate each target (plate type or cylinder type)
Which method would be better?
Our sputter gun equipped the gun top side and sample holder bottom side.
IGZO target (contaminate) ZnO target
/ → \
------ (sample holder)
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The cross contamination is a problem. According to your photo, the shutters seem to be very small and will not provide 100% shielding. Putting a plate can decrease the cross contamination but will also affect the plasma. You must ask a question - do I need both targets? Because if the answer is not, you can cover target on the second cathode by aluminum foil until you will need it. If the answer is yes, you should clean both targets prior the experiment by sputtering into the shutters or into the empty chamber/substrate holder.
Good luck.
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I am trying to do 2 probe measyrement using 4 probe system. I am applying to the force terminal to the outermost probe tips. Each tip is separated by 0.5 mm. I tries with lateral configuration device where I am using ruthenium as a contact. I am observing evertime same kind of plot having two different voltage for zero current. Also plot is same when i am removing tips from sample but with less current vales. The inner tips are also touching the sample but connected with anything.
I can't understand if its sample problem or instrument problem. Please give me your suggestion about.
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welcome!
My question is why do you want to disqualify the four probe system to two probe
system.
The 4 prove system is thought to overcome the contact resistance between the metal probes and the semiconductor specimen.
In fact you measure the resistance between the inner probes without having the effect of the contact resistance.
So, my proposal is to pass the current between the outer probe and consider it as a current source feeding the current between the two inner probes.
So, Rin = Vin/Iout
where Rin the resistance between the two inner probes,
Vin is the voltage measured by the two inner probes,
and Iout is the current injected by the two outer probes.
Otherwise you have to connect the inner probes to the voltmeter of the two inner probes and do not set the two inner probes.
or electrically disconnect them.
Best wishes
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I have 2 leak valves (1 for oxygen and other for argon). I want to grow my material with the different ratio of Ar:O2. In every growth, my base pressure is different.
How can I know the exact ratio or how can I control the ratio?
I am not sure with the exact value of final pressure because the gauge doesnt work when plasma is running. I can measure only when the plasme is stopped. Usually with 1 leak valve, I have set the point where I have to stop the rotation of valve. Almost everytime, I get the approx. same value.
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Thomas Breuer
Hello, I am sorry for late response. Right now I am using the concept of partial pressure from Korneli G. Grigorov . I did not get good results but concept seems to be working for me.
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Are there interlayer materials like TaN for copper nano film deposition, so that copper doesn't diffuse into a silicon wafer, are there any such materials for tungsten deposition?
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It looks like Ti/TiN are common to be used as adhesion layer as the adhesion is usually poor between W and dielectrics.
Ref:
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I'm trying to prepare a clean Cu(001) surface for a low-temperature STM experiment. We usually sputter (with Neon ions) and anneal to get the surface clean. However, at the beginning of the cleaning stage, we had an ion gun misalignment that resulted in Mo particles (from the sample holder made of Mo) sputter-coated onto the Copper surface.
Now after fixing the alignment, with repeated cleaning cycles of 1kV ion sputter(5min) and 530C anneal (5-10min), the Cu(001) surface still has many sub-surface defects as well as impurities (as shown in the STM image). The sub-surface defects appear as ripples in the constant-current STM image while other impurities are either tiny depression or protrusion in the image.
I don't know what these can be as we don't have LEED or XPS instruments in our system. But I'm wondering if there's something wrong I did for the cleaning (e.g. wrong temperature /heating time), and if it's ever possible to get rid of these impurities/sub-surface defects through the regular sputtering and annealing cycles.
I'd appreciate any opinions/experience that might be relevant to my problem.
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There is no guarantee where they will diffuse. In the worst case, they disassemble and Mo atoms go deep into the solid. So if your sputter+anneal cycles didn't solve it this far, you probably shouldn't proceed with it.
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I had an idea to directly magnetron sputtering ALN thin films on high resistivity GaN substrates. Two-dimensional electron gas was generated at AlN/GaN interface by magnetron sputtering of ALN thin films. I can't find any literature on this kind of experiment. The difficulty lies in the poor quality of the ALN films deposited by magnetron sputtering, which may be difficult to polarize, and the exposure of the Gan substrate to air before sputtering. (GaN substrate is grown by MOCVD) , how the substrate is treated after air exposure makes the sputtering AlN/GaN interface produce two-dimensional electron gas better.
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I hope this article will help you. 10.3390/ma14040826
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It seems that the aluminum target you are currently using is very contaminated.
Is there any way to restore it back to its original state?
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The above suggestion is the best one. Thank you professor.
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Currently, aluminum is deposited using arc sputtering on PVDF nanofibers.
However, as the deposition progresses, the inside of the chamber and the aluminum target seem to be severely contaminated.
Is it like this originally?
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If your target turns black, you might have CO or CO2 in the chamber. A former colleague of mine once tried to make Aluminium mirrors which came out glossy and black; in the XPS we saw that there was almost as much C as Al in the film (plus a lot of oxygen).
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