<div dir="ltr"><div>I generally avoid hitting the whole list with a response, but spacers have been so wildly successful at UC Berkeley that I feel obligated to express good confidence in the method:</div><div><br></div>The primary difficulty with most of the materials discussed in this thread is that most 2.2cc crucibles have thin walls and do not take to thermal shock very well. The crucible liner itself has low mass and often a low thermal mass (Specific heat * mass). A molten metal drastically increases the thermal mass of the liner wherever it has good contact. If you miss with your e-beam you can easily hit the crucible liner wall directly, and doing so will create a hot spot. Generating a hot spot while having your crucible cooled on all sides will cause massive thermal gradients across the crucible wherever you do *not* have conformal contact of metal inside the crucible. If you have a cup-shaped crucible with a 300C+ thermal gradient across a 1cm space, it's going to shatter from internal stress in most ceramic materials. Often, it will shatter with enough force to eject pieces from the pocket. That includes graphite, Al2O3, or most other materials. Copper liners won't do that but they introduce other alloying problems that can be a pain to deal with.<br><br>We use spacers in all of our evaporators at the UC Berkeley NanoLab. Spacing your ceramic liner off the floor of your hearth or pocket allows you to use smaller beam currents to get the same temperature (effectively, evaporation dep rate). Removing the sidewall of the liner from cooling contact ensures that the cooling contact to the liner is always on a surface in good contact with molten thermal mass during operation, because liquid metal pools at the bottom of the liner. <b>That outright prevents almost all forms of cracking.</b> We routinely do nickel, titanium, aluminum, iron, and many more in FABMATE coated graphite. (Fabmate is a silicon coating that just keeps the graphite dust down dramatically). Anything FABMATE can't handle (e.g., Silver, Gold due to various material incompatibilities and "Wierd stuff" that can happen.) Tungsten usually can, especially if you coat it in ZrO2. We've got a very healthy evaporation usage in the lab, and I haven't had a graphite crucible shatter since 2014 when we implemented spacers.<br><div><br>One last note - 2.2 cc tools are incredibly sensitive to beam focus. (Deformed e-beams can overheat the top edge of your liner and shatter it) Almost all research labs will tolerate a level of buildup on your focus pole pieces that is unhealthy for a 2.2cc e-beam tool. Removing and cleaning those pieces every couple months helps a ton. Also making sure that there's no dust that worked its way under the pole pieces and air-gapping your magnetic fields.</div><div><br></div><div>Hope this helps.</div><div><br></div><div>-Ryan</div></div><br><div class="gmail_quote gmail_quote_container"><div dir="ltr" class="gmail_attr">On Fri, Dec 13, 2024 at 1:13 PM Martin, Michael <<a href="mailto:michael.martin@louisville.edu">michael.martin@louisville.edu</a>> wrote:<br></div><blockquote class="gmail_quote" style="margin:0px 0px 0px 0.8ex;border-left:1px solid rgb(204,204,204);padding-left:1ex"><div class="msg-1412536831603883057">
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LOL, TY for that info Michael. I guess that will be our new M.O. for aluminum then. </div>
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<b>Sent:</b> Thursday, December 12, 2024 8:28 PM<br>
<b>To:</b> <a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a> <<a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a>><br>
<b>Subject:</b> Re: [labnetwork] [Non-DoD Source] Re: question about Liner for Ni Ebeam Evaporation</font>
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For whatever reason, Aluminum doesn't wet copper when molten in the hearth. Evaporation temperature is above Cu melting point, but still that's what I see. There may still be some Cu diffusion - but I saw no damage to hearth after a few depositions (disclaimer
- I am not a fan of direct loading)</div>
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Also, I tried real hard - although nonintentionally and fortunately unsuccessfully! - to burn a hole in a copper hearth. It's much harder than you think, I could only put a small dent in there. That is a
<i>huge</i> chunk of highly heat conductive copper that is water-cooled from the back. Makes me really wonder if there is actually liquid Al(or Ni) in contact with the copper at any point in the process, or liquid from above comes into contact with Cu and crystallizes
right there. Certainly direct load would require higher beam power because of those things, with all associated effects like more outgassing and sample heating.</div>
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On a separate note, there was a similar discussion about Al a year or two ago. The best idea I saw is exactly opposite to direct load - it was about using graphite spacer under Fabmate crucible to prevent heat contact of crucible walls and Cu hearth. Intermetallic
crucibles are a second option. </div>
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Makes me wonder if spacer is worth trying with Ni.</div>
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Just my $0.02</div>
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Mike</div>
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_______________________________________________</div>
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<p style="margin:0px;font-family:Calibri,sans-serif;font-size:11pt"><span style="color:black">Michael Yakimov</span></p>
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<div id="m_-1412536831603883057x_divRplyFwdMsg" dir="ltr"><font face="Calibri, sans-serif" color="#000000" style="font-size:11pt"><b>From:</b> labnetwork <<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank">labnetwork-bounces@mtl.mit.edu</a>> on behalf of Martin, Michael <<a href="mailto:michael.martin@louisville.edu" target="_blank">michael.martin@louisville.edu</a>><br>
<b>Sent:</b> Thursday, December 12, 2024 12:41 PM<br>
<b>To:</b> EDWARDS, JASON R CTR USAF AFMC AFRL/RYDD <<a href="mailto:jason.edwards.30.ctr@us.af.mil" target="_blank">jason.edwards.30.ctr@us.af.mil</a>>; Beaudoin, Mario <<a href="mailto:beaudoin@physics.ubc.ca" target="_blank">beaudoin@physics.ubc.ca</a>>; Graham Gibson <<a href="mailto:gibsong@queensu.ca" target="_blank">gibsong@queensu.ca</a>>; Owain Clark <<a href="mailto:odc1n08@soton.ac.uk" target="_blank">odc1n08@soton.ac.uk</a>>; shokoofe haghighi <<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank">shokoofe_haghighi@yahoo.com</a>>; <a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a>
<<a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a>><br>
<b>Subject:</b> Re: [labnetwork] [Non-DoD Source] Re: question about Liner for Ni Ebeam Evaporation</font>
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Personally, I'm terrified that without a liner we will punch a hole in the pocket. This would be catastrophic since then coolant would spray into the chamber just a couple of cm away from both high voltage and high current electrodes.</div>
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Jason (and others who go liner-less), wouldn't you be concerned about alloying the target material to the copper liner, I guess not? We have issues similar to Ni with aluminum. Almost every liner material seems incompatible with Al in one way or another yet
ebeam Al can be very low stress. BTW, I believe lesker suggests to use thermal evaporation for Al. However, if you just put the Al in the pocket without a liner I would expect a copper-aluminum alloy to form. Didn't Al-ebeam come up not so long ago in this
group with several mentioning they put the material directly in the pocket? </div>
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<div id="m_-1412536831603883057x_x_divRplyFwdMsg" dir="ltr"><font face="Calibri, sans-serif" color="#000000" style="font-size:11pt"><b>From:</b> labnetwork <<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank">labnetwork-bounces@mtl.mit.edu</a>> on behalf of EDWARDS, JASON R CTR USAF AFMC AFRL/RYDD <<a href="mailto:jason.edwards.30.ctr@us.af.mil" target="_blank">jason.edwards.30.ctr@us.af.mil</a>><br>
<b>Sent:</b> Thursday, December 12, 2024 6:57 AM<br>
<b>To:</b> Beaudoin, Mario <<a href="mailto:beaudoin@physics.ubc.ca" target="_blank">beaudoin@physics.ubc.ca</a>>; Graham Gibson <<a href="mailto:gibsong@queensu.ca" target="_blank">gibsong@queensu.ca</a>>; Owain Clark <<a href="mailto:odc1n08@soton.ac.uk" target="_blank">odc1n08@soton.ac.uk</a>>; shokoofe haghighi <<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank">shokoofe_haghighi@yahoo.com</a>>; <a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a> <<a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a>><br>
<b>Subject:</b> Re: [labnetwork] [Non-DoD Source] Re: question about Liner for Ni Ebeam Evaporation</font>
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<p><span style="font-size:11pt">We evaporate straight out of the pocket for most of our metals, it’s interesting to hear that this may not be standard procedure for most labs. Not to draw attention away from the original question in
this thread but I would like to hear more about what benefits you are getting from using liners. Is it just for ease of swapping metals in the pockets? In the instance of a Cu liner for Ni are you able to make a proper melt slug with the Ni considering you
are unable to get the beam too close to the Cu liner? Thanks in advance.</span></p>
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<p><b><span style="font-family:"Century Gothic",sans-serif;color:rgb(0,73,135)">Jason Edwards</span></b><span style="font-size:11pt"></span></p>
<p><span style="font-size:8pt;font-family:"Century Gothic",sans-serif;color:rgb(84,87,97)">KBR | Clean Room Facilities Manager , Defense Systems Engineering</span></p>
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<p><b><span style="font-size:11pt;font-family:Calibri,sans-serif">From:</span></b><span style="font-size:11pt;font-family:Calibri,sans-serif"> labnetwork <<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank">labnetwork-bounces@mtl.mit.edu</a>>
<b>On Behalf Of </b>Beaudoin, Mario<br>
<b>Sent:</b> Wednesday, December 11, 2024 5:07 PM<br>
<b>To:</b> Graham Gibson <<a href="mailto:gibsong@queensu.ca" target="_blank">gibsong@queensu.ca</a>>; Owain Clark <<a href="mailto:odc1n08@soton.ac.uk" target="_blank">odc1n08@soton.ac.uk</a>>; shokoofe haghighi <<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank">shokoofe_haghighi@yahoo.com</a>>; <a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a><br>
<b>Subject:</b> [Non-DoD Source] Re: [labnetwork] question about Liner for Ni Ebeam Evaporation</span></p>
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<p> </p>
<p>We use a Cu crucible (4.4cc in a 7cc pocket) with good results.<span style="font-size:12pt"></span></p>
<p>Mario</p>
<p> </p>
<div>
<p>On 2024-12-11 9:11 a.m., Graham Gibson wrote:</p>
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<p><span style="font-size:9pt;font-family:Arial,sans-serif;color:black;background:rgb(255,236,179)">[<strong><span style="font-family:Arial,sans-serif">CAUTION:</span></strong> Non-UBC Email]</span><span style="font-size:12pt"></span></p>
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<p><span style="font-size:11pt"> It’s interesting to see such a wide variety of experiences. I’m too chicken to evaporate right out of the pocket, so we went through a lot of liners, too, before settling on something.
</span></p>
<p><span style="font-size:11pt"> </span></p>
<p><span style="font-size:11pt"> We have had good luck with Cu liners for Ni e-beam evaporation, but with a 2.2 cc pocket, we have to be very careful to keep the beam away from the walls and limit the deposition rate to 1 Angstrom/s.</span></p>
<p><span style="font-size:11pt"> </span></p>
<p><span style="font-size:11pt"> Hope you find something that works, liners get expensive!</span></p>
<p><span style="font-size:11pt"> </span></p>
<p><span style="font-size:11pt"> </span></p>
<p><span style="font-size:11pt">Graham Gibson</span></p>
<p><span style="font-size:11pt"> </span></p>
<p><span style="font-size:9pt">Operations Manager, NanoFabrication Kingston</span></p>
<p><span style="font-size:9pt">Queen’s University</span></p>
<p><span style="font-size:9pt">945 Princess Street</span></p>
<p><span style="font-size:9pt">Kingston, Ontario, Canada</span></p>
<p><span style="font-size:9pt">K7L 0E9</span></p>
<p><span style="font-size:9pt"><a href="mailto:gibsong@queensu.ca" target="_blank"><span style="color:rgb(5,99,193)">gibsong@queensu.ca</span></a></span></p>
<p><span style="font-size:9pt"><a href="http://www.nanofabkingston.ca/" target="_blank"><span style="color:rgb(5,99,193)">www.nanofabkingston.ca</span></a></span></p>
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<p><b><span style="font-size:11pt;font-family:Calibri,sans-serif">From:</span></b><span style="font-size:11pt;font-family:Calibri,sans-serif"> labnetwork
<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank"><labnetwork-bounces@mtl.mit.edu></a>
<b>On Behalf Of </b>Owain Clark<br>
<b>Sent:</b> December 5, 2024 3:48 AM<br>
<b>To:</b> Jeff Salzmann <a href="mailto:jks7@buffalo.edu" target="_blank"><jks7@buffalo.edu></a>; Bernhard Reineke
<a href="mailto:bernhard.reineke@uni-paderborn.de" target="_blank"><bernhard.reineke@uni-paderborn.de></a>; shokoofe haghighi
<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank"><shokoofe_haghighi@yahoo.com></a>; <a href="mailto:labnetwork@mtl.mit.edu" target="_blank">
labnetwork@mtl.mit.edu</a><br>
<b>Subject:</b> Re: [labnetwork] question about Liner for Ni Ebeam Evaporation</span></p>
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<p> </p>
<p><span lang="EN-GB" style="font-size:11pt">Interestingly we have no trouble with Ni, it is one of our most stable materials and the crucible has not been changed in years. I believe it is W.
</span></p>
<p><span lang="EN-GB" style="font-size:11pt"> </span></p>
<p><span lang="EN-GB" style="font-size:11pt">I suspect reading these comments it is because we have larger 40cc crucibles and we only melt a spot in the center with a small beam deflection. The crucible walls never see melted Ni.
</span></p>
<p><span lang="EN-GB" style="font-size:11pt"> </span></p>
<p><span lang="EN-GB" style="font-size:11pt">BR, Owain</span></p>
<p><span lang="EN-GB" style="font-size:11pt"> </span></p>
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<p><b><span style="font-size:11pt;font-family:Calibri,sans-serif">From:</span></b><span style="font-size:11pt;font-family:Calibri,sans-serif"> labnetwork <<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank">labnetwork-bounces@mtl.mit.edu</a>>
<b>On Behalf Of </b>Jeff Salzmann<br>
<b>Sent:</b> 04 December 2024 17:15<br>
<b>To:</b> Bernhard Reineke <<a href="mailto:bernhard.reineke@uni-paderborn.de" target="_blank">bernhard.reineke@uni-paderborn.de</a>>; shokoofe haghighi <<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank">shokoofe_haghighi@yahoo.com</a>>;
<a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a><br>
<b>Subject:</b> Re: [labnetwork] question about Liner for Ni Ebeam Evaporation</span></p>
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<p><span lang="EN-GB"> </span></p>
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<p><span style="font-size:12pt">Haghighi,</span></p>
<p><span style="font-size:12pt"> </span></p>
<p><span style="font-size:12pt">This is my collection of failed crucibles used to evaporate Ni.
</span></p>
<p><span style="font-size:12pt"> </span></p>
<p><span style="font-size:12pt">We decided on graphite, because copper was worse. We limit our deposition rate to 0.2</span><span style="font-size:10.5pt;font-family:Arial,sans-serif;color:black;background:rgb(248,249,250)">
</span><span style="font-size:12pt">Å/sec to help extend the lifespan of the crucibles. They still fail after 2-3 depositions.</span></p>
<p><span style="font-size:12pt"> </span></p>
<p><span style="font-size:12pt">Regards,</span></p>
<p><span style="font-size:12pt">Jeff</span></p>
<p><span style="font-size:12pt"> </span></p>
<p><span style="font-size:12pt"> </span></p>
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<p><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">Jeff Salzmann</span></p>
<p><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">Assistant Professor of Research</span></p>
<p><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">Cleanroom Manager, Shared Instrumentation Laboratories</span></p>
<p><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">School of Engineering and Applied Sciences</span></p>
<p><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">University at Buffalo</span></p>
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<p><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">Tel: 716.645.2584</span></p>
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<p style="margin-bottom:12pt"><b><span style="font-size:12pt;color:black">From:
</span></b><span style="font-size:12pt;color:black">labnetwork <<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank">labnetwork-bounces@mtl.mit.edu</a>> on behalf of Bernhard Reineke <<a href="mailto:bernhard.reineke@uni-paderborn.de" target="_blank">bernhard.reineke@uni-paderborn.de</a>><br>
<b>Date: </b>Wednesday, December 4, 2024 at 11:46<br>
<b>To: </b>shokoofe haghighi <<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank">shokoofe_haghighi@yahoo.com</a>>,
<a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a> <<a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a>><br>
<b>Subject: </b>Re: [labnetwork] question about Liner for Ni Ebeam Evaporation</span></p>
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<p><span style="font-size:12pt">Hi Haghighi,<br>
<br>
we tried this once, same result. All liners will crack. Lesker has some recommendations on Ebeam evaporation of Ni: slow power ramp up and down (works well to prevent cracking for ~2-4 Runs, with fabmate). A Cu liner should work better but we never tested that.<br>
<br>
<a href="https://www.lesker.com/newweb/deposition_materials/depositionmaterials_evaporationmaterials_1.cfm?pgid=ni1" target="_blank">https://www.lesker.com/newweb/deposition_materials/depositionmaterials_evaporationmaterials_1.cfm?pgid=ni1</a><br>
<br>
Best,<br>
<br>
Bernhard </span></p>
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<p><b><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black">Von:</span></b><span style="font-size:11pt;font-family:Calibri,sans-serif;color:black"> labnetwork <<a href="mailto:labnetwork-bounces@mtl.mit.edu" target="_blank">labnetwork-bounces@mtl.mit.edu</a>>
im Auftrag von shokoofe haghighi <<a href="mailto:shokoofe_haghighi@yahoo.com" target="_blank">shokoofe_haghighi@yahoo.com</a>><br>
<b>Gesendet:</b> Mittwoch, 4. Dezember 2024 10:35:19<br>
<b>An:</b> <a href="mailto:labnetwork@mtl.mit.edu" target="_blank">labnetwork@mtl.mit.edu</a><br>
<b>Betreff:</b> [labnetwork] question about Liner for Ni Ebeam Evaporation</span><span style="font-size:12pt">
</span></p>
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<p><span style="font-size:12pt"> </span></p>
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<p><span style="font-family:"Helvetica Neue"">Hi, hope you are having good days, </span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue"">this is Haghighi, working on metallization by a PVD, using thermal and Ebeam evaporation. </span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue"">I have some issues choosing the right liner for Ni Ebeam evaporating, hope you find time to guide me through it. </span></p>
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<p><span style="font-family:"Helvetica Neue"">We have tested graphite, glassy carbon coated graphite, Al2O3, Mo, W and Cu liners so far. </span></p>
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<p><span style="font-family:"Helvetica Neue""> Graphite liner just broke after first run from the border line of Ni surface. <span style="color:black">Glassy carbon coated graphite was more or less the same,</span></span></p>
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<p><span style="font-family:"Helvetica Neue""> Al2O3 endured for 4-5 runs before breaking but there were cracks on it, </span></p>
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<p><span style="font-family:"Helvetica Neue""> Mo liner totally melted and some kind of alloy was produced,</span></p>
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<p><span style="font-family:"Helvetica Neue""> W and Cu endured but their internal walls were some how melted and we can't be sure about pureness of evaporated Ni and final produced thin films.</span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue"">do you have any other suggestions? </span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue"">high voltage: 6.1 KV</span></p>
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<p><span style="font-family:"Helvetica Neue"">emission current: 3 - 5 A</span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue"">Thanks for your time and attention in advance, I hope you kindly find time and consider replying me, </span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-family:"Helvetica Neue"">Dr. Haghighi</span></p>
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<p><span style="font-family:"Helvetica Neue""> </span></p>
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<p><span style="font-size:12pt"><br>
<br>
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