====== ATC Sputtering System manual ======= {{ ::atc_and_atc_orion_manual_-_march_2009_-_ce.pdf |Link to the manual}} ====== Description ====== The ATC-1800 sputtering system is feature-rich 4-magnetron system with a large deposition pressure range, 10e-8 mbar range background pressure, substrate heating, substrate RF bias, variable working distance, in-situ gun tilt on all sources, substrate rotation and multi-channel gas blending. The gas inlets are connected to both the chamber and the sources. The system has a loadlock for high throughput and a vacuum chamber that is easily accessible for all non-standard work. ===== DONT's ===== * **Never make a modification** to the system without consulting a technician * **Never transfer a hot sample holder** (cold is, say, 50 °C) * **Never hot-switch the switchbox** (switch off power first!) * **Never exceed 50W RF power for substrate bias** * **Never transfer a sample without checking that BOTH loadlock and chamber are at vacuum (<1e-6 mbar)** * **Never sputter without a sample holder in place** ===== Do's ===== * write the logbook * keep an eye on changing voltage to indicate you sputtered through the target ===== Before you start ===== Check the logbook and reservation system to see if you are interfering with someone else. Fill in your name, date and time in the logbook before you start. ====== USING THE SYSTEM ===== ===== Venting the loadlock and loading the substrates ===== - Wear //powder free// gloves! - **Check if the gate valve between the chamber and the loadlock is closed** before venting the loadlock - Vent loadlock to get the sample holder - Switch off the loadlock pumpgroup - In small steps introduce N₂ in the loadlock - Mount the substrates on the sample holder with silverpaint, leave paint to dry at least 5min - Put the sample holder in the loadlock with the alignment slit towards the right viewport. - Close the loadlock ===== Pumping down the loadlock ===== - Switch on the loadlock pumpgroup - Pump until the pressure in the loadlock is <10^-6 mbar ===== Transfer ===== - Check whether both chamber and loadlock are at vacuum - Open the gate valve - make sure sample stage is completely up - Slide the magnetic drive slowly until the end stop - Rotate the propeller to align it with the slits in the sample holder - Lower the sample stage carefully: be very careful not to bend the transfer arm - Rotate the propeller __clockwise__ manually, **DO NOT USE FORCE** - Pull the sample stage up one cm using the joystick, rotate to see if it's levelled - Raise the sample stage all the way up - Switch on rotation (if rotation speed>40, higher risk of dropping the sample holder during heating) - Slide back the magnetic drive slowly until the end stop - Close the gate valve - Lower sample stage fully (or to desired working distance) ===== Sputtering ===== - Set the substrate temperature to the desired value, let the heater bake until the desired pressure/Temperature is reached - Set the switchbox to the desired gun - Open the gases you need on the touch screen - Set the gasflows - Switch the VAT-valve to pressure mode (typical setpoint is 5mTorr) - close shutters of chamber before sputtering - set the settings on the power supply (to not go over ~500V/100W) - press start on power supply to ignite plasma - Presputter with shutter closed - If RF/bias is needed, switch off the gun, set the pressure to 25 µbar, ignite the bias, set the pressure to the process value, adjust RF matching and restart the gun - Open shutter and start timer - When done, switch off the gun and bias immediately - Switch off the heater and gases (probably you also want to do this immediately) - Open VAT-valve fully - Switch off rotation - When the sample stage has cooled to <50°C, transfer your sample to loadlock ===== Removing the sample ===== - Move sample stage fully up - Open gate valve - Move transfer arm to end stop - lower sample stage and drop sample holder on transfer arm - Put sample stage fully up - move transfer arm to the loadlock - close gate valve - Vent the loadlock as described above in order to remove your samples - **Check whether the sample holder is really cold** - Remove the samples from the sample holder, put sample holder back and pump down the loadlock as described above - Fill out the logbook with all required information. ====== Leaving the system ====== ====== Common problems and tips&tricks ===== * power supply is off: * not all safety interlocks are met (cooling water flow or pressure) * flickering, unstable plasma * optimize process conditions * to thick backing plate * cannot ignite plasma * to thick backing plate * optimize process conditions * faulty power supply * target not conducting ====== Deposition rates ====== Source tilt angle, substrate angle and source-substrate distance are process parameters that should be mentioned here! Current configuration: ^ Material ^ Date ^ Sample ID ^ Process parameters ^ Measured with ^ Result ^ Rate ^ | Fe| 20161222| on Si | 5mTorr, 400mA, 7 min | XRR |41 nm | 5.8nm/min | | Fe| 20161107| MgO/03 | 5mTorr, 200mA | X-ray + profilometer, 20 min, 10 min | 2 thicknesses: 51, 25nm | 2.52 nm/min| |Nd|20161019+20|MgO/021,22|5mTorr, 30mA, 25 & 50 min|XRR tough fit, profilometer|25 & 50 nm approx | 1nm/min| | W | 20161011+12 | MgO/011,012| 5 mTorr, 100mA, 25min, 37.5min | XRR | |1.48nm/min| Older rates ^ Material ^ Date ^ Sample ID ^ Process parameters ^ Measured with ^ Result ^ Rate ^ | Co | 20160111 | Co | 5 mTorr, 200 mA, 22 min | X-ray | 70.6 nm | 3.21/min | | Ag | 20150402 | Ag_cal | 5 mTorr, 100 mA, 5 min | X-ray | 39.0 nm | 7.8 nm/min | | Co | 20150402 | Co_cal | 5 mTorr, 200 mA, 15min | X-ray | 27.5 nm | 1.83 nm/min | | Cu | 20150402 | Cu_cal | 5 mTorr, 100 mA, 10 min | X-ray | 31.1 nm | 3.11 nm/min | | Nb | 20150402 | Nb_cal | 5 mTorr, 300 mA, 10 min | X-ray | 48.0 nm | 4.80 nm/min | | Ag | 20131104 | Ag10min | 5 mTorr, 100 mA, 10 min, 4 mm tilt | X-ray | 82.8 nm | 8.28 nm/min | | Co | 20130911 | Co_cal | 5 mTorr, 100 mA, 15 min | X-ray | 11.48 nm | 0.765 nm/min | | Cr | 20130911 | Cr_cal | 5 mTorr, 100 mA, 15 min | X-ray | 14.79 nm | 0.985 nm/min | | Cu | 20130911 | Cu_cal | 5 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 51.1 nm | 17.03 nm/min | | Cu | 20131104 | Cu3min | 5 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 49.8 nm | 16.6 nm/min | | Nb | 20131104 | Nb3min | 5 mTorr, 300 mA, 3 min, 4 mm tilt | X-ray | 14.8 nm | 4.93 nm/min | | Pd | 20131212 | Pd | 5 mTorr, 100 mA, 4 min, 4 mm tilt | X-ray | ? | 4.92 nm/min | | Py | 20130911 | Py_cal | 5 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 21.9 nm | 7.296 nm/min | | Py | 20130911 | Py_cal_3mT | 3 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 24.9 nm | 8.3 nm/min | | Py | 20131104 | Py3min_holder_a | 3 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 26.3 nm | 8.7 nm/min | | Py | 20131104 | Py3min_holder_b | 3 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 26.2 nm | 8.7 nm/min | | Py | 20131112 | Py1mTorr_holder | 1 mTorr, 350 mA, 3 min, 4 mm tilt | X-ray | 30.4 nm | 10.13 nm/min | | Py | 20131112 | Py2mTorr_holder | 2 mTorr, 350 mA, 3 min, 4 mm tilt | X-ray | 27.3 nm | 9.1 nm/min | | Py | 20131112 | Py4mTorr_holder | 4 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 22.1 nm | 7.4 nm/min | | Py | 20131212 | Py3mTorr_holder | 3 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 28.7 nm | 8.1 nm/min | | Py | 20131212 | Py3mTorr | 3 mTorr, 400 mA, 3 min, 4 mm tilt | X-ray | 26.7 nm | 7.6 nm/min | [[old_rates_atc|Archived rates]] ====== Target Materials ====== The following materials are available * NiFe * Co * Al₂O₃ * Al * Nb * Cr * Py * Cu * Mo * Fe * Ag * Ni * Nd * W ====== Recipes ====== ===== AuFe samples ===== In AuFe run 200511 AuFe current was kept constant at 100mA and Au current was changed to obtain 6, 4, 3 and 1.5% samples. Linear approx. of concentration: Assume for both Au and AuFe 1 nm = n atoms (Fe conc. is low, atoms have similar size), Au rate is r_Au and AuFe rate is r_AuFe. The rates at 100mA have been measured by x-ray, they are r_Au,100 and r_AuFe,100. Au source: r_Au n atoms/min. AuFe source: 0.06 r_AuFe n Fe atoms/min + 0.94 r_AuFe n Au atoms/min Fe/Au = Fe (atoms/min) / Au (atoms/min) = 0.06 r_AuFe n / (0.94 r_AuFe n + r_Au n) AuFe current is kept at 100mA: Fe/Au = 0.06 r_AuFe,100 / (0.94 r_AuFe,100 + r_Au) r_Au = 0.06 r_AuFe,100 (Au/Fe)-0.94r_AuFe,100 I_Au = 100 r_Au / r_Au,100 mA ===== Flat Au films on Mica ===== Substrate Mica, punched into 8 or 2.5 mm disks, freshly cleaved just before loading into ATC. Use a Cu holder for the mica, no adhesives Pressure 20 mTorr setpoint, low -7 background Ar Flow 24 Temperature 300deg C for deposition. Current 200 mA for 20 minutes, then 2 minutes 45 mA Voltage Around 500 / 380 O2 flow 1 Heating/cooling rate Heating: Heat up before deposition to 450 to bake out the dirt from chamber, holder & substrate. Radiative cooldown to 300 for deposition. Anneal for 1-2hrs postdeposition at 300. Cooldown radiative by switching off heat. and RMS roughness (and better roughness data if available) I think a picture says more than 1000 roughness values.. Picture: stm image in air, with a lot of vibrations. Image size 740x640 nm. Shows the typical variation of terrace sizes you find on these samples. Note 1: This recipe has been taken over (mutatis mutandis) from the attached article by kawasaki et al. Some details on the growth mechanism and origin of the triangular facets on the surface can be found in Lussem et aL, applied surface science 249 (2005) 197-202 Note 2: The parameters I used were not systematically optimized. I happened to stumble over something that worked good enough for me almost immediately. The low growth rate (high pressure/low current) of the last step is most probably important. Lower currents could be a thing to try, higher pressure is probably less useful (?). A higher growth rate for the first step might be advantageous, too (lower pressure?). Higher temperature might not be a bad idea, but going over 500 deg C is not advised, since mica starts to decompose at these temperatures. Note 3: Film thickness has up to now not been calibrated. SEM imaging of film grown at room temperature in otherwise same process suggests around 80 nm thickness. {{:wiki:kawasaki-uchiki_sputter-flat-gold-mica_surf.sci.lett_1997.pdf|}} {{:wiki:gold740x630nm.png|}} ===== Cu on Al2O3 ===== Presputter: Cu 5 min 100 mA, 25 sccm Ar, 5 mTorr, 100% rotation, 90 C (on lamp) Sputter: Cu 60 min 400 mA, 25 sccm Ar, 5 mTorr, 100% rotation, 90 C (on lamp) ====== Miscellaneous ====== * The digital log sheet: {{wiki:atc_logbook.doc}} * The new digital log sheet: {{:atc_logbook1.pdf|}} ====== Maintenance ======