NorthStar ALD Operation Manual
Contents
1. E Products being returned to COMPANY must be returned in the condition originally received by the CUSTOMER and free from damage use or modification which would render the product unusable for resale by SVT Associates F All applicable taxes duties insurance and shipping charges shall be the sole responsibility of the CUSTOMER SVT Associates Proprietary Information 2012 SVT Associates Inc All Rights Reserved Page 10 of 11 7620 Executive Drive Eden Prairie MN 55344 3677 USA Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com Version 12 09 26 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 RE G Goods being returned for other than warranty repair shall be subject to a restocking charge of twenty 20 percent of the original sales price of the returned item Returning Equipment for Repair or Servicing Before shipping equipment for repair or servicing obtain a Return Authorization Number assigned by SVT Associates Inc Liability Disclaimer SVT Associates Inc takes steps to assure that its published specifications and manuals are correct however errors do occur SVT Associates Inc reserves the right to correct any such errors and disclaims liability resulting therefrom No Liability for Consequential Damage In no event shall SVT Associates Inc or anyone else involved in the creation production or delivery of the accompanying product includi2. SVT Associates Proprietary Information Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com po dd c ae au dee levee en Version 12 09 26 Page 5 of 11 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 An example of a recipe program SVT Associates Robo File Setup Chamber View LogFile Interlocks u o NEM end Total Recipe Time Time Remaining Total Steps Steps Remaining 107 22 12 00 01 16 02 00 Time Left Set RF Fi ward 176 000 TI pL o e Shutters for 0 300 sec TX X X X Shutters for 30 000 sec X X X Shutters for 25 000 sec X X KK Shutters for 5 000 sec TK KX BE ER Ds He We I ES Set RF Foward 0 000 Table 1 A sample recipe for PEALD Al203 in RoboALD program format TMAI ALD valve for TMAI precursor source 1 SS2 ALD valves for spare precursor sources CG carrier gas on off valve for MFC control P1 Auto stop valve for exhaust and pump 1 S2 spare function controls RF plasma power control RFV On off valve for top sealing Ar gas and reactive gases for RF plasma See RF Plasma source Manual for operation of the RF source Run the Recipe Start the recipe as described in the Robo Control User s Manual Always make certain that the Hot Trap is in operation and at desired temperature before starting a recipe Make certain that all utilities such as exhaust abatement
3. System Shutdown for Extended Period of Time Certain ALD precursors can degrade with repeated heat and cool cycles If precursors must be cooled or are accidentally cooled as a result of a power failure we recommend the precursors remain at room temperature until needed to run process Complete System Shutdown Confirm that the manual precursor isolation valves are closed Close manual gate valve between chamber and loadlock Set all MFC flows to 0 sccm Close Process gas isolation valves Shut off all heaters Lamp heater chamber wall heater manifold heaters exhaust heater hot trap and precursor heaters Close load lock roughing valve Close chamber pumping gate valve Turn off the turbo pump leave the Turbo backing pump run until the turbo stops spinning Turn off the load lock rough pump Power down Eurotherms RF power supply Ozone generator Turn off water Close air supply to system Close Robo program Shut off computer Remove main power to the system Precautions Do not heat the ALD system to temperatures above those recommended by the manufacturer Note the maximum temperature settings for different parts ALD pulse valves are rated to 200 C and should not be heated above that temperature The lamp heater maximum temperature is 500 C while outer chamber wall heaters should not be set gt 150 200 C because of the o ring The precursor delivery lines and exhaust lines should not be heated above 200 C Temperature
4. and cooling water etc are in operation before starting a recipe Upon completion of the recipe turn off the bubbler manual shutoff valves set the growth parameters in the standby mode either manually or by recipe not provided Suggested standby conditions include setting up the substrate temperatures to gt 100 C for overnight running low carrier gas flow constantly Extract the Substrate Reverse the procedure of introducing a sample EE QS LL 7620 Executive Drive Eden Prairie MN 55344 3677 USA SVT Associates Proprietary Information Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com pon sd guae eT Version 12 09 26 Page 6 of 11 Version 12 09 26 Engines for Thin Film Innovation PROPRIETARY INFORMATION C ERE ALD System Safety oafety Interlocks The system has 3 safety interlocks to handle possible emergency situations 1 Growth chamber interlock If the growth chamber has any leaks or the pressure rises above a set level say 5 Torr in the middle of the growth process the controller and the pneumatic throttle valve software can automatically shut down and isolate all ALD valves and MFCs so no precursor vapor or by product can leak into the growth chamber or leak outside if the system is vented 2 Emergency stop button There is a manual stop button In case of an emergency push the emergency stop button All ALD valves MFCs and the pneumatic throttle valve will shut
5. down and the growth chamber is sealed to prevent any possible precursor vapor leaking outside 3 Exhaust for the console There is an exhaust port for the console All precursor bubblers are located in the console In case of precursor bubbler leakage the exhaust can prevent the vapor from leaking outside Make sure both front and back doors of the console are properly closed at all the times to maximize the exhaust flow It is strongly recommended that a gas sensor alarm system working for a specific vapor material be installed near the ALD system For example if you work with chloride such SiCl material an HCl sensor should be installed inside the console or near the growth chamber Precursor Bubbler Handling The source of the precursor chemicals is generically referred to as a bubbler A bubbler passes a carrier gas through a liquid chemical to pick up the chemical Alternatively for high vapor pressure materials it is not necessary to pass the carrier gas through the liquid but simply have a cylinder of the material at a controlled temperature which feeds directly into the ALD valve called direct vapor drawing Know the nature of the precursors with which you are working and read the Material Safety Data Sheet MSDS which is available from the chemical supplier Many ALD precursors are flammable corrosive or toxic For example TMA is pyrophoric it burns upon exposure to air It is thus crucial to handle the precursor bub
6. the chamber The H2O reacts with the surface removing the CH3 groups CH methane is formed as a gaseous byproduct creating Al O Al bridges and passivating the surface with Al OH once again on the surface 4 The unreacted H O and gaseous byproduct CH4 are pumped away with the help of the inert carrier gas These 4 steps of the cycle can be set up in a recipe as a loop Each cycle produces up to 1 1 A 0 11 nm of Al O5 depending on temperature For recipe setup see the SVT Associates Robo Control User s Manual The ALD process is distinct from Chemical Vapor Deposition CVD in that the reactions occur sequentially CVD mode reactions occur when both reacting precursor chemicals arrive on the surface in the ALD chamber at the same time and not sequentially To avoid undesired spurious CVD reactions it is Critical that the purging steps be complete sufficient time and all excess precursor be pumped away before pulsing of the second precursor Only one of the precursors should be exposed to the substrate at a time CVD reactions in the ALD system will produce non uniform and excessive deposits a SVT Associates Proprietary Information 2012 SVT Associates Inc All Rights Reserved Page 3 of 11 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 ERR Depositing a film using ALD NorthStar ALD system may be operated in either the thermal ALD or the plasma enhanced ALD methods There are two modes of operation in
7. the thermal ALD method 1 Regular mode with continuously flowing carrier gas and pulsing precursor chemicals while continuously pumping 2 Soak mode for very high aspect ratio structures Pulsing a precursor with the exhaust valve closed to allow sufficient exposure and saturation of all the surfaces and then opening the valve to pump purge This is then repeated for the other precursor In thermal mode a small internal chamber with lid is preferred Plasma enhanced ALD mode PEALD A remote plasma source is designed to enhance the reactivity of many gas species such as No O2 H2 NH3 etc and lower growth temperatures A reactive gas sometimes balanced with Ar in order to boost plasma efficiency is used PEALD and thermal ALD can be switched easily by removing or putting on an internal lid Key growth parameters include precursor pulse time pulse strength and purge time for each precursor Carrier gas and sealing gas flow rates are also important There are parameter tradeoffs in an ALD process Longer precursor pulse times can assure that the surface to be coated is saturated with the precursor but precursor consumption will go up and cycle time is prolonged Higher carrier gas flow rates help purge the excess precursor faster but may increase base pressure in the chamber thus reducing precursor pulse strength In the NorthStar ALD system there is an internal deposition chamber within the vacuum chamber A flow of inert gas from th
8. 2 months from the date of shipment from SVT Associates manufacturing facility This warranty is subject to SVT Associates equipment being installed maintained and operated in accordance with the operating and maintenance instructions accompanying each item manufactured by SVT Associates Warranty shall be void if SVT Associates equipment is modified by the CUSTOMER or used in other than the recommended manner or applications Purchased equipment incorporated into any item supplied by SVT Associates will be covered by said manufacturer s warranty SVT Associates warrants that at the time of delivery any other products processed or manufactured and sold by it hereunder are free of defects in material and workmanship and conform to COMPANY specifications No warranty is provided by SVT Associates for products sold hereunder which are not manufactured or processed by SVT Associates but the manufacturer s warranty for such products if any shall be assigned to the CUSTOMER without recourse to SVT Associates The foregoing warranties are in lieu of and exclude all other warranties not expressly set forth herein whether expressed or implied by law or otherwise including without limitation any warranty of merchantability or fitness for a particular purpose In no event will SVT Associates be liable for any consequential damages IN THE EVENT OF SVT ASSOCIATES LIABLITY WHETHER BASED ON CONTRACT TORT INCLUDING BUT NOT LIMITED TO NEGLIGENCE AND STRICT LIAB
9. LITY OR OTHERWISE THE CUSTOMER S SOLE AND EXCLUSIVE REMEDY WILL BE LIMITED SVT ASSOCIATES HAS THE FOLLOWING OPTIONS TO REPAIR OR REPLACEMENT F O B SVT ASSOCIATES MANUFACTURING PLANT BY THE COMPANY OF ANY NON CONFORMING ITEM FOR WHICH CLAIM IS MADE BY THE CUSTOMER OR TO REPAYMENT OF THE PORTION OF THE PURCHASE PRICE PAID BY THE CUSTOMER ATTRIBUTABLE TO THE NON CONFORMING ITEM SVT ASSOCIATES WILL NOT BE LIABLE FOR ANY OTHER DAMAGES WHETHER DIRECT INCIDENTAL CONSEQUENTIAL OR OTHERWISE Return Policy Any request by the CUSTOMER for return of standard products other than for warranty claims under warranty hereof for all or any part of purchase order accepted by SVT Associates shall be subject to the following conditions A Notification must be made to SVT Associates by the CUSTOMER within thirty 30 days of original shipping date B A RETURN GOODS AUTHORIZATION number must be assigned to and accompany all goods or materials being returned by the CUSTOMER to SVT Associates Said number must be assigned by SVT Associates prior to any and all returns Goods not accompanied by a RETURN GOODS AUTHORIZATION number will be refused by SVT Associates and returned at the CUSTOMER S expense C CUSTOMER shall prepay shipping charges for products being returned to SVT Associates D Products being returned to SVT Associates should be properly crated for shipment and the CUSTOMER shall bear the risk of loss until delivered to SVT Associates
10. Procedure sssssssssssssesssesssese nennen nne nne nne nne sre sse sie sia sierra rase rase nnns 8 ALD System Shutdown for Extended Period of Time cccccccccceseecceeeceeeeeeese esse cess eeseeeseeeseeeseesaeeegeees 9 Complete System SDUldOWl ue necp itera tinere utate siq usus etui ek nada dedu xiu deme cdita dutiaiuuie crt gun vul ics etel 9 OC ACCOUNTS e r 9 acis i o cE 9 Warranty and Limitations of Remedies ssssssssssssssesseesseee nennen nennen nnne nennen sanas n anne rase nn nean 10 aciem ago e rH 10 Returning Equipment for Repair or Servicing ssesssssessssssssssseseeeennen nennen nennen sensn 11 7620 Executive Drive Eden Prairie MN 55344 3677 USA SVT Associates Proprietary Information Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com o du M p tl Version 12 09 26 iis 7620 Executive Drive Eden Prairie MN 55344 3677 USA Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com Version 12 09 26 Engines for Thin Film Innovation PROPRIETARY INFORMATION C ERR ALD System Operation Read all of the manuals including the Safety sections prior to operating the system ALD Operation Principle Atomic Layer Deposition ALD is a vapor phase technique that depos
11. S V I PROPRIETARY INFORMATION Engines for Thin Film Innovation SVT Associates Inc THIS DOCUMENT CONTAINS PROPRIETARY INFORMATION OF SVT ASSOCIATES INC AND SHALL NOT BE USED DISCLOSED OR REPRODUCED IN WHOLE OR IN PART WITHOUT THE PRIOR WRITTEN CONSENT OF SVT ASSOCIATES INC ee 7620 Executive Drive Eden Prairie MN 55344 3677 USA SVT Associates Proprietary Information Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com Scere taper bene A Aus Page 1 of 11 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 RR Table of Contents ALD Y ogg 0 92 10 9 ene ete ee meee ee mmt 3 ALD Op raton PrNCIDIE resosi e E E EEEE ATRE AE TERE EERE EEEE EE EE pe SHE uS 3 W JereiieleE ail ein oEz ND E E E E ER 4 ee ELO EEES E EE T E E EAA AEE A NES 4 Establish Good Vacuum and Temperature Stability cece ccccceeceeeeeeeeeeeeee esse eeseeeseeeeeeesaeeseeeeeeeees 5 OOLUD SG a 212 oe ne DH RERO a E E I PURI NR ee T eee ere 5 RUN UNG FR CCID Ciao 6 EXACTING UDS gt eee er ec ene een eee enn E ee ene EM MN IUE eee ere 6 ALD System MN NIRE Et 7 sis IOOC EMEN m 7 Precursor BUDDIeF Handling s sess e na EAE E iaar T Pe UIC UDA UD DIG E E E E E E E 8 Mechanical Pump Safety Maintenance essssssssssssssssseeeeene nennen nnns nnne nne rsen sensa rna rns nnns 8 Emergency Shutdown
12. blers safely which includes knowing how to connect and disconnect a bubbler to the ALD valve and how to store a bubbler if it is not in use When connecting a filled bubbler to an ALD valve make sure to wear a proper mask or respirator clear the ALD area of irrelevant personnel double check to make sure the manual on off valve on the bubbler is closed tightly before loosening the VCR fitting Loosen the VCR sealing cap in a chemical hood with proper vent system Ideally there should be a gas sensor around to check if there is a possible leakage from the bubbler Immediately transfer the bubbler to the ALD console and connect to the ALD fitting and tighten it Make sure the line between ALD valve and the bubbler is purged by opening the ALD valve for a short period of time before you open the manual on off switch assuming the system is under vacuum If the base pressure is not recovered and is higher than the original point there could be leakage from the bubbler connecting area When disconnecting a filled bubbler from an ALD valve make sure to wear proper mask or respirator clear the ALD area of irrelevant personnel double check to make sure the manual on off valve on the bubbler is closed tightly before loosening the VCR fitting purge the line between ALD valve and the bubbler to remove any residual precursor in the line loosen the connecting fitting and cap the bubbler immediately with a VCR cap and gasket ee 7620 Executive Drive E
13. den Prairie MN 55344 3677 USA Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com SVT Associates Proprietary Information 2012 SVT Associates Inc All Rights Reserved Page 7 of 11 7620 Executive Drive Eden Prairie MN 55344 3677 USA Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com Version 12 09 26 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 o ERERRRE When a filled precursor bubbler is taken out of use it is the best to put it back in the original package and store in a safe properly vented area or chemical hood area Make sure the on off valve is tightly sealed and the VCR cap is tightened Heating up a Bubbler Depending on precursor volatility a bubbler sometime has to be heated to certain temperatures to get sufficient vapor pressure 1 Torr for example Hf precursors of TDMAH TEMAH and TDEAH Please pay attention to the key properties such as working temperature decomposition temperatures and maximal ALD growth temperature of the precursor used This information may be found in the literature Make sure the thermocouple of a bubbler heater has good thermal contact with the bubbler and has good measurement stability and accuracy so that the temperature readings are real ensure the working temperature never goes beyond the decomposition temperature in addition when heated it is recommended that you keep the precursor constantly at th
14. e Eden Prairie MN 55344 3677 USA SVT Associates Proprietary Information Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com ro duce at a dee eee en Version 12 09 26 Page 4 of 11 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 The use of the optional Load Lock Introduction system allows exchange of substrates while keeping the growth chamber in vacuum minimizing exposure to moisture and other contaminants Establish Good Vacuum and Temperature Stability Turn the lamp heaters on using the Robo control system It may take 30 minutes for temperatures to stabilize Set up a Recipe See Robo Control User s Manual Creating Recipes The following are two examples of Al20 deposition recipes in both thermal and plasma enhanced modes for your reference Internal lid or insert on for thermal mode the lid or insert removed for plasma mode All manifolds including precursor delivery lines and exhaust line should be heated to gt 100 C The outer chamber wall temperature should also be gt 100 C These exposure conditions for Al2O3 coating including pulse time pulse strength pressure and purge time for TMAI and O plasma are experimentally determined and meet saturation conditions You may use them as a reference Some adjustments of the recipe parameters are necessary depending on growth temperatures and individual systems 7620 Executive Drive Eden Prairie MN 55344 3677 USA
15. e top of the chamber into the outer chamber space is used as a sealing gas in the thermal mode to help seal the internal lid and suppress precursor from leaking out of the internal chamber Preparation Make sure the system has been properly outgassed e run the in vacuum heaters at gt 100 C to outgas all internal surfaces e the precursor bubblers should be installed and any headspace between the manual shutoff valves and the ALD valves evacuated Check and make sure the cooling water line o rings for the Growth Chamber and the Plasma Source are sealing Make sure the carrier gas and gases for the Plasma source are ready Power up the system pumps and computer Start the Robo Control software program and turn on the system electronics Prior to any use of chemical precursors the Hot Trap should be on and operating Leave the Hot Trap on during the use of precursors If you are working in the thermal ALD mode the internal lid cover must be in place and properly sealed if you are working in plasma enhanced ALD mode remove the internal lid or insert Introduce the Substrate into the ALD Chamber Vent the deposition chamber to atmosphere and open the outer vacuum chamber lid Internal surface should be kept gt 100 C to suppress moisture adsorption during exposure to atmosphere to avoid injury avoid touching hot surfaces Place the substrate on the pedestal Close the lid and evacuate the system Ao om 7620 Executive Driv
16. e working temperature or slightly below this minimizes the thermal cycling of a precursor to avoid degradation Mechanical Pump Safety Maintenance 1 In principle the ALD process should work in a slightly over saturated exposure condition and almost 100 of the precursors are consumed and very little excessive vapor going into the exhaust and the pump The saturation condition for an ALD system has to be experimentally determined However if precursor vapor pulses are oversaturated too much or too excessively or there is not sufficient purge a severe CVD reaction can happen which generates a lot of powders or particles inside the growth chamber down the exhaust and even into the pump It is thus strongly recommended that you use recipes approved by SVT Associates or minimize precursor use to avoid exhaust problems This is the fundamental the most important root protection for the pump 2 n practice it is hard to identify exact saturation conditions or it takes many test runs Condensation of excessive precursors particles or other by products could still be built up gradually along the exhaust line or even precursor delivery lines If the exhaust line is heated and there is not any filter or trap installed down the exhaust line most are dumped in the pump A hot trap or filter is needed which becomes the secondary defense line A hot trap is capable of decomposing or neutralizing excessive metal organic precursor vapor into less volatile pr
17. its thin films sequentially atomic layer by layer ALD has been described in the literature It is based on sequential reactions of vapor phase chemicals with the surface of the substrate The reactions are self limiting The surface is first saturated with one chemical precursor and the excess pumped away It is then exposed to a second chemical precursor and the excess is pumped away The technique provides excellent coverage of topographical features Relative to other techniques in its standard mode the deposition rate is slow For more information on ALD see review articles in the literature such as Atomic Layer Deposition An Overview by Steven M George Chem Rev 2010 110 111 131 As an example of a thermal ALD process AlzO3 can be deposited using precursors of trimethylaluminum TMA and water Alternative recipes and recipes for other materials can be found in the literature The substrate is introduced into the deposition chamber which is evacuated The surface of the substrate is hydroxylated from exposure to the atmosphere One cycle of the deposition sequence can be described as following two half reaction cycles 1 TMA pulse is admitted into the chamber and allowed to react with hydroxyl groups on the surface This reaction proceeds until the surface reaction reaches completion 2 he unreacted TMA is pumped away with the help of an inert carrier gas such as Nitrogen or Argon 3 A water pulse H2O is admitted into
18. ng hardware and software be liable for any damages whatsoever including without limitation damages for loss of business profits business interruption loss of business information or other pecuniary loss arising out of the use of or the results of use of or inability to use such product even if SVT Associates Inc has been advised of the possibility of such damages SVT Associates Proprietary Information 2012 SVT Associates Inc All Rights Reserved Page 11 of 11
19. oducts and hydrocarbon gas which do not harm the pump and reduce hazard 3 A chemical corrosive resistant pump use of Fomblin oil are recommended Fomblin is ideal but expensive However it is a trade off of the oil price and pump repair cost If ordinary mechanical oil is used frequent replacement is necessary once a month or even more frequent if in heavy use or very aggressive chemicals are used Some other types of pump oil which are resistant to O H20 and metal organics such as AJ Elite Z synthetic vacuum pump fluid from A amp J vacuum can last longer than the ordinary one Emergency Shutdown Procedure In an emergency situation such as system malfunction power shut down system vent failure e Stop the program if you are in the middle of the growth e Manually shut down shutoff valves of all bubblers in use e When the RF plasma unit is on turn off zero all MFCs and switch off all master pneumatic valves to prevent any gas in and shut down the gas cylinder e Shut down the lamp heater manifold heater exhaust heater and chamber wall heater e Close the automatic throttle valve to isolate from the pump and shut down the pump itself manually e Identify the reason of the failure or malfunction and correct it before restarting the system ZA M SVT Associates Proprietary Information 2012 SVT Associates Inc All Rights Reserved Page 8 of 11 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 a ALD
20. of the precursors should not exceed safety or decomposition temperature of the chemical used The maximum temperature for the precursor heater jacket is 200 C Chamber Cleaning After many depositions are performed in the ALD system deposits build up on the internal surfaces Depending on the materials deposited thermal cycling of the system can eventually cause cracking and flaking of the deposit If flakes are visible clean the chamber with a lint free cloth using the appropriate solvents On systems that are equipped with the plasma source an Oxygen plasma can be used to clean by combustion excessive organic deposits in the chamber Similarly a Hydrogen plasma can be used to prepare an ALD chamber for nitride deposition to Suppress oxygen inclusion into the film ee 7620 Executive Drive Eden Prairie MN 55344 3677 USA SVT Associates Proprietary Information Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com po a eee eee at a ee ee een Version 12 09 26 Page 9 of 11 7620 Executive Drive Eden Prairie MN 55344 3677 USA Phone 952 934 2100 Fax 952 934 2737 Email sales svta com www svta com Version 12 09 26 Engines for Thin Film Innovation PROPRIETARY INFORMATION 8 a Warranty and Limitations of Remedies SVT Associates warrants that all equipment manufactured by it shall be free from defects in materials and workmanship under normal use and service for a period of twelve 1
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