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Interfacing Oxides

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Process database::

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                  List of all processes             
 [-] Example Growth of nm YIG on substrate   
 [-] Step 1: Substrate cleaning  
  Equipment used: Beaker; ultrasonic cleaner; tube oven
  Substrate/Starting material: substrate
  Temperature: 30 min @ 950°C; ramp up time 2 hr, ramp down 5°C/min
  Time: 15 min
 [-] Extra process parameters:
  rinsing time acetone; ultrasonic power: 10min;100W
  rinsing time isopropanol; ultrasonic power: 10min;100W
 [-] Other chemicals involved:
  Chemical 1: acetone; Role: cleaning solvent
  Chemical 2: isopropanol; Role: cleaning solvent
  Special comments:

two step cleaning by rinsing in solvents, followed by thermal anneal

 [-] Step 2: PLD deposition  
  Equipment used: PLD system
  Target/Source material: YIG
  Atmosphere: O2
  (Partial) Pressures: 0.025 mbar
  Temperature: 650 °C
  Time: 2,5 hr
 [-] Extra process parameters:
  specific deposition parameters: spot fluence 1,5J/cm²; spot size 1,8 mm²; rep rate laser 2Hz
  heatup ramp time: 50min
  cooldown ramp time: 50min
 [-] Other chemicals involved:
  Chemical 1: GGG,monocristalline; Role: substrate
  Chemical 2: YIG, polykristaline; Role: target
 [-] LAO on STO dry etching after lithography      => heterostructure No.: 2 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: substrate preparation   
  Equipment used: beaker
  Substrate/Starting material: LAO on STO substrate
  Atmosphere: air
  (Partial) Pressures: ambient
  Temperature: room temperature
  Time: 10 minutes
 [-] Extra process parameters:
  agitation: slightly move sample while cleaning
 [-] Other chemicals involved:
  Chemical 1: acetone; Role: solvent use for five minutes
  Chemical 2: propanole; Role: solvent use for five minutes
  Special comments:

rinse in deioniesed water for one minute after cleaning is finished;
dry sample with nitrogene brush at moderate pressure and flow;

 [-] Step 2: dry etching   
  Equipment used: ICP RIE
  Substrate/Starting material: LAO on STO substrate
  Atmosphere: plasma gas: BCl3
  (Partial) Pressures: chamber pressure: 6 mTorr
  Temperature: 5 °C
  Time: rate: (16 +/- 5) nm / minute
 [-] Extra process parameters:
  RF power: 230 W
  ICP power: 1,200 W
  helium backside contact: 10 Torr
 [-] Other chemicals involved:
  Chemical 1: deionised water; Role: solvent to remove residual chlorine compounds
  Special comments:

for chamber conditioning apply recipe for 5 minutes without sample;
sample fixed with one drop of fombline onto a 6"-wafer as carrier;
bevore locking out sample, allow to pump at chamber base pressure for 5 minutes;
rinse sample in deionised water for 5 minutes after locking out followed by drying with nitrogen brush;
always use special chamber cleaning procedures afterwards;

 [-] Step 3: resist removal   
  Equipment used: beaker
  Substrate/Starting material: LAO on STO substrate
  Atmosphere: air
  (Partial) Pressures: ambient
 [-] Extra process parameters:
  maceration I: 120 minutes; room temperature
  maceration II: 60 minutes; 60 °C
  ultrasonic agitation: 5 minutes; 60 °C; 100 W
 [-] Other chemicals involved:
  Chemical 1: N-ethyl-pyrrolidon; Role: solvent for maceration and ultrasonic agitation
  Chemical 2: acetone; Role: solvent for final cleaning
  Chemical 3: propanole; Role: solvent for final cleaning
  Chemical 4: deionised water; Role: solvent for final cleaning
  Chemical 5: nitrogene; Role: drying with brush
  Special comments:

according to etch time, maceration needs to be prolongated, e.g.: 2-4 hours per 1 minute exposition;
use oxygene plasma icinerator afterwards if necessary;

 [-] (ZnO/PCMO/LSMO) on (SRO) on (CeO2)/YsZ on Si substrate      => heterostructure No.: 1/4 contact: Eddy Rodijk  
 [-] Step 1: PLD deposition of YsZ on 4'' Si for oxygen scavenging   
  Equipment used: PLD system
  Substrate/Starting material: Si substrate
  Target/Source material: YsZ
  Atmosphere: Argon
  (Partial) Pressures: 0.02mbar
  Temperature: 850C
  Time: 4min
 [-] Extra process parameters:
  Fluence: 2.3J/cm2
  Spotsize: 2.5mm^2
  Laser reprate: 10hz
  Target-substrate distance: 55mm
 [-] Step 2: PLD deposition of YsZ on 4'' Si   
  Equipment used: PLD system
  Substrate/Starting material: YsZ/Si substrate
  Atmosphere: Oxygen
  (Partial) Pressures: 0.02mbar
  Temperature: 850C
  Time: 35min (100nm)
 [-] Extra process parameters:
  Fluence: 2.3J/cm2
  Spotsize: 2.5mm2
  Laser reprate: 20hz
  Target-substrate distance: 55mm
 [-] Step 3: PLD deposition of CeO2 on 4'' YsZ/Si   
  Equipment used: PLD system
  Substrate/Starting material: YsZ/Si substrate
  Target/Source material: CeO2
  Atmosphere: Oxygen
  (Partial) Pressures: 0.02mbar
  Temperature: 850C
  Time: 8min (30nm)
 [-] Extra process parameters:
  Fluence: 2.3J/cm2
  Spotsize: 2.5mm2
  Reprate: 10hz
  Target-substrate distance: 55mm
 [-] Step 4: PLD deposition of SRO on 4'' (CeO2)/YsZ/Si   
  Equipment used: PLD
  Substrate/Starting material: (CeO2)/YsZ/Si
  Atmosphere: vacuum
  (Partial) Pressures: base pressure
  Temperature: 850C
  Time: 4min (2nm)
 [-] Extra process parameters:
  Fluence: 2.2J/cm2
  Spotsize: 2.5J/cm^2
  Reprate: 10hz
  Target substrate distance: 55mm
 [-] Step 5: PLD deposition of electrode layer SRO on 4'' (CeO2)/YsZ/Si   
  Equipment used: PLD system
  Substrate/Starting material: (CeO2)YsZ/Si substrate
  Target/Source material: SRO
  Atmosphere: oxygen
  (Partial) Pressures: 0.1mbar
  Temperature: 800
  Time: 35min
 [-] Extra process parameters:
  fluence: 2.5J/cm^2
  spotsize: 2.5mm2
  laser reprate: 20hz
  cooldown: 30C/min
  target-substrate distance: 55mm
 [-] Step 6: PLD deposition of ZnO/LSMO/PCMO on (SRO) on 4'' (CeO2)/YsZ/Si   
  Equipment used: PLD system
  Substrate/Starting material: (CeO2)/YsZ/Si
  Target/Source material: LSMO
  Atmosphere: Oxygen
  (Partial) Pressures: 0.1mbar
  Temperature: 800C
  Time: 35min (100nm)
 [-] Extra process parameters:
  Fluence: 2.3J/cm2
  Spotsize: 2.5mm2
  Reprate: 20hz
  Target-substrate distance: 50mm
  Cooldown ramp: 30C/min
 [-] LaAlO3 growth on TiO2 terminated SrTiO3      => heterostructure No.: 2 contact: Prof. Dr. Ing. Guus Rijnders  
 [-] Step 1: SrTiO3 substrate treatment   
  Equipment used: tube oven
  Substrate/Starting material: SrTiO3
  Atmosphere: ambient
  (Partial) Pressures: 1 Bar
  Temperature: 950 C
  Time: 30 min
 [-] Extra process parameters:
  Sr-Hydroxide formation in H2O using beaker (ultrasonic): 30 min
  HF etching of Sr-hydroxide using beaker (Ultrasonic): 30 sec
  rinsing in H2O using beaker (ultrasonic): 3 times
  cleaning in alcohol: 2 times
  Drying with N2 gun: 1 time
 [-] Step 2: 10 uc layers LaAlO3 growth by PLD   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3
  Target/Source material: crystalline LaAlO3
  Atmosphere: O2
  (Partial) Pressures: 2*10-3 mBar
  Temperature: 850 C
  Time: ~ 3min
 [-] Extra process parameters:
  cooldown in dep pressure: 2*10-3 mBar O2
  Laser energy density in spot: 1.3 J/cm2
  Laser repetition rate: 1Hz
 [-] Growth of SrRuO3 on SrTiO3 substrates by PLD      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: PLD of SrRuO3   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3
  Target/Source material: SrRuO3
  Atmosphere: O2
  (Partial) Pressures: 0.1 mbar
  Temperature: 700 C
  Time: 30 minutes
 [-] Extra process parameters:
  Fluence: 1.3 J/cm2
  Repetition rate: 5 Hz
  Target thickness: 50 nm
 [-] [(LMO (2 u.c.)) + (SMO (1 u.c.))]16 - stacks on STO - dry etching after lithography      => heterostructure No.: 6 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: substrate preparation   
  Equipment used: beaker
  Substrate/Starting material: [(LMO (2 u.c.)) + (SMO (1 u.c.))]16 - stacks on STO
  Atmosphere: air
  (Partial) Pressures: ambient
  Temperature: room temperature
  Time: 10 minutes
 [-] Extra process parameters:
  agitation: slightly move sample in each solvent while cleaning
 [-] Other chemicals involved:
  Chemical 1: acetone; Role: solvent use for five minutes
  Chemical 2: propanole; Role: solvent use for five minutes
  Chemical 3: deionised water; Role: final rinsing for one minute
  Special comments:

dry sample with nitrogene brush at moderate pressure and flow;

 [-] Step 2: dry etching   
  Equipment used: ICP RIE
  Substrate/Starting material: [(LMO (2 u.c.)) + (SMO (1 u.c.))]16 - stacks on STO
  Atmosphere: plasma gas: BCl3
  (Partial) Pressures: chamber pressure: 6 mTorr
  Temperature: 5 °C
  Time: rate: (13 +/- 3) nm / minute
 [-] Extra process parameters:
  RF power: 230 W
  ICP power: 1,200 W
  helium backside contact: 10 Torr
 [-] Other chemicals involved:
  Chemical 1: deionised water; Role: solvent to remove residual chlorine compounds
  Special comments:

for chamber conditioning apply recipe for 5 minutes without sample;
sample fixed with one drop of fombline onto a 6"-wafer as carrier;
bevore locking out sample, allow to pump at chamber base pressure for 5 minutes;
rinse sample in deionised water for 5 minutes after locking out followed by drying with nitrogen brush;
always use special chamber cleaning procedures afterwards;

 [-] Step 3: resist removal   
  Equipment used: beaker
  Substrate/Starting material: [(LMO (2 u.c.)) + (SMO (1 u.c.))]16 - stacks on STO
  Atmosphere: air
  (Partial) Pressures: ambient
 [-] Extra process parameters:
  maceration I: 120 minutes; room temperature
  maceration II: 60 minutes; 60 °C
  ultrasonic agitation: 5 minutes; 60 °C; 100 W
 [-] Other chemicals involved:
  Chemical 1: N-ethyl-pyrrolidon; Role: solvent for maceration and ultrasonic agitation
  Chemical 2: acetone; Role: solvent for final cleaning
  Chemical 3: propanole; Role: solvent for final cleaning
  Chemical 4: deionised water; Role: solvent for final cleaning
  Chemical 5: nitrogene; Role: drying with brush
  Special comments:

according to etch time, maceration needs to be prolongated, e.g.: 2-4 hours per 1 minute exposition;
use oxygene plasma icinerator afterwards if necessary;

 [-] YSZ Sputter Deposition on 3      => heterostructure No.: 4 contact: Gerardo Coletta  
 [-] Step 1: Substrate Cleaning   
  Equipment used: beaker
  Substrate/Starting material: Si substrate
  Temperature: <55°C
  Time: 2-10 minutes
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Organic solvent
  Chemical 2: Methanol; Role: Organic solvent
  Chemical 3: H2O2; Role: RCA1 solution component
  Chemical 4: NH4OH; Role: RCA1 solution component
  Chemical 5: Ar; Role: Flushing gas to remove water from sample surfaces
  Special comments:

The cleaning is a multi-steps process which foresees
1) immersion of the material into warm (<55°C) acetone (10')
2) immersion of the material into warm methanol (<55°C - 2-5')
3) rinsing with D-I water and flushing with pressurised filtered Ar
4) immersion of the material into warm (70°C) RCA1 solution (15')
5) rinsing with D-I water and dryin by flushing with pressurised filtered Ar

 [-] Step 2: YSZ sputter deposition on Silicon   
  Equipment used: PVD equipment
  Substrate/Starting material: Si substrate
  Target/Source material: YsZ
  Atmosphere: Ar
  (Partial) Pressures: 0,008
  Temperature: ranging 300 - 500 °C
  Time: ranging 1.5-4 hours
 [-] Extra process parameters:
  flow: 10-17 sccm
  power: 60-100 W
  voltage: 200-300 V
  time: 1.5-4 h
  Special comments:

Material is loaded into the PVD chamber nad located in the sample holder. The chamber is, hence, evacuated, down to a base pressure of 10-6 mbar. Ar is hence inserted into the chamber till an operative pressure in the range of 10-3 mbar. Chamber is heated to the desired process temperature (tested 300 and 500 °C). The PVD process is hence started.

 [-] LaAlO3 deposition on SrTiO3 substrate by Pulsed Laser Deposition (PLD)      => heterostructure No.: 2 contact: Mohsin Z. Minhas  
 [-] Step 1: Cleaning of SrTiO3 substrate   
  Equipment used: Ultrasonic Cleaner
  Substrate/Starting material: SrTiO3
  Atmosphere: Air
  Temperature: Room Temperature
 [-] Extra process parameters:
  Acetone: 10 min in Ultrasonic bath
  Ethanol: 10 min in Ultrasonic bath
  Isoproponal: 10 min in Ultrasonic bath
  dry with nitrogen:
  DI water: 30 min in Ultrasonic bath
  Special comments:

check with microscope if surface are clean!
if not:clean the surface with ethanol wetted lens tissue, repeat the ethanol cleaning step before doing the DI water step.

 [-] Step 2: TiO2 terminated SrTiO3 substrate   
  Equipment used: Beaker
  Substrate/Starting material: SrTiO3
  Temperature: RT
 [-] Extra process parameters:
  etching the substrates with bHF(12.5%): for 30 sec
  Rinsing in DI water: 3 times after the etching
  cleaning with Ethanol: 10 min in Ultrasonic bath
  dry the substrates with nitrogen:
 [-] Step 3: Thermal treatment of STO   
  Equipment used: tube oven
  Atmosphere: O2 flow 150l/h
  Temperature: 950C
  Time: 2h
  Special comments:

After cleaning and etching the thermal treatment was done at 950C in O2 flow.

 [-] Step 4: Deposition of LaAlO3 by PLD   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3
  Target/Source material: LaAlO3
  Atmosphere: O2 as background
  (Partial) Pressures: O2=0.001mbar
  Temperature: 850C
  Time: 23-27 Sec per monolayer of LAO
 [-] Extra process parameters:
  Laser fluency [J/cm²]: 2
  Rep. rate [Hz]: 2
 [-] Patterning of LAO/STO interface      => heterostructure No.: 2 contact: Mohsin Z. Minhas  
 [-] Step 1: Spincoating   
  Equipment used: Spin Coater
  Substrate/Starting material: AR-U 4060 Uralt photoresist
  Atmosphere: Air
 [-] Extra process parameters:
  Rotations: first 300rmp for 15sec
  Rotations: then 5000rmp for 90sec
  Bakeout: at 90C for 15min
  Special comments:

Used it for +ve process.

 [-] Step 1: Photolithography   
  Equipment used: Mask Aligner
 [-] Extra process parameters:
  Filter: UV-filter
  Exposure time: 40sec
  Contact mode: Soft
  Developing material: AR 300-26, 1:4(diluted in water)
  Developing time: 60sec
  Rinsing: Rinsing in deionised water
  Rinsing time: 60sec
 [-] Step 3: Reactive Ion etching   
  Equipment used: ICP RIE Chamber
  Substrate/Starting material: LAO on STO substrate
  Atmosphere: BCl3
  (Partial) Pressures: 6mTorr
  Temperature: 5C
  Time: 13+/-3 nm/min for LAO samples
 [-] Extra process parameters:
  Gas flow: 30sccm
  Chamber pressure: 6mTorr
  Exposition time: depending of thickness and type of material
 [-] Step 4: Resist removal   
  Equipment used: Beaker
  Substrate/Starting material: LAO on top of STO substrate
  Temperature: RT
  Time: 2h
 [-] Extra process parameters:
  NEP (AR 300-70): for 2h at room temperature
 [-] Fabrication of field effect device by LAO / STO interface      => heterostructure No.: 2 contact: Mohsin Z. Minhas  
 [-] Step 1: Patterning of samples   
  Special comments:

Samples are patterned as described in detail 'Patterning of LAO/STO interface'

 [-] Step 2: Deposition of dielectric layer   
  Equipment used: MSEB400 (E-beam)
  Substrate/Starting material: Patterned LAO/STO interface
  Target/Source material: AlOx
 [-] Extra process parameters:
  AlOx deposited by e-beam evaporation: 10nm thickness
  Special comments:

AlOx blanket was deposited on the patterned Hall Bar structures. The liftoff was done by Acetone for 5 min and also with Isopropanol.

 [-] Step 3: Deposition of Metal Gate   
  Equipment used: MSEB400 (E-beam)
  Substrate/Starting material: Patterned LAO/STO interface with AlOx blanket
  Target/Source material: Ti/Au
 [-] Extra process parameters:
  Ti/Au Metal gate: 10/100nm
  Special comments:

The process is not fully reliable for field effect device. Still need to improve the parameters.

 [-] Growth of LSMO on STO by sputtering      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: LSMO sputtering   
  Equipment used: Sputtering system
  Substrate/Starting material: SrTiO3
  Target/Source material: LSMO
  Temperature: 520 C
  Time: 30m
 [-] Extra process parameters:
  Power: 150 W
  Argon flow: 20 SCCM
  Oxygen flow: 10 SCCM
  Sputtering method: DC
  Target size: 76mm
 [-] Growth of NFO on STO by sputtering      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: NFO sputtering   
  Equipment used: Sputtering system
  Substrate/Starting material: SrTiO3
  Target/Source material: NFO
  Temperature: 530 C
  Time: 40m
 [-] Extra process parameters:
  Power: 50 W
  Argon flow: 18 SCCM
  Oxygen flow: 8 SCCM
  Sputtering method: RF
  Target size: 52mm
 [-] Growth of BTO on STO by sputtering      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: BTO sputtering   
  Equipment used: Sputtering system
  Substrate/Starting material: SrTiO3
  Target/Source material: BTO
  Temperature: 530 C
  Time: 30m
 [-] Extra process parameters:
  Power: 40 W
  Argon flow: 14 SCCM
  Oxygen flow: 8 SCCM
  Sputtering method: RF
  Target style: Target facing target
 [-] TiN buffer layers on Si for integration of spinels by sputtering      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: Ta backcoat of Si substrate   
  Equipment used: Sputtering system
  Substrate/Starting material: Si substrate
  Target/Source material: Ta
  Temperature: RT
  Time: 60m
 [-] Extra process parameters:
  Power: 200 W
  Argon flow: 40 SCCM
  Sputtering method: DC
  Target style: 3" S-gun
  Film thickness: 100 nm
  Special comments:

Helps improve heating of Si

 [-] Step 2: Substrate HF etch   
  Equipment used: HF bath
  Substrate/Starting material: Si substrate
  Temperature: RT
  Time: 1m
  Special comments:

Removal of native oxide

 [-] Step 3: Initial TiN seed layer   
  Equipment used: Sputtering system
  Substrate/Starting material: Si substrate
  Target/Source material: Ti
  Temperature: 540 C
  Time: 10m
 [-] Extra process parameters:
  Power: 160W
  Argon flow: 12 SCCM (local injection)
  Nitrogen flow: 7 SCCM
  Sputtering method: Pulsed DC
  Target size: 52mm
  Special comments:

Reactive sputtering of Ti target

 [-] Step 4: Thicker TiN layers   
  Equipment used: Sputtering system
  Substrate/Starting material: Si substrate
  Target/Source material: Ti
  Temperature: 540 C
  Time: 30m
 [-] Extra process parameters:
  Power: 170W
  Argon flow: 12 SCCM (local injection)
  Nitrogen flow: 7 SCCM
  Sputtering method: DC
  Target size: 52mm
  Special comments:

Ti target is burned off for 5m every 10m of sputtering to prevent excessive poisoning of target

 [-] LSMO based MTJ      => heterostructure No.: 7 contact: Dr. Ilaria Bergenti  
 [-] Step 1: STO preparation   
  Equipment used: tube oven
  Substrate/Starting material: SrTiO3 (100) substrate
  Atmosphere: air
  Temperature: 950
  Time: 8h
  Special comments:

STO substrate is first washed in deionized water for 30min then annealed

 [-] Step 2: LSMO deposition   
  Equipment used: CSA
  Substrate/Starting material: SrTiO3
  Target/Source material: LSMO
  Atmosphere: Oxygen
  (Partial) Pressures: 10-2 mbar
  Temperature: 800
 [-] Extra process parameters:
  frequency: 2-5Hz
  Voltage: 12KV
  postannealing @450C in vacuum: time= 0.5 deposition time
  Special comments:

typically 20 nm thick LSMO

 [-] Step 3: STO barrier deposition   
  Equipment used: CSA
  Substrate/Starting material: LSMO/STO
  Target/Source material: STO
  Atmosphere: Oxygen
  (Partial) Pressures: 10-2 mbar
  Temperature: 750 C
 [-] Extra process parameters:
  frequency: 2-5Hz
  Special comments:

sample quenched to RT after deposition

 [-] Step 4: Cobalt Top contact   
  Equipment used: e-beam evaporator
  Substrate/Starting material: STO/LSMO/STO
  Target/Source material: Co
  Atmosphere: -
  (Partial) Pressures: 10-9 mbar
  Temperature: RT
 [-] Growth of ZnO as semiconductor on substrate by PPD Gen IV      => heterostructure No.: 4 contact: Valeria Sanginario  
 [-] Step 1: Substrate cleaning   
  Equipment used: ultrasonic cleaner;RF plasma cleaner
  Substrate/Starting material: substrate
  Temperature: ambient in both cases
  Time: 15 min for ultrasonic bath; 5 minutes for RF plasma cleaner
 [-] Extra process parameters:
  Ultrasonic cleaner power: 100W
  RF cleaner power:: 20 W
 [-] Other chemicals involved:
  Chemical 1: acetone; Role: cleaning solvent
  Chemical 2: isopropanol; Role: cleaning solvent
  Special comments:

Complete cleaning procedure: ultrasonic bath followed by substrate mounting on sample holder and RF Plasma cleaning inside PPD System

 [-] Step 2: PPD deposition   
  Equipment used: PPD Gen IV Gun Dep System
  Target/Source material: ZnO
  Atmosphere: Operational Gas: Oxygen
  (Partial) Pressures: Chamber Pressure: 10-4 Torr
  Temperature: 25°C
  Time: 30 minutes
 [-] Extra process parameters:
  PPD Gun Voltage:: 14 KV
  Gun Frequency:: 70 Hz
  Pulse Energy: 18 J/cm²
  target rotational speed: 20r/m
  substrate rotational speed: 20r/m
  substrate target distance: 75 mm
 [-] Other chemicals involved:
  Chemical 1: PET, any; Role: substrate
 [-] Growth of Fe3O4 as magnetic material on substrate by PPD Gen IV contact: Valeria Sanginario  
 [-] Step 1: Substrate cleaning   
  Equipment used: ultrasonic cleaner;RF plasma cleaner
  Substrate/Starting material: substrate
  Temperature: ambient in both cases
  Time: 15 min for ultrasonic bath; 5 minutes for RF plasma cleaner
 [-] Extra process parameters:
  Ultrasonic cleaner power: 100 W
  RF cleaner power: 20 W
 [-] Other chemicals involved:
  Chemical 1: acetone; Role: cleaning solvent
  Chemical 2: isopropanol; Role: cleaning solvent
  Special comments:

cleaning procedure: ultrasonic, followed by substrate mounting on sample holder and RF Plasma cleaning inside PPD System

 [-] Step 2: PPD deposition   
  Equipment used: PPD Gen IV Gun Dep System
  Target/Source material: Fe3O4
  Atmosphere: Operational gas: Oxygen
  (Partial) Pressures: 6x10-4 Torr
  Temperature: 25 °C
  Time: 30 minutes
 [-] Extra process parameters:
  PPD Gun Voltage: 14 KV
  Frequency: 100 Hz
  Pulse Energy: 18 J/cm²
  target rotational speed: 20r/m
  substrate rotational speed: 20r/m
  substrate target distance: 600 mm
 [-] Growth of ZnO as semiconductor on large substrate by PPD Gen IV      => heterostructure No.: 4 contact: Valeria Sanginario  
 [-] Step 1: Substrate cleaning   
  Equipment used: ultrasonic cleaner;RF plasma cleaner
  Substrate/Starting material: substrate
  Temperature: 25°C
  Time: 15 min for ultrasonic bath; 5 minutes for RF plasma cleaner
 [-] Extra process parameters:
  Ultrasonic cleaner power: 100 W
  RF cleaner power: 20 W
 [-] Other chemicals involved:
  Chemical 1: acetone; Role: cleaning solvent
  Chemical 2: isopropanol; Role: cleaning solvent
  Special comments:

Cleaning Procedure: ultrasonic, followed by substrate mounting on sample holder and RF Plasma cleaning inside PPD System

 [-] Step 2: PPD deposition   
  Equipment used: PPD Gen IV Gun Dep System
  Target/Source material: ZnO
  Atmosphere: Operational Gas: Oxygen
  (Partial) Pressures: 10-4 Torr
  Temperature: 25°C
  Time: 50 minutes
 [-] Extra process parameters:
  PPD Gun Voltage: 14 KV
  Frequency: 80 Hz
  Pulse Energy: 18 J/cm²
  Target rotational speed: 20r/m
  Substrate rotational speed: 20r/m
  substrate target distance: 75 mm
 [-] Other chemicals involved:
  Chemical 1: PET; Role: substrate
 [-] SRO on TiO2 terminated STO substrate contact: Dr. Gertjan Koster  
 [-] Step 1: SRO on STO substrate   
  Equipment used: PLD system
  Substrate/Starting material: STO substrate
  Target/Source material: SRO
  Atmosphere: oxygen/argon
  (Partial) Pressures: 0.15/0.15mbar
  Temperature: 700C
  Time: 15min
 [-] Extra process parameters:
  fluence: 2.1J/cm2
  spotsize: 2.3mm2
  Laser rep.rate: 2hz
  target-substrate distance: 50mm
  cooldown procedure: 30C/min
  moon cycle: full
 [-] Growth of NiFe2O4 on SrTiO3 sustrates by PLD      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: PLD of NiFe2O4   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3
  Target/Source material: NiFe2O4
  Atmosphere: O2
  (Partial) Pressures: 0.045 mbar
  Temperature: 400 C
  Time: 15 minutes
 [-] Extra process parameters:
  Fluence: 0.5 J/cm2
  Repetition rate: 5 Hz
  Target Thickness: 5 nm
 [-] Growth of BaTiO3 on SrTiO3 substrates by PLD      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: PLD of BaTiO3   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3
  Target/Source material: BaTiO3
  Atmosphere: O2
  (Partial) Pressures: 0.075 mbar
  Temperature: 700
  Time: 3 minutes
 [-] Extra process parameters:
  Fluence: 1 J/cm2
  Repetition rate: 5 Hz
  Target thickness: 5 nm
 [-] MTJ fabrication 1: Procedure for Au alignment markers      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: Clean in acetone   
  Equipment used: Ultrasonic Cleaner
  Substrate/Starting material: MTJ stack
  Atmosphere: Air
  (Partial) Pressures: Atm
  Temperature: Room
  Time: 60 s
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Solvent for cleaning
 [-] Step 2: Clean in IPA   
  Equipment used: Ultrasonic Cleaner
  Substrate/Starting material: MTJ stack
  Atmosphere: Air
  (Partial) Pressures: Atm
  Temperature: Room
  Time: 60 s
 [-] Other chemicals involved:
  Chemical 1: Propan-2-ol (IPA); Role: Solvent for cleaning
 [-] Step 3: Clean in O-plasma   
  Equipment used: RF plasma cleaner
  Substrate/Starting material: MTJ stack
  Atmosphere: O2
  (Partial) Pressures: 40 mTorr
  Temperature: 19 C
  Time: 15 s
 [-] Extra process parameters:
  Power: 40 W
  Bias: 100 V
 [-] Step 4: Spin coat resist   
  Equipment used: Spin Coater
  Substrate/Starting material: MTJ stack
  Target/Source material: 950 k PMMA 8% anisol
  Atmosphere: Air
  (Partial) Pressures: Atm
  Time: 60s
 [-] Extra process parameters:
  Rotation: 4000 rpm
  Ramp: 300 rpm/s
  Bake: 150 C /60 s
 [-] Step 5: EBL exposure   
  Equipment used: EBL
  Substrate/Starting material: MTJ stack
 [-] Extra process parameters:
  EBL exposure: 700 uC/cm2
 [-] Step 6: Developement   
  Equipment used: Beaker
  Substrate/Starting material: MTJ stack
  Atmosphere: Air
  (Partial) Pressures: Atm
 [-] Extra process parameters:
  Developer: 7:3 IPA/H2O
 [-] Step 7: Clean in O-plasma   
  Equipment used: RF plasma cleaner
  Substrate/Starting material: MTJ stack
  Atmosphere: O2
  (Partial) Pressures: 40 mTorr
  Time: 60 s
 [-] Extra process parameters:
  Power: 40 W
  Bias: 100 V
 [-] Step 8: Deposit 3 nm Cr   
  Equipment used: Thermal evaporator
  Substrate/Starting material: MTJ stack
  Target/Source material: Cr
 [-] Step 9: Deposit 80 nm Au   
  Equipment used: Thermal evaporator
  Substrate/Starting material: MTJ stack
  Target/Source material: Au
 [-] Step 10: Lift off   
  Equipment used: Beaker
  Substrate/Starting material: MTJ stack
  Atmosphere: Air
  (Partial) Pressures: Atm
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Lift off
  Chemical 2: Propan-2-ol (IPA); Role: rinse
 [-] Growth of SRO/BFO/LSMO heterostructure      => heterostructure No.: 5 contact: Dr. Mehran Vafaee Khanjani  
 [-] Step 1: Substrate treatment   
  Equipment used: tube oven;Ultrasonic Cleaner: Buffered HF solution
  Substrate/Starting material: SrTiO3 (100) substrate
  Atmosphere: O2
  (Partial) Pressures: ambient
  Temperature: 900
  Time: 1 hr
 [-] Extra process parameters:
  ultrasonic for 30 min in deionized water:
  ultrasonic for 30 s in buffered HF:
  3 times rinsing with deionized water:
  cleaning with isopropanol:
 [-] Other chemicals involved:
  Chemical 1: isopropanol; Role: cleaning
  Chemical 2: deionized water; Role: cleaning
 [-] Step 2: PLD growth of SRO   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3 (100) substrate
  Target/Source material: SrRuO3
  Atmosphere: O2
  (Partial) Pressures: 0.1 mbar
  Temperature: 650
 [-] Step 3: PLD growth of BFO   
  Equipment used: PLD system
  Substrate/Starting material: SrTiO3 (100) substrate
  Target/Source material: BiFeO3
  Atmosphere: O2
  (Partial) Pressures: 0.01 mbar
  Temperature: 580
 [-] Step 4: PLD Growth of LSMO   
  Equipment used: PLD
  Substrate/Starting material: SrTiO3 (100) substrate
  Target/Source material: LSMO
  Atmosphere: O2
  (Partial) Pressures: 0.2 mbar
  Temperature: 700
 [-] CeO2 Sputter Deposition on 3      => heterostructure No.: 4 contact: Gerardo Coletta  
 [-] Step 1: Substrate Cleaning   
  Equipment used: Beaker
  Substrate/Starting material: Si substrate
  Temperature: 55 - 70 °C
  Time: 2 - 15 min
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Organic solvent
  Chemical 2: Methanol; Role: Organic solvent
  Chemical 3: H2O2; Role: RCA1 solution component
  Chemical 4: NH4OH; Role: RCA1 solution component
  Chemical 5: Ar; Role: Flushing gas to remove water from sample surfaces
  Special comments:

The cleaning is a multi-steps process which foresees
1) immersion of the material into warm (<55°C) acetone (10')
2) immersion of the material into warm methanol (<55°C - 2-5')
3) rinsing with D-I water and flushing with pressurised filtered Ar
4) immersion of the material into warm (70°C) RCA1 solution (15')
5) rinsing with D-I water and dryin by flushing with pressurised filtered Ar

 [-] Step 2: CeO2 Sputter Deposition on Silicon   
  Equipment used: PVD equipment
  Substrate/Starting material: Si substrate
  Target/Source material: CeO2
  Atmosphere: Ar
  (Partial) Pressures: 0,008 mbar
  Temperature: ranging RT - 300 - 500 °C
  Time: 3 hours
 [-] Extra process parameters:
  flow: 13 - 15 sccm
  power: 80 W
  voltage: 240 - 320 V
  Special comments:

Material is loaded into the PVD chamber nad located in the sample holder. The chamber is, hence, evacuated, down to a base pressure of 10-6 mbar. Ar is hence inserted into the chamber till an operative pressure in the range of 10-3 mbar. Chamber is heated to the desired process temperature (tested RT, 300 and 500 °C). The PVD process is hence started.

 [-] STO Sputter Deposition on 3      => heterostructure No.: 6 contact: Gerardo Coletta  
 [-] Step 2: Substrate Cleaning   
  Equipment used: Beaker
  Substrate/Starting material: Si substrate
  Temperature: 55 - 70 °C
  Time: 2 - 15 minutes
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Organic solvent
  Chemical 2: Methanol; Role: Organic solvent
  Chemical 3: H2O2; Role: RCA1 solution component
  Chemical 4: NH4OH; Role: RCA1 solution component
  Chemical 5: Ar; Role: Flushing gas to remove water from sample surfaces
  Special comments:

The cleaning is a multi-steps process which foresees
1) immersion of the material into warm (<55°C) acetone (10')
2) immersion of the material into warm methanol (<55°C - 2-5')
3) rinsing with D-I water and flushing with pressurised filtered Ar
4) immersion of the material into warm (70°C) RCA1 solution (15')
5) rinsing with D-I water and dryin by flushing with pressurised filtered Ar

 [-] Step 2: STO Sputter Deposition on Silicon   
  Equipment used: PVD equipment
  Substrate/Starting material: Si substrate
  Target/Source material: STO
  Atmosphere: Ar
  (Partial) Pressures: 0,008 mbar
  Temperature: Ranging RT - 300 - 500 - 600 °C
  Time: 3 hours
 [-] Extra process parameters:
  flow: 12 - 15 sccm
  power: 70 W
  voltage: 130 - 170 V
  Special comments:

Material is loaded into the PVD chamber nad located in the sample holder. The chamber is, hence, evacuated, down to a base pressure of 10-6 mbar. Ar is hence inserted into the chamber till an operative pressure in the range of 10-3 mbar. Chamber is heated to the desired process temperature (tested RT, 300, 500 and 600 °C). The PVD process is hence started

 [-] MTJ fabrication 2: Procedure for nLof resit mask for Ar ion etching      => heterostructure No.: 3 contact: Karsten Rode  
 [-] Step 1: Spin coating of primer   
  Equipment used: Spin Coater
  Substrate/Starting material: MTJ stack
  Target/Source material: Ti-primer
  Atmosphere: Air
  (Partial) Pressures: Atm
  Temperature: Room
  Time: 60 s
 [-] Extra process parameters:
  Rotation: 4000 rpm
  Ramp: 1300 rpm/s
  Bake: 100 C/ 60 s
 [-] Step 2: Spin coat nLof   
  Equipment used: Spin Coater
  Substrate/Starting material: MTJ stack
  Target/Source material: nLof resist
  Atmosphere: Air
  (Partial) Pressures: Atm
  Time: 60 s
 [-] Extra process parameters:
  Rotation: 4000 rpm
  Ramp: 1300 rpm/s
  Bake: 100 C/60 s
 [-] Step 3: EBL exposure   
  Equipment used: EBL
  Substrate/Starting material: MTJ stack
 [-] Extra process parameters:
  EBL exposiure: 300 uC/cm2
  Hardbake after exposure: 110 C/ 60 s
 [-] Step 4: Develop   
  Equipment used: Beaker
  Substrate/Starting material: MTJ stack
  Target/Source material: AZ 820 MIF
  Atmosphere: Air
  (Partial) Pressures: Atm
  Time: 90 s
 [-] creating of hallbar structures on LMO/SMO or LSMO/LCMO layers      => heterostructure No.: 6 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: application of resist   
  Equipment used: Spin Coater
  Target/Source material: PMMA resist (600k 4% & 950k 3%)
  Atmosphere: room
  Temperature: bakeout: 1h at 200°C (first layer) or 180°C (second layer)
  Time: 2h
 [-] Extra process parameters:
  rotation speed: 5000 rpm
 [-] Step 2: structuring of the resist for the contact pads   
  Equipment used: EBL
  (Partial) Pressures: HV
  Time: 6h
 [-] Extra process parameters:
  nominal dose: 580 uC/cm2
  develop: 60s Isopropanol
 [-] Other chemicals involved:
  Chemical 1: Isopropanol; Role: developer
  Chemical 2: deionised water; Role: stoper
 [-] Step 3: deposition of contact pads   
  Equipment used: e-beam evaporator
  Target/Source material: Cr / Au
  (Partial) Pressures: 10-7 mbar
  Time: 1h
 [-] Extra process parameters:
  layer thicknesses: Cr=10nm Au=150nm
  liftoff: aceton at 50°C for a few minutes
 [-] Other chemicals involved:
  Chemical 1: aceton; Role: remover
  Chemical 2: isopropanol,water; Role:
 [-] Step 4: application of resist   
  Equipment used: Spin Coater
  Target/Source material: resist AR-U4060 (Allresist)
  Temperature: bakeout: 15min @ 90°C;
  Time: 1h
 [-] Extra process parameters:
  rotation speed: 6000 rpm
 [-] Step 5: structuring of the resist for bars   
  Equipment used: EBL
  (Partial) Pressures: HV
  Temperature: PostBake: 5min @ 110°C
 [-] Extra process parameters:
  nominal dose: 105 uC/cm2
  develop: 60s (AR300-26 1:4 H2O)
  flood exposure: 30s UV
 [-] Other chemicals involved:
  Chemical 1: AR300-26; Role: developer
  Chemical 2: deionised water; Role: stoper
 [-] Step 6: dry etching   
  Equipment used: ICP RIE
  Atmosphere: plasma gas: BCl3
  (Partial) Pressures: chamber pressure: 6 mTorr
  Temperature: 5 °C
  Time: rate: (13 +/- 3) nm / minute
 [-] Extra process parameters:
  RF power: 230 W
  ICP power: 1,200 W
  helium backside contact: 10 Torr
 [-] Other chemicals involved:
  Chemical 1: deionised water; Role: solvent to remove residual chlorine compounds
  Special comments:

for chamber conditioning apply recipe for 5 minutes without sample;
sample fixed with one drop of fombline onto a 6"-wafer as carrier;
bevore locking out sample, allow to pump at chamber base pressure for 5 minutes;
rinse sample in deionised water for 5 minutes after locking out followed by drying with nitrogen brush;
always use special chamber cleaning procedures afterwards;

 [-] Step 7: resist removal   
  Equipment used: beaker
 [-] Extra process parameters:
  maceration I: 120 minutes; room temperature
  maceration II: 60 minutes; 60 °C
  ultrasonic agitation: 5 minutes; 60 °C; 100 W
 [-] Other chemicals involved:
  Chemical 1: N-ethyl-pyrrolidon; Role: solvent for maceration and ultrasonic agitation
  Chemical 2: acetone; Role: solvent for final cleaning
  Chemical 3: propanole; Role: solvent for final cleaning
  Chemical 4: deionised water; Role: solvent for final cleaning
  Chemical 5: nitrogene; Role: drying with brush
 [-] Ti / Pt pads on PCMO / Si substrates      => heterostructure No.: 1 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: application of resist   
  Equipment used: Spin Coater
  Target/Source material: PMMA resist (600k 4% & 950k 3%)
  Atmosphere: room
  Temperature: bakeout: 1h at 200°C (first layer) or 180°C (second layer)
  Time: 2h
 [-] Extra process parameters:
  rotation speed: 5000 rpm
 [-] Step 2: structuring of the resist   
  (Partial) Pressures: HV
 [-] Extra process parameters:
  nominal dose: 570 uC/cm2
  develop: 60s Isopropanol
 [-] Other chemicals involved:
  Chemical 1: Isopropanol; Role: developer
  Chemical 2: deionised water; Role: stoper
 [-] Step 3: deposition of metal pads   
  Equipment used: e-beam evaporator
  Target/Source material: Ti / Pt
  (Partial) Pressures: 10-8 mbar
  Time: 1h
 [-] Extra process parameters:
  layer thicknesses: Ti=15nm Pt=20nm
  liftoff: aceton at 50°C for 20 minutes
 [-] Other chemicals involved:
  Chemical 1: aceton; Role: remover
  Chemical 2: isopropanol,water; Role: final cleaning
 [-] Processing of SRO/BFO/LSMO heterostructure => heterostructure No.: 5      => heterostructure No.: 5 contact: Dr. Mehran Vafaee Khanjani  
 [-] Step 1: Spin coating the resist   
  Equipment used: Beaker;Spin Coater;Ultrasonic Cleaner;Hot plate
  Substrate/Starting material: STO/SRO/BFO/LSMO
  Target/Source material: AR-N 7520.18
  Atmosphere: air
  (Partial) Pressures: ambient
  Temperature: ambient
  Time: 60
 [-] Extra process parameters:
  cleaning the samples with isopropanol in ultrasonic:
  spin coating:
  post spin baking for 1 min at 85°C:
 [-] Step 2: EBL Exposure   
  Equipment used: EBL
 [-] Step 3: Development   
  Equipment used: Beaker
  Substrate/Starting material: STO/SRO/BFO/LSMO
  Target/Source material: AR 300-47
  Atmosphere: air
  (Partial) Pressures: ambient
  Temperature: ambient
  Time: 5 min
 [-] Extra process parameters:
  soaking in H2O before development for 15 sec:
  soaking in H2O after development for 1 min:
  post baking at 100 °C for 1 min:
 [-] Step 4: Ion beam etching   
  Equipment used: IBE
  Substrate/Starting material: STO/SRO/BFO/LSMO
  Atmosphere: Ar
  Temperature: ambient
  Time: Rate of 5 nm/min
 [-] Growth of LMO/SMO superlattices      => heterostructure No.: 6 contact: Prof. Dr. Vasily Moshnyaga  
 [-] Step 1: Growth of LMO/SMO superlattices (HS6)   
  Equipment used: MAD
  Substrate/Starting material: STO substrate
  Target/Source material: metalorganic precursors
  Atmosphere: ambient oxygen
  (Partial) Pressures: 20 % O2
  Temperature: 800-900°C
  Time: 2-10 min
 [-] Extra process parameters:
  precursor molarity: 0.01-0.04M
  grwoth rate: 0.1-10 nm/min
  substrate area: 1-3 cm2
  spraying gas flow: 1-2 m3/hour
 [-] Other chemicals involved:
  Chemical 1: La-acetylacetonate; Role: precursor material
  Chemical 2: Sr-acetyacetonate; Role: precursor material
  Chemical 3: Mn-acetylacetonate; Role: precursor material
  Special comments:

MAD technique uses aersols of solutions of metalorganic precusrors, sprayed by a spraying gas onto the heated substrate, where a heterogeneous pyrolisis reaction takes place and the oxide film grows.

 [-] direct patterning      => heterostructure No.: HS4 contact: Dr. Daniele Pullini  
 [-] Step 1: direct patterning of ZnO and Au film (contacting)   
  Equipment used: clean room photolitography (1 micron mininum detail)
  Substrate/Starting material: YSZ/Si or CeO2/Si
  Target/Source material: N.A
  Atmosphere: N.A.
  (Partial) Pressures: N.A.
  Temperature: NA
  Time: NA
 [-] Extra process parameters:
  AZ4562 (1:3)m photoresisit spinning: 100rpm for 30 sec
  PR soft backing: 90°C per 30 sec
  PR exposure: 470W for 30 sec
  PR development: KOH 1% for 60 sec
 [-] first lithography step for defining pillar structure in LSMO based MTJ      => heterostructure No.: 7 contact: Dr. Carlos Vaz  
 [-] Step 1: spin coating   
  Equipment used: Spin Coater
  Substrate/Starting material: 7
 [-] Extra process parameters:
  spin-coat Ti primer: 4000 rmp/60s acc=2000 rmp/s
 [-] Step 2: baking   
  Equipment used: Hot plate
  Substrate/Starting material: 7
  Temperature: 100 C
  Time: 60sec
 [-] Step 3: spin coating   
  Equipment used: Spin Coater
  Substrate/Starting material: 7
 [-] Extra process parameters:
  spin-coat nLof 2010:EBR 1:0.5: 4000 rpm/60s a=2000rpm/s
 [-] Step 4: baking   
  Equipment used: Hot plate
  Substrate/Starting material: 7
  Temperature: 100 C
  Time: 60sec
 [-] Step 5: Lithography   
  Equipment used: EBL
  Substrate/Starting material: 7
 [-] Extra process parameters:
  expose at 320 uC/cm2:
 [-] Step 6: post baking   
  Equipment used: Hot plate
  Substrate/Starting material: 7
  Temperature: 110 C
  Time: 60sec
 [-] Step 7: development   
  Equipment used: beaker
  Substrate/Starting material: 7
 [-] Extra process parameters:
  develop in AZ826MIF/1min 15s:
 [-] Step 8: rinsing   
  Equipment used: beaker
  Substrate/Starting material: 7
 [-] Extra process parameters:
  rinse in DI water:
 [-] third lithography step for defining pillar structure in LSMO based MTJ      => heterostructure No.: 7 contact: Dr. Carlos Vaz  
 [-] Step 1: O plasma etching   
  Equipment used: RF plasma cleaner
  Substrate/Starting material: 7
  Atmosphere: 40 mtorr O2
  Temperature: 18 C
  Time: 11-13 min
 [-] Extra process parameters:
  O-plasma ashing (20 sccm O2, 40 mtorr O2, 40 W, 200 V, T=18 oC:
  Special comments:

etching was done in steps of 2 min

 [-] YSZ Sputter Deposition on 4" Silicon wafers      => heterostructure No.: 4 contact: Gerardo Coletta  
 [-] Step 1: Substrate Cleaning   
  Equipment used: beaker
  Substrate/Starting material: Si substrate
  Temperature: <55°C
  Time: 2-10 minutes
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Organic solvent
  Chemical 2: Methanol; Role: Organic solvent
  Chemical 3: H2O2; Role: RCA1 solution component
  Chemical 4: NH4OH; Role: RCA1 solution component
  Chemical 5: HF; Role: Silicon oxide stripper
  Chemical 6: Ar; Role: Flushing gas to remove water from the wafer surface
  Special comments:

The cleaning is a multi-steps process which foresees
1) immersion of the material into warm (<55°C) acetone (10')
2) immersion of the material into warm methanol (<55°C - 2-5')
3) rinsing with D-I water and flushing with pressurised filtered Ar
4) immersion of the material into warm (70°C) RCA1 solution (15')
5) rinsing with D-I water and flushing with pressurised filtered Ar
6) immersion of the material into RT HF (1')
7) rinsing with D-I water and dryin by flushing with pressurised filtered Ar

 [-] STO Sputter Deposition on 4" Silicon wafers      => heterostructure No.: 6 contact: Gerardo Coletta  
 [-] Step 1: Substrate Cleaning   
  Equipment used: beaker
  Substrate/Starting material: Si substrate
  Temperature: <55°C
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Organic solvent
  Chemical 2: Methanol; Role: Organic solvent
  Chemical 3: H2O2; Role: RCA1 solution component
  Chemical 4: NH4OH; Role: RCA1 solution component
  Chemical 5: HF; Role: Silicon oxide stripper
  Chemical 6: Ar; Role: Flushing gas to remove water from wafer surface
  Special comments:

The cleaning is a multi-steps process which foresees
1) immersion of the material into warm (<55°C) acetone (10')
2) immersion of the material into warm methanol (<55°C - 2-5')
3) rinsing with D-I water and flushing with pressurised filtered Ar
4) immersion of the material into warm (70°C) RCA1 solution (15')
5) rinsing with D-I water and flushing with pressurised filtered Ar
6) immersion of the material into RT HF (1')
7) rinsing with D-I water and dryin by flushing with pressurised filtered Ar

 [-] YSZ/CeO2 Sputter deposition on 4" SputterSi wafers      => heterostructure No.: 4 contact: Gerardo Coletta  
 [-] Step 1: Substrate Cleaning   
  Equipment used: beaker
  Substrate/Starting material: Si substrate
  Temperature: <55°C
 [-] Other chemicals involved:
  Chemical 1: Acetone; Role: Organic solvent
  Chemical 2: Methanol; Role: Organic solvent
  Chemical 3: H2O2; Role: RCA1 Solution component
  Chemical 4: NH4OH; Role: RCA1 Solution Component
  Chemical 5: HF; Role: Silicon Oxide stripper
  Chemical 6: Ar; Role: Flushing gas to remove water from wafer surface
  Special comments:

The cleaning is a multi-steps process which foresees
1) immersion of the material into warm (<55°C) acetone (10')
2) immersion of the material into warm methanol (<55°C - 2-5')
3) rinsing with D-I water and flushing with pressurised filtered Ar
4) immersion of the material into warm (70°C) RCA1 solution (15')
5) rinsing with D-I water and flushing with pressurised filtered Ar
6) immersion of the material into RT HF (1')
7) rinsing with D-I water and dryin by flushing with pressurised filtered Ar

 [-] Step 2: YSZ sputter deposition on Silicon   
  Equipment used: PVD equipment
  Substrate/Starting material: Si substrate
  Target/Source material: YsZ
  Atmosphere: Ar
  (Partial) Pressures: 0,008
  Temperature: ranging RT - 300 - 500 °C
  Time: 3 hours
 [-] Extra process parameters:
  flow: 10-17 sccm
  power: 60-100 W
  Voltage: 200-300 V
  time: 3 hrs
  Special comments:

Material is loaded into the PVD chamber nad located in the sample holder. The chamber is, hence, evacuated, down to a base pressure of 10-6 mbar. Ar is hence inserted into the chamber till an operative pressure in the range of 10-3 mbar. Chamber is heated to the desired process temperature (500 °C). The PVD process is hence started.

 [-] second lithography step for defining pillar structure in LSMO based MTJ => heterostructure No.: 7      => heterostructure No.: 7 contact: Dr. Mehran Vafaee Khanjani  
 [-] Step 1: IBE   
  Equipment used: IBE
  Substrate/Starting material: 7
  Atmosphere: Ar
  Temperature: ambient
  Time: 5 nm/min
 [-] Extra process parameters:
  Microwave power: 330 W
  Beam extractor: 300 V
  Accelerator: 400 V
 [-] Pattering of heterostructure (Ru+Cu+Ta+Ru+NFO+BTO+LSMO++STO) # 2775c      => heterostructure No.: 3 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: spincoating   
  Equipment used: Spin Coater
 [-] Extra process parameters:
  spinning, step a: 5"@300/minute
  spinning, step b: 45"@5,000/minute
  baking: 15'@90°C
 [-] Other chemicals involved:
  Chemical 1: AR 4060 P; Role: photo resist
 [-] Step 2: photo lithography   
  Equipment used: Mask Aligner
 [-] Extra process parameters:
  exposition: 10"
  Special comments:

no filter, mask: layer 1

 [-] Step 3: developing   
  Equipment used: beaker
  Temperature: RT
  Time: 60"
 [-] Other chemicals involved:
  Chemical 1: AR 300-26; 1:4; Role: developer
 [-] Step 4: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  application Ti (bonding agent): 10 nm
  application Au: 150 nm
  Special comments:

both evaporations in situ

 [-] Step 5: liftoff   
  Equipment used: beaker
  Atmosphere: ambient
  Temperature: room temperature
 [-] Extra process parameters:
  acetone: 3 minutes
  acetone and ultrasonic: 10 seconds
  Special comments:

rinsing in di-water and drying with nitrogene-brush at moderate flow

 [-] Step 6: examination   
  Equipment used: Optical Microscope
  Special comments:

checking results of previous processes and storing of images

 [-] Step 7: etching of Ru-Cu-Ta-Ru-stack   
  Equipment used: Argon Ion Mill
  Temperature: room temperature
  Time: appr. 00:01:00
 [-] Extra process parameters:
  Ar process gas: 50 sccm per minute
  tilt angle: 80°
  sample rotation speed: 6 per minute
  Special comments:

beam neutralisation used, process controlled by quadrupole mass spectrometry (process stopped after Ru vanished)

 [-] Step 8: eching of NFO+BTO+LSMO   
  Equipment used: ICP RIE
  (Partial) Pressures: 6 mTorr
  Temperature: 5°C
  Time: 00:00:42
 [-] Extra process parameters:
  BCl3 process gas: 30 sccm per minute
  RF power: 150 W
  ICP power: 1,000 W
  Special comments:

etch rates of combined recipe:
NFO (19+/-2) nm per minute
BTO (10+/-3) nm per minute
LSMO (7+/-1) nm per minute
Bias Voltage -460 V
allow vacuum to drop until 10e-6 mTorr before locking out sample
rinse sample immediately in di-water
dry with nitrogene brush

 [-] Step 9: cleaning and preparation   
  Equipment used: Oxigene plasma icinerator
  Atmosphere: Oxygen
  (Partial) Pressures: 8E-2 mbar
  Temperature: room temperature
  Time: 00:00:36
 [-] Extra process parameters:
  RF power: 90 W
 [-] Step 10: spincoating   
  Equipment used: Spincoater
 [-] Extra process parameters:
  spincoating AR 300-80: 5
  : 45
  baking: 3 minutes @ 180°C
  spincoating AR-U 4060S1: 5
  : 45
  baking: 15 minutes @ 90°C
 [-] Step 11: photo lithography   
  Equipment used: Mask Aligner
 [-] Extra process parameters:
  exposition: 10
  post exposure bake: 5 minutes @ 110°C
  flood exposure: 30 s
  developing: AR-U 300-26: H2O 1:4
  Special comments:

mask layer 3; no filter

 [-] Step 12: cleaning and preparation   
  Equipment used: Oxigene plasma icinerator
  Atmosphere: Oxygen
  (Partial) Pressures: 8E-2 mbar
  Temperature: room temperature
  Time: 00:00:36
 [-] Extra process parameters:
  RF power: 90 W
 [-] Step 13: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  Al2O3 deposition: 150 nm
  Lifoff: 90 minutes in acetone @ 75°C
 [-] Step 14: examination   
  Equipment used: Optical Microscope
  Special comments:

checking results of previous processes and storing of images

 [-] Step 15: spincoating   
  Equipment used: spin coater;heating plate
 [-] Extra process parameters:
  spincoating AR 300-80: 3"@300/minute
  : 45"@4,000/minute
  baking: 3 minutes @ 180°C
  spincoating AR-U 4060: 3"@300/minute
  : 45"@5,000/minute
  : 15 minutes @ 90°C
 [-] Step 16: photo lithography   
  Equipment used: Mask Aligner
 [-] Extra process parameters:
  exposition: 10
  developing AR-U 300-26 1:4 H2O:
  Special comments:

no filter, mask layer 4

 [-] Step 17: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  deposition Ti: 10 nm
  depositon Au: 170 nm
  Lifoff: 60 minutes in acetone @ 75°C
 [-] Step 18: examination   
  Equipment used: Optical Microscope
  Special comments:

checking results of previous processes and storing of images

 [-] Pattering of heterostructure (LSMO+BTO+NFO+SRO++STO) # 2829      => heterostructure No.: 3 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: spincoating   
  Equipment used: spin coater;heating plate
 [-] Extra process parameters:
  spinning, step a: 5"@300/minute
  spinning, step b: 45"@5,000/minute
  baking: 15'@90°C
 [-] Other chemicals involved:
  Chemical 1: AR-U 4060; Role: photo resist
 [-] Step 2: photo lithography   
  Equipment used: Mask Aligner
 [-] Extra process parameters:
  exposition: 10"
  Special comments:

no filter, mask: layer 1

 [-] Step 3: developing   
  Equipment used: beaker
  Temperature: room temperature
  Time: 60"
 [-] Other chemicals involved:
  Chemical 1: AR 300-26; 1:4; Role: developer
 [-] Step 4: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  deposition Ti (bonding agent): 10 nm
  depositon Au: 150 nm
  Special comments:

both evaporations in situ

 [-] Step 5: liftoff   
  Equipment used: beaker
  Atmosphere: ambient
  Temperature: room temperature
 [-] Extra process parameters:
  acetone: 3 minutes
  acetone and ultrasonic: 10 seconds
  Special comments:

rinsing in di-water and drying with nitrogene-brush at moderate flow

 [-] Step 6: dry etching of LSMO-BTO-NFO-stack   
  Equipment used: ICP RIE
  (Partial) Pressures: 6 mTorr
  Temperature: 15°C
  Time: 00:02:06
 [-] Extra process parameters:
  BCl3 process gas: 30 sccm per minute
  RF power: 150 W
  ICP power: 1,000 W
  Special comments:

etch rates of combined recipe:
NFO (19+/-2) nm per minute
BTO (10+/-3) nm per minute
LSMO (7+/-1) nm per minute
Bias Voltage -460 V
allow vacuum to drop until 10e-6 mTorr before locking out sample
rinse sample immediately in di-water
dry with nitrogene brush

 [-] Step 7: cleaning and preparation   
  Equipment used: Oxigene plasma icinerator
  Atmosphere: Oxygen
  (Partial) Pressures: 8E-2 mbar
  Temperature: Room Temperature
  Time: 00:00:36
 [-] Extra process parameters:
  RF power: 90 W
 [-] Step 8: spincoating   
  Equipment used: spin coater;heating plate
 [-] Extra process parameters:
  spincoating AR 300-80: 5s @ 300/min
  : 45s @ 4000/min
  baking: 3 minutes @ 180°C
  spincoating AR-U 4060 S1: 5s @ 300/min
  : 45s @ 5000/min
  baking: 15 minutes @ 90°C
 [-] Step 9: e-beam lithography   
  Equipment used: Raith system
  Special comments:

Structure:TMR_MASKE1_JK-FINAL/MaskFinal_mirrored_reduced/3; PositionList:2829_L2; Type:LiftOff; Modus:Meander;LongitMode
WF:100 [980x]µm; 30kV;239pA;Ap:30µm;FD:10.007 (corrected)mm
Align:0.97166,0.95349,-0.009,0.015,-0.175,-0.321 Factor:1.003,1.003
AreaDose:200µC/cm² [0.008x0.013]µm²;
Bake:10m@105°C
30kV;AP30;S:-7.2,1.1;A:7.0,1.0

 [-] Step 10: developing   
  Equipment used: mask aligner;heating plate;beaker
 [-] Extra process parameters:
  post exposure bake: 10 minutes@105°C
  flood exposure: 30 seconds
  developing AR-U 300-26 1:2 H2O: 60 seconds
 [-] Step 11: cleaning and preparation   
  Equipment used: Oxigene plasma icinerator
  Atmosphere: Oxygen
  (Partial) Pressures: 8E-2 mbar
  Temperature: room temperature
  Time: 00:00:36
 [-] Extra process parameters:
  RF power: 90 W
 [-] Step 12: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  deposition Al2O3: 150 nm
  liftoff: 60 minutes in acetone @ 80°C
 [-] Step 13: spincoating   
  Equipment used: spin coater;heating plate
 [-] Extra process parameters:
  spincoating AR 300-80: 5s @ 300/min
  : 45s @ 5000/min
  baking: 3 minutes @ 180°C
  spincoating AR-U 4060: 5s @ 300/min
  : 45s @ 5000/min
  baking: 15 minutes @ 90°C
 [-] Step 14: photo lithography   
  Equipment used: mask aligner;beaker
 [-] Extra process parameters:
  exposition: 10
  developing AR-U 300-26 1:4 H2O: 60 seconds
  Special comments:

no filter, TMR Mask layer 4

 [-] Step 15: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  deposition Ti (bonding agent): 10 nm
  depositon Au: 170 nm
  liftoff: 5 minutes in acetone @ 80°C and ultrasonic
 [-] Step 16: examination   
  Equipment used: Optical Microscope;Profilometer
  Special comments:

checking results of previous processes and storing of images

 [-] Pattering of heterostructure (Ru+NFO+BTO+LSMO++STO) # 2832      => heterostructure No.: 3 contact: Prof. Dr. Georg Schmidt  
 [-] Step 1: spincoating   
  Equipment used: spin coater;heating plate
 [-] Extra process parameters:
  spinning, step a: 5"@300/minute
  spinning, step b: 45"@5,000/minute
  baking: 15 minutes @ 90°C
 [-] Other chemicals involved:
  Chemical 1: AR-U 4060; Role: photo resist
 [-] Step 2: photo lithography   
  Equipment used: Mask Aligner
 [-] Extra process parameters:
  exposition: 10"
  Special comments:

no filter, mask: layer 1

 [-] Step 3: developing   
  Equipment used: beaker
  Temperature: room temperature
  Time: 60"
 [-] Other chemicals involved:
  Chemical 1: AR 300-26; 1:4; Role: developer
 [-] Step 4: metal deposition   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  deposition Ti (bonding agent): 10 nm
  depositon Au: 150 nm
  liftoff: 60 minutes in acetone @ 75°C
 [-] Step 5: etching Ru-layer   
  Equipment used: Argon Ion Mill
  Temperature: room temperature
  Time: appr. 00:01:00
 [-] Extra process parameters:
  tilt angle: 80°
  sample rotation speed: 6 per minute
  Special comments:

beam neutralisation used, process controlled by quadrupole mass spectrometry (process stopped after Ru vanished)

 [-] Step 6: dry etching of LSMO-BTO-NFO-stack   
  Equipment used: ICP RIE
  (Partial) Pressures: 6 mTorr
  Temperature: 5°C
  Time: 00:00:19
 [-] Extra process parameters:
  BCl3 process gas: 30 sccm per minute
  RF power: 150 W
  ICP power: 1,000 W
  Special comments:

Special comments:

etch rates of combined recipe:
NFO (19+/-2) nm per minute
BTO (10+/-3) nm per minute
LSMO (7+/-1) nm per minute
Bias Voltage -460 V
allow vacuum to drop until 10e-6 mTorr before locking out sample
rinse sample immediately in di-water
dry with nitrogene brush

 [-] Step 7: cleaning and preparation   
  Equipment used: Oxigene plasma icinerator
  Atmosphere: Oxygen
  (Partial) Pressures: 8E-2 mbar
  Temperature: Room Temperature
  Time: 00:00:36
 [-] Extra process parameters:
  RF power: 90 W
 [-] Step 8: spincoating   
  Equipment used: spin coater;heating plate
 [-] Extra process parameters:
  spincoating AR 300-80: 5
  : 45
  baking: 3 minutes @ 180°C
  spincoating AR-U 4060S1: 5
  : 45
  baking: 15 minutes @ 90°C
 [-] Step 9: e-beam lithography   
  Equipment used: Raith system
  Special comments:

Structure:TMR_Maske1_JK-Final.csf/MaskFinal_mirrored_2832b/3; PositionList:2832a_L2; Modus:Meander;LongitMode
WF:100 [980x]µm; 30kV;248pA;Ap:30µm;FD:10.025 (corrected)mm
Align:0.97080,0.95259,-0.002,0.014,0.410,0.285 Factor:1.003,1.003
AreaDose:200µC/cm² [0.008x0.013]µm²;

30kV;AP30;S:-7.3,0.9;A:7.0,1.0

 [-] Step 10: developing   
  Equipment used: beaker
  Special comments:

post exposure bake: 10 minutes@105°C
flood exposure: 30 seconds
developing AR-U 300-26 1:2 H2O: 60 seconds

 [-] Step 11: cleaning and preparation   
  Equipment used: Oxigene plasma icinerator
  Atmosphere: Oxygen
  (Partial) Pressures: 8E-2 mbar
  Temperature: room temperature
  Time: 00:00:36
 [-] Extra process parameters:
  RF power: 90 W
 [-] Step 12: metal deposition   
  Equipment used: E-Beam Evaporator;beaker
 [-] Extra process parameters:
  deposition Al2O3: 150 nm
  liftoff: 60 minutes in acetone @ 70°C
 [-] Step 13: Spincoating   
  Equipment used: heating plate;spin coater
 [-] Extra process parameters:
  spincoating AR 300-80: 5s @ 300/min
  : 45s @ 4000/min
  baking: 3min @ 180°C
  spincoating AR-U 4060: 5s @ 300/min
  : 45s @ 5000/min
  baking: 15min@90°C
 [-] Step 14: photo lithography   
  Equipment used: mask aligner
 [-] Extra process parameters:
  expositon: 10s
  developing: AR-U 300-26 1:4 H2O: 60 seconds
  Special comments:

Mask: TMR Layer 4, no filter

 [-] Step 15: metal depositon   
  Equipment used: E-Beam Evaporator
 [-] Extra process parameters:
  deposition Ti (bonding agent): 10 nm
  depositon Au: 170 nm
  liftoff: 5 minutes in acetone @ 80°C and ultrasonic
 [-] Step 16: Examination   
  Equipment used: Optical Microscope;Profilometer
  Special comments:

checking results of previous processes and storing of images

  PLD deposition of SRO on 4'' (CeO2)/YsZ/Si      => heterostructure No.: 1, 4 contact: Eddy Rodijk