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2016-03
2016-03Edit

    01/03

    Summary:

    • BPC6 : wafer batch 3481 rho>20kohm.cm; LAYER1 on AZ5214 inversed; 100 nm Al; lift-off acetoneLAYER2 on BCB; BCB bake 1hr;

    • BPC7 Si intrinsic [100] 5-10 kΩ.cm ; clean HF ; 100 nm Al; LAYER1 on S1813 + Al etch; remove resist; LAYER2 on BCB; BCB clean; BCB bake 1hr; 

    • BCB-TEST3 : on non-oxidized standard Si; temoin of LAYER2 on BPC7; currently test LAYER3 with S1828 and inversed mask.

    • BPC8 : Si intrinsic [100]  rho > 20kohm.cm; clean HF ; LAYER1 on AZ5214 inversed; 100 nm Al; lift-off acetone;  

    • BPCT8 :  Done in parallel with BPC8. LAYER1 on AZ5214 inversed; BILAYER test: 150 nm Al/5nm Pd; lift-off remover PG; Measure Tc=935mK

    PMGI-AZ5214-TEST

     02/03

    I prepared a little bottle of PMGI SF15. It is transparent.

    • Layer 3: PMGI-AZ MASK (on two Si waffer called A and B)
    heat waffer in hotplate at 110°C for 10min
    spin TI primer 60sec at 4000rpm
    bake Ti primer at 110°C for 2min
    
    spin PMGI SF15 60" @ 1krpm (with a first step of 10sec at 300rpm to distribute the resist)
    

    Comment1: There are still "angel hairs" formed at the edges of the waffer. I have decided to clean them with Remover PG using and isope. This has to be done very carefully.

    Comment2: It is better to dispense the PMGI just after taking it out from the bottle in the syringue.

    filmetrics.JPG

    The resulting width is in agreement with expected according to datasheet.

    bake PMGI 5min at 220°C
    spin AZ5214E (per 16/12/2014) 60" @ 4krpm
    bake 2' @ 110°C
    

    In order to test the mask I use the mask I fabricated, i.e. the inversed layer 3

    Expo 62mJ/cm2 (6.2" @ 11mW) , Vacuum contact
    bake 3' @ 120°C (=setpoint). 
    Flood expo 45"  
    I decide to separate samples:
    A: Dev MIF726 1min @ 19.0°C, rinse ODI 60" beaker + 30" water tap
    B: Dev MIF726 50sec+10+10 @ 19.0°C, rinse ODI 60" beaker + 30" water tap 
    
    result A:
    pmgiaz-testA-resume.jpg
     
    I didn't know at the moment but what we observe is PMGI in the middle of the motifs.
     
    result B:
    pmgiaz-testB-resume.jpg
     
    Plasma clean for A and B
    Plasma Oxi : Pr=200ubar , P=100W, 40 sec
    I took sample A to evap.
     03/03

    Evap on PMGI-AZ-TEST-A

    In a quarter of waffer I etched and evaporated and in the other one I just evaporated 

    A1-Etch Ar 500V 130mA for 1min40 + Evap 100nm Al @ 1nm/s
    A2-Evap 100nm Al @ 1nm/s
    

    Result Etch and evap:

    pmgiaz-testA_01b.JPG

    pmgiaz-testA_02.jpg

     

    Essentialy PMGI didn't left in the developer. maybe heating 220deg is too much. Development time too short?

     

    • PMGI-AZ-TEST-C and D
    heat waffer in hotplate at 110°C for 10min
    spin TI primer 60sec at 4000rpm
    bake Ti primer at 110°C for 2min
    
    spin PMGI SF15 60" @ 1krpm (with a first step of 10sec at 300rpm to distribute the resist)
    bake PMGI 5min at 200°C
    spin AZ5214E (per 16/12/2014) 60" @ 4krpm
    bake 2' @ 110°C

    PMGI-AZ-TEST C- In order to test the mask I use the mask fabricated IEF

    Expo 62mJ/cm2-64mJ/cm2-66, Vacuum contact
    bake 3' @ 120°C (=setpoint). 
    Flood expo 50"
    Dev MIF726 3min @ 19.0°C, rinse ODI 60" beaker + 30" water tap
    I took three minutes to the resist to leave. This mask is useful to verify this.
    !!! This indicates that in PMGIAZ-TESTA and B I was far away in the development time. !!!
     
    lithoIEF-3min_01.JPGlithoIEF-3min_03.JPG
     
    I try 20 more seconds
    PMGIAZ-TESTC-3min-plus20sec_02.jpg
    the undercut after 3min 20sec
    lithoIEF-3min-plus20sec_01.JPG
    PMGIAZ-TESTC-3min-plus20sec.jpg
     

    PMGI-AZ-TEST D- I use the mask Layer 3 

    Expo 62mJ/cm2, Vacuum contact
    bake 3' @ 120°C (=setpoint). 
    Flood expo 50"
    Dev MIF726 3min @ 19.0°C, rinse ODI 60" beaker + 30" water tap
     
    PMGIAZ-TEST-D-3min_01.JPGPMGIAZ-TEST-D-3min_02.JPG
     07/03
    • PMGI spinning test

    I prepare three recup waffers to try different spinning procedures to avoid "ugly hair" from PMGI

    • 10sec 350rpm acc200; 60sec 1000rpm acc200 ---> result: OK. Some hairs 
    • 5sec 300rpm acc200; 5sec 500rpm acc200; 60sec 1000rpm acc200 ---> result: really OK. Some hairs still
    • 5sec 300rpm acc200; 5sec 500rpm acc200; 60sec 1000rpm acc200; 5sec 7000rpm acc4000 ---> result: awful, hairs over the chip- Do not accelerate

    I remove the resist in Remover PG to re-check the removal of the edges with an isope and the baking.

    I do 5sec 300rpm acc200; 5sec 500rpm acc200; 60sec 1000rpm acc200 + clean edges with remover + baked 5min @ 200deg---> result: OK in the three waffers. All hairs left. In one case I don't even have to remove the hairs.

    New wafers BPC9 & BPCT9

    As BPC8 was badly injured at step 3, I decide to process 2 new wafers. 
    Note that the conclusion drawn from BPC8 was that we should not use PMGI baked at 200°C, because de development differential becomes too big with AZ : after 5'15, the PMGI is not fully etched in all patterns, while the aluminium layer is already etched from the developper.
    Consequence: go back to LOR30B, and bake it a bit harder than the test performed at 170°C, or use PMGI and bake it lower.
    See corresponding page BPC9

    LOR or PMGI development time versus temperature

    After having messed up with BPC8, I decide to make a test of development versus baking temperature, to define the optimum (planarization / dev time)

    The spinning procedure is now well defined:

    wafer Si/SiO2 standard
    bake the wafer @ 110°C for water removal
    tape the wafer on blue clean room tape, cut to a ~3" size
    dispense 1-1.5mL resist slowly from a pipette (well centered on wafer)
    2" @ 300rpm acc 250rpm/s
    3" @ 800rpm acc 500rpm/s
    60" @ 1500rpm acc 500rpm/s
    Cut the edges of the spun resist on all sides of the wafer before untaping
    
    NB: some condition, either acc on final spin step or resist quantity
    acc=750 and/or >2mL makes the tape bend upward (tensile strength)
    acc=500 and/or <1.5mL resist makes the tape bend downward (compressive)
    We should probably be compressive, to insure the bridge does not open more when we open it
    OBS: it happens that on one side, the tape is lifted up, on the other side lifted down. 
    Where it is lifted up, there is a lot of resist (continuous film) wherea where lift down
    there are only angel hairs.
    The resist quantity is probably responsible for tensile / compressive strength
    

    characterization procedure:

    after spin
    bake 5' @ XX °C
    develop in MFCD26 until end of intereferences (MFCD26 equivalent to MF726 which is empty)
    • PMGI SF15

    temp
    °C
    interf start
    min  ss
    interf stop
    min  ss
    comment
    150 1' 1'15 4.8µm - 5.2µm (edges)
    fresh dev
    very homogeneous
    160 1'10 1'35 fresh dev
    170 1'25 1'50 2nd wafer dev
    180 1'35 2'07 3rd wafer dev
    190 1'50 2'20 fresh dev
    very homogeneous (spin also probably), almost no pattern
    200 1'55 2'45 4th wafer dev
    much more inhomogeneous

    According to observations on BPC8: baked at 200°C, after 5'15 still residues in some patterns, should indeed double the "interference" stop time for actual development.
    Even at 160°C this is not really secure for Al (would mean 3'10 dev time)

    • LOR30B
      resist is perempted since 2006, alsmost nothing left in the main bottle, and Camille bottle seems spoiled with crystals!!! Bottle was not really closed !!
      at 2000rpm (with same procedure as before) ellipso tells 6.5µm (according to DS shoudl be 4µm)

    temperature
    °C
    interf start
    min  ss
    interf stop
    min  ss
    comment
    160      
    170      
    180      
    190   1'40 (??) 2nd dev
    no clear interfence
    200      
    • LOR20B
      resist is perempted since 2010, main bottle is almost full
      I take Camille bottle for spin tests. It is clean. Spin really perfect, except the edges are crusty (probably because resist perempted)
      at 1500rpm (with same procedure as before) ellipso tells 4.55µm in the center, 5µm on the edge
      (according to DS shoudl be 3µm)

    temperature
    °C
    interf start
    min  ss
    interf stop
    min  ss
    comment
    160 28" 40" 4.8 µm
    170 30" 45" - 50" 4.7 - 5.2µm
    180 37" 57" 4.7µm
    25" 2nd dev + fresh
    190 40" 1'05 - 1'25 fresh dev
    not homogeneous
    200      

    Note: the dev turns red, so cannot be used for 2 wafers. Use scarcely as there is almost no left.

    PMGI SF15 - AZ development time

    • Procedure
    spin SF15 as above
    bake 5" @ 110°C -> bake 5' @ 150°C
    spin AZ5214E 4krpm
    bake 1' @ 110°C
    exp dose 5" @ 9.5mW/cm2 (47.5mJ/cm2)
    bake xx @ 120°C
    flood exp 45" @ 9.5mW/cm2
    dev MFCD26 @ 21.2°C

    Tests: (14/03/2016)

    wafer exp bake development comments
    red AZ
    start
    interf start
    min  ss
    interf stop
    min  ss
    spin, dev obs + conclusion
    1 47.5 120°C, 4' 20" 1'15 1'40 - 1'52 4.8µm - 4.9µm (edges)
    2nd dev
    stupid me: put it in another dev bath instead of water!
    2 47.5 120°C, 3' 25"-30" 1'35 2' 4.77µm - 5.2µm (edges)
    3rd dev
    very homogeneous
    AZ was not strong enough, got developped -> bake harder
    3 47.5 125, 4'30 not seen 2'15 3'15 fresh dev
    very inhomogeneous!!
    AZ unexposed patteerns were hardened at cure
    Development inhomogeneous and much longer!!
    -> do not bake harder
    In fact the mask used was shit (problem on AZ came from that)
    4 47.5 120°C, 4' not seen not seen not seen PMGI bake 17' (forgot)
    mask layer 3
    Lots of little cracks in AZ
    But dev 2' looks good -> OK
    Do not exceed initial baking time for AZ otherwise becomes brittle
    5             reprocess
    6           spin absolutely perfect (no interferences) reprocess

     

    Test 2: focus on top show AZ is damaged. Bottom shows normal undercut (~ PMGI thickness)
    SF15-1500rpm_150°C_AZ_110°C_exp-47.5mJ_bake-120°C-3'_flood-427.5mJ_devMFCD26-2'05_2.JPG
    SF15-1500rpm_150°C_AZ_110°C_exp-47.5mJ_bake-120°C-3'_flood-427.5mJ_devMFCD26-2'05.JPG

    Test3: the fact the AZ was too baked rendered development inhomogeneous.
    Consequently, dev too much on patterns.
    test3_SF15-1500rpm_150°C_AZ_110°C_exp-47.5mJ_bake-125°C-4'30_flood-427.5mJ_devMFCD26-3'15.JPG

    NB: after test 3, observed mask from IEF (transferred) and found out it was shit!!! -> impossible to developp a process with this kind of mask!!.                                                         Right, after etching it 15" in Anne de Vismes Cr etch
    Mask ffrom IEF!!!.JPGMask ffrom IEF_add15''-Cr-etch.JPG

    Test 4 done with CPBv2 mask layer 3 (should have done with mask layer 2 to have a chance to see interferences)
    Problems:
    - Patterns are cleared, but see small residues on the bottom. Ozone plasma 100W 200µb for 2 min -> no effect, exactly the same before and after.
    - Small cracks all over AZ, probably because layers were too much baked (PMGI was baked 17', and AZ was baked 4')
    -> DO NOT EXCEED BAKING TIMES (MOSTLY FOR AZ) OTHERWISE RESIST BECOMES BRITTLE
    test4_SF15-1500rpm_150°C_AZ_110°C_exp-47.5mJ_bake-120°C-4'_flood-427.5mJ_devMFCD26-2'_residues.JPGtest4_SF15-1500rpm_150°C_AZ_110°C_exp-47.5mJ_bake-120°C-4'_flood-427.5mJ_devMFCD26-2'_cracks.JPG

    I had no specific trouble on tests with this process, though when I try it on BPCT8 and BPCT9, the PMGI layer unsticked, and developer ran below the resist over large distances.
    As I already saw on BPCv1, this issue is solved only by baking PMGI harder. Maybe TI prime could improve a bit.
    I will do one more try with TI prime, but otherwise, PMGI/AZ bilayer is close to be abandonned.

    LOR20B - AZ development time

    • Procedure
    spin LOR20B as above (same as SF15, same thickness)
    bake 5" @ 110°C -> bake 5' @ 180°C
    spin AZ5214E 4krpm
    bake 1' @ 110°C
    exp dose 5" @ 9.5mW/cm2 (47.5mJ/cm2)
    bake xx @ 120°C
    flood exp 45" @ 9.5mW/cm2
    dev MFCD26 @ 21.2°C

    Tests: (15/03/2016)

    wafer exp bake development comments
    red AZ
    start
    interf start
    min  ss
    interf stop
    min  ss
    spin, dev obs + conclusion
    1 47.5 120°C, 3'       µm - µm (edges)
    fresh dev
     

     

     

    PMGI SF15 - LOR20B - AZ5214 development time in AZ developer

    21/03/16

    I want to check if it is possible to develop AZ5214 in AZ Developer which does not attack aluminium.

    • Check on AZ5214
    spin AZ5214E 4krpm
    bake 1' @ 110°C
    exp dose 5" @ 9.5mW/cm2 (47.5mJ/cm2)
    dev Az developer 1:2 HDI @ 21.2°C 
    

    Result: The resist does not leave after 8min... dose is not enough for a process without inversion.

    spin AZ5214E 4krpm
    bake 1' @ 110°C
    exp dose 45" @ 9.5mW/cm2 (47.5mJ/cm2)
    1- dev Az developer 1:2 HDI @ 21.2°C 
    

    Result

    wafer exp bake development comments
    red AZ
    start
    interf start
    min  ss
    interf stop
    min  ss
    spin, dev obs + conclusion
    1 flood 120°C, 3'   29" 1'    

     

    • Check on AZ5214 inversed
    spin AZ5214E 4krpm
    bake 1' @ 110°C
    exp dose 5" @ 9.5mW/cm2 (47.5mJ/cm2) IEF mask
    bake 3min @ 120°C
    flood exp 45" @ 9.5mW/cm2
    2-exp dose 5" @ 9.5mW/cm2 (47.5mJ/cm2) IEF mask
    bake 3min @ 120°C
    flood exp 45" @ 9.5mW/cm2
    dev Az developer 1:2 HDI @ 21.2°C 
    
    3- exp dose 4" @ 9.5mW/cm2 (47.5mJ/cm2) IEF mask
    bake 3min @ 120°C
    flood exp 45" @ 9.5mW/cm2
    dev Az developer 1:2 HDI @ 21.2°C 
    
    Result
    wafer exp bake development comments
    red AZ
    start
    interf start
    min  ss
    interf stop
    min  ss
    spin, dev obs + conclusion
    2 47.5 120°C, 3' 10" 29" 1'20"    
    3 36.0 120°C, 3' 12" 25" 1'15"    

     

    LithoAZ-devAZdeveloper-test-summary.jpg

    I think that to assure a good development the best 1min50sec

    • Check on PMGI SF15

    The first thing to know is how long it takes for the PMGI to leave in the AZ Developer after being baked at a temperature X for 5min 

    -----After first tests with LOR20B it could be concluded that AZ developer has no effect on LOR and PMGI resists.

    • Check on LOR20B

    wafer Si/SiO2 standard
    bake the wafer @ 110°C for water removal
    tape the wafer on blue clean room tape, cut to a ~3" size
    dispense 1-1.5mL resist slowly from a pipette (well centered on wafer)
    2" @ 300rpm acc 250rpm/s
    3" @ 800rpm acc 500rpm/s
    60" @ 1500rpm acc 500rpm/s
    Cut the edges of the spun resist on all sides of the wafer before untaping
    bake 5' @ XX °C
    develop in AZ Developer 1:2 HDI  until end of intereferences

    Results NO EFFECT

    • LOR20B+AZ5214 Mask

    I decide to spin AZ5214 on the waffers with LOR to do a two-steps development process. Develop AZ in AZ developer to get a good mask and then, develop LOR in MIF726 using the times well stablished by HLS.

    spin AZ5214 60" @ 4000rpm
    bake 1min @110deg
    expo 5" IEF mask
    bake 3min @120deg
    flood expo 45"
    develop in AZ Developer 1:2 HDI until end of intereferences + obs
    develop in MF726 until end of intereferences

     

    temperature
    °C

    AZ developer

    turn blue

    interf start

    interf end MF726- interf start interf stop comment
    170 15" 35" not observed - ended at 2min 46" 1min18"  
    180 21" 40" not observed - ended at 2min 58" 1min25"-1min40" inhomogen. first inthe center
    190 20" 40" idem 1min 1min 45"  
    200 20" 1min idem 1min10sec 2min06sec  

     

    In all cases, the undercut is very large!

    Two-step-development-test-summary-small.jpg

    21/03/16

    I want to check if it is possible to develop AZ5214 in AZ Developer which does not attack aluminium.Two-step-development-test-summary2-small.jpg

    22?/03/16

     

    I want to check if it is possible to etch the LOR resist with plasma oxigen.

    • Check Plasma O2 on LOR20B

    wafer Si/SiO2 standard
    bake the wafer @ 110°C for water removal
    tape the wafer on blue clean room tape, cut to a ~3" size
    dispense 1-1.5mL resist slowly from a pipette (well centered on wafer)
    2" @ 300rpm acc 250rpm/s
    3" @ 800rpm acc 500rpm/s
    60" @ 1500rpm acc 500rpm/s
    Cut the edges of the spun resist on all sides of the wafer before untaping
    bake 5' @ 170°C
    

    Results PUT RESULTS

     

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