Tuesday, October 18, 2022, 13:52

38 pieces of samples made of TiO2/C/PVP loaded into a target boat wrapped with 2 layers of Ta-heat shield.

Samples will be heated to 1700, 1800, 1900, and 2000 C

Some of the pieces will be removed after each target temperature 

Target chamber has been pumping down and the current pressure reading is 6.62e-6 T

 Tuesday, October 18, 2022, 14:12

TGHT will be autoramped to 250 A

Good vacuum: 3e-5 Torr

Bad vacuum: 5e-5 Torr

Omega slope: 0.99

Initiate autoramp: 1 A/min

Hannah Toy wrote:

Tuesday, October 18, 2022, 13:52 38 pieces of samples made of TiO2/C/PVP loaded into a target boat wrapped with 2 layers of Ta-heat shield. Samples will be heated to 1700, 1800, 1900, and 2000 C Some of the pieces will be removed after each target temperature  Target chamber has been pumping down and the current pressure reading is 6.62e-6 T  Tuesday, October 18, 2022, 14:12 TGHT will be autoramped to 250 A Good vacuum: 3e-5 Torr Bad vacuum: 5e-5 Torr Omega slope: 0.99 Initiate autoramp: 1 A/min

 Wednesday, October 19, 2022, 09:42

TGHT has reached to 250A/3.95V, Temp at ~1100 C.  (The archiver is currently not working; already contacted Control to look into it.)

Pressure reached below 4.9 e-7 Torr. 

Auto-ramp to 300 A at 2A/min.  Continue to monitor.

 Wednesday, October 19, 2022, 10:24

TGHT reached to 300 A/4.89V.  Temp at 1206 C. 

Pressure went up slightly and came down after the TGHT setpoint was reached, see attachment#1.

Continue to auto-ramp to 350A at 2A/min.

 Wednesday, October 19, 2022, 11:35

TGHT reached to 350A/5.8V.  Temp at 1360C.

Pressure reached above 1e-6 Torr and came down after TGHT reached the setpoint. 

Continue to auto-ramp to 400 A at 2A/min

 Wednesday, October 19, 2022, 11:57

TGHT reached to 400 A/6.89V.  Temp at 1485C.

Pressure went up to 3.3e-6 Torr and came down after TGHT reached the setpoint,  see attachment#2.

A temp vs current plot has been generated (see shared folder \Hannah\) - est TGHT 480A to reach 1700 (T1).

Auto-ramp to 420 at 1A/min.  Continue to monitor closely...

 Wednesday, October 19, 2022, 13:01

TGHT reached 420A/7.23V, Temp at 1520 C.

Continue auto-ramping to 440A at 1A/min.

 Wednesday, October 19, 2022, 13:42

TGHT reached 440A/7.65V.  Temp at 1572 C

Continue auto-ramping to 460A at 1A/min.

Wednesday, October 19, 2022, 14:10

TGHT reached to 460A/8.10 V.  Temp at 1628 C.

Tapping up TGHT to reach 1700 C

 Wednesday, October 19, 2022, 15:33

TGHT was tapped up to 474A, Temp reached to 1700 C since 14:30.

Pressure is slowing coming down, currently at 1.4 e-6 Torr.

Will hold at this target current for a few hours.

 Wednesday, October 19, 2022, 16:58

Temp went up slightly to 1713 C as the pressure is coming down. 

Lower TGHT to 468A/8.45V to maintain the temp at 1700 C.

 Wednesday, October 19, 2022, 19:55

Temp went up again to 1716 C, but this time the pressure also went up, see attachment#3.  Not sure why the target got hotter... the voltage seems normal and consistent. 

Lower TGHT to 462A/8.44V to maintain at 1700 C. 

Continue monitoring...

 Wednesday, October 19, 2022, 22:56

Temp went up another 10 C, to 1710 C, TGHT is holding at 462 A/8.48V.  Notice the TGHT current readback is fluctuating between 458A - 463 A. 

Initiated cooling.. 2A/min

 Friday, October 21, 2022, 08:55

 All the samples were taken out from the Evap on Thursday Oct 20.  We decided to do so because there was not enough sample in each batch for XRD analysis.  All the sample will be analyzed as treated at 1700 C. 

See attachement #$ for the overall TGHT/Vac plot.

Tuesday, October 25, 2022, 12:18

Container wrapped in 4 Ta foil heatshields

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= 230A

Final TGHT current= ~420A (adjustable)

Heating autoramp started at 2A/min on both TGHT and TBHT to40A

Then at 1A/min on both heaters to 120A.

Good vacuum = 5.0 e-04 Torr

Bad vacuum = 5.0E-02 Torr

Wednesday, October 26, 2022, 07:07

IGP1= 7.5e-7 Torr

start ramp at 2A/min to 40A

Ramped at 1A/min to 120A then held until pressure drop.  Then ramped @ 4A/min to 400A on TGHT.

Wednesday, October 26, 2022, 14:09 

Manually rampted TGHT to 415A, 6.9V will hold for 4 hours 

OMEGA reads 1870 C initially

Thursday, October 27, 2022, 09:44

was held for 5 hours due to technical issues but should be ok.

OMEGA @ time of rampdown = 1830C

Rampdown @-2A/min TGHT and -1A/min TBHT

IGP1= 3.5e-07 Torr

Friday, October 28, 2022, 07:58

The coated container was wrapped in four Ta foil heatshields.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= 230A

Final TGHT current= ~420A (adjustable)

Heating autoramp starged at 4A/min on both TGHT and TBHT to 40A

Then at 1A/min on both heaters to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initial = 4.5e-07 Torr

Friday, October 28, 2022, 10:50

after reaching 120A and leaving until pressure drop, autoramp at 2.5A/30s (5A/min) towards 400A TGHT and 230A TBHT.

Friday, October 28, 2022, 11:22

OMEGA= 1890 @ 412A, 7.1 V on TGHT

Leaving for 4 hours

Tuesday, November 01, 2022, 17:24

2 samples of np-TiO2/C fibres were produced using the e-spinner.  Each sample was wrapped with a piece of graphite sheet, and then loaded into a target container. 

Sample will be heated to 1700 C.

TGHT will be autoramped to 450 A; this should be close to 1600 C. (see elog#596)

Good vacuum: 3e-5 Torr

Bad vacuum: 5e-5 Torr

Omega slope: 0.99

Initiate autoramp: 1 A/min

Chamber has been pumped down below 4.2e-6 Torr.

 Tuesday, November 01, 2022, 22:46

 Pressure currently at 6.4e-7 Torr.

Initiated auto-ramping

 Wednesday, November 02, 2022, 09:37

TGHT was ramped up to 448A (readback 445-452A / 8.05V - 8.11V).  The voltage is much higher than the last process, see elog #596.

Temperature is much higher at this current, reading at 1870 - 1872 C. 

Will keep at this setting for now and continue to monitor.

See attachment#1 for the TGHT-Pressure plot.

 Wednesday, November 02, 2022, 21:35

Samples have been heated for over 16 hours; temp has been stabilized at 1875 C, vacuum at 7.3 e-7 Torr. 

Initiated cooling at 1A/min.

Chamber will be vented tomorrow morning.

Monday, November 07, 2022, 14:24

The coated container tube was wrapped in four Ta foil heatshields.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final TGHT current= ~400A (adjustable)

Heating autoramp starged at 4A/min to 40A

Then at 1A/min on both heaters to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initial =

Thursday, November 10, 2022, 07:40

The coated container was wrapped in four Ta foil heatshields.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= 230A

Final TGHT current= ~400A (adjustable)

Heating autoramp starged at 4A/min on both TGHT and TBHT to 40A

Then at 1A/min on both heaters to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initial = 2.8e-07 Torr

Thursday, November 10, 2022, 10:31

 TGHT 230A 3.4V and TBHT at 230A , 3.9V

Continue ramp up for TGHT at 4A/min (2A/30s) to 380A

Thursday, November 10, 2022, 11:30

OMEGA =1886 C @ 430A, 7.1V TGHT; will leave for 4 hours

Thursday, November 10, 2022, 15:43

rampdown at -2A/min TGHT and -1A/min TBHT

Thursday, November 17, 2022, 08:11

The coated container was wrapped in four Ta foil heatshields.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= N/A

Final TGHT current= ~400A (adjustable)

Heating autoramp starged at 4A/min on  TGHT  40A

Then at 2A/min on both heaters to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initial = 2.7e-07 Torr

Thursday, November 17, 2022, 10:41

OMEGA=1897C at 358A, 6.0V

Will ramp down at 230 pm

Thursday, November 17, 2022, 14:34

starting rampdown at -2A/min

OMEGA reads 1865C and IGP1=7.6e-07 Torr

Friday, November 18, 2022, 15:08

The coated container was wrapped in four Ta foil heatshields.

Target temperature on OMEGA= 1860-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= 230A

Final TGHT current= ~400A (adjustable)

Heating autoramp starged at 4A/min on both TGHT and TBHT to 40A

Then at 2A/min on both heaters to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

leaving to pressure down over weekend

Sunday, November 20, 2022, 12:11

start heatup IGP1=1.63e-07 Torr

Sunday, November 20, 2022, 14:21

OMEGA= 1900 at 395A, 6.6V on TGHT

Will leave until 6;20 pm

Tuesday, November 22, 2022, 14:58

The coated container was wrapped in four Ta foil heatshields.

Target temperature on OMEGA= 1860-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= 230A

Final TGHT current= ~400A (adjustable)

Heating autoramp starged at 4A/min on both TGHT and TBHT to 40A

Then at 2A/min on both heaters to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

leaving to pressure down. 

 Wednesday, November 22, 2022, 19:10 

OMEGA = 1942 C @ 396A on TGHT

lowered to 386A to 1900 and left for 4 hours.

After four hours, started rampdown at-2A/min TGHT and -1A/min TBHT

Thursday, November 24, 2022, 11:01

Target container contains one disc of e-spun TiO2/PAN fibrous disc, (Ref sample P-134).

Sample will be heated to 1875C, similar to the previous process, see e-log ID#599.

TGHT will be autoramped to 350 A and monitor the conditions before ramping up further.

Good vacuum: 3e-5 Torr

Bad vacuum: 5e-5 Torr

Omega slope: 0.99

Initiate autoramp: 1 A/min

Chamber has been pumped down below 5.0e-6 Torr.

 Friday, November 25, 2022, 08:38

TGHT reached to 348A/5.8V; temp is holding at 1600 C since 19:00 yesterday, see attachment#1.

Stepping up TGHT to 400A and continue to monitor.

 Friday, November 25, 2022, 09:45

TGHT reached to 400A/6.8V; temp holding at 1758C.  Pressure coming down from 6.6e-7 Torr.

Ramping up to 410A.

 Friday, November 25, 2022, 12:28

TGHT reached 410A/7.08V.  temp holding at 1790 C.  Pressure coming down from 6.9e-7 Torr. 

Ramping up to 430A.

 Friday, November 25, 2022, 13:01

TGHT reached 430A/7.4V. Temp holding at 1837 C.  Pressure coming down from 7.73e-7 Torr.

Ramping up to 440A.

 Friday, November 25, 2022, 13:50

TGHT reached to 440A/7.6V.  Temp holding at 1864C.  Tapping TGHT to 444A (readback 443A - 449 A)/7.7V. 

Desired Temp has reached, 1875 C.  Will continue to hold on this temp over the weekend.

 Sunday, November 27, 2022, 21:14

TGHT has been holding at 442A (lowered by 2 A on Fri to maintain 1875C).  Temp increased to 1887C.  Pressure at 2.5e-7 Torr. 

See attachment#2 for plots/temp. 

Initiated cooling at 1A/min.

Friday, December 02, 2022, 09:46

297 graphite discs packed into a Ta tube wrapped in four heatshields.

Good vacuum 5.0e-04 Torr

Bad vacuum 5.0 e-02 Torr

Will be conditioned @ 2000 C for 5 hours and then for one hour at 10A greater than final current.  Final current will be calculated from

regression.

 IGP1= 5.7 e-07 Torr

ramping to 40A @ 2A/min TGHT

Friday, December 02, 2022, 20:59

Was ramped to 320A but the window must be coated because Temperature readings are drastically off. Will cool down and repeat on Monday after cleaning window.  Will ramp down at -2A/min

OMEGA= 1360 C, expect much higher.

Tuesday, December 06, 2022, 10:58

ramp started at 4A/min .  Initial pressure was 2.6 e-07 Torr

Tuesday, December 06, 2022, 12:45

OMEGA readings low (1290 @ 331A, 5.6V )

Will tap up until pressure bump observed.

Tuesday, December 06, 2022, 13:04

 Pressure bump observed around 440 A, 7.9 V

IGP1= 8.4 e-06 Torr. 

Current stopped and will keep at this current for 10 hours (11 pm rampdown)

Tuesday, December 06, 2022, 13:24

Ramped to 500A, Will leave at 500A for the rest of the conditioning.

Tuesday, December 06, 2022, 23:05

Starting rampdown at -2A/min

IGP1= 4.9e-07 Torr

TGHT= 500A, 9.3V

Wednesday, December 07, 2022, 09:43

Dismounting today.

IGP1 final = 9.6e-08 Torr

Wednesday, December 07, 2022, 13:29

Reinstalled in the evaporator.  Window was not shaded.  Will try heating to 500A once more.

ramp at 6A/min

4 TaC coated springs and 4 Tac coated caps loaded into a target boat.

Target boat wrapped in 4 Ta heatshields

Target boat type was with endcaps at both ends.

Left in Evap2 over previous night to depressurize.

Target temperature= 1850-1900C for 4 hours

Good vacuum = 5e-04 Torr

Bad vacuum = 5e-02 Torr

Friday, December 16, 2022, 10:01

Heated @1A/min to 100A on TGHT

Then heated 2A/min to 120A

Friday, December 16, 2022, 10:08

started autoramp @4A/min  to 300A

Friday, December 16, 2022, 11:15

TGHT=450 A, 7.6 V

OMEGA= 1863 C

IGP1= 7.2e-06 Torr

Will keep for 4 hours

Monday, December 19, 2022, 10:30

Sintering was perfect.  Repeat same configuration next time.

Thursday, February 09, 2023, 09:47

Target boat with a layer of niobium foil on the bottom is used to heat up Nb samples to 1400 C for 4 hrs.

The niobium samples are wrapped in a Nb foil.

Boat is wrapped with 2 layers of Ta foil, careful to avoid touching samples.

Samples left in Evap2 overnight (pumping down).

Good vacuum = 5.0e-04 Torr

Bad vacuum = 5.0e-02 Torr

Thursday, February 09, 2023, 09:48

IGP1= 6.19e-07 Torr

Autoramping to 100A @1A/min

Thursday, February 09, 2023, 09:57

Vacuum stable. ramp at 6A/min to 50 A instead

Thursday, February 09, 2023, 10:09

ramping at 2A/min to 100A

Thursday, February 09, 2023, 11:29

1400C on OMEGA reached @ 341A, 5.5V  Will stop and watch until stable

Thursday, February 09, 2023, 15:29

OMEGA= 1408 C

IGP1= 7.97e-07 Torr

Start rampdown @ -1A/min

Thursday, February 23, 2023, 18:20

Ta HP-FEBIAD was coated with TaC and wrapped with Ta heat-shields (3 layers) and 1 under layer that doesn't cover the middle section.

Desired temperature = 1800 C , TBHT will be set fixed at 230A (max).

Evap 2 will be pumped down to 5e-06 Torr range

OMEGA slope= 0.990

Good vacuum = 5.00 e-4 Torr

Bad vacuum = 5.00 e-2 Torr

IGP1=2.5 e-06 Torr

Start autoramp @1A/min to 80 A then autoramp heat @1A/min to 150 A.  Then autoramp TGHT to approx 675A and TBHT to 230A.1

Friday, February 24, 2023, 09:10

heated overnight @0.5 A/min to 400 A.  Then started heating at 1A/min to 600 A while taking readings for current/Temp regression.

regression so far points to 682A to get to 1800C.  Will continue taking readings and possible heat to 1850 C. 

Friday, February 24, 2023, 09:43

autoramping to 690A at 1A/min

Friday, February 24, 2023, 11:24

ramping manually to 690A from 650A

Friday, February 24, 2023, 11:32

4 hours at 330pm

TGHT 492A, 10.6V

TBHT = 230A, 3.2V

IGP1=5.11e-06 Torr

OMEGA =1840 C

Friday, February 24, 2023, 15:36

TGHT = 692A, 10.6V

TBHT = 230 A, 3.2V

OMEGA = 1835 C

IGP1= 2.4e-06 Torr

Starting rampdown at -2A/min TGHT and -1A/min TBHT

Tuesday, February 28, 2023, 07:19

Ta LP-FEBIAD was coated with TaC and wrapped with Ta heat-shields (4 layers)

Desired temperature = 1850 C , TBHT will be set fixed at 230A (max).

Evap 2 will be pumped down over previous night

OMEGA slope= 0.990

Good vacuum = 5.00 e-4 Torr

Bad vacuum = 5.00 e-2 Torr

IGP1= 1.2 e-06 Torr

Start autoramp @1A/min to 80 A then autoramp heat @1A/min to 150 A.  Then autoramp TGHT to 400 A and TBHT to 230A.1

Tuesday, February 28, 2023, 15:39

Will ramp to 426A to 1850C as per regression line. 

Tuesday, February 28, 2023, 15:57

Will start cooling at 8 pm

OMEGA= 1858 C

IGP1= 2.12e-06 Torr

TGHT =426 A, 7.5 V

TBHT = 230 A, 3.2 V

Tuesday, February 28, 2023, 19:58

OMEGA = 1858 C

IGP1 = 1.04e-06 Torr

TGHT =426 A, 7.6 V

TBHT = 230 A, 3.2 V

rampdown TGHT at -2A/min and TBHT @ -1A/min

Wednesday, March 01, 2023, 21:46

Ta HP-SIS was coated with TaC and wrapped with Ta heat-shields (3 layers + 1 inner layer around fins)

Desired temperature = 1850 C , TBHT will be set fixed at 230A (max).

Evap 2 will be pumped down over previous night

OMEGA slope= 0.990

Good vacuum = 5.00 e-4 Torr

Bad vacuum = 5.00 e-2 Torr

IGP1= 5.7 e-07 Torr

Start autoramp @1A/min to 500 A on TGHT and 230A TBHT. 

Thursday, March 02, 2023, 10:10

ramping to 600A on TGHT @ 2A/30s, TBHT at 230A, 3.2V

Thursday, March 02, 2023, 11:22

At 11 am reached 1800s C and 1851C @1120 am. 

TGHT = 690 A, 10.5V

TBHT = 230 A, 3.3V

Cool down to start at 3 pm

Saturday, March 04, 2023, 08:29

Ta LP-FEBIAD with 369 discs plus 5 removable discs wrapped with 3 Ta heat-shields (in layers)

Evap 2 will be pumped down over previous night

Desired temperature = 1500 C as in Elog #52 , TGHT will be ramped up to 300 A and then adjusted manually to 1500C if temperature readings are ok

otherwise will use plot from coating sintering to approximate 1500C.

TBHT will be set fixed at 230A (max).

Good vacuum = 5.00 e-4 Torr

Bad vacuum = 5.00 e-2 Torr

IGP1= 3.4 e-07 Torr

Start autoramp @2A/min to 80 A then autoramp heat @1A/min to 230 A (both TGHT and TBHT)

  Then autoramp TGHT to 300 A

-

Saturday, March 04, 2023, 22:27

At 332 A, 5.6V on TGHT, 230 A, 3.3 V TBHT

OMEGA = 1370 C

Will autoramp to 375A on TGHT @0.25A/min then leave for 4 hours at 1500C

Cooling should start at 6 am march 5th

OMEGA reading 1498 @ 2 am

Sunday, March 05, 2023, 06:03

OMEGA reading 1442 C @550am

ramped up to 394 A on TGHT and OMEGA reads 1500 C

will leave for 40 minutes than test ramp up to observe outgassing

d until 715 am then begin rampdown.

Sunday, March 05, 2023, 07:22

ramped to 425 to test further outgassing temperature increase observed but only while increasing current.

OMEGA = 1590 C

TGHT= 425A, 7.6V

TBHT= 230A, 3.3V

IGP1=2.0e-06 Torr

ramping down @-2A/min on TGHT and -1A/min TBHT

Monday, March 06, 2023, 21:29

Total number of foils:382 ( including 5 analysis discs on the right side of the container)

Total length packed 17 cm (excluding 5 analysis discs that will be removed)

container has 4 Ta heat shields (one inner only around fins)

No endcaps inserted to facilitate out-gassing

Ta coated spring at  both ends

ramp to 500A @ 1A/min TGHT and to 230A on TBHT

max approx 700A on TGHT and 230A on TBHT (Omega slope set = 0.990)

Then temperature = 1800C

TBHT will be set fixed at 230 A (max).  TBHT heated manually and automatically to max.

Good vac at 5.00 e -4 Torr

Bad vac at 5.00 e-2 Torr

 IGP1= 3e-06 Torr at start of initial ramp.

Tuesday, March 07, 2023, 07:23

IGP1= 1.2e-05 Torr

OMEGA = 1288 C

Tuesday, March 07, 2023, 10:01

Will ramp to 715 A and keep there for 4 hours.  OMEGA readings not reliable beyond this point due to coating on EVAP2 window.

Tuesday, March 07, 2023, 11:10

TGHT = 715A, 11.0V

TBHT = 230A, 3.2V

OMEGA = 1750 C (but not reliable)

Maintaining for 4 hours then will ramp down @ -2A/min TGHT and -1A/min TBHT

Wednesday, March 08, 2023, 07:27

Final IGP1= 1.3e-07 Torr (before shutting down pumps)

Thursday, March 09, 2023, 06:53

2 TaC coated springs and  12 Tac coated caps loaded into a target boat (in packs of 4 wrapped in graphite foil).

Target boat wrapped in 4 Ta heatshields

Target boat type was with endcaps at both ends.

Left in Evap2 over previous night to depressurize.

Target temperature= 1850-1900C for 4 hours

Good vacuum = 5e-04 Torr

Bad vacuum = 5e-02 Torr

Start autoramp at 2A/min to 50A on  TGHT

 Thursday, March 09, 2023, 07:22

at 44A switched ramping rate to 1A/min to 120 A

Thursday, March 09, 2023, 09:53

ramping at 4A/min (2A/30s) to 400A

IGP1= 9.9e-07 Torr

Thursday, March 09, 2023, 11:26

1130 am  reaching 425A on TGHT 

1850 C OMEGA

Thursday, March 09, 2023, 15:37

TGHT 425 A, 7.1V

OMEGA = 1850 C

Starting rampdown @ -2A/min

endcaps and spring looked really good.