Previous TP would only spin up to 4KRPM. New TP installed.

Monday, June 05, 2023, 14:50: Roughing. 

Monday, June 05, 2023, 15:10: Controller reset. TP on. 

Thursday, June 08, 2023, 09:28

Using smaller particle size TaC no ball mill procedure.

Loaded 2 TaC coated end caps and 1 TaC coated springs.

OMEGA Slope 0.99

Will heat to 1850-1900 C and hold for 4 hours

Good Vac = 5.0e-4 Torr

Bad Vac= 5.0 e-02 Torr

 Initial IGP1= 4.07E-06 Torr

Thursday, June 08, 2023, 10:36

ramped @ 2A/min to 100A.  Then after pressure stabilized starting ramp at 4A/min (2A/30s) to 400A

Thursday, June 08, 2023, 12:24

reached 1850 C with Set current = 480 and RD current = 470.6A, V = 7.7

Will leave for 4 hours.

Thursday, June 08, 2023, 15:31

ramping down at -2A/min (-1A/30s)

Monday, January 29, 2024, 16:36

LP FEBIAD

wrapped in 4 Ta heatshields.

Will heat at 2A/min to 95A on TGHT and TBHT

Then will heat at 3A/min to 1800 C ~400A on TGHT and 230A on TBHT

Monday, January 29, 2024, 16:45

Initial IGP1= 5e-05 Torr

Monday, January 29, 2024, 20:35

1800C was at TGHT 410A, 6.9V  RD and set current 418A

TBHT= 233 RD A, 3.2V

Wednesday, February 21, 2024, 06:22

Ta container tube, wrapped in 4 Ta foil heat-shields, and loaded with 201 D shaped discs in a 12mm graphite cartridge with usable 11mm

conditioning tube WO = 44692-13

End-caps on the graphite cartridge have holes for outgassing.  One spring each end in the Ta container

initial heating @ 2A/min to 90 A then 1A/min to 120A TGHT

OMEGA slope = 0.99

Vacuum limits up to 400A: 5.0e-04 Torr -- 1.0e-02 Torr

Wednesday, February 21, 2024, 09:12

IGP1 initial = 9e-07 Torr

Starte at 3A/min to 90A

Wednesday, February 21, 2024, 09:21

increased autoramp to 4 A/min until pressure starts rising, then will slow down or pause

Wednesday, February 21, 2024, 09:32

At 74A, paused.  Will continue at 2A/min TGHT

Wednesday, February 21, 2024, 09:40

Pausing at 87A. 

Wednesday, February 21, 2024, 10:34

pressure dropping.  restarting ramp up to 120A at 2A/min

Wednesday, February 21, 2024, 10:37

From previous TiC 220206, will heat up fast until 250A and then at 1A/min until 300A to better resolve out-gassing profile

Wednesday, February 21, 2024, 12:05

Changed ramp to 1A/min to 300A

Wednesday, February 21, 2024, 13:10

Manually ramped up for a while

increased ramp speed to 2A/min

regression line started to match previous one after 1300C

Wednesday, February 21, 2024, 13:16

increased ramp rate to 4A/min to 420A

Wednesday, February 21, 2024, 13:37

Note: the temperature became unrealistic.  suspect window condensate.  Will use regression and to to 441A

Wednesday, February 21, 2024, 13:54

reached 441A, 7.6V

leaving for 3.5 hours or when pressure drops to 2-3 e-06 Torr

Wednesday, February 21, 2024, 18:56

IGP1=2.9e-06 Torr

starting rampdown at -2A/min

Thursday, February 29, 2024, 07:40

Ta container tube, wrapped in 4 Ta foil heat-shields, and loaded with _________ D shaped discs in a 12mm graphite cartridge with usable 11mm

conditioning tube WO = 44692-13

End-caps on the graphite cartridge have holes for outgassing.  One spring each end in the Ta container

initial heating @ 2A/min to 85 A then 2A/min to 120A TGHT

OMEGA slope = 0.99

Vacuum limits up to 400A: 5.0e-04 Torr -- 1.0e-02 Torr

Thursday, February 29, 2024, 07:43

Initial IGP1=  9.31e-7 Torr

Thursday, February 29, 2024, 17:43

Temperature profile suggests 1900 C at 400A.  Now at 400A.  Will keep at this current for 4 hours.

manually ramped the last few amps.

TGHT= 400A, 7.3 V OMEGA = 1901C

Thursday, February 29, 2024, 22:20

IGP1=2.1e-6 Torr

started ramping down at -2A/min

Wednesday, April 03, 2024, 06:46

Ta container tube, wrapped in 4 Ta foil heat-shields, and loaded with _________ D shaped discs in a 12mm graphite cartridge with usable 11mm

conditioning tube WO = 44692-13

End-caps on the graphite cartridge have holes for outgassing.  One spring each end in the Ta container

initial heating @ 2A/min to 85 A then 2A/min to 120A TGHT

OMEGA slope = 0.99

Vacuum limits up to 400A: 5.0e-04 Torr -- 1.0e-02 Torr

Wednesday, April 03, 2024, 06:49

initial IGP1= 1.28e-06 Torr

Wednesday, April 03, 2024, 09:26

IGP1= 2.3e-05 Torr

TGHT = 78 A, 1.3V

Will continue ramp as planned.

Wednesday, April 03, 2024, 11:37

Ramping at 2A./min to 400A

Wednesday, April 03, 2024, 14:01

expected 1900C at 401A

leaving at 402A for 4 hours.  Rampdown start at 4:10 pm at -2A/min

Thursday, April 04, 2024, 12:06

Ta container tube, wrapped in 4 Ta foil heat-shields, and loaded with _________ D shaped discs in a 12mm graphite cartridge with usable 11mm

conditioning tube WO = 44692-13 (4th conditioning with this tube)

End-caps on the graphite cartridge have holes for outgassing.  One spring each end in the Ta container

initial heating @ 2A/min to 85 A then 2A/min to 120A TGHT

OMEGA slope = 0.99

Vacuum limits up to 400A: 5.0e-04 Torr -- 1.0e-02 Torr

Mas current~400A (1900 C)

Friday, April 05, 2024, 09:04  

Ramping to 85A done and pressure trending down.  Will continue ramp to 120A

Friday, April 05, 2024, 16:01

Starting rampdown at -2A/min

IGP1= 3.2e-06 Torr

Tuesday, May 07, 2024, 06:16

TP was swapped on previous day (May 6th)

protective screen installed.

Loaded 9 TaC coated end caps (groups of 4 and 5) and 2 TaC coated springs.

OMEGA Slope 0.99

Will heat to 1850-1900 C and hold for 4 hours

Good Vac = 5.0e-4 Torr

Bad Vac= 5.0 e-02 Torr

 Initial IGP1=6.7E-07 Torr

Monday, May 27, 2024, 07:09

Small graphite cartridge was loaded with SiC discs 240523-1 and 240523-2.  Discs produced without milling using PAA as a dispersant.

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

two Tac Coated springs at the ends in case plugs are pushed outwards.

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 2A/min to 90 A

Then at 2A/min to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initial 4.8e-07 Torr

Monday, May 27, 2024, 09:13

Pressure started coming down.  Heat at 2A/min to 120A.

Monday, May 27, 2024, 10:21

Started ramp 2A/30s  to 400A will monitor temperature

stopped at 490A and will hold for 4  hours. 

Monday, May 27, 2024, 12:41

temperature started creeping up past 1870C so decreased current to 461A

Current temperature is 1842 C at 461A, 7.6V

Monday, May 27, 2024, 12:55

dropped current to 441 because temperature climbed to 1899 C

Monday, May 27, 2024, 15:08

final pressure IGP1 =9.9 e-07 Torr

OMEGA= 1830 C at 410 A (reduced as needed)

Start rampdown at -2A/min

Wednesday, May 29, 2024, 10:07

Final pressure is 2.7e-7 Torr

Wednesday, May 29, 2024, 14:42

Experiment failed.  Too hot probably.  Bad temperature readings.  Will repeat after redesigning experiment.

Wednesday, May 29, 2024, 22:52

Small graphite cartridge was loaded with SiC discs 240523-1 and 240523-2 and 220727-2 (baseline discs).  Test Discs produced without milling using PAA as a dispersant.

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

two Tac Coated springs at the ends in case plugs are pushed outwards.

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 2A/min to 90 A

Then at 2A/min to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initial 4.8e-07 Torr

Wednesday, May 29, 2024, 22:54

Kept at 400 A for 4 hours. 

Starting autoramp down at -2A/min

Wednesday, June 05, 2024, 07:14

SiC discs loaded into tantalum tube.  New mixing (two types) and old mixing.

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

Tac Coated springs at the ends in case plugs are pushed outwards.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:=* 0.980*

Target time at max temperature = 4 hours

Final TGHT current= ~400A (adjustable)

Heating autoramp 1A/min to 90 A

Then at 2A/min to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

 IGP1 initia1.3e-06Torr

Wednesday, June 05, 2024, 11:04

Continuing to ramp at 2A/min to 350A

Wednesday, June 05, 2024, 12:22

Leaving at 369 A for 4 hours (until 4 pm).  Temperature readings do not appear good.

Wednesday, June 05, 2024, 16:01

Start rampdown at -2A/min

IGP1=2.0 e-6 Torr

 Thursday, July 25, 2024, 15:18

Target container consists of two np-Ta fibres disk samples. Both disks are made from heat stabilized np-Ta fibres (150 C for 17 hours) and were pressed at 8 tons / 300 MPa.

Sample 1 was made from np-Ta fibres spun using Dope solution #1. Sample 1 disk has an average thickness of 0.727 mm and a diameter of 17.113 mm. Mass of the green sample 1 disk is 0.1957 g. 

Sample 2 was made from np-Ta fibres spun using Dope solution #6. Sample 2 disk has an average thickness of 0.688 mm and a diameter of 17.123 mm. Mass of the heat stabilized fibres used to make the green sample 2 disk is 0.1860 g. Mass loss from pressing the heat stabilized fibres was virtually zero. Therefore, although the mass of the green sample 2 disk was not measured, it can be extrapolated to be 0.1860 g. 

Target container was wrapped with Ta foil. Each sample disk was wrapped in graphite foil and placed inside the target container horizontally near the center. 

Omega slope was initially set to 0.980. After reviewing previous logbook on np-Ti (e-log ID#633), changed the Omega slope to 0.990. 

Chamber is currently being pumped down. The current reading (as of 15:40) is 4.70e-05 Torr. 

Two heating schedules will be tested. Heating schedule 1 entails heating both sample disks at ~1000 C until the pressure reaches below 1.00e-06 Torr. Once heating schedule 1 is completed, sample 1 will be removed. Heating schedule 2 entails heating sample 2 to ~1800 C until the pressure reaches below 1.00e-06 Torr. TGHT is estimated to be approximately 440A/7.6V to reach 1875 C (348A/5.8V to hold temperature at 1600 C). Refer to e-log ID#605. 

Angelina Chen wrote:

Thursday, July 25, 2024, 15:18 Target container consists of two np-Ta fibres disk samples. Both disks are made from heat stabilized np-Ta fibres (150 C for 17 hours) and were pressed at 8 tons / 300 MPa. Sample 1 was made from np-Ta fibres spun using Dope solution #1. The sample 1 disk has an average thickness of 0.727 mm and a diameter of 17.113 mm. The mass of the green sample 1 disk is 0.1957 g.  Sample 2 was made from np-Ta fibres spun using Dope solution #6. The sample 2 disk has an average thickness of 0.688 mm and a diameter of 17.123 mm. The mass of the heat stabilized fibres used to make the green sample 2 disk is 0.1860 g. The mass loss from pressing the heat stabilized fibres was virtually zero. Therefore, while the mass of the green sample 2 disk was not measured, it can be extrapolated to be 0.1860 g.  The target container was wrapped with Ta foil. Each sample disk was wrapped in graphite foil and placed inside the target container horizontally near the center.  The Omega slope was initially set to 0.980. After reviewing previous logbook on np-Ti The chamber is currently being pumped down. The current reading (as of 15:40) is 4.70e-05 Torr.  Two heating schedules will be tested. Heating schedule 1 entails heating both sample disks at ~1000 C until the pressure reaches below 1.00e-06 Torr. Once heating schedule 1 is completed, sample 1 will be removed. Heating schedule 2 entails heating sample 2 to ~1800 C until the pressure reaches below 1.00e-06 Torr. TGHT is estimated to be approximately 440A/7.6V to reach 1875 C (348A/5.8V to hold temperature at 1600 C). Refer to e-log ID#605.

 Friday, July 26, 2024, 09:52

Chamber has been pumped down overnight, pressure currently at 1e-6 Torr.

Initiate auto ramping 1A/min to reach 200 A. 

Good vac = 3 e-5 Torr

Bad vac = 5 e-5 Torr. 

Continue to monitor.

 Friday, July 26, 2024, 17:06

Gas evolution has seen observed to be completed as TGHT slowly ramping up.  Temp is currently reading at 1015 C, TGHT 164A/2.43V.  Pressure holding at 2.4e-6 Torr but slowly coming down, see attachment 1.  Will keep this setting and cool it down on Sunday.

 Sunday, July 28, 2024, 11:27

Temperature has been holding sturdy at ~1000C for over 36 hours, TGHT at 164A/2.59V (a slight increase in the voltage).  Pressure is currentlyat 4.5e-7 Torr (see attachment #2 for the archiver).

Ramping down TGHT at 1A/min. 

Will remove both samples on Monday to measure the mass loss.  Sample 1 will be analyzed.  Sample 2 will be loaded back to the Evap 2 for further heating to reach about 1800 C.

 Monday, July 29, 2024, 14:29

Both samples were removed from the chamber and measured for weight loss, and Sample 2 was put back for further heating; Thanks Darwin for helping up with this. 

Chamber is currently pump down, pressure at 6.0e-5 Torr. Will ramp up TGHT once the pressure has come down to 10e-6 Torr. 

 Monday, July 29, 2024, 16:52

Pressure at 6.5e-6 Torr.  Ramping up TGHT at 2A/min to reach 164A (previous setting at ~1000C).

 Tuesday, July 30, 2024, 09:02

Temperature has been holding at about 1000C. THGT at 160A(readback,, 164A setpoint)/2.56V.  Pressure 7e-7 Torr.

Stepping up 1A/min in 20A increment to reach 1800C. 

Continue to monitor.

 Tuesday, July 30, 2024, 10:07

Plotting out THGT (readback) vs Temp:

181 A/2.91V, 1070C

206A/3.34V, 1153C

225A/3.7V, 1213C

245A/4.1V, 1277C

Wednesday, July 31, 2024, 11:26

TGHT tripped off due to HS water flow NOT oK,  Attempted to clear it but did not work, see attachment #3. 

Will stop the process for now and investigate the problem. 

 Wednesday, July 31, 2024, 12:10

Darwin helped to check the surrounding of the lab for water leaks; everything was good and the chamber remained under vacuum. 

All the water paddle wheels were moving.  A slight touch of the HS paddle wheel somehow cleared the interlock. Maybe the connection was loose. 

We checked all the paddle wheels by shutting and opening the water valves.  All the interlocks responded correctly. 

Continue with the heating process...

Ramping up TGHT at 2A/min to reach 300A.

 Wednesday, July 31, 2024, 15:27

TGHT vs temp:

294A/5.1V 1477C

343A/6.0A, 1633C

402A/7.2V, 1818C

Will keep TGHT at 410A (setpoint) for night.(see attachment#4)

 Tuesday, August 06, 2024, 10:00

Venting Evap 2; the process is done.

The sample will be analyzed. 

Wednesday, August 07, 2024, 15:36: Roughing. Had initially been roughed & TP started w/ Marla CS, however it timed out. Restarting.

Wednesday, August 07, 2024, 15:37: TP on.

Wednesday, August 07, 2024, 15:46: Tripped at 4 KRPM. Restarted. Up to 5 KRPM.

Failed to start.

Thursday, August 08, 2024, 10:00: TP started. 

Thursday, August 08, 2024, 10:12: TP Tripped but nearly spun up. Reset & Restarted. TP Green / on.

Monday, August 19, 2024, 13:06

Target container consists of 2 samples, and both samples were heat stabilized at 150 C for 24 hours then pre-oxidized at 360 C for 4 hours:

1.  PVP (7% wt/v) spun fibres 0.0569 g

2.  np-Ta (Dope 7) spun fibres: 0.1730 g

Samples are wrapped in graphite foil and loaded into a target boat which is wrapped with Ta foil.

Omega slope set at 0.99.

Similar heat treatment as the 1st attempt, see e-log #667 (1800 C = 402A/7.2V).

Good vac = 3 e-5 Torr

Bad vac = 5 e-5 Torr.

Chamber is currently pumping down.

 Monday, August 19, 2024, 16:52

Chamber pressure @ 4.6e-6 Torr.

Initiate auto-ramping at 1A/min to reach 400A.

Continue to monitor the pressure and TGHT.

Tuesday, August 20, 2024, 09:48

TGHT reached 400 A/6.87V about 10 hr ago.  But the temperature has been holding at 1665 C. 

The voltage is much lower this time compared to the previous heat treatment.  See attachment #1 for the overall process.

Ramping up to 450A.  Continue monitoring..

Tuesday, August 20, 2024, 15:43

TGHT at 450A (readback 441A)/7.892V, temperature holding at 1803C

Pressure coming down from 1.62e-6 Torr. 

Continue to hold on the temperature for a few more hours before cooling it down

 Wednesday, August 21, 2024, 09:40

Temperature was holding for about 18 hours before ramping down TGHT was initiated at 2A/min.

The samples can be taken out after 2 pm.

Monday, September 09, 2024, 19:06

The coated container was wrapped in 4 Ta foil heatshields.

Vacuum IGP1 initial =2.6 e-06 Torr

Target temperature on OMEGA= 1800-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final Current TBHT= 230 A

Final TGHT current= ~400A (adjustable)

Heating autoramp starged at 1A/min on  TGHT   and TBHT until outgassin peak passed

Then at 1A/min  to =400 A TGHT and 230A TBHT

Good vacuum = 5.0 e-04 Torr

Bad vacuum = 5.0E-02 Torr

Monday, September 09, 2024, 19:08

Peak passed around 70A will continue ramp up at 1A/min to 400A on TGHT and 230A TBHT

Tuesday, September 10, 2024, 13:13

Was ramped down at -2 A/min TGHT and -1 A/min TBHT

A boat lined up with graphite and wrapped in 3 Ta heatshileds

Vacuum IGP1 initial =6.1 e-06 Torr

Target temperature on OMEGA= 1800-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final TGHT current= ~400A (adjustable)

Heating autoramp started semi-manually on  TGHT  to 65A and then at continue to 100A

After peak heat at 1A/min  to =400 A TGHT

Good vacuum = 5.0 e-04 Torr

Bad vacuum = 5.0E-02 Torr

Tuesday, September 10, 2024, 22:22

1810C OMEGA at 439A TGHT readback

Wednesday, October 02, 2024, 19:21

Ta endcup at front end of container

End-caps on the graphite cartridge have holes for outgassing. 

initial heating @ 2A/min to 85 A then 2A/min to 120A TGHT.  Allow pressure to drop and then ramp to 400 A at 2A/min, leave 4 hours and start ramp down.

OMEGA slope = 0.99

Vacuum limits up to 400A: 5.0e-04 Torr -- 1.0e-02 Torr

Max current~400A (1900 C)

Wednesday, October 02, 2024, 19:25

Starting IGP1 = 6.65e-06 Torr

Thursday, October 03, 2024, 05:09

Starting rampdown.  Pressure stable at 4.5 e-06 Torr

Top temperature 1850 C on OMEGA

ramping down at -2A/min

Saturday, November 23, 2024, 11:08

 No milling ZrC material sintering inside graphite cartridge

baseline standard discs included for comparison. 

4 Ta foils wrapped around  container

one spring at the back end to retain the graphite cartridge

One Ta cap with perforations at the front for T readings

initial heating at 2A/min to 50A, followed by heating at 1A/min to 90 A

Initial IGP1= 1.0e-6 Torr

OMEGA slope =0.990

Good and bad vacuum =5.0e-5 Torr and 5e-4 torr

Saturday, November 23, 2024, 11:20

autoramp start at 2A/min to 50A on tght

Saturday, November 23, 2024, 20:11

allowed pressure to drop to 3.3e-6 Torr after degassing. 

Started ramp to 90A at 1A/min

Saturday, November 23, 2024, 23:46

started ramping at 1.5A/120s or 0.75A/min to 400A

Sunday, November 24, 2024, 07:55

Reached 1900 C at 410 A setpoint and 402 A on RD

Pressure did not increase after bumping up to 410 setpoint so will keep at this current until 11 am (four hours near 1900 C in total)

Sunday, November 24, 2024, 10:58

Final IGP1 at start of rampdown = 2.9e-6 Torr

Ramping down at -2A/min