Wednesday, September 27, 2017, 18:05

 3 samples from NS-npSiC pellets, pressured at 10T  (see lab book pg 53)

3 samples from B3 pellets, 600MPa (see lab book pg 50)

Desired temperature = 1550C, est current = 450A

 Thursday, September 28, 2017, 11:17

Vac at 8.8e-7 Torr.  

Ramping TGHT up to 450A at 0.2A/min

 Thursday, September 28, 2017, 17:54

Setup screen capture, see pg 53 for saved directory

 Friday, September 29, 2017, 23:54

TGHT reached to 450A/7.9V, temp at 1510C.

Tapping up TGHT to 465/8.2V to reach 1550C

Pressure coming down from 1.6e-6 Torr.

See attachment 1 for the 20-hour plot

 Sunday, October 01, 2017, 00:30

At around 20:00 on Sep 30, there was an increase of ~0.1 V which caused a rise in temp from 1550 to 1576C (see screen capture).  Pressure increased slightly.

Tapped down TGHT to 445A/8.05V; temp maintained at 1550C.

 Monday, October 02, 2017, 17:55

Cooling TGHT from 445A/8.07V, 1500oC to room temperature at 1A/min

 Tuesday, October 03, 2017, 11:09

Target has been cooled for over 10 hours. 

Venting chamber

Wednesday, October 04, 2017, 16:37

3 samples of npSiC/PAN cast-pellets, see lab book p. 57 for details.

Desired temperature 1550C, expected TGHT ~450A.

Chamber pumped down.

TGHT ramping at 0.2A/min

 Friday, October 06, 2017, 10:45

TGHt at 450A/7.7A, temp at 1510C.  (p.s voltage is lower than before, elog 389).

Tapped up to 466A/8.08v, temp reached to 1550C.  A slight increase in pressure when tapping up TGHT. (see attached screen capture)

Will maintain heating temperature for several days before cooling down

 Tuesday, October 10, 2017, 10:50

Samples was heated for several days at 1550C. 

Cooling down initiated at 2A/min.

 Tuesday, October 10, 2017, 18:07

Chamber is vented.

Process done

Monday, November 06, 2017, 18:21

Samples of Horn and Probe - npSiC. see pg 74.

6 samples in total, to be heated to 1550C, about 450A.  Set ramping rate at 0.2A/min.  

Chamber pumping down

 Tuesday, November 07, 2017, 15:01

TGHT reached to 450A/8.2V, temperature measured at 1460C.  See attachment 1.

Increased ramping to 480A, targeting 1550C.

 Tuesday, November 07, 2017, 22:26

Samples have been heating at 1550C with TGHT at 480A/8.78V for about 8 hours.

Vacuum stabilizes at 8.4e-7 Torr.

Initial cooling at 2A/min.

 Wednesday, November 08, 2017, 10:36

Venting chamber.

Saturday, April 28, 2018, 16:09

Container is coated with TaC and wrapped with TaC heatshield. 

Will be used for carbonizing nanoSiC target materials.

Chamber is pumping down...

Sintering temp 1800C, est TGHT ~550A

 Saturday, April 28, 2018, 18:08

Pressure at 5.e-6 Torr. 

Initial auto-ramp at 1.0A/min reaching TGHT 500A.  Monitoring temp.

 Sunday, April 29, 2018, 23:37

Target temp stabilizes at 1800C with TGHT holding at 400A/7.02V for 24 hours.  Pressure at 4.4 e-7 Torr.

Lower TGHT to 338A/5.51V to reach 1600C - This will temp/current will be used for carbonizing the nanoSiC fibers.

Holding TGHT overnight to determine temp stability.

 Monday, April 30, 2018, 18:04

Temp is holding at 1600C, TGHT 338A/5.5V.  Pressure at 3.0 e-7 Torr. 

Initiated cooling down at 2A/min.

Tuesday, May 01, 2018, 18:06

21 fibrous discs of nanoSiC are loaded into a tube container (coated/Sintered with TaC). 

Thermal treatment temperature at 1600C, TGHT is ~338A/5.5V, according to elog #407.

 Wednesday, May 02, 2018, 08:27

20 mins ago... initiate auto ramping at 0.2A to reach TGHT 250A.  Instead of ramping incrementally, TGHT jumped straight to 250A; vacuum shot up to milli torr.

Turn off TGHT immediately to let vacuum stable down to 10-6 Torr. 

System problem??  Archive striptool for more details. 

Re-activate auto-ramping - OK!

Once TGHT reached 250A (18 hours later from now), will continue ramping up to reach 1600C

 Friday, May 04, 2018, 01:09

TGHT just reach 250A, temp at about 1190C.  Pressure remained high at 4.2e-5 Torr. 

Continue autoramping to reach TGHT 300A.

 Friday, May 04, 2018, 11:07

TGHT at 300A for about 1.5 hr.  Temp at 1315C.  Pressure at 5.7e-6 Torr.

Autoramp to 320A.

 Friday, May 04, 2018, 14:39

Tapping up to 330A; temp at 1560C with slope changed to 1.05 (for carbide material). Will keep at this current/temp.

 Sunday, May 06, 2018, 13:25

TGHT at 330A/5.2V; holding temp at 1550C.  No coating on windows.  Pressure at 1.6e-7 Torr.

Cooling down at 2A/min. 

 Monday, May 07, 2018, 10:49

Evap cooled.  Venting chamber. 

Inspection of the discs next...

mass loss = 6.79 - 3.62 = 3.1 g (46%) [in agreement, good]

Tuesday, May 08, 2018, 15:02

22 np-SiC fibrous discs loaded in the tube container (coated and sintered with TaC)

Heat treatment is similar to previous process, see elog #408. 

TGHT should be set at 330A/5.2V to reach temp 1575C (+/- 25).

Omega slope set at 1.05 (for carbide)

Chamber is currently being pumped down

 Tuesday, May 08, 2018, 22:46

Pressure at 2.2e-6 Torr.

Initiated autoramping at 0.2A/min to reach 330A

 Friday, May 11, 2018, 11:11

TGHT reached to 330A/5.1V but temp was measured at 1400A; It was held at that current for about 10 hours.

Increased TGHT to 335A/5.2V - temp is holding at 1420C (Will check the window if there is any coating that might have caused the discrepancy)

 Sunday, May 13, 2018, 00:25

In fact, the window is slightly coated.  The temperature should already be at optimum, 1600C.  Will keep heating for another day.

 Sunday, May 13, 2018, 14:10

Temp holding up well.. Pressure at 1.8e-7 torr. 

cooling down at 2A/min.

 Monday, May 14, 2018, 09:33

Target has been cooled for over 18 hours.  Pressure at 1.1e-7 Torr.

Venting chamber.

mass loss = (8.65 - 4.32)g = 4.33 g (50%) [slightly higher than expected, likely due to increase of 5A on TGHT]

Tuesday, July 03, 2018, 17:02

49 discs/ 15.42g np-SiC fibrous discs loaded into the tube container

Heat treatment is similar to previous process, see elog#408/409.

TGHt should be set at 330A/5.2V to reach temp 1575C (+/- 25C)

Omega slope set at 1.05 (for carbide)

Chamber is currently being pumped down

 Wednesday, July 04, 2018, 10:38

Pressure at 1.5 e-6 Torr.

Initiated auto-ramping at 0.2A/min to reach 330A/5.2V.

 Monday, July 09, 2018, 14:44

TGHT has been stabilized at 330A/5.2V for 24 hours.  Pressure at 3.7e-7 Torr.

Temp was measured at 1400C - light coating on window likely affected the measurements.

Measured with one-color pyrometer on Ta body inside the target container = 1550 C (with the correction of 250C for Ta). 

Adjusted OMEGA slope to 1.18, temp currently at 1580 C.

 Monday, July 09, 2018, 16:42

Pressure stabilized at 3.5e-7 Torr. 

Initiated auto-cooling at 1A/min.

 Tuesday, July 10, 2018, 11:11

Target is at room temperature. 

Process completed; see attachment for the data retrieval and dropbox (np-SiC production folder) for screen capture.

mass loss = (15.42 - 8.09) g = 7..33 g (47.5%) [in agreement - good!]

Tuesday, July 10, 2018, 16:40

Container was flashed with TaC solution and let dry in air. 

No Ta heat shield is used. 

Desired temperature 1900C, ramp up TGHT accordingly. (Take note at 1500 and 1600 C).  

OMEGA slope setting = 0.98

TBHT set at 250A (as usual)

Chamber is currently being pump down.

 Wednesday, July 11, 2018, 10:54

Pressure at 4.5 e-7 Torr. 

Autoramping TGHT at 0.1A/min to reach 300A and TBHT at 0.1A/min to reach 230A. 

Once TGHT setting is reached, it will be further increased according to the temp measurement. 

 Friday, July 13, 2018, 10:57

TGHT at 300A/4.02V but temp is still too low to be detected. 

Increase TGHT to 400A, ramping at 1A/min.  TBHT is already at 230A/4.0V.

Current pressure at 4.4e-7 Torr.

 Friday, July 13, 2018, 13:09

TGHT reached 400A/5.85V, temp reading 1112C.

Ramping up to 500A

 TGHT reached 500A/7.9V.  temp reading 1250 C.

Ramping up to 600A

 Friday, July 13, 2018, 17:13

TGHT reached 600A/10.74V, temp reading 1742 C.

Ramping up to 650A

 Wednesday, July 18, 2018, 11:54

TGHT has remained at 650A/12.05V since Friday July 13.

Temperature check:

pyrometer: 1650 (250 correction) = 1900 C

OMEGA:  1-color (e= 0.32 for spectral hemispherical) = 1910 C

OMEGA: 2-color (slope @ 0.99) = 1905 C

Measurements are in agreement

Cooling TGHT at 2A/min, TBHT at 1A/min. Current pressure 3.7e-7 Torr.

 Wednesday, July 18, 2018, 13:47

TGHT at 500A, 8.4V, temp at 1600 C (4.2 kW)

TGHT at 475/7.84V, temp at 1550 C (3.72 kW - Max operating target heating power)

TGHT at 450/7.31V, temp at 1500 C (3.28 kW)

With TBHT set for 230A, usual operation setting, the temperature on the transfer tube is to exceed 2000 C.  Keeping TBHT at that setting may affect the overall temperature.

Note:  To condition the nanoSiC, it is better to keep TBHT at 0A and ramp up TGHT to 475A while monitoring the vacuum.  Then step up TBHT; any increase in vacuum would indicate a local evaporation of nanoSiC close to the ionizer. 

Temp measurement is complete, cooling down TGHT/TBHT to zero.

 Thursday, July 19, 2018, 12:23

TGHT has been at 0A for over 18 hours.  Vacuum pressure at 7e-8 Torr.

Venting chamber.

Wednesday, July 25, 2018, 17:32

Container is coated with TaC and wrapped with 3 layers of Ta heat-shields.

Desired sintering temperature ~1900 C, TGHT is estimated to be ~ 445A (3.3 kW), TBHT set to 230A (as usual).

OMEGA slope set to 0.99

Good vac = 3.0 e-5 Torr, Bad vac = 5.0 e-5 Torr.

Chamber is currently being pumped down.

 Friday, July 27, 2018, 10:32

Vacuum at 9.9 e-7 Torr. 

Autoramp TGHT at 1A/min to 300A and TBHT at 1A/min to 230A. Will monitor temp and adjust TGHT to reach the desire temp.

 Friday, July 27, 2018, 16:31

TGHT reached to 1500 C, and TBHT at 230A, Temp at 1480 C, pressure at 2.e-6 Torr.

Autoramp TGHt at 1A/min to 400A.  Continue monitoring temp.

 Saturday, July 28, 2018, 12:41

TGHT at 400A/6.2V. Temp at 1730 C.  Pressure 7.4 e-7 Torr.

Tapped up TGHT to 450A/7.2V, temp at 1891 C. Holding at this current... Pressure coming down from 1.2e-6 Torr.

 Monday, July 30, 2018, 22:40

Target temp has been held at 1880 C, TGHT at 450A/7.57V, TBHT 230/4.18V, vaccum at 3.8 e-7 Torr. 

Cooling TGHT and TBHT at 2A/min and 1A/min, respectively. 

 Tuesday, July 31, 2018, 10:23

TGHT/TBHT at 0A.  Pressure at 1.5e-7 Torr. 

Process completed. 

Venting chamber.

Target containers looks good.  Transferred to Ar glovebox.

Monday, August 20, 2018, 17:58

14.9 g of np-SiC fibrous target discs are loaded into the container (previously coated with TaC and sintered, see elog ID 414).

Total loaded length 9.5 cm. 

A 1.5" width graphite sheet is used as under layer to prevent TaC diffused to the discs; this was observed during the heat treatment, (see dropbox SEM images).

Both end caps are in.  With ionizer pointing out, right cap is expended BUT NOT left cap - will need to expend this after the conditioning.

No Ta heat-shield is used.

Final conditioning temperature:  1500 C (As per e-log 414, TGHT = 450A/7.31V, 3.28kW) 

Keeping TBHT at 0A for now - will ramp up after TGHT reach to the desired temperature. 

OMEGA slope set at 0.99

Good vac = 3.0e-5 Torr,

Bad vac = 5.0e-5 Torr.

 Tuesday, August 21, 2018, 10:24

Pressure at 1.2e-6 Torr. 

Initiated autoramping at 2A/min for TGHT to reach 400A - monitoring temp and vacuum.

TBHT set at 10A. 

 Tuesday, August 21, 2018, 15:13

Temp reached to 1350C. TGHT at 400A/6.7V. Pressure at 1.9e-6 Torr after holding at the temp for 100 min.

 Tuesday, August 21, 2018, 15:28

Tapped up TGHT to 450A/7.8V (3.5kW).  Temp measured at 1465 +/- 5 C.  Pressure coming down from 3.5 e-6 Torr.

 Tuesday, August 21, 2018, 15:32

Tapping up TBHT to 230A

 Tuesday, August 21, 2018, 16:25

TBHT at 230A/4.33V.  Pressure started to increase from 150A, and reached to 3.3e-6 Torr after TGHT reached to the setting.

Temperature measured at 1475 C +/- 5C.  Holding at this temperature until vacuum comes to stabilization (est.2-3 hours)

 Tuesday, August 21, 2018, 16:45

Checked with Mikron (slope set at 0.99); temp on left end-cap measured at 1490 +/- 20C (that's close enough).  Temp on ionizer tube about 1900C

 Tuesday, August 21, 2018, 22:12

Pressure at 1.7e-6 Torr.  Temp holding at 1480C, TGHT at 450/7.7V, TBHT 230A/4.27V.

Cooling down at 2A/min for TGHT and 1A/min for TBHT

Tuesday, September 04, 2018, 16:58

Container is coated with TaC and wrapped with Ta heat-shield ( 3 layers)

Desired temp = 1900 C (expected TGHT ~445A/7.5V), TBHT will be set fixed at 230A (max).

Good vac at 3.00-5 Torr

Bad vac at 5.0e-5 Torr.

Chamber is currently being pumped down

 Wednesday, September 05, 2018, 10:53

Pressure at 9.5-7 Torr. 

Auto ramping TGHT at 1A/min to reach 400A, and TBHT at 1A/min to reach 230A.

 Wednesday, September 05, 2018, 17:52

Problem with TGHT readback vs setpoint.  TGHT ramped up to 400A, temp measured at 1830C.  However, the setup remained at 228A (see attachment).  The autoramping program only sees the readback; in this case, the TGHT would continue to keep ramping up until the target breaks.  The autoramping program has stopped just in time. 

TGHT stepped down to 400A (setpoint), readback at 206A/6.59V.  TGHT at 230A/4.16V.  Temperature holding at 1783C. 

Control has been informed.

 Thursday, September 06, 2018, 10:54

Target temp holding at 1773C.  Pressure at 8.5e-7 Torr. 

Ramping down TGHT and TBHT, and inspect the container later. 

Problem with the TGHT readback/setpoint will need to be investigated.

 Friday, September 07, 2018, 16:03

Target container is nicely sintered.

Awaiting for Control group to investigate with the problem on TGHT readback/setpoint. 

Darwin Ortiz Rosales wrote:

Tuesday, July 30, 2019, 15:33 ZrC backup Target 12.6 cm disc length, 465 g total weight (no springs and no analysis discs). Total weight= 470 g. 20 Analysis discs weighing 2.368 g (10 at each end). Two springs (one at each end). OMEGA slope initially = 0.990  (was changed to 1.09 at higher Temperature as per eLog #434 Target is being pumped down. Wednesday, July 31, 2019, 09:31 Desired temp = 1900 C, Auto ramping TGHT at  0.1 A/min to reach 400A then  TGHT will be tapped up accordingly to reach desired temperature. (eLog 434) TBHT will be set fixed at 230A (max). TBHT at 0.1 A/min to reach 230A. Note: Initially both TGHT and TBHT will be ramped up at 0.3A/min up to 30A each. IGP1= 1.35e-06 Torr Good vac at 3.00-5 Torr Bad vac at 5.0e-5 Torr. Wednesday, July 31, 2019, 12:02 At 30A pressure was increasing a bit fast, therefore, the ramp was changed to increments of .1A every 120s (.05A/min).  Thursday, August 01, 2019, 08:42 TGHT = 54.7 TBHT = 54.3 IGP1 = 3.86e-5 Torr Will changer heat ramp to .1A/min by changing wait interval to 60s Tuesday, August 06, 2019, 07:14 OMEGA = 1212 C TGHT = 344.7 A, 5.79 V TBHT = 233 A, 4.17 V IGP1 = 1.05 e-06 Torr Autoramping to 400A at increments of 0.1A/min Tuesday, August 06, 2019, 09:50 OMEGA = 1233 C TGHT = 360 A, 6.05 V TBHT = 233 A, 4.18 V IGP1 = 1.21 e-06 Torr increasing autoramp increments to .5A/min Tuesday, August 06, 2019, 12:27 OMEGA = 1356 C TGHT = 400.6 A, 6.92 V TBHT = 233.8 A, 4.20 V IGP1 = 1.95 e-06 Torr Autoramping to 430 A on TGHT at 0.5 A/min Tuesday, August 06, 2019, 14:02 OMEGA = 1447 C TGHT= 430.9 A, 7.66V TBHT = 233.2A, 4.2 V IGP1= 2.01e-06 Torr Autoramping to 440 A on TGHT at 0.5 A/min Wednesday, August 07, 2019, 09:10 OMEGA = 1548 TGHT = 441.56 A, 8.2 V TBHT = 233.3 A, 4.2 V IGP1 = 6.21e-07 Torr Manually ramping up to 1900C @ 1A/min Wednesday, August 07, 2019, 09:43 Changed OMEGA slope to 1.09 as per eLog #434 OMEGA reads 1773 C @ TGHT 451A, 8.4V IGP1 = 7.02 e-07 Wednesday, August 07, 2019, 10:56 OMEGA = 1903 C TGHT = 483.5 A, 9.2V TBHT = 233.3 A, 4.3V IGP1 = 1.7 e-06 Torr trending down Wednesday, August 07, 2019, 11:40 OMEGA = 1914 C TGHT = 483.5 A, 9.3V TBHT = 233.3 A, 4.3V IGP1 = 1.5 e-06 Torr trending down Decrease TGHT current to 480.4 A Wednesday, August 07, 2019, 13:04 OMEGA = 1918 C TGHT = 480.3 A, 9.4V TBHT = 233.3 A, 4.3V IGP1 = 1.28e-06 Torr Decrease TGHT current to 474.5 A Wednesday, August 07, 2019, 13:26 OMEGA = 1904 C TGHT = 474.8 A, 9.3V TBHT = 233.3 A, 4.3V IGP1 = 1.11e-06 Torr Wednesday, August 07, 2019, 13:47 OMEGA = 1912 C TGHT = 474.8 A, 9.3V TBHT = 233.3 A, 4.3V IGP1 = 1.10e-06 Torr Decrease TGHT to 471.8 A OMEGA temperature went down to 1904 C Wednesday, August 07, 2019, 14:26 OMEGA = 1911 C TGHT = 471.8 A, 9.3V TBHT = 233.3 A, 4.3V IGP1 = 1.00e-06 Torr Decrease TGHT to 469.0 A OMEGA temperature down to 1904C Wednesday, August 07, 2019, 15:45 OMEGA = 1912 C TGHT = 468.8.8 A, 9.2V TBHT = 233.3 A, 4.3V IGP1 = 9.2e-07 Torr Decrease TGHT to 466.0 A OMEGA temperature down to 1903C   Wednesday, August 07, 2019, 22:09 OMEGA = 1924 C TGHT = 466.8. A, 9.3V TBHT = 233.3 A, 4.3V IGP1 = 7.6e-07 Torr Cooling at 2A/min TGHT to 456.0 A, 9.0 V and 1A/min TBHT to 230.1 A, 4.2 V OMEGA = 1900 C Will allow Pressure to stabilize    Thursday, August 08, 2019, 06:54 OMEGA = 1919 C TGHT = 456.9 A, 9.1V TBHT = 230.3 A, 4.2 V IGP1 =5.7e-07 Torr Cooling at 2A/min TGHT and 1A/min TBHT Thursday, August 08, 2019, 13:30 Target removed from Evap2.  Awaiting inspection by John.

 Monday, August 12, 2019, 15:45

Visual inspection on the target was performed today.  See attachment for details.

Target container is slightly bent, and some visible crystallization on the container surface.  

The discs are nicely packed with only a slight expansion in length was measured.

No clogging inside the container nor the ionizer tube. 

Some sintered discs samples were collected and SEM will be perform later. 

Darwin Ortiz Rosales wrote:

Tuesday, November 26, 2019, 14:53 Total number of foils: 504 Total length packed 17.4 cm container has 3 Ta heat shields. No endcaps inserted to facilitate out-gassing Two TaC coated Ta wire springs inserted at either end. Initially to ramp TGHT and TBHT to 50A at 1A/min Then heat manually to OMEGA ~1400 C , ramping TGHT manually and automatically  to reach 530A A (Omega slope set = 0.990) Then temperature= 1900 C (Correction = 1800 C, NOT 1900 - JW), Omega Slope set = 0.990 (use 1.08, check temp, JW), manually and automatically ramp to 700A (check temp to see if it's matching with the 1.08 slope), TGHT will be tapped up accordingly to reach desired Temp. TBHT will be set fixed at 230 A (max).  TBHT heated manually and automatically to max. Good vac at 3.00 e -5 Torr Bad vac at 5.00 e-5 Torr System experienced some vacuum issues due to cooling water leak in a heatshield line.  Evaluation discs not included because no space. Total Green disc mass measured = 58.250 g   Tuesday, November 26, 2019, 15:00 IGP1= 7.4e-06 Torr.  No leak issues found after last fix (Anders will add details). Tuesday, November 26, 2019, 15:33 TGHT= 52.7A, .22V   TBHT= 49.3A, .52V IGP1= 7.202 e-06 Torr (trending up so will allow to stabilize).

 Wednesday, November 27, 2019, 17:44

I'll take over from here to step up the target heater, and I'll coordinate it with Darwin. 

 Wednesday, November 27, 2019, 20:36

Note: Sintering temp should be at 1800 C, NOT 1900.  Use Omega slope 1.08 and check temperature.  Correction made on elog #471.

Continue to step up TGHT and TBHT, keeping vacuum below 1.5 e-5 Torr. 

 Thursday, November 28, 2019, 03:06

TGHT reached to 400A/5.29V, TBHT at 230A/3.13V. 

Vacuum coming down from 1.3 e-5 Torr.

OMEGA = 1105 C (slope at 0.99).

Instructions for Darwin:

1.  Confirm temperature - check the temp plot from the TaC coating step. 

2.  Change OMEGA slop to 1.08 - check to see if this matches the temp plot.  If not, bring it back to 0.99.

3.  Continue to step up TGHT, check temp at 1400C (change slop 1.08 and check), 1500 C, 1600 C (check windows for coating - if any coating, then OMEGA is no longer useful hereon)

4.  Use the temp plot and continue to tap up TGHT to reach 1800 C and hold it for at least 4 hours or until the vacuum goes below 1 e-6 Torr then proceed with cooling down.

5.  Use the auto cooling program for TGHT (-2A/min) and TBHT (-1A/min)

Note:  For ramping up TGHT, keep vacuum below 1.5 e-4 Torr and keep tapping up to reach 1800 C.  Above 1100 C, this should be a quick step to get to 1800 C; should take < 2 hrs to get there.  

See the striptool or the attachment below to see how I did it. 

Once the chamber is cool down, take out a few samples for SEM analysis. 

Good luck!

Darwin Ortiz Rosales wrote:

Friday, September 25, 2020, 10:30  Target boat with a layer of niobium foil on the bottom is used to heat up Nb samples to 1400 C for 4 hrs. OMEGA slope = 0.99 The niobium samples are wrapped in two layers of  Nb foil. Boat is wrapped with 2 layers of Ta foil, careful to avoid touching samples.  Friday, September 25, 2020, 10:35 Manually ramped TGHT to 40 A and kept at that current for approximately 15 minutes.   Then started autoramp at  1A/min up to 100 A  Friday, September 25, 2020, 16:58 IPG1= 4.7e-07 Torr TGHT =100.0 A, 1.3 V Start autoramp to TGHT to 300 A  @ 2A/min  @ 300A temperature = 1179 C   Friday, September 25, 2020, 20:00  autoramp to 345 A  Friday, September 25, 2020, 20:39 TGHT = 345 A, 5.4 V OMEGA = 1296 C IPG1= 8.1 e-07 Torr Ramp manually to 1400 C  Friday, September 25, 2020, 20:51 reached 1400 C on OMEGA at TGHT = 476 A Friday, September 25, 2020, 20:59 OMEGA increased to 1410, lowered TGHT to 468 A to get back to 1400 C on OMEGA  Friday, September 25, 2020, 21:40 Lowered TGHT to 463 A,  5.79 V to bring OMEGA to 1400 C from 1404 C  Saturday, September 26, 2020, 00:51 Sample has been at 1400 C for 4 hours. IGP1= 7.2 e-07 Torr Cooling at- 2A/min

 Monday, September 28, 2020, 09:36

Vented chamber - for Darwin.

Monday, September 28, 2020, 11:49

6 discs of np-SiC were loaded to the target boat wrapped with 3 layers of heat shields.

Desired temperature at 1500 C, (As per e-log 414/416, TGHT = 450A/7.31V, 3.28kW) 

Omega slope set at 1.05 (for carbide)

Good vac = 3.0e-5 Torr,

Bad vac = 5.0e-5 Torr.

Pumping down in progress

 Monday, September 28, 2020, 21:44

Pressure at 1e-6 Torr.  Initiated autoramping at 0.2A/min to reach 300 A.  Monitor temp.

 Wednesday, September 30, 2020, 11:39

TGHT reached to 300 A/ 4.5V, temp at 1130 C.  No coating on windows.

Continue to ramp up 330A.  Monitor temp.

 Wednesday, September 30, 2020, 16:38

TGHT reached 330 A / 5.04 V, temp at 1190 C. 

Ramp up to 400 A. Current pressure at 9.8 e-7 Torr.

Thursday, October 01, 2020, 10:28

TGHT reached 400 A/ 6.3V, temp at 1320 C.  Continue to ramp up to 450 A.

 Thursday, October 01, 2020, 16:44

TGHT reached to 450 A/ 7.4 V.  TEmp at 1500 C. 

Pressure at 1.35 e-6 Torr and coming down.   Continue to hold TGHT at 1500 C for at least 24 hr.

 Sunday, October 04, 2020, 16:49

TGHT has been holding at 450 A/ 7.3 V for nearly 3 days; temp has gone up and stabilized at 1554 C; pressure at 2.13 e -7 Torr.

Initiated cooling down at -2A/min.

 Monday, October 05, 2020, 10:02

Chamber vented.

Flora Wu wrote:

Thursday, June 09, 2022, 11:25 Total number of foils: 14 electrospun fiber pellets  Total weight = 208.3 g container has 3 Ta heat shields. Desired temperature at 1800 C Omega slope set at 0.990  Good vac = 3.0e-5 Torr, Bad vac = 5.0e-5 Torr. Pumping down in progress  Thursday, June 09, 2022, 11:25 chamber pumped down below 5e-5 initiate auto ramping, 1A/min ----> 100 A

 Thursday, June 09, 2022, 19:16

Pressure came down below 10e-5 Torr as TGHT ramped up to 100A.

Continue auto ramping to reach 250A at 1A/min.

 Thursday, June 09, 2022, 22:52

TGHT is hovering around 127A/1.68 V due to erractic pressure, see attachment #1..  Notice the backing line is at atm pressure - I don't recall this happened in the past. 

Temp is still low to be detected on Omega.  Will leave this overnight.

 Friday, June 10, 2022, 09:07

TGHT has been holding at 250A/3.76V since 2:45am.  Pressure comes down as THGT above 200 A.  Backing line is back down normal.

Temp reading at 1040 C. 

see attachment #2.

Continue to ramp up to 300A, monitoring temp/pressure.

 Friday, June 10, 2022, 10:31

TGHT reached to 300A/4.63V, temp at 1145C.  Pressure at 1.8e-6 and coming down. 

Continue to ramp up to 350A.

 Friday, June 10, 2022, 11:59

TGHT at 350A/5.66V, temp at 1300 C, Pressure at 8.1e-7 Torr, and coming down.

Continue to ramp up to 400A.

Friday, June 10, 2022, 13:19

TGHT reached to 400A/6.73V.  Pressure coming down from 1.04e-6 Torr. 

Temp at 1690.  Will set up manually to reach 1800 C. 

 Friday, June 10, 2022, 13:50

TGHT stepped up to 432A/7.42V.  Pressure coming down from 1.3 e-6 Torr. 

Temp at 1800 C.  See attachment#3 and #4 for the screenshot and temp-current plot.

Dumped striptool data to /usr1/evpr/carbonize_pan10_elog581_a and b.

Will keep at this setting over the weekend, and cooling down will take place on Sunday evening. 

 Sunday, June 12, 2022, 22:30

TGHT has been holding at 432A/7.40V since Friday.  Temperature has gone up slightly to 1825. 

See attachment#5 for the overall process. 

Initiated cooling down at -2A/min.

Chamber will be vented on Monday morning.

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, 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.

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.

Carla Babcock wrote:

Darwin Ortiz Rosales wrote: Wednesday, April 26, 2023, 09:32 LP FEBIAD loaded with 367 TiC discs and 4 TiC removable discs for analyses 50 packs of 5 and the rest are singles TaC coated (sintered) springs placed at both ends Initial total Weight = 521.83 g Initial heating @ 1A/min to 400 A on TGHT and 280A on TBHT OMEGA slope = 0.99 Vacuum limits up to 200A:  3.0e-05 Torr -- 5.0e-04 Torr Vacuum limit up after 200A: 3.0e-05 Torr -- 5.5e-05 Torr No Ta heat-shields used Initial IGP1 = 4.1e-07 Torr Wednesday, April 26, 2023, 09:49 Starting initial ramp up to 200A on both TGHT and TBHT @ 1A/min Wednesday, April 26, 2023, 12:50 Around 120A on TGHT, the pressure started to slowly drop.  First outgassing done. Wednesday, April 26, 2023, 14:03 IGP1 = 6.0 e-05 Torr TGHT = 200 A, 2.7V TBHT = 200 A, 2.6 v OMEGA = Below lower limit Waiting for pressure to fall below 5e0-5 Torr.  Will change bad vacuum to 5.0e-05 Torr and then continue ramping @1A/min to 400 A on TGHT and 280 A on TBHT. Wednesday, April 26, 2023, 14:13 IGPI= 4.2 e-05 Torr starting ramping to 400 A on TGHT and 280A on TBHT  Wednesday, April 26, 2023, 14:26 The IGP1 pressure just fell below 3.0e-05 Torr and ramping has resumed Wednesday, April 26, 2023, 14:42 pressure hovering around good vacuum so very slow progress. Wednesday, April 26, 2023, 15:12 TGHT= 223 A, 3.1 V TBHT = 226 A, 3.0 V Set ramp rate is 1A/min but real rate is slightly less than 0.5A/min due to pressure fluctuation.  Vacuum spike at 300A. Currently: TGHT= 316A, 4.6V TBHT=283A, 3.9V Wednesday, April 26, 2023, 18:18 Ramping TBHT down from 280A to 270A

 Wednesday, April 26, 2023, 22:12

TGHT = 400A, 6.1V; TBHT = 274A/3.7V. Temp is holding sturdy ~1100 C and will leave it overnight.

Pressure is coming down, currently at 8.8 e-6 Torr.  See attachment for the overview. 

TGHT will continue to ramp up tomorrow morning; check the pressure to ensure it has come down below 5e-6 Torr before proceeding.  Refer to the instructions for details.