Started Ta#47 heating at Evap2 using the autoramp program. The TGHT current is setup to go to 300A (for now) and the TBHT to 230A (final value).

Friday, February 26, 2016, 15:44

5 samples were prepared at UBC MTRL using Sol-gel tetraethyl orthosilicate (TEOS) coated on electrospun polyacrylonitrate (PAN). 

Each sample is sandwiched in between graphite foils. 

Sample labeling:

Direct, 0.2358g

Mix, 0.3486g

3X, 0.2273g

5x, 0.2079g

7x, 0.1735g

All samples are loaded in the target boat, stacking on each other.  The Container is wrapped with 2X- Ta shields.

Chamber is pumping down. 

Step#1 Carbonization temperature: 1600C

 Saturday, February 27, 2016, 10:07

Vac at 2.5e-7 torr.

Ramping up TGHT to 300A at 1A/min. monitoring temp.

Saturday, February 27, 2016, 17:38

TGHT at 400A, temp at 1600C. Vac 1.34e-6 Torr.

 Monday, February 29, 2016, 13:04

Samples have been heated at 1635C for almost 2 days. 

Pressure at 2.1e-7 Torr.

Initiated cooling at 2A/min.

 Thursday, March 24, 2016, 11:26

Samples were analyzed for Si using EDX.  Unfortunately, no Si was found.  The vapour pressure of SiO was too high for it to react with PAN to carbonize in a vacuum environment.  

Will look into a different technique.

Thursday, February 25, 2016, 18:04 Wednesday, February 24, 2016, 17:29

Heat treatment of 2 bullet-shaped Nb samples in a LP-SIS container; it is just that we don't have a target boat. 

Container is wrapped with 12" in total length.  A strip of Nb foil is used as an underlayer for the samples to sit on top. 

Chamber has been pumped down and current vacuum at 1e-6 Torr. 

HS water check - good.

Target temperature 1400C

Ramping up to 250A; this should get to ~1300C.  Will let it heat for over night and step up to 1400C tomorrow. 

 Wednesday, February 24, 2016, 17:59

I'm stopping the heating process because the camera is not working.  I can't monitor the temperature.  Tried to fit the camera; don't now why it fails to connect to the server. 

Will look in to it tomorrow...

 Thursday, February 25, 2016, 08:17

Initiated auto ramping TGHT at 2A/min.

Thursday, February 25, 2016, 17:33  

Finally the camera is fixed.  

Current temperature is at 1126C, TGHT at 250A.  Will step up to reach 1400C. 

Thursday, February 25, 2016, 18:04  

TGHT stepped up to 335A to reach 1400C.  (see attachment) 

Will heat this for few hours and cool it at around 11pm tonight.

 Thursday, February 25, 2016, 22:19

Samples have been heated over 4.5 hours. 

Initiated cool down at 1A/min.

 Friday, February 26, 2016, 15:43

done! all good.

John Wong wrote:

Laura Lambert wrote:  Tuesday, February 16, 2016, 14:19 coated with TaC yesterday and let dry overnight. wrapped with one long Ta heat shield - wrapped around tube 3x, with Ta wire to offset Ta foil away from container loaded into evap2 and currently pumping down.  Wednesday, February 17, 2016, 10:51 HS water valves opened, no leaks detected. Tapped up manually to 35A. Waited ~20min, vacuum stable. IGP1 = 5.9e-7 Torr. Initiating auto-ramp at 0.2A/min to a final setpoint of 400A. Final desired temperature = 1900C  Thursday, February 18, 2016, 09:16 IGP1 = 6.6e-7 Torr. TGHT = 303A, 4.3V OMEGA = 1311C Increasing ramping rate to 1.0A/min.    Thursday, February 18, 2016, 13:10 TGHT reached to 450A, temp at 1800C.  Stepped up TGHT 490A, temp measured at ~1900C.

Thursday, February 18, 2016, 17:21

TGHT remained at max setpoint for 4hrs.

IGP1 = 6.6e-7 Torr.

OMEGA = 1913C

Initiating auto-cool for TGHT at 2.0A/min.

 Friday, February 19, 2016, 14:17

evap2 vented and opened up this morning.

container looks good.

Laura Lambert wrote:

Tuesday, February 16, 2016, 14:19 coated with TaC yesterday and let dry overnight. wrapped with one long Ta heat shield - wrapped around tube 3x, with Ta wire to offset Ta foil away from container loaded into evap2 and currently pumping down.  Wednesday, February 17, 2016, 10:51 HS water valves opened, no leaks detected. Tapped up manually to 35A. Waited ~20min, vacuum stable. IGP1 = 5.9e-7 Torr. Initiating auto-ramp at 0.2A/min to a final setpoint of 400A. Final desired temperature = 1900C  Thursday, February 18, 2016, 09:16 IGP1 = 6.6e-7 Torr. TGHT = 303A, 4.3V OMEGA = 1311C Increasing ramping rate to 1.0A/min.

 Thursday, February 18, 2016, 13:10

TGHT reached to 450A, temp at 1800C.  Stepped up TGHT 490A, temp measured at ~1900C. 

 Tuesday, February 16, 2016, 14:19

coated with TaC yesterday and let dry overnight.

wrapped with one long Ta heat shield - wrapped around tube 3x, with Ta wire to offset Ta foil away from container

loaded into evap2 and currently pumping down.

 Wednesday, February 17, 2016, 10:51

HS water valves opened, no leaks detected.

Tapped up manually to 35A.

Waited ~20min, vacuum stable.

IGP1 = 5.9e-7 Torr.

Initiating auto-ramp at 0.2A/min to a final setpoint of 400A.

Final desired temperature = 1900C

 Thursday, February 18, 2016, 09:16

IGP1 = 6.6e-7 Torr.

TGHT = 303A, 4.3V

OMEGA = 1311C

Increasing ramping rate to 1.0A/min.

 Friday, February 12, 2016, 11:01

Container coated with TaC with new method - ends tapped off,  liquid poured/swirled around container, then poured back out - 'flushing technique'.

Container wrapped with 3 x Ta heat shields, incl center block - new method of each layer being one long single Ta foil covering entire container incl center block

IGP1 = 6.3e-7Torr

HS water valves opened, no leaks detected.

Tapped up manually to 35A.

Waited ~20min.

Vacuum stable, IGP1 = 1.3e-6 Torr.

Initiated auto-ramp at 0.2A/min and 0.1A/min for the TGHT and TBHT respectively with final setpoints of 400A and 230A.

 Monday, February 15, 2016, 08:56

IGP1 = 3.9e-7 Torr.

TBHT = 230A, 4.0V

TGHT = 400A, 6.58V

OMEGA = 1766C

Tapping up manually to 1900C...

 Monday, February 15, 2016, 10:18

IGP1 = 5e-7 Torr

TGHT = 450A, 7.55V

OMEGA = 1913C

 Monday, February 15, 2016, 14:30

IGP1 = 4.9e-7 Torr.

TGHT = 450A, 7.55V.

Material remained at ~1910C for ~4hrs.

Initiating auto-cool at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

 Tuesday, February 16, 2016, 14:17

vented in air and opened up this morning.

target container sintered nicely.

 Tuesday, January 19, 2016, 14:19

SiC nanofiber was prepared at UBC Material Engineering Sci.  

4 samples are loaded in a Ta target contained (sintered with TaC coating): 

Sample 1: 

size:  21.70 x 21.54 mm, mass: 0.0762g, thick: 0.224mm

Sample 2: 

size: 20.89mm x 23.95mm, mass: 0.0954g, thick: 0.232mm 

--> Sample 1 and 2 with graphite backing foil 

Sample 3: 

size: 22.55 x 25.56mm, mass: 0.0082g, thick: 0.110mm

Sample 4: 16.93 x 23.82mm, mass: 0.0048g, thick: 0.086mm

--> Sample 3 and 4 with no graphite backing foil. 

(see attachment) 

Test#1:  Heating temperature at 1600C for 24hrs. 

TGHT will be adjusted accordingly.  There are 2 Ta-heat shields wrapped around the container. 

Chamber is currently being pumped down.

 Tuesday, January 19, 2016, 16:19

Vacuum at 2.0e-6 Torr.

For 1600C, expected current is around 350A.

Stepping up TGHT gradually...

 Wednesday, January 20, 2016, 14:34

TGHT was ramped up to 390A/6.63V to reach 1600C.  Samples have been heated at that temp since 11pm last night.

Visual check on the fibers seem ok (see attachment).

Will continue to heat this for a total time of 24hours.

 Wednesday, January 20, 2016, 22:57

Samples have been heated at 1600C for 24hours. 

Initiated cooling at 1A/min.

 Wednesday, January 27, 2016, 12:34

First attempt - heating 1600C.  XRD result showed board "bumps" that could be SiO2? It is inconclusive. 

Second attempt - re-heating the same samples, namely

Sample 1 - only the fiber

Sample 2 - with graphite backing.  This sample is loaded with the fiber facing down to see how well it holds on the graphite foil.  (see attachment)

TGHT will be ramped up to reach 1800C

Chamber is currently being pumped down.

 Wednesday, January 27, 2016, 14:04

Water valves open; no leaks detected.

Ramping up TGHT to 400A at 2A/min

 Wednesday, January 27, 2016, 18:08

TGHT is at 481A to obtain 1800C.

Visual check on Sample 2 - fiber has fallen off graphite backing foil.

Will remain heated at this temperature for over night.

 Friday, February 12, 2016, 11:11

Heat treatment test#1 is complete.  XRD results are inconclusive.  Need to do EDX to determine Si/SiO2.  

(See my dropbox for more details)

 Thursday, January 14, 2016, 11:47

Backing pump was making very loud high pitched noises during last couple processes in the evaporator.

Replaced with a new one this morning.

Monday, January 11, 2016, 15:25

Small center block LP-SIS container previously sintered with TaC coating

3x Ta heat shields

Container is loaded with 260 discs of SiC with a total length of 8.5cm

Loaded into evap2 and pumped down this morning

HS water valves opened up, no leaks detected

Tapped up manually to 30A

Vacuum stable

IGP1 = 1e-6 Torr

Initiating auto-ramp at 0.2A/min and 0.1A/min for the TGHT and TBHT respectively

Final setpoints: 400A for the TGHT and 230A for the TBHT

Final desired temperature: 1700C

 Tuesday, January 12, 2016, 12:55

TGHT = 138A, TBHT = 80A

IGP1 =  7.7e-6 Torr.

Vacuum stable and coming down.

Increasing ramping rate to 0.5A/min and 0.2A/min for the TGHT and TBHT respectively.

 Wednesday, January 13, 2016, 09:32

TGHT reached 400A ~11.5hrs ago

TBHT reached 230A ~8hrs ago

OMEGA = 1400C

IGP1 = 1.75e-7 Torr

Tapping up manually to 1700C...

 Wednesday, January 13, 2016, 10:14

Previous temperature measurement of OMEGA = 1400C is wrong due to window port being coated with SiC [see attached photos]

Will remain at TGHT = 420A for 4hrs then cool down this afternoon

Wednesday, January 13, 2016, 14:29

Remained at max setpoints for 4.5hrs.

Initiating auto-cool at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

 Thursday, January 14, 2016, 09:47

Vented in air and opened up this morning

Target looks good

Will insert and expand endcaps this afternoon

Aurelia Laxdal wrote:

Temperature measurements in progress this week for Ta HP-SIS.

 Friday, January 08, 2016, 10:49

Rh foil added.

endcaps inserted and expanded.

total length of target with end caps = 3.45cm

spot weld one thermocouple onto center block and one thermocouple onto target leg [left side wrt ionizer tube into page].

 see elog id# 268 for more info regarding measurements taken and state of TBHT power supply...

Temperature measurements in progress this week for Ta HP-SIS.

See attachment for the current settings and rampings of the TGHT/TBHT  for the temperature measurements taken on  Jan. 9-10, 2016 .

Note: TBHT PS tripped off on Jan. 9, 2016 (see first page of the attached file) and couldn't turn it ON again over the week-end.

 Wednesday, December 16, 2015, 10:09

Target consists of 505 discs.

Total packed length 3.4cm.

*same parameters at Ta#46*

Total mass of target materials 53.9381g [4 packs of 20 with Ta wire + 425 single discs].

3 x Ta Heat shields.

No Re foil inserted.

No endcaps inserted.

Chamber pumped down overnight.

IGP1 = 5.1e-7 Torr.

Tapped up manually to 35A.

IGP1 = 5.2e-7 Torr.

Vacuum stable, initiating auto-ramp.

TBHT will be ramped up to 230A at 1.0A/min.

TGHT will be ramped up to 1800C, auto ramp to 600A at 2.0A/min [estimated final value of 720A according to elog ID 239]

 Wednesday, December 16, 2015, 15:08

TBHT reached max setpoint of 230A, 3.3V

TGHT = 600A, 8.9V

IGP1 = 1.1e-6 Torr.

OMEGA = 1543C

Increasing final setpoint of TGHT to 700A and re-initiating auto-ramp.

 Wednesday, December 16, 2015, 16:02

TGHT = 700A, 10.6V

IGP1 = 2.1e-6 Torr.

OMEGA = 1740C

Tapping up manually to 1800C.

 Wednesday, December 16, 2015, 16:28

TGHT = 730A, 11.2V

Vacuum is coming down from IGP1 = 2.6e-6 Torr.

OMEGA = 1800C

Will condition the target at 1800C overnight and ramp down in the morning.

 Thursday, December 17, 2015, 09:31

OMEGA = 1802C on right side

Temp on leg of left side = 2150C, the hottest point - measured with the Mikron pyrometer.

 Friday, December 18, 2015, 08:53

Evap2 remained at 1800C for ~26.5hrs

Auto-ramped down to TGHT = 300A and TBHT = 90A at a rate of 2.0A/min and 1.0A/min respectively.

Conditioning complete.

TGHT will be ramped up later today for emissivity measurements.

 Monday, January 04, 2016, 11:21

the following was performed by aurelia.

emissivity measurements were taken late december.

evap2 was cooled down and left under vacuum over the xmas break.

currently ramping back up for more emissivity measurements.

 Friday, January 08, 2016, 10:47

Aurelia done measurements.

vented and opened this morning.

 Monday, December 07, 2015, 09:04

No heat shields.

Container empty.

IGP1 = 1.1e-7 Torr.

Slope of OMEGA = 0.98

Tapped up manually to 35A.

Vacuum stable, initiating auto-ramp at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

Final setpoints: TBHT = 90A, TGHT = 360A

Will tap up with the same parameters as last round to confirm results.

 Friday, December 11, 2015, 11:44

Took out of evap2 yesterday.

Aurelia took many emissivity measurements to compare with previous data - which matched up.

The dip in emissivity before going up again around ~560A could be due to oxidation of the materials.

 Data from thermocouple attached. Raw data and Excel sheet with plot.

 Monday, November 30, 2015, 15:37

No heat shields.

Container empty.

Loaded into evap2 and currently pumping down.

Tuesday, December 01, 2015, 10:07 

HS water valves opened this morning, no leaks detected.

IGP1 = 4.3e-7 Torr.

Slope of OMEGA = 0.98

Tapped up manually to 35A.

Vacuum stable, initiating auto-ramp at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

Final setpoints: TBHT = 90A, TGHT = 360A

Once final setpoints reached, will tap up manually to max 1800C [legs = 2000C]

 Monday, December 07, 2015, 09:06

Container was tapped up manually with emissivity measurements taken every 50A starting at 360A.

The final measurement was taken at 640A.

Container was ramped down for the weekend.

See attachment for raw data.

Monday, November 23, 2015, 14:29

No heat shields.

Container empty.

Loaded into evap2 and currently pumping down.

 Tuesday, November 24, 2015, 09:36

HS water valves opened this morning, no leaks detected.

IGP1 = 4.5e-7 Torr.

Changed slope of OMEGA IR to 0.98 for empty container.

Tapped up manually to 35A.

IGP1 = 4.7e-7 Torr.

Vacuum stable, initiating auto-ramp at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

Final setpoints: TBHT = 230A, TGHT = 300A

Will tap up manually to 2000C

 Tuesday, November 24, 2015, 14:00

TGHT = 300A, 3.75V

TBHT = 230A, 3.08V

IGP1 = 4.7e-7 Torr

No reading yet on the OMEGA.

Re-initiating auto-ramp to final setpoint TGHT = 450A

 Wednesday, November 25, 2015, 09:11

IGP1 = 3.0e-7Torr.

TGHT = 450A, 6.37V

Tapping up manually to 2000C

 Wednesday, November 25, 2015, 15:31

container was tapped up manually to 650A, slope/emissivity settings were checked.

ramped back down to 450A and tapped up manually while recording data up to 1800C [legs = 2000C]

once reached 1800C, tapped TBHT down manually to see relation of TBHT to temperature/ TGHT

remained at 1800C for ~1hr [while tapping down TBHT] before initiating auto-cool at 2.0A/min for the TGHT

see attachment for raw data.

 Thursday, November 26, 2015, 10:08

Vented in air and took out this morning.

 Tuesday, November 10, 2015, 14:20

Container previously sintered with TaC coating and temperature measurements taken [see elog ID# 256, 257, 258]

3x Ta heat shields

2 packs of 5 SiC discs ~2inches from the end of the right side wrt ionizer tube into page.

Loaded into evap2 and currently pumping down.

see photos attached.

 Monday, November 16, 2015, 11:24

HS water valves opened up this morning, no leaks detected.

Tapped up manually to 35A.

Vacuum stable.

IGP1 = 3.4e-7 Torr.

Initiating auto-ramp at 1.0A/min and 0.5A/min for the TGHT and TBHT respectively.

Final setpoints: 250A for the TGHT and 230A for the TBHT

Monday, November 16, 2015, 13:29

Vacuum too high.

IGP1 = 2.9e-5 Torr.

Decreasing ramping rate down to 0.5A/min and 0.2A/min for the TGHT and TBHT respectively.

 Tuesday, November 17, 2015, 09:12

IGP1 = 1.45e-7 Torr.

TGHT = 250A, 3.28V

TBHT = 230A, 3.33V

OMEGA = 1194C

Tapping up manually to 1900C

 Tuesday, November 17, 2015, 11:22

Tapped up manually to 1800C, realized SiC should only be tapped up to 1700C, backed off immediately down to 415A from 460A/ 1800C.

See attachment for photo of striptool/ time spent above 1700C [~20min].

 Tuesday, November 17, 2015, 15:46

TGHT remained at 1700C for ~4hrs.

TGHT = 420A, 6.44V.

IGP1 = 2.3e-7 Torr.

Initiating cool-down at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

See attachment for raw data of temperature measurements.

 Wednesday, November 18, 2015, 13:32

Vented in air and took out this morning.

Looks good, no visual changes with the container.

John Wong wrote:

Laura Lambert wrote:  Thursday, November 05, 2015, 16:19 Springs coated with TaC and loaded into container for sintering. 3x Ta heat shield. EVAP2 currently pumping down.  Friday, November 06, 2015, 08:39 Opened HS water valves, no leaks detected. Tapped up manually to 35A. IGP1 = 5.5e-7 Torr.  Friday, November 06, 2015, 10:08 IGP1 = 5.8e-7 Torr. Vacuum stable. Initiating auto-ramp at 0.2A/min and 0.1A/min with final setpoints of 450A and 230A for the TGHT and TBHT respectively. See photos attached to view how springs were coated and loaded into container.  Monday, November 09, 2015, 09:07 TGHT reached 450A, 7.2V ~8pm sat, nov 7th. OMEGA = 1775C IGP1 = 3.2e-7 Torr. Tapping up manually to 1900C.    Monday, November 09, 2015, 12:30 Checked the temp on the inner surface (not at the spring) of the container was around 2050C at 500A.  The TaC coated spring is reading at 1900C; that's what the OMEGA is reading with the setting for 2-colors and slope at 0.98. Lower TGHT to 450A/ 7.12V. By comparing the data from the previous temp curve (OMEGA slope at 0.98) with no material inside the container,  the voltage and current plot is aligned with the curve. Changed OMEGA setting slope to 1.04.  Current temp is reading at 1917C at 450A. For 2-Color setting, the emissivity should be negligible.  That makes me believe that different materials has different slope setting for the temp reading.   One thing to note is that, the sintering temp of TaC is around 1900-2000C.  It was clear that the container was fully sintered with TGHT at 450A. Will need to gather more data with different material to understand the slope setting better.  Try:  SiC at 1700C, slope at 1.04 ZrC at 1900C, slope at 104 Ta at 1900C, slope at 0.98. Compare the data...

 Monday, November 09, 2015, 14:20

IGP1 = 3.3e-7 Torr.

TGHT = 450A, 7.12V

OMEGA = 1915C

Initiating auto-cool at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

 Tuesday, November 10, 2015, 13:23

Vented and opened this morning.

springs look [mostly] sintered.

see photo attached.

Laura Lambert wrote:

Thursday, November 05, 2015, 16:19 Springs coated with TaC and loaded into container for sintering. 3x Ta heat shield. EVAP2 currently pumping down.  Friday, November 06, 2015, 08:39 Opened HS water valves, no leaks detected. Tapped up manually to 35A. IGP1 = 5.5e-7 Torr.  Friday, November 06, 2015, 10:08 IGP1 = 5.8e-7 Torr. Vacuum stable. Initiating auto-ramp at 0.2A/min and 0.1A/min with final setpoints of 450A and 230A for the TGHT and TBHT respectively. See photos attached to view how springs were coated and loaded into container.  Monday, November 09, 2015, 09:07 TGHT reached 450A, 7.2V ~8pm sat, nov 7th. OMEGA = 1775C IGP1 = 3.2e-7 Torr. Tapping up manually to 1900C.

 Monday, November 09, 2015, 12:30

Checked the temp on the inner surface (not at the spring) of the container was around 2050C at 500A. 

The TaC coated spring is reading at 1900C; that's what the OMEGA is reading with the setting for 2-colors and slope at 0.98.

Lower TGHT to 450A/ 7.12V.

By comparing the data from the previous temp curve (OMEGA slope at 0.98) with no material inside the container,  the voltage and current plot is aligned with the curve.

Changed OMEGA setting slope to 1.04.  Current temp is reading at 1917C at 450A.

For 2-Color setting, the emissivity should be negligible.  That makes me believe that different materials has different slope setting for the temp reading.  

One thing to note is that, the sintering temp of TaC is around 1900-2000C.  It was clear that the container was fully sintered with TGHT at 450A.

Will need to gather more data with different material to understand the slope setting better. 

Try: 

SiC at 1700C, slope at 1.04

ZrC at 1900C, slope at 104

Ta at 1900C, slope at 0.98.

Compare the data...