John Wong wrote:

Aurelia Laxdal wrote: Aurelia Laxdal wrote: Aurelia Laxdal wrote: Aurelia Laxdal wrote: Anders Mjos wrote: Laura Lambert wrote: Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.    Monday, March 14, 2016, 13:12: Stopped turbo pump  After EVAP2 was vented the thermocouple problem was fixed: it was the wire at on connector inside the box not making proper contact. The lid of the heat shield was also replaced since the one initially mounted had no holes, so one couldn't see the center block. Restarted pumping down at 4:30pm. Just started again the autoramp program: TGHT set to 300A (for the time being) and TBHT to 230A. Temperature measurements will resume tomorrow morning.  Raised the TGHT at 620A. The TBHT was already set at 230A. The temperature is at 1902 deg C. As per John's instructions the target will condition at these setpoints over the week-end. Today, lowered the TGHT from 620A (at 1894 deg C) to 300A.  TBHT is still at 230A.  Cooling down the target.   Thursday, March 24, 2016, 11:29  Target was removed from the Evaporator.   The thermocouples broke off.   Need to insert Re foil prior to installing

 Tuesday, April 19, 2016, 09:28: Uploaded thermoucouple data.

Thursday, April 07, 2016, 15:18

E-spun SiC/PAN fiber mats were produced at UBC.

12%PAN solution; 50% SiC to weight of PAN.

Materials used:

1.2g PAN, 8.8g DMF, 0.6g SiC, SDS ~0.1% to SiC

Fiber mats were heat treated at 250C in air.  Then cut into 18" discs and loaded into Ta target boat with heatshield wrapped. 

3 temperature treatments will carry out: 1200C, 1400C and 1600C

Chamber is being pumped down

 Friday, April 08, 2016, 10:02

TGHT at 285A, Temp at ~1200C.  Will remain at this temp for a few hours before cooling down. 

Some samples will be taken out for analysis. 

Next week, temperature treatment will continue at 1400C

 Friday, April 08, 2016, 14:26

Samples have been heated at 1200C for just over 4 hours.

Initiated auto-cooling at 2A/min

 Tuesday, April 12, 2016, 17:51

Heat treatment #2 - 1400C. 

Initial mass after 1200C = 0.0312g

 Monday, April 18, 2016, 12:55

Samples was heated at 1400C (TGHT maintained at ~370A) for 4 days (see attachment 1).

Chamber is vented; samples will be inspected.

 Tuesday, April 19, 2016, 17:49

Results

Sample mass after 1200C = 0.0312g

Sample mass after 1400C = 0.0294g

~5.78% mass  loss. 

Tuesday, April 19, 2016, 17:57

Heat Treatment#3: 1600C

sample mass before heating = 0.0238g (this sample is taken from the batch after it was heated at 1400C)

Chamber is being pumped.

 Thursday, April 21, 2016, 11:07

TGHT stepped up to 330A, temp measured at 1422C.

 Thursday, April 21, 2016, 12:05

TGHT at 415A/7.16V; temp at 1610C

 Thursday, April 21, 2016, 17:49

Temp dropped to 1590.  Increased TGHT to 425A; temp reads 1602A.

 Friday, April 22, 2016, 10:57

Voltage increased to 7.33V, TGHT stepped down to 418A, temp maintained at 1610A.

 Monday, April 25, 2016, 12:08

Sample was heat treated for almost 4 days.  Temperature dropped to 1578C, TGHT at 418/7.26V.  (see attachment #2)

Ramping down TGHT 2A/min.

 Monday, April 25, 2016, 16:00

Result:

Mass after 1600C = 0.0104g, 5.63% mass loss. 

Will do XRD/EDX

Wednesday, March 30, 2016, 11:30

Polycarbosilane fibers were prepared by UBC MTRL. 

Two samples with different fiber sizes were loaded in target boat and wrapped with heat shields.

Samples will be heated up to 1600C.

Chamber is currently being pumped down

 Thursday, March 31, 2016, 16:49

Ramping up TGHT to 300A at 1A/min

 Tuesday, April 05, 2016, 13:02

Samples was heated at 1600C for about 3 hours.  

Then it was cooled down at 2A/min. 

The process is complete. 

Thursday, March 24, 2016, 11:37  

SiC powder (<1um) [10%] was mixed with PAN solution [10%].  Solution was sonicated before e-spinning.  

Fiber mat was binded to graphite foil and heat treated to 250C in air for 1 hour.  

Samples were cut in pieces and rolled up and inserted in Ta target container (TaC coated).  Heat shield was added.

Heat Treatment #1:  

Temperature:  1600C (~350A)

Ramping up TGHT to 300A at 1A/min.  

 Tuesday, March 29, 2016, 11:11

TGHT was maintained at 410A for 1600C for 2 days (see attachment 1).  However at around 22:30 on March 28, there was a sudden increase in voltage.

Temperature raised up to 1750C.  Not sure there was a fault with the control system and it was caused by the Ta-heat shield. (see attachment #2).

 Target was cooled down around 2am on March 29. 

Samples will be removed from the chamber.

Aurelia Laxdal wrote:

Aurelia Laxdal wrote: Aurelia Laxdal wrote: Aurelia Laxdal wrote: Anders Mjos wrote: Laura Lambert wrote: Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.    Monday, March 14, 2016, 13:12: Stopped turbo pump  After EVAP2 was vented the thermocouple problem was fixed: it was the wire at on connector inside the box not making proper contact. The lid of the heat shield was also replaced since the one initially mounted had no holes, so one couldn't see the center block. Restarted pumping down at 4:30pm. Just started again the autoramp program: TGHT set to 300A (for the time being) and TBHT to 230A. Temperature measurements will resume tomorrow morning.  Raised the TGHT at 620A. The TBHT was already set at 230A. The temperature is at 1902 deg C. As per John's instructions the target will condition at these setpoints over the week-end. Today, lowered the TGHT from 620A (at 1894 deg C) to 300A.  TBHT is still at 230A.  Cooling down the target.

Thursday, March 24, 2016, 11:29 

Target was removed from the Evaporator.  

The thermocouples broke off.  

Need to insert Re foil prior to installing

Aurelia Laxdal wrote:

Aurelia Laxdal wrote: Aurelia Laxdal wrote: Anders Mjos wrote: Laura Lambert wrote: Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.    Monday, March 14, 2016, 13:12: Stopped turbo pump  After EVAP2 was vented the thermocouple problem was fixed: it was the wire at on connector inside the box not making proper contact. The lid of the heat shield was also replaced since the one initially mounted had no holes, so one couldn't see the center block. Restarted pumping down at 4:30pm. Just started again the autoramp program: TGHT set to 300A (for the time being) and TBHT to 230A. Temperature measurements will resume tomorrow morning.  Raised the TGHT at 620A. The TBHT was already set at 230A. The temperature is at 1902 deg C. As per John's instructions the target will condition at these setpoints over the week-end. Today, lowered the TGHT from 620A (at 1894 deg C) to 300A.  TBHT is still at 230A.

 Cooling down the target.

Aurelia Laxdal wrote:

Aurelia Laxdal wrote: Anders Mjos wrote: Laura Lambert wrote: Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.    Monday, March 14, 2016, 13:12: Stopped turbo pump  After EVAP2 was vented the thermocouple problem was fixed: it was the wire at on connector inside the box not making proper contact. The lid of the heat shield was also replaced since the one initially mounted had no holes, so one couldn't see the center block. Restarted pumping down at 4:30pm. Just started again the autoramp program: TGHT set to 300A (for the time being) and TBHT to 230A. Temperature measurements will resume tomorrow morning.  Raised the TGHT at 620A. The TBHT was already set at 230A. The temperature is at 1902 deg C. As per John's instructions the target will condition at these setpoints over the week-end.

Today, lowered the TGHT from 620A (at 1894 deg C) to 300A.  TBHT is still at 230A.

Aurelia Laxdal wrote:

Anders Mjos wrote: Laura Lambert wrote: Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.    Monday, March 14, 2016, 13:12: Stopped turbo pump  After EVAP2 was vented the thermocouple problem was fixed: it was the wire at on connector inside the box not making proper contact. The lid of the heat shield was also replaced since the one initially mounted had no holes, so one couldn't see the center block. Restarted pumping down at 4:30pm. Just started again the autoramp program: TGHT set to 300A (for the time being) and TBHT to 230A. Temperature measurements will resume tomorrow morning.

 Raised the TGHT at 620A. The TBHT was already set at 230A. The temperature is at 1902 deg C. As per John's instructions the target will condition at these setpoints over the week-end.

Anders Mjos wrote:

Laura Lambert wrote: Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.    Monday, March 14, 2016, 13:12: Stopped turbo pump

 After EVAP2 was vented the thermocouple problem was fixed: it was the wire at on connector inside the box not making proper contact. The lid of the heat shield was also replaced since the one initially mounted had no holes, so one couldn't see the center block. Restarted pumping down at 4:30pm. Just started again the autoramp program: TGHT set to 300A (for the time being) and TBHT to 230A. Temperature measurements will resume tomorrow morning.

Laura Lambert wrote:

Aurelia Laxdal wrote: 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).  Monday, March 14, 2016, 09:20 One thermocouple was not welded on correctly and is not working.  Cooling evap2 back down, to remove target and re-weld thermocouple. Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.

 Monday, March 14, 2016, 13:12: Stopped turbo pump

Aurelia Laxdal wrote:

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).

 Monday, March 14, 2016, 09:20

One thermocouple was not welded on correctly and is not working. 

Cooling evap2 back down, to remove target and re-weld thermocouple.

Once thermocouple replaced, will ramp back up and continue with tests/ conditioning of target.

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.