Thursday, February 09, 2017, 11:47

A new heatshield with flexible water lines has been put into evap2 last Friday Feb3rd

Thursday, February 09, 2017, 23:26

There are two types of samples being test for thermal stability:

1.  SiC-SiO2-Lys nanofiber mats

2.  SiC pellets

(see Lab Book for more info)

Desired temperature: ~1500C

One-Ta heat shield is used, est. TGHT 450A.

 Thursday, February 09, 2017, 23:38

TGHT currently at 322A/5.28V, OMEGA 1204C.

Vac 2.9e-6 Torr.

 Friday, February 10, 2017, 08:58

TGHT at 400A, temp at 1425C for 8 hours.

Decided to cool down for analysis.  Check for carboreduction for SiO2 at 1400C.  Then continue to ramp up to 1500C. 

Ramping down at 2A/min

 Friday, February 10, 2017, 10:47

Rapid out-gas (2.7e-6 to 3.8e-6 Torr) from TGHT 330A until current stopped at 400A (see attachment).  Could be the evolution of O2 from SiO2... 

Laura Lambert wrote:

Friday, February 03, 2017, 14:17 The endcaps are stacked together with a punched out disc of graphite foil placed in between each endcap for separation so endcaps won't fuse together. The end caps are further wrapped in a larger piece of graphite foil to hold together as a tube [same method used in elogID # 158 and 235] There are also 4 coated springs, 2 on each side of the endcaps tube, with the endcaps tube residing in the middle of the boat. The boat is wrapped with 3-layers of Ta heatshields. Chamber is currently being pumped down. Good vac at 3.0e-5, bad vac at 4.0e-5 Torr. OMEGA slope = 0.98  Monday, February 06, 2017, 09:29 Power outage this weekend and evap2 tripped off. Re-pumping down now...  Tuesday, February 07, 2017, 08:54 HS water valves opened, no leaks detected. IGP1 = 1.9e-7 Torr Tapped up manually to 35A Vacuum stable. IGP1 = 2.0e-7 Torr Initiating auto-ramp at 0.2A/min with a final setpoint of 450A. Final desired temperature = 1800C  Wednesday, February 08, 2017, 09:52 IGP1 = 2.98e-7 Torr TGHT = 325A, 3.5V Vacuum stable. Increasing ramping rate to 1.0A/min  Wednesday, February 08, 2017, 11:46 IGP1 = 6.3e-7 Torr TGHT = 433A, 4.89V Increasing max setpoint to TGHT = 500A OMEGA has still yet to show a temperature...should be reading points at this high in current Will go down to the lab and follow up on OMEGA settings to confirm everything is set up ok before proceeding to a higher current...  Wednesday, February 08, 2017, 16:03 IGP1 = 4e-7 Torr TGHT = 500A, 5.75V OMEGA still not reading Initiating auto-cool at -2A/min Will update elog with more details tomorrow  Thursday, February 09, 2017, 10:52 Evap2 was cooled down and opened up this morning. Turns out both legs on the target boat were touching the new heatshield and therefore had been loosing power. Normally a boat at 500A would read ~1800C, in this scenario at 500A the boat read ~1000C. A lot of power was being lost into the heatshield. See photos attached of target boat sitting at 500A. The heatshield is currently being ground down in those two spots to accommodate the target boat.

 Tuesday, February 14, 2017, 15:43

Heatshield was ground back and target boat now fits nicely into heatshield without contact.

Laura Lambert wrote:

Laura Lambert wrote:  Friday, February 03, 2017, 14:17 The endcaps are stacked together with a punched out disc of graphite foil placed in between each endcap for separation so endcaps won't fuse together. The end caps are further wrapped in a larger piece of graphite foil to hold together as a tube [same method used in elogID # 158 and 235] There are also 4 coated springs, 2 on each side of the endcaps tube, with the endcaps tube residing in the middle of the boat. The boat is wrapped with 3-layers of Ta heatshields. Chamber is currently being pumped down. Good vac at 3.0e-5, bad vac at 4.0e-5 Torr. OMEGA slope = 0.98  Monday, February 06, 2017, 09:29 Power outage this weekend and evap2 tripped off. Re-pumping down now...  Tuesday, February 07, 2017, 08:54 HS water valves opened, no leaks detected. IGP1 = 1.9e-7 Torr Tapped up manually to 35A Vacuum stable. IGP1 = 2.0e-7 Torr Initiating auto-ramp at 0.2A/min with a final setpoint of 450A. Final desired temperature = 1800C  Wednesday, February 08, 2017, 09:52 IGP1 = 2.98e-7 Torr TGHT = 325A, 3.5V Vacuum stable. Increasing ramping rate to 1.0A/min  Wednesday, February 08, 2017, 11:46 IGP1 = 6.3e-7 Torr TGHT = 433A, 4.89V Increasing max setpoint to TGHT = 500A OMEGA has still yet to show a temperature...should be reading points at this high in current Will go down to the lab and follow up on OMEGA settings to confirm everything is set up ok before proceeding to a higher current...  Wednesday, February 08, 2017, 16:03 IGP1 = 4e-7 Torr TGHT = 500A, 5.75V OMEGA still not reading Initiating auto-cool at -2A/min Will update elog with more details tomorrow  Thursday, February 09, 2017, 10:52 Evap2 was cooled down and opened up this morning. Turns out both legs on the target boat were touching the new heatshield and therefore had been loosing power. Normally a boat at 500A would read ~1800C, in this scenario at 500A the boat read ~1000C. A lot of power was being lost into the heatshield. See photos attached of target boat sitting at 500A. The heatshield is currently being ground down in those two spots to accommodate the target boat.    Tuesday, February 14, 2017, 15:43 Heatshield was ground back and target boat now fits nicely into heatshield without contact.

 Tuesday, February 14, 2017, 15:44

Boat with endcaps and springs reloaded today and pumped back down this afternoon.

HS water valves opened, no leaks detected.

Tapped up manually to 35A

Vacuum stable.

IGP1 = 3.5e-6 Torr

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

Final desired temperature = 1800C

 Wednesday, February 15, 2017, 10:24

IGP1 = 7.2e-7 Torr

TGHT = 260A, 3.95V

OMEGA = 1158C

Vacuum stable.

Increasing ramping rate to 1.0A/min.

 Wednesday, February 15, 2017, 13:02

IGP1 = 2.0e-6 Torr

TGHT = 400A, 6.67V

OMEGA = 1530C

Increasing final setpoint to 450A

 Wednesday, February 15, 2017, 13:55

IGP1 = 2.5e-6 Torr

TGHT =450A, 7.7V

OMEGA = 1640C

Increasing final setpoint to 500A

 Wednesday, February 15, 2017, 15:13

IGP1 = 1.8e-6 Torr

TGHT = 500A, 8.59V

OMEGA = 1770C

MIKRON = 1740C

Tapping up manually to ~1800C...

 Thursday, February 16, 2017, 09:09

IGP1 = 5.28e-7 Torr

TGHT = 520A, 9.1V

OMEGA = 1821C

Target boat has remained at max setpoints for 17.5hrs.

Initiating auto-cool at 1A/min

 Thursday, February 16, 2017, 13:49

Increasing auto-cool to 2.0A/min

 Friday, February 17, 2017, 16:00

Vented in air and opened up today.

Endcaps looks good  see photos attached

Friday, March 10, 2017, 17:29

Three B3 pellets are loaded into the container for thermo test. 

(see lab book1 Pg 26, 28-30 for more detail about the materials)

Desired temp ~1500C; one long-sheet of Ta foil is used, est 400A. 

Auto ramping 0.5A/min to 300A first.  Check later...

 Saturday, March 11, 2017, 11:58

Increased TGHT from 300A to 350A last night at ramping rate of 0.5A/min.

Tapped up further from 350A to 400A, 6.92V (2.8kW), Temp measured at ~1550C. 

Pressure peaked at 1.5e-6 Torr and coming down when ramping TGHT from 350A to 400A. (see attachment1)

Will remain at the current.  Continue monitoring..

 Monday, March 13, 2017, 01:14

Temp was held at 1550C for about 1.5days. Vac stabilized at 3.08e-7 torr.  TGHT 400A/6.94V.

Initiated cooling at 1A/min. 

Next, Materials inspection.

 Monday, March 13, 2017, 11:24

Target has been at room temp for about 4 hours.  Venting chamber.

Friday, March 31, 2017, 12:21

Two compressed pellets loaded into the target boat and wrapped with Ta foil.  (see lab book p32 for details).

Chamber is pumping down.

Desired temp 1550C, TGHT expected to be around 400A.

 Friday, March 31, 2017, 16:31

Auto-ramp at 0.5A/min to reach 350A.

 Saturday, April 01, 2017, 12:30

TGHT reached to 350A/5.7V, temp around 1200C - notice voltage is much lower than previous process (ID 351), possible target/heat shield shorted therefore lower temp observed. (This should not cause any damage to the container.) 

Continue to ramp up to 400A.  Notice some evolution of gasses similar to the previous process (ID351) during ramping up of TGHT around 220A . (see attachment1)

 Saturday, April 01, 2017, 13:52

TGHT reached to 400A/6.7V; temp stabilized at 1400C. 

Tap up to 1550, TGHT 456A/8.08V (3.7KW, about 1KW higher than before).

Pressure coming down (see attachment 2)

Hold temp for several days.

 Saturday, April 01, 2017, 17:22

Temp went up by 10C. Lowered TGHT to 450A.

 Wednesday, April 05, 2017, 15:36

Coated container with TaC coating using spray technique this morning and let dry.

Wrapped with one long layer of Ta heat shield, wrapped around boat 3x

No ends to target boat

Installed in evap2 and pumping down now...

Laura Lambert wrote:

Wednesday, April 05, 2017, 15:36 Coated container with TaC coating using spray technique this morning and let dry. Wrapped with one long layer of Ta heat shield, wrapped around boat 3x No ends to target boat Installed in evap2 and pumping down now...

 Thursday, April 06, 2017, 08:56

Problems with IGP2

Won't turn on, has low voltage output.

See screenshot attached.

Laura Lambert wrote:

Laura Lambert wrote:  Wednesday, April 05, 2017, 15:36 Coated container with TaC coating using spray technique this morning and let dry. Wrapped with one long layer of Ta heat shield, wrapped around boat 3x No ends to target boat Installed in evap2 and pumping down now...    Thursday, April 06, 2017, 08:56 Problems with IGP2 Won't turn on, has low voltage output. See screenshot attached.

 Thursday, April 06, 2017, 11:12

Turns out it was just a bad connection.

See attached photos.

 Thursday, April 13, 2017, 12:01

Pellets made this morning and weighed.

Placed in a graphite boat which is placed inside a previously TaC coated boat.

Boat is wrapped with 3x Ta heat shields.

Loaded into evap2.

Chamber currently pumping down.

 Tuesday, April 18, 2017, 13:53

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

Tapped up manually to 100A, 1.28V

Vacuum stable.

IGP1 = 3.63e-6 Torr.

Initiating auto ramp at a rate of 1.0A/min to 150A

Final desired temperature of 1100C

 Tuesday, April 18, 2017, 14:57

TGHT = 150A, 2.08V

Still no temperature reading on OMEGA.

Vacuum stable, IGP1 = 1.16e-6 Torr.

Initiating auto ramp at the same rate of 1.0A/min up to 200A.

 Tuesday, April 18, 2017, 15:56

TGHT = 200A, 2.91V

OMEGA = 990C

IGP1 = 8.59e-7 Torr

Tapping up manually to 1100C...

 Wednesday, April 19, 2017, 08:34

TGHT = 235A, 3.47V

OMEGA = 1090C

IGP1 = 1.6e-7 Torr.

Has remained at ~1100C since 16:30 yesterday.

Intitiating auto-cool at 2.0A/min

 Thursday, April 20, 2017, 08:40

Vented in air and taken out yesterday.

Pellets look good.

No obvious colour change.

Thursday, April 20, 2017, 12:38

3 samples are loaded into the Ta boat and wrapped with heat shield (1 long piece, 3 rounds):  2x of B3-92Mpa pellets and 10% pure PAN pellet as control.  See lab book page 32 for more details.

The B3-92Mpa pellets were previously heated to 1550C (TGHT 400A/6.94V), see elog#351

Attempting to heat samples up to 1800C to determine the weight loss and shrinkage. 

Est. TGHT 480A.

OK to auto ramp to 400A at 1A/min.  Check for coating on the window. 

Chamber is currently being pumped down.

 Thursday, April 20, 2017, 14:28

Pressure 3.14e-6 Torr.  Auto ramp TGHT at 1A/min to reach 400A. 

 Friday, April 21, 2017, 10:56

TGHT at 400A/6.75V, temp at 1475C (75C/0.19V lower). 

Tapping up TGHT

 Friday, April 21, 2017, 12:32

TGHT ramped up to 530A/9.85V, temp at 1800C. 

 Friday, April 21, 2017, 15:38

TGHT dropped slightly, no coating on windows. 

Checked with Mikron, agreed with the dropped temp. 

Tapped up TGHt to 545A/10.1V to reach 1800C.  Will keep at that temp for several days.

 Wednesday, April 26, 2017, 17:06

Samples have been heated at 1800C (-25C) for 7 days now (see attachment for archiver). 

Cooling down TGHT at 1A/min.

 Monday, May 08, 2017, 10:05

Turbo pump control box died last week.

Replaced with a new one.

 Wednesday, May 10, 2017, 16:05

Loaded.

HS water valves opened, no leaks detected.

Started auto-ramp at a rate of 1A/30sec to a final setpoint of 580A

Laura Lambert wrote:

Wednesday, May 10, 2017, 16:05 Loaded. HS water valves opened, no leaks detected. Started auto-ramp at a rate of 1A/30sec to a final setpoint of 580A

 Wednesday, May 10, 2017, 21:31: TGHT at 580 A for 1 h. Vacuum came down to 1.4E-6 Torr. TGHT voltage stable. Ramping down.

Anders Mjos wrote:

Laura Lambert wrote:  Wednesday, May 10, 2017, 16:05 Loaded. HS water valves opened, no leaks detected. Started auto-ramp at a rate of 1A/30sec to a final setpoint of 580A    Wednesday, May 10, 2017, 21:31: TGHT at 580 A for 1 h. Vacuum came down to 1.4E-6 Torr. TGHT voltage stable. Ramping down.

 Thursday, May 11, 2017, 10:51

vented in air and opened it up this morning.

Heat shield looks good!

 Thursday, May 11, 2017, 11:25

IGP2 has been having problems where sometimes it turns off and requires simply unplugging and plugging back in.

Ion gauge has been replaced.

At first the vacuum box appeared red on epics and when attempting to reset everything nothing would work and the backing pump would try and turn on then timeout.

Apparently this new ion gauge draws slightly more than the old one and this blew a fuse in the PLC.

Old fuse was 2A, so a new 3A fuse has been replaced - seems to be working fine now. 

Monday, July 10, 2017, 17:28

Two np-SiC fibrous pellets with different applied pressure:

1) 200MPa, 2)  335 MPa (see logbook pg 36 for more details). 

Desired heating temperature: 1550C (Previous setting: TGHT 400A/6.94V)

Two layers of Ta foils wrapped around the target boat.

Chamber is pumping down...

 Tuesday, July 11, 2017, 11:11

Pressured came down to 1.0e-6 Torr. 

Tapping up TGHT.

 Tuesday, July 11, 2017, 11:24

Tapped TGHT up to 45A - pressure stabilized at around 3.0e-5 Torr. 

Auto ramp 1.0A/min to reach 350A before tapping up further.

 Wednesday, July 12, 2017, 10:59

TGHT reached to 350A/5.5V, temp @ 1270C - much lower than expected; could be a short between the target container and the heat shield.  I actually had a had time adjusting the target legs to avoid shorting the cu-heat shield. 

Tapped TGHT further up to 375A/6.07V, Omega Temp at 1340C.  Holding current for about 50 mins, re-measured with pyrometer - temperature matches.

Wednesday, July 12, 2017, 14:49 

TGHT set at 450A/7.7A.  Temp at ~1550C.  See attachment for temp plot

Holding at temp for 5 days before cooling down on Monday July 17.

 Thursday, July 13, 2017, 17:52

TGHT tripped off due to bad IEVAP2:WFB1 water flow.  Not sure what was the cause.  Will leave the heater off for now and investigate this tomorrow.

 Friday, July 14, 2017, 11:48

Investigated the bad water flow situation.  It was due to a faulty water flow sensor.  The paddle wheel stopped turning until I gave it a tab.  We had a similar problem before with the water sensor, see elog ID 109.  It is probably the time to replace all the water sensors. 

 Tuesday, July 18, 2017, 15:26

Problems occured with TGHT water supply paddle wheel stopped and therefore tripped off evap2 last week.

All paddle wheels were replaced today for evap2 [other than the chiller].

A build up of dirt was found on all wheels replaced.

Evap2 good to go.

Will test flow meters before heating up to higher setpoints to confirm everything is working.

Monday, July 31, 2017, 15:24

Turned on BV and TP this afternoon.

Started ramping down, ~1min after turned on both tripped off.

Vacuum box turned red.

IGP1 appears yellow but still registering a vacuum.

TP interlocks: requires IEVAP2:IGP1 < 500mTorr but IGP1 = 6mTorr when tripped off.

Should have been satisfied and therefore not tripped but IGP1 not communicating?

Nothing wrong with ion gauge in person, vacuum good on direct read out.

When attempting 'Global Reset', nothing would reset - vacuum box remained red etc.

See screenshot attached of errors.

 Tuesday, August 01, 2017, 15:31

Had kept BP, PV and RV overnight.

This morning vacuum fine, everything had reset except "IEVAP2:TP on" under device notes for IEVAP2:TP remained red.

Turned on BV and TP, once turbo pump registered on, red wording went away.

Currently pumping down - everything looks fine now.

Still unsure of reason for these errors...

 Friday, August 04, 2017, 10:55

Happened again last night at ~5:45 while evaps at ~420A - see elog i.d. 383 for photos and details.

 Tuesday, August 08, 2017, 14:57

See elog i.d's #384 and #381

Investigated wiring in PLC.

Some wires in PLC were not creating a good contact - could be problem re: IGP1 tripping off.

Wires replaced by Gelo.

Pumped down and turned on power supplies over weekend.

Everything remained on - IGP1 did not trip system off.

May proceed with regular use.