Tuesday, April 26, 2016, 13:32

Container coated with TaC using 'flushing technique'.

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

Currently pumping down in evap2

 Wednesday, April 27, 2016, 10:25

IGP1 = 2.6e-7 Torr.

HS water valves opened, no leaks detected.

Tapped up manually to 35A.

Waited ~35min

Vacuum stable, IGP1 = 6.7e-7 Torr

Initiated auto-ramp at 0.2A/min for the TGHT with a final setpoint of 400A

Final desired temperature = 1900C

 Thursday, April 28, 2016, 14:41

Previously TBHT not on when sintering IGLIS container [since no ionizer tube] - John decided will turn on for this round

Tapped up TBHT manually to 140A, 1.69V

IGP1 = 4.5e-7 Torr

OMEGA = 1635C

TGHT = 382A, 5.8V

Initiating auto-ramp of TBHT at 0.1A/min with a final setpoint of 230A.

Friday, April 29, 2016, 08:40

IGP1 = 2.22-7 Torr

TGHT = 400A, 6.1V

TBHT = 233A, 2.9V

OMEGA = 1719C

Tapping up manually to OMEGA = 1900C

Friday, April 29, 2016, 15:22

IGP1 = 3.0e-7 Torr

TGHT = 460A, 7.52V

TBHT =230A, 2.93V

OMEGA = 1904C

Target container has remained at max temperature setpoint of 1900C for 4.5hrs.

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

 Monday, May 02, 2016, 08:35

Vented in air and opened up this morning.

Container looks good.

See attached photos.

John Wong wrote:

Laura Lambert wrote:  Wednesday, May 04, 2016, 13:28 Target boat has a layer of niobium foil on the bottom of the boat. A niobium foil has been made with slots to hold samples [similar to when sintering endcaps] *See attached photos Larger niobium samples are placed in the slots, holding in place, to avoid warping; smaller niobium sample sitting inside the boat by itself. Smaller sample closest to OMEGA IR reading [right side] Boat is wrapped with 1 large layer of Ta foil, wrapped around the boat 3x, careful to avoid touching samples. Loaded into evap2 yesterday. Vacuum pump bearings gone - pump replaced this morning by vacuum group. Pumping down now...  Friday, May 06, 2016, 13:36 HS water valves opened, no leaks detected. Tapped up manually to 35A. IGP1 = 2.4e-7 Torr Setting auto-ramp rate at 0.2A/min to 250A over the weekend. Will tap up manually monday to final desired temperature of 1400C.  Monday, May 09, 2016, 09:38 OMEGA = 1128C IGP1 = 1.3e-7 Torr TGHT = 250A, 3.7V Tapping up manually to 1400C...  Monday, May 09, 2016, 14:05 Evap2 has reached ~1405C TGHT = 341A, 5.34V IGP1 = 1.9e-7 Torr Will remain at max setpoints for min 4hrs then initiate cool down.    Monday, May 09, 2016, 18:18 TGHT at 341A/5.34V for over 4 hours.  Vac stables at 1.78e-7 Torr. Cooling down at 2A/min

 Tuesday, May 10, 2016, 08:45

Vented in air and opened up this morning.

Samples look good!

Wednesday, May 11, 2016, 17:15

Nanofiber SiC (~50nm grain size)/PAN was prepared at UBC. 

SiC 0.50g, DMF 9.0g, PAN 1.0g, tiny bit of SDS.

The fiber mat was stabilized in air at 250C and then cut into discs, initial mass = 0.1072g

Discs were then bounded with PVA on 9 pieces of rounded graphite foil  (green mass gained to 0.6031g)

The stack of naofiber SiC/PAN was loaded on to Ta boated (coated) and wrapped with Ta heat shield. 

Chamber is currently being pumped down.

 Friday, May 13, 2016, 15:00

TGHT at 390A/6.966V.  Temp measured at 1615C. 

Will keep at that temperature for a few days.

 Monday, May 16, 2016, 15:44

Sample has been heated at ~1600C for 4 days.  TGHT at 400A/7.02V. 

Cooling down at 2A/min

 Tuesday, May 17, 2016, 11:18

Chamber vented.  Inspecting samples.

Laura Lambert wrote:

Wednesday, May 25, 2016, 11:37 Container coated with TaC using 'flushing technique' [cleaned ionizer tube with acetone, so no coating inside ionizer tube] Wrapped with 2 x Ta heat shields - one full height of Ta foil wrapped around cooling fins twice Currently pumping down in evap2  Thursday, May 26, 2016, 09:28 Tapped up manually to 40A IGP1 = 6.6e-7 Torr Initiating auto-ramp at 0.2A/min and 0.1A/min for the TGHT and TBHT respectively. Final setpoints for TGHT = 650A and TBHT = 230A Once max setpoints reached will continue to tap up manually while monitoring temperature to 1900C

 Tuesday, May 31, 2016, 11:09

TGHT at 615A/9.08V, temp = 1610C.  Vacuum at 1.8e-7 Torr. 

Tapping up TGHT to reach 1900C

 Tuesday, May 31, 2016, 12:04

TGHT at 765A/11.90V.  Temp at 1900C.  Pressure is coming down from 8.7e-7Torr. 

Will keep at this temperature for a day.

 Wednesday, June 01, 2016, 15:22

Temperature has been stable at 1900C.  Pressure is coming down from 3.4e-7 Torr. 

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

 Friday, June 03, 2016, 12:10

TGHT/TBHT at 0A.  Target can be remained under vacuum until Monday.

 Monday, June 06, 2016, 16:54

Target container was inspected; it looks good

John Wong wrote:

Laura Lambert wrote: John Wong wrote:   Laura Lambert wrote:  Thursday, June 09, 2016, 15:39 First target using beta-SiC material! Target container contains 450 discs of SiC [4 x 5 packs + 430 single discs] Target packed length = 16cm.  Mass of 533 discs SiC(green)  = 53.8758g Container is wrapped with 3 heatshields; no end caps are inserted yet - coated spring inserted both sides to hold discs in place. Sintering temp = 1800C, TGHT will be set accordingly.  TBHT max at 230A.  Chamber is currently being pumped down.  Friday, June 10, 2016, 13:24 HS water valves opened, no leaks detected. Tapping up manually to 70A... Auto ramp will be set for TGHT = 0.2A/min to a final setpoint of 520A Auto-ramp for TBHT = 0.1A/min to a final setpoint of 230A.      Friday, June 10, 2016, 16:27 TGHT stepped up to 70A/0.55V.  TGHT at 50A/0.62V.  Pressure stabilized at 5.5e-5 Torr. Initiated auto ramping.  TGHT at 0.2A/min --> 520A.  TBHT at 0.1A/min --> 230A.    Monday, June 13, 2016, 09:51 TGHT = 425A, 5.65V TBHT = 225A, 3.7V IGP1 = 8.7e-6 Torr. Increasing ramping rate to 1.0A/min...  Monday, June 13, 2016, 15:56 Tapped up manually from 520A to 1800C Extrapolated data on graph to determine correct current required to reach desired max temperature. Will remain at 1800C for ~48hrs See attachements for excel sheet and screenshot of striptool.    Wednesday, June 15, 2016, 17:54 TGHT at 710A, 11.35V.  TBHT at 230A/3.86V.  Omega reading droppd to 1130C due to coating on windows.  Ionizer tube was measured (center) at around 1900C Cooling down at 2A/min for TGHT, 1A/min for TBHT.  Samples will be collected prior to cleaning the windows. NEXT:  Conditioning.

Thursday, June 16, 2016, 09:29

vented in air and opened up this morning.

took some samples to be tested.

 Thursday, June 16, 2016, 10:59

Previously sintered over weekend [see elog i.d 306]

Target container contains 450 discs of SiC [4 x 5 packs + 430 single discs]

Target packed length = 16cm. 

Mass of 533 discs SiC(green)  = 53.8758g

Container is wrapped with 3 heatshields; no end caps are inserted yet - coated spring inserted both sides to hold discs in place.

Conditioning temp = 1800C.

TGHT max = 710A according to sintering data.  TBHT max = 230A. 

Chamber is currently being pumped down. 

 Thursday, June 16, 2016, 15:43

Target was not removed from evap2 after sintering, vented and cleaned windows only.

HS water valves already open.

Stepped up manually to 70A, vacuum stable.

Initiated auto-ramp at 1.0A/min for the TGHT and 0.5A/min for the TBHT with max setpoints of 600A and 230A respectively.

TGHT = 118A, 0.9V

TBHT = 90A, 1.1V

IGP1 = 7.3e-7 Torr

 Friday, June 17, 2016, 12:14

TGHT has been tapped up manually to reach max desired temperature of 1800C

TGHT = 690A, 10.85V

TBHT = 230A, 3.88V

IGP1 = 4.9e-7 Torr

This is a lower current than the current required to reach 1800C during the sintering process.

For sintering, the max current was determined via extrapolation of trendline from raw data due to interference of coating on window and unable to take reliable readings from OMEGA.

For this conditioning process ~1800C is reached on the OMEGA since the window is still ~un-coated.

Will remain at 690A, ~1800C for several days to maximize conditioning process.

See attachment for raw data.

 Monday, June 20, 2016, 09:01

At the end of the day on friday 17th, OMEGA read ~1750C - no change in the current or voltage, vacuum was stable, this was the max setpoints used to reach 1800C.

This morning OMEGA = 2040C

TGHT = 690A, 10.95V

vacuum stable at IGP1 = 1.8e-7 Torr.

Slightly more noticeable coating on window port, looks like a thin ink layer, still relatively thin coating [ see attached image]

Also attached is archive from over wknd to show vacuum stable, current unchanged and voltage negligibly changed [only gone up by ~0.1V]

 Friday, June 24, 2016, 13:52

Container has remained at max setpoints for 7 days.

Initiating auto-cool for TGHT @ 2.0A/min and for TBHT @ 1.0A/min.

Will vent chamber and remove from evap2 to pass off for assembly monday morning.

See attachment for updated excel on temperature readings for the conditioning process.

 Monday, June 27, 2016, 08:28

vented in air and removed this morning.

target looks good!

all discs remained nicely alligned.

discs expanded outwards ~1cm, pushed back in to keep target length at 16cm

no visible yellow crystals like previous SiC targets 

endcaps inserted and expanded.

Rh foil inserted.

Ta heat shield foils removed, fins look good.

see photos attached for pictures of target - post conditioning.

coating on window very hard to remove. looked like a light sharpy pen coating on window. ended up scratching off with acetone and screw driver. couldn't remove all of it...

 Monday, June 27, 2016, 11:07

Container coated with TaC using 'flushing technique'.

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

Currently pumping down in evap2

 Monday, June 27, 2016, 13:23

HS water valves opened

Tapped up manually to 35A

Waited ~1hr, vacuum stable

IGP1 = 1.8e-6 Torr

Initiating auto ramp for TGHT @ 0.2A/min to a max setpoint of 400A

Initiating auto ramp for TBHT @ 0.1A/min to a max setpoint of 230A

Once max setpoints achieved, will tap up manually to final desired temperature of 1900C

 Wednesday, June 29, 2016, 11:33

IGP1 = 1.9e-7

TGHT = 400A, 6.0V

TBHT = 223A, 3.9V

OMEGA = 1885C

Remained at these settings for ~13hrs

Increased TBHT max voltage to 4.3V to achieve 230A

TBHT = 230A, 4.1V

OMEGA = 1890C

Tapped up to TGHT = 405A, 6.17V to achieve 1900C...OMEGA reached 1915C

Lowered TGHT to = 403A, 6.12V

OMEGA = 1905C

Measured ~1870C with the mikron, same window the OMEGA measurements are taken out of.

IGP1 = 2.1e-7

 Thursday, June 30, 2016, 08:44

TGHT = 403A, 6.07V

OMEGA = 1886C

Tapped back up to 1900C

TGHT = 410A, 6.22V

OMEGA = 1911C

Thursday, June 30, 2016, 16:01

OMEGA = 1911C

Container has remained at ~1900C for ~1.5 days

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

 Monday, July 04, 2016, 09:59

Vented in air and opened up this morning.

Container looks good.

Confirmed coating fully sintered with J.Wong.

Photos attached.

 Friday, July 15, 2016, 11:49

Container previously coated with TaC using 'flushing technique', cleaned ionizer tube with acetone, so no coating inside ionizer tube

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

Currently pumping down in evap2

 Friday, July 15, 2016, 14:35

Turbo pump broken 

Currently being replaced...

 Friday, July 15, 2016, 17:04

Turns out its not the turbo pump...TP controls and pump replaced, problem still happening.

Took out heat shield and used a closed loop to rule out leak in chamber, emptied all water lines - turbo pump now on.

Took v.long time to pump down. TP will remain on over wknd.

BP turns on, PV1 turns on, RV turns on - then takes very long time for vacuum to drop ~45min? before BV and TP can be turned on.

Possibly problem with threads on heat shield and not creating proper seal?

Will continue monday with evap2 mystery problem solving...

Monday, July 18, 2016, 16:14

Replaced heat shield and copper seals.

Container re-loaded.

Turbo pump on and good vacuum achieved! YAY!

Finished pumping down, opened HS water valves - no leaks detected.

Tapped up manually to 35A

Vacuum stable, IGP1 = 3e-6 Torr

Initiating auto ramp for TGHT @ 0.2A/min to a max setpoint of 400A

Initiating auto ramp for TBHT @ 0.1A/min to a max setpoint of 230A

Once max setpoints achieved, will tap up manually to final desired temperature of 1900C

 Tuesday, July 19, 2016, 09:21

TGHT = 242A, 2.76V

TBHT = 162A

IGP1 = 5.05e-6 Torr

Increasing ramping rate to 1.0A/min and 0.5A/min for the TGHT and TBHT respectively.

 Tuesday, July 19, 2016, 13:04

TGHT = 400A, 4.4V

TBHT = 230A, 2.6V

OMEGA = 1120C

Reached max setpoints ~1hr ago.

Tapping up manually to 1900C...

Tuesday, July 19, 2016, 16:32

MORE problems with evap2 

TGHT reads 460A, 5.1V, 1170C - a lot of power is being lost somewhere...

Comparison from elog i.d. 291 [the last IGLIS container sintering of TaC coating] the TGHT read 460A, 7.5V, 1900C

Another problem: the read out on the power supply and read out on epics of the TBHT reads 215A; however, the 'current set' says 177A - two very different numbers?!

Ramping down evap2 at 2.0A/min and 1.0A/min for the TGHT and TBHT respectively to further inspect chamber and hopefully solve this...

 Wednesday, July 20, 2016, 13:34

Chamber was vented in air and opened up for inspecting.

Fixed!

One of the steel plates used to stop reflection onto the door of the chamber was inserted improperly, resting on top of the 2 negative copper lines to the target leg, this was causing a short.

There was also a short from the right target leg touching the copper heat shield, the heat shield has been shaved down and corrected. It is no longer touching.

There were also 2 brackets that had fallen behind evap2 inside the cage, one was touching the positive lines - it wasn't quite touching the ground, but may have grounded it, causing another possible short.

The chamber was pumped back down and the HS water valves re-opened. No leaks detected.

Evap2 was tapped up manually to 35A.

Vacuum stable = 1.0e-6 Torr.

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

Final setpoints are TGHT = 400A and TBHT = 230A

 Wednesday, July 20, 2016, 16:25

TGHT = 315A, 4.5V

TBHT = 174A, 2.1V

IGP1 = 2e-6 Torr

OMEGA = 1518C

Lowering auto-ramp to 0.2A/min and 0.1A/min for the TGHT and TBHT overnight while unable to keep watch on the vacuum.

 Thursday, July 21, 2016, 09:09

Evap 2 reached max setpoints ~7.5hrs ago.

TGHT = 400A, 6.3V

TBHT = 230A, 2.9V

IGP1 = 5.1e-7 Torr.

OMEGA = 1882C

Tapping up manually to 1900C...

 Friday, July 22, 2016, 16:18

Container has remained at ~1900C for ~31hrs

TGHT reached 405A/1900C - then after ~23hrs dropped in temperature down to 1895C so was tapped up further to 410A/1910C for another ~8hrs.

TGHT = 410A, 6.57V

IGP1 = 3.1e-7 Torr

TBHT = 230A, 2.9V

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

Will remove from evap2 after the weekend.

 Tuesday, July 26, 2016, 16:49

vented in air.

container looks good, fully sintered.

will update with photos tomorrow...

 Tuesday, July 26, 2016, 16:50

loaded into evap2

pumped down, HS water valves opened, no leaks detected.

tapped up manually to 35A

vacuum stable = 3.8e-6 Torr

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

Final setpoints at 230A for the TBHT and 600A for the TGHT.

Final desired temperature = 1800C

 Wednesday, July 27, 2016, 09:20

IGP1 = 6.3e-7 Torr, vacuum stable.

TGHT = 232A, 2.7V

TBHT = 131A, 1.76V

Increasing ramping rate to 1.0A/min and 0.5A/min for the TGHT and TBHT respectively.

 Wednesday, July 27, 2016, 15:46

TGHT = 600A, 8.87V

TBHT = 230A, 3.7V

IGP1 = 1.37e-6 Torr

OMEGA = 1640C

Increased max TGHT voltage to 12V

Tapped up manually to OMEGA = 1810C

TGHT = 675A, 10.21V

IGP1 = 2.2e-6 Torr

Will remain at max setpoints for the rest of the week and cool down over weekend.

 Thursday, July 28, 2016, 08:34

TGHT = 675A, 10.41V

OMEGA = 1833C

Tapped down to 660A, 10.09V

OMEGA = 1805C

 Friday, July 29, 2016, 13:57

OMEGA = 1814C

TGHT = 660A, 10.16V

TBHT = 230A, 3.72V

IGP1 = 3.43e-7 Torr

evap2 has remained at max setpoints for ~42hrs

conditioning complete.

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

 Tuesday, August 02, 2016, 13:39

vented in air and removed from evap2 this morning.

target looks good!

 Tuesday, August 02, 2016, 13:41

Target container contains 471 discs of SiC [6 x 5 packs + 441 single discs]

Target packed length = 16cm. 

Mass of SiC(green)  = 52.7172g

Container is wrapped with 3 heatshields; no end caps are inserted yet - coated spring inserted both sides to hold discs in place.

Sintering temp = 1800C

TGHT max = 350A.  TBHT max at 230A. 

Chamber is currently being pumped down. 

Slope on OMEGA = 1.04

Tuesday, August 02, 2016, 16:00

Tapped up manually to 30A - vacuum to high, lowered down to 20A to be able to initiate auto-ramp.

IGP1 = 2.3e-5 Torr

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

 Friday, August 05, 2016, 11:57

Evap2 has reached TGHT = 350A, 5.33V

TBHT = 187A, 2.31V and still climbing...

OMEGA = 1365C

IGP1 = 7.88e-7 Torr

Increased max setpoint for TGHT to 400A.

 Friday, August 05, 2016, 13:33

TGHT = 380A, 5.97V

TBHT = 197A, 2.45V

OMEGA = 1396C

IGP1 = 8.75e-7 Torr

Increasing ramping rate to 2.0A/min and 1.0A/min for the TGHT and TBHT respectively.

New final setpoint for the TGHT = 450A

 Friday, August 05, 2016, 14:17

TBHT = 230A, 2.97V

TGHT = 450A, 7.4V

OMEGA = 1572C

IGP1 = 3.2e-6 Torr

Increasing max setpoint for TGHT to 500A and re-initiating auto-ramp.

 Friday, August 05, 2016, 15:18

At TGHT = 480A, OMEGA temperature dropped to 1400C due to coating on window.

Last reading was ~1600C

Tapped up manually to TGHT = 500A, 8.61V

Window fully coated therefore OMEGA reading is negligible at this point

Attempted to take temperature reading with other OMEGA from behind evaporator or using handheld manual temperature reader - all windows have a coating, therefore unsuccessful.

IGP1 = 1.75e-6 Torr

Reduced max voltage set for TGHT to 9.0V to minimize possibly voltage 'creep'

Will remain at these setpoints over wknd and ramp down monday morning.

 Monday, August 08, 2016, 08:45

TGHT = 500A on the 'current set' and 466A on the readout, 8.74V

TBHT = 230A, 2.99V

IGP1 = 6.6e-8 Torr

OMEGA = 1460C [reading through coating on window port]

Evap2 has been at these setpoints for the wknd.

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

 Monday, August 08, 2016, 10:38

Quick observational note:

while ramping down OMEGA readings have slowly increased.

At ~350A OMEGA = ~1500C

At ~300A, OMEGA = ~1750C

Currently at 280A, OMEGA = ~2800C

Coating on window has affected the OMEGA readings in a weird way...

 Monday, August 08, 2016, 15:17

Vented in air and opened up this afternoon.

Cleaned windows but left target loaded in evap2 for conditioning process.

Laura Lambert wrote:

Wednesday, August 17, 2016, 17:30 Container coated with TaC using 'flushing technique', cleaned ionizer tube with acetone, so no coating inside ionizer tube Wrapped with 3 x Ta heat shields, incl center block Currently pumping down in evap2 Thursday, August 18, 2016, 10:14  HS water valves opened...leak detected  see attachment for photo from archives Vented and opened up. Anders performed leak check, nothing found. Replaced all seals with blue seals. Pumping down now  Thursday, August 18, 2016, 16:12 HS water valves opened...leak detected again  see attachment for photo of striptool Vented and opened up. working with Anders on finding leak...  Monday, August 22, 2016, 10:38 leaks FIXED! HS water valves opened, NO leaks detected! Tapped up manually to 70A Vacuum stable, IGP1 = 2.5e-6 Torr Initiating auto ramp for TGHT @ 0.2A/min to a max setpoint of 350A Initiating auto ramp for TBHT @ 0.1A/min to a max setpoint of 230A Once max setpoints achieved, will tap up manually to final desired temperature of 1900C  Monday, August 22, 2016, 14:58 TGHT = 115A, 1.3V TBHT = 89A, 0.97V IGP1 = 4.1e-7 Torr. Increasing ramping rate to 1.0A/min and 0.5A/min for the TGHT and TBHT respectively.  Monday, August 22, 2016, 16:01 IGP1 = 1.25e-6 torr TGHT = 174A, 2.2V TBHT = 118A, 1.4V Lowering ramping rate to 0.2A/min and 0.1A/min for the TGHT and TBHT respectively for overnight ramping.

 Tuesday, August 23, 2016, 12:14

Initiate TGHT autoramping to 400A at 2A/min.  Vac 3.5e-7 Torr. 

 Tuesday, August 23, 2016, 14:48

TGHt tapped up to 420A/7.01V.  Local temp read at ~1900C.  Will sinter at this temp for a few hours before cooling down.

 Tuesday, August 23, 2016, 17:20

TGHT at been at 420A/7.01V for over 4 hours.  Vac at 4.8e-7 Torr.

Cooling TGHT and TBHT at 1A/min.

 Wednesday, August 24, 2016, 10:35

TGHT/TBHT at 0A.

Venting chamber.

Container looks good.

Wednesday, August 24, 2016, 17:05

Target container was previously coated with TaC and sintered up to 1900C at 420A/7.01V

Container is loaded with beta-SiC 432 discs at 16cm in length. 

Container is wrapped with Ta-heat shield; no end-caps are used at this time.

Chamber is being pumped down.

 Thursday, August 25, 2016, 12:04

Chamber has been pumped down overnight.  Pressure at 5.9e-7 Torr.

HS water valve opened; no leaks were detected.

Sintering temperature 1800C. TGHT will be set accordingly to get the desired temperature.  TBHT max at 230A.

Thursday, August 25, 2016, 12:12

Tapped up TGHT/TBHT to 40A.  Vac at 7e-6 and slowly going up  but still below limit.

 Monday, August 29, 2016, 11:04

TGHT and TBHT reached to 250A (3.65V)//230A(3.02V), respectively, and kept stable over the weekend. 

Temp measured at 1372C with slope set at 1.04 (1230C at slope 0.98). 

No visible coating on windows. 

Setting up TGHT to reach 1800C; monitoring locally

 Monday, August 29, 2016, 14:35

Stepped up TGHT to 390A/6.54V; light coating was observed on the windows.  The temperature should be around 1800C which should be in line with the power (current) deposited in the container during the TaC coat sintering process (1900A at 420A); however, with the light coating the reading may be off.  

Mikron was used to measured inside of the tube (away from the discs); temperature was measured at ~1800C, (see attachment)  [adjusted slope at 1.00 to compensate the SiC disc and Ta]  

Omega was used to measured the temperature of the discs.  It is difficult to know what's the temperature inside the tube, so this measurement  is only taken as a guideline.  Slope changed from 1.04 to 1.15 to match Mikron's reading.  

After heated at  390A for 30 mins, the windows are now coated.  Temp reading is no longer reliable.  The temperature could be above 1800C.  Keeping a close monitor!!!

No blockage inside the tube was observed.  

Will remain heating at 390A/6.44V for overnight before proceeding with the re-conditioning. 

 Tuesday, August 30, 2016, 10:41

Target was heated at 390A  for over 10 hours and then cool down at 1A/min (see attachment#2).  Windows were fully coated and Omega couldn't register any reading. 

Chamber will be vented and target will be inspected before proceeding with the re-conditioning step.

Tuesday, August 30, 2016, 12:13  

Target was inspected; no visible damage was observed (see attachment)

Material coated on the windows and the cu heat shields;  all parts were wiped off with acetone. 

No visible material build up inside the container. 

Chamber is now being pumped down for re-conditiing.  

 Tuesday, August 30, 2016, 13:05

HS water valves open; no leaks detected.  

Vac at 3.6 e-6 Torr.  

Ready to set up TGHT/TBHT

 Tuesday, August 30, 2016, 16:41

TGHT/TBHT stepped up to 340A (5.40V) /230A (3.1V), respectively. 

Temperature was measured at 1835C at TGHT of 340A.  Omega, Mikron and analogue pyrometer were all reading ~1800C inside the tube (not on the SiC surface).  For that reason, I decided to stop the current at 340A, instead of 390A.  

TGHT voltage is running stable.  

No visible coating or blockage inside the tube was observed.  

Wednesday, August 31, 2016, 11:53

A thin layer of coating is observed on both the side windows (see attachment 5).  The temp reading is no longer reliable.

TGHT remains at 340A/5.45V.  P/S voltage is performing steadily.  

No clogging inside the tube is observed. 

Setting up another Omega reader to measure temperature from the front window since this window is clear and won't get coated (see attachment #6).

Temperature measurement from the front window is ~1140C; this corresponds to the measurement from the analogue pyrometer with the correction of e=~0.2 for tantalum at 1100C.

Note:  The temperature measurements should be taken as relative.  Since the reading from the side windows isn't reliable any longer, the centre window will give some information how stable the temperature is holding during the reconditioning process.  Continue to monitor.

 Wednesday, August 31, 2016, 16:24

About two hours ago, I increased TGHT to 350A and stayed there for a few mins (see attachment 7).  No change in temp was observed - that's mainly due to the coating on the windows.  As for the temp measurement from the center window, a more power current input would require to see the change as heat is slowly propagating through the layers of Ta heatshields.

Local inspection on the target: no clogging inside the tube. Voltage/Current is stable at 340A/5.45V.  Vac at 1.43e-7 Torr.

 Wednesday, August 31, 2016, 23:00

Strange observation:  Temperature readers on both omega have gone up. (see attachment 8).

I'm not sure if the temperature is reiiable.  I actually saw the increase in temperature ~1850C  last night around the same time; no change in TGHT current/voltage.  By the next morning, it went back down to 1400C with significant coating on the windows.

 Wednesday, August 31, 2016, 23:28

I had ISAC Op (Justin) to help me go into the Hotlab and take a look at the reading on Mikron.  Indeed, it is reading about 2000C which is close to the Omega reading.  He also looked into the tube through Mikron scope and found no clogging inside the tube.

To be safe, I am going to lower the TGHT heater down to reach ~1800C.

Wednesday, August 31, 2016, 23:41

Lower TGHT to 305A/4.81V; OMEGA reading at 1830C.  Vac at 1.27e-7 Torr.  Will remain at this current over night. 

 Thursday, September 01, 2016, 12:16

Checked on the target.  

Temperature readings, right windows (omega)= 1726C, centre = 1100C (omega), left (Mikron) = 1720C.  

No blockage inside the tube.  

TGHT stabilizes at 305A/4.79V.  Vac at 1.09e-7 Torr.  

 Thursday, September 01, 2016, 16:32

 About an hour ago, the temp dropped to 1660C with no change in TGHT current/voltage (see attachment 9).

Vac is a 1.06e-7 Torr. 

After consulting with Friedhelm, we decided to cool the target down and inspect it tomorrow.

Ramping TGHT/TBHT at 2A/min.

 Wednesday, September 07, 2016, 15:13

The target was removed from the Evap and inspected. 

Some spots on both ends and ionizer tube were crystalized.  (see attachment 10). 

No blockage inside the tube was observed. 

End caps were inserted.

The target was assembled and tested - All seems fine. 

John Wong wrote:

John Wong wrote:  Wednesday, September 07, 2016, 14:45 Container was previously coated with TaC solution and wrapped with 1-full length layer of Ta- heat shield around the fins.   Chamber is being pumped down.  Vac at 5.6e-7 Torr before HS water valves were open; no leaks were detected.  Sintering Temperature 1900C (Omega slope @ 0.98); expected TGHT ~765A/11.90V, TGHT max at 230A.  Thursday, September 08, 2016, 18:14 At about 1600C, it was observed that the coating inside the tube seems to chip off (see attachment 1). TGHT was ramped up to 745A/11.85V and TBHT to 230A/3.25V.  Temperature measured on OMEGA/Mikron = 1914C/1881C; both instruments slopes set at 0.98. Will remain at this TGHT current over night Vac at 3.0e-6 Torr and coming down. Friday, September 09, 2016, 11:01  Target has been heated at the stable temperature at 1914C (for OMEGA) and 1881C (for Mikron) with current at 745A/11.94V (see attachment 2) for almost 19 hours.  No fluctuation in p/s current or temperature was observed.  The ramping up process is captured and can be view from the link below: https://www.dropbox.com/sh/9lgtin54o17ds6j/AABn1-XjvK44mm74TjqTAmvta?dl=0 Pressure at 1.07e-6 Torr.  Cooling down TGHT at 2A/min and TBHT at 1A/min.  Continue to capture the cooling down process.   Friday, September 09, 2016, 15:17  While the target container was cooling down, the chip-like particle began obvious (see attachment 3).   Will inspect the container.. TGHT currently at 260A.    Monday, September 12, 2016, 16:54 The TaC coating chipped off from the surface and didn't get sintered with the container.  (See attachment1).  There are a few possible reasons why this happened: 1.  The coating was too think.  This may cause the TaC  layer to curl up while the heater was ramped up.  2.  The coated material got brittle.  The container was flushed with TaC (probably a few weeks ago?) before it went through the sintering process.  Prolong exposure to air/light usually degrade the polymers viscoelasticity. 3.  TaC solution has got bad.  The particles can agglomerate over time and this can cause uneven surface. 4.  Combination of all... ??? Anyway, the chipped off TaC layer was gently scraped off with a stainless steel rod.  Then using kimwipes, i was able to remove most of the chipped off coating; it was not easy - especially trying to remove it from the inner tube. Instead of "flushing" the tube with TaC, I decided to spray it with thin layer.  And using the air supply, I could quickly dry the coating and installed it back to the evaporator for 2nd Round sintering as we are approaching the deadline! .

 Monday, September 12, 2016, 17:24

Chamber was pumped down to low 10e-6 Torr before HS water valves were open - no leaks detected.

TGHT/TBHT auto ramped at 2A/min to 600A/230A.

Will continue to monitor..

 Wednesday, September 14, 2016, 17:04

TGHT was stepped up to 700A and temp 1851C (OMEGA), 1930C(Mikron).  (see attachment 1).  The container was heated over night before it was cool down at 2A/min. 

Target container seems to properly sintered with TaC (see attachment 2); it will be used for SiC#35. 

John Wong wrote:

Laura Lambert wrote: John Wong wrote: Laura Lambert wrote:  Thursday, September 15, 2016, 16:23 Target container contains 487 discs of SiC  Target packed length = 16cm.  Mass of SiC(green)  = 58.8795g Container is wrapped with 1x heatshield around each side of cooling fins; no end caps are inserted yet - coated spring inserted both sides to hold discs in place. Sintering temp = 1800C Chamber is currently being pumped down.   Friday, September 16, 2016, 10:50 Tapped up manually to 50A Waited ~1hr , vacuum stable. IGP1 = 1.24e-5 Torr Initiating auto-ramp at 0.2A/min and 0.1A/min for the TGHT and TBHT respectively. TGHT max = 500A.  TBHT max at 230A.  Slope on OMEGA = 1.15  Monday, September 19, 2016, 10:53 OMEGA = 1230C TGHT = 360A, 4.75V TBHT = 204A, 2.68V IGP1 = 5.3e-6 Torr Increasing ramping rate to 1.0A/min and 0.5A/min for the TGHT and TBHT respectively.  Monday, September 19, 2016, 11:57 OMEGA = ~1300C TBHT = 230A, 3.16V TGHT = 409A, 5.55V Lowering ramping rate to 0.2A/min while vaccum high IGP1 = 3.05e-5 Torr  Monday, September 19, 2016, 13:22 OMEGA = 1350C TGHT = 425A, 5.82V IGP1 = 1.97e-5 Torr Stepping ramping rate back up to 1.0A/min    Monday, September 19, 2016, 18:24 Measuring the temperature on the SiC is difficult due to the changing in emissivity as the temperature goes up.  So, I will use the MIKRON to measure the temperature on the Ta surface near the end of the tube and OMEGA for measuring the inside.   Using the analogue pyrometer, the temperature on the Ta surface at the end of the tube was measured at around ~1450C; this temperature match the temperature on the Mikron at slope 0.98 (as usual).  To match it with OMEGA, I changed the slope to 1.04 since this measurement is taking readings on the  inside of the tube and on the SiC material.    Note:  The measurements are NOT the absolute temperature.  These are relative temperature measurements  which give some guideline where the target current should be at for the sintering process.  Please plot the temp vs current as the TGHT is being ramped up.  At some point, the windows will get coated and the measurement is no longer reliable.   The plot will be used to give an estimation of the current for 1800C.        Tuesday, September 20, 2016, 15:18 there was a temperature fluctuation resulting in the MIKRON no longer matching the readout on the OMEGA this prompted another change in the slope on the OMEGA to 1.08 TGHT was then tapped up manually to 600A/ 1800C will remain at this max setpoint for a few days before ramping down see attachment for raw data  Wednesday, September 21, 2016, 11:34 temperatures dropped a small amount overnight. tapped up manually to 625A/ 1810C still no coating on window. see attachment for updated raw data    Thursday, September 22, 2016, 12:07 Temperature reader on OMEGA dropped slightly to 1785C overnight.  The temperature on the leg remained at 1800C (MIKRON).  No coating on windows.   Increased TGHT to 635A/10.12V (local 10.40V).  OMEGA reads 1800C, MIKRON ~1817C.   Continue to monitor… (see dropbox for captured photos)

 Monday, September 26, 2016, 13:24

Temperature decreased over weekend.

MIKRON dropped from ~1800C to ~1670C, OMEGA on right side remained ~1800C

Comparing screen shots of temperature readings and camera looking at target from left side, changes can be seen:

-darker area on top edge of target tube, above inside tube, grows larger when temperature drops - indicating 'cooler area' has grown

-initially darker area covers top above target materials on tube, when drops to ~1670C darker area extends down sides of target tube and reaches past target material area

See attached picture showing these details

Target has remained at this max setpoint for ~4-5 days

Windows remain un-coated.

Current and voltage readings remain un-changed.

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

 Wednesday, September 28, 2016, 17:05

Vented in air, target taken out today.

Target looks good!

A small amount of material was removed from the windows in evap2, very thin layer of coating.

Will update tomorrow with photos

Endcaps inserted.

 Wednesday, September 28, 2016, 17:08

Container coated with TaC using 'flushing technique' today, cleaned ionizer tube with acetone, no coating inside ionizer tube

Dried by blowing air into tube

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

Currently pumping down in evap2

 Thursday, September 29, 2016, 11:11

HS water valves opened

Tapped up to 35A

Waited ~45min, vacuum stable

IGP1 = 1.4e-6 Torr

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

Max setpoints for TGHT = 350A and TBHT  = 230A

Once max setpoints achieved, will tap up manually to final desired temperature of 1900C

 Friday, September 30, 2016, 10:51

IGP1 = 7.8e-7 Torr

TGHT = 315A, 4.57V

TBHT = 174A, 2.8V

Increasing ramping rate to 1.0A/min and 0.5A/min for the TGHT and TBHT respectively.

 Friday, September 30, 2016, 11:44

Changed OMEGA slope to 0.98

IGP1 = 1e-6 Torr

TGHT = 350A, 5.2V

TBHT = 201A, 3.4V

Increasing ramping rate of TBHT to 1.0A/min

OMEGA = 1625C / MIKRON = 1625C

 Friday, September 30, 2016, 15:45

IGP1 = 1.1e-6 Torr

TGHT = 430A, 6.79V

TBHT = 230A, 4.07V

OMEGA = 1903C

Will remain at max setpoints over weekend.

See attached link for raw data of manual tap up.

Also see attached photos of screenshots showing oval - not circular - tube of target container at two different temperatures...

 Monday, October 03, 2016, 13:28

IGP1 = 1.79e-7 Torr

TGHT = 430A, 6.87V

TBHT = 230A, 4.06V

OMEGA = 1892C

MIKRON = 1847C

Attached is a picture taken through the MIKRON, the slight oval shape appears to be a minor bend in the target container:

With the ionizer tube facing into the page, the bend appears to be in the center with both ends of the container bent slightly towards the page

This possible bend in the container gives the appearance of the oval shape through the camera while it is being heated, due to the angle of the camera

Remained at max setpoints over weekend.

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

 Tuesday, October 04, 2016, 13:40

Vented in air and opened up this morning.

Container done, TaC coating looks good.

Waiting further inspection...

 Tuesday, October 04, 2016, 14:48

Container placed on jig and inspected.

Approved to go ahead for use online by Anders and Friedhelm.

John Wong wrote:

Laura Lambert wrote: Friday, October 07, 2016, 16:40 Target consists of 470 discs. Total packed length 3.4cm [exactly 7.8cm space on both sides] Total mass g [Incl foils + Ta wire on 6 packs] Note: Target consists of 350 single discs and 6x20 packs of Ta discs 3x Ta Heat shields. No endcaps inserted, no Rh foil inserted. Chamber currently pumping down. TBHT will be ramped up to 230A at 1.0A/min. TGHT will be ramped up to 300A at 2.0A/min. Final desired temperature = 1900C  Tuesday, October 11, 2016, 10:02   HS water valves opened, no leaks detected   Tapped up manually to 35A   Vacuum stable, IGP1 = 2e-7 Torr   Initiating auto-ramp.   OMEGA slope = 0.98  Wednesday, October 12, 2016, 16:15 Tapped up to 1900C? [see attached link for data concerning temperature readings] TGHT = 450A, 7.16V TBHT = 230A, 4.1V OMEGA = 1748C IGP1 = 6.1e-7 Torr    Wednesday, October 12, 2016, 21:14 Current status before cooling down: TGHT at 450A/7.32V; TBHT at 230A/4.10V; OMEGA at 1747C Vacuum at 4.05 e-7 Torr. Initiate auto-rampping at 2A/min for TGHT and 1A/min for TBHT

 Thursday, October 13, 2016, 17:32

vented in air and opened up this morning.

target looks good.

Aurelia Laxdal wrote:

Aurelia Laxdal wrote: Laura Lambert wrote: Thursday, October 13, 2016, 18:04 Target loaded into evap2 No heat shields. Both endcaps inserted and expanded. Rh foil inserted [when inserting, the Ta rod used to expand the Rh foil inside the ionizer tube snapped off inside the container - this piece was able to be shaken out and is no longer inside] Chamber pumped down. HS water valves opened, no leaks detected   Tapped up manually to 35A   Vacuum stable, IGP1 = 5e-7 Torr   Initiating auto-ramp.   OMEGA slope = 0.98 TBHT will be ramped up to 230A at 1.0A/min. TGHT will be ramped up to 300A at 2.0A/min. Final desired temperature = 1900C Friday, October 14, 2016, 13:28 TGHT and TBHT had reached 300A/ 230A respectively. Power bump ~10min ago caused evap2 to trip off. Tapped back up manually to 35A. Re-initiating auto ramp now.   Friday October 14: the target was ramp up to 300A/230A after Laura started it. Then, I cooled down at 6pm before leaving TRIUMF. <br> Saturday October 15: restated the auto-ramp for Ta#50 in EVAP2. It's currently set to go to 300A/230A.  Sunday October 16: the target temperature measurements up to 620A/230A were performed today not on October 15 (yesterday, it was cooled down before reaching 300A/230A). Currently the target is cooling down, to be ready tomorrow morning for the Test Stand.

 Monday, October 17, 2016, 09:21

Vented in air and taken out this morning.

Target looks good!

Monday, October 24, 2016, 17:43

Two samples were prepared and loaded into the target boat with 1 layer of heat-shied as shown in the attachment#1.

Ingredients used: np-SiC and very small about of 5% PVA to hold the powder together. 

Samples were dried in the oven at 110C before loaded in Evap#2. 

After dried:

Sample #1 (larger graphite boat, mass =0.3779) = 0.4259g (PVA mass unknown due to solution leaking out from the boat)

Sample #2 = 0.2306g (with 5% PVA of 0.4111g)

Test temperature at 1600C, expect TGHT to be around 400A. 

Monday, October 24, 2016, 17:50

Ramping up TGHT to 300A at 0.5A/min. Vac at 2.3e-6 Torr. 

 Tuesday, October 25, 2016, 12:59

TGHT reached to 300A and stabilized for 10 hours.  OMEGA temp reader at 1150C

Continue to ramp up TGHT

 Wednesday, October 26, 2016, 15:49

TGHT was ramped up to 450A/7.91V; the temp readers on MIKON and OMEGA were 1489 and 1535, respectively (see attachment).

The temperature was much lower than the previous two tests (see elog #296 and #335).  Not sure why... 

Will do composition analysis on the sample... 

Cooling down at 2A/min.

Laura Lambert wrote:

John Wong wrote: Tuesday, November 15, 2016, 16:48 Three samples were prepared  (see my logbook#1 page 3, preparing for carbonization). One layer of Ta foil was used to wrap around the target boat.  Chamber is currently being pumped down  Wednesday, November 16, 2016, 11:04 Ramping up TGHT at 2A/min, set at 350A. Desired temperature, ~1530C (similar heating condition as raw npSiC heat treatment, elog ID335)  Thursday, November 17, 2016, 10:09 TGHT reached to 350A/5.80V, stayed for over 20 hours.  Temp measured at 1276 C (Mikon) and 1270 (Omega), vac at 6.07e-7 Torr.  Stepping up TGHT to reach the desired temp.    Thursday, November 17, 2016, 11:13 TGHT = 400A, 6.73V IGP1 = 8.2e-7 Torr OMEGA = 1385C MIKRON = 1389C Tapping up manually to 1500C or a max setpoint of 450A Thursday, November 17, 2016, 11:56 TGHT = 450A, 7.85V IGP1 = 1.7e-6 Torr OMEGA = 1502C MIKRON = 1510C  Friday, November 18, 2016, 10:08 IGP1 = 5.3e-7 Torr TGHT = 450A, 7.9V OMEGA = 1510C MIKRON = 1515C Evap2 has remained at max setpoints for 23hrs. Initiating auto-cool at 2.0A/min

 Friday, November 18, 2016, 17:27

The heat treatment of the fiber mats is done. 

Analyzing steps...

Tuesday, November 22, 2016, 15:53

Target boat has a layer of niobium foil on the bottom of the boat.

A niobium foil has been made with slots to hold samples [similar to when sintering endcaps] *See attached photos

Niobium samples are placed in slots, holding in place, to avoid warping.

Smaller samples closest to MIKRON IR reading [left side]

Boat is wrapped with 1 large layer of Ta foil, wrapped around the boat 3x, careful to avoid touching samples.

Loaded into evap2 today.

Pumping down now...

 Wednesday, November 23, 2016, 11:45

HS water valves opened, no leaks detected.

Tapped up manually to 35A.

IGP1 = 6.4e-7 Torr

Setting auto-ramp rate at 0.2A/min to max setpoint of 250A.

Will tap up manually to final desired temperature of 1400C.

 Wednesday, November 23, 2016, 13:17

IGP1 = 5.9e-7

TGHT = 66A, 0.51V

Vacuum stable.

Increasing ramping rate to 1.0A/min

 Thursday, November 24, 2016, 08:46

IGP1 = 3.9e-7 Torr

TGHT = 250A, 3.41V      *NOTE: the current set reads 243.8A but the readout is 250A

OMEGA = 1013C

MIKRON has no reading yet

Tapping up manually to 1400C

 Thursday, November 24, 2016, 15:42

Samples have remained at ~1400C for 5hrs.

IGP1 = 5.8e-7 Torr

TGHT = 420A, 6.5V

OMEGA = 1410C

MIKRON = 1420C

Initiating auto-cool at 2.0A/min

 Friday, November 25, 2016, 11:39

Vented in air and opened up this morning.

Samples look good!