John Wong wrote:

Nikita Bernier wrote: Wednesday, June 20, 2012, 17:23 New Target boat, with no coating, wrapped with a 0.002 inches thick Ta foil, contains NiO D-shape discs : Sample,   # Disks,    Mass (g),    Thickness (mm) 1    12,  1.9396,  1.938 2    13,  0.9592,  0.847 3    25,  2.6675,  3.06 See John's Ipad for their recipes. Evaporator #2 is now auto-ramping overnight at 0.5 A/min, up to 580 A, with the maximum voltage limited at 14 V, between 3.00e-05 (Good vacuum) and 4.00e-05 Torr (Bad vacuum).   Wednesday, June 20, 2012, 22:28 TGHT tripped off at 78A due to high out-gassing pressure.  The current was tapped down to 75A before it was turned back on.  Changed ramping rate from 0.5A/min to 0.2A/min.   Initiate auto-ramping...   Thursday, June 21, 2012, 08:35 Vacuum has come down to 7e-7 as TGHT is being ramped up at 0.2A/min. (see attachment#1). Increase TGHT rate to 2A/min. The temperature should be measured when the heater gets up to around 500A.

 Thursday, June 21, 2012, 17:37

The NiO discs were heated up to 1500C at 560A.  The target heater was lowered in steps and the temperature was measured.  At 320A, the target container was ~1110C.  (see attachment #1) 

There was a sign of resistant on the target container as the p/s voltage started to go up at a higher rate.  (see attachment#2, 3, 4 for the archived striptool).

Unfortunately, the target container was broken; it was most likely reacted with the Ni.  (see attachment#5)

So.... the possible solution?!  TRY coating the container with Ta2O5.  Will discuss more in the Friday Jun 22 meeting. 

Wednesday, June 20, 2012, 17:23

New Target boat, with no coating, wrapped with a 0.002 inches thick Ta foil, contains 3 NiO pellets :

Sample,   # Disks,    Mass (g),    Thickness (mm)

1    12,  1.9396,  1.938

2    13,  0.9592,  0.847

3    25,  2.6675,  3.06

See John's Ipad for their recipes.

Evaporator #2 is now auto-ramping overnight at 0.5 A/min, up to 580 A, with the maximum voltage limited at 14 V, between 3.00e-05 (Good vacuum) and 4.00e-05 Torr (Bad vacuum).

Thursday, June 21, 2012, 18:14  

See attachment #1, 2 for the density measurements and the graph for the disc thickness  -JW 

Nikita Bernier wrote:

Wednesday, June 20, 2012, 17:23 New Target boat, with no coating, wrapped with a 0.002 inches thick Ta foil, contains NiO D-shape discs : Sample,   # Disks,    Mass (g),    Thickness (mm) 1    12,  1.9396,  1.938 2    13,  0.9592,  0.847 3    25,  2.6675,  3.06 See John's Ipad for their recipes. Evaporator #2 is now auto-ramping overnight at 0.5 A/min, up to 580 A, with the maximum voltage limited at 14 V, between 3.00e-05 (Good vacuum) and 4.00e-05 Torr (Bad vacuum).

Wednesday, June 20, 2012, 22:28

TGHT tripped off at 78A due to high out-gassing pressure.  The current was tapped down to 75A before it was turned back on. 

Changed ramping rate from 0.5A/min to 0.2A/min.  

Initiate auto-ramping... 

 Thursday, June 21, 2012, 08:35

Vacuum has come down to 7e-7 as TGHT is being ramped up at 0.2A/min. (see attachment#1).

Increase TGHT rate to 2A/min.

The temperature should be measured when the heater gets up to around 500A.

 Thursday, February 09, 2017, 11:47

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

 Dan made a set of new cooling lines for the Source Tray Heat Shield cooling yesterday. No joints on the lines. Use same VCR fitting 3/8 -> 1/4" as for the Heat Shield. The old lines had worn threads on the male VCR nut.

 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. 

Old HS sprang a leak in the copper tubing.  

HS#44378-15

Tuesday, April 12, 2022, 13:35: Roughing. 

Tuesday, April 12, 2022, 13:49: TP1 switched on. 

Tuesday, April 12, 2022, 13:57: TP1 stable (green).

Tuesday, April 12, 2022, 14:10: Vacuum @ 3.71e-05T & dropping.

Tuesday, April 12, 2022, 14:11: HS waterline opened. 

Tuesday, April 12, 2022, 14:12: Vacuum @ 3.32e-05T.

Tuesday, April 12, 2022, 14:22: Vacuum @ 2.19e-05T (Stable).

 Friday, June 11, 2021, 08:05

Target boat with a layer of niobium foil on the bottom is used to heat up Nb samples to 1100 C for 4 hrs.

OMEGA slope = 0.99

The niobium samples are wrapped in a layer of  Nb foil.

Boat is wrapped with 2 layers of Nb foil.

Good vacuum 3.00e-02 Torr

Bad vacuum 5.00e-02 Torr

Autoramping TGHT at 2A/min to 50A then to 100A, then monitor until desired temperature

Initial IGP1= 9.4e-07 Torr

Friday, June 11, 2021, 09:59

TGHT = 200 A, 2.7V

IGP1=  9.8e-07 Torr

Tap to 1100C

Friday, June 11, 2021, 10:09 

Temperature reached at 10:05 am.

TGHT = 224A, 3.1V

IGP1= 1.0e-06 Torr

OMEGA= 1100C +/- 10C fluctuations

Friday, June 11, 2021, 14:10

TGHT = 224A, 3.1V

IGP1= 9.2e-.07 Torr

OMEGA = 1100C +/-  10C fluctuations

Started rampdown at -3A/min

Tuesday, September 17, 2013, 11:14

Target boat contains 5 Nb discs.  3 discs are wraps with 0.001" thin of Nb foil (99.8% pure), and 2 are wraps with 0.001" Ta foil (see attachment#1)

Chamber has been pumped down over night.  Pressure is currently at 9.8e-7 Torr. 

Heating instructions:

Samples will be heated up to 800C.  TGHT will be ramped up accordingly. (Two thermocouples are wielded on the target container.)

Once at the desired temperature; the samples will be heat for 4 hours before cooling down.

 Tuesday, September 17, 2013, 14:37

Target temperature has reached to 800C at around 13:00 (see attachment#2)

TGHT @ 230A/3.07V (local 233A/3.25V). 

IG @ 1.06e-6 Torr. 

The heater will be ramped down at ~17:00 at 2A/min.

 Tuesday, September 17, 2013, 17:36

Target temp: T1 = 805C, T2=797.6C

IG @ 9.4e-7 Torr.

Cooling down initiated. 

 Wednesday, September 18, 2013, 11:34

TGHT at 0A.  Temp at 22C. 

IG @ 5.8e-7 Torr.

Venting chamber.

John Wong wrote:

Tuesday, September 17, 2013, 11:14 Target boat contains 5 Nb discs.  3 discs are wraps with 0.001" thin of Nb foil (99.8% pure), and 2 are wraps with 0.001" Ta foil (see attachment#1) Chamber has been pumped down over night.  Pressure is currently at 9.8e-7 Torr.  Heating instructions: Samples will be heated up to 800C.  TGHT will be ramped up accordingly. (Two thermocouples are wielded on the target container.) Once at the desired temperature; the samples will be heat for 4 hours before cooling down.  Tuesday, September 17, 2013, 14:37 Target temperature has reached to 800C at around 13:00 (see attachment#2) TGHT @ 230A/3.07V (local 233A/3.25V).  IG @ 1.06e-6 Torr.  The heater will be ramped down at ~17:00 at 2A/min.  Tuesday, September 17, 2013, 17:36 Target temp: T1 = 805C, T2=797.6C IG @ 9.4e-7 Torr. Cooling down initiated.   Wednesday, September 18, 2013, 11:34 TGHT at 0A.  Temp at 22C.  IG @ 5.8e-7 Torr. Venting chamber.

 Thursday, September 19, 2013, 11:41

Target boat contains batch#2 Nb samples (see attachment #1)

Chamber has been pumped down over night.  

IG @ 5.5e-07 Torr. 

CG1B @ 0.033 T

CG1A @ 0.127 T

There is a leak in the backing line.  BV1 was bypassed in order to turn on the turbo pump. (Will investigate the leaks after the processes are done)  

*See attached picture to view samples

Laura Lambert wrote:

John Wong wrote: Tuesday, September 17, 2013, 11:14 Target boat contains 5 Nb discs.  3 discs are wraps with 0.001" thin of Nb foil (99.8% pure), and 2 are wraps with 0.001" Ta foil (see attachment#1) Chamber has been pumped down over night.  Pressure is currently at 9.8e-7 Torr.  Heating instructions: Samples will be heated up to 800C.  TGHT will be ramped up accordingly. (Two thermocouples are wielded on the target container.) Once at the desired temperature; the samples will be heat for 4 hours before cooling down.  Tuesday, September 17, 2013, 14:37 Target temperature has reached to 800C at around 13:00 (see attachment#2) TGHT @ 230A/3.07V (local 233A/3.25V).  IG @ 1.06e-6 Torr.  The heater will be ramped down at ~17:00 at 2A/min.  Tuesday, September 17, 2013, 17:36 Target temp: T1 = 805C, T2=797.6C IG @ 9.4e-7 Torr. Cooling down initiated.   Wednesday, September 18, 2013, 11:34 TGHT at 0A.  Temp at 22C.  IG @ 5.8e-7 Torr. Venting chamber.    Thursday, September 19, 2013, 11:41 Target boat contains batch#2 Nb samples (see attachment #1) Chamber has been pumped down over night.   IG @ 5.5e-07 Torr.  CG1B @ 0.033 T CG1A @ 0.127 T There is a leak in the backing line.  BV1 was bypassed in order to turn on the turbo pump. (Will investigate the leaks after the processes are done)   *See attached picture to view samples

Thursday, September 19, 2013, 17:01  

TGHT reached to 800A.  Temp at 795.9C for 4 hours.  Vac at 5.8e-7 Torr.

Cooling down initiated.  ramping rate at 2A/min. 

John Wong wrote:

Tuesday, September 17, 2013, 11:14 Target boat contains 5 Nb discs.  3 discs are wraps with 0.001" thin of Nb foil (99.8% pure), and 2 are wraps with 0.001" Ta foil (see attachment#1) Chamber has been pumped down over night.  Pressure is currently at 9.8e-7 Torr.  Heating instructions: Samples will be heated up to 800C.  TGHT will be ramped up accordingly. (Two thermocouples are wielded on the target container.) Once at the desired temperature; the samples will be heat for 4 hours before cooling down.  Tuesday, September 17, 2013, 14:37 Target temperature has reached to 800C at around 13:00 (see attachment#2) TGHT @ 230A/3.07V (local 233A/3.25V).  IG @ 1.06e-6 Torr.  The heater will be ramped down at ~17:00 at 2A/min.  Tuesday, September 17, 2013, 17:36 Target temp: T1 = 805C, T2=797.6C IG @ 9.4e-7 Torr. Cooling down initiated.   Wednesday, September 18, 2013, 11:34 TGHT at 0A.  Temp at 22C.  IG @ 5.8e-7 Torr. Venting chamber.

 Friday, September 20, 2013, 14:56

Target contains batch#3 sample wrapped with Nb foil. 

Chamber has been pumped down to 1.03e-6 Torr. 

Samples will be heated up to 1200C for 4 hours.  

 Friday, September 20, 2013, 16:54

TGHT at 450A, temp stabilizes at 1238C.

Will cool down at 20:30 tonight.

Friday, September 20, 2013, 20:40  

Samples has been heated for 4 hours at 1235C.  

Cooling down initiated. 

 Monday, September 23, 2013, 14:40

Chamber was vented.

Batch#3 process completed.

John Wong wrote:

John Wong wrote: Tuesday, September 17, 2013, 11:14 Target boat contains 5 Nb discs.  3 discs are wraps with 0.001" thin of Nb foil (99.8% pure), and 2 are wraps with 0.001" Ta foil (see attachment#1) Chamber has been pumped down over night.  Pressure is currently at 9.8e-7 Torr.  Heating instructions: Samples will be heated up to 800C.  TGHT will be ramped up accordingly. (Two thermocouples are wielded on the target container.) Once at the desired temperature; the samples will be heat for 4 hours before cooling down.  Tuesday, September 17, 2013, 14:37 Target temperature has reached to 800C at around 13:00 (see attachment#2) TGHT @ 230A/3.07V (local 233A/3.25V).  IG @ 1.06e-6 Torr.  The heater will be ramped down at ~17:00 at 2A/min.  Tuesday, September 17, 2013, 17:36 Target temp: T1 = 805C, T2=797.6C IG @ 9.4e-7 Torr. Cooling down initiated.   Wednesday, September 18, 2013, 11:34 TGHT at 0A.  Temp at 22C.  IG @ 5.8e-7 Torr. Venting chamber.    Friday, September 20, 2013, 14:56 Target contains batch#3 sample wrapped with Nb foil.  Chamber has been pumped down to 1.03e-6 Torr.  Samples will be heated up to 1200C for 4 hours.    Friday, September 20, 2013, 16:54 TGHT at 450A, temp stabilizes at 1238C. Will cool down at 20:30 tonight. Friday, September 20, 2013, 20:40   Samples has been heated for 4 hours at 1235C.   Cooling down initiated.   Monday, September 23, 2013, 14:40 Chamber was vented. Batch#3 process completed.

 Monday, September 23, 2013, 16:14

Batch#4.  Target container contains 2 Nb stables (a bullet type and a disc).  

Samples are wrapped with "dimpled" Nb foil to prevent diffusion bonding. 

Chamber has been pumped down to 8.3e-7 Torr, CG1B @ 30mT, CG1A @ 118mT. 

Samples will be heated up to 1400C for 4 hours. 

Monday, September 23, 2013, 17:46

TGHT at 620A. Temp at 1400C. Current pressure @ 2.5e-6 Torr. 

Tuesday, September 24, 2013, 16:45

Sample#4 was heated up to 1400C and after about 3hrs, the target container started to break.

See the link below for more details:

https://www.dropbox.com/s/9mhpkz66u6yqldm/Nb_1400C.mp4

Wednesday, February 09, 2022, 06:55 

Target boat with a layer of niobium foil on the bottom used to heat up Nb samples to 1100 C for 4 hrs.

OMEGA slope = 0.99

The niobium samples are wrapped in a layer of  Nb foil.

Boat is wrapped with 2 layers of Nb foil.

Good vacuum 3.00e-02 Torr

Bad vacuum 5.00e-02 Torr

Autoramping TGHT at 3A/min to 180A, then monitor until desired temperature (based on eLog 550)

Initial IGP1=9.9e-07 Torr

Wednesday, February 09, 2022, 08:00

TGHT = 225 A, 3.2V

IGP1=  1.17e-06 Torr

OMEGA= 1100C +/- 12C fluctuations 

Wednesday, February 09, 2022, 11:55

TGHT=  225 A, 3.3 V

IGP1= 9.7e-07 Torr

OMEGA=1100C +/- 10C fluctuations

Wednesday, February 09, 2022, 11:56

Start cooling @-2A/min 

Wednesday, February 09, 2022, 06:55 

Target boat with a layer of niobium foil on the bottom used to heat up Nb samples to 1400 C for 4 hrs.

OMEGA slope = 0.99

The niobium samples are wrapped in a layer of  Nb foil.

Boat is wrapped with 2 layers of Nb foil.

Good vacuum 3.00e-02 Torr

Bad vacuum 5.00e-02 Torr

Autoramping TGHT at 2A/min to 200A, then monitor until desired temperature

Initial IGP1=6.0e-06 Torr

Tuesday, February 15, 2022, 12:44

Increasing ramp up to 3A/min to 220 A as pressure very stable

Tuesday, February 15, 2022, 14:04

ramped up manually to 1400C

IGP1 =3.9 e-06 Torr

TGHT = 340A, 5.5V

OMEGA = 1400 C

Tuesday, February 15, 2022, 14:21

Temperature on OMEGA up to 1413 C

Lowering current to 332A , OMEGA = 1400 +/- 5C

Wednesday, February 16, 2022, 11:43

On Tuesday February15, 2020 @18:04 started ramp down @-3A/min

Sample loaded into a vertical target boat. Flex line HS removed, SS waterline HS installed -AS.

Thursday, September 24, 2020, 13:22: Roughing.

Thursday, September 24, 2020, 13:54: Turbo pump on. 

Tuesday, May 08, 2018, 15:02

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

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

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

Omega slope set at 1.05 (for carbide)

Chamber is currently being pumped down

 Tuesday, May 08, 2018, 22:46

Pressure at 2.2e-6 Torr.

Initiated autoramping at 0.2A/min to reach 330A

 Friday, May 11, 2018, 11:11

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

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

 Sunday, May 13, 2018, 00:25

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

 Sunday, May 13, 2018, 14:10

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

cooling down at 2A/min.

 Monday, May 14, 2018, 09:33

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

Venting chamber.

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

Tuesday, May 01, 2018, 18:06

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

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

 Wednesday, May 02, 2018, 08:27

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

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

System problem??  Archive striptool for more details. 

Re-activate auto-ramping - OK!

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

 Friday, May 04, 2018, 01:09

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

Continue autoramping to reach TGHT 300A.

 Friday, May 04, 2018, 11:07

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

Autoramp to 320A.

 Friday, May 04, 2018, 14:39

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

 Sunday, May 06, 2018, 13:25

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

Cooling down at 2A/min. 

 Monday, May 07, 2018, 10:49

Evap cooled.  Venting chamber. 

Inspection of the discs next...

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

Tuesday, July 03, 2018, 17:02

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

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

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

Omega slope set at 1.05 (for carbide)

Chamber is currently being pumped down

 Wednesday, July 04, 2018, 10:38

Pressure at 1.5 e-6 Torr.

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

 Monday, July 09, 2018, 14:44

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

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

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

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

 Monday, July 09, 2018, 16:42

Pressure stabilized at 3.5e-7 Torr. 

Initiated auto-cooling at 1A/min.

 Tuesday, July 10, 2018, 11:11

Target is at room temperature. 

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

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

Wednesday, September 27, 2017, 18:05

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

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

Desired temperature = 1550C, est current = 450A

 Thursday, September 28, 2017, 11:17

Vac at 8.8e-7 Torr.  

Ramping TGHT up to 450A at 0.2A/min

 Thursday, September 28, 2017, 17:54

Setup screen capture, see pg 53 for saved directory

 Friday, September 29, 2017, 23:54

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

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

Pressure coming down from 1.6e-6 Torr.

See attachment 1 for the 20-hour plot

 Sunday, October 01, 2017, 00:30

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

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

 Monday, October 02, 2017, 17:55

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

 Tuesday, October 03, 2017, 11:09

Target has been cooled for over 10 hours. 

Venting chamber