Thursday, March 07, 2019, 09:09

Transfer tube from Legnaro was coated with TaC.

The transfer tube was set in a tantalum boat and wrapped with 3 heat shields,

the legs of the transfer tube were let out of the shielding sheets.

Chamber pump down was started on Wednesday March 06, 2019.

Desired temperature TGHT = 1800 C, Omega slope set = 0.990.

IGP1= 4.48e-07 Torr

Will tap up TGHT manually to 40-50 A and monitor pressure.

 Thursday, March 07, 2019, 10:57

The TGHT current was left at 40 A for 50 min, the pressure achieved was 6.15e-7 Torr

The TGHT was rised to 45 A 11:00 am the pressure rised to 6.18e-7 Torr (11:10am)

The TGHT was rised to 50 A 11:10 am the pressure rised to 6.81e-7 Torr (11:32am)

auto ramp was set to 1 A/min to 300 A

Good vacuum 3e-5 Torr

Bad vaccum 5e-5 Torr

auto ramp was set to 1 A/min to 400 A

auto ramp was set to 1 A/min to 470 A

Final conditions TGHT = 485 A, 8.25V Temperature = 1800 C

The transfer tube stayed at 1800 C for 4 hours

auto ramp was set to -1 A/min to 0 A. 

Friday, March 08, 2019, 16:53 

EVAP2 was vented with air and the transfer tube was unloaded

 Wednesday, July 17, 2019, 10:57

Annealing of five RRR Nb samples following cold-working and resistance measurements.  Used to validate computational annealing model developed for SRF studies.  For more information contact Norman Muller, x6398.

Desired temperature 1025 C.

Five Nb samples wrapped with Nb foil were set on a tantalum boat (coated with TaC)

the tantalum boat was wrapped with two tantalum sheets.

The boat was installed in the EVAP2.

The initial vacuum was IGP1 = 1.26e-6 Torr.

Ramping rate 5 A/min to final current of 200 A.

Wednesday, July 17, 2019, 11:18 

At 155 A, the ramping rate was changed to 1 A/min 

Wednesday, July 17, 2019, 11:28 

The ramping was stopped at 167 A.

 Wednesday, July 17, 2019, 11:57

Conditions:

IGP1 = 1.65e-6 Torr

TGHT = 2.54 V, 174.46 A

Temperature ~ 950 C

Wednesday, July 17, 2019, 18:07

IGP1 = 1.16 e-6

TGHT = 3.18 V, 206.7 A

Temperature ~950 C

Cooling ramp 10 A/min 

 Vented with air

Suggestion for future annealing:

  Use tantalum boat without TaC coating.

Monday, November 04, 2019, 14:19 

Each endcap is separated with a disc of graphite foil and rolled into packs one pack of 4 and one pack of 8 within a foil envelope in a target boat.

There are also 3 coated springs interspersed.

The boat is wrapped with 3-layers of Ta heatshields.

Chamber pumped down overnight.

OMEGA slope = 0.99

Will Tap TGHT up to 40 A then autoramp to 400A at 1A/min.

Final desired temperature on OMEGA (tap)= 1800C

 Tuesday, November 05, 2019, 11:30

IGP1 = 9.6e-7 Torr

Autoramp TGHT to 40A at 1A/min

Tuesday, November 05, 2019, 11:44

IGP1= 2.6e-06 Torr

TGHT = 40.8 A, 0.37V

Will leave at 40 A for 1 hour

 Tuesday, November 05, 2019, 12:39

 IGP1=2.5e-6 Torr

TGHT =40.0A, .33V

Start ramping TGHT to 400A at 0.1A/min

Wednesday, November 06, 2019, 09:32

IGP1=7.8e-7 Torr

TGHT = 168.4A, 2.38V

increase ramp speed to 1A/min

 Wednesday, November 06, 2019, 14:07

IGP1= 2.34e-6 Torr

TGHT=400.0 A, 6.98V

set TGHT autoramp to 460A @ 1A/min aiming for 1850C (see attached plot)

Wednesday, November 06, 2019, 15:18

OMEGA = 1776 C

TGHT = 460.0A, 8.52V

IGP1= 4.7e-6 Torr

Starting manual tap up to 1810C

Wednesday, November 06, 2019, 15:36

OMEGA=1810 C

TGHT = 468.8A, 8.74V

IGP1=4.14e-6

Wednesday, November 06, 2019, 19:04

OMEGA=1822 C (has been between 1817-1824 C over 3.5 hours )

TGHT=468.8A, 8.67V

IGP1=1.9498e-06 Torr

Start TGHT ramp down at -2A/min

Thursday, November 07, 2019, 09:55

THGT = 0A, 0V overnight

IGP1= 3.2 e-07 Torr

Proceeding with unloading.

End caps looked good for online use.

Monday, February 01, 2021, 13:52  

Ta boat loaded with 20 Disc on either end capped with Ta springs to prevent overexpansion.   discs wrapped Graphite foil and boat wrapped in Ta heat-shields (3 layers).

Sample A on left side and sample B on right side.

Desired temperature= 1800C (expected TGHT 410 A).

good vacuum = 3.00 e-05 Torr

bad vacuum = 5.00 e-05 Torr

Evap2 left to pump down over night.

 Tuesday, February 02, 2021, 10:01

Pressure stable at IGP1= 7.8e-7 Torr

TGHT autoramp  set to 50 A @ 1/min

Tuesday, February 02, 2021, 13:45

IGP1=3.5e-6 Torr

TGHT =49.9 A, 0.56 V

Ramp at 1A/min to 100A

Wednesday, February 03, 2021, 08:25

IGP1= 5.5 e-07 Torr

TGHT = 100 A, , 1.2 V

Yesterday the camera failed to operate.  Cloud service discontinued.  The TS camera is offline but it is a different provider.  Will start ramping to 400A .

Ramp rate 2A/min

Wednesday, February 03, 2021, 15:55

ramped up to 520 A and 9.1V TGHT

Temperature average 1644 C but suspect actual temperature higher.

Held for 5 hours and started ramp down at -2A/min

Thursday, February 04, 2021, 9:35

IGP1= 2.99e-7 Torr

Begin pumpdown procedure and remove container

Note:  SiC evaporation on most discs.  The temperature was too high.  Need to repeat.

 Tuesday, February 18, 2014, 12:12

A new target boat was sprayed with TaC coating and let dry.
The target boat is NOT wrapped with Ta-heat shield.

Thermocouples have been attached to the target boat in order to monitor the internal temperature of the new target boat design. 

The boat was installed in Evap#2, chamber is currently being pumped down.

 Tuesday, February 18, 2014, 14:20

Chamber was pumped down this morning to 2.9e-6 Torr. HS cooling water valves were opened, no leaks detected.

TGHT was stepped up to 35A, voltage max set at 14V. TBHT currently at 0A.

Waited ~20min, current stabilized, vacuum started to drop, auto-ramp initiated at 0.2A/min and max setpoint to 700A.

Good vacuum: 3.00e-5 Torr; Bad vacuum: 4.00e-5 Torr.

Temperature reading on left: thermocouple touching edge of target boat; temperature reading on right: thermocouple floating in center of target boat.

 Wednesday, February 19, 2014, 09:11

TGHT has been slowly ramping up overnight at a rate of 0.2A/min

IGP1 = 3.9e-7 Torr, TGHT = 260A; stepping ramping rate up to 2.0A/min

 Wednesday, February 19, 2014, 15:25

IGP1 = 9.4e-7 Torr

Thermocouple T2 = 1267.8C

Internal temp measured with Mikron = 1600C

Increasing max setpoint to 720A due to previous not fully sintered new design of target boat.

 Thursday, February 20, 2014, 09:17

Thermocouple T2 = 1254.5C

Internal temp measured with Mikron = 1811C

IGP1 = 2.6e-7 Torr

Reached max setpoint yesterday evening.

Initiating auto-cooling at 2.0A/min.

 Friday, February 21, 2014, 10:47

Vented and opened chamber this morning.

Target boat not fully sintered. [see attached photos]

Close to a full sinter, and will re-sinter next week with endcaps, so will not re-sinter by itself.

 Tuesday, February 25, 2014, 16:08

The target containers end-caps were coated with TaC spray and let dry.

The caps are inserted in the target boat vertically with no heat shield and no graphite foil. [see attached photo]

The chamber is currently being pumped down overnight.

 Wednesday, February 26, 2014, 09:54

Chamber was pumped down overnight to 4.2e-7 Torr.

HS cooling water valves opened; no leaks detected.

TGHT was stepped up to 35A, voltage max set at 14V. TBHT currently at 0A.

Waited ~20min, current stabilized, vacuum started to drop, auto-ramp initiated at 0.2A/min and max setpoint to 700A.

Will ramp up to 700A rather than the usual 580A due to last round of endcaps not fully sintering at 580A with new target boat design.

Good vacuum: 3.00e-5 Torr; Bad vacuum: 4.00e-5 Torr.

 Thursday, February 27, 2014, 09:38

TGHT has been slowly ramping up overnight at a rate of 0.2A/min.

IGP1 = 2.8e-7 Torr; TGHT = 311A, 4.3V

Stepping ramping rate up to 2.0A/min.

 Friday, February 28, 2014, 08:53

TGHT reached max setpoint of 700A yesterday evening.

Internal temp measured with Mikron = 1700C

IGP1 = 3e-7 Torr 

Power = 12.95V

Initiating auto-cooling at 2.0A/min.

 Monday, March 03, 2014, 11:46

Vented and opened chamber this morning.

End caps not fully sintered! 

See attached photo comparison of fully sintered [grey], partially sintered from this round [light green] and pre-sinter [dark green].

Will not bother re-sintering, as partial sinter is enough.

 Friday, March 07, 2014, 11:41

The target container end-caps were sintered previously, but did not fully complete the sintering process [See elog entry # 119 EVAP2]

The caps are inserted in the target boat wrapped in graphite foils with 3 x Ta-heat shields.

The chamber was pumped down overnight.

IGP1 = 2e-7 Torr

HS cooling water valves were opened; no leaks detected.

TGHT was stepped up to 35A, voltage max set at 9.05V. TBHT currently at 0A.

 Friday, March 07, 2014, 11:52

Waited ~20min, current stabilized, vacuum started to drop, auto-ramp initiated at 0.5A/min and max setpoint to 500A.

Will ramp to 500A due to last failed round of end caps breaking with 3-ta heat shields at 580A.

Good vacuum: 3.00e-5 Torr; Bad vacuum: 4.00e-5 Torr.

 Friday, March 07, 2014, 13:21

IGP1 = 8e-7 Torr.

TGHT = 72A

Vacuum stable; therefore, increasing ramping rate up to 1.0A/min

 Friday, March 07, 2014, 14:20

IGP1 = 9.8e-7 Torr

TGHT = 130A

Vacuum stable; therefore, increasing ramping rate up to 2.0A/min

Laura Lambert wrote:

Friday, March 07, 2014, 11:41 The target container end-caps were sintered previously, but did not fully complete the sintering process [See elog entry # 119 EVAP2] The caps are inserted in the target boat wrapped in graphite foils with 3 x Ta-heat shields. The chamber was pumped down overnight. IGP1 = 2e-7 Torr HS cooling water valves were opened; no leaks detected. TGHT was stepped up to 35A, voltage max set at 9.05V. TBHT currently at 0A.  Friday, March 07, 2014, 11:52 Waited ~20min, current stabilized, vacuum started to drop, auto-ramp initiated at 0.5A/min and max setpoint to 500A. Will ramp to 500A due to last failed round of end caps breaking with 3-ta heat shields at 580A. Good vacuum: 3.00e-5 Torr; Bad vacuum: 4.00e-5 Torr.  Friday, March 07, 2014, 13:21 IGP1 = 8e-7 Torr. TGHT = 72A Vacuum stable; therefore, increasing ramping rate up to 1.0A/min  Friday, March 07, 2014, 14:20 IGP1 = 9.8e-7 Torr TGHT = 130A Vacuum stable; therefore, increasing ramping rate up to 2.0A/min

Friday, March 07, 2014, 22:22  

Target current was at 500A before it tripped off on the chiller.   Tried to reset the chiller but to no avail.  Don't know what is going on yet. 

The TGHT/TBHT cooling water is still on, and this should OK while the HOT target boat is cooling down at the moment. 

Will leave it for now and further investigate on Monday

Wednesday, July 23, 2014, 15:07

Target container is coated with TaC.  No Ta-heat shields are used.

TGHT will be ramped up to 580A at 0.2A/min.

TBHT will be ramped up to 230A at 0.2A/min.

Chamber is currently being pumped down

 Wednesday, July 23, 2014, 17:40

Vacuum came down to mid 10-6 Torr.

Stepped up TGHT and TBHT to 30A - IG1 @ 1.4e-5 Torr.

Initiated auto-ramping.

 Thursday, July 24, 2014, 17:19

TGHT and TBHT have reached to 100A, and vacuum is coming down to 1.4e-6 Torr.

Increase ramping rate, TGHT to 1A/min, TBHT 0.5A/min.

 Friday, July 25, 2014, 11:26

Target container temperature reaches ~1550C at 580A on TGHT and 230A TBHT, and it has been heated for ~10 hrs.

Auto-cooling initiated at 2A/min.

John Wong wrote:

Wednesday, July 23, 2014, 15:07 Target container is coated with TaC.  No Ta-heat shields are used. TGHT will be ramped up to 580A at 0.2A/min. TBHT will be ramped up to 230A at 0.2A/min. Chamber is currently being pumped down  Wednesday, July 23, 2014, 17:40 Vacuum came down to mid 10-6 Torr. Stepped up TGHT and TBHT to 30A - IG1 @ 1.4e-5 Torr. Initiated auto-ramping.  Thursday, July 24, 2014, 17:19 TGHT and TBHT have reached to 100A, and vacuum is coming down to 1.4e-6 Torr. Increase ramping rate, TGHT to 1A/min, TBHT 0.5A/min.  Friday, July 25, 2014, 11:26 Target container temperature reaches ~1550C at 580A on TGHT and 230A TBHT, and it has been heated for ~10 hrs. Auto-cooling initiated at 2A/min.

 Monday, July 28, 2014, 10:50

vented in air and opened this morning. successful run

 Monday, July 28, 2014, 14:41

Total number of foils: 445 discs

Total mass of materials [incl graphite foils]: 49.027 g

Total length packed: 11.2 cm

Container has no Ta heat shields.

Currently being pumped down.

Laura Lambert wrote:

Monday, July 28, 2014, 14:41 Total number of foils: 445 discs Total mass of materials [incl graphite foils]: 49.027 g Total length packed: 11.2 cm Container has no Ta heat shields. Currently being pumped down.

 Tuesday, July 29, 2014, 11:19

Chamber was pumped down overnight to ~5.5e-7 torr.

HS water valve opened; no leaks were detected.

Stepped up TGHT/TBHT to 40A. IG went up 8e-6 Torr and stabilized. 

Initiated auto-ramping TGHT @ 580A, TBHt @ 230A at 0.2A/min

The maximum current of 580A was reached at 9:15.

TGHT:RDCUR 578 A

TGHT:RDVOL 9.87 V

IGP1:RDVAC 3.8e-6

The temperature was measured with the Minolta 2-color pyrometer:

from the side - inside target container : ~1200 deg C

from the front trough hole in the heat shield : ~1800 deg C

Target was conditioned for 4 hours at 580A.

Initiating ramp-down sequence @ 2A/min

Peter Kunz wrote:

Target was conditioned for 4 hours at 580A. Initiating ramp-down sequence @ 2A/min

 Tuesday, August 05, 2014, 12:00

target vented in air and taken out this morning

 Thursday, September 11, 2014, 13:14

The target container end caps were coated with TaC spray and let dry.

The caps are inserted in the target boat wrapped in graphite foil with 3 x Ta-heat shields.

The chamber is currently pumping down.

 Friday, September 12, 2014, 14:17

Chamber was pumped down overnight.

HS cooling water valves opened, no leaks detected.

IGP1 = 7.2e-7 Torr.

TGHT stepped up to 35A, TBHT at 0A.

Waited ~30min, current stabilized, vacuum started to drop, auto-ramp initiated at 0.2A/min.

Will ramp TGHT to 580A with a max 10V.

Good vacuum: 3.00e-5 Torr; Bad vacuum: 4.00e-5 Torr.

 Monday, September 15, 2014, 11:31

TGHT stopped at 500A due to not high enough voltage max.

Increased max voltage to 12V

 Monday, September 15, 2014, 14:17

IGP1 = 6.3e-7 Torr

Increasing ramping rate to 1.0A/min

 Tuesday, September 16, 2014, 09:04

TGHT reached 577A and finished auto-ramping, then proceeded to drop down to 560A overnight.

Increased max voltage to 13.05A and TGHT to 580A.

 Tuesday, September 16, 2014, 13:52

TGHT reached 580A and sat there for ~5hrs.

IGP1 = 6.1e-7 Torr.

Initiating auto-cool at 2.0A/min.

 Wednesday, September 17, 2014, 13:03

Vented in air.

Opened up....looked 'deceivingly' ok.

then i took a layer of Ta off....grrrr  

the 1st layer of Ta was holding the boat together. as soon as that layer was taken off the target boat broke.

see attached photos.

 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.

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

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!

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!