ELOG Evaporator

Small graphite cartridge was loaded with SiC discs 240523-1 and 240523-2 and 220727-2 (baseline discs). Test Discs produced without milling using PAA as a dispersant.

The coated container tube was wrapped in four Ta foil heatshields.

two Tac Coated springs at the ends in case plugs are pushed outwards.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:= 0.990

Target time at max temperature = 4 hours

Final TGHT current= ~400A (adjustable)

Heating autoramp 2A/min to 90 A

Then at 2A/min to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

IGP1 initial 4.8e-07 Torr

Wednesday, May 29, 2024, 22:54

Kept at 400 A for 4 hours.

Starting autoramp down at -2A/min

664

Wednesday, June 05, 2024, 07:18

sinterin experiment 240604

Wednesday, June 05, 2024, 07:14

SiC discs loaded into tantalum tube. New mixing (two types) and old mixing.

The coated container tube was wrapped in four Ta foil heatshields.

Tac Coated springs at the ends in case plugs are pushed outwards.

Target temperature on OMEGA= 1850-1900 C

OMEGA slope:=* 0.980*

Target time at max temperature = 4 hours

Final TGHT current= ~400A (adjustable)

Heating autoramp 1A/min to 90 A

Then at 2A/min to 120A.

Good vacuum = 5.0 e-02 Torr

Bad vacuum = 5.0E-04 Torr

IGP1 initia1.3e-06Torr

Wednesday, June 05, 2024, 11:04

Continuing to ramp at 2A/min to 350A

Wednesday, June 05, 2024, 12:22

Leaving at 369 A for 4 hours (until 4 pm). Temperature readings do not appear good.

Wednesday, June 05, 2024, 16:01

Start rampdown at -2A/min

IGP1=2.0 e-6 Torr

669

Thursday, August 08, 2024, 11:17

Graphite foils conditioning

Aaron Schmidt wrote:

Wednesday, August 07, 2024, 15:36: Roughing. Had initially been roughed & TP started w/ Marla CS, however it timed out. Restarting.

Wednesday, August 07, 2024, 15:37: TP on.

Wednesday, August 07, 2024, 15:46: Tripped at 4 KRPM. Restarted. Up to 5 KRPM.

Failed to start.

Thursday, August 08, 2024, 10:00: TP started.

Thursday, August 08, 2024, 10:12: TP Tripped but nearly spun up. Reset & Restarted. TP Green / on.

Thursday, August 08, 2024, 10:43

A cartridge was filled with graphite foils and loaded in an uncoated tantalum tube. The tube was wrapped with four Ta-sheets. A Ta-foil was placed in the tube's right end for measuring the temperature.

Green graphite target characteristics
Number of discs	822
Mass of discs	11.74 g
Mass of loaded cartridge with normal cap and hole-cap	31.1290 g
Mass of tube loaded, w/shields and tantalum cap	250 g

Note: A cartridge loaded with graphite foils has not been conditioned before. Thus, there is no reference on what current to use to reach 2000 °C.

The conditioning of a graphite composite target will be used as a reference, but note that the graphite foils are not expected to outgas as the composites since the foils do not contain binders and plasticizers.

Reference: Elog 636 Graphite inside insert Experiment 2 (regular formulation discs)

Initial ramps used in elog 636:

1A/min to 200A
0.5A/min while taking temperature readings periodically until 250A
At 250 A will let pressure stabilize and then ramp at 1A/min to 2000C or 480A

Currently waiting for vacuum to reduce to IGP1= 8.2e-07

Thursday, August 08, 2024, 11:23

Slope: 0.98 (same as slope used for tantalum targets since temperature is measured on Ta foil)

Friday, August 09, 2024, 08:50

Good vacuum 3e-5 Torr

Bad vacuum 5e-5 Torr

Initial IGP1 = 5.06E-7 Torr

Starting ramp at 1A/min to 200 A

Friday, August 09, 2024, 09:40 Pressure started to rise, but temperature is not within pyrometer range yet. Current 42 A, Voltage 0.5 V

Friday, August 09, 2024, 10:46 Pressure started to reduce (peak 1.4e-5 Torr). Temperature is not within pyrometer range yet Current 100 A, Voltage 1.3 V

Friday, August 09, 2024, 11:28 Temperature started to be detected, but not stable enough. Current 135 A, Voltage 1.9 V

Friday, August 09, 2024, 12:54 Temperature 1129 °C, current 196 A, voltage 3 V.

Friday, August 09, 2024, 12:56

Next ramp 0.5A/min while taking temperature readings periodically until 250A

Friday, August 09, 2024, 14:45

IGP1 = 1.0e-6 Torr

Next ramp 1A/min to 480 A aiming at 2000 °C

Friday, August 09, 2024, 17:13

IGP1 = 1.9e-6 Torr, Current 327A, Voltage 5.3V

Ramp changed to 2A/min to 480 A aiming at 2000 °C

Coolded down after 4 hours at ~2000°C

at -2A/min

Attachment 1: GraphiteFoil-Conditioning-EVAP2.JPG

670

Wednesday, August 14, 2024, 07:23

EVAP2 Calibration - Vanadium

Tuesday, August 13, 2024, 17:20 Pressure kept increasing when turning the turbo pump on

Tuesday, August 13, 2024, 18:00 Pressure stayed constant when turning the turbo pump on

Attachment 1: TP-not_speeding_up.JPG

671

Wednesday, August 14, 2024, 16:22

EVAP2 Calibration - Vanadium

Marla Cervantes wrote:

Tuesday, August 13, 2024, 17:20 Pressure kept increasing when turning the turbo pump on

Tuesday, August 13, 2024, 18:00 Pressure stayed constant when turning the turbo pump on

Wednesday, August 14, 2024, 10:18

The turbo pump started up normally. System is purging. and tomorrow the target will be heated.

672

Wednesday, August 14, 2024, 16:24

EVAP2 Calibration - Vanadium

Marla Cervantes wrote:

Marla Cervantes wrote:

Tuesday, August 13, 2024, 17:20 Pressure kept increasing when turning the turbo pump on

Tuesday, August 13, 2024, 18:00 Pressure stayed constant when turning the turbo pump on

Wednesday, August 14, 2024, 10:18

The turbo pump started up normally. System is purging. and tomorrow the target will be heated.

Wednesday, August 14, 2024, 16:19

A vanadium wire was introduced in a tantalum pouch and snug among the graphite foils of a conditioned graphite target. The V wire was introduced in the Ta pouch to prevent the direct contact of the wire with the carbon and avoid the reaction between them.

As a first approach, the target will be heated to approximately 1377 °C, aiming at the vaporization temperature of the V wire. If the wire does not vaporize, heating with the turbo pump off would be considered to aim at the vanadium's melting point of 1910 °C.

Plan:

The temperature of the tube will be measured from the side on a Ta-foil cap with a two-colour pyrometer, and from the center with a filament pyrometer (a pinhole was made on the tantalum tube heat shields to allow looking at the tube.
The temperature registered by the omega will be used as a rough reference of the temperature range at which the V wire is either melting or vaporizing.
- The pressure will be closely monitored to have a reference for the V vaporization.

Vanadium	Temperature (°C)
Vaporization (at 3e-6 Torr)	1377
Melting	1910

Initial ramping: 2 A/min to 200 A.
Expected temperature: approx. 1100 °C. Estimated ramping duration

In case of outgassing, let the pressure reduce

Next ramping: 0.5 A/ 2min to 250 A.

Very slow rate to allow thermal equilibrium and temperature measurements. Estimated time 3h.

Thursday, August 15, 2024, 08:21

IGP1 = 5.3e-7 Torr

Good vacuum 3e-5 Torr

Bad vacuum 5e-5 Torr

Initial ramping: 2 A/min to 200 A.

Thursday, August 15, 2024, 09:01. Pressure starting to increase at 74 A

Thursday, August 15, 2024, 09:15. Pressure stabilizing 1.8e-6 Torr. Current 103 A, voltage 1.3 V

Thursday, August 15, 2024, 09:21. Pressure increasing (116 A).

Thursday, August 15, 2024, 09:29 Pressure dropping (Current approx. 120 A)

Thursday, August 15, 2024, 10:54

Started ramping to find a pressure peak corresponding to V vaporization.

IGP1 = 6.4e-7

TGHT = 200 A, 2.9 V, omega 1152 °C

Next ramping: 0.5 A/ 2min to 250 A

Thursday, August 15, 2024, 11:17

Ramp seem to slow. The temperature change was too subtle (according to the omega).

IGP1 = 6.5e-7

TGHT = 205 A, 3.03 V, omega 1157 °C

Next ramping: 1 A/ 2min to 250 A

Thursday, August 15, 2024, 11:32

Ramp changed to 0.5 A/min

Thursday, August 15, 2024, 11:54

Ramp was stopped because the pressure was increasing, suggesting the V vaporization.

IGP1 = 6.9e-7

TGHT = 222 A, 3.3 V

Omega 1210 °C, filament 1280 °C

The difference between pyrometers is negligible, suggesting that the V vaporization temperature at 6e-7 Torr of approx. 1300 °C

Thursday, August 15, 2024, 13:15

IGP1 = 7.9e-7

TGHT = 250 A, 3.8 V

Omega 1289 °C

Thursday, August 15, 2024, 13:16

Ramp set to 0.5 A/min to 300 A

Pressure mini-spike at 13:18

Omega reading 1291 °C

Thursday, August 15, 2024, 14:08

IGP1 = 8.5e-7

TGHT = 270 A, 4.18 V

Omega 1375 °C, filament 1400 °C

The system stayed at those conditions for 15min

Thursday, August 15, 2024, 14:11

Ramping to 0A at 2A/min

678

Wednesday, October 02, 2024, 19:24

sintering TiC Experiment

Wednesday, October 02, 2024, 19:21

Ta endcup at front end of container

End-caps on the graphite cartridge have holes for outgassing.

initial heating @ 2A/min to 85 A then 2A/min to 120A TGHT. Allow pressure to drop and then ramp to 400 A at 2A/min, leave 4 hours and start ramp down.

OMEGA slope = 0.99

Vacuum limits up to 400A: 5.0e-04 Torr -- 1.0e-02 Torr

Max current~400A (1900 C)

Wednesday, October 02, 2024, 19:25

Starting IGP1 = 6.65e-06 Torr

Thursday, October 03, 2024, 05:09

Starting rampdown. Pressure stable at 4.5 e-06 Torr

Top temperature 1850 C on OMEGA

ramping down at -2A/min

679

Saturday, November 23, 2024, 11:11

ZrC 24E9T1 + std conditioning and sintering

Saturday, November 23, 2024, 11:08

No milling ZrC material sintering inside graphite cartridge

baseline standard discs included for comparison.

4 Ta foils wrapped around container

one spring at the back end to retain the graphite cartridge

One Ta cap with perforations at the front for T readings

initial heating at 2A/min to 50A, followed by heating at 1A/min to 90 A

Initial IGP1= 1.0e-6 Torr

OMEGA slope =0.990

Good and bad vacuum =5.0e-5 Torr and 5e-4 torr

Saturday, November 23, 2024, 11:20

autoramp start at 2A/min to 50A on tght

Saturday, November 23, 2024, 20:11

allowed pressure to drop to 3.3e-6 Torr after degassing.

Started ramp to 90A at 1A/min

Saturday, November 23, 2024, 23:46

started ramping at 1.5A/120s or 0.75A/min to 400A

Sunday, November 24, 2024, 07:55

Reached 1900 C at 410 A setpoint and 402 A on RD

Pressure did not increase after bumping up to 410 setpoint so will keep at this current until 11 am (four hours near 1900 C in total)

Sunday, November 24, 2024, 10:58

Final IGP1 at start of rampdown = 2.9e-6 Torr

Ramping down at -2A/min

Tuesday, May 15, 2012, 12:26

Re-condition the HP-SIS SiC target

Tuesday, May 15, 2012, 12:24

The HP-SIS SiC target was made on Nov 03, 2010. The target consists of 405 discs, 18.5cm in length. It was sintered in the Evaporator#1.

This target is going into Evap#2 for re-conditioning. It is currently being pumped down.

Friday, May 18, 2012, 12:19

Re-condition the HP-SIS SiC target

John Wong wrote:

Tuesday, May 15, 2012, 12:24

The HP-SIS SiC target was made on Nov 03, 2010. The target consists of 405 discs, 18.5cm in length. It was sintered in the Evaporator#1.

This target is going into Evap#2 for re-conditioning. It is currently being pumped down.

Friday, May 18, 2012, 12:19

The target is wrapped with only one heat shield.

Evaporator #2 Target Heater is now auto-ramping at 0.5 A/min, up to 820 A, with the maximum voltage limited at 2 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum). Tube Heater is auto-ramping at 0.5 A/min, up to 230 A, with the maximum voltage limited at 1 V. See attachments.

Attachment 1: autoramp1.png

Attachment 2: ievap2autoheat1.png

Friday, May 18, 2012, 13:17

Re-condition the HP-SIS SiC target

Nikita Bernier wrote:

John Wong wrote:

Tuesday, May 15, 2012, 12:24

The HP-SIS SiC target was made on Nov 03, 2010. The target consists of 405 discs, 18.5cm in length. It was sintered in the Evaporator#1.

This target is going into Evap#2 for re-conditioning. It is currently being pumped down.

Friday, May 18, 2012, 12:19

The target is wrapped with only one heat shield.

Evaporator #2 Target Heater is now auto-ramping at 0.5 A/min, up to 820 A, with the maximum voltage limited at 2 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum). Tube Heater is auto-ramping at 0.5 A/min, up to 230 A, with the maximum voltage limited at 1 V. See attachments.

Friday, May 18, 2012, 13:15

Increased TBHT voltage to 5V, and TGHT to 15V. Currently, TBHT =83A, 0.986V, TGHT= 144A, 1.65V, IGP1 = 5.2e-7 Torr, IGP2 = 4.3e-7 Torr.

Continue ramping up...

Tuesday, May 22, 2012, 12:02

TGHT and TBHT were ramped up to 830A/13.65V (local), and 235A/3.85V, respectively. The target was conditioned over the long weekend.

Tuesday, May 22, 2012, 12:15

Re-condition the HP-SIS SiC target

John Wong wrote:

Nikita Bernier wrote:

John Wong wrote:

Tuesday, May 15, 2012, 12:24

The HP-SIS SiC target was made on Nov 03, 2010. The target consists of 405 discs, 18.5cm in length. It was sintered in the Evaporator#1.

This target is going into Evap#2 for re-conditioning. It is currently being pumped down.

Friday, May 18, 2012, 12:19

The target is wrapped with only one heat shield.

Evaporator #2 Target Heater is now auto-ramping at 0.5 A/min, up to 820 A, with the maximum voltage limited at 2 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum). Tube Heater is auto-ramping at 0.5 A/min, up to 230 A, with the maximum voltage limited at 1 V. See attachments.

Friday, May 18, 2012, 13:15

Increased TBHT voltage to 5V, and TGHT to 15V. Currently, TBHT =83A, 0.986V, TGHT= 144A, 1.65V, IGP1 = 5.2e-7 Torr, IGP2 = 4.3e-7 Torr.

Continue ramping up...

Tuesday, May 22, 2012, 12:02

TGHT and TBHT were ramped up to 830A/13.65V (local), and 235A/3.85V, respectively. The target was conditioned over the long weekend.

Tuesday, May 22, 2012, 12:13

Initiating the cool-down process at 5 A/min.

See archive plots of the Target Heater (Attachment 1) and the Tube Heater (Attachment 2).

Attachment 1: TGHT-VAC1.JPG

Attachment 2: TBHT-VAC1.JPG

Tuesday, May 22, 2012, 15:26

Re-condition the HP-SIS SiC target

Nikita Bernier wrote:

John Wong wrote:

Nikita Bernier wrote:

John Wong wrote:

Tuesday, May 15, 2012, 12:24

The HP-SIS SiC target was made on Nov 03, 2010. The target consists of 405 discs, 18.5cm in length. It was sintered in the Evaporator#1.

This target is going into Evap#2 for re-conditioning. It is currently being pumped down.

Friday, May 18, 2012, 12:19

The target is wrapped with only one heat shield.

Evaporator #2 Target Heater is now auto-ramping at 0.5 A/min, up to 820 A, with the maximum voltage limited at 2 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum). Tube Heater is auto-ramping at 0.5 A/min, up to 230 A, with the maximum voltage limited at 1 V. See attachments.

Friday, May 18, 2012, 13:15

Increased TBHT voltage to 5V, and TGHT to 15V. Currently, TBHT =83A, 0.986V, TGHT= 144A, 1.65V, IGP1 = 5.2e-7 Torr, IGP2 = 4.3e-7 Torr.

Continue ramping up...

Tuesday, May 22, 2012, 12:02

TGHT and TBHT were ramped up to 830A/13.65V (local), and 235A/3.85V, respectively. The target was conditioned over the long weekend.

Tuesday, May 22, 2012, 12:13

Initiating the cool-down process at 5 A/min.

See archive plots of the Target Heater (Attachment 1) and the Tube Heater (Attachment 2).

Tuesday, May 22, 2012, 15:24

TGHT/TBHT were ramped down to 0A. The target has cooled for about 45 min. All pumps and chillers are off. The chamber has been vented.

Monday, June 11, 2012, 12:26

John Wong wrote:

Nikita Bernier wrote:

John Wong wrote:

Nikita Bernier wrote:

John Wong wrote:

Tuesday, May 15, 2012, 12:24

The HP-SIS SiC target was made on Nov 03, 2010. The target consists of 405 discs, 18.5cm in length. It was sintered in the Evaporator#1.

This target is going into Evap#2 for re-conditioning. It is currently being pumped down.

Friday, May 18, 2012, 12:19

The target is wrapped with only one heat shield.

Evaporator #2 Target Heater is now auto-ramping at 0.5 A/min, up to 820 A, with the maximum voltage limited at 2 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum). Tube Heater is auto-ramping at 0.5 A/min, up to 230 A, with the maximum voltage limited at 1 V. See attachments.

Friday, May 18, 2012, 13:15

Increased TBHT voltage to 5V, and TGHT to 15V. Currently, TBHT =83A, 0.986V, TGHT= 144A, 1.65V, IGP1 = 5.2e-7 Torr, IGP2 = 4.3e-7 Torr.

Continue ramping up...

Tuesday, May 22, 2012, 12:02

TGHT and TBHT were ramped up to 830A/13.65V (local), and 235A/3.85V, respectively. The target was conditioned over the long weekend.

Tuesday, May 22, 2012, 12:13

Initiating the cool-down process at 5 A/min.

See archive plots of the Target Heater (Attachment 1) and the Tube Heater (Attachment 2).

Tuesday, May 22, 2012, 15:24

TGHT/TBHT were ramped down to 0A. The target has cooled for about 45 min. All pumps and chillers are off. The chamber has been vented.

Monday, June 11, 2012, 12:20

After the re-conditioning, the target's end-caps vaporized. This is something happened before (see elog entries below):

https://elog.triumf.ca/TIS/Evaporator_1/20

https://elog.triumf.ca/TIS/Evaporator_1/22

The caps were removed and yellow crystals were observed. (see attachment#1).

The D-caps will be inserted in both ends and will be re-conditioned again to see if the yellow crystals can be removed at high temperature.

Attachment 1: Photo_2012-06-11_12_06_19_PM.jpg

Wednesday, August 21, 2013, 12:30

Conditioning Ta target

Wednesday, August 21, 2013, 12:28

Container is filled with 400 discs of Ta foils, and wrapped with 3 layers of Ta heat shields.

No caps are inserted during the conditioning.

Chamber is currently being pumped down.

Wednesday, August 21, 2013, 15:54

HS cooling water valves opened, no leaks were detected.

IG @ 2.9e-6 Torr.

Heating setting:

TGHT max = 820A,

TBHT max = 230A

ramping rate 2A/min.

Thursday, August 22, 2013, 12:45

TGHT/TBHT reached to 820A/230A, respectively.

So much out-gassing was observed at the max currents. (see attachment#1).

TGHT/TBHT are ramping down at 4A/min.

Chamber will be vented in air.

The target will will be inspected.

More info later...

Thursday, August 22, 2013, 16:44

Target was removed from the evaporator and inspected.

The container and the Ta materials look OK.

The outgassing could be from the Ta-heat shields; they look burnt and brittle.

Overall, the target is good.

Attachment 1: Ta#41_conditioning.PNG

117

Tuesday, February 11, 2014, 13:49

Sintering TaC coating container for TiC

Tuesday, February 11, 2014, 13:43

Target container is coated with TaC and wrapped with 3-Ta heat shields.

TGHT and TBHT will be ramped up to 820A and 300A, respectively.

Ramping rate set to 0.2A/min.

Good vac = 3e-5 Torr, Bad vac = 4e-5 Torr.

Chamber currently being pumped down...

Tuesday, February 11, 2014, 16:33

Chamber pumped down to 2e-6 Torr.

HS cooling water valves opened; no leaks detected.

Will step up in the a.m.

Wednesday, February 12, 2014, 11:41

IGP1 = 1.5e-7 Torr

TGHT max voltage = 17.05V, TBHT max voltage = 5V

Stepped TGHT and TBHT up to 35A

Waited 1hr15 before vacuum stabilized/ started to drop.

Initiating auto-ramping.

Thursday, February 13, 2014, 10:19

TBHT and TGHT have both reached 300A

IGP1 = 2.4e-7 Torr.

Increasing TGHT auto-ramp to 2.0A/min

Friday, February 14, 2014, 08:58

TGHT reached 820A yesterday afternoon. Measured internal temp this morning at 1300C.

Initiated TGHT auto-cooling at 2.0A/min and TBHT at 1.0A/min.

IGP1 = 3.2e-7 Torr.

Monday, February 17, 2014, 12:02

Cooled down friday. Vented this morning.

Container fully sintered, smooth run!

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ELOG V2.9.2-2455