Friday, June 20, 2014, 11:14

Made from batch's: oct 23/2013, oct 31/2013 and june 2012

Total number of foils: 515 discs

Total mass of materials [incl graphite foils]: 64.7224g

Total length packed: 17.8cm

Container is wrapped with 3x Ta-heat shields.

Currently being pumped down.

 Friday, June 20, 2014, 14:56

HS cooling water valves opened, no leaks detected.

IGP1 = 6.2e-6 Torr

TGHT max = 820A/ 17V

TBHT max = 300A/ 5V

Stepping up manually to 40A

 Friday, June 20, 2014, 16:04

IGP1 = 8e-6 Torr

Slowly stepped up to 35A manually.

Vacuum has stabilized.

Initiating auto-ramp at 0.1A/min

 Tuesday, June 17, 2014, 13:11

Target container is coated with TaC.

Container is wrapped with 3x Ta-heat shields.

Currently being pumped down.

For sintering process:

TGHT and TBHT will be ramped up to 820A and 300A respectively at 0.1A/min

 Tuesday, June 17, 2014, 14:22

HS water cooling valves opened, no leaks detected.

IGP1 @1.8e-6 Torr

TGHT max = 820A/ 17V

TBHT max = 300A/ 5V

Stepped up manually to 40A, waited ~20min, vacuum stable.

Initiating auto-ramp @ 1.0A/min

 Wednesday, June 18, 2014, 11:24

TGHT and TBHT reached their respective 820A and 300A last night.

Internal temp measured from side of EVAP2 with mikron = 1830C

IGP1 = 7.6e-7 Torr

Initiating auto-cool down process at 2.0A/min and 1.0A/min for TGHT and TBHT respectively

vented and opened this morning.

smooth run

John Wong wrote:

Laura Lambert wrote:  Friday, June 13, 2014, 14:53 Container is filled with 400 discs of Ta foils. No Ta foil heat shield. No caps inserted. Chamber pumped down this morning. HS cooling water valves opened, no leaks detected. IG @ 5.8e-6 Torr. TGHT max = 580A TBHT max = 230A Ramping rate 0.2A/min.  Monday, June 16, 2014, 11:46 TGHT and TBHT reached their respective 580A and 230A over the weekend. IGP1 currently at 3.2e-7 Torr. Internal temp [measured using mikron, right side of EVAP2, pointed at discs inside] = 1375C    Monday, June 16, 2014, 17:21 Further stepping up TGHT to 650A. Temperature measured on target discs = 1542C. Vac @ 3.28e-7 Torr. Initiate cooling down process; 2A/min for TGHT; 1A/min for TBHT

 Tuesday, June 17, 2014, 10:08

TGHT and TBHT reached 0A last night.

Turned off EVAP2

Venting chamber

Process Complete

Laura Lambert wrote:

Friday, June 13, 2014, 14:53 Container is filled with 400 discs of Ta foils. No Ta foil heat shield. No caps inserted. Chamber pumped down this morning. HS cooling water valves opened, no leaks detected. IG @ 5.8e-6 Torr. TGHT max = 580A TBHT max = 230A Ramping rate 0.2A/min.  Monday, June 16, 2014, 11:46 TGHT and TBHT reached their respective 580A and 230A over the weekend. IGP1 currently at 3.2e-7 Torr. Internal temp [measured using mikron, right side of EVAP2, pointed at discs inside] = 1375C

 Monday, June 16, 2014, 17:21

Further stepping up TGHT to 650A.

Temperature measured on target discs = 1542C. Vac @ 3.28e-7 Torr.

Initiate cooling down process; 2A/min for TGHT; 1A/min for TBHT

 Friday, June 13, 2014, 14:53

Container is filled with 400 discs of Ta foils; target length = 5.2cm;

Total mass ( Ta foils + wire) = 45.92g

No Ta foil heat shield.

No caps inserted.

Chamber pumped down this morning.

HS cooling water valves opened, no leaks detected.

IG @ 5.8e-6 Torr.

TGHT max = 580A

TBHT max = 230A

Ramping rate 0.2A/min.

 Monday, June 16, 2014, 11:46

TGHT and TBHT reached their respective 580A and 230A over the weekend.

IGP1 currently at 3.2e-7 Torr.

Internal temp [measured using mikron, right side of EVAP2, pointed at discs inside] = 1375C

 Target boat is now being cooled at 1 A/min from the starting point (616 A) down to 0 A. 

Manually changed current from 500 to 615 A, monitoring the temperature. Temperature went from 1657 C up to 1838 C. Pressure increased up to 7.2e-7 T. Samples should be left for about 4 hours (615 A started just before 13:00), then the goal is to ramp current back to zero.

Auto-ramp started. Max current = 500 A, voltage = 11.05 V. Current is being increased at 2 A/min. In the first 20 minutes, the pressure went up to about 10E-6 T, but has slowly decreased since then. Everything looks ok. The system will be left until Monday morning (June 9th). 

 Pressure down to 7.1e-7 Torr. Water valve to heat shield was opened; pressure remained stable. 

Current turned up to 40 A for now.  Will increase at 2 A/min up to 500 A over the weekend, then on Monday we will turn it up to 600 A and check the temperature. 

Purpose: Sinter one sample of each of TiC, VC, Cr3C2, ZrC, NbC, Mo2C, TaC, and WC on 5x10 mm tantalum foil to see if the samples are usable for SEM.

Samples were prepared using a solution of PEG (2.56 g), PVB (2.45 g), paraffin oil (1.12 g), MEK (15 mL), and EtOH (23 mL). Slurries made using 0.0013 mol of each carbide with ~230 uL of the solution. Applied via paintbrush onto 5x10 mm tantalum foil. 

The samples were placed directly on the target boat, no graphite layer between. We will check to see if the tantalum foil fuses to the boat or not.

Currently (May 29th), the chamber is still pumping down. John and I will continue the procedure tomorrow.

 Thursday, April 24, 2014, 17:25

The purpose of this experiment is to see if the carbon mesh is suitable for coating and sintering with uranium carbide.  For this test, the mesh is coated with WC slurry (previously prepared).

 The carbon mesh disks are bought from ERG aerospace corporation; the specifications of the mesh can be found on the link:  http://www.ergaerospace.com/RVC-properties.htm

Photos, EDX, SEM, RGA, etc... and be found on this link:  https://www.dropbox.com/sh/6ic932wu8yl9ad2/7rHFTiSzLY

Thursday, April 24, 2014, 17:51 

TEST #1:  Carbon Mesh, WC - RF sputtered - Then WC coated and sintered.

Target boat is loaded with a piece of WC coated carbon mesh (1/4 size cut out with the laser cutter).  Chamber is pumping down, currently at 3.2e-6 Torr.

HS water valve open - no leaks are detected. 

TGHT will be ramped up to 500A at 1.0A/min. 

RGA is running.  

Material temp will be measured... 

Monday, May 05, 2014, 17:35

Test #1:

TGHT was ramped up to 680A/13.77V.  Vacuum was at 1.62e-6 Torr (and coming down).  Carbon mesh was heated up to 1900C.   See the link to the dropbox above for more results.

Monday, May 05, 2014, 17:39

Test #2:  Carbon mesh (pure) coated with WC - then sintered. 

Chamber has been pumped down to 3.5 e-6 Torr. 

Sample will be heated up to 500A at 1.0A/min.  (Then step up to 680A while monitoring the vacuum).

RGA is running. 

 Wednesday, May 07, 2014, 14:36

Observations:

TGHT was at 650A/12.96V for 6 hrs and temperature was measured at 1930C. 

At some point after that (~20:40hr on May 6), the voltage went up to 14.77V (current remained constant at 650A), the temp went up 2110C - for only about 45 minute before the voltage dropped

back down to 12.53V and the temperature ~1800C.  Is the boat creaking more??? There were a few crack lines on the boat after Test#1. 

Today, TGHT was raised up to 725A and after an hour at that current the temperature was measured at 1930A. 

Now, at Wednesday, May 07, 2014, 14:47 - Lowered the current back to 685A/13.78V - temperature measured at 1900C. 

One thing to note... the vacuum is showing a lot of spikes but remains at around 7.5e-7 Torr. 

The RGA/Current/Voltage/Temp can be found here: https://www.dropbox.com/sh/1yaa7ez3nydl67m/8v4ZRT2slq

Thursday, May 29, 2014, 16:56 

The process is done. Chamber was vented...

Thursday, March 27, 2014, 17:38

TEST #1

WC slurry was prepared in non-aqueous environment (see lab book for procedures).  The solution was dripped on two Ta plates (3.1cm2) and let dry. 

Another Ta plate (3.1 cm2) was sprayed with TaC coating (for comparison).

All 3 coated Ta plates are put in a target boat and the boat is wrapped with 3 layers of Ta-heat shields.

HS water valves open; no leaks detected.

TGHT will be ramped up to 700A at 2.0A/min.

RGA is running and gases are being monitored.  See link:

https://www.dropbox.com/sh/625xl7zgepbybmu/GQJTlMo-5a

 Friday, March 28, 2014, 09:13

TGHT reached to 700A and samples were heated up over night. 

Cooling down Evap at 4A/min. 

 Tuesday, April 01, 2014, 17:37

Previous samples, namely WC#1, #2, TC#1 were fully sinterred.  See above link for photos.

TEST#2

Samples WC#3, #4, #5 are sprayed coated with WC solution.  Grains were pre-treated at 400RPM.

These 3 new samples are loaded in a boat, wrapped with 3 layers of Ta-heat shields.

Chamber is pumped down; no water leaks are detected.

TGHT will be ramped up to 700A at 2.0A/min

RGA is running.

Samples were analyzed with SEM/EDX.  The results are inconclusive because W and Ta peaks are very close together.  And WC coated layer may be even too thin to analyze. 

 Monday, April 14, 2014, 16:32

Test#3:  Coated WC on Endcap.  Total mass WC ~350mg.

Sintered at 500A/9.5V; measure temperature on actual sample surface ~1700C.  Sample heated >24hr.

Cooling down TGHT at 2A/min.  IG currently at 3.1e-7 Torr.

Laura Lambert wrote:

John Wong wrote:  Friday, March 21, 2014, 16:09 Target container is loaded with 360 Discs of TiC.   Target length = 11.7cm.   Total green mass = 40.945g  Container is wrapped with 3 Ta-heat shields, and have been pumped down in the chamber.  For the sintering process:  TGHT ramp up to 820A, and TGHT to 300A at 0.1A/min.  Friday, March 21, 2014, 16:15 TGHT/TBHT were manually stepped up to 40A.   Vac stabilizes at 1.7e-6 Torr.   Initiate auto-ramping...     Wednesday, March 26, 2014, 11:05 TBHT reached max desired current of 300A IGP1 = 1.4e-6 Torr TGHT = 543A Increasing TGHT auto-ramp to 2.0A/min

 Wednesday, March 26, 2014, 18:18

TGHT has reached to 820A\13.4V and target has been heated at that current for 4.5 hours.

Vac is coming down to 1.1e-6 Torr.

See link for RGA results: https://www.dropbox.com/sh/08dcxskux21aqap/1SF_dTJB4l

Cooling down in process at 2A/min for TGHT and 1A/min for TBHT.

 Thursday, March 27, 2014, 11:14

Target is cooled down.  TGHT/TBHT have reached to 0A. 

All pumps off; chamber will be vented soon. 

 Friday, March 28, 2014, 15:00

Target has been assembled.  Heat shield WO#39956-10

John Wong wrote:

Friday, March 21, 2014, 16:09 Target container is loaded with 360 Discs of TiC.   Target length = 11.7cm.   Total green mass = 40.945g  Container is wrapped with 3 Ta-heat shields, and have been pumped down in the chamber.  For the sintering process:  TGHT ramp up to 820A, and TGHT to 300A at 0.1A/min.  Friday, March 21, 2014, 16:15 TGHT/TBHT were manually stepped up to 40A.   Vac stabilizes at 1.7e-6 Torr.   Initiate auto-ramping...

 Wednesday, March 26, 2014, 11:05

TBHT reached max desired current of 300A

IGP1 = 1.4e-6 Torr

TGHT = 543A

Increasing TGHT auto-ramp to 2.0A/min

 Friday, March 21, 2014, 16:09

Target container is loaded with 360 Discs of TiC.  

Target length = 11.7cm.  

Total green mass = 40.945g 

Container is wrapped with 3 Ta-heat shields, and have been pumped down in the chamber. 

For the sintering process: 

TGHT ramp up to 820A, and TGHT to 300A at 0.1A/min. 

Friday, March 21, 2014, 16:15

TGHT/TBHT were manually stepped up to 40A.  

Vac stabilizes at 1.7e-6 Torr.  

Initiate auto-ramping... 

Monday, March 10, 2014, 11:45

The chiller tripped off on March 7, 2014.

• Water is not flowing into the chiller; paddle wheel shows no signal.
• Tried turning on the chiller locally; a few seconds later, it tripped off. 
• Motor is not responding;
• EPICS is not responding;
• All other water flow signals to TGHT, TBHT, HS, are responding;

Continue investigating...

 Monday, March 10, 2014, 14:36

The water line to the chiller is disconnected, and is re-connected straight to the TGHT power supply.  The paddle wheel is responding - the cooling line in the power supply is not blocked.

It is confirmed the chiller is broken. 

Will discuss if we can use the Evaporator without a chiller but with the DI water connected directly to the TGHT power supply....

Friday, March 14, 2014, 14:50  

The chiller was replaced with a "new" one.  

Checked the chiller interlock - It's working.  

The evaporator is now operational. 

 Friday, March 21, 2014, 16:19

Note about Auto-ramping program.

Previously the auto-rampiong program takes the Chiller as part of the reference to the interlocks.  Because the New chiller is not connected to EPICS; all the references to the Chiller on the auto-ramping program has been removed in order for it to function. 

Monday, March 10, 2014, 11:44

Rick replaced the backing pump hose from 1.5" to 2.0" for better flow.  And the HEPA filter was checked - it looks OK.

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

 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

There was no signal going from the coils to the PLC. After manipulating the connection points on the coil a signal could again be established. Frequency is ~ 40Hz.