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.

Tuesday, May 14, 2013, 17:04

Target oven 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 1A/min.

Good Vac at 3.e-5 Torr, Bad Vac @ 4.0e-5 Torr.

Chamber is currently being pumped...

 Wednesday, May 15, 2013, 10:56

Chamber has pumped down to 4.5e-7 Torr. 

HS cooling water valves opened; no leaks were detected.

Stepping up TGHT/TBHT to 80A; monitoring vacuum.

 Wednesday, May 15, 2013, 11:26

Pressure is increasing.  TGHT setpoint @ 80A, readback @ 88.6A/0.603V, local @ 83A/0.80V.

 Wednesday, May 15, 2013, 12:08

TGHT/TBHT stepped up to 140A and tripped off at high limit vacuum.

Restarted p/s and set TBHT/TGHT at 100A

Initiated auto ramping...

 Friday, May 17, 2013, 11:39

TGHT and TBHT reached to 820A and 300A, respectively.  Target has been heating at the max currents for ~12hrs. 

Vacuum is coming down to 4.3e-7 Torr. 

The TaC coating sintering is completed.

Autocooling is initiated.  TGHT ramping rate @ 2A/min, and 1A/min for TBHT.

Wednesday, May 22, 2013, 10:43

Sintering complete.

Chamber will be vented

 Wednesday, May 06, 2015, 13:54

Two different samples of ZrC are wrapped in graphite sheet and loaded into the target boat.

Sample #1 = ZrC

Sample #2 = ZrC+C

Both samples are hand punched with a 18mm die.

The target boat is wrapped with 3x Ta heat shield.

Pumped down this morning.

HS water valves opened, no leaks detected.

IGP1 = 1.5e-6 Torr.

Tapping up manually to 35A...

 Waited ~50min for vacuum to stabilize.

IGP1 = 5.3e-6 Torr.

Initiating auto-ramp at 0.1A/min for the TGHT with a max setpoint of 275A/ 10V

Good vacuum = 3.00e-5 Torr. Bad vacuum = 4.00e-5 Torr.

Wednesday, May 06, 2015, 15:37  

Increasing ramping rate to 0.2A/min

 Thursday, May 07, 2015, 11:15

Stopping auto ramp.

TGHT = 273A.

Tapping up manually and recording data...

IGP1 = 6.6e-7 Torr.

 Thursday, May 07, 2015, 14:21

Increased max voltage to 14V

 Friday, May 08, 2015, 09:33

EVAP2 reached 2000C yesterday evening and remained at max setpoint overnight.

IGP1 = 3.8e-7 Torr

Initiated auto-cool this morning at 2.0A/min.

 Friday, May 08, 2015, 11:32

IGP1 = 2.1e-7 Torr

TGHT = 221A, 3.21V

OMEGA = 1100C

Increasing auto-cool to 5.0A/min.

 Friday, May 08, 2015, 15:53

Vented in air and opened up this afternoon.

See attachment for data results.

 Wednesday, May 13, 2015, 15:21

Three different samples of ZrC are loaded into a target boat.

Sample A: ZrC + NO graphite

Sample B: ZrC + graphite [1:0.5 molar ratio]

Sample C: ZrC + graphite [1:1 molar ratio]

Each sample consists of 20 discs, stacked together and wrapped in graphite sheet

The target boat is wrapped with 3 x Ta heat shield.

EVAP2 pumping down overnight...

 Thursday, May 14, 2015, 08:20

HS water valves opened up this a.m, no leaks detected.

IGP1 = 6.6e-7 Torr

Tapping up manually to 35A.

Good Vacuum = 3.00 e-5 Torr. Bad Vacuum = 4.00 e-5 Torr.

Thursday, May 14, 2015, 09:51

Tapped up manually to 30A.

After ~25min, vacuum gone up to IGP1 = 3.5e-5 Torr!

Backed off to 20A.

Waited ~10min. IGP1 = 1.75e-5 Torr.

Tapped back up to 25A.

Waited ~20min, IGP1 = 1.4e-5 Torr.

Tapped up to 30A.

Waited ~20min, IGP1 = 2.2e-5 Torr.

Tapped up to 35A

Waited ~50min, IGP1 = 2.5e-5 Torr.

Continuing manual tap-up...

 Thursday, May 14, 2015, 13:27

IGP1 = 9e-6 Torr

Tapped up to 40A.

Waited ~45min, IGP1 = 1e-5 Torr

Initiating auto-ramp at 0.1A/min for the TGHT with a max setpoint of 275A/ 8.0V

 Friday, May 15, 2015, 08:25

Max setpoints were changed to 400A/ 8.0V last night.

Reached 400A ~4.5hrs ago.

IGP1 = 4.9e-5 Torr

Initiating manual tap up and recording data.

 Friday, May 15, 2015, 15:50

Samples remained at ~2000C for ~4 hours [see attachment for data]

IGP1 = 7.8e-7 Torr.

Initiating auto-cool at 1.0A/min.

 Tuesday, May 19, 2015, 08:27

Vented in air and opened up this morning.

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.

 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. 

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). 

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.

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

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. 

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.

Monday, June 17, 2013, 16:57

Target is loaded with 510 SiC discs

Container was previously coated with TaC and sintered

SiC is wrapped with tantalum heat shield

Chamber is currently being pumped down

Laura Lambert wrote:

Monday, June 17, 2013, 16:57 Target is loaded with 510 SiC discs Container was previously coated with TaC and sintered SiC is wrapped with tantalum heat shield Chamber is currently being pumped down

 Tuesday, June 18, 2013, 16:16

HS water valves opened; no leaks were detected.

IG @ 8.9e-7 Torr.

Note: This target has a regular end cap inserted on one end, and the other with a D-cap. 

TGHT will be heated up to 820A and TBHT to 300A; ramping rate at 1A/min.

Stepped up TGHT/TBHT to 60A.  Vacuum slowly increasing... 

 Tuesday, June 18, 2013, 17:55

Stepped up TGHT/TBTH to 80A.  10 mins later, pressure went beyond the limit and tripped of the p/s.  F!

Allowed vacuum to come down below 8e-5 Torr.  Stepped down TGHT/TBHT to 50A.

Currently IG @ 4.8-5 Torr. 

Initiated auto-ramping:  setting: Good Vac = 3e-5 Torr, Bad Vac = 4.0e-5 Torr. 

 Thursday, June 20, 2013, 06:21

About 10 min ago, Evap tripped off due to high vacuum. 

Vacuum came back down below the trip limit and both TGHT/TBHT p/s were stepped down to 40A and turned back on.

Changed auto ramping rate to 05A/120min.  

The process continues...  (And I'm going back to sleep!) 

 Friday, June 21, 2013, 15:19

Vacuum is close to the trip limit. 

Change the ramping rate to 0.2A/120min. 

 Monday, June 24, 2013, 17:04

Organic burnt out is complete and vacuum has come down to ~9.0e-6 Torr.

Increase ramping rate to 0.2A/60min - The sintering process should take about another 2 days if everything goes smoothly. 

 Wednesday, June 26, 2013, 17:29

TGHT & TBHT have reached to 820A and 300A, respectively, for 4 hours.

Vacuum is at 9e-7 Torr. 

Cooling down is in progress, at a rate of 1.0A/min for TGHT and 0.5A/min for TBHT.

The target will be ready to come out by tomorrow.

 Thursday, June 27, 2013, 11:02

TGHT/TBHT reached to 0A.  Vacuum is leveled at 1.2e-7 Torr. 

Chamber will be vented in air soon.

 Thursday, March 29, 2012, 19:17

Target boat contains 3 BeO pellets :

Sample,   Thickness (mm),   Mass (g),  Density (g/cm3)

1    9.06,  1.9713,  1.413

2    9.11,  1.9900,  1.419

3  13.54,  1.9916,  0.956

Samples 1 and 2 are made of BeO powder with 30% PVB which was washed with excess acetone and let to dry on a greased baking sheet (with PAM Butter flavoured). The flakes were then milled for 26 minutes at 400 RPM. It resulted in a very fine grey powder, much denser than the BeO powder with 30% PVB (not washed with acetone) that was used for Sample 3.

The initial settings on Evaporator #2 were 100 A and 0.83 V until the vacuum increased.

Evaporator #2 is now auto-ramping overnight at 1 A/min, up to 700 A, with the maximum voltage limited at 14 V, between 5.00e-05 (Good vacuum) and 6.00e-05 Torr (Bad vacuum).

Nikita Bernier wrote:

Thursday, March 29, 2012, 19:17   Target boat contains 3 BeO pellets : Sample,   Thickness (mm),   Mass (g),  Density (g/cm3) 1    9.06,  1.9713,  1.413 2    9.11,  1.9900,  1.416 3  13.54,  1.9916,  0.956   Samples 1 and 2 are made of BeO powder with 30% PVB which was washed with excess acetone and let to dry on a greased baking sheet (with PAM Butter flavoured). The flakes were then milled for 26 minutes at 400 RPM. It resulted in a very fine grey powder, much denser than the BeO powder with 30% PVB (not washed with acetone) that was used for Sample 3. The initial settings on Evaporator #2 were 100 A and 0.83 V until the vacuum increased. Evaporator #2 is now auto-ramping overnight at 1 A/min, up to 700 A, with the maximum voltage limited at 14 V, between 5.00e-05 (Good vacuum) and 6.00e-05 Torr (Bad vacuum).

 Thursday, March 29, 2012, 22:31:

TGHT tripped off a few times over the past hours.  After changing the Good Vac to 2.00e-5 torr and Bad Vac to 3.00e-5 Torr, the target heater are regulating properly and the max pressure is well maintained below 6.5e-5 Torr [Trip point @ 8.0e-5 Torr].  (see attachment#1: parameter.jpg)

John Wong wrote:

Nikita Bernier wrote:  Thursday, March 29, 2012, 19:17   Target boat contains 3 BeO pellets : Sample,   Thickness (mm),   Mass (g),  Density (g/cm3) 1    9.06,  1.9713,  1.413 2    9.11,  1.9900,  1.416 3  13.54,  1.9916,  0.956   Samples 1 and 2 are made of BeO powder with 30% PVB which was washed with excess acetone and let to dry on a greased baking sheet (with PAM Butter flavoured). The flakes were then milled for 26 minutes at 400 RPM. It resulted in a very fine grey powder, much denser than the BeO powder with 30% PVB (not washed with acetone) that was used for Sample 3. The initial settings on Evaporator #2 were 100 A and 0.83 V until the vacuum increased. Evaporator #2 is now auto-ramping overnight at 1 A/min, up to 700 A, with the maximum voltage limited at 14 V, between 5.00e-05 (Good vacuum) and 6.00e-05 Torr (Bad vacuum).        Thursday, March 29, 2012, 22:31: TGHT tripped off a few times over the past hours.  After changing the Good Vac to 2.00e-5 torr and Bad Vac to 3.00e-5 Torr, the target heater are regulating properly and the max pressure is well maintained below 6.5e-5 Torr [Trip point @ 8.0e-5 Torr].  (see attachment#1: parameter.jpg)

Friday, March 30, 2012, 23:19  

Archive of the target current and vacuum over the past 24 hours.  (see attachment #1: archive_24hr)

Saturday, March 31, 2012, 12:12

The organic materials have been burnt off.  The target heater ramping up is no longer restricted by the vacuum limit. 

Archive of the target current and vacuum over the past 10 hours. (see attachment #2: TGHT@240A). 

 Saturday, March 31, 2012, 22:52

TGHT has stayed at 700A/12.37V, local @ 693A/12.43 = Temp @ 1780C.  

The striptool shows some out-gassing when TGHT reached to 700A. (see attachment #3 marked with black circle: TGHT@700A.jpg)

Increasing TGHT to 750A to see if there is any further reaction...  

Sunday, April 01, 2012, 10:24  

TGHT was ramped up to 750A, local 730A/13.90V.  The pressure has come down to low 10e-6 but not stable;  Some reaction may be ongoing therefore it's causing the vacuum excursion.  (See attachment #4: TGHT @ 750A).  Notice the current readback is not constant and it's slowly decreasing as the voltage readback is increasing.  There might be some resistant building up.

--> Initiating the cool-down process at 2A/min. 

Sunday, April 01, 2012, 19:30  

TGHT has ramped down to 0A, and the pressure is going down (currently at 7.e-8 Torr) with no excursion.  (see attachment #5: TGHT@0A). 

The chamber will be vented tomorrow, and the target materials will be inspected. 

John Wong wrote:

John Wong wrote: Nikita Bernier wrote:  Thursday, March 29, 2012, 19:17   Target boat contains 3 BeO pellets : Sample,   Thickness (mm),   Mass (g),  Density (g/cm3) 1    9.06,  1.9713,  1.413 2    9.11,  1.9900,  1.416 3  13.54,  1.9916,  0.956   Samples 1 and 2 are made of BeO powder with 30% PVB which was washed with excess acetone and let to dry on a greased baking sheet (with PAM Butter flavoured). The flakes were then milled for 26 minutes at 400 RPM. It resulted in a very fine grey powder, much denser than the BeO powder with 30% PVB (not washed with acetone) that was used for Sample 3. The initial settings on Evaporator #2 were 100 A and 0.83 V until the vacuum increased. Evaporator #2 is now auto-ramping overnight at 1 A/min, up to 700 A, with the maximum voltage limited at 14 V, between 5.00e-05 (Good vacuum) and 6.00e-05 Torr (Bad vacuum).        Thursday, March 29, 2012, 22:31: TGHT tripped off a few times over the past hours.  After changing the Good Vac to 2.00e-5 torr and Bad Vac to 3.00e-5 Torr, the target heater are regulating properly and the max pressure is well maintained below 6.5e-5 Torr [Trip point @ 8.0e-5 Torr].  (see attachment#1: parameter.jpg) Friday, March 30, 2012, 23:19   Archive of the target current and vacuum over the past 24 hours.  (see attachment #1: archive_24hr) Saturday, March 31, 2012, 12:12 The organic materials have been burnt off.  The target heater ramping up is no longer restricted by the vacuum limit.  Archive of the target current and vacuum over the past 10 hours. (see attachment #2: TGHT@240A).   Saturday, March 31, 2012, 22:52 TGHT has stayed at 700A/12.37V, local @ 693A/12.43 = Temp @ 1780C.   The striptool shows some out-gassing when TGHT reached to 700A. (see attachment #3 marked with black circle: TGHT@700A.jpg) Increasing TGHT to 750A to see if there is any further reaction...   Sunday, April 01, 2012, 10:24   TGHT was ramped up to 750A, local 730A/13.90V.  The pressure has come down to low 10e-6 but not stable;  Some reaction may be ongoing therefore it's causing the vacuum excursion.  (See attachment #4: TGHT @ 750A).  Notice the current readback is not constant and it's slowly decreasing as the voltage readback is increasing.  There might be some resistant building up. --> Initiating the cool-down process at 2A/min.  Sunday, April 01, 2012, 19:30   TGHT has ramped down to 0A, and the pressure is going down (currently at 7.e-8 Torr) with no excursion.  (see attachment #5: TGHT@0A).  The chamber will be vented tomorrow, and the target materials will be inspected.

 Monday, April 02, 2012, 16:11

After sintering , the 3 BeO pellets have shrunk and feel robust.

The first sample ate through the Ta target boat, shrank a lot and has white and black marks. We suspect the PAM (mostly made of canola oil) to be responsible for the boat damage and the weird sintering process (see John's posts).

Sample 2 is holding well.

Sample 3, which was not washed with acetone, shows some cracks.

Sample,   Thickness (mm),   Mass (g),  Density (g/cm3)

1    -----,  0.6254,  -----

2   5.81,  0.9229,  1.032

3   8.89,  1.1073,  0.809

The average mass before sintering was 1.9843 g. After sintering, 0.8852 g. Thus the average mass loss is 0.9757  (49.0%).

We are starting a new batch of treated powder washed with acetone without PAM.

 Friday, May 01, 2015, 10:27

Four different samples of ZrC are loaded into a target boat.

Sample A: ZrC + NO graphite / hand cut

Sample B: ZrC + NO graphite / laser cut

Sample C: ZrC + graphite / hand cut

Sample D: ZrC + graphite / laser cut

A picture showing the different samples is attached [one face-up/ one face-down sample of each side-by-side]

Each sample consists of ~20-25 discs, stacked together and wrapped in graphite sheet [see attachment for photo]

The target boat is wrapped with 3 x Ta heat shield.

EVAP1 pumped down overnight.

HS water valves were opened this morning, no leaks detected.

IGP1 = 5.5e-7 Torr.

Tapping up TGHT manually to 30A...

 Friday, May 01, 2015, 10:54

Tapped up manually to 30A.

Over the course of 20min the vacuum climbed to IGP1 = 1.0 e-5 Torr.

Backed off TGHT to 20A to allow vacuum to stabilize.

Waited ~10min.

Vacuum dropped to IGP1 = 6.5e-6 Torr.

Tapped back-up manually to 30A.

Waited ~45min.

Vacuum stable, IGP1 = 1.2e-5 Torr.

Initiating auto-ramp at 0.1A/min for the TGHT with a max setpoint of 300A / 5.00V.

Good Vacuum = 3.00e-5 Torr. Bad vacuum = 4.00e-5 Torr.

 Monday, May 04, 2015, 11:17

IGP1 = 2e-7 Torr.

TGHT = 274A, 4.75V

Ramp-up limited to 275A due to max voltage being set at 5.0V

Increased max voltage to 10V

Tapping up manually to 1800C and recording data.

Laura Lambert wrote:

Friday, May 01, 2015, 10:27 Four different samples of ZrC are loaded into a target boat. Sample A: ZrC + NO graphite / hand cut Sample B: ZrC + NO graphite / laser cut Sample C: ZrC + graphite / hand cut Sample D: ZrC + graphite / laser cut A picture showing the different samples is attached [one face-up/ one face-down sample of each side-by-side] Each sample consists of ~20-25 discs, stacked together and wrapped in graphite sheet [see attachment for photo] The target boat is wrapped with 3 x Ta heat shield. EVAP1 pumped down overnight. HS water valves were opened this morning, no leaks detected. IGP1 = 5.5e-7 Torr. Tapping up TGHT manually to 30A...  Friday, May 01, 2015, 10:54 Tapped up manually to 30A. Over the course of 20min the vacuum climbed to IGP1 = 1.0 e-5 Torr. Backed off TGHT to 20A to allow vacuum to stabilize. Waited ~10min. Vacuum dropped to IGP1 = 6.5e-6 Torr. Tapped back-up manually to 30A. Waited ~45min. Vacuum stable, IGP1 = 1.2e-5 Torr. Initiating auto-ramp at 0.1A/min for the TGHT with a max setpoint of 300A / 5.00V. Good Vacuum = 3.00e-5 Torr. Bad vacuum = 4.00e-5 Torr.  Monday, May 04, 2015, 11:17 IGP1 = 2e-7 Torr. TGHT = 274A, 4.75V Ramp-up limited to 275A due to max voltage being set at 5.0V Increased max voltage to 10V Tapping up manually to 1800C and recording data.

 Monday, May 04, 2015, 17:24

Samples have been heated at 1800C for >2 hours. 

Vaccum at 4.3e-7 Torr, TGHT 475A/9.1V. (Direct Vol = 5.3V).

Initiated cooling down process.  Chamber will be vented tomorrow.

 Tuesday, May 05, 2015, 10:22

TGHT reached to 0A. Chamber has already vented. 

Samples will be taken out for examination.

John Wong wrote:

Laura Lambert wrote:  Friday, May 01, 2015, 10:27 Four different samples of ZrC are loaded into a target boat. Sample A: ZrC + NO graphite / hand cut Sample B: ZrC + NO graphite / laser cut Sample C: ZrC + graphite / hand cut Sample D: ZrC + graphite / laser cut A picture showing the different samples is attached [one face-up/ one face-down sample of each side-by-side] Each sample consists of ~20-25 discs, stacked together and wrapped in graphite sheet [see attachment for photo] The target boat is wrapped with 3 x Ta heat shield. EVAP1 pumped down overnight. HS water valves were opened this morning, no leaks detected. IGP1 = 5.5e-7 Torr. Tapping up TGHT manually to 30A...  Friday, May 01, 2015, 10:54 Tapped up manually to 30A. Over the course of 20min the vacuum climbed to IGP1 = 1.0 e-5 Torr. Backed off TGHT to 20A to allow vacuum to stabilize. Waited ~10min. Vacuum dropped to IGP1 = 6.5e-6 Torr. Tapped back-up manually to 30A. Waited ~45min. Vacuum stable, IGP1 = 1.2e-5 Torr. Initiating auto-ramp at 0.1A/min for the TGHT with a max setpoint of 300A / 5.00V. Good Vacuum = 3.00e-5 Torr. Bad vacuum = 4.00e-5 Torr.  Monday, May 04, 2015, 11:17 IGP1 = 2e-7 Torr. TGHT = 274A, 4.75V Ramp-up limited to 275A due to max voltage being set at 5.0V Increased max voltage to 10V Tapping up manually to 1800C and recording data.    Monday, May 04, 2015, 17:24 Samples have been heated at 1800C for >2 hours.  Vaccum at 4.3e-7 Torr, TGHT 475A/9.1V. (Direct Vol = 5.3V). Initiated cooling down process.  Chamber will be vented tomorrow.  Tuesday, May 05, 2015, 10:22 TGHT reached to 0A. Chamber has already vented.  Samples will be taken out for examination.

 Friday, May 08, 2015, 15:55

see attachment for data results.