Nikita Bernier wrote:

Nikita Bernier wrote: Nikita Bernier wrote:  Friday, August 10, 2012, 19:54   Target boat with TaC coating, inside covered with a 0.002 inches thick Ta foil, wrapped with a 0.002 inches thick Ta foil, contains a Ta foil with TaO coating. See John's Ipad for their recipes. Evaporator #2 is now auto-ramping overnight at 0.2 A/min, up to 830 A, with the maximum voltage limited at 14 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum).    Saturday, August 11, 2012, 19:15 Heating process was going smoothly up to 400 A. See Attachment 1. Around 420 A, vacuum went up again and the voltage increased more quickly. It seems like resistance is building up. After reaching 530 A, the current was tapped down to 420 A in an effort to save the Ta boat. See Attachment 2. The current will stay at 420 A for the weekend until John takes a look at this.    Monday, August 13, 2012, 13:46  TGHT was ramped down at 2 A/min and then tapped down to 0A. See Attachment 1.  The target boat will be cooled down for about an hour before turning off the chiller.

 Tuesday, August 14, 2012, 16:56

Summary:

The purpose of this experiment is to test the chemical and high temperature (1600C) resistance of a Ta foil (0.001" thick) coated with Ta2O5, so it can be used as the under-layer for the BeO sintering process.

The Ta2O5 (white powder, -325 mesh) was prepared in a non-aqueous solution and was sprayed on a piece of Ta foil. 

The coated foil was rolled up and inserted in a Ta-coated (previously sintered) target boat for heating.

The foil was heated up to 520A (~1200C) and evidently,Ta2O5 started to react with Ta foil, and the foil became brittle and cracked (see attachment#1).

In conclusion, Ta2O5 is not a good protection layer for Ta material - at least for our applications.

 Monday, September 24, 2012, 15:01

The target boat with TaC coating is being used again. The inside of the boat is covered with a 0.002 inches thick Ta foil with TaC coating, wrapped with a 0.002 inches thick Ta foil.

Chamber was pumped down to 6e-6 Torr before the Heat Shield cooling water valve was opened. A small vacuum bump was detected (See attachment #1). It is not clear if it was caused by a water leak or not.

After consulting with Peter, I will wait for the vacuum to be below e-07 Torr before turning the target heater on.

Nikita Bernier wrote:

Monday, September 24, 2012, 15:01 The target boat with TaC coating is being used again. The inside of the boat is covered with a 0.002 inches thick Ta foil with TaC coating, wrapped with a 0.002 inches thick Ta foil. Chamber was pumped down to 6e-6 Torr before the Heat Shield cooling water valve was opened. A small vacuum bump was detected (See attachment #1). It is not clear if it was caused by a water leak or not. After consulting with Peter, I will wait for the vacuum to be below e-07 Torr before turning the target heater on.

 Monday, September 24, 2012, 18:02

The vacuum was stable until 1e-06 Torr. The target heater was turned on and tapped up to 60 A (0.8 V). 

Evaporator #2 is now auto-ramping overnight at 0.2 A/min, up to 800-850 A, with the maximum voltage limited at 14 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum). 

 Tuesday, September 25, 2012, 15:11

Sintering process is going smoothly. See Attachment 1. The auto-ramping was increased to 1 A/min up to 800-850 A.

Tuesday, September 25, 2012, 16:11 

And the voltage limit was increased to 18 V ! See Attachment 2.

 Tuesday, September 25, 2012, 19:13

Around 806 A (readback), voltage increased more quickly than the current. It seems like resistance is building up. After reaching 836 A (readback), the current was tapped down to 800 A (readback)/ 816 A (setting) in an effort to save the Ta boat. See Attachment 3. The current will stay at 800 A for ~4 hours before ramping down.

Nikita Bernier wrote:

Nikita Bernier wrote:  Monday, September 24, 2012, 15:01 The target boat with TaC coating is being used again. The inside of the boat is covered with a 0.002 inches thick Ta foil with TaC coating, wrapped with a 0.002 inches thick Ta foil. Chamber was pumped down to 6e-6 Torr before the Heat Shield cooling water valve was opened. A small vacuum bump was detected (See attachment #1). It is not clear if it was caused by a water leak or not. After consulting with Peter, I will wait for the vacuum to be below e-07 Torr before turning the target heater on.        Monday, September 24, 2012, 18:02 The vacuum was stable until 1e-06 Torr. The target heater was turned on and tapped up to 60 A (0.8 V).  Evaporator #2 is now auto-ramping overnight at 0.2 A/min, up to 800-850 A, with the maximum voltage limited at 14 V, between 2.00e-05 (Good vacuum) and 3.00e-05 Torr (Bad vacuum).     Tuesday, September 25, 2012, 15:11 Sintering process is going smoothly. See Attachment 1. The auto-ramping was increased to 1 A/min up to 800-850 A.     Tuesday, September 25, 2012, 16:11  And the voltage limit was increased to 18 V ! See Attachment 2.    Tuesday, September 25, 2012, 19:13 Around 806 A (readback), voltage increased more quickly than the current. It seems like resistance is building up. After reaching 836 A (readback), the current was tapped down to 800 A (readback)/ 816 A (setting) in an effort to save the Ta boat. See Attachment 3. The current will stay at 800 A for ~4 hours before ramping down.

 Wednesday, September 26, 2012, 14:31

The current was tapped down twice as resistance was building up. After 4 hours at ~800 A, the TGHT was ramped down at 2 A/min. See Attachment 1. The target boat was cooled down for 4 hours before the chiller was turned off.

Also I had trouble measuring the temperature. I was unable to get a clear picture with the pyrometer. Therefore the exact temperature remains unknown, but from previous experiments, 800 A was about 1400°C.

The TaC coated Ta foil is very brittle. There is a lot of crystallisation on the Ta boat. See attachment 2. It is unlikely that the boat would survive many more sintering. Therefore it will be used for BeO pellets tests. 

When John gets back, I suggest we use a new boat coated with TaC, without additional layers. (See message #15 when this target boat was sintered up to 900A (local 893A/16.88V), Measured temp @ 1500°C)

 Wednesday, September 26, 2012, 15:07

The samples were made of BeO powder with 30% PVB which was treated at 400 RPM for 26 minutes. A ratio of 10:1 of mineral oil was added before another high speed treatment for 10 minutes. The powder was then pressed into pellets.

Three pellets were loaded on the target boat coated with TaC, with an extra layer of TaC coated Ta foil. See Attachment 1. The target boat is wrapped with a Ta foil that is 0.002 inches thick.

Target chamber was pumped down. The cooling water was turned on and no leak were observed.

TGHT was stepped up to 55A before the auto ramping was initiated at 0.5 A/min.  The vacuum limit parameter was set for good vac at <3.0 e-5 Torr and bad vac at >4.0 e0-5 Torr.  

Nikita Bernier wrote:

Wednesday, September 26, 2012, 15:07   The samples were made of BeO powder with 30% PVB which was treated at 400 RPM for 26 minutes. A ratio of 10:1 of mineral oil was added before another high speed treatment for 10 minutes. The powder was then pressed into pellets. Three pellets were loaded on the target boat coated with TaC, with an extra layer of TaC coated Ta foil. See Attachment 1. The target boat is wrapped with a Ta foil that is 0.002 inches thick. Target chamber was pumped down. The cooling water was turned on and no leak were observed. TGHT was stepped up to 55A before the auto ramping was initiated at 0.5 A/min.  The vacuum limit parameter was set for good vac at <3.0 e-5 Torr and bad vac at >4.0 e0-5 Torr.

 Friday, September 28, 2012, 12:50

Sintering was coming up smoothly. As expected, resistance started building up quickly at higher temperatures (above 600°C). See Attachment 1. The target heater tripped off twice this morning. I was able to ramp up the current after the first trip until it tripped again. After the second time, the voltage went crazy and I had to ramp down the current. Attachment 2 shows the whole process.

Evap2 will be vented out shortly and the pellets will be examined.

Friday, September 28, 2012, 15:52  

 The boat comes in two parts. One pellet is missing. The two remaining pellets are black and grey. Also they shrank a lot. See Attachment 3.

So once again, a new batch of BeO pellets will have to be prepared and sintered in order to determine the dimensions of the final die. Therefore the best approach is still loading the pellets on a target boat coated/sintered with TaC and wrapped with a Ta foil.

Friday, January 11, 2013, 10:59

The insulator that holds the terminals was broken when a target container was installed.  The insulator had seen so much heat shine from the Cu heat-shield gaps, see attachment.  Tightening the bolts on the target container might further put more force on the insulator and eventually broke it.

To prevent this to happen again.  The Cu-heat shield gaps have covered with Ta-foil to prevent any shine from the target  container onto the insulator.  Also, a torque wrench will be used to tighten the bolts on the terminals.  At this point, we don't know the max torque the insulator can tolerate.  Some measurements were done on the target resistant (ohm) as a function of torque (in pounds).  The best torque to tighten the terminal bolts is 150 lbs. 

John Wong wrote:

Friday, January 11, 2013, 10:59 The insulator that holds the terminals was broken when a target container was installed.  The insulator had seen so much heat shine from the Cu heat-shield gaps, see attachment.  Tightening the bolts on the target container might further put more force on the insulator and eventually broke it. To prevent this to happen again.  The Cu-heat shield gaps have covered with Ta-foil to prevent any shine from the target  container onto the insulator.  Also, a torque wrench will be used to tighten the bolts on the terminals.  At this point, we don't know the max torque the insulator can tolerate.  Some measurements were done on the target resistant (ohm) as a function of torque (in pounds).  The best torque to tighten the terminal bolts is 150 lbs.

The insulators were installed with torques as indicated in the attached PDF ITD0052. A torque test was performed on the broken insulator before installation. No damage was seen on torques of up to 60 in lbs for the 1/4-20 bolts, however for torques in excess of 50 in lbs the insulator material seems to "give".

 Tuesday, January 22, 2013, 12:38

This is to test the newly developed RFQ target to be commissioned this year.  The purpose of this test is to see how well the RFQ components can sustain the high temperature.  One thermocouple is connected inside the target and the other is connect outside of the Cu heat-shield.  RGA will be running to analyze the gasses. 

TGHT will be auto-ramped up at the rate of 5A/20min to max current at 1000A.  

More info later... 

Wednesday, February 06, 2013, 16:11 

Heat testing Test#1 complete.  Data acquisition in progress....  The test was successful. 

Re-heating Test#2 is in progress.  This time, with a new re-design target container (less black block mass).  Two thermocouples are connected:  One on the back block and the other inside the RFQ components.  

The TGHT current will go up to at least 580A and the gasses will be monitored with the RGA. Ramping rate:  0.5A/min.  Set final current at 400A for now. 

TBHT will remain off at this point until we can know the temperature when TGHT is up to 580A.  

 Thursday, February 07, 2013, 11:39

TGHT reached to 400A/6.30V. 

Back block temperature measured at 18.307mV = 1003 C. 

RFQ component temperature measured at  = 143 C.

TGHT will be ramped up to 580A. 

Continue to monitor...

 Saturday, February 09, 2013, 09:40

TGHT at 580A, TBHT at 271A (setpoint).  Seeing CO2 gassing out.  Ramped down TBHT to zero A and continue to monitor.

Tuesday, February 12, 2013, 16:39  

TGHT heated up to 580A and remained at that current over the long weekend.  

The thermocouple on the back block was reading wrong because the wires away from the tip were fused to the container at high current.  (see attachment #1) 

TBHT was ramped up to 300A and then lower to 280A; mass 32 (CH3OH), and 44 (CO2) were detected.  This is unusual at 580A = 1200C. 

Both TBHT and TGHT were ramped down to zero and the outgassing of these molecules continue to detect on the RGA. (see attachment #2).  Suspect of these gasses from the Cu heat-shield or the thermocouple SiO insulator.

For complete process on screenshots, see my dropbox.

Next:  Coat this container with TaC and use for the SiC target.

 Monday, February 18, 2013, 16:28

The RFQ target container is coated with TaC and ready to be sintered.  No Ta-heat shields are used.  This container will be used for the SiC#28-LPSIS-RFQ. 

Two thermocouples are welded on the container:  One on the end cap and the other on the back block (see attachment#1)

The target will be heated to at least  TGHT at 580A and TBHT at 300A; the vacuum and gasses will be monitored.  

The chamber is currently being pumped down...  

 Friday, February 22, 2013, 14:24

The gasses were analyzed with the RGA:

TGHT @ 520A, TBHT @ 300A:  Mass 28 (CO) reached to max current of ~5pA before the current started to decrease, (see attachment #2).  This could be the indication of the material(s) in the target container was "sort of" fully reduced. 

TGHT was further ramped up  to 600A and heated for a few hours.  The temperature on the end was measured at 1252C and the center block was at 1580C.  (see attachment #3).

The container was successfully sintered with TaC. 

Friday, February 22, 2013, 15:49

The LP-SIS RFQ target container was previously coated with TaC and sintered up to ~1500C (TGHT @ 600A, TBHT @ 300A). 

The container is loaded with 325 discs of SiC, a total of 10.9cm in length. 

For this process,

TGHT will be ramped up to 600A and at the same time TBHT will go up to 300A.  No Ta-heat shield is used. 

The ramping rate is set to 0.2A/min.

The chamber is currently being pumped down. 

 Friday, March 01, 2013, 15:57

The target was further heated up to 650A TGHT and 300A TBHT for 4 hours yesterday; then it was cooled down.  

Some reactions on the target end (where the D-cap inserted) was observed.  

Yellow crystals on the D-cap was formed, just as we have seen before.  

Overall, the target looks good!  

See attachment#2 for the target production. 

More about the gasses analyst from the RGA later...  

 A thermocouple feedthru was installed via 9 pin sub-D connector. It runs from the the conflat cross on the top of the evaporator to the upper 9 pin connector of the target mounting plate.

 Tuesday, May 07, 2013, 16:48

5 BeO pellets were made.  Each weights about 1.3 g (including org mass). 

A piece of Re foil (0.002" thick) is used as the under layer to protect the reaction between Be(g) and the Ta-boat.  (see Pictures)

Another layer of Ta-foil is used as the heat-shield to wrap around the Ta-boat.

The chamber was pumped down. 

TGHT will be ramped up to 600 A (~1360°C) at 0.2 A/min. The vacuum limit parameter was set for good vacuum at < 3.0e-5 Torr and bad vacuum at > 4.0e0-5 Torr.

The pressure, voltage and current will be closely monitored. 

If the Ta-boat survives, the TGHT will continue to ramp up to max 800 A (~1580°C).

Nikita Bernier wrote:

Tuesday, May 07, 2013, 16:48   5 BeO pellets were made.  Each weights about 1.3 g (including org mass).  A piece of Re foil (0.002" thick) is used as the under layer to protect the reaction between Be(g) and the Ta-boat.  (see Attachments) Another layer of Ta-foil is used as the heat-shield to wrap around the Ta-boat. The chamber was pumped down.  TGHT will be ramped up to 600 A (~1360°C) at 0.2 A/min. The vacuum limit parameter was set for good vacuum at < 3.0e-5 Torr and bad vacuum at > 4.0e0-5 Torr. The pressure, voltage and current will be closely monitored.  If the Ta-boat survives, the TGHT will continue to ramp up to max 800 A (~1580°C).

 Monday, May 13, 2013, 12:48

TGHT has been at 600 A for about 13 hours with stable very low vacuum (10^-7). See Attachment #1.

Temperature measurement has been lost on Saturday. Last measurement was was above 1350°C, at around 480 A.

TGHT was ramped down at 1 A/min.

The chamber will be vented later today. The pellets and the thermocouples will be inspected.

Nikita Bernier wrote:

Nikita Bernier wrote:  Tuesday, May 07, 2013, 16:48   5 BeO pellets were made.  Each weights about 1.3 g (including org mass).  A piece of Re foil (0.002" thick) is used as the under layer to protect the reaction between Be(g) and the Ta-boat.  (see Attachments) Another layer of Ta-foil is used as the heat-shield to wrap around the Ta-boat. The chamber was pumped down.  TGHT will be ramped up to 600 A (~1360°C) at 0.2 A/min. The vacuum limit parameter was set for good vacuum at < 3.0e-5 Torr and bad vacuum at > 4.0e0-5 Torr. The pressure, voltage and current will be closely monitored.  If the Ta-boat survives, the TGHT will continue to ramp up to max 800 A (~1580°C).    Monday, May 13, 2013, 12:48   TGHT has been at 600 A for about 13 hours with stable very low vacuum (10^-7). See Attachment #1. Temperature measurement has been lost on Saturday. Last measurement was was above 1350°C, at around 480 A. TGHT was ramped down at 1 A/min. The chamber will be vented later today. The pellets and the thermocouples will be inspected.

 Monday, May 13, 2013, 17:21

The following table shows the characteristics of the pellets after sintering at 600 A for 13 hours.

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

1    0.8904 4.875 1.364 13.058

2    0.8991 4.744 1.396 13.148

3    0.8846 4.579 1.482 12.884

4    0.9142 4.981 1.254 13.650

5    0.9022 4.978 1.250 13.586

Avg 0.8981 4.831 1.345 13.265

Friday, October 04, 2013, 15:37

A LP target container is coated with TaC.  The container is wrapped with 3 layers to heat shield.  

This container will be used for the graphite tube test.  

Chamber is being pumped down.

 The HS cooling water valves are open and no leaks are detected. 

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

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

The temperature will be monitored and measured. 

 Sunday, October 06, 2013, 19:55

Tuesday, October 22, 2013, 16:49

The target was heated up to 580A and the temperature inside the tube was measured to be ~1800C and the outside surface was ~1400C.

The target was cooled down.  Then the graphite tube was inserted.

There are two thermcouples inserted inside the tube on both ends.

Chamber has been pumped down to 4.33 e-7 Torr.  No leaks were detected.

Target will be heated up again to TGHT @ 580A / TBHT @ 230A at 0.2A/min.

The temperatures will be monitored.

T1 = left (floating)

T2 = right (toughing C-grv tube)

(wtf ionizer pointing into the page).

 Thursday, October 24, 2013, 16:35

TGHT/TBHT reached to 580A/230A. 

T1 = 1642C

T2 = Error?? Reading goes on/off intermittently, showing 900 - 1900C

Thursday, October 24, 2013, 16:45 

Ramping up TGHT to 680A to see if T1 can reach 1700C.

IG1 currently at 5.2e-7 Torr.

 Friday, October 25, 2013, 12:30

TGHT was ramped up to 632A (stopped due to voltage limiting). 

T1 was measured at 1960C.  Vac went up as it was heated up.  (see attachment #2)

Target was cooled down at 5A/min, now at 0A.

The chamber will be vented and the target will be inspected.

This run is complete.

 Tuesday, October 29, 2013, 15:50: Pumping down

Wednesday, October 30, 2013, 09:32: Turbo started

Wednesday, October 30, 2013, 14:50: The Cu-bars were heated to 600A and 300A for TGHT and TBHT respectively.

Wednesday, October 30, 2013, 15:17: PS off. Turbo off.

Results can be found on DocuShare and in the attached plot.

The source of the poor vacuum in the backing line seems to be related to a dirty filter. We will try to find a replacement filter next week.

The problem seem to have started September 17th, when backing preassure CG1A went from 40 mTorr to 130 mTorr. CG1B remained around 30 mTorr.

With the help of Anthony Ip from vacuum group, the problem was diagnosed to be the roughing pump itself. The pump was replaced and pumping improved. The chamber can now be evacuated and turbo ready to start in less than 10 minutes.

The filter is not stocked by vacuum group and could not be replaced.

Last week parts of the roughing line was cleaned by Rick. The PVC roughing line has been replaced with a SST bellows. The SST bellows is KF25 and should be replaced by a KF40 bellows in the long run.

See attached photo.

The Heat Shield has been taken to the Machine Shop for repair.

Friday, November 08, 2013

 The Heat Shield cooling line has been repaired and the lid re-installed in the evaporator. Photo attached.

Friday, November 08, 2013, 10:58 : Roughing Started

Friday, November 08, 2013, 11:05: Turbo started 

Friday, November 08, 2013, 11:15: Turbo at speed Vacuum at (IGP1) 5.7E-5 T