Manual_Annealing

For temperatue regulation by PID controller see here.

Annealing

Note that these values have been recorded for a sample holder at room temperature (no LN2 cooling).
Please read the section Cooling for information on Annealing with the LN2 and LHe cooled sample holder and for the
COLD FINGER HEATER (TOP CONNECTOR of the manipulator)

PBN SAMPLE HOLDER HEATER New (May 2015)

Curret (A)	Voltage (V)	Temperature(°C), 4.5 min from RT	Temperature(°C), 16 min from RT
0.3	5.6	100
0.4	7.2	150	233
0.5	9.3	200
0.7	13.3	300	427
0.9	15.1	400
1.2	18.2	500

PBN All Metal (Sept2017)

Curret (A)	Voltage (V)	Temperature(°C)
0.1	2.9	35 (after 40')
0.3	6.1	70
0.5	9.1	120 (after ~30')
1	14.3	300

1.5

19.4

500

E BEAM SAMPLE HOLDERS (2018)

ATTENZIONE:

• !! Rimuovere la termocoppia di PID prima di applicare HV nella camera Main.
• !!! Annealing nella camera Prep: Uno dei pin del filamento deve essere messo a terra!

 

SMALL e beam (3.0cm)
22/10/2018
Thermocouple calibration
2.0Ax3.1V 493K (after 17min, p=1x10-7mbar)
2.2Ax3.8V 539K after 12min
2.3Ax4.1V 559K after 15 min
2.4Ax4.4V 572K after 14min
 
(from RT after 2min 530K increasing fast, p=5x10-6mbar with 3.0A)
 
10/12/2018
Pyrometer (reading is lower by 50°C with respect to the therm); Air gas flow
3.2Ax6.2V 370C on the Mo plate (real T~420°C) (no HV)
 
LARGE e beam
24/9/2018
No LN2 cooling. Thermoucouple reading (CHECK AGAIN THESE VALUES)
2.5Ax4.5V 407K=134°C
3.2Ax6.6V 491K=218°C (after11min)
3.9Ax9.0V 587K=314°C

LN2 COOLING ON; T=112K
2.7Ax5.5V 300K in 10 min; 325K in 15min (10+5)
3.3Ax6.7V 434K in 10min
3.7Ax8.1V 523K (250°C) 
4.0Ax9.3V 600K

HV ON 750V (no cooling)
3.5Ax7.4V 14mA 430°C
3.7Ax8.0V 22mA 500°C 2x10-7mbar
3.8Ax8.2V 25mA 560°C
3.9Ax8.4V 30mA 615°C
3.9x8.5V 32.6mA 638°C
WITH 3x10-7 mbar O2: 27.8 mA 630°C
45.5 mA T=730*C

Ebeamcalibration 16/11/2017 (small or large?)
No LN2 cooling. Thermoucouple reading. HV off
0.9Vx1A (elind set 0.8): T=60°C after 35 minutes
1.1Vx1.1A (elind set 1): T=73°C after 35 min (starting from 60*C)
1.4x1.3 (elind set 1.3): T=98.1 °C after 35 min

*For the annealing in the presence of LN2 see the section Cooling

PBN sample carriers

"Old" PBN sample holder

- Manipulator cooled by air flow

Note: The temperatuers are about 100°C higher when annealed in preparation chamber.

Curret (A)	Voltage (V)	Temperature (°C)
0.4	6	100°C
0.6	8	150°C
0.7-0.8	10	200°C
1.1	13.6	300°C
1.2	15	327°C
1.6	18.1	400°C
2.1	22.4	500°C

"New" PBN sample holder

- Manipulator cooled by air flow

Curret (A)	Voltage (V)	Temperature (°C)
0.5	7.5	100°C
0.8	11.3	200°C
1.3	15.3	300°C
1.7	18.7	400°C
2.1	22.2	500°C

 

"All metal" PBN sample holder

- Manipulator cooled by air flow

Curret (A)	Voltage (V)	Temperature (°C)
1	12.2	270°C
1.2	14.5	327°C
1.8	19.4	470°C
2.0	21.4	504°C

"Elena" PBN sample holder

- Manipulator cooled by air flow

Curret (A)	Voltage (V)	Temperature (°C)
1.0-1.1	9.2	256°C
1.8-1.9	14.4	420°C

 

Large E-beam sample carrier

Filament radiation annealing, manipulator cooled by air flow

Technical Note: Thoriated W filament, 0.2mm, 13-14 threads

Current (A)	Voltage (V)	Power (W)	Temperature(°C)
1.4	1.8	2.5	50°C
1.8	2.5	4.5	100°C
2.5	4.4	11	210°C
2.9	5.4	15.7	265°C
3.0	5.7	17.1	283°C
3.2	6.3	20.2	300°C
3.5	7.4	25.9	350°C
3.6	7.5	27	361°C
3.8	8.3	31.5	388°C
3.9	8.6	33.5	402°C

Estimated sample temperature vs heater current

HV E-beam annealing, manipulator cooled by air flow

Warning 1: HV on thermocouple pins!
Warning 2: Operation allowed ontly to the staff.
Warning 3: Filament must be grounded.
Warning 4: Never use PID box to monitor the temperature.

Note: Following data (collected in November 2018) are only approximate, they depend on the filament shape and distance from the Mo plate; the pressure and nature of the used gas.

HV = 750 V, Prep chamber

Filament (A)	Emission (mA)	Pyrometer (°C) Emis.=16	Temperature (°C) +- 30°C	Comment
2.3	30	420	506
2.4	35	550	623
3.8	40-42.3	570-600	638-665	pO2=5x10-7 mbar
3.8	51.2	660	736
3.8	57.4	690	760	pN3B3H6=5x10-7mbar

Small E-beam sample carrier

Filament radiation annealing, manipulator cooled by air flow

Technical Note: Thoriated W filament, 0.2mm, 13-14 threads

Current (A)	Voltage (V)	Power (W)	Temperature(°C)	Comment
1.4	1.8	2.5	102	After >10 minutes
3.2	6.2	20	430 +- 30 °C

HV E-beam annealing, manipulator cooled by air flow

Warning 1: HV on thermocouple pins!
Warning 2: Operation allowed ontly to the staff.
Warning 3: Filament must be grounded.
Warning 4: Never use PID box to monitor the temperature.

Note: December 2018, HV switched on when Filament current is below 1.5A. Pyrometer aimed on the Mo plate close to the crystal sample.

HV = 750V, Prep. Chamber

Filament (A)	Emission (mA)	Pyrometer (°C) Emis.=16	Temperature (°C) +- 30°C	Comment
3.7	6	440°C	500°C	pO2=2x10-6 mbar
3.8	13.2	548°C	600°C	pO2=2x10-6 mbar

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