MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
STANDARD OPERATING PROCEDURE
NUMBER: SOP L 100
Use of Advanced Spectroscopy Laboratory
ISSUE:
2
Prepared by: Paolo Olivero
Signature:
Date: 05 / 01 / 2006
Review Frequency
Annually from date of issue/review.
1.
PURPOSE
This Standard Operating Procedure (SOP) describes the procedures to use
the equipment in the Advanced Spectroscopy Laboratory in the Centre of
Excellence Cleanroom.
2.
SCOPE
This SOP refers to the Centre of Excellence for Quantum Computer
Technology Cleanroom located in the basement of the School of Physics at The
University of Melbourne.
3.
RESPONSIBILITIES
It is the responsibility of the Area Responsible Personnel (ARP) of the
Advanced Spectroscopy Laboratory to ensure that these procedures are
periodically updated and followed by all the users of the laboratory.
4.
REFERENCES
Forms:
SOPs:
OI’s:
Programs:
Other:
5.
Lab permit - ASL
N/A
Wire 1.3 Raman software manual
LinkamTM stage reference manual
Facilities and Infrastructure Program
N/A
DEFINITIONS
NIL
6.
SAFETY INSTRUCTIONS
Follow standard laboratory safety protocols at all times.
7.
EQUIPMENT
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
RenishawTM Raman Spectrometer
Optical table: filter and alignment components
514 Ar+ laser
325 Cd laser
244 Ar+ laser
LinkamTM cooling stage
9.
LASER STARTUP AND SHUTDOWN PROCEDURES
10.
9.1.
Spectra Physics 2016-5 Argon Ion Laser (488, 514 nm)

page 3
9.2.
Kimmon 325 Cd Laser (325 nm)

page 5
9.3.
Coherent INNOVA (FreD) Ar Ion Laser (244nm)

page 6
9.4.
Coherent INNOVA (FreD) Ar Ion Laser (514nm)

page 8
OPEARATIONS WITH RENISHAW SPECTROMETER

page 10
IMPORTANT SAFETY RULES
!
!
 From outside the laboratory, you can check if there are lasers on inside the
lab from the red light “LASER ON” indicator
 If the “LASER ON” indicator is flashing, before entering you must knock at
the lab door or call the laboratory phone and wait for the lab users to open
you the door
 For the safety of all personnel, always turn on the “LASER ON” indicator
whenever using any laser
 Whenever the lasers are on, every user must wear:
 Laser eye safety goggles
 Gloves
 Users cannot wear jewellery (e.g. rings or watches) that may reflect the
beam, particularly during alignment. In addition, users should be aware of
any clothing (e.g. ties) or hair that could fall into and scatter or ignite in the
beam
 Entering in the lab without overriding the Laser Interlock will close all laser
shutters, independently from the experiments being performed in the
laboratory
 Area Responsible Personnel: Paolo Olivero (ext: 44012)
SOP L 100
05/01/2006
 Laser Protection Officer: Paul Spizzirri (ext: 44012)
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
9.1. Spectra Physics 2016-5 Argon Ion Laser
(1.5W maximum @  = 488 and 514.5 nm)
Startup and Shutdown procedures
Class IV lasers are used in the UV Raman Laboratory.
This facility may be operated only by suitably trained and
authorized personnel.
Operation of the Spectra Physics 2016-5 Argon Ion Laser
Startup Procedure:
1.
2.
3.
4.
5.
6.
7.
8.
Switch on (Power) the Interlock Control Unit located inside the lab near
the door. The Laser On indicators will light up.
Switch on the interlock actuators power supply located under the
optical table.
Check that the external loop water temperature is within specs*.
Thermometer alarm set at 24 ºC
Open both taps of external loop water.
Turn on the cooling water chiller:
at the floor mains socket with the orange extension lead plugged in.
Turn on the “Laser Air Purge” pump located under the optical table.
Insure that the Argon Ion laser power supply is plugged into the mains
socket and turn the switch on.
Set the Remote Control switches to the following values:
Range = 2W
Head = A
Meter = Watts Current = Minimum
Mode = Current
9.
10.
11.
12.
13.
14.
15.
16.
Control = Remote
Power = Minimum
Insert key into the Remote Control unit and switch ON.
Once started, slowly increase the current to maximum.
Adjust the end mirror mount for maximum power. Use in sequence
vertical and horizontal adjustments at the back of the laser.
Record the maximum power in the Laboratory Log Book.
Leave the Laser to warm up for about 15 minutes with these settings.
Insure that the cooling water temperature remains within specs*.
After the warm up period, set the power control to 50% of full scale and
switch the Mode from Current to Power control.
Place the Laser Power Meter Head into the beam path, after the first
mirror in front of laser.
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
AT THIS STAGE YOU SHOULD BE WEARING SAFETY GOGGLES!
17.
18.
Enable (Reset) interlock shutter at Interlock Control Unit.
Open the shutter and adjust the position of the Laser Power Meter
head for maximum readout.
GLOVES ARE MANDATORY ! AVOID INTERSECTING THE BEAM
WITH YOUR HANDS!
19.
Set the output power as required by the experiment and record in the
log book:
DO NOT EXCEED THE MAXIMUM OF 20 mW AS SPECIFIED FOR
THE RENISHAM RAMAN SPECTROMETER INPUT
Shutdown Procedure:
1.
2.
3.
4.
5.
6.
7.
8.
9.
Close any instrument Laser shutters.
Turn the Laser power down to 0 on the Remote Control.
Turn the Laser Current down to 0 on the Remote control.
Switch off the Remote Control using the key.
Switch off the Laser Power Supply at the Mains Isolator switch.
Switch off the Interlock Control Unit and any additional Laser On
indicators.
Let the Laser cool down for ~10 minutes.
Switch off the Laser Air Purge pump and the Water Chiller.
Close the external loop water taps.
_________________________________________________________
*External loop temperature: <20ºC (normal operation)
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
9.2. Kimmon 325 Cd Laser
( 15mW @ 325 nm)
Startup and Shutdown procedures
Class IV lasers are used in the UV Raman Laboratory.
This facility may be operated only by suitably trained and
authorized personnel.
Operation of the Kimmon 325 Cd Laser
Startup Procedure:
1.
2.
3.
4.
Switch on (Power) the Interlock Control Unit located inside the lab near
the door. The Laser On indicators will light up.
Switch on the interlock actuators power supply located under the
optical table.
Switch on the Kimmon Power Supply.
Leave the Laser to warm up for about 30 minutes.
AT THIS STAGE YOU SHOULD BE WEARING SAFETY GOGGLES !
GLOVES ARE MANDATORY ! AVOID INTERSECTING THE BEAM
WITH YOUR HANDS!
5.
6.
7.
Enable (Reset) interlock shutter at Interlock Control Unit.
Open the shutter and adjust the position of the Laser Power Meter
head for maximum readout.
Record the power in the Laboratory Log Book.
Shutdown Procedure:
1.
2.
3.
Close any instrument Laser shutters.
Switch off the Laser Power Supply.
Switch off the Interlock Control Unit and any additional Laser On
indicators.
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
9.3. Coherent INNOVA (FreD) Ar Ion Laser
(200mW @ 244 nm)
Startup and Shutdown procedures
Class IV lasers are used in the UV Raman Laboratory.
This facility may be operated only by suitably trained and
authorized personnel.
Operation in UV mode @ 244 nm
Startup Procedure:
1.
2.
3.
4.
5.
Switch on (Power) the Interlock Control Unit located inside the lab near
the door. The Laser On indicators will light up.
Switch on the interlock actuators power supply located under the
optical table.
Check that the external loop water temperature is within specs*.
Thermometer alarm set at 24 ºC
Open both taps of external loop water.
Turn on the cooling water chiller:
at the floor mains socket with the orange extension lead plugged in.
For trained users ONLY:
6.
Establish N2 flow of 0.4 to 0.5 scfs by setting the line pressure to ~ 0.5
Bar, or first division on 0-15 Bar gauge at rear of laser. Check high
purity N2 cylinders in service bay and switch over if empty (note: 25
days @ 0.4 scfs per cylinder).
7.
Install frequency doubling BBO crystal in housing according to
instructions in INNOVA manual.
8.
Insure that the INNOVA laser power supply is plugged into the mains
socket and turn the key-switch to stand-by.
Turn on the unit at the remote control box and wait for warm-up
Set the mode to current. After delay (loud noise!) slowly increase
current to ~38A.
9.
AT THIS STAGE YOU SHOULD BE WEARING SAFETY GOGGLES !
10.
11.
Open the intra-cavity shutter and set aperture to 10-12.
Adjust the end mirror mount and the frequency doubling crystal stage
for maximum power reading on remote. Use in sequence vertical and
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
12.
13.
14.
horizontal fine adjustments at the front of the laser. Make only small
adjustments at a time.
Slowly increase/decrease the current to reach the required beam
power.
Leave the Laser to warm up for about 15 minutes with these settings.
Insure that the cooling water temperature remains within specs*.
GLOVES ARE MANDATORY! AVOID INTERSECTING THE BEAM
WITH YOUR HANDS!
15.
16.
17.
Enable (Reset) interlock shutter at Interlock Control Unit.
Open the shutter and adjust the position of the Laser Power Meter
head for maximum readout.
Record the power in the Laboratory Log Book.
DO NOT EXCEED THE MAXIMUM OF 20 mW AS SPECIFIED FOR
THE RENISHAM RAMAN SPECTROMETER INPUT
Shutdown Procedure:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
Close any instrument Laser shutters.
Turn the Laser power down to 0 on the Remote Control.
Turn off the current on the Remote control.
If the BBO crystal is left in place, switch the Laser Power Supply to
stand-by mode and keep the N2 flowing.
Switch off the Interlock Control Unit and any additional Laser On
indicators.
Let the Laser cool down for ~10 minutes.
Switch off the Water Chiller.
Close the external loop water taps.
Store BBO crystal in desiccators if 244 not used for extended periods.
Turn off N2 supply and switch off the power supply.
_________________________________________________________
*External loop temperature: <20ºC (normal operation)
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
9.4. Coherent INNOVA (FreD) Ar Ion Laser
(1.5W maximum @  = 488 and 514.5 nm)
Startup and Shutdown procedures
Class IV lasers are used in the UV Raman Laboratory.
This facility may be operated only by suitably trained and
authorized personnel.
Operation in Visible mode @ 514 nm
Startup Procedure:
1.
2.
3.
4.
5.
6.
7.
Switch on (Power) the Interlock Control Unit located inside the lab near
the door. The Laser On indicators will light up.
Switch on the interlock actuators power supply located under the
optical table.
Check that the external loop water temperature is within specs*.
Thermometer alarm set at 24 ºC
Open both taps of external loop water.
Turn on the cooling water chiller:
at the floor mains socket with the orange extension lead plugged in.
Insure that the INNOVA laser power supply is plugged into the mains
socket and turn the key-switch to stand-by.
Turn on the unit at the remote control box and wait for warm-up
Set the mode to current. After delay (loud noise!) slowly increase
current to ~15A.
AT THIS STAGE YOU SHOULD BE WEARING SAFETY GOGGLES !
8.
9.
11.
12.
13.
Open the intra-cavity shutter and set aperture to 10-12.
Adjust the end mirror mount for maximum power reading on remote.
The output should be ~ 100 mW.
Use in sequence vertical and horizontal fine adjustments at the front of
the laser. Make only small adjustments at a time.
Slowly increase/decrease the current to reach the required beam
power.
Leave the Laser to warm up for about 15 minutes with these settings.
Insure that the cooling water temperature remains within specs*.
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
GLOVES ARE MANDATORY! AVOID INTERSECTING THE BEAM
WITH YOUR HANDS!
15.
16.
17.
Enable (Reset) interlock shutter at Interlock Control Unit.
Open the shutter and adjust the position of the Laser Power Meter
head for maximum readout.
Record the power in the Laboratory Log Book.
DO NOT EXCEED THE MAXIMUM OF 20 mW AS SPECIFIED FOR
THE RENISHAM RAMAN SPECTROMETER INPUT
Shutdown Procedure:
11.
12.
13.
14.
15.
16.
17.
18.
Close any instrument Laser shutters.
Turn the Laser power down to 0 on the Remote Control.
Turn off the current on the Remote control.
Switch off the Laser Power Supply and the Mains Isolator switch.
Switch off the Interlock Control Unit and any additional Laser On
indicators.
Let the Laser cool down for ~10 minutes.
Switch off the Water Chiller.
Close the external loop water taps.
_________________________________________________________
*External loop temperature: <20ºC (normal operation)
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
9.4. Measurements with Renishaw
Raman Spectrometer
1. Startup procedures
1.1. Follow the laser startup procedures, if appropriately trained (see sections 9.1,
1.2. 9.2, 9.3, 9.4)
1.3. Switch on the “LASER ON” red indicator
1.4. Switch on the interlock (box at the wall): POWER, ENABLE (key), RESET
1.5. With the power meter, check that the laser light intensity at the input of the
Renishaw spectrometer is below 25 mW (use gloves!)
1.6. Turn on the microscope
1.7. Turn on the Renishaw spectrometer
1.8. Turn on the “ProScan II” module
1.9. Start the “Renishaw – WiRE” software (icon accessible from the desktop of the
PC)
1.9.1.
Click “OK” on the start-up window
1.9.2.
Select “Check motors”, unless you are using the software only for data
analysis (“Skip check”)
1.9.3.
Wait until the checking procedures are completed by the software
2. Raman / PL measurements – basic operations
2.1. Microscope:
When operating in standard microscopy mode, the rotating selectors must
be in the “2 -1” position:
2 – eyepiece
1 – white light
When acquiring a spectrum, the rotating selectors must be in the “1 - 2”
position:
1 – laser
2 – measure
The sample is brought into focus by adjusting the z position with the knob on
the right side (coarse and fine adjust).
The light intensity can be adjusted with the knob on the left side (only
reflected light images can be acquired).
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
2.2. Check before acquiring a spectrum:
2.2.1.
Laser shutter: OPEN
2.2.2.
Interlock: ON and ENABLED (RESET if tripped)
2.2.3.
Module “S - 8RMN - 1384” (shutter control on the optical table, to the
right with respect to the Renishaw box): “Auto” position
2.2.4.
Microscope in the “1-2” position
2.3. Setting the acquisition parameters:
The “Experiment setup” window can be accessed from the main menu
(Collect  Experimental Setup) or from button “A” (see Fig. 1). The
acquisition parameters (static / dynamic spectrum, center wavelength /
range, units, acquisition time, accumulation, objective, laser type, grating,
power %) can be set on such window.
B C A
D
Fig. 1: screen of “Renishaw – WiRE” software.
2.4. Starting the spectrum acquisition:
The acquisition of a single spectrum is started by selecting “Collect  Get”
from the main menu, or by clicking button “B” (see Fig. 1).
The continuous acquisition of subsequent spectra is started by selecting
“Collect  Cycle” from the main menu, or by clicking button “C” (see Fig. 2).
In both case, the acquisition can be aborted by clicking a second time on
button “B” and clicking on “Abort”; the “Abort” button is already available after
the first click of button “C”, in the case of continuous acquisition.
2.5. Controlling the sample position:
The sample position can be visualized on the PC screen after setting the
microscope in the “2 -1” position, and clicking on button “D” (see Fig. 1) or
selecting from the main menu “Collect  Applications  Display live video”.
Images of the sample can be saved in *.bmp format with crosshairs and
scale.
The sample can be moved automatically by setting the coordinates on the
“Live Video” screen, or by using the joystick which is interfaced to the
“ProScan II” module.
SOP L 100
05/01/2006
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
3. Test measurements
3.1. Before conducting any kind of experiment, every user must collect 1 reference
spectrum from a test sample in standard conditions, in order to check the
operational status of the apparatus
3.2. Test sample: diamond sample on glass slide
3.3. Standard measurement conditions:
3.3.1.
3.3.2.
3.3.3.
3.3.4.
3.3.5.
3.3.6.
Laser power at the spectrometer input:
Microscope objective:
Confocal aperture:
CCD aperture:
Spectrum:
Acquisition time:
5 mW
×50 mag
5
10 pixels
static, centered at 1332 cm-1
10 sec
3.4. Logbook filling: the user must save the test spectrum in his working directory and
record the peak position (expected to be 1332 cm-1) and intensity on the
Logbook, together with name user, date and all requested information.
3.5. If any of the features in the test spectrum are unusual (high background signal,
low signal intensity, wrong peak position) the user must immediately report to
the ARP or end immediately the experiment. Experienced users may
re-configure the laser, the elements on the optical table or the calibration of the
Renishaw spectrometer, in accord with their training.
4. Raman / PL measurements – advanced options
The Wire software offers many options, both as regards the setting of the
instrumentation (calibrate system, running maps…) and the data analysis (import /
export files, fitting, overlay plots…). There are too many options to be covered in the
present document, therefore the users must refer to:
4.1. Induction by the Area Responsible Personnel (ARP) or by users who received the
induction “Employ the Renishaw Raman Spectrometer”; the ARP and enabled
users are listed in the Safety Folder
4.2. “Wire 1.3 Raman software” manual, available in locker #6 (Raman Lab Storage)
in the entrance of the Cleanroom
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MARC/CENTRE OF EXCELLENCE FOR QUANTUM COMPUTER TECHNOLOGY
5. Shutdown procedures
5.1. Close the “Renishaw – WiRE” software
5.2. Turn off the “ProScan II” module
5.3. Turn off the Renishaw spectrometer
5.4. Turn off the microscope
5.5. Follow the laser shutdown procedures, if appropriately trained (see sections 9.1,
9.2 or 9.3)
5.6. Turn off the “LASER ON” indicator
5.7. Turn off the interlock (box at the wall): DISABLE (key), POWER
6. Working after hours
Only users who have been explicitly authorized by the ARP can use the ASL after
hours; non-authorized users can work after hours only if assisted by authorized users.
All users working after hours must refer to the standard Cleanroom procedures (work
buddy, time limitations, …).
7. Unattended equipment left on during working hours
Leaving equipment ON and UNATTENDED during working hours is tolerated in the
Advanced Spectroscopy Laboratory. Users MUST leave clear contact details in the
laboratory logbook. The laboratory should not be left unattended for long periods
(>3 hours).
8. Unattended equipment left on after hours
Leaving any equipment ON and UNATTENDED after hours is STRICTLY FORBIDDEN
in the Advanced Spectroscopy Laboratory, under any circumstances.
DOCUMENT END
SOP L 100
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