P10 Coherence Beamline User Guide
Contents
1. button serves to view a selected image 3 2 MAXIPIX 2x2 The Maxipix detector in 2x2 configuration is a 2D detector developed at ESRF which has a pixel size of 55x55um 516x516 px 28 4x28 4 mm active area dynamic range count rate of 100000 cps pixel at 10 dead time and maximum frame rate of 350 Hz 0 3 ms readout The quantum efficiency is 100 at 8 keV 68 at 15 keV and 37 at 20 keV In the following it is explained how the Maxipix detector is implemented at the P10 beamline 1 A ssh connection to the Maxipix control computer needs to be established via gt ssh opidOO mpxdesy2 desy de There exists an auto login from the experimental control computers haspp10el or haspp10e2 Please check at this point of the network storage of P10 is mounted by testing the command cd data 2 The program Dserverl 5x1 or Dserver2 2x2 needs to be started from the command line on the Maxipix computer Once these steps are finished the Maxipix device definitions can be activated in the online xml file and Online tki can be called on the experimental control computer hasppl0el or haspp10e The Maxipix detector can now be controlled from Online in a variety of ways a A widget has been created on the Online TKI Window under Misc b Several Perl scripts are available to take a single image or a time series of images c The Maxipix detector has been implemented as virtual counter d The Maxipix dete2. move USAXS photodiode EHI in the beam extract USAXS photodiode from the beam Here ehN means either ehl or eh2 for experimental hutch 1 or 2 respectively gt ish ehN open open interlock shutter usually after the interlock is set by searching the hutch gt ish ehN close gt sh ehN break close interlock shutter without breaking the door interlock close interlock shutter and break the door interlock Before entering the hutch be sure the door lights are switched off Commands to control slow and fast shutters gt osh open fast shutter 32 gt csh close fast shutter gt OSS open slow shutter gt CSS close slow shutter gt fastshutter in insert fast shutter in the beam path gt fastshutter out extract fast shutter from the beam path Absorber commands gt abs show currently used absorber set all possible absorber combinations are also displayed gt abs n insert absorber in the beam n is an integer number from 0 to 192 possible number of 25 um thick Si plates Au foils 0 1 2 3 4 6 8 9 12 16 18 24 32 33 36 48 64 66 72 96 128 129 132 144 192 gt abs 0 move absorbers out no absorber in the beam use with care Caution When working with 2D detectors be sure to have fastshutter inserted in the beam gt fastshutter in Commands to move scan motors gt wm mot mot2 mot3 display
3. power off of the fan unit underneath the VME see Fig 17 After a 10 second waiting time the VME power can be switched back on and the Tango Server can be restarted by using the Start All button _ EV i es um Fig 17 View of the VME crate Power on off button 29 Restarting the control computer If the control computer is frozen then it might need to be reset Before using the hardware reset switch one can try to use another control computer of the P10 beamline to ssh into the problematic control computer e g opening a new terminal and typing gt ssh haspp10opt el or e2 The shutdown command would be gt sudo sbin restart P now If this doesn t work the square reset button under the front cover should be used Hopefully the computer comes up normally and the user can login as plOuser The password should have been provided at the start of the beamtime Restoring the control computer After the control computer is restarted and the user logged back on as p10user it is necessary to recover the session The p10 control computer has in the standard configuration six desktop panels which can be accessed from the taskbar located on the bottom of the screen The six panels are called Online Optics X Ray Eye Interlock Macros and Other The Online panel In this panel the ONLINE session and the Tango Device Manager for EHI amp EH2 should run It is recommended to open three t
4. retractable monitor unit is installed The sample chamber is based on a DN100 6 flange OD UHV cube The cube is mounted on a 4 axis Huber tower X Y Z and RZ The cube is fully vacuum integrated using DN 2 75 flange OD bellows along the X ray beam direction Multiple different sample inserts have been developed to be housed in the sample chamber transmission and reflection setups which are listed under EH2 Standard Setup Sample Inserts The sample position is followed by a DN100 6 flange OD 6 way cross This 6 way cross allows e g to mount in vacuum detector e g diodes as well as a vacuum pumping system The last piece of the sample environment is a DN100 gate valve before the scattered signal is transported to the end of the hutch in a 4 ID tube There the tube diameter increases to 8 ID and the beam transport continues to the detector stage in the 2nd experimental hutch By using a detector position at the end of EH2 a sample to detector distance of 20 m is possible The setup is modular and it is envisioned that components can be removed from the IDT 5 axis table to make room for more complicated experimental setups The optical table is equipped with a 1 5x1 0 m breadboard mounting holes are M6 on a 25x25mm grid All optical tables at P10 are designed to have a 600 mm distance between X ray beam and table top surface Fig 6 Soft matter CDI XPCS USAXS setup of EH1 Six circle diffractometer Experimental h
5. C c The low temperature insert with an additional holder for small magnetic fields The holder is based on electromagnets and produces variable fields up to 0 1 T d A sample insert for reflection experiments in a temperature range from 0 200 pe Nanofocusing setup at P10 The group of Prof T Salditt of University of G ttingen designed and installed the experimental setup GINIX for holographic imaging at P10 The setup is placed on a 5 axis table IDT This table is movable on air pads and can be exchanged with the standard CDI XPCS setup Further details can be found in 1 Kalbfleisch S Neubauer H Kr ger S P Bartels M Osterhoff M Mai D D Giewekemeyer K Hartmann B Sprung M amp Salditt T 2011 AIP Conf Proc 1365 96 99 2 Kalbfleisch S 2012 PhD thesis Georg August Universit t G ttingen Germany 14 Flight path and detector stage The detector stage in experimental hutch EH2 of P10 is based on a 3 5 m long translation mounted on a granite block at the end of the experimental hutch Fig 13 The granite block is rotated by 15 from the perpendicular direction to the beam This setup allows to rotate the 5m long flight path and detectors around the sample position by 30 degrees in the horizontal direction which makes it possible to perform coherent scattering experiments at large Q values 2 A 8keV A set of different detectors currently in use at P10 is described in secti
6. basis 2 4 Preparing the beam After the synchrotron beam is provided by the machine division the message on the PETRA III status panel has turned to User Experiments one can proceed to start the experiment as follows gt First all beamline hutches optics hutch experimental hutch 1 experimental hutch 2 have to be set up see 2 1 gt Next one should close the undulator gap to the required value 16 3 mm for photon energy of E 8 keV This can be done by moving the virtual motor UNDULATOR in lt ONLINE gt GUI to the desired energy in eV Note that for energies above 12 keV one has to use 3 harmonic of an undulator i e energy divided by a factor of 3 has to be applied The process of closing the undulator from opened state to a closed state may take several minutes During this time it is highly recommended not to launch any other commands in lt online gt session gt The motor FMBEnergy Bragg angle of double crystal monochromator has to be also set to the required photon energy in eV gt After closing the undulator gap one should wait for about 15 minutes until the monochromator optics reaches the thermally stable state After that one can open safety shutter s Namely all shutters in interlock GUI Fig 18 15 panel 10 1 optics hutch panel 10 2 EHI panel 10 3 EH2 have to be opened The sizes of Galil slits G1 and G2 should be checked These slits define an
7. current position of a specific motor can be applied to up to 6 motors simultaneously gt mva motl xl move absolute motor motl to position x1 gt mva motl x1 mot2 x2 mot3 x3 Move absolute a maximum number of 6 motors simultaneously gt mvr motl x1 move relative motor mot1 to position x1 gt myr mot x1 mot2 x2 mot3 x3 Move relative a maximum number of 6 motors simultaneously gt whereslit n display the positions of blades of JJ slit n n 1 2 or 3 correspond to JJ1 JJ2 pair of collimating slits before a sample and JJ3 detector slits in front of CyberStar APD gt moveslit n hgap hcenter vgap vcenter move JJ slit n n 1 2 or 3 to horizontal gap hgap horizontal center hcenter vertical gap 33 to vgap and vertical center of vcenter all target values are in mm gt ascan mot x1 x2 npoints ctime absolute scan of a motor mot1 from position xl to position x2 with number of points npoints and exposure ctime gt dscan motl x1 x2 npoints ctime relative scan of a motor motl from position xl to position x2 with number of points npoints and exposure ctime gt amesh mot x1 x2 NP1 mot2 yl y2 NP2 ctime absolute mesh scan of motor mot1 in a range from xl to x2 with NP1 points at different positions of motor mot2 in a range from y1 to
8. filedir is the directory where the data will be stored filename is the file root name startnum is the number of 1 frame gt dettake exptime acquire a single frame with exposure time exptime in seconds gt detseries numframes exptime delaytime acquire a series of numframes frames with with exposure time exptime and optional delay time in seconds Mesh scans with 2D detectors gt detamesh mot x1 x2 NPI mot2 yl y2 NP2 nframes ctime absolute mesh scan with two motors and acquisition by 2D detector gt detdmesh motl x1 x2 NP1 mot2 yl y2 NP2 nframes ctime relative mesh scan with two motors and acquisition by 2D detector Operating the CRL transfocator gt wm ehcrl display the currently used CRL combination gt mya ehcrl lt combi gt insert the lens combination combi in the beam read also 2 7 gt mva ehcrl 0 extract CRLs from the beam path gt mva ehcrl 4095 insert all CRLs in the beam path for testing only gt mva ecrlx2 dist move absolute the CRL transfocator along the beam to the position dist in mm DAC control gt p10dac dacchannel voltage set voltage in V toa selected DAC channel i e e2_dac03 35 Lakeshore temperature controller commands gt lake on start LakeShore controller gt lake off stop LakeShore controller gt lake pow lt P gt set heater power level Possible values are 0 1 2 3 4 5 which corr
9. of 15 C The Andor camera acquires images tif edf with 16 bit resolution 27 4 Recovery steps in case of computer failures General information The P10 beamline is controlled by a Linux based computing system Each area of P10 has its own control computer These computers are called 1 Optics hutch haspp10opt 2 Experimental hutch 1 haspp10e1 3 Experimental hutch 2 haspp10e2 Each of these computers controls hardware via an independent VME controller and an independent Tango Device Manager called by astor Additionally the P10 beamline has 2 more control computers 1 P10 E Lab haspp10lab 2 Vacuum interlock PC hasp10vil Some possible scenarios The users will use ONLINE to control their experiments most of the time So if ONLINE hangs than it should be restarted first In general the instruction manuals to ONLINE and other experimental control software can be found on the web pages of FS EC under computing manuals http hasylab desy de infrastructure experiment_control index_eng html Terminating Online To kill Online open a new terminal and type gt ps a grep gra main This command searches for the process identity pid of the ONLINE process This process identity is listed in the first column Try to kill the ONLINE process by typing kill 1 pid If the process persists use the more brutal command kill 9 pid After ONLINE has been terminated it can be restarted by switching to the ONLINE dat
10. y2 with NP points at exposure time ctime gt dmesh motl x1 x2 NP1 mot2 yl y2 NP2 ctime relative mesh scan In case the motor movement scan has been stopped by pressing Stop button in ONLINE GUI for restoring the ability to move motors one needs to execute the command gt reset_stop Commands to move the selected detector in its working position gt det cbs move in the point detector CyberStar APD gt det xray move in the X ray Eye camera gt det max22 move in the MAXIPIX 2x2 detector gt det lex move in the LCX CCD detector gt det pixis move in the Pixis CCD detector gt det p300 macro command to move in the PILATUS 300K detector In the case when count command for monitoring beam intensity with the flight tube diode diode in is used after previous use of 2D detector LCX Pixis Maxipix or Pilatus one has to take over fastshutter control by applying a macro command s gt ecdloff to take over from LCX Pixis detector gt ccd2off to take over from Maxipix detector 34 gt ccd3off to take over from Pilatus detector Commands for 2D detector acquisition Before starting acquisition with 2D detector one has to setup the detector by gt detsetup filedir filename startnum where det stands for p300 Pilatus300K detector max22 Maxipix detector Icx LCX detector or pixis Pixis detector
11. Go and 2 Status The Go command starts a series of NumFrames frames with the exposure time ExpTime and the delay time DelayTime between frames Both time parameters are in seconds The data are stored under SavingPath with the file name constructed by FileNamestart followed by a 4 digit frame number The frame numbering starts with FirstFrame and the images are stored as spe files If NumFrames is smaller or equal to 256 and the DelayTime is set to zero than the data are stored in multi image files This has the advantage that an additional overhead between frames of 0 6seconds can be prevented The time between frames for a full frame exposure can be estimated as Readout time 1 8s ExpTime DelayTime Overhead 0 6s 3 4 PI Pixis The Pixis detector Princeton Instruments is a new generation of CCD detector from Princeton Instruments having mainly the same as in LCX CCD chip installed pixel size 20x201um 1340 h x1300 v px The detector requires no water cooling circle otherwise the installation procedure is same as in the LCX case 3 5 Andor iKon L The Andor iKon L is a high resolution CCD camera with chip area of 2048x2048 px and pixel size of 13 5x13 5 um Readout frequency up to 5 MHz is possible with this detector In order to operate the peltier cooled chip working at 65 C the camera requires water cooling cycle normal setting
12. PETRA Il synchrotron at DESY Hamburg A HELMHOLTZ GEMEINSCHAFT P10 Coherence Beamline User Guide Version 01 October 2013 Contents 1 Overview of the P10 Coherence Beamline 1 1 P10 scope 1 2 P10 layout 2 Starting the experiment 2 1 The hutch search 2 2 The Interlock Control System 2 3 Coordinate system at P10 2 4 Sample mounting 2 5 Preparing the beam 2 6 JJ X ray slits calibration 2 7 CRL transfocator alignment 3 2D detectors at the P10 3 1 PILATUS 300K 3 2 MAXIPIX 2x2 3 4 PI LCX 3 4 PI Pixis 3 5 Andor iKon L 4 Recovery steps in case of computer failures 5 Commands and macros at P10 Phonebook P10 experimental hutch I EH 1 P10 experimental hutch EH 2 P10 mechanical lab M lab P10 preparation lab P lab P10 electronics lab E lab Schichtdienst PETRA III Control Room Michael Sprung Tel 4680 Mobil 96110 Daniel Weschke Tel 1920 Alexey Zozulya Tel 4798 Fabian Westermeier Tel 4217 Alessandro Ricci Tel 3799 Alexander Schavkan Tel 3128 Eric Stellamans RheoSAXS setup Tel 4216 Birgit Fischer P lab contact Tel 4478 6110 6120 6130 6140 5746 3868 3650 1 Overview of the P10 Coherence Beamline 1 1 P10 scope The Coherence Beamline P10 at the PETRA III synchrotron at DESY Hamburg is dedicated to experiments using coherent x rays and to advance its major experimental techniques These are x ray photon co
13. a directory normally something like data YEAR CYCLE DATE and typing online tki Terminating Tango Servers Please read the description for the ASTOR Tango Device Manager It explains how Tango Servers are killed and restarted Generally one can try Stop All see Fig 16 wait until all servers shut down turn red and then Start All it takes several minutes until all servers get on i e green 28 haspp10opt Control Start New Start All Stop All Display All Controlled Servers on haspp10opt Level 1 DGG2 PETRA 3 FMBOXfDCMEnergy PETRA 3 MCA8715 PETRA 3 Oms me58 PETRA 3 SIS3610 PETRA 3 SIS3820 PETRA 3 SIt PETRA 3 TITGW Petra 3 TITGW Shutter ZMX pzmx011 ZMX pzmx059 Level 2 Petra3Shutter p10 Petra3Undulator p10 Dismiss Fig 16 Dialog window of the Astor Tango server manager Note If the above steps did not solve the problems then it might be necessary to reboot the VME and or the control computers However the previous steps should always be tried first Rebooting the VME crate In order to restart the VME crate the Tango Servers of all to the VME connected devices should be stopped Looking at this screen shot Fig 16 the Stop All button should be used It is necessary to wait until all green indicators are turned red before proceeding to restart the VME The VME is stopped by turning the
14. as finished go to the center of the scanned maximum Next we scan the horizontal gap SLT2 dx in a range 0 02 0 02 note JJ slits are made such that negative gaps are possible while the blades can go behind each other without clashing The last scan should 21 have a step function profile The point where intensity starts to linearly increase is the actual zero of horizontal gap To calibrate both Left and Right blade positions one selects Properties by right click then puts Register to zero followed by Apply and then one puts Position to zero also followed by Apply OK with that horizontal gap is calibrated 3 Now the vertical slit has to be adjusted For that we open horizontal gap to 0 4 and repeat steps 1 3 for the vertical center cy and gap dy To adjust the first slit SLT1 one has to open the SLT2 gt moveslit 2 2 0 2 0 and follow steps 1 4 2 7 CRL transfocator alignment The CRL x ray transfocator based on beryllium CRLs is installed at the EH2 at a distance of 86 1 m from a source The CRLs with different curvature radii 50 to 1000 um are grouped in 12 stacks The first 4 stacks contain 1D lenses and the other 8 stacks contain 2D lenses There are in total 2 4096 possible lens combinations In order to select the best combination for a given photon energy and image distance all possible combinations should be scrolled For this purpose a Matlab script was written whi
15. ch calculates the correct lens combination as well as the optical parameters of a focused beam offset distance focal spot size efficiency gain and depth of focus The script is available on the Windows analysis PC of EH2 control hutch Start Matlab and browse to the directory C Matlab tools The script is called P10lens_v2 and expects two input parameters the x ray energy in keV and the distance from lens center to sample in meters At the standard lens position this distance is 1 574 m The Matlab call P1Olens_v2 8 0 1 574 generates the following output ans bestcombi 768 bestbinary 000000001100 bgoal 1 5740 dist 0 0489 bfinal 1 6229 deltadist 1 5616e 005 verticalsize 2 5189e 007 horizontalsize 1 5113e 006 bestefficiency 78 2624 bestgain 3 2894e 005 nstacks 2 DOF_v 0 1045 DOF_h 0 1045 v_size_diff 3 0788e 006 h_size_diff 3 4204e 006 Note all the output distances are in meters 22 For transfocator alignment the following parameters are important gt bestcombi This parameter is the value needed to select the correct CRL stack combination These stacks are moved into the beam by typing the command online gt mva eherl bestcombi The lens is moved out of the beam by typing online gt mva eherl 0 gt dist This value describes an offset value for the motor ecrlx2 This motor moves the whole lens tower along the beam direction to bring the focal spot to the sample The command is on
16. ctor has been implemented into the XPCS measurement scripts 25 There are typical three Perl scripts setup series and take for 2D detector operation at the P10 beamline These can be called from the command line in the following way 1 max22setup network storage directory firstframenumber 2 max22series nframes exposuretime 3 max22take exposuretime Note The Tango server for the Maxipix detector loads by default an incomplete configuration and it is advisable to run the setup script max51setup or max22setup once at startup to define all necessary parameters Id 6 filenamestart_ 3 3 PI LCX The LCX detector is a CCD detector Princeton Instruments with a pixel size of 20x20um 1340x1300 pixel active area 16 bit dynamic range effective 5 6 bit dynamic range and readout time about 1 7s The quantum efficiency is 75 at 5 keV 50 at 8 keV and lt 5 at 12 keV The operation of the LCX camera from Online Tango is not straight forward The momentary solution communicates via a Perl server script with the Roper Scientific Winview software This communication is one sided meaning that Winview is not providing any information output about its status This means that the Tango Online control has to be very careful Any error message in Winview will cause severe problems which will need several steps to recover up to restart Winview Perl Server and Tango Server The WinView program is ins
17. d for this purpose and this method will be described here One user has to start the search procedure by placing a valid DACHS card over the DACHS card reader Fig 14 near the main door All other doors and gates need to be closed in advance This starts a warning message for the area and activates the light barrier which acts as a person counter and the first search button a green button near the door inside the area lights up The user proceeds by entering the hutch searching the hutch and doing so pressing all necessary search buttons green buttons After the user is finished with the search the user returns to the hutch door and presses the yellow button near the door to deactivate the light barrier for 5 seconds Only then the user is able to leave the area and to close the door If the user has succeeded to follow this procedure an orange light will come up near the door The search is finished by pressing the last Final search green button outside of the area followed by placing the DACHS card over the DACHS card terminal again An additional red light will show up on top of the orange light The warning message will sound for a short moment before the Permit Beam Operation button gets enabled on the Interlock Control System web page Pressing this button locks the doors and enables the Open BS button on the area panel Signal red light Sperrbereich 4 4 44 a Prohibited Area Final search Ligh
18. e beam downwards Fig 10c This enables studies of liquid surfaces in grazing incidence conditions i e no full reflectivities up to large angles but enough to reach incidence angles of up to 2x the critical angle of most liquids Details on the construction can be found in the diploma thesis of Milenko Prodan and the apprenticeship report of Serge Bondarenko both are in German Fig 9 Schematic view of the 2nd experimental hutch with control hutch c Sabi N Upstream gate valve d Y Fig 10 Optical elements on OT2 of EH2 a pink beam slits Galil 2 b CRL transfocator c beam deflection unit 12 Standard CDI XPCS setup at EH2 The standard CDVXPCS setup in EH2 is based on a 2 circle Huber diffractometer in horizontal geometry Fig 11a This diffractometer is mounted on a granite support and can be moved out of the beam path on air pads The diffractometer is based on a combination of a Huber 440 and 430 goniometer sitting on a YZ translation For most experiments the 440 goniometer is used as the rotational bearing for the 5 m long detector arm On top of the goniometers a tower of Huber stages 170x170mm size is mounted In the typical configuration it offers XYZ translations XY Huber 5102 20 Z Huber 5103 A20 40 as well as a 2 circle segment Huber 5203 20 for rotations around X amp Y A DN100 6 flange OD vacuum cube is used as the standard cell for the sample environment Exam
19. erminals The first terminal should just start a Tango Device Manager The command is astor amp The second terminal should connect to the other control computer via ssh The command is ssh hasppl0el or ssh haspp10e2 depending on which control hutch is occupied The Tango Device Manager is called again by astor amp The third terminal should be used to call ONLINE The user should first change to the data collection directory the standard directory would be of the form dat YEAR CYCLE DATE ONLINE is started then by typing online tk1 The Optics panel This panel should be used to control components connected to the optics control computer haspp10opt Again the user should open two terminals and use both to ssh to the optics computer via ssh haspp10opt The first terminal should be used to start the Tango Device Manager via astor amp and the second terminal should be used to open Jive via jive amp From the Jive panel the user should open the Undulator control window This can be done by opening the tree Petra3Undulator p10 and Petra3Undulator till the p10 undulator 1 device is found A right click on p10 undulator 1 opens a context menu and the selection Monitor Device opens the undulator control window 30 The Interlock panel This panel should be used to start Firefox browser The homepage of Firefox is set to the following tabs Tab 1 Interlock control system Tab 2 Vacuum interlock control s
20. es different optical components EH2 contains an identical optical table to allow sharing of optical components between the experimental hutches The first element is water cooled slit system operated in closed loop with a maximum opening of 10x10mm and a resolution of 0 2 um The second element is a dual fast shutter system for 2D detectors One system is based on amplified piezo actuators similar to a design by Cedrat Ims and the second system is based on magnetic coupling 30ms This is followed by an absorber system and a retractable monitor unit to check the beam intensity Shared optical components in EH The first component in the first experimental hutch EH1 is a FMB Oxford beam positioning monitor BPM A water cooled diamond window 5 mm OD 60 micron thickness is connected downstream to the BPM This device combination sits on a granite post and can be aligned vertical and horizontal to the beam using two Huber stages Fig 5a The travel ranges allow to shift between pink and monochromatic beam options It is possible to stabilize the beam position at the BPM using vertical and or horizontal feedback programs The next object in EHI is a 2 7m long optical table This 5 axis table Q SYS carries several shared components for the beamline Situated on a granite spacer are a pink beam capable piezo driven slit system Galil 1 with a nominal opening of 10 x10 mm as well as a fast shutter system an absorber system and a f
21. espond to heater power of 10 mW 100 mW W 10 W 92 W gt lake T show actual temperature gt lake T AK show actual temperature of channel A in K gt lake T B C show actual temperature of channel B in C gt lake setp lt T gt set setpoint temperature gt lake PID lt P gt lt I gt lt D gt set PID parameters of temperature control see LakeShore manual When using sample inserts equipped with Peltier element one has to switch on the Kepko current supply and set correct DAC voltage For heating above 100 C one has to apply command gt plOdac e2 _dac02 2 this command applies 2V voltage to DAC channel e2_ dac02 which converts to 1 6 A current setting of Kepko supply For RT measurement and cooling down below RT one has to apply following DAC voltages gt pl0dac e2_ dac02 0 5 for T range 285 305 K gt pl0dac e2_dac02 1 for T range 270 290 K gt pl0dac e2 dac020 for T range 300 350 K 36 Notes comments 37
22. eta straight section of sector 7 of the PETRA III storage ring The source size is On X Oy 36 X 6um The beamline layout includes front end slits optics hutch OH experimental hutch 1 EH1 experimental hutch 2 EH2 Beamline infrastructure includes preparation laboratory P lab mechanical workshop M lab electronics workshop E lab and a storage room Fig 2 G1 G2 CRL Sample D EH2 0 20 33 35 38 68 84 85 4 87 7 93 108m E E N P10 P10 P10 2 Exp Hutch 2 Control Hutch 1 Exp Hutch 1 Control Hutch P08 P09 P10 Optics Hutch Store M Lab P Lab P10 EH2 P10 CH2 P10 EH1 P10 CH1 AFM LAB P10 OH Fig 2 P10 infrastructure 1 2 1 Optics hutch The Optics Hutch OH is situated 33 46 m from the middle of the straight section There is some space available at the beginning of the optics hutch which is reserved for a high heat load flat mirror to enable pink beam operation of the beamline The standard PETRA II high heat load monochromator is the next major component Fig 3a It is located at 38 m and cooled by liquid nitrogen Currently it is equipped with an independent Si 111 crystal pair 2 7 30 0keV and an unpolished Si 111 channel cut 7 0 17 0keV In the future it is planned to replace the independent Si 111 crystal pair with a Si 311 channel cut Both channel cuts will be polished The channel cut design offers a much higher angular stability of the beam at the price of reduced energy
23. insert 2 Close the manual vent valve near the sample cell 3 Press Close Vent on the turbo pump touch panel 4 Press Start on the turbo pump touch panel 5 Wait until the pressure sensor P3 reads a pressure lt le 03 mbar 6 Open both gate valves by turning the Output of the HAMEG power supply on Now you are ready to search the hutch and start measuring your new samples 20 2 6 JJ X ray slits calibration The paragraph describes a procedure to calibrate the JJ X Ray slits pair of slits in front of a sample Fig 10a on a micro meter level The first step for a rough alignment should be to look at the beam with the x ray eye Use the macro det xray The user should close the slit blades one by one roughly centered over the beam on the x ray eye This way the user should produce a small square beam on the x ray eye display Beam sizes smaller than 100 microns by 100 microns can easily produced this way Now change to the Cyberstar detector using the det cbs macro currently Si diode inside the flight tube is used instead command gt diode in Now the user should close the slit by moving the top blade and perform an absolute scan 5 micron step size towards positive values In this direction the top blade has no backslash The scan should be flat in the beginning close position and start to increase linearly at some point After the scan is finished return to this turning point and perform a fine scan 1 micron step si
24. irst monitor unit Fig 5b The fast shutter unit houses two separate shutter systems A water cooled piezo driven shutter system with Ims response time and a slower 30ms actuator driven shutter The fast system has a small opening of 0 7 mm and can be moved out of the beam by a linear translation The absorber consists of two linear translations Each translations is equipped to hold 9 different absorbers Currently the center position is left empty on both stages and two different materials are mounted on the different sides One half holds Silver absorber for X ray photon energies above 12 keV and the other half holds both sided polished thin Silicon crystals for lower X ray energies Finally the monitor unit is based on scattering of a thin Kapton foil under 45 in combination with a Cyberstar scintillator detector Fig 5 Shared optical components in the EH1 a BPM b slit system Galil 1 fast shutter absorber unit and beam intensity monitor Soft matter CDI XPCS setup of EH1 The setup for soft matter CDI XPCS of EHI Fig 6 is very similar to the standard CDI XPCS setup in EH2 It is mounted on a 5 axis optical table from IDT In front of the sample position it features a pair of slit from JJ X Ray IB C30 HV These slits are 700mm apart The first slit defines the size of the X ray beam and the second slit acts as a guard to suppress most of the slit scattering of the first slit Between the slits an in vacuum
25. ith a 20x20 um pixel size and 1340x1300 pixels has been used intensively at coherence beamlines around the world A Mythen 1K detector PSI is used as a fast 1D detector at P10 having 1280 strips As a point detector an avalanche photo diode ESRF is available in combination with an hardware autocorrelator Correlator com 3 1 PILATUS 300K The PILATUS 300K detector is a 2D detector developed by PSI and sold by Dectris with a pixel size of 172x172um 487x619 pixel active area 20 bit pixel dynamic range and readout time of 7 ms The quantum efficiency is 91 at 5 4 keV 96 at 8 keV and 37 at 17 5 keV To start operating the Pilatus one has to proceed as follows 1 From the experimental terminal in EH2 plOuser haspp 10e2 gt ssh 1 det haspp1 Opilatus gt cdp2_det gt runtvx 2 Start Pilatus Tango server Pilatus P10E2 from the Astor panel 3 Make sure the detector is active uncommented in the online xml file 4 restart lt online gt GUI 24 5 Setup working directory lt online gt p300setup directory name_of_file 1 6 Use p300take or p300series commands to record images To start the P10 image viewer 1 pl0user haspp10e2 gt cd beamline matlabmacros plOuser haspp 10e2 gt cp P10show2_pilatus300K ini P10show2 ini 2 Start image viewer GUI by double clicking the desktop shortcut Show Pilatus 3 Enter relevant file path and prefix Update
26. line gt mva ecrlx2 dist Here dist is an offset distance in mm During the transfocator alignment both JJ1 and JJ2 slits should be opened 1 x 1 mm Alignment of the transfocator is done by scanning the whole device in vertical and horizontal directions perpendicular to the beam G2 should be set to 0 2x0 2 mm Corresponding motors ecrly and ecrlz should be scanned in a relevant range 0 5 mm Additionally the two tilts ecrlry and ecrlrz have to be used for final alignment of the transfocator axis which should be parallel to the beam Once these commands are executed the G2 slit size should be set to 100 200 um vertically and 75 100 um horizontally a trade off opening of 150 V x 75 H um provides high spatial coherence at optimal coherent flux in a focused beam In addition the user can close the JJ2 slit to about 0 05 x 0 05 mm around the beam for reduction of a background scattering 23 3 Detectors at P10 The Coherence beamline P10 has several different detectors in use and it is possible to reserve additional specialized detectors via the DESY detector pool O Pilatus 300K detector Dectris 487x619 pixels Pixel size of 172x172 um A Maxipix 2x2 detector ESRF is often is use at P10 516x516 pixels Pixel size of 55x55 um As the work horse 2D detector for XPCS CDI experiments a PI LCX detector Princeton Instruments is available This slow direct illumination CCD w
27. mline macros python folder on the experimental control PC hasppl0el or haspp10e2 for experiments carried out at the EHI or EH2 correspondingly Note that for repeating monochromator pitch the bpmcontrol py script has to disabled first Further steps concern the alignment of JJ slits focusing optics beamstops detector and a sample which will be described further in the User Guide 2 5 Sample mounting The procedure of mounting changing the sample depends on the type of executed experiment For in vacuum sample mounting the first step is to vent the sample area After the venting is done the sample can be changed The last step is evacuating of the sample cell How to vent and pump the sample area The sample cell is connected to a turbo pump stage and two gate valves can be used to separate the sample from the flight path before and after the sample To safely change a sample several steps are necessary and described here 1 Vent the sample cell 1 Close both gate vales by turning the Output of the HAMEG power supply off 2 Press Stop on the turbo pump touch panel 3 Press Open Vent on the turbo pump touch panel 4 Open the manual vent valve near the sample cell slightly 20 30mbar on P3 and wait for the turbo pump to spin down 10 000 rpm 5 Fully open the manual valve and wait till the pressure is equalized 6 Remove the sample insert and change your sample 2 Pump the sample cell 1 Remount the sample cell
28. neral components The first element in experimental hutch EH2 is a DN200 8 tube ID gate valve which is not shown in the following This page describes components which are situated on a 2 7m long optical table in EH2 The 5 axis table is similar to the optical table at the beginning of EH1 The table can be moved out of the beam to install a DN200 8 tube ID flight tube which allows to have a sample in EH1 and use the detectors in EH2 A piezo drien water cooled slit system Galil 2 followed by a monitor unit are sitting on a granite block at the start of the optical table in EH2 Fig 10a The maximum nominal slit opening is 10x10 mm and the resolution of the slit position is 0 2 microns Similar to EH1 the monitor unit is based on scattering of a thin Kapton foil under 45 in combination with a Cyberstar scintillator detector The beamline uses Beryllium lenses to reach focal spot sizes between 3 5 microns in both vertical and horizontal direction The lens changer transfocator design is equipped with 12 stacks of interchangeable Beryllium lenses which allows to have the correct lens combination for the desired focal distances of several meter and for X ray energies between 5 18 keV Fig 10b A Matlab macro can be used to calculate the best lens combination and best lens to sample distance for the chosen X ray energy The beamline has developed a beam deflection unit BDU The BDU uses two Ge 111 crystals to slightly tilt th
29. on 3 20 detectors Detector table are Fig 13 a View of the standard CDI XPCS setup in EH2 1 2 4 Support laboratories Coherence Beamline P10 has three supporting laboratories A mechanical laboratory P10 MLab an electronic laboratory P10 ELab and a sample preparation laboratory P10 PLab The names are an indicator of their main use The mechanical laboratory is dedicated to preassembling of sample environments testing of vacuum windows and whatever tasks seems to fit It is equipped with a small working bench a water sink supply of compressed air and some standard gases as well as cooling water The electronic laboratory is equipped with an additional electronic rack which includes a VME and a NIM crate This allows testing of new motor stages or detectors offline from the beamline Again cooling water compressed air and standard gases are available The sample preparation laboratory is not a full chemical laboratory but it allows simple tasks with harmless chemicals to be undertaken e g cleaning of vacuum components Access to a fully equipped chemical laboratory can be obtained via the DOOR system 2 Starting the Experiment 2 1 Hutch search procedure All areas of a beamline at PETRA III need to be searched before the x ray beam can be turned on The purpose of the search is to make sure that nobody is inside of the area when the x ray beam is on The interlock system of PETRA III has developed a metho
30. onochromator b the mirror pair and c the 1D lens changer in the optics hutch of P10 1 2 2 Experimental hutch 1 EHI is a 12m long hutch situated 67 79m from the source Figure 4 shows the experimental setups installed and foreseen in EHI After some optical components explained in more detail below three different sample environments follow First a specialized setup for soft matter CDI XPCS experiments with a sample to detector distance of 20 m and relatively large beam sizes is installed The accessible Q range is limited Q lt 2x10 A 8keV but the reduced flux density can be beneficial for many soft matter systems This sample environment is followed by the large 6 circle diffractometer which is currently under commissioning Finally a rheology setup is installed which allows to conduct experiments in vertical scattering geometry The first 3m of the hutch are dedicated to house a set of shared optical components for the complete beamline Fig 5 The first element in EHI is a combination of beam positioning monitor BPM by FMBOxford and diamond window situated on a granite block The beam position is estimated from the backscattered intensity of 0 5 um thick foils Titanium or Nickel The water cooled diamond window 5 mm diameter 60 um thick is connected to the BPM This is the only window of the beamline separating the ring vacuum from the beamline vacuum These components are followed by an optical table that hous
31. optical axis for the whole beamline path and only horizontal and vertical gap values need to be set center positions should remain Usually the G1 is set to 0 60 6 mm and the G2 to 0 3x0 3 mm If the undulator gap was set to a new setting it has to be scanned anew The UNDULATOR virtual motor has to be scanned in a relevant range and set to a peak position In case the beamline was previously aligned there should be already beam intensity counted by the Cyberstar beam monitors in EHI and EH2 Usual command is gt osh count csh This command opens fast shutter counts the intensity for 1 s and closes fast shutter Fine alignment of the monochromator is executed by the virtual motor XTAL2_ PITCH which should be scanned in a proper range the stored setting should normally be correct in case of doubt please ask the local contact After a scan is finished the motor has to be set to a center of mass position Next the 2 mirror should be scanned using the motor MIR2RZ which is a pitch angle for this mirror default range should be right otherwise a range of 0 002 deg is sufficient The position should be set to a center of mass value After scanning the 2 mirror a monochromator pitch scan should be repeated After this is done the optical alignment is mainly completed and the vertical beam position stabilisation should be turned on by launching the python script bpmcontrol py located at the bea
32. ples for different sample cell inserts are displayed when clicking on the navigation button left side For experiments in SAXS geometry the sample cell is fully vacuum integrated It is connected along the X ray beam direction with DN40 2 75 Flange OD bellows Upstream of the sample environment sits a pair of JJ X Ray slits IB C30 HV on a Huber YZ stage Between the slits is a vacuum integrated monitor unit Downstream of the sample environment a 6 way cross 4 tube ID followed by a DN100 gate valve connects the sample region via a 5 m long flight path to the detector region Fig 11b Fig 11 a Schematic view of the standard XPCS CDI setup in EH2 b Schematics of the standard sample setup integrated to the detector stages Sample inserts The main idea of using a DN100 vacuum cube as an experimental chamber is the possibility to easily change between different experimental conditions P10 has developed a set of standard sample inserts but it should be easily possible to design a sample insert for almost any arbitrary experimental condition Additional possibilities are e g a stress strain insert Fig 12 shows the drawings of currently available sample inserts Fig 12 a The transmission sample insert This insert allows to study samples in vacuum sealed capillaries at temperatures in between 0 200 C b The low temperature transmission sample insert This insert covers a temperature range in between 150 50
33. ranges and energy dependent exit offsets Next is a pair of flat R gt 100km horizontally reflecting mirrors Fig 3b The mirrors are coated with a Rhodium and a Platinum stripe to match the cutoff energy for higher energies to the experimental conditions The mirrors are followed by the bremsstrahlung shield often termed beamstop in the optics hutch The beamstop is a water cooled Densimet collimator with holes for the pink beam 4mm diameter and the monochromatic beam 4x11 mm Both beams need to be offset from the white beam position by a minimum of 20 mm A girder with several optical elements has been installed after the beamstop Site note Currently the lowest reachable energy 3 8keV of the beamline is given by the minimum gap of the undulator of 9 8mm It is foreseen to install the lens changer in the optics hutch of P10 installation is planned for the summer shutdown in 2013 The lens changer will be equipped with vertical focusing 1D Beryllium lenses Fig 3c A total of 6 different lens stacks will allow to match the horizontal and vertical transverse coherence length at a 2nd lens changer in the experimental hutch This focusing scheme maximizes the available coherent flux for the experiment The 6 stacks will be equipped with the following lenses number of lenses x radius of lens curvature mm 1 8x 0 5mm 2 4x 0 5mm 3 2 x 0 5mm 4 1 x 0 5mm 5 2 x 1 5mm 6 1x 1 5mm Fig 3 a High heat load m
34. rosoft Outlook We Y Beamline P10 Beam Permission G10 3 Fig 15 Screenshot of the web interface of P10 interlock control system 17 2 3 Coordinate system at P10 P10 uses a right handed coordinate system which is defined by the x ray beam direction The X axis is parallel to the beam direction going to positive values away from the x ray source The Y axis is perpendicular to the beam direction X lying horizontal The Y axis goes to positive values outboard from electron positron accelerator ring The Z axis is perpendicular to the beam direction X standing vertical The Z axis goes to positive values from the floor up Standard translation are called X Y amp Z The names is derived by starting with a descriptive part followed by an underscore and the following letter X Y or Z indicates along which axis the translation is Standard rotation are called RX RY amp RZ The name is derived by starting with a descriptive part followed by an underscore The R indicates that it is a rotation and the following letter X Y or Z indicates which axis the rotation turns around The sense of the positional values are defined due to the fact that all rotations are right handed i e use the right hand rule from your undergraduate physics course Exceptions to this system will be explained on a case by case
35. rrelation spectroscopy XPCS and coherent diffraction imaging CDI XPCS is the x ray analogue of dynamic light scattering DLS in the visible light range By monitoring changes of speckled diffraction pattern in the time domain this technique allows it to study slow collective motions on length scales unobservable by visible light CDI is an x ray imaging technique which uses phase retrieval algorithms to reconstruct small objects from a coherent x ray scattering pattern Using advantages of x rays like e g element sensitivity or the high penetration depth it is possible to image objects with a resolution of several tens of nanometers or to look at strain fields inside of nanocrystals The P10 beamline is located at a low beta section and takes advantage of the extreme brightness of the PETRA III storage ring Currently the PETRA III synchrotron is operating at 100 mA in top up mode which provides a coherent flux superior to all existing coherent beamlines at storage ring based x ray sources see Table below Coherent photon flux at P10 ANA E Flux n Energy 6 10 pink beam 1st 0 025um 1 4 101 8keV harmonic 1 104 Si 111 1 5m 23 10 8keV 3 105 Si 311 5 0um 6 1010 8keV 2 10 pink beam 3rd 0 054um 1 4 10 2 12keV harmonic 1 2 P10 infrastructure Overall layout of the P10 beamline is shown in Fig 1 The source of x rays for the P10 beamline is a 5m long U29 undulator located in the low b
36. t barrier Fig 14 Interlock panel of P10 beamline OH DACHS sensor 2 2 The interlock control system The interlock control system is controlled by a web based interface It can be found on the 1 tap of the Firefox P10 homepage of the control computers haspp10e1 amp haspp10e2 The link is http ics index php The web site is divided into two parts The top part indicates the layout of the beamline In the case of P10 it shows three areas optics hutch experimental hutch 1 and experimental hutch 2 divided by beamshutters The lower panel shows the current status of a particular area in this case Area 3 which is the experimental hutch 2 Clicking at the areas switches the panels At the moment of the screen shot Fig 15 the x ray beam was passing into the end station of P10 To close the shutter and to enter the hutch it is necessary to a press Close BS 10 2 b press G 10 3 Cancel Beam Permission and c unlock the doors by pressing Break door interlock G10 3 Each of these actions needs to be confirmed by pressing Ok Before the shutter can be reopened the hutch needs to be searched see 2 1 After the warning message has finished the G10 3 Permit Beam Operation button needs to be pressed this locks the doors before the shutter can be opened by pressing Open BS10 2 gt eray os ser userl x PETRA Operation Ove 6 petra_status_1280 pn Mic
37. talled on haso052Icx desy de and the account Icxuser should be used Before launching the Winview software shortcuts can be found on the desktop and the quick launch toolbar the PI LCX camera should be connected to the ST133 camera controller which can be sub sequentially turned on The next step involves mounting the network storage The network storage drive is mounted as disk Y It must be mounted from the p10user After launching the Winview software the cooling for the CCD chip should be turned on and be set to 40degC This can be done in Winview under Setup Detector temperature Also the image orientation should be set under Setup Hardware on the display tab The Reverse and Flip flag should be set Once these steps are finished the Perl server program Icx_xpcs_server pl must be launched by clicking the shortcut StartPerlServer bat again on the desktop or on the quick launch toolbar The Perl server program as well as the other Perl scripts can be found in D Perl The file StartPixisPerlServer bat should be used for the PIXIS detector Now all necessary steps on haso052Icx are finished and the user should restart the Tango Server LCXCamera PIOE2 to re establish the communications 26 The Perl Server can read and write the following attributes 1 SavingPath 2 FileNameStart 3 FirstFrame 4 NumFrames 5 ExpTime 6 DelayTime as well as the following commands 1
38. utch EHI is housing a large 6 circle Huber diffractometer Fig 7 which enables scattering diffraction experiments at large scattering vectors Q The diffractometer is very similar to a diffractometer installed in the first experimental hutch of P09 More detailed information will become available as soon as the first standard components have been adapted to the diffractometer environment Fig 7 Huber 6 circle diffractometer Rheology setup Finally the experimental hutch EH1 houses a rheology setup Fig 8 This setup allows to conduct experiments in vertical scattering geometry with a rheometer to detector distance of 3 m using a HAAKE rheometer Fig 8 RheoSAXS setup 1 2 3 Experimental hutch 2 The second experimental hutch EH2 is located at 83 95m from the X ray source Fig 9 It is home to the standard CDI XPCS setup as well as to the holography setup Most experiments performed at Coherence Beamline P10 have the sample located at 87 8 m from the source The standard setup and the holography setup are movable on air pads and can be easily exchanged Both setups share an 5m long flight path as well as the motorized detector stage The optical table in EH2 carries a water cooled closed loop slit system followed by a retractable monitor device to define the beam direction as well as a micro focusing lens changer 1D amp 2D focusing capability and a beam deflection unit BDU to enable studies on liquid surfaces Ge
39. ystem Tab 3 PETRA III infoscreen Tab 4 PETRA III machine log book The X Ray Eye panel This panel is used to start the X ray Eye beam camera The software for the X ray Eye is installed on the optics control computer so it is necessary to open a terminal and to use ssh haspp10opt The X ray Eye software is started by typing SampleViewer case sensitive This opens the control window and by clicking on the Eye symbol the camera display window is opened and by clicking on the Wrench symbol the settings window is opened The other panels are currently not used 31 5 Commands and macros at P10 To start the Online GUI interface PerlTk interface one has to launch plOuser hasp10e2 online tki from a Linux terminal on control PC example of EH2 Once the ONLINE session is started the control commands can be executed from a command line of GUI In following the commonly used macro commands syntax emulating SPEC commands are listed Counting commands gt count exptime gt diode in gt diode out gt refdiode in gt refdiode out gt udiode in gt udiode out Interlock shutter control macros execute acquisition by selected counters for exptime in seconds move photodiode inside flight tube in the beam extract photodiode from the beam move reference photodiode after the sample in the beam extract reference diode after the sample from the beam
40. ze around this position The turning point found during this fine scan should be used to set both the top and the bottom blade to zero Now the slit should be opened to 50micrometers in the vertical direction and the procedure should be repeated in the horizontal direction Here the slit needs to be closed by the left blade The left blade in than scan in positive direction without backslash as in the vertical direction Once the slit size is defined in both direction the slit center can be scanned The slit are setup in a way that the center scans are performed without backslash Once the center are found the positions of all four blades should be reset The following example sequence of commands serves to adjust JJ X ray slits SLT1 SLT2 using Si diode One of JJ X ray slits for instance SLT1 has to be fully opened gt moveslit 1 2 0 2 0 while the other SLT2 is getting adjusted All the positions mentioned further are in mm Diode has to be in gt diode in 1 Adjust SLT2 horizontally by setting its size to 0 5 mm and check transmitted intensity gt moveslit 2 0 5 0 2 0 count Make slit gap smaller until the transmitted intesity starts to decrease at this point one should roughly adjust the horizontal center SLT cx Slit down horizontal gap to 0 1 gt moveslit 20 1020 and do scan of horizontal center ONLINE GUI Scans Slit gt SLT2 gt cx the range is 0 8 number of points 41 2 After the scan h
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