國家同步輻射研究中心
出國報告書
出國人姓名：吳宇瀚
出國日期：102.06.24-102.12.31
目的地 (國家、城市)：日本兵庫縣光都
參加會議名稱或考察、研究訓練地點：
常駐日本兵庫縣 SPring-8
(請自下一頁開始撰寫)
20130624WuYuHan 出國報告書
一、目的
To help the operation and maintenance of side line and
main line of BL12XU beamline at SPring-8 is the main
objective for this business travel. To fulfill the requests from
BL12XU users, cooperators and the supervisors to run their
experiments or missions smoothly is another goal of this
travel.
二、行程
102.06.24 台灣新竹國家同步輻射研究中心=>台灣桃
園國際機場=>日本大阪關西國際機場=>日本大阪府=>日
本兵庫縣相生市=>102.06.24 日本兵庫縣光都 SPring-8
三、內容摘要：
The main purpose of undulator BL12XU beamline at
SPring-8 was designed for non-resonant and resonant inelastic
X-ray scattering experiments to measure the energy
distribution of scattered photons via a Rowland-circle type
spectrometer and multiple analyzers. The beamline consists of
a sideline to carry out hard X-ray photoelectron spectroscopy.
The basic components and operations of side line were
described in some details in my previous business travel
report. Thus, this report mainly covers the basic operation of
the main line of BL12XU that was not reported. It should be
noted that the procedures below still need to be corrected and
supplied for more details. It can be changed due to different
requirements of experiments or types of specimens. All the
numerical values in “spec” commands are just for reference.
1. In general, the front end slit size: horizontal 1.5 mm*
vertical 0.5 mm;
2. To show the calibration files: “on( )”(show the running
calibration files); close unwanted calibration macros: ”close
20130624WuYuHan 出國報告書
(“LR-TaL3_TaL2……cal (file name)”)”; “p LR_E”(show the
low resolution energy of beam from DCM)
3. Load old calibration file with the energy range near the
energy to run the experiment: “ls *.cal” (show the calibration
files in the folder); “qdo_LR…….cal (file name)” (recall the
calibration file); “Load_File_Cal“ if necessary; BOS will
show the beamline operation status;
4. Set gains if necessary: “gt”(read the gain and suppress
current); “keithley_set_gain 16 3” (set gain at 3 of the no.6
Keithley); set suppress current to reduce dark counts::
“keithley_set_supress 1320.2;ct” try the other current values
to check the counts; use “umv wheel 6;ct” or the other
attenuator to reduce the intensity of direct beam;
5. Optional: change the two pairs of channel cuts
(high-resolution monochromator, HRM) inside the He gas box
of experimental hutch2. The HRM consists of high-precision
co-axial goniometers to form various combinations of
2-bounce or 4-bounce (inline or nested) channel-cut crystals.
After remove the box cover and crystals, “umv cg1th1 0
cg2th1 0”; “umv cg1dth1 0 cg2dth1 0”, where dth1 for coarse
th angle adjustment and th1 for fine th angle adjustment. Then,
mount the new crystal to be used. Crystals with a larger gap
exhibit a higher resolution. Remember to check the horizontal
level of the crystals. The crystal surface should be aligned.
6. Move away channel cuts: “move cg1z 12”; “move cg2z
12” to do alignment and low resolution energy calibration;
7. Move cylindrical collimating mirror (CM) to the suitable
position. CM with partly-coated Pt layer also functions as a
higher-order light filter. Si (regions without coating) and Pt
for the energy ranges of 5 ∼ 12 (or 10) keV (“move_CM_x
10”) and 12 (or 10) ∼ 30 keV (“move_CM_x -10”),
respectively;
20130624WuYuHan 出國報告書
8. Establish a new file: “new file alignement_25Oct2013”;
9. Scan the parallel of Si (111) double-crystal
pre-monochromator (DCM):”psp PN1”; “DCM_dth1rscan
1000 20 1”; “move _DCM_dth1 PK (CEN)”; If the motor of
dth1 of DCM does not work properly, try to use dth2 of DCM.
Note that change dth2 of DCM will also change the energy. If
the energy is calibrated and fixed, scan the DCMpiezo to
adjust the angle;
10. Scan the height of CM if necessary: “wm s1up
s1dn”;”umv s1up 3 s1dn3”; “CM_zrscan 1 20
1”;”move_CM_z CEN (PK) ”;
11. Align slit 1: “umv s1up 0.1 s1dn 0.1” (close the vertical
direction of slit1 if necessary);“dscan s1z -2 2 40 0.5”;”umv
s1z CEN”; “umv s1up 0.5 s1dn 0.5” (open the vertical
direction of slit1); “umv s1h 0.1 s1r 0.1” (close the
horizontical direction of slit1 if necessary);”dscan s1x -2 2 40
0.5”; “umv s1x CEN”; ”umv s1h 1.5 s1r 1.5”; slit 1 is more
critical than FM slit and JJ slit; the latter two are usually
opened wider;
12. Stick a burn paper after HRM to check the position of the
beam;
13. Scan the focusing mirror: “PSP pn4”; ”wm kup kdn kr
kh”; “umv kup 4 kdn 4”(if necessary); ”FM_zrscan 1 20 1”;
“move_FM_z CEN”. After the HRM and the PRP, the beam is
delivered to the Pt-coated focusing mirror and focused both
vertically and horizontally to ∼ 80 (V) × 120 (H) µm2.
14. Align Kohzu slit: ”psp PN5”; ”wm kup kdn kr
kh ”; ”umv kup 0.05 kdn 0.05”; ”dscan kz -1 1 40 0.5”; “umv
kz CEN (PK)”; “umv kup 0.3(0.1) kdn 0.3 (0.1)”; “umv kr 0.1
kh 0.1”; ”dscan kx -1 1 40 0.5”; “umv kx CEN”; “umv kup 3
kdn 3 kr 3 kh 3”(open the slit if necessary);
20130624WuYuHan 出國報告書
15. Align JJ slit: “umv wheel 0;ct”; “umv jjup 0;ct”; “psp
PN5”; “dscan jjup -2 2 40 0.5”; “umv jjup 1.3 (position to
go);ct“; “set jjup 0”; “umv jjup 3”; “umv jjdn -1.3;ct”; “dscan
jjdn -2 2 40 0.5”; “umv jjdn (position to go)”; “set jjdn 0”;
“umv jjdn 3”; “umv jjh 0”; “dscan jjh -2 2 40 0.5”; “umv jjh
-0.9 (position to go);ct”; “set jjh 0”; “umv jjh 3”; “umv jjr
0.9;ct”; “dscan jjr -2 2 40 0.5”……;
16. Align the aperture (exit slit) before sample: ”psp PN6”
(without a sample, the intensity should be ~ 1000000 counts/s;
check towerz to see if the intensity changes) ”dscan esz -1 1
40 1”; “umv esz CEN”; “dscan esx -1 1 40 1”; “umv esx
CEN” (the position of half intensity); “umvr towerz -0.1;ct”
(to cut a half intensity?)
17. To adjust the vertical and horizontal focus mirror to reach
the maximum intensity: vertical VTL and horizontal HTL?:
“timescan”
18. Insert a pin on the sample holder and use the auto level
outside the hutch to check the position of the tip of pin;
change towerz and ccy to move the pin tip to the center of
crosshair (e.g.: ”umvr towerz 1”; “umvr ccy -1”); rotate phi
180 and 90 degree to check it again;
19. Use the auto level at the end of beamline to check the
position of tip of pin: “umvr ccx 1”; “umvr towerz -0.1”;
20. Scan sample holder position: “dscan ccx(ccz, ccy) -0.1
0.1 80 0.5”; “umv towerx 0;ct”; ”dscan towerx – 2 2 20
0.5”; ”umv towerx MN (minima)”; “dscan towerz -0.4 0.4 40
0.5”; “umv towerz MN”;
21. Energy calibration of the beam from monochromator:
(1) Put a standard metal foil to be measured in the sample
holder; “Keilthley_set_gain 17 6”; “umv wheel 3;ct”;
“p_LR_E”; “mv_LR_E 9881;ct”; “psp PN7”(set a pin diode
20130624WuYuHan 出國報告書
near the standard metal foil at first); “LR_Escan 9981+30
9981-20 10 1”(a rough scan to see if the edge shows up; check
the count rate to avoid the saturating); “LR_Escan 9981+30
9981-20 100 1” (fine scan; check if the count rate is suitable);
“mv_LR_E 9983.57;ct”(move the energy to the peak of
derivative of the edge, or inflection point of edge jump);
(2) Scan undulator gap: “UGscan 21.56 21.16 40 1”(+0.2 and
-0.2 of the original value); “move_UG PK”;
“Write_Cal_File_Part1” (LR=0, HR=1, input file name, for
example: LR_TaL3_TaL2_25Oct2013.cal; input reference
value of edge position and the angle of DCM from the
beamline terminal computer);
(3) Calibrate another absorption edge (change to another
standard metal foil if necessary): “mv_LR_E 11636+30;ct”;
“LR_Escan 11636+30 11636-20 10 1”; “LR_Escan 11636+30
11636-20 100 1”; “mv_LR_E 11636.5;ct”(move the energy to
the peak of derivative of the edge or inflection point of edge
jump);
(4) Scan undulator gap: “UGscan 21.52 21.12 40 1”(+0.2 and
-0.2 of the original value); “move_UG PK”;
“Write_Cal_File_Part2” (LR=0, HR=1, input file name, for
example: LR_TaL3_TaL2_25Oct2013.cal; input reference
value of edge position and the angle of DCM from the
beamline terminal computer);
(5) Load the calibration file into memory: “ls *.cal”; “qdo
LR_TaL3_TaL2_25Oct2013.cal (file name)” (recall the
calibration file); “Load_Cal_File”; “p LR_E”
(6) Return to the first absorption edge to confirm the energy
position again (change back to the previous standard metal
foil if necessary): “mv_LR_E 9981+10”; “LR_Escan 9981+10
9981-10 40 1”;
22. Align the parallel of HRM crystals on the beam:
20130624WuYuHan 出國報告書
(1) The first set of channel cut: “wm cg1z cg2z cg1x
cg2x”; ”umv cg1z 0”; “psp PN2”; ”dscan cg1z -2 2 20
0.5”; ”umv cg1z (half intensity)”; “set cg1z 0” “dscan cg1dth
-2 2 20 0.5”; “umv cg1dth PK”; “dscan cg1dth -1 1 40 0.5”;
“umv cg1dth PK”; “set cg1dth 0”; “dscan cg1z -1 1 40 0.5”;
“umv cg1z (half intensity)”; “set cg1z 0”; ”dscan cg1x -10 10
40 0.5”; ”umv cg1x CEN”; “set cg1x 0”;
(2) The second set of channel cut: “umv cg2z 0”;“umvr cg1z
2”; “psp PN3”; ”dscan cg2z -2 2 20 0.5”; ”umv cg2z (half
intensity)”; ”dscan cg2dth -2 2 20 0.5”; “umv cg1dth PK”;
“dscan cg2dth -1 1 40 0.5”; “umv cg2dth PK”; “set cg2dth 0”;
“dscan cg2z -1 1 40 0.5”; “umv cg2z (half intensity)”; “set
cg2z 0”; ”dscan cg2x -10 10 40 0.5”; ”umv cg2x CEN”; “set
cg2x 0”; “umv cg1z 0”
23. Rotate the channel cut crystal: calculate the Bragg angle
of
channel
cut:
for
Si(333):
“p
deg(asin(12.398/11.215/2/5.4308*sqrt(27))” (=31.222); “umv
cg1dth -31.222” (counterclockwise); “umv cg2dth 31.222”
(clockwise); “BOS”(show the energy pass through channel
cut); “p HRM_H”; “p HRM_K”; “p HRM_L” (change hkl to
333)
24. Find the reflection beam of HRM (very narrow in
FWHM) : insert a Scotch tape at the sample position; “umv
wheel 4(5);ct”; ” “dscan cg1dth -1(0.5) 1(0.5) 400(200) 0.2”
(rough scan of th angle);”umv cg1dth PK”. If there are two (or
more) peaks (due to different reflection), check both (all) of
them (if necessary). In general, we may try the stronger one at
first. Only the right reflection beam can reach the sample.
“dscan cg1th1 +30 -30 40 0.5”(fine scan of th angle); “umv
cg1th1 CEN”; “dscan cg1dchi -4(-2) 4(2) 40 0.5”(go to the
region between two peaks); “dscan cg1th1 +5 -5 40 0.5”;
“umv cg1th1 CEN”; “dscan cg1dchi -2 2 40 0.5”; ”umv
cg1dchi CEN”. For the second crystal, the same procedure
20130624WuYuHan 出國報告書
can be followed: “dscan cg2dth -1 1 800 0.2”; ”umv cg2dth
PK”; “dscan cg2th1 +20 -20 40 0.5”; ”umv cg2th1 CEN”;
“dscan cg2dchi -2 2 40 0.5”; ”umv cg2dchi CEN”; “dscan
cg2th1 +5 -5 40 0.5”; “umv cg2th1 CEN”; ”ct”; calculate the
transmission ratio of reflection beam (reasonable value: ~1%)
25. “BOS” to show the energy from HRM crystals and tune
the energy into the calibrated energy: ”set cg2dth 3.19……”;
“set cg2th1 ……”; “Write_Cal_File_Part1” (HR=1, input file
name, for example: HR_Si333_11215_26Oct2013.cal);
26. Move LR energy to HR energy by moving cg1th1 and
cg2th1. It should be noted that change the set value of cg2th1
will shift the energy while cg1th1 can be reset as 0;
27. Scan post-sample slit (for NIXS) : “umv wheel 7”;
“mv_LR_E EE (elastic energy)”;”psp det”;“dscan psx -4 4 40
0.5”; “umv psx PK”; “dscan psz -4 4 40 0.5”; ”umv psz CEN”
28. For NIXS, scan the analyzers to be used. Find the achi1
(or the other no.) and set its peak or center as zero at first.
Then, scan ath1 (or the corresponding no.) and move it to
center. Finally, scan achi1 again, move it to center and set
achi1 and ath1 as zero. To scan next analyzer, move achi1 (or
the other no. just aligned) to +0.5 and check the position of
achi2 (or next no.) of next analyzer. Move achi2 to zero. For
example, “dscan achi1 -0.2 0.2 40 0.5”; “umv achi1 CEN”;
“set achi1 0”; “dscan ath1 -0.1 0.1 40 1”; “umv ath1 CEN”;
“dscan achi1 -0.1 0.1 40 0.5”; “umv achi1 CEN”; “set achi1
0”; “set ath1 0”; “umv achi1 0.5”; “wm achi2”; “umv achi2 0”;
“umv wheel 3;ct”; “dscan achi2 -0.2 0.2 40 0.5”; “umv achi2
PK”; “umv wheel5;ct”; “dscan ath2 -0.2 0.2 40 0.5”; “umv
ath2 CEN”; dscan achi2 -0.1 0.1 40 0.5”; “umv achi2 CEN”;
“set achi2 0”; “set ath2 0”; “umv achi2 0.5 achi3 0”; “dscan
achi3 -0.2 0.4 40 0.5”…… For the analyzer no.>5, it is a good
idea to move ath5 (or 6-9) -0.1 degree (relatively) to find
20130624WuYuHan 出國報告書
achi5 (or 6-9); “dscan dz -2 2 40 0.5”; rescan DCMdth1rscan,
psx, psz, esx, esz, towerx or towerz are often necessary during
NIXS alignment process;
29. Measure elastic line: LR_Escan (initial energy) (final
energy) (No. of points) (counting time); ”EE=CEN”; “pplot”;
measure inelastic features: “mv_LR_E (initial energy)”; “umv
wheel 0”; LR_Escan EE+402 (initial energy) EE+2 (final
energy) 200 (No. of points) 2 (counting time);
30. For RIXS, scan dth1 (most sensitive), dth2(optional) and
check ay and dy to set up the Rowland circle (radius=1 m or 2
m)
31. Turn on the DCM piezo in another window during
measurement; it will optimize the intensity.
四、心得概述與建議
I did not have much experience to go to Spring-8 to run
experiments like inelastic X-ray scattering experiments or
hard X-ray photoelectron spectroscopy when I was a student.
As a result, I am not quite familiar with these two kinds of
material characterization techniques before. It is a nice
chance for me to learn more analytical methods at the most
brilliant synchrotron source. I shall try to learn them more
completely and quickly during the limited beamtime. It
would be better if a new employee can receive some suitable
documents to learn or the senior ones could delivery their
knowledge slowly and patiently. Moreover, we should try to
encourage more domestic users to try to do the inelastic
scattering experiments. For now, the numbers of users of
BL12XU from Taiwan are still limited within a few groups.
There would be good chances to promote this beamline at
the international conferences, like the “HAXPES 2015”,
20130624WuYuHan 出國報告書
hold by NSRRC.
註：
1. 本報告須於回國後 30 日內上網繳交，文字篇幅約 2~4 頁。
2. 回國後之口頭報告可為附件，但不得替代報告本文。
20130624WuYuHan 出國報告書