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Rigaku Smart Lab X Ray diffractometer operation

procedure.

Ragesh Kumar T P
Project Fellow
Department of Physics
Indian Institute of Science, Bangalore, India.

1) Switching ON the machine


Before starting the instrument check water supply from the chiller and its temperature. Make
sure that temperature is below 22, if not wait till the time. If chiller condition is perfect, switch
on the power supply to the Rigaku XRD instrument. Now the instrument is ready for Switching
ON, for switching ON the instrument press green button located in the bottom right corner of the
instrument, which is shown in the fig 1.1, make sure that ON button lights up. If the instrument is
properly switched ON an OPERATE lamp will lights up in green. After switching ON the
instrument, high voltage supply to the X ray tube should be enabled, for that rotate the High
Voltage enable key in clock wise direction for a few seconds. Now the X ray tube is ready for
producing X rays.

Figure 1.1 Power switch and High Voltage enable key.

Open Rigaku smart lab guidance software from the desktop of the system. The login name for
the software is administrator and there is no password for the software. In the top left side
corner of the software, there are two options START UP and SHUT DOWN, which is shown in
the fig 1.2. For starting the aging process and switching on the X ray tube, click START UP,
then a small dialogue box will appear and click EXECUTE option in the dialogue box, it will
slowly increase the current and voltage. If we are not giving any value to current and voltage, X
ray tube will attain standard 40KV voltage and 30mA current. If we gave any specific value for
current and voltage, it will slowly attain that particular value. The time required for attaining that
current and voltage will show in the left bottom corner of the window, which is shown in the fig

1.3. Now the X ray tube is ready for any kind of measurement. After attaining sufficient current
and voltage wait some 10 minutes before starting any measurement.

Figure 1.2 Dialogue box for starting up the instrument.

Figure 1.3 Dialogue box showing the time required for turning ON the X rays.

2) Various kinds of measurements possible in the Rigaku smart lab X ray diffractometer.
2.1)

Normal powder X ray diffraction


From the TASK option at the top side of the software, take PACKAGE

MEASUREMENT option, in the different packages click GENERAL MEASURMNET.


General measurement contain several options like General (Bragg-Brentano focusing), General
(Bragg-Brentano focusing) D/tex, General (Medium resolution PB), General (High resolution
PB-Ge[220]2) e.t.c. For normal powder X ray diffraction choose General (Bragg-Brentano
focusing) option, which is shown in the fig 2.1. In the case of BB (Bragg-Brento focusing)
mode, X ray beam will be diverging kind. The optics for the BB mode is shown in the fig 2.2.

Figure 2.1 Choosing different measurement packages from Package Measurement option.

Figure 2.2 Optics of Bragg Brentano focusing X ray.

If we click General (Bragg-Brentano focusing), three different steps (Optics alignment (BB),
Sample alignment and General measurement) will appear in the left middle side of the software,
which is shown in the fig 2.1. Before starting any alignment or BB measurement, the mode of the
instrument have to change into BB by inserting BB selection slit. How to change BB selection
slit is shown in the fig 2.3 (a). Length limiting slit of 10mm also have to insert along with BB
selection slit, which is shown in the fig 2.3 (b). Once we have inserted the BB selection slit and
length limiting slit, start the optics alignment.

Figure 2.3 (a) changing to Bragg-Brentano mode for General BB measurements. b) Inserting of 10 mm
length limiting slit.

If we click on optics alignment, a small OPTICS ALIGNMENT (BB) dialogue box will
appear, uncheck print result for avoiding unnecessary printing of result and then execute it by
clicking execute, which is shown in the fig 2.4. It will ask to insert center slit, which can be
inserted as shown in the fig 2.5. If we inserted it properly and fixed at appropriate position,
instrument will start optics alignment. The various kind of optics alignment performed by the
instrument can be seen in the software. A

mark will start blinking near OPTICS

ALIGNMENT (BB) during the alignments; it will stop only after finishing the optics alignment.

Figure 2.4 Dialogue box showing optics alignment.

Figure 2.5 Inserting the center slit.

Figure 2.6 Dialogue box asking to insert center slit

The main alignments performing in optics alignment are omega alignment, Theta_d alignment,
Theta_s alignment, Zd, and Zs alignment e.tc, which are shown in the fig 2.7. The omega
alignment will take care about the bending of X ray beam. For the omega alignment, source and
detector will move simultaneously, so that it will get a maximum peak position at which the
upper surface of the slit and X ray beam would become parallel. The source arm and detector
arm will move simultaneously to the selected peak position after the omega scan. During the
Theta_d and Theta_s alignment, detector and source angle will adjust, so that it will get
maximum intensity and move the source arm and detector arm to the selected angle. It takes
about 10 minutes for the optics alignment to complete.

Figure 2.7 Various optics alignments.

After finishing optical alignment, we can go for SAMPLE ALIGNMENT (BB). Click on
sample alignment, a dialogue box Sample Alignment (BB) as shown in the fig 2.8 will appear.
Chose the option use the height reference sample plate (no height alignment) for powder
kind of samples and start the alignment by clicking execute, it will complete in few minutes.
Uncheck print alignment result for not printing the results. For flat pellet kind of sample choose
Flat sample alignment option and put the approximate sample thickness. If we execute sample
alignment, it will ask to load samples. How to load powder kind of sample is demonstrated in the
fig 2.9 (a) and fig 2.9 (b). Placing pellet kind of sample in disc shaped sample mount is shown in
the fig 2.10 (a). The fig 2.10 (b) will give the idea about loading the flat kind of sample. For flat
kind of samples, instrument has to perform omega and z alignments, it will take about 10 minute
to complete sample alignment for flat kind of sample. If we are choosing customize conditions in
the sample alignment (BB), it is possible to set range of scanning and its speed by setting
appropriate values. Sample alignment will come good in recommended values itself. Once the

sample alignment finishes, blinking of

mark will stop and we can proceed with GENERAL

MEASUREMENT (BB). Before starting General Measurement (BB), insert Kb filter for
filtering out Kb X rays. The way to insert Kb filter is shown in the fig 2.11.

Figure 2.8 Sample Alignment dialogue box.

Figure 2.9 (a) Filling powder kind of samples in sample plate, b) loading powder sample to the
instrument.

Figure 2.10 (a) loading powder kind of samples, b) placing pellet or film kind of samples c) loading pellet
sample in the instrument.

Figure 2.11 Inserting Kb filter to remove Kb X rays.

Select General Measurement (BB) for starting the measurement. A dialog box will open
for General Measurement. In the dialog box we can set the folder directory for saving the result.
Click read current slits; it will read the slit that we are inserted for the measurement. In the scan
axis select Theta/2-Theta for normal X ray diffraction measurement, select mode as continuous,
Range absolute. The rest of the parameter like range and speed can be set according to our
convenience. The time to be taken for the total measurement will show at the bottom side of the
software. The measurement can be split into different parts by selecting 1, 2, 3, 4, e.tc options
and set the range accordingly. These entire things are shown in the fig 2.12. If the ranges and
parameters are properly set, start the measurement by clicking execute.

Figure 2.12 General Measurement (BB) dialogue box.

3)

Thin film X ray diffraction with medium resolution


From the different measurement packages select General (medium resolution PB) as

shown in the fig 3.1. For the PB mode, shape of the X ray beam will be parallel. The optics used
for PB mode is shown in the fig 3.2.

Figure 3.1 Selecting General Measurement (medium resolution PB).

Figure 3.2 Optics of Parallel beam mode.

If we select General (medium resolution PB), three conditions (Optics alignment (PB), Sample
alignment, and General Measurement) will appear in the left middle side of the window. As
discussed previously, insert centre slit and start optics alignment. All the alignments for PB
optics alignment are same as that in BB mode, the only thing we need to do is inserting PB
selection slit.

Before starting the sample alignment, place the sample carefully on a disc shaped sample mount.
Fig 3.3 (a) and (b) shows how to place the sample on the disc and attaching to the instrument.
Make sure that K b filter is removed for sample alignment. If we place the sample properly and
mounted correctly, click on the sample alignment. A dialogue box as shown in the fig 3.5 will
open for setting the sample dimensions. Put the approximate sample thickness, sample width and
sample height in nm. Fig 3.4 shows the way to put sample width and sample height.

Figure 3.3 (a) placing the film sample in the disc shaped sample mount, b) attaching the sample mount
to the instrument.

Figure 3.4 sample dimensions.

Figure 3.5 Dialogue box showing Sample Alignment.

If the thickness of the coated sample (excluded substrate) is very less, choose Alignment criteria
as precise and surface density as high. After setting all the parameters in the dialogue box,
execute it and start the alignment. Main sample alignments are omega for tilt in the sample, z for
height alignment, which is shown in the fig 3.6. Once the sample alignments are completed, the
blinking of mark

will stop and can be proceed further with General measurement (PB).

In the General Measurement, a dialogue box will open. Set the folder directory for
saving the measured data. Click read current slits for reading the current slit widths. Select scan
axis as Theta/2-theta, mode continuous. Set appropriate range, step, speed and other slit widths.
Fig 3.7 shows the dialogue box. After setting all the parameters, we can start the measurements
by clicking execute, then the blinking of

will start.

Figure 3.7 Dialogue box for General Measurement PB.

4)

Thin film X ray diffraction with high resolution

For high resolution thin film X ray diffraction measurement, select General (high
resolution PB-Ge(220)2) from the General measurement packages. Three conditions will
appear, Optics Alignment (PB-Ge(220)2), Sample Alignment and General Measurement as
shown in the fig 4.1.

Figure 4.1 Selecting General Measurement (high resolution PB) package from General Measurement
packages.

Insert center slit and start the Optics Alignment. The way of inserting center slit has shown in the
fig 4.2 (a) and (b). After inserting the center slit, click on OPTICS ALIGNMENT, a dialogue
box will open as shown in the fig 4.3. Starts the optics alignment by clicking execute option in
the dialogue box. It will do the same optics alignment as discussed earlier. The blinking of
mark corresponds to Optics Alignment is indicating the progress of Optics Alignment. Once the
optics alignment has finished, the blinking of

mark will stop and we can proceed further with

Sample Alignment.

Figure 4.2 (a) and (b) inserting center slit.

Figure 4.3 Dialogue box showing Optics Alignment (PB-Ge(220)2)

Before starting the SAMPLE ALIGNMENT, place the sample carefully on disc shaped
sample plate as shown in the fig 4.4 (a) and (b). Vaccume greese can be applied for fixing the
sample properly on the disc shaped sample plate. If the sample is fixed properly, take disc shaped
sample plate and mount it to the instrument as shown in the fig 4.4 (b).

Figure 4.4 (a) placing the sample on disc shaped sample mount, b) attaching the sample mount to the
instrument.

Once we have mounted the sample, click on SAMPLE ALIGNMENT. A dialogue box will open
for setting the sample dimension and starting the sample alignment. Put appropriate sample
thickness, sample width and sample height in mm. If the sample thickness is very less (excluding
substrate) choose alignment criteria as precise and Surface density as High. It will increase the
accuracy of sample alignment for very thin samples. Fig 4.5 shows an example of sample
alignment dialogue box. If we executed the sample alignment, a dialogue box as shown in the fig
4.6 will open and ask to insert sample. Since we already inserted the sample, click ok to continue
the sample alignment. Major sample alignments are z alignment and omega alignment, the
details about z alignment and omega alignments are discussed previously.

Figure 4.5 Dialogue box showing Sample Alignment.

Figure 4.6 Dialogue box asking to mount the sample.

The stopping of

mark will indicate the completion of sample alignment. Now the sample is

aligned properly and we can proceed to General Measurement for starting the measurement. If
we click on the General measurement a big dialogue box will open as shown in the fig 4.7. In
the dialogue box set folder directory for saving the measured data. Click on Read current slits, it
will read the current values of slit widths. Set the scan axis as Theta/2-Theta, mode is
continuous. Set appropriate range and speed of scan. We can split one full scan into number of
scans by checking 1, 2, 3, e.t.c. if we click drive 4 axis to the current zero position after the
measurement completed, all the axis like 2-Theta, Z, Omega, Phi will come to zero position
after the measurement.

Figure 4.6 Dialogue box for performing General Measurement.

5)

Reflectivity measurements of thin film sample.


The reflectivity measurement can be done in two different ways, one is using film

thickness analysis package and the other is using General measurement packages.

5.1)

Reflectivity measurement using Film Thickness Analysis packages.


If we are using medium resolution mode, select Reflectivity (medium resolution PB)

from Film Thickness analysis packages as shown in the fig 5.1.1. Upon the selection, optics
alignment, sample alignment and Reflectivity Measurement will appear in the left bottom side
of the window. Select optics alignment for initial alignment of the instrument. After inserting the
center slit, execute optics alignment as shown in the fig 5.1.2. Various kinds of alignments like
Theta_d, Theta_s, Zd, Zs, 2-Theta will perform during the optics alignment. Once finishes the
optics alignment blinking of
alignment.

mark will stop and we can proceed further with sample

Figure 5.1.1 Selecting Reflectivity (medium resolution PB) from Film Thickness Analysis packages.

Figure 5.1.2 Optics alignment dialogue box.

In the sample alignment, place the sample on a disc shaped sample plate and mount on the
instrument as discussed previously. If the sample is properly mounted, execute sample alignment
as shown in the fig 5.1.3.

Figure 5.1.3 Sample Alignment dialogue box.

If the sample alignment is completed, blinking of

mark will stop and can be proceed further

with Reflectivity Measurement. Open the Reflectivity measurement dialogue box by clicking the
Reflectivity Measurement, which is shown in the fig 5.1.4. Select the folder directory for saving
the measured data. For customizing the measurement conditions, click on customize conditions.
If we click on customize conditions customize Reflectivity Measurement dialogue box will
open. Fig 5.1.5 displays the customize Reflectivity Measurement dialogue box. If we dont
need a pre measurement, uncheck pre measurement conditions in the dialogue box. In the data
measurement conditions, we can set the starting, stoping range of scan, scan speed, and scan step
e.t.c. According to the given scan speed, it will show the total time needed for entire scan in the
bottom side of the dialogue box. After setting the scan speed, step size and other parameters
close the dialogue box and return to Reflectivity Measurement dialogue box. For starting the
reflectivity measurement click execute in the Reflectivity Measurement dialogue box. If we need
a pre measurement before starting the actual measurement, click on pre measurement conditions
in the customize Reflectivity Measurement dialogue box. The range of pre measurement, step
size and speed of the scan can be set in the pre measurement conditions by putting appropriate
values. During the reflectivity measurements it will first show pre measurement plot and
followed by actual measurement. The blinking of
completed.

mark will stop if the measurement is

Figure 5.1.4 Reflectivity Measurement dialogue box.

Figure 5.1.5 Customizing conditions in Reflectivity Measurement.

5.2) Reflectivity measurement using General measurement packages.


From the General Measurement package select General (medium resolution PB) and do
the optics alignment and sample alignment as discussed in General Measurement (medium
resolution PB) X ray diffraction. After finishing the optics alignment and sample alignment open
the General Measurement dialogue box as shown in the fig 5.2.1. Select the folder directory for
saving the reflectivity measured data. Click on read current slits for considering the current slit
widths. Select scan axis as 2-Theta/Omega for reflectivity measurement, the other changes

needed for reflectivity measurement are adjusting Incident (IS) and receiving (RS1, RS2) slit
widths. Change the incident slit (IS) width to 0.1, receiving slit 1 (RS1) width to 0.2, and second
receiving slit (RS2) width to 0.4. Select the attenuator as auto. The total measurement can be
split into different parts and set the according scan speed and step sizes in each parts. Time taken
for full scan will show in the bottom side of the dialogue box. After setting all the parameters,
click execute and start the measurement.

Figure 5.2.1 General Measurement dialogue box for Reflectivity measurement.

6)

Powder X ray diffraction measurement using D/teX Ultra detector.


Rigaku Smart lab X ray diffractometer have two detectors, one is scintillation counter

and the other one is D/teX Ultra detector. D/teX Ultra detector is normally using for powder
sample X ray diffraction study.
6.1)

Changing the scintillation counter into D/teX Ultra detector


The first step for changing the detector is removal of +ROD adaptor from the detector

arm, how to remove +ROD adaptor is shown in the fig 6.1.1 (a). Remove the cable
corresponding ROD adaptor, and loose the screw of ROD adaptor as shown in the figure. Then
lift the ROD adaptor upward and place it carefully in a safer position. After removing the ROD

adaptor move RPS adaptor, standard receiving slit#2 and standard attenuator towards sample
position as shown in the fig 6.1.1 (b).

Figure 6.1.1 (a) Removing +ROD adaptor, b) Moving of RPS adaptor, Standard receiving slit box #2, and
standard attenuator towards sample side.

Once it moved towards sample position, remove the Scintillation counter by loosing the screw as
shown in the fig 6.1.2. Pull the scintillation counter towards our side after loosen the screw.
Cover the Beryllium window of the counter with its cover and place it carefully in a safer
position.

Figure 6.1.2 Removing Scintillation counter.

Remove the cover of beryllium window of D/teX Ultra detector and make it ready for
installation. If we removed the scintillation counter carefully, fix the D/teX Ultra detector as
shown in the fig 6.1.3. Tighten the screw of D/teX Ultra detector and make sure that the detector
is fixed properly. If we fixed everything properly, the detector arm will look like fig 6.1.4.

Figure 6.1.3 Installing D/teX Ultra detector.

Figure 6.1.4 Detector arm after installing the D/teX Ultra detector.

Update the hardware using smartlab guidance software. Select General (Bragg-Brentano
focusing) D/teX from General Measurement packages, which is shown in the fig 6.1.5.

Figure 6.1.5 Selecting General (Bragg-Brentano focusing) D/teX from the General Measurement
packages.

Perform the optics alignment as discussed previously. Select D/teX Detector center correction
for detector alignment. A dialogue box will open for detector alignment as shown in the fig 6.1.6.
Select use direct beam for detector center correction. There is an option for customizing the
scan conditions, if it needed put appropriate scan speed and range.

Figure 6.1.6 Dialogue box for detector center correction.

After the detector center correction alignment, start Sample Alignment. The sample alignment is
same as we discussed previously for General (Bragg-Brentano focusing) X ray diffraction.
After sample alignment, go for General Measurement (BB). Open the dialogue box for General
Measurement, set the folder directory, scan range slit width, scan speed e.t.c. If we put every
parameter correctly, starts the measurements by clicking execute as shown in the fig 6.1.7.

Figure 6.1.7 Dialogue box for General Measurement (BB) using D/teX Ultra detector.

7)

Changing Z-Phi stage into Alpha-Bheta or Chi standard stage.


In Z-Phi stage, Z and Phi movement only permissible. For some kind of measurement

like Reciprocal space mapping, Chi movement is necessary. The Phi and Chi movement is
described in the fig 7.1. For enabling Chi movement, Alpha-Beta or Chi standard stage have to
install. For removing the Z-Phi stage, detach the cable carefully as shown in the fig 7.2.

Figure 7.1 Chi and Phi rotation of the sample

Figure 7.2 Detaching the cable for removing Z-Phi stage.

Z-Phi stage is attached using a single screw, loose the single screw for removing the Z-Phi stage,
how to loose the screw is shown in the fig 7.3. Loose the screw to some extend and lift the Z-Phi
stage gently upward. Release the stage from the triangular slot; keep it carefully in a safer place.

Figure 7.3 Removing of Z-Phi stage by loosing the screw.

Take the Chi stage and attach to the instrument as shown in the fig 7.4 (a). Tight the screw using
screw driver and make sure that the stage is attached properly. After tighten the screw, connect
the Chi stage cable to the port as shown in the fig 7.4 (b). Update the hardware status in the
Rigaku Smartlab software.

Figure 7.4 (a) Attaching the Chi stage, b) connecting the Chi stage cable.

8)

Switching OFF the instrument


Open the Rigaku Smartlab software for switching OFF the X ray diffractometer. Click

on SHUT DOWN, a small dialogue box will open as shown in the fig 8.1 and execute it by
clicking execute. Within some few minutes, X ray tube will turn off. Wait for some 20 to 30
minutes and switch off the water supply from the chiller also. Press the white color power OFF
button as shown in the fig 8.2, it will power off the instrument.

Figure 8.1 Dialogue box for shutting down the instrument.

Figure 8.2 Power OFF button of the instrument.