Jonathan Cardoso

49 Symphony Road Apt. 2

Boston, MA 02115

14 October 2018

Dr. Suzanne Romaine

Research Physicist - HEA
Harvard-Smithsonian Center for Astrophysics
60 Garden Street
Cambridge, MA

Dear Dr. Romaine:

Hard x-ray optics are designed to record exterior features of a planet by grazing incident high
energy x-rays upon the surface of the optic, like a telescope. During my summer at Harvard characterizing
highly refined optics, x-ray reflectometry (XRR) was a common mechanism of measurement. XRR, a
surface sensitive scattering technique used to reflect upon, and within, multilayer optics, is paramount in
producing accurate space ready optics. I have familiarized myself with the setup through guided
instruction from the only existing staff member with XRR operating capabilities, repeated independent
usage, and extensive modeling of the resultant scans.
Unfortunately, our current system has extremely minimal documentation. Commands lines given
to the computer by the user during operation do exist, but the literature is woefully incomplete. The list of
handwritten command lines with no context or explanation prepare the operator only for idyllic scenarios
where following line-by-line execution is sufficient. No basic information is given on (1) how our XRR
works, (2) what the commands do, and (3) what to expect as a result. It is virtually impossible to conduct
accurate scans without extensive prior first-hand experience with similar XRR setups, precisely loading,
manipulating degrees of freedom, and aligning a sample.
I hope this “Operating Manual for XRR” can curb this learning process for subsequent students
and fill gaps in knowledge of Harvard unique XRR motor setup. I believe this should be laminated and
placed in the XRR lab room as a guiding resource for future students. If you have any questions or
concerns regarding the guide, please feel free to contact me via email. Thank you for taking the time to
review and consider this reference document.

Sincerely,

Jonathan Cardoso
Physical Science Technician
cardoso.jo@husky.neu.edu
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Operating Manual for XRR

Jonathan Cardoso

Abstract

This guide will provide the broad steps for getting started in XRR. While the steps are
laid out in sequential order care should be taken to understand the purpose and results
of each step, ensuring the individual characteristics of the sample are not overlooked.
The terminology in the guide will be as follows:

+ or ’ ’ indicates a direct command line to be given to the XRR computer. Bold red
lettering indicates a result or note that must be recorded in the lab notebook, but the
list is not absolute and extra pertinent information can and should be provided.

I. SLITS AND DEGREES OF FREEDOM

In our reflectometer a CuKα x-ray radiation source is monochromatized by a germanium crystal. The
exiting beam is then collimated by a series of slits in order to minimize divergence. The electron
emissions in the x-ray tube carry with them a Kα1 and Kα2 spectral line. Slit widths are chosen in order to
ensure only the strongest portion of the beam, Kα1, is present during the reflectivity tests. The focused
beam is incident at a small graving angle upon the sample attached to a goniometer. This goniometer
carries a number of degrees of freedom in order to align the sample’s deposited surface with the beam’s
center. Once the sample is aligned measuring the reflectivity across a series of graving angles is achieved
by engaging a stage motor to push the tail end of the sample. Controlling this incident angle θ allows for
the generation of reflectivity curves (reflectivity as a function of graving angle) to be modeled for an
estimation of the deposited films’ thickness, densities, roughness, etc. According to the law of reflection
at the same time the detector must sweep out an angle 2θ to intercept the reflected x-ray beam. The
detection of nonspecular radiation is reduced by placing a slit directly before the face of the detector. This
setup can be found in Fig 1.
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Certain motors such as phi and slit 3 commonly go unchanged unless faced with major misalignment or a
recalibration. Other motors are repeatedly changed during the sample loading and alignment process. A
read out of the current motor positions can be found by using the command ’wa’, one is included for
reference. The first and second row under each variable name represent the currently set and absolute
positions. Some motors are slits, or shutters, with a left (l) and right (r) side that act independently.

Figure 2: Table displayed when program is given the where all command ‘wa’

Figure 3: Goniometer Degrees of Freedom

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II. MOUNTING SAMPLES

While mounting a sample is a small amount of time in relation to the duration of a long scan, it is by far
the most vital. An incorrectly mounted sample can waste a 20-hour scan if the tape begins to peel or the
sample was never flat against the holder in the first place.

1. Close slit 2 to protect yourself from x-ray radiation. ‘mv’ denotes the command to move.

+ mv sl2r 0.1
+ mv sl2l -0.1

2. Begin by putting on a pair of gloves and using the Allen wrench to remove the holder from the
goniometer. Locate the sample to be loaded into XRR. Take note of the run information (SiW112) as
well as its location in the deposition chamber (270◦)

3. Grip the sample with tweezers. Grabbing the center with tweezers will destroy the integrity of the
deposition and render the sample untestable.

4. Place the sample on the holder centered at the notch in the holder with the deposition side of the sample
facing you. You want to maximize the length exposed to the beam, so in the case of a rectangle to longer
side should run parallel to the beam / notch.

5. When the sample is in place cut two small rectangles of Kapton tape by first sticking the tape to a glass
microscope slide.

6. Place the tape ensuring the sample is perfectly flat against the holder. You may need to make tiny
adjustments to pull the sample flat. Use a Q-tip to flatten the tape without touching the tip to the sample.
This may leave residual fibers and scratches.

7. Place holder back, close the sliding window, and open slit 2

This is what your samples should look like after steps (1) through (7):

Figure 4: Mounted sample that does not obscure the beam

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III. SCANNING STEPS

III.i. File Storage

We want to make a new directory for a new mounted sample

+ mkdir /home/randd2/RandD2_SiW112_1october2018_270deg_Witness

The naming convention should follow the format

/home/randd2/RandD2_samplename_datecreated_chamberlocation_sampletype

The base directory /home/randd2 already exists and is a common repository for scans, whereas everything
that follows it is specific information related to the deposition of the flat. Record the new directory as
well as the date of scan in the log notebook. This directory information will vary depending on the run,
the deposition date, and the location in the sputter chamber. As well as whether the scan is of a flat,
endring, or optic. Once a new sample is created in the directory we supply a title SiW112 and filename
align1. The title changes based on the deposition information of the sample while the filename is changed
repeatedly during the process of scanning.

+ newsample
+ SiW112
+ align1

III.ii. Finding FWHM

We need to set the plot to a useful scale (139 is linear and 171 is semi-log) and check to see where all the
motors currently are.

+ setplot 139
+ wa

Care should first be taken to the locations of slit 2 and slit 4. Slit 2 closest to the monochromator
effectively acts as a means of shutting off the beam by closing the slits. How far slit 2 is open determines
the contributions of to the incident beam. If it is not already - open slit 2.

+ mv sl2l 0.05
+ mv sl2r 0.1
Note: The closed position for slit 2 is sl2l -0.1 and sl2r 0.1 rather than a zero-zero positioning

During alignment we want to narrow the beam right before it reaches the detector to 100um. This helps to
ensure proper alignment at the center of the beam before opening up to 400um for the duration of the
scan. This is controlled by slit 4.

+ mv sl4l 0.05
+ mv sl4r 0.05

Now we must move the sample and holder completely away from the beam (z) while we line up the in-
cident angle (th) and the detector angle (tth). We run an ascan of tth. An important distinction must be
made between the two types of scans: ascan and dscan. An ascan is absolute, that is to say it sends the
 Cardoso 6

motor to a position related to its 0 position. This scan will also leave the motor at the end point of the
sweep. A dscan sweeps between two positions relative to the current position, returning motor to its
original position.

+ mv z -10
+ mv th 0
+ ascan tth -0.1 0.1 40 1
Note: scanning format is as follows:
ascan (motor) (start position) (end position) (steps) (time spent col- lecting detector counts)

The plotted result of this scan yields the FWHM and position of the peak. Normal values for FWHM
are about 0.27 to 0.33 depending on the slit calibration. Check back to the immediately preceding entries
in the log book to ensure you are not misaligned. Move to the centroid (CEN) of this region:

+ mv tth CEN
+ set tth 0

Once tth is in the new position we want to count for 10 seconds to find and record Io. This provides the
counts per second (cps) for 100um slit width and serves as a base level of counts to work toward during
alignment. We then do the same for 400um. For an average scan at the current x-ray source setting these
tend to be close to 10,000 cps and 15,000 cps respectively.

+ ct 10
+ mv sl4l 0.2
+ mv sl4r 0.2
+ ct 10
+ mv sl4l 0.05
+ mv sl4r 0.05
+ wa

Now we run a scan to push sample back into the beam and hopefully capture a full cutoff to center at. The
plot should appear as a continuously high level of counts (since the surface of the sample is approaching
from the negative z direction and the beam is unobscured). The plot will then drop to zero like the falling
edge of a pulse as the beam is completely obscured. Moving to the centroid in this case puts z in the
middle of that falling edge - splitting the beam.

+ ascan z -0.25 0.25 20 1

+ mv z CEN
+ set z 0

Now this is the ideal result of running the z scan in which the sample is mounted perfectly flat, the de-
position surface has minimal imperfections, and most importantly that the ascan limits are set correctly to
capture the beam cutoff. The most common issue is that the curve is offset, so you need to either broaden
or shift your scan limits. In the most extreme case you are receiving scan results of only high counts or
only zero counts and small alterations to the z limits yields (1) no change to the plots (2) directionally
incorrect cutoffs or (3) broad beam cutoffs. In these cases you will need to scan z over a very broad range
like -5 to 5 or -10 to 10 because you all likely not looking at the sample’s surface.
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Now we alternate scans of z and th to refine their position. Repeat the following 9 commands until setting
theta to 0 yields a result sufficiently small. This is based on the current project the lab is working on.

+ ascan th -0.5 0.5 20 1

+ mv th CEN
+ set th 0
+ ascan z -0.25 0.25 20 1
+ mv z CEN
+ set z 0
+ ascan th -0.5 0.5 20 1
+ mv th CEN
+ set th 0

III.iii. Quick Scan

We want to run a quick scan to see the initial reflectivity plateau (IRP) as well as the first two Bragg
peaks. Low counts in these regions would indicate that a long scan would not be sufficient for modeling.

+ newfile
+ quick1 400um 15712cps
Note: the naming method is not required, but helpful. 400um indicates the slit 4 width and 15712cps is Io
for 400um noted in the lab logbook.
+ mv sl4l 0.2
+ mv sl4r 0.2
+ setplot 171

 STOP 

Take special care in the next step for setting the limits of th and tth as well as the total number of points in
the scan. A typical reflectivity vs. graving angle (th) plot will have an IRP at ~ 0.3 degrees, the first Bragg
peak at ~ 1.5 degrees, a second peak at ~ 3 degrees, and a final peak out between 4 and 6 degrees. As you
will see when modeling in IMD this is a generalization as multilayer spacing / thickness alone can shift
these values tremendously. The point being to take care during quick and long scans to know (1) the
expected characteristics of the deposition and (2) what you want out of the scan. Mistakes here cost hours.

+ a2scan th 0 3 tth 0 6 180 1

III.iv. Realignment

We now want to align tth and th on either (1) a strong Bragg peak or (2) IRP. This is up to the discretion
and experience of the XRR operator. One requirement to consider is the counts. Realignment on a second
Bragg peak with <25cps would yield weak results during the long scan. Aligning on a second peak,
however, will increase the likelihood that the third peak in the long scan has sufficient counts to model.

+ newfile
+ align1b
+ mv tth (value of first peak)
+ mv th (half the value of the first peak)
+ ct
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III.v. Long Scan

We will not start a long scan. Again, care should be taken to th and tth bounds as well as the points per
degree. We will also increase the time spent counting at each point. Scanning 360 points for 10 seconds
each will yield a 1-hour scan that you can quickly model while waiting for a longer scan. This will
maximize catching mistakes in mounting and alignment before running a very long scan.

+ newfile
+ long1 400um 15712cps
+ setplot 171
+ a2scan th 0 6 tth 0 12 360 10

IV. LOOKING AHEAD

Figure 5: A typical reflectivity vs. graving angle (th) plot

This is an example of my measured data using XRR (red) and modeled using IMD (green). While each
sample is unique in reflectivity features due to micro roughness, d-spacing and deposition metals – this
should give a rough guide of what to look for. In this case the command given to initiate this scan was
+ a2scan th 0 4 tth 0 8 720 10

Notice the initial reflectivity plateau (IRP) found between 0 and 0.35 degrees incidence. There is a
discrepancy between the expected model counts and measured data. This is a normal occurrence. Special
care taken during monthly calibrations, precise individual sample alignment, and minimizing surface
anomalies can soften this affect – but it will never go away completely.