Operation Notes on High-energy X-ray Diffraction Measurements at

APS Beamline 11 ID-C

 

Overview – Measurement of diffraction between 0.35 and 35 -1

Procedure

 

 

Diagram of 11 ID-C, High Energy X-Ray Diffraction measurement

 

Install sample

Search and Close hutch

Open beam

Position detector at 2 -1 driveq(2) [high energy]

Scan the horizontal sample position to locate sample center [Scan]

                  motor = slr

                  filename = position

                  step size = 0.2mm*

                  range = -6mm to 2mm*

                  count time = 1 second

Set horizontal position to the obtained value, motor = s1r [huberfoe]

Scan the vertical sample position to locate sample center [Scan]

            motor = sll

                  filename = position

                  step size = 0.2mm*

                  range = 6mm to 12mm*

                  count time = 1 second

Update macro for automated running, [user-macrosE] [bychkov18()]

Start the macro bychkov18() [high energy]

Macro information

 

Syntax

mv motor,position

Example

mv sll,8.0

Action

Move sample stage to vertical position = 8.0mm

 

Syntax

mv motor,position

Example

mv s1r,-1.4

Action

Move sample stage to horizontal position = -1.4mm

 

Syntax

ScanPowderAimShort(filename,start,end,step,count_time,unkown)

Example

ScanPowderAimShort(50CsBr – Ga2S3,0.3,35,0.025,5,0)

Action

Perform data acquisition from Q = 0.3 to Q = 35 with a step size of 0.025 and a measurement of 5 seconds. File name for results 50CsBr – Ga2S3

 

 

Example of macro to run 2 entire Q range acquisitions followed by 3 high Q range runs*

 

mv sll,8.0

mv s1r,-1.4

mv s1r,-1.4

 

ScanPowderAimShort(50CsBr – Ga2S3,0.3,35,0.025,5,0)

ScanPowderAimShort(50CsBr – Ga2S3,0.3,35,0.025,5,0)

ScanPowderAimShort(50CsBr – Ga2S3H,15,35,0.05,5,0)

ScanPowderAimShort(50CsBr – Ga2S3H,15,35,0.05,5,0)

ScanPowderAimShort(50CsBr – Ga2S3H,15,35,0.05,5,0)

 

 

* example used on March 2003

 

APS instructions

 

 

How to open the door?

 

1               Verify that the computer has stopped working (while working the cursor is a white and black spinning circle). Move the detector to the 2 A-1 position by entering the command driveq(2) at the command line of the window named high energy: the detector should move to the correct position .

2               Close the shutter by pressing the button on the panel to the right of the door. Then open the hutch door by pressing the big red button on the panel named station C.

 

The door opens

 

How to install the sample?

 

 

1               Place the holder containing the sample in the holder with the Kapton tape closest to the X-ray source.

2               Use the theodolite (alignment telescope) to check that the sample is in the correct position.

 

How to search and close the hutch?

 

1               Push the two buttons situated on each side off the hutch

2               On the panel named station C, push (keep depressed) the green button until the door is closed and locked

3               Open the shutter (button on the panel named station C)

 

How to optimize the sample position?

 

It is possible to move the sample with translation stage to place the beam in the middle of the sample.

 

Translate the sample in horizontal (X) direction

 

Go in the window named scan. Change the name of your data. Choose s1r motor and scan the sample between two positions with steps equal to 0,2 mm (for example -4 mm to 4 mm ), count equal 1 second.

The detected signal should increase when the beam enters the sample. The curve allows you to determinate the horizontal center of the sample.

 

Return the stage to this central position using the green window where you see s1r, enter center position in the target and push enter. The sample should now be horizontally centered.

 

Translate the sample in vertical (Y) direction

 

Go in the window named scan. Give a new name to your data. Choose s1l motor and scan the sample between two positions with steps equal to 0,2 mm (for example 6 mm to 12 mm ), count equal 1 second. Again you can determinate the vertical center of the sample.

 

Go to the green window where you see s1l, enter the vertical center position and push enter. The sample should now be centered horizontally and vertically.

 

How to change the beam power?

 

If you have too much power or power is too low you can open or close the slits.

In another green window, you have KS1, KS2. You can change the dimensions of the slits by moving these parameters.

 

Automation of the work

 

Go to the window named user-macrosE. After mv s1l, put the position of the vertical center of the sample. After mv s1r, put the position of the horizontal center of the sample. Be careful, mv s1r appears two times. Update the number for the both.

 

After the three mv lines, you see four scanpower lines. The first is a general scan. The others are a repeat of the noisiest part of the measurement. Put the name of the sample/scan in the green part of these lines. Except for the first, put H at the end of the name. Then press in compile.

 

In the window named high energy, write bychkov18 ( ) and push enter.

 

The data collection will begin