X-ray Powder Diffraction

(1) Turn on the computer

(2) Switch on the power supply for the chiller

(3) Switch on the power supply for the XRD

(4) Turn on the chiller’s switch

(5) Turn on the XRD machine mains switch by rotating clockwise from “0” to “1” (the switch is on the left wall of the machine, towards the lower region)

(6) Push the green “I” power-up button to the left of the main switch.

(7) On the front wall of the XRD, towards the left edge, wait for the upper-left generator screen-key button to stop blinking and display an “I” symbol against a white background. Press this screen-key button to activate the X-ray generator and wait for the screen key to change to an “X-ray ON” symbol.

(8) On the right wall of the XRD, access the lower panel (normally closed) to reach the LynxEye detector’s controller. Press the green “BIAS” button to turn on the high voltage for the detector. The “BIAS READY” LED indicator (yellow) will start blinking, then stabilize to be permanently on.

(1) Put the powder sample evenly on the sample holder. The amount of sample is recommended to be > 0.5 g.
(2) Press the sample powder to make it rigid using a glass slide.You can put some ethanol to avoid the sample powder flying off.
(3) Remove excessive sample powders using a glass slide. You can label you sample holder using marker pen as 1, 2, and 3

(1) Under the diffrac.commander software, click on the Wizard tab to access the XRD.Wizard function.

(2) Under the Wizard menu drop list, click on “New”, select “XRD” from the pop-up list, and click “OK”.

(3) On the new diagram screen which appears, click on the X-Ray Tube diagram, select 40 kV & 30 mA, then go down to the bottom of the page. Optional – if the sample rotation is desired, click on the Flipstick diagram and activate the checkbox. Click “Next” to continue.

(4) On the next page, the updated setting will be displayed. Go down to the bottom of the page and click “Next”, and repeat until the SCAN PARAMETERS page is reached.

(5) At the SCAN PARAMETERS page, change the parameters according to the requirements:

• “Start” and “Stop” define the scanning range. It is recommended that the value Min-Max is 5^O to 80^O.

• “Time/Step” defines the amount of time (in seconds) spent on collecting signals at each step position. It affects the total scan time and detects signal intensity (y-axis in the analysis output graph).

• “Step size” defines the x-axis interval between data points in the analysis. It affects the total scan time as well as the “smoothness” of the analysis output graph. The recommended value is ~ 0.02.

• “Number of steps” is calculated from the “Scanning Range” divided by the “Step size”. It defined the total number of data points of the analysis output graph. It affects the total scan time, as well as the “smoothness” of the analysis output graph.

• “Total scan time” displays the expected amount of time required to complete a single scan using the entered setting. You can hover the mouse cursor over the text to display the time in hour: min: sec format.

(6) Review the overall scan range and scan time, then go to the bottom of the page and click “Next”.

(7) Go to the “Wizard” menu drop list, then click on “Save As” to save the defined scan setting as “*.bsml” file; use a corresponding folder under “Libraries => XRD Data”.

(8)After the setting have been saved, click on the “Wizard” menu drop list, then use the “Close” function to clear the screen until it is reset to a blank (grey).

Note: After characterization is complete, remove all the samples and clean up the area and the used sample holders. As the Bruker XRD setup is designed for continuous operation, the machine shall be left for other users.

If the machine will not be used for extended periods and you want to shut it down:

(1) Turn off the computer

(2) On the front wall of the XRD, towards the left edge, press the upper left generator screen-key button and wait for it to stop blinking and display an “I” symbol against a white background.

(3) On the right wall of the XRD, access the lower panel (normally closed) to reach the LynxEye detector’s controller. Press the green “BIAS” button to turn off the high voltage for the detector. Wait for the “BIAS READY” LED indicator (yellow) to deactivate.

(4) On the left wall of the machine, toward the lower region, press the red “O” power-down button (located to the left of the main switch).

(5) Turn off the XRD machine mains switch, by rotating anti-clockwise from “1” to “0”.

(6) Wait for at least 10-15 minutes for the XRD to cool down before turning off the cooling water circulator.

(7) Switch off the power supply for all equipment.