bruker d5005 user manual (version: 2013.03.19) · bruker d5005 user manual (version: 2013.03.19)...

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University of Minnesota College of Science and Engineering Characterization Facility Bruker D5005 User Manual (Version: 2013.03.19) Initial Setup 1) Check out and put on a TLD ring on from counter in room 22. Log into the D5005 computer using your x500 username and password (Domain = AD). 2) If the x-ray generator is off and has an error code see Appendix A. 3) If you are a University of Minnesota user, log into Charfac’s online reservation system. Make sure to enter your TLD ring number, the x-ray generator counter time, and the correct budget number. 4) Prepare sample in appropriate sample holder. 5) Start the MDI DataScan software. If an icon is not present on the desktop, perform a windows search Datascan*.*, and create a shortcut to your desktop. 6) Check the scattering slits: They should be from left to right 1, 1, empty, 0.6, 0.6. 7) Select the Control tab Open Siemens D5005, and the following window will appear:

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Page 1: Bruker D5005 User Manual (Version: 2013.03.19) · Bruker D5005 User Manual (Version: 2013.03.19) ... 10) Check the detector ... You will need to contact an XRD staff member to perform

University of Minnesota

College of Science and Engineering Characterization Facility

Bruker D5005 User Manual

(Version: 2013.03.19)

Initial Setup

1) Check out and put on a TLD ring on from counter in room 22. Log into the D5005 computer

using your x500 username and password (Domain = AD).

2) If the x-ray generator is off and has an error code see Appendix A.

3) If you are a University of Minnesota user, log into Charfac’s online reservation system. Make

sure to enter your TLD ring number, the x-ray generator counter time, and the correct budget

number.

4) Prepare sample in appropriate sample holder.

5) Start the MDI DataScan software. If an icon is not present on the desktop, perform a

windows search Datascan*.*, and create a shortcut to your desktop.

6) Check the scattering slits: They should be from left to right 1, 1, empty, 0.6, 0.6.

7) Select the Control tab → Open Siemens D5005, and the following window will appear:

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8) Check the status of the D5005 goniometer position. Does Theta read ½ of Detector/2Theta?

If not see Appendix B.

9) Set the generator operating power by choosing the X-ray tab.

a) Increase generator voltage from 20 kV to 45 kV (always turn up voltage first!). Be sure

to press Set after entering the correct value in the Voltage field.

b) Increase generator current to from 5 mA to 40 mA. Be sure to press Set after entering the

correct value in the Current field.

10) Check the detector settings by choosing the PHA option (see image below).

a) Pha Baseline: 0.49 V

b) Window: 1.0 (or 0.9) V

c) High Voltage: 740 V

d) Channel Gain: 600

e) Channel: 1

f) If these values are different than listed above, please contact the XRD staff.

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11) IMPORTANT: Make sure that the axes are calibrated. To do this, go to the Control tab →

Open Siemens D5005 → Control → Init. Goniometer → Press Ok if prompted. When the

calibration is done, the angles should be at 59.308o and 29.654

o for 2Theta and Theta,

respectively (do not change the angle values.)

12) Before you begin your sample measurements, it is a good idea to check the machine

calibration with the corundum standard.

a) Load the corundum standard (large white rectangular shape piece, located at the base of

the goniometer, inside of the enclosure) onto the sample holder—taking care that the

sample is securely held to the top three pins of the holder by the springs of the sample

holder (center circular plunger).

b) Close the door.

c) Choose the Scan tab → Routine Scan and the following window will appear. For new

users there will be no scans in the window. Press the “New Scan” icon at the top of the

window (the blank page icon).

d) The following window will appear—enter the values below and save the scan for future

use.

i) Setting ID: Type (excluding quotations) “Corundum calibration peak scan”

ii) Filename: Type (excluding quotations) “Corundum_Year_Month_Date_User_Extra”

(1) Year: Year of measurement (i.e. 2013).

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(2) Month: Month of measurement (e.g. 06, two digits!).

(3) Date: Date of measurement (e.g. 07, two digits!).

(4) User: 4-digit User number.

(5) Extra: Extra numbers if scanned more than once (e.g. 001, 002, 003,…)

iii) Scan ID: Type (excluding quotations) “Corundum scan on Year.Month.Date by User

User.”

(1) Year, Month, Date, and User are values listed above.

e) To input a scan range, press the “New scan range” icon (the bland sheet) and the

following window will appear:

i) Start: Starting angle (set to 34.0o for corundum calibration)

ii) End: Starting angle (set to 36.0o for corundum calibration)

iii) Step: 2theta angle degree step (set to 0.02o for corundum calibration)

iv) Dwell: Collection time at each angle (set to 1.0 s for corundum calibration)

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f) Select OK and you will the New Scan Job window again with the inputted scan

parameters. NOTE: For first-time users, a New tab will show up instead of a list of scans.

g) Hit OK again to go back to the Setup Scan window. Make sure the Output Dir: is set to

your user directory for the corundum calibration scan. Finally select only your Corundum

scan (or your regular scan sequence for sample scans) by checking its filename box and

unchecking (if there are other scans listed) all other scans.

h) Run the scan and check the peak position using JADE. Overlay the scan with the PDF

Corundum file # 00-046-1212 - the line should be at the center of the peak (2θ =

35.153o). The peak looks centered proceed ahead. If there is large shift first check to

see that the sample is held in place tightly. If it’s loose, peaks will shift due to sample

displacement. If the shift is still there after remounting the samples a few times,

contact the XRD staff.

Data Collection

1) Load your sample into the goniometer taking care that the sample is level and flush with the

top of the holder.

2) Choose the Scan tab on the toolbar and create a scan profile using the corundum procedure as

a template. If you would like to start your scan with 2theta < 5o, please contact the XRD

staff. Running at a lower angle requires special precautions in order to protect the detector.

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3) Click on Start to begin data collection. NOTE: Clicking on the clock in the upper right corner

will tell you how long the run will take.

Data Analysis

1) Click on the MDI Jade 8.0 icon on the desktop.

2) Select the File tab → Patterns to open your file.

3) To convert your data to a format that you can use in a plotting program go to the File tab →

Save as → *.dif, or *.txt for an ascii file.

4) JADE has numerous functions to help in the identification and analysis of your XRD pattern,

and explaining all these functions can encompass an entire book! It is best to sit down with

JADE for a while and play with the program to get a feel for its functions.

a) Use the toolbar help during analysis—the left mouse key executes the command, the right

mouse key provides the set-up menu for that particular command.

b) Refer to the manual or the “help” key for specific information.

c) If you need to add the PDF database to JADE, see the Appendix C.

5) To print your scan Go to the File tab → Print setup. To add a printer to the PC computer, see

the Appendix D.

Instrument Shutdown 1) Return generator power to the standby power:

a) Select Control tab → Open Siemens D5005.

b) Change generator current from 40 mA to 5 mA (always turn down current first!)

(Remember to click “set” after entering the 5 into the box.)

c) Change generator voltage from 45 kV to 20 kV (Remember to click “set” after entering

the 20 into the box.).

2) Exit control dialog.

3) Close Datascan.

4) The preferred method of data transfer is using either email, UMN Netfiles account, or UMN

Google Drive account.

5) Remember to sign off the instrument with Charfac’s online reservation system and entering

the final meter reading.

6) Return your TLD ring to the visitor drawer.

Please keep the work area tidy by cleaning the sample area and

sample holder. Remember Charfac is a user facility, and we all need

to do our part to keep the work are clean!

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Appendix A: How to restart the x-ray generator

1) Restart the computer.

2) Restart the D5005 goniometer. Push the green switch Netz located above time meter towards

the “O” symbol. Wait 10 seconds and push the green switch back towards the “|” symbol.

Leave the key in Position |.

3) After everything is back ON, locate the the three square black buttons located below the red

Push/Pull button.

4) Press the center button (with the white circle on it) and if the small LED Ready light

illuminates green (located below the X-RAYS ON light panel); press the ON button and the x-

rays should turn on.

5) When everything has been shut off and turned back on again, you may need to change the

detector channel gain from 0 to 600 in the control, and PHA window of the DataScan

program. You will need to contact an XRD staff member to perform this step.

6) Record the event in the D5005 maintenance binder, and email an XRD staff member.

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Appendix B: What if Theta is not ½ of 2Theta

1) Select the Control tab → Siemens D5005. Check to see if the Detector angle is two times the

Theta value in the Drive tab. If not proceed to Step 2.

2) Select the Control tab from the pop-up window and choose Init. Goniometer. The goniometer

will recalibrate itself with optical sensors to known angular values. When the calibration is

complete the angles should be at 59.308o and 29.654

o for 2Theta/Detector and Theta,

respectively in the Drive tab.

3) In the Drive to tab set Drive to = 60o (making sure that the Axis field reads Both Axis). Hit the

Go button and the goniometer should drive to a position where Detector/2Theta = 60o and

Theta = 30o. The goniometer should now be calibrated.