Bruker D8 Discover Manuel

Standard Operating Procedure:

Bruker D8 Discover X-Ray Diffractometer

(You MUST be trained by an authorized BSCMC trainer to use this instrument)

Hazards: This unit produces a high intensity X-ray beam. Take all precautions to avoid exposure to the x-rays.

Warning: Beryllium! Do not touch the front window of either detector as they both contain Beryllium. Fumes

of the dust from Beryllium and its compounds can be hazardous if inhaled!

Typical Experiment Sequence:

1. Sign in on the electronic calendar

2. Visually check the diffractometer for instrument status.

3. Open the cooling water valves and turn the x-ray generator ON.

4. Launch the D8Tools software to check the system status and ramp the power up.

5. Launch the operating software:

a. GADDS for use with the HI-STAR area detector

b. Commander for use with the Scintillation detector.

6. Check the x-ray beam intensity

7. Load and align sample

a. Use the Laser-Video System with GADDS and the HI-STAR area detector

b. Use a Z-scan and half intensity method or the Laser-Video System with

Commander and the Scintillation detector.

8. Set up scan and save data.

9. Remove sample, reduce power, turn the generator off and shut off the cooling water

10. Sign out on the Sign electronic calendar Be sure that the calendar accurately

displays the number of hours the XRD was OCCUPIED by your experiment.

Procedures for ALL X-Ray Diffraction Experiments on the Bruker D-8 Discover:

1. Sign in on the electronic calendar at https://boisestate.ilabsolutions.com

2. Visually check the diffractometer for instrument status. Check the machine status on

either left or right column before using the machine. The “Ready” and “On” lights

should be on. There might be an “alarm” due to the x-ray generator being OFF. The

“X-Ray ON” lights on top of machine should be on.

a. Left Control Column:

i. STOP button: If hit it switches off the control electronics. The X-Ray source is

turned off and all moving drives will stop instantly. The stop button should only be used

in emergency situations and not for normal shut down of the diffractometer system.

ii. Light button: This button turns ON/OFF the fluorescent tube located at the ceiling

of the enclosure.

iii. Fan button: This button turns the fan located on top of the enclosure ON or OFF.

iv. System Instrument-Key Switch: This key will lock/unlock the system. During normal

operation the switch must be in position “unlocked”.

v. Open Door button: This button must be pressed to open the front door. If the

Open Door button is activated while the tube window is open the X-ray shutter will close

automatically and it will disrupt the experiment.

vi. Ready light: Status of High Voltage Generator. Illuminated orange display indicates that

the high voltage generator is operating. Flashing display indicates the high voltage

generator is ramping up.

vii. On light: Illuminated green display indicates the control electronics are ready.

viii. Alarm light: Illuminated red display indicates a pending system alarm, flashing red light

indicates a pending warning.

ix. Busy light: Illuminated yellow display indicates that a measurement is in progress.

Flashing yellow display means that the system is not ready.

b. Right Control Column:

i. Stop button: Functions the same as the Stop button on left column.

“X-Rays ON”

ii. Power OFF button: It switches off the control electronics, the high voltage generator

and all components connected to the AC outlets.

iii. Power ON button: It switches on the control electronics, the high voltage generator

and all components connected to the AC outlets.

iv. High Voltage- Rotary Switch: Used for turning high voltage on or off.

v. Open Door button: Functions the same as the button on the left column

vi. Ready, On, Alarm and Busy lights have same functions as those on the left column.

3. Starting your session

a. Open the cooling water valves (on the wall behind the instrument) and check for any leaks.

b. Turn the x-ray generator ON by flipping the HV switch clockwise for few seconds and this will

automatically set the power to 20kV and 5 mA.

c. Open the D8 tools and heck the system status.

(→Online Status, →Online Refresh)

d. Check for any alarms

(An alarm or warning will prompt a red or orange box)

i. If they appear, click on the red or orange box to be directed to the cause

e. Ramp up the X-ray power(→X-Ray Generator, →Utilities, →Set kV/mA).

i. Set 30 kV, 10 mA and wait 2-3 minutes

ii. Set 40 kV, 15 mA and wait 2-3 minutes

iii. Set 40 kV, 30 mA and wait 2-3 minutes

iv. Set 40 kV, 40 mA

f. Check the status of the drives

i. Are the drives initiated? (Make sure the drives have significant figures (i.e. 23.047 vs.

23.---)) i. If not, initiate them by performing the following:

a. Click on the green box next to the drive to be initiated, then check the

settings of the drive (→Settings)

b. Check the reference position of the drive

Needs

initialized

c. Then physically look at the drive to determine which way it needs to go in

order to be at the reference position

i. If it needs to go in the positive direction to fulfill the reference

position, push the find reference up button. Likewise, if the drive

needs to go in the negative direction, push the find reference down

button (→)

NOTE: Be sure to have the mouse on the STOP icon to be able to stop the drive if it looks as

though it will crash (this will require you to watch each drive as it is initiated!)

d. Once the drive has stopped moving, push the adjust button (→)

e. Repeat steps a. and b. for any of the drives that need to be initiated.

ii. Do the drives appear to be in the indicated position? (Look at the values in D8 Tools for

θ1and θ2and compare them to the physical locations of θ1and θ2on the goniometer).

g. Close the D8Tools software.

Procedures for X-Ray Diffraction Experiments using the point detector:

4. Launch the operating software:

a. Open the Commander program for use with the point detector

5. Check the x-ray beam intensity (Make sure there is no sample or sample holder that

will interfere with the path of the x-rays)

NOTE: It is imperative that the copper absorbers are in place! If not, the

detector could be damaged!

a. Make sure the following slits are in place:

i. 1.2mm slit in the Goebel mirror exit slit (furthest left)

ii. 6.0mm slit with the TWO copper absorbers in the next slit

b. Set up a detector scan from -1 to 1 degree

i. Select Detector scan from the pull down menu

ii. Make sure that all of the drives are at 0

1. Type a 0 in each drive command window and then click on the Move Drives icon

to move the drives to 0 position.

Göbel

mirror

6.0 mm

slit and 2

Copper

absorbers

1.2 mm

slit

X-Ray

Tube

iii. Make sure the y-scale is in CPS

iv. Set the increment to 0.01°/step and the scan speed to 0.2 sec/step

v. Press the icon.

c. Make sure that the max count rate is 65000 CPS or more. If not, please contact an authorized

BSCMC trainer.

d. Make sure the peak is approximately centered about 0. If not, please contact an authorized

BSCMC trainer.

6. Load and align the sample (Depending on the sample and the stage, this can be done

using the Laser-Video System or using a Z-scan)

NOTE: Things to be careful of when loading your sample:

•Do not touch the sollar slits

•Be gentle with the laser/video system

oThese are precisely aligned to give you “good” data

•Do not bump the X-ray optics

oA very slight bump could easily result in a loss of 30% of your beam intensity

a. Open the doors to the XRD (Push Open Door button on either side of control column, then open

the window.) or

b. Put your sample on the XYZ table (stage will depend on preference, special instruction may be

required) and position it directly under the camera.

6.a Align the Z-height using the Laser Video System

i. Align the sample to the instrument using the Laser-Video System

NOTE: All of the components including the X-ray beam, camera, and laser have been aligned to aim at a point

which is called universal center of the goniometer. To align your sample surface at this universal center, you

need to use the Manual Controller to move the XYZ table.

ii. Activate the Manual controller and turn the laser on:

1. Press the Direct Mode icon to get to the command prompt window.

2. Type “RC1” and press “Send Command” to give the computer control.

3. Type “OC16,1” and press “Send Command” to turn the laser on.

4. Type “RC0” and press “Send Command” to give command to the manual

controller.

5. Position the stage and sample accordingly.

iii. Understanding the Manual Controller functions. The drives used are as follows (the

numbers on the controller correspond to the following drive numbers):

1. Θ1–X-ray source (aka tube)

2. Θ2–Detector (In this case the HI-STAR area detector)

3. φ(phi) –Rotation of the sample about the z-axis

4. χ(chi/psi)–Rotation of the sample about the Eularian cradle

5. X

6. Y

7. Z

8. Camera Zoom (1X ≤ Zoom ≤ 7X)

iv. The Manual controller has two functions:

1. Command (set point) mode (access by pushing the “F1/DRVC”button on the

controller)

a. Enter three commands (Drive #, Instruction, Location)

i. Drive # is where the drive you want to move is called on

ii. Instruction is what you want the drive to do (“Go To” is always

the number 2)

iii. Location is where you want the drive to move to

iv. (i.e. if you want the video zoom to go to 7X, you would type in

“8,2,7” and then press “ENTER”. The zoom will automatically go

to 7X)

2. Manual (video game) mode (access by pushing “SHIFT” then “F1/DRVC” on

the controller)

a. Identify the drive you want to move (1-8, see above)

b. To change the position of the drive, use the arrows (↓or ↑).

c. To change the speed of movement of the drive, use the “+” or “-“buttons.

!!!Warning: Make sure that none of the drives will run into each other when they are moved since there are NO

safety switches installed for this purpose. The “Emergency Stop” buttons can be used if

needed but it is preferred to use the ESC/STOP button on the controller is you see a potential problem.

v. Open VIDEO program, Turn on the light in the XRD chamber as needed

vi. Zoom the camera out (zoom = 1) to help easily find your sample in the video window.

vii. Move the X and Y drives to the area of interest on your sample (using the controller in

manual mode).

viii. Move Z to focus the laser on your sample (The laser spot should be in the center of video

window)

1. The laser might be difficult to see on reflective samples. If this is the case, move

Chi/psi to 22.5 degrees (splitting the angle between the laser and the video) to

cause the laser to reflect back into the camera.

Zoom = 1X Zoom = 7X

!!! Warning: Always leave one finger on “ESC/STOP” button when you are using command mode. Press

“ESC/STOP” button immediately if the moving part is going to hit other part.

ix. Once your sample is in focus and the laser is in the center of the video window (centered

on the crosshairs), zoom the camera in (zoom = 7) to fine tune your sample position.

x. Once the laser spot is centered, the sample is aligned and ready to take data (return

chi/phi to 0 (if applicable)).

!!!Warning: You can use the controller to move Θ1and Θ2to the desired 2θ angle. Make sure the detector will

not get hit by the direct beam (as a rule of thumb, always keep Θ1+ Θ2> 15°).

1. Back in the Direct Command window in Commander, type “RC1” and press

“Send Command” to give control back to the computer.

2. Type “OC16,0” and press “Send Command” to turn the laser off.

xi. Exit the Direct Command window by closing the prompt window.

6.b Align the Z-height the Z-scan half intensity method.

i. Align the sample to the instrument using a Z-scan and half beam intensity method.

ii. In the Scantype drop down menu, choose “Z”

iii. Set the scan at -1.25mm and end the scan at 1.9 mm

iv. Set the Increment to 0.01°/step and the Scanspeed to 0.2sec/step and click .

v. Note the average max intensity. (i.e. ~ 9750 CPS)

vi. Typically run a fast scan to start, then zoom in on the area of interest, click .

vii. Set the Increment to 0.005°/step and the Scanspeed to 1sec/step and click .

viii. Once the scan is completed, double click on the where the beam intensity is

approximately one half of the maximum intensity. (i.e. 4875 CPS). Once you double

click on the scan, the Z-position is automatically stored in the Z-drive command

window.

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