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====Loading specimen==== | ====Loading specimen==== | ||
Carefully carry your prepared sample to the XRD. | |||
Make sure X-rays are off. | |||
Open XRD door (lift up) | |||
Sample stage consists of a spring-loaded platform that holds the sample in place. | |||
Pull spring-loaded platform down far enough to slide your sample in. | |||
Very carefully slide sample in and center the sample with the stage. | |||
Close the XRD door (pull down) | |||
Hit the Red button. | |||
You are now ready to run the scan. | |||
====Running the XRD scan==== | |||
Revision as of 15:06, 27 September 2012
Work in progress!
To determine concentration using XRD:
The rule of mixtures aka Vegard's Law allows concentration of a component in a mixture to be calculated by comparing the current lattice parameter to that of each pure substance, see Wikipedia: Wikipedia:Vegard's_law
How to do XRD:
Before beginning XRD
Contact the lab director/supervisor: For MTU:
- Ed Laitila (ealaitil@mtu.edu), Office #: 628 M&M
- XRD Lab - Room #: 629 [XRD webpage]
Ed will guide you through the XRD process & assign you a X-ray badge #. This outline here is just for review & as a procedure for what was done.
You must sign up for a time at the XRD webpage above after talking with Ed, in order to schedule your session.
How to prepare sample
XRD is generally for powder, but can be done on thin films/wet samples/etc. Consult Ed for specifics on how you should prepare your material.
1. Put on gloves
For powders:
2. Obtain alligator clip, glass, slide, spatula, and a powder sample holder (consult Ed on whether you need a special holder, ie. small amount or zero background)
3. Wash all of the above items/tools with alcohol/ethanol? in the sample prep area.
4. Clip glass slide onto powder sample holder.
5. Fill & pack w/sample powder using spatula.
6. Tap setup vertically on counter to pack and plunge spatula to free up loose areas and pack them.
7. Once the powder sample holder is packed, take off alligator clips and carefully remove slide.
8. Wipe off edges of holder w/kam wipes & alcohol?, so that the XRD does not get contaminated w/loose powder. Be careful not to ruin powder surface (You need as flat of surface as possible).
9. Now you're ready to load.
For thin films(as used in this example):
2. Obtain a small piece of clay, weight, glass slide, and specimen holder from sample prep area.
3. Clean all of the above items (except clay) with alcohol? in the prep area.
4. Make sure your sample will fit into holder. You want it to fit within the edges.
5. Ball up clay and make into a cylinder slightly higher than edges.
6. Stick clay onto sample holder.
7. Stick sample centered on top of clay.
8. Take glass slide & press it down onto the specimen to even the specimen w/holder edges. Keep glass on specimen (don't take off!)
9. Take weight while holding glass slide and put it on top of the setup.
10. Make sure specimen is larger than clay surface (no clay peeking out!)
11. Wait 5 minutes so clay doesn't shift.
12. Carefully remove weight/glass.
13. Now you're ready to load.
For others:
I've never done this, consult Ed.
Loading specimen
Carefully carry your prepared sample to the XRD.
Make sure X-rays are off.
Open XRD door (lift up)
Sample stage consists of a spring-loaded platform that holds the sample in place.
Pull spring-loaded platform down far enough to slide your sample in.
Very carefully slide sample in and center the sample with the stage.
Close the XRD door (pull down)
Hit the Red button.
You are now ready to run the scan.