BL08W XAFS SAMPLE MAKING
Table of Contents
- Powder sample
- Pellet sample
- Liquid sample
- Large sample(Bulk Materials, Thin-Film Substrates, etc.)
- Sample Preparation Example Download Link
Powder Samples
Required Materials
Carbon tape
Weighing paper
Tweezers
Spatula
①Cut the carbon tape and place it with the release liner facing downward.
②Place the sample onto the tape.
③Level the sample using the flat edge of the spatula.
④Gently tap to remove excess sample.
⑤Peel off the release liner.
⑥Attach the tape to the sample plate (BL equipment).
⑦Final setup.
⑧When using a slide mount for ambient conditions.
⑨When using an ion chamber for Conversion Electron Yield (CEY) measurements.
Ex:For High Sample Concentration
①Transfer the sample onto weighing paper.
②Lightly press the release liner onto the sample to allow a thin layer to adhere.
③Gently press the liner onto the carbon tape to transfer the sample.
④Attach to the sample plate.
Pellet Samples
Required Materials
①BN(boron nitride)
②Analytical balance
③Weighing paper
④Mortar ⑤Pestle ⑥Spatula
⑦Hydraulic press
⑧Pellet die set
⑨Zip-lock bag ⑩Heat sealer
⑪Kimwipes ⑫Ethanol
①Weigh the sample and BN using an analytical balance and dilute to an appropriate concentration.
(Reference: SPring-8 Industrial Application Promotion Office-Sample Preparation Guide Program)
②Mix the sample in a mortar for approximately 20 minutes.
(Sample homogeneity has a significant impact on XAFS spectral quality)
③Assemble the pellet die set.
④Apply pressure using a hydraulic press.
Example:Diameter: 10 mm, Thickness: 1 mm
Pressure: 10 MPa, Pressing time: 10 minutes
Adjust conditions as appropriate for the sample used.
⑤Reconfigure the pellet die set.
①Remove the outer sleeve and base, leaving only the inner cylinder.
②Insert the ejector rod into the top of the inner cylinder.
③Holding both the ejector rod and inner cylinder, carefully invert the assembly vertically.
④While holding the inner cylinder in place, attach the sample holder.
⑤Remove the pellet from the pellet die set.
①While holding the sample holder, apply slight pressure using the hydraulic press to gently push it in.
②Release the pressure and remove the pellet die set from the hydraulic press.
③Remove the sample holder.The pellet positioned between the mirror plates is exposed.
④Carefully remove the mirror plates to avoid cracking the pellet.
⑥Pellet Packaging
①Seal the lower half of the opening using a heat sealer.
②Place the pellet inside.
③Seal the upper half of the opening.
④Final setup.
Liquid Samples
Required Materials
①Kapton film:5um
②Teflon film:1.0mm
③Double-sided Kapton tape:145um
Hole punch (5.5 or 7 mm diameter)
Sizes are for reference only. Adjust as appropriate for the sample used.
①Cut the double-sided Kapton tape into the required size.
②Peel off the transparent protective film from one side of the Kapton tape.
③Attach the Kapton tape to both sides of the Teflon film.
④Cut out the Teflon film with the attached Kapton tape to the desired shape.
⑤Punch a hole at the center of the Teflon film with attached Kapton tape (snowman-like shape).
⑥Cut out the cell structure.
⑦Peel off the transparent protective film from one side of the Kapton tape on the cell.
⑧Attach the cell to the Kapton film to complete the empty cell before solution injection.
⑨Peel off the remaining transparent protective film from the Kapton tape.
⑩Inject the solution carefully to avoid overflow.
⑪Cover the filled cell with another Kapton film.
⑫Final setup.
Large Samples(Bulk Materials, Thin-Film Substrates, etc.)
Required Materials
Carbon tape
Tester (multimeter)
①Cut the carbon tape and attach it to the sample plate.
②Attach the sample.
Ex: For Insulating Materials or Thin-Film Substrates with Poor Electrical Conductivity
①Cut the carbon tape and attach it to the sample plate.
②Attach the sample.
③Apply carbon tape from the top surface of the sample to the plate to ensure electrical continuity.
④Final setup.
⑤When using an ion chamber for Conversion Electron Yield (CEY) measurements.
Sample Preparation Example Download Link