How do We Prepare Your Samples?

Learn how samples are prepared to ensure accurate and reliable measurement results.

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Table of Contents

Sample Preparation Tools Sample Holder Powder Loading Tools Sample Windows and ID Sticker How We Prepare the Samples Step 1: Place first window. Step 2: Secure window with clip. Step 3: Flip and inspect. Step 4: Place powder funnel. Step 5: Load and pack powder. Step 6: Check filling level. Step 7: Place second window. Step 8: Place second clips. Step 9: Place QR label.

Our high-throughput measurements are possible through a unique system that can cycle samples through the X-ray beam in seconds per measurement. In order to accomplish this, we prepare them in specially designed sample holders.

Here we demonstrate how the samples are loaded into the holder for best quality measurements.

Sample Preparation Tools

Descriptions of the sample holder components and tools used are listed below:

Sample Holder

holder contains slots for up to 16 individual samples; each slot consists of a cylindrical well approximately 1 mm thick and 2.5 mm in diameter

Powder Loading Tools

funnel to direct powder into the sample well

Sample Windows and ID Sticker

clips to hold the windows tightly in place

sticker with QR code for sample identification

How We Prepare the Samples

**Two finished samples, let’s do the next!** Positions 1 and 2 show two finished samples completed with QR codes.

It is important that the QR codes are placed in the square positions and on the side shown in the picture (with the slanted notch on the left). The holes to the left of the QR code are for laser alignment and should not be covered over.

We ensure a clean working surface. You’ll also notice that at position 4 all sample slots not currently being filled are covered with tape. This helps to avoid cross-contamination while filling the powder; in this case everything except slot 3 is covered.

Step 1: Place first window.

The back side of an empty well is covered with a fresh polyimide window. The window is centered over the opening for optimal surface contact.

Step 2: Secure window with clip.

The windows is fixed into place using one of the black clips.

The three prongs of the clip snap into three of the six openings around the central window holding the window tightly in place. Though tightly fitted, it is not perfectly sealed against ambient air. For air sensitive materials, preparations can be performed in a glove box and stored under inert gas until the measurements are performed.

Step 3: Flip and inspect.

The sample holder is flipped over, ensuring that the black prongs are gripped onto the edges.

Step 4: Place powder funnel.

A funnel holder is positioned into the three remaining open slots around the window, and a clean funnel is inserted.

Step 5: Load and pack powder.

The sample is poured into the funnel and packed into place using the plunger.

For best quality measurements, the powder is filled completely and densely into the well. is ensures that the maximum sample cross section is available for best possible data statistics, and it maximizes the orientation distribution of the crystallites for acquisition of complete Debye-Scherrer rings. During measurements, we additionally shake the sample holder and scan the beam across the window to further improve the sampled volume.

Step 6: Check filling level.

Powder is filled completely and densely into the sample holder well.

Over-filling the well is avoided to keep the polyimide windows flat and maintain a consistent background signal.

Step 7: Place second window.

The open side of the filled well is fitted with another fresh polyimide window.

Step 8: Place second clips.

A second clip is placed, clipping the three prongs into the remaining open holes as before.

Step 9: Place QR label.

The sample is labelled with a QR code sticker in the square frame below the sample.

Sample QR codes are registered in our app https://app.momentum-transfer.com for robust sample tracking.

sample holder preparation