You can put on the bottom of the cuvette a sheet of thin glass, after this placed sample from above. Distribute the sample so as to obtain a spot of greater diameter than the diameter of the X-ray beam. It is desirable that the sample does not protrude beyond the edge of the cell.

You can also record the IR spectrum, get the phase composition. For this method sample is sufficient.

Best regard.

In general it is not important that all the sample holder is filled. You can put your sample in the central part, that is really hitted by X-ray and try to collect the pattern. I also have a Bruker diffractometer and I bought from Bruker other thinner sample holder, suitable for small amount of sample, with silicon slice at the bottom that does not produce diffraction effects. In your institution there is a mechanical technician? You can try to make him build some sample holder with low thickness. I have many kinds of home made sample holder: in plexiglass, stainless steel, aluminum suitable for different cases

The XRD pattern you are obtained from the characterization is also affected by the amount of sample. If the sample holder is not necessary full, so the XRD pattern might be no good enough. I agree with other suggestions. It is important to note that the sample must be good distributed  on the sample holder. You may place other material under the sample.

thanks

thank all of you for your kindly help, what you mention benefit me a lot, which helps me to understand the XRD analysis better. I will try the oritention method.

best wishes!

peixin du

I find that using a low background sample holder for an acetone smear of a small sample always helps, so try using a silicon wafer which has been cut in a direction not coinciding with an X-ray reflecting plane.

thank you, ROSS

i will have a try

best wishes

peixin du

@ Ross: I fully agree, we have a Philipps/PanAlytical multi-purpose diffractometer, and in the standard sample holder set delivered with the instrument, we got a so-called "zero-background holder", which is actually a Si single crystal with a huge miscut, so that there are no diffraction peaks disturbing / influencing the actual measurement. In contrast to a glass holder, with a continuouslky varying background intensity as a function of Bragg angle, the miscut single crystal has a rather constant background.

In addition to this, I would propose to rotate the sample during the measurements, which further improves counting statistics, as all particles then have the chance to contribute to the diffractogram!

Using such a setup, we have measured almost perfect diffractograms of sample quantities of several mg only ... see e.g. the attached data from ca. 10 mg of SnO dispersed on the zero-background holder recorded in about 10 minutes acquisition time. So if the scan is integrated longer, much better data quality may be achieved.

Greetings to all, Dirk

Hello，Dirk:

Thank you for your instructive reply. Could you please show me the photo of your miscut Si single crystal and its constant background?

As i have mentioned, my sample will show its diagnostic peak in low angel (2-20 degree), but the diagram you added does not contain the data of low angel. Is your method suituable for my sample analysis? 

Best wishes

Peixin Du

Try to fill your sample in capillary tube,usually we do this for liquid crystal sample.

Dear Peixin, there is nothing special on the zero-background holde  - you may simply buy it from Panalytical, the name is PW1817/32. See enclosure files! Good luck, Dirk

The most simple method is to use a  small glass slide (buy or cut it), the area of which fits well into the sample holder cavity and the thickness of which is smaller than the depth of the cavity (1 mm should do). Roughen the glass surface with emery paper and give your powder onto the rough surface, distribute evenly and smooth the surface to a possibly large and compact area using a stable glass disk (clean before use thoroughly with e.g. acetone). Put some plasticine pebble on the ground of the sample holder cavity and place your sample glass slide on it. It certainly will hang out rather skew on the pebble; adjust the surface of the glass slide sample evenly to the level of the sample holder rim by pressing down with the glass disk. I used the method when investigating of corrosion phenomena at precious medieval bronze monuments (sample amounts about 5 mg). Using glass slides is also a fine method in clay mineralogy by coating series of glass slides with clay slurries. Annotations: some glasses may become uneven when repeatedly tempered at T > 600 ºC (clay mineralogy); if necessary check for possible amorphous X-ray background effects of glass slide by running blinds).

Good luck

D. Zachmann

0.2 g sample is enough for xrd. u can try this way..dissolve ur powder sample in little DI water and sonicate, after that cut a  plastic pipette tip to a small size and put grease on the sides of that pipette  tip and put it on a glass slide which will adhere to the glass slide. make sure the portion of  glass to be inserted into the machine holder, leaving that portion u have to put the pipette tip and then add ur sample dissolved in water in micro pipette. then dry it in oven . after that u can remove the pipette tip. even if u have less sample u can do it easily in this method. plz check the attached file for ur clarity.

With thin self support vapor I hope one can do X-ray diffraction.  Another alternative method  is by using single crystal.

thank all of you for your good introductions and/or advice 

dear Dirk, it's very kind of you to give your helpful reply. i will try your method.

dear Zachmann, what you said is very specific, i will have a try.

dear Sanjit, thank you for your advice and providing me the attachment for clarity,  the holder for Bruker D8 Advance X-ray diffractometer is round in shape, i will think how to carry out your advice.

dear Artur, Kenneth and Venkatathri, thank you for your kindly help, too.

best wishes

peixin Du

With a small powder sample we normally sprinkle the powder on double-sided scotch tape which is stuck to a substrate chosen with an appropriate thickness to fill the holder. We have used stainless steel and glass substrates for that purpose. The layer of the powder should be uniform, covering the substrate area. Our layers gave high quality diffraction patterns. In this case, however, the material may not be useful for other types of measurements such as magnetic measurements.

dear Sami,

i want to recover my sample after examination, so scotch tape is not a good choice. but using a substrate chosen with an appropriate thickness to fill the holder is a good idea, and i can drop several drops of suspension prepared by sonics on the substrate, thank you. 

best wishes

peixin Du

Bruker sells sample holders (we use round ones for a Phaser II or a da Vinci) that has a "variable height" insert. I get zero background diffraction plates that fit the sample "hole" and epoxy them onto the plastic "plunger". It gives me a height of zero to about a mm or so for various volumes.

In Rigaku MiniFlex 6G for the small amount of samples they have zero background sample holders which can take samples from miligram size.