Have you already tried to simply increase your acquisition time? What are your experimental conditions?

Hi Shreejith! Remember me ? :) I think longer scan time should help you in getting more photon counts and thus intensity. Also don't keep the 2theta increment too small, a good value will be 0.02. This will help in getting the right statistics,as you would not want too many background points as compared to the data points in peak.

Sure, there are lots of ways.  A few have already been mentioned, but there are more:

... Probably more, but your problem will most likely be one of those.  Be sure to do #9!

Thanks David. It seems my acquisition time is quite low (30 mins) and my step size is 0.004 @David Bérardan. I will try increasing acquisition time.

Thanks Prachi for your suggestion (off course I do remember you.. :-) ). I will try step size of 0.02.

Thank you very much for your extensive list of suggestions @w.s.l. Boyer. 

Dear Sreejith,

all already mentioned points may hep you with the problem.

Additionally, if you are using so small step size of 0.004, as described, and if it takes only 30 min of scan time, you are trying to probe a very small angle range. I suppose you should try your experiment in a large angle range, check the peaks and only in the case you have a very intense peak around it, eliminate such angle from your experiment. Even with a large acquisition time in a very short angular range you still with very low intensity peak, since the background of your sample will increase in the same way and your peak will spread over a reasonable large portion of your small scanned angle range, it will still very low intensity and very broad. Try first an experiment with 0.01 degree 2 theta as step size, increase your angular range and check the instrumental parameters for such angular range condition, like instrumental width, mismatched position, crystallinity.... Use one good quality standard to evaluate this condition. Once you are sure the instrumental are ok, get your experiment in a large angle range, and if necessary, goes a way down in successive low angular range. Check if it will give you the necessary information/relation signal intensity. Have in mind that you will lose intensity as you spread your peak in short angular range. It still there, however very broad making the fitting as you like almost impossible.

Another try, you may use a pollycapilar setup to increase the x-ray flux over your sample, in several conditions it will significantly increase the signal/background, as it uses parallel beam.

I can help you with pollycapilar experiment to get your x-ray in parallel condition if you like or need.

Good look

Good luck

You can use oriented samples for selective peak intensity enhancement. The suitable way of obtaining such samples is crystalline deposition on microscope glass slide. In case of oriented samples certain peaks will be more intensive but other will be reduced. 

But Maciej,

preferred orientation is that thing, which should be omitted in XRD  measurement at all costs  especially when a refinement will be the goal, such as it is the case for Sreejith's application.

In case of getting a hard copy of the obtained peaks, you can re-photo copy it with larger scale factor, also check the facilities of your XRD rig.

Emad

1. Prepare samples with fine particles (this will increase the probability of random orientation)

2. Increase scan time

3. If above conditions are not giving results then try to change (IF POSSIBLE) wavelength of x-rays, and slit settings (as already suggested by Dr. w.s.l. Boyer ) 

4. If third option is not possible, (since machine(instrument)  measures relative intensity of peaks, therefore you can multiply the scale factor to experimental values (preferably before background subtraction) to have higher relative intensity peaks 

Regards,

0.004 deg step size is highly unusual.  It's been said before, but it's worth emphasizing.  Use 0.02 steps size with a 0.04 degree receiving slit.

It is important  to post the picture of your diffractogram, or else Treor.

If your sample contain one of these elements: Co, Mn, Fe. And you source is Copper than nothing can make it better unless you have Co-source or monochromator or energy discriminative detector.

It can also be that you are in one of the premier educational institutions in the world, IIT-M, but yet brain washed into using an archaic tool almost as old as when the Braggs conceived it and are still employing the eubiquitous 0D point counter, a fancy Geiger counter. You have no clue what odds the Braggs had to overcome in terms of technology to win their Nobel prize :-) They actually used photographic film to meticulously understand this stuff and built the Bragg Spectrometer, the ADAM & EVE of all diffractometers.

Go tell your XRD lab manager and director to unshackle you from the past and give you LIBERTY with a real time 2D detector in order to observe Nano structural causes in situ. If they can avoid the "fear factor" I'll even volunteer to demo the tool on your diffractometer early 2018. It is presently installed at CeNSE/IISc Bengaluru.

With such a tool you'd know instantaneously whether there is strong preferred orientation or not. You may even quantify your real time observations. You may observe large swaths of the reciprocal space simultaneously to detect & quantify in situ phase transformations. Detect evidence of fluourescence. You may harness all the 3D reciprocal space data that most of us routinely discard just to CONFORM.

Break out! Welcome to The Brave New World of real time in situ 2D Bragg XRD Microscopy & Recoprocal Space Imaging!

Rip Van Winkle!

In order to take full advantage of the expertise available to all of us through RG, here are some suggestions:

https://www.researchgate.net/post/How_do_I_calibrate_the_diffractometer_2Theta_angles_with_this_powder_diffractogram_of_corundum_standard_from_a_Bruker_D8_XRD_instrument?

Since I've taken on the roll of the "SHOCK JOCK" for this discussion I'll delve into some of the prior suggestions for conventional "powder XRD observations" and explore the potential detrement to precise Nano structural analyses. Meaning, avoiding equivocation and enhance precision!

• "larger divergence slit", combined with the conventional 0D point counter will blurr the data further. But, will improve count rate :-)
• "use a flourescent screen in the sample position to verify", you should have seen me strugling with this in my XRD lab 3 decades ago with all lights out but with a lot better eye sight :-) Highly subjective! BTW when is the last time you verified that your incident beam direction was parallel to your diffractometer plane and perpendicular to the diffractometer axis? How did you do so?
• "I can help you with pollycapilar experiment to get your x-ray in parallel condition if you like or need". I'd love to know the details of this procedure. How long does it usually take?
• "preferred orientation is that thing, which should be omitted in XRD measurement at all costs". Fact of the matter is "preferred orientation" is unavoidable and may be detected and quantified using XRD. However, as pointed out deftly, such Nano structural features including amorphous phase tend to befuddle many popular XRD analytical techniques.
• "SAMPLE PREP", modifies the in situ Nano structure in the specimen. Stress/strain induced phase transformations may also occur in some materials. In fact, the resolution available with XRD allows us to quantify the Nano structural stress/strain state precisely in terms of lattice dilatation and defect density.
• "make sure your x-ray tube is ok - tube gradually accumulate tungsten evaporating from the cathod (filament), this not only contaminates the spectrum with W L lines, but greatly reduces the Cu K alpha intensity" - This one alone may disqualify the powder methodology as "unreliable". However, this is not so. XRD is actually a "forensically precise" method used to determine guilt/innocence in some cases. The incident beam integrity is perhaps the best reason to always record the incident beam, Io, along with a reference standard prior to each XRD observation. Thus, minimizing speculation. Seldom seen it done.
• Avoid using the "black box" approach with analytical software and techniques. Don't get lost in the minutia. Understand the basics. Verify!
• more to come :-)