Relevant Screenshots of XRD Analysis:

Step 1: Customize > Manage Database> Add Highscore Database>Select

Figure 01: Screenshot of XRD analysis (Database Adding)

Step 2: File> open >.XRDML

Figure 02: Screenshot for XRD analysis

Step 2: Treatment >Search peaks >Minimum Significance (10.00) >accept.

Figure 03: Screenshot for XRD analysis

Step 3: Analysis >Search and Match >Execute search and match >Restriction >edit restriction set
>periodic table > select element >ok > add rest of none >close > search > reference code, score,
compound name > drag and drop.

Figure 04: Screenshot for XRD analysis

 Figure 05: Screenshot for XRD analysis

Figure 06: Screenshot for XRD analysis

Question 1. What are the information you can obtain from any XRD data file?
Answer: We can obtain following information from XRD data file [2] :
• Crystalline materials characterization.
 • Sample purity measurement
• Crystalline phase and chemical composition determination.
• Unit cell dimensions measurement
• Crystal structures determination using rietveld refinement
• Modal amounts of minerals (quantitative analysis)
• Dislocation density and quality of the film determination by rocking curve
measurements
• Measuring superlattices in multilayered epitaxial structures
• The thickness, roughness and density of the film measurement using glancing
incidence x-ray reflectivity measurements
• Make textural measurements, such as the orientation of grains, in a polycrystalline
sample
• Fine-grained minerals identification such as clays and mixed layer clays that are
difficult to determine optically

Question 2. How did you analyze the given XRD file? What are the phases you've found?
What are their space groups?
Answer: I have given all screenshot of the XRD analysis above.
Phase:

Figure 07: Phases found in XRD analysis

Percentage of Bismuth iron (III) oxide is 87.

Percentage of Bi2O3 is 13.

Space Group: (From XRD data)

Bismuth iron (III) oxide: R 3 c
Bi2O3: F m -3 m

Question 3. Find out the crystallite size using Scherrer equation.

Answer:
Peak selection and FWHM determination:

Figure 08: XRD pattern plotting in Origin Pro Software

 Figure 09: Peak Selection for FWHM calculation

Figure 10: Curve Fit for FWHM Calculation

Data from the Curve:

FWHM = 0.63864
2θ=31.8571
Crystallite Size calculation:
𝑘𝜆
We know, Scherrer equation, 𝐷 = 𝐹𝑊𝐻𝑀∗𝐶𝑂𝑆θ

k = 0.9

λ = 1.5604 Å
0.9 ∗ 1.5604
𝐷=
0.63864 ∗ 𝐶𝑂𝑆 (15.929)

𝐷 = 2.287 Å (Ans)

Question 4. Find out the d spacings for at least 3 crystallographic planes. If you
couldn't find it, give appropriate reasons behind it in the discussion section.
Answer:

Figure 11: Peak selection to determine 2θ value

 Figure 12: Value of 2θ of the 8 selected peak

d spacing calculation for crystallographic planes:

For Bismuth iron (III) oxide:

2θ Sin θ d spacing hkl

nλ
(𝑑 = 2𝑆𝑖𝑛θ)

22.36107 0.1939 4.024 012

31.85741 0.2744 2.843 104
39.44002 0.3374 2.312 202

For Bi2O3:

2θ Sin θ d spacing hkl

45.83092 0.3894 2.004 022

27.90266 0.2411 3.236 111

For Bi2O3, only two plane (hkl) is found.

We know, XRD Diffraction occurs only when Bragg’s Law (2𝑑 𝑆𝑖𝑛𝜃 = 𝑛𝜆) is satisfied Condition
for constructive interference from planes with spacing d. Different planes have different spacings.
As d changes, θ will also change. All planes do not show satisfy condition for constructive
interference in XRD analysis. Diffraction of planes depends on the crystal structure.
Reference:
[1] Class Lecture Provided by Course Teachers.
[2] X-ray Powder Diffraction (XRD). (n.d.). Techniques. Retrieved January 20, 2021, from

https://serc.carleton.edu/research_education/geochemsheets/techniques/XRD.html