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Silicon XRD Peaks Analysis Report

The sample is 99.7% calcium phosphate (Ca3(PO4)2) and 0.3% silicon dioxide (SiO2). The elemental composition is 41.3% oxygen, 38.65% calcium, 19.91% phosphorus, and 0.14% silicon. The peaks in the XRD pattern were indexed and matched to calcium phosphate and silicon dioxide entries in the inorganic crystal structure database.

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63 views3 pages

Silicon XRD Peaks Analysis Report

The sample is 99.7% calcium phosphate (Ca3(PO4)2) and 0.3% silicon dioxide (SiO2). The elemental composition is 41.3% oxygen, 38.65% calcium, 19.91% phosphorus, and 0.14% silicon. The peaks in the XRD pattern were indexed and matched to calcium phosphate and silicon dioxide entries in the inorganic crystal structure database.

Uploaded by

Nazar Jabbar
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

Match!

Phase Analysis Report

Sample: 371
Sample Data
File name [Link]
File path C:/Users/nzsh/Desktop/xrd/FIRST GROUP/371
Data collected Feb 28, 2022 20:00:28
Data range 10.000º - 90.000º
Original data range 10.000º - 90.000º
Number of points 2401
Orig. number of points 401
Step size 0.033
Original step size 0.200
Rietveld refinement converged No
Alpha2 subtracted No
Background subtr. No
Data smoothed No
Radiation X-rays
Wavelength 1.541874 Å

Matched Phases
Index Amount (%) Name Formula sum
A 99.7 Ca3 (P O4)2 Ca3 O8 P2
B 0.3 Si O2 O2 Si
32.2 Unidentified peak area
Amounts calculated by RIR (Reference Intensity Ratio) method after manual adjustment of intensity scaling factor(s)

Elemental composition of sample (identified crystalline phases only)

Element Amount (weight %)


O 41.30%
Ca 38.65%
P 19.91%
Si 0.14%
LE (sum) 41.30%

Matching entry details

A: Ca3 (P O4)2 (99.7 %)*


Formula sum Ca3 O8 P2
Entry number 96-151-7239
Figure-of-Merit (FoM) 0.636781*
Total number of peaks 250
Peaks in range 250
Peaks matched 76
Intensity scale factor 0.49*
Space group R3c
Crystal system trigonal (hexagonal axes)
Unit cell a= 10.4352 Å c= 37.4029 Å
I/Ic 1.22
Calc. density 3.058 g/cm³
Reference Kamiyama T., Hoshikawa A., Yashima M., Sakai A., "Crystal structure analysis of beta-tricalcium phosphate
Ca3(PO4)2 byneutron powder diffraction", Journal of Solid State Chemistry 175, 272-277 (2003)

B: Si O2 (0.3 %)*
Formula sum O2 Si
Entry number 96-810-3727
Figure-of-Merit (FoM) 0.236134*
Total number of peaks 192
Peaks in range 74
Peaks matched 20
Intensity scale factor 0.00*
Space group P 63/m m c
Crystal system hexagonal
Unit cell a= 5.0520 Å c= 8.2700 Å
I/Ic 3.04
Calc. density 2.183 g/cm³
Reference Kihara K., "Thermal change in unit-cell dimensions, and a hexagonal structure oftridymite", Zeitschrift fuer
Kristallographie, Kristallgeometrie, Kristallphysik,Kristallchemie (145,1977-148,1979) 148, 237-253 (1978)
(*)2theta values have been shifted internally for the calculation of the amounts, the intensity scaling factors as well as the figure-of-merit (FoM), due to
the active search-match option 'Automatic zero point adaption'.

Search-Match
Settings
Reference database used COD-Inorg 2021.12.14
Automatic zeropoint adaptation Yes
Downgrade entries with low scaling factorsYes
Minimum figure-of-merit (FoM) 0.60
2theta window for peak corr. 0.30 deg.
Minimum rel. int. for peak corr. 0
Parameter/influence 2theta 0.50
Parameter/influence intensities 0.50
Parameter multiple/single phase(s) 0.50

Criteria for entries added by user


Reference:

Entry number: 96-151-7239;96-152-1427;96-210-6195;96-900-5866;96-101-0922;96-101-0939;96-101-0945;96-101-


0955;96-101-1098;96-101-1160;96-101-1173;96-101-1177;96-101-1201;96-110-0020;96-150-5107;96-152-
6861;96-153-0729;96-153-2513;96-153-2514;96-153-2515;96-153-5067;96-153-6390;96-153-6407;96-153-
6410;96-153-6929;96-153-7208;96-153-8065;96-153-9864;96-153-9935;96-154-4732;96-154-4733;96-154-
4734;96-154-4735;96-154-4736;96-154-4737;96-154-5150;96-154-5151;96-154-5152;96-154-6346;96-210-
0189;96-210-0336;96-210-6356;96-230-0111;96-230-0371;96-400-2432;96-400-2433;96-400-2434;96-400-
2435;96-400-2436;96-400-2438;96-400-2439;96-400-2440;96-400-2441;96-400-3211;96-411-0503;96-411-
5457;96-411-5458;96-411-5459;96-411-7379;96-412-4028;96-412-4029;96-412-4030;96-412-4031;96-412-
4032;96-412-4033;96-412-4034;96-412-4035;96-412-4036;96-412-4037;96-412-4038;96-412-4039;96-412-
4040;96-412-4041;96-412-4042;96-412-4043;96-412-4044;96-412-4045;96-412-4046;96-412-4047;96-412-
4048;96-412-4049;96-412-4050;96-412-4051;96-412-4052;96-412-4053;96-412-4054;96-412-4055;96-412-
4056;96-412-4057;96-412-4058;96-412-4059;96-412-4060;96-412-4061;96-412-4062;96-412-4063;96-412-
4064;96-412-4065;96-412-4066;96-412-4067;96-412-4068;96-412-4069;96-412-4070;96-412-4071;96-412-
4072;96-412-4073;96-412-4074;96-412-4075;96-412-4076;96-412-4077;96-412-4078;96-412-4079;96-412-
4080;96-412-4081;96-412-4082;96-412-4083;96-412-4084;96-412-4085;96-412-4119;96-412-4490;96-412-
4646;96-500-0036;96-591-0148;96-710-3015;96-720-2757;96-720-2758;96-720-2759;96-722-4241;96-722-
4242;96-722-4243;96-722-4244;96-810-3514;96-810-3692;96-810-3727;96-810-4323;96-810-4535;96-810-
4536;96-810-4537;96-810-4538;96-810-4539;96-810-4540;96-810-4541;96-900-0521;96-900-0776;96-900-
0777;96-900-0778;96-900-0779;96-900-0780;96-900-0781;96-900-0803;96-900-0804;96-900-0805;96-900-
0806;96-900-0807;96-900-0808;96-900-0809;96-900-1277;96-900-1278;96-900-1279;96-900-1280;96-900-
1281;96-900-1282;96-900-1283;96-900-1284;96-900-1579;96-900-1580;96-900-1581;96-900-1582;96-900-
1683;96-900-1684;96-900-2649;96-900-2650;96-900-2783;96-900-5018;96-900-5019;96-900-5020;96-900-
5021;96-900-5022;96-900-5023;96-900-5024;96-900-5025;96-900-5026;96-900-5027;96-900-5028;96-900-
5029;96-900-5030;96-900-5031;96-900-5032;96-900-5033;96-900-5034;96-900-5116;96-900-5270;96-900-
5271;96-900-5797;96-900-5798;96-900-5799;96-900-5800;96-900-5801;96-900-5853;96-900-5854;96-900-
5855;96-900-5856;96-900-6285;96-900-6286;96-900-6287;96-900-6288;96-900-6289;96-900-6290;96-900-
6291;96-900-6292;96-900-6293;96-900-6294;96-900-6295;96-900-6296;96-900-6297;96-900-6298;96-900-
6299;96-900-6300;96-900-6301;96-900-6302;96-900-6303;96-900-6304;96-900-6305;96-900-6306;96-900-
6307;96-900-6308;96-900-6969;96-900-7151;96-900-7152;96-900-7153;96-900-7154;96-900-7155;96-900-
7162;96-900-7163;96-900-7164;96-900-7165;96-900-7166;96-900-7167;96-900-7168;96-900-7169;96-900-
7170;96-900-7171;96-900-7172;96-900-7379;96-900-7531;96-900-8093;96-900-8094;96-900-8111;96-900-
8177;96-900-8225;96-900-8226;96-900-8227;96-900-8228;96-900-8229;96-900-8230;96-900-8231;96-900-
8232;96-900-8233;96-900-8234;96-900-8235;96-900-8281;96-900-8309;96-900-8416;96-900-8417;96-900-
9219;96-900-9239;96-900-9667;96-900-9686;96-900-9687;96-900-9688;96-901-0144;96-901-0145;96-901-
0146;96-901-0147;96-901-1481;96-901-1494;96-901-1495;96-901-1496;96-901-1497;96-901-2601;96-901-
2602;96-901-2603;96-901-2604;96-901-2605;96-901-2606;96-901-2692;96-901-3322;96-901-3394;96-901-
3427;96-901-3428;96-901-3492;96-901-3493;96-901-3494;96-901-4260;96-901-4437;96-901-4487;96-901-
5023;96-901-5088;96-901-5310;96-901-5393;96-901-5792;96-901-6226;96-901-6250;96-901-6401;96-901-
6404

Peak List
No. 2theta [º] d [Å] I/I0 (peak height) Counts (peak area) FWHM Matched
1 14.30 6.1939 76.36 10.27 0.4000 A
2 17.60 5.0393 175.16 23.56 0.4000
3 22.50 3.9517 150.96 20.31 0.4000 A
4 26.50 3.3636 442.98 59.59 0.4000 A
5 28.50 3.1319 567.01 76.27 0.4000 A
6 31.70 2.8227 1000.00 134.52 0.4000
7 33.60 2.6673 448.46 60.33 0.4000 A
8 35.10 2.5567 823.59 110.79 0.4000 A
9 36.20 2.4815 164.07 44.14 0.8000 A
10 38.00 2.3680 136.34 36.68 0.8000 A
11 40.50 2.2274 285.39 38.39 0.4000 A
12 42.50 2.1271 184.84 37.30 0.6000 B
13 44.10 2.0536 135.00 54.48 1.2000 A,B
14 45.60 1.9894 99.98 40.35 1.2000 A
15 47.70 1.9066 384.03 51.66 0.4000 A
16 48.80 1.8662 352.00 71.03 0.6000 B
17 50.10 1.8208 271.05 36.46 0.4000 A
18 51.10 1.7875 205.46 27.64 0.4000 A
19 53.70 1.7069 490.32 98.94 0.6000 A,B
20 55.10 1.6668 82.10 11.04 0.4000 A
21 56.60 1.6261 72.96 14.72 0.6000 A,B
22 58.30 1.5827 71.10 9.56 0.4000 A
23 60.30 1.5349 207.02 27.85 0.4000 A,B
24 62.30 1.4904 113.28 22.86 0.6000 A
25 64.40 1.4467 191.71 51.58 0.8000
26 67.00 1.3968 86.92 11.69 0.4000
27 68.20 1.3751 76.44 10.28 0.4000 B
28 71.90 1.3132 102.02 27.45 0.8000 B
29 74.20 1.2781 112.29 30.21 0.8000
30 77.10 1.2371 203.31 82.05 1.2000
31 78.90 1.2133 96.47 12.98 0.4000 B
32 84.00 1.1521 96.81 13.02 0.4000
33 87.30 1.1169 294.24 118.74 1.2000
34 89.20 1.0980 126.77 17.05 0.4000

Integrated Profile Areas


Based on calculated profile

Profile area Counts Amount


Overall diffraction profile 107219 100.00%
Background radiation 60686 56.60%
Diffraction peaks 46533 43.40%
Peak area belonging to selected phases 11957 11.15%
Peak area of phase A (Ca3 (P O4)2) 11892 11.09%
Peak area of phase B (Si O2) 65 0.06%
Unidentified peak area 34576 32.25%

Diffraction Pattern Graphics

Match! Copyright © 2003-2022 CRYSTAL IMPACT, Bonn, Germany

Common questions

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The intensity scale factors adjust the relative heights of peaks in the diffraction pattern to account for differences in sample preparation or measurement conditions. In this report, adjusting these factors was crucial for accurate quantification using the RIR method, ensuring the intensity values properly reflect the true composition of the phases present .

Unidentified peak areas, which constitute 32.25% of the total diffraction profile, pose significant challenges to the phase analysis by introducing uncertainties into the identification and quantification of phases. This results in possible misidentification and inaccurate reporting of sample composition, as the presence of unknown phases can interfere with the determined proportions of identified phases .

The reference intensity ratio (RIR) method is used to quantify phases by comparing the intensities of a sample's peaks to those of known standards. In this analysis, the RIR method was applied after manual adjustment of the intensity scaling factor, allowing the quantification of Ca3(PO4)2 and SiO2 in terms of weight percentages within the sample .

The calculated density of Ca3(PO4)2 is 3.058 g/cm³ and that for SiO2 is 2.183 g/cm³. These values are derived from the crystallographic parameters such as unit cell dimensions and atomic weights within the respective crystal structures. Accurate determination of these parameters allows calculation of the density, which relates to the packing arrangement and mass of the elements within the unit cell .

For Ca3(PO4)2, the unit cell parameters are a = 10.4352 Å and c = 37.4029 Å, characteristic of its trigonal crystal system with space group R 3 c. For SiO2, the parameters are a = 5.0520 Å and c = 8.2700 Å, reflecting its hexagonal crystal system with space group P 63/m m c .

The primary phases identified in the X-ray diffraction analysis are Ca3(PO4)2, accounting for 99.7%, and SiO2, which comprises 0.3% of the sample. These proportions were calculated after manual adjustment of intensity scaling factors using the RIR method .

The figure-of-merit (FoM) indicates the quality of match between observed and reference diffraction patterns. For Ca3(PO4)2, the FoM is 0.636781, suggesting a high degree of confidence in phase identification, whereas the FoM for SiO2 is lower at 0.236134, indicating less confidence. This suggests that the phase identification of Ca3(PO4)2 is more reliable than that of SiO2 due to better alignment with referenced data .

In the given data, the X-ray diffraction pattern is unsmoothed, meaning that no processing was used to reduce noise or enhance peak visibility. Smoothing is typically used to make peaks more discernible by reducing random noise, but it can also obscure subtle details. The decision not to smooth the data may be aimed at preserving the fidelity of original signals for accurate phase identification and quantification .

Space groups determine the symmetry and possible atomic arrangements within a crystal, affecting its physical properties. Ca3(PO4)2 belongs to space group R 3 c, resulting in trigonal symmetry, which can affect its stability and optical properties. SiO2's space group, P 63/m m c, implies hexagonal symmetry, impacting properties like thermal expansion and elastic anisotropy. These symmetries and atomic arrangements significantly influence how these materials interact with external forces or energy .

Automatic zeropoint adaptation adjusts the 2theta values to correct for any misalignment of the instrumental zero point. This ensures the accuracy of the peak positions during the search-match process. In this analysis, it allowed for more reliable determination of the substances present by aligning the two-theta values correctly with reference database entries .

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