Steel Slag

Information Given
Components Mass%
Other information Provided
Al2O3 0.858
CaO 39.664 XRD Raw data of Batch T1 – T3
Fe2O3 22.168 Info of Sample – NaHCO3 + Slag
K2O 0.068
MgO 2.424 As your sample contains, Iron Oxide, SiO2 as major phases,
Na2O 0.069
P2O5 6.749 it is very important to know all the possible phases to
SiO2 18.566 analyse the XRD data
TiO2 0.929
NiO 0
MnO 0.709 Conditions of generated patterns [Slide 3]
Total 92.204 Cu kα = 1.542 Å
Shape factor = 0.94
XRF data of Tata Steel BOF slag (as it is Peak profile = Gaussian
was used _ No Sieving) Scherrer Crystal size / nm = 85
Intensity Normalized to 100 units
5 August 2023 Information provided or Analyzed is only for Academic Use [HEMANTH] 1
Understand the Phases of your sample
Improper labelling Proper labelling Comments
Al2O3 α - Al2O3 Most stable phase of Alumina @ high temp.
CaO CaO -
α - Fe2O3
Both α & γ - Fe2O3 are stable at relatively high temperature.
Fe2O3 β - Fe2O3
Steel slag might contain any of them.
γ - Fe2O3
K2O K2O -
MgO MgO -
Na2O Na2O -
P2O5 P2O5 -
SiO2 SiO2 Multiple phases are possible with many fusions need to check
Anatase, Rutile &

TiO2 Anatase is very stable at high temperature
Brookite
NiO NiO -
Manganese Oxides have too many phases with wide range of
MnO MnO
stabilities (most misunderstood compound in phase analysis)
XRD patterns of different phases
α - Al2O3 CaO
α - Fe2O3 K2O
Trigonal system
MgO Na2O
P2O5 SiO2
Hexagonal
SiO2 TO2
Cubic Tetragonal
Anatase
NiO MnO
Cubic Cubic
Comparison of all the XRD patterns
All the XRD patterns

are same
Matching patterns of the sample
Link  Your slag XRD mostly matches with (b)
which is Cu / SiO2 sample (composite)
 As your sample doesn’t contain Cu, this
possibility is too less.
 But looking at very broad peak from 20 –
30, the sample contains either Silicon or
Carbon or a blend of it.
 Other possibilities are Silicon dioxide, but
the size is too less
5 August 2023 10
Matching patterns of the sample
Link
 Here it is similar to SiC/C

composite material
 However, it is not good idea to
to deconvolute XRD peaks and
match as it has too many
possibilities.
Problems in the data
 The quality of Raw data given in the sample is very poor. See the counts on Y – axis, it goes to a
maximum of 2000. Good data will have more counts.
 Your sample analysis has been performed on PANalytical Empyrean XRD. That machine has following
problems: a) Slit width is too less for a 2D XRD detector, hence area covered will be lesser. It is advised
to use more slit width for that kind of a machine. b) For that instrument there is no proper Beam
conditioning (used to alter the focus of the incoming X – Rays, if this is not good then at certain angles,
rays will spill off.).
 The sample orientation is not proper. The problem is your sample is not ground into fine powder or it is
not placed on the sample holder properly. This is the reason why your XRD baseline is not straight but
slant and is moving higher. Another reason is presence of Silicon compounds. For this machine, there
will be black colour sample holder which is called Zero background sample holder made of Silicon.
Silicon crystal structure is cracked in such a way that the orientation of the inline beam X-Rays doesn’t
diffract but just will pass through it creating no background. Similar aspect is happening with the sample
as it contains Silicon or its composites, the orientation will never be proper.
 The broad peak from 20 – 34 might correspond to Carbon, Silicon or Silicon dioxide or their composites.
There is a possibility that the sharp peak at 48 might be from the sample holder. The sample holder for
this machine is Aluminium based sample holder. It is advised to perform on Zero background holder or
to use Xpert model of XRD. A simple way to check this is perform a scan off empty sample holder for 10
min. This will clearly differentiate or clarify the doubt.
Problems in the data
 To improve the quality of your data, the following things can be done –
 Grind your sample well, there should be no lumps or chunks
 Perform beam conditioning on the machine
 If the sample shows Fluorescence, increase the step size to 0.05 and increase the scan time.
 The present sample scan time is too less, perform at least 90 min to get good XRD (step size = 0.05)
 Your sample doesn’t have much problem of fluorescence. If you adopt the above two methods, the
problem will be solved. No need to use Cobalt or any other source rays.
 Though your sample contains too many metal oxides as confirmed by XRF data, your XRD doesn’t
show up anything. Deconvoluting XRD data is generally a bad process when these many oxides are
present. This might be due to the presence of too much of Carbon possibly on the surface covering the
oxides. It is either advised to burn this carbon off at high temperature or to finely grind your sample to
20 micron.
 Though you have identified the composition with XRF, it is advised to do the same with EDS. One of the
best complementary method to check the presence of metals is ICP MS and this will be more accurate.
This will not tell you composition, but it will give you a list of metals in it which can be verified with XRF.
 In most papers I have seen there is no proper mentioning of the phases using XRD. This can be
addressed clearly.
 Possibility of formation of composites with other compounds can also be checked.
 If your application is to extract these metals, try leaching with DES (very powerful and effective)

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Steel Slag

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Anatase, Rutile &

All the XRD patterns

 Here it is similar to SiC/C

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