Ordnance Factory Inst.

Course: Defect Investigation Analysis with case studies

[1]

Defect Investigation and Metallurgical Tools Used

Debalay Chakrabarti
Professor
Department of Metallurgical & Materials Engineering
Indian Institute of Technology Kharagpur
February, 2023
 [2]
Failure tree:
Indication, Symptom
(noise, vibration etc.)

Visible causes

Hidden causes
 [3]
Improving the quality of cast ingot for
the production of defect-free rolled and
polished blanks of Silver-Copper
coinage alloy

Debalay Chakrabarti,
Prof. Sanat Kumar Roy, Prof Ajit Kumar
IIT Kharagpur Chakrabarti,
IIEST Shibpur
[4]
 [5]
Surface Laps
 [6]

Inclusions

Micro-Porosity

Ag-rich phase

Cu-rich phase

10 m
10 m
 [7]

Pores

200 m
 [8]

Sulphide

Crack

RD

ND
 [9]
Ca, C and O

20 m
20 m
 [10]
Borax + CaCO3
(a) (b)
Al-deoxidized

20 m 2020mm
20 m
(c)
Cu-P (d)
Mg-deoxidized

20 m 20 m
20 m 20 m
 [11]
A case study on tank barrel steel
Chemical Composition (wt%.) of T-72/T-90 barrel used in this study
C Si S P Mn Ni Cr Mo V H N O
0.3- 0.2- 0.01 0.01 0.2- 3.0- 0.8- 0.5- 0.1- 2 ppm 120 30
0.4 0.4 0.5 3.5 1.2 0.7 0.2 ppm ppm
 [12]

Streaking after Nital etching

 [13]

Optical micrographs of the cross-sections of the failed barrels (etched with Picral
solution) showing banded patterns in longitudinal (Long) section

The tank-barrel material was failing in fracture toughness test and it

was non-responsive to tempering treatment
 [14]

Dendritic-type pattern in transverse (trans) section at

different locations of the barrel
Sample – 1: Longitudinal direction [15]

BSE Image

Band 1

Band 2

Band 3

Band 4

Area that was scanned

BSE image of the actual area that has been scanned as mentioned in
the last photograph – generated from EPMA [16]

200 m
 EPMA analysis of elemental distribution [17]

Chromium Manganese

Molybdenum Nickel
 [18]

In the longitudinal sample, a smaller area

encompassing the rectangle was also scanned

The scan area has two bands as seen within the

rectangle

In this case the step size was kept 1 µm and dwell time of 30 msec.
Silicon was also scanned with other elements
Chromium Manganese Molybdenum [19]

Silicon Nickel Phosphorous

Sulphur

• Segregation is seen for Chromium, Manganese, Silicon

and Molybdenum.
• Segregation is very mild for Nickel and Phosphorous.
• Segregation of Sulphur could not be detected.
Sample – 1: Transverse direction [20]

BSE Image
Band 1

Band 2

Band 3

Band 4
Chromium Manganese Molybdenum [21]

Nickel Phosphorous Sulphur

 [22]
𝑆𝑒𝑔𝑟𝑒𝑔𝑎𝑡𝑖𝑜𝑛 𝐿𝑒𝑣𝑒𝑙 %

𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝐶𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑖𝑜𝑛 𝑤𝑡. % − 𝑀𝑖𝑛𝑖𝑚𝑢𝑚 𝐶𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑖𝑜𝑛 (𝑤𝑡. %ሻ

=
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐶𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑖𝑜𝑛 (𝑤𝑡. %ሻ
Sl. Element Level of Segregation
1 Cr 20%
2 Si 20%
3 Mn 15%
4 Mo 15%
5 Ni 5%
6 S Localized
P Localized
Although the elemental distribution obtained from EPMA analysis is more of a qualitative nature,
the level of segregation of different alloying elements are estimated from the quantitative
information obtained in the form of variation in elemental contrast (in wt. %)
 [23]
In order to analyse the severity of segregation in the tank-barrel steel of the Metal
and Steel Factory, Ishapore, a recent study of segregation performed at the
University of Warwick in UK is presented

Study on the detection of Mn-segregation bands in rolled steel.

 [24]

Segregation of
elements in as-
cast structure
 [25]
Segregation of Nb in dendritic cast structure of HSLA steel

(a)
(b)

If 0.05% Nb is added, Nb content will be higher at interdendritic solute-rich

regions (say, 0.08%) and lower at dendritic solute-depleted regions (say, 0.02%)
Typical microstructures from different locations [26]
 [27]
Typical microstructure: Tempered martensite
Samples not responding to tempering [28]
Samples not responding to tempering [29]
 [30]

0.1 C/s

1 C/s
10 C/s

100 C/s

CCT diagram of the investigated steel

predicted from JMatPro® software,
considering the nominal composition of
the investigated steel.

According to the CCT diagram, a cooling-rate higher than 0.85 C/s is required to avoid the
bainite-bay and achieve a fully martensitic microstructure. If the cooling-rate remains lower
than the above-mentioned critical value, then bainite is expected to form. Slower the cooling-
rate, higher is the bainite fraction expected even if a completely uniform composition is
considered throughout the microstructure. Such a situation can particularly arise near the
mid-thickness of the barrel cross-section where the cooling-rate is expected to be the lowest
(compared to the outer and inner surfaces).
 [31]
CCT diagram of the investigated steel
predicted from JMatPro® software,
considering the compositions of
solute-enriched regions (+10%) and
solute-depleted regions (-10%). P and
B stand for pearlite and bainite
transformation lines.

If segregation is considered, at the solute-depleted regions, the hardenability is lower, i.e., the
critical cooling-rate required for achieving complete martensite microstructure (avoiding the
bainite formation) is higher (3.1 C/s), as compared to the solute-enriched regions (0.75 C/s).
Therefore, whenever the cooling during oil-quenching is not sufficiently strong for any reason,
significantly bainite transformation (particularly upper bainite formation) is expected
particularly at the solute-depleted regions.
 [32]
Recommendation:
For any quenched and tempered steel, quenching is a very important step that needs to be
performed carefully and rapidly. Although the investigated steel is a medium C steel (0.33-
0.40 wt.% C), it contains several carbide formers like Cr, Mo and V. As those elements form
carbides, the C content in solution reduces that consequently reduces the hardenability of the
steel. If the cooling-rate is not sufficiently strong during oil quenching, there is a high change
of bainite formation. Since the steel contains coarse carbide particles and some inclusions as
the crack initiators, presence of large upper bainite regions with as-cooled martensite
(untampered) helps the propagation of the crack and leads to the final failure. Therefore, the
oil quenching treatment should be done properly. Besides, drive should continue to make the
steel cleaner. A systematic experimental study can be undertaken on the ‘temper
embrittlement’ phenomenon in the barrel steel.
 [33]
Conclusions:

• Formation of bainitic ferrite rejects carbon which stabilizes the surrounding

martensite into retained austenite in the as-quenched structure. Upon tempering
retained austenite releases additional C and alloying elements in the form of carbide-
precipitates and become unstable. As a result blocky regions of untampered
martensite can form the in the final tempered microstructure. Such regions can be
the potential sites for the initiation and propagation of cleavage cracks.
• More the tempering is performed, more retained austenite transform into
untampered martensite and carbides, and the toughness can deteriorate upon
tempering, overcoming the beneficial effect of tempering by softening the
microstructure.
• In Certain samples clusters of coarse non-metallic inclusions (MnS, CaS, Al2O3 and
cuboidal TiN) were detected. Such inclusions, their combinations and clusters can
significantly affect the toughness of the steel.
 [34]

Defect generation in metal processing

Debalay Chakrabarti
Professor
Department of Metallurgical & Materials Engineering
Indian Institute of Technology Kharagpur
February, 2023
 [35]
Preparation of melt:
• Liquid metal – containing other elements,

• Alloy preparation – substation / addition of elements,

• Ladle treatment, secondary refining / desulphurization –

compositional adjustment,

• AOD / VOD –Degassing,

Desired (Specified) composition range must be ensured. Avoid dross,

deoxidation, desulphurization products, refractory pick-up –
dissolved gasses. Removal of inclusions and gases is the key.
 [36]
Casting defects
• Slag entrapment, Sand pick-up, Refractory entrapment,
• Dimensional inaccuracy.
• Hot-tearing / solidification cracking.
• Segregation – macro/Micro.
• Non-uniform cooling – hard/soft spot formation.
• Solidification shrinkage - micro/macro,
• Gas porosity – pouring temperature, degassing treatment,
• Residual stress generation.
• Improper mould filling – laps.
• Surface defects,
• Mould vibration marks in continuous casting,
• Hot cracking,
• Nozzle clogging.
 [37]
Casting defects – Crack, porosity

Typical Problems:
 [38]
Casting defects –
macro / micro -
segregation

Top
Mould
wall

Liquid

Solid
Dendrite

Bottom
[Flemings 1967]
 [39]
Casting defects – Edge / Corner Crack
 [40]
Casting defects – Oscillation mark, hook
 [41]
Defects in reheating / soaking

• Oxidation, Reaction,

• Grain Coarsening,

• Localized melting,

• Lack of homogenization,
 [42]
Reheating of cast slab

Cast structure Reheat structure

More
100 m
homogeneous
Cast structure Reheat structure
[43]

100 m
More homogeneous

900C 1050C 1200C

 Slab De-scaling [44]

Rolled-in Oxides
 [45]
Hot-deformation: Plate rolling
Manufacturing / Processing: [46]

• Dimensional inaccuracy – Elastic deformation, Flattening, Wear and

Tear of the tool, die, roll, platen etc.,

• Incorrect profile – bending, waviness,

• Cracking and fracture, Splitting – different types of cracks,

• Hot-tearing,

• Microstructural banding, Mechanical fibering, flow lines – Anisotropy,

• Structure and property variation through the thickness, local scale

heterogeneity,

• Strain-hardening and brittleness.

• Poor surface finish.

 [47]

Rolling

Hot rolling Cold rolling

Typically, T > 0.5 Tm Typically, at R.T

Above Recrystallization Temperature Below Recrystallization Temperature

 [48]
Hot-rolling: Microstructural Banding due to segregation

TiN

❑ Banding leads to
cracking and anisotropy

❑ H - Cracking
 [49]
Inhomogeneous Deformation

Partial recrystallization, Temperature-Strain-Microstructure variation,

Overheating / undercooling of the surface
 Grain size variation along the thickness [50]

Sub Surface Mid-thickness

Grain size increases with the increase in distance from the surface
 Alignment and Cracking along with inclusions
[51]
Remedy: Use low S (clean) steel Use vacuum degassing to remove gases, (O, H)

Mechanical Fibering
Development of Metallurgical Structure during cooling [52]
 [53]
Coiling
Accelerated cooling
Hot-rolling
Quenching of rolled plates [54]
[55]
 [56]
Roll radius and roll gap

R o
hmin =
E

hmin: Limiting thickness in rolling

 [57]
Deflection of roll – Change in profile

Burn-out

Edge camber

Out of square ness

Defects due to roll deflection [58]
Wavy edge and Zipper creak [59]
Edge cracking, splitting, alligatoring [60]

Through thickness
variation in deformation.

Surface under tension and

Centre under compression.
Preferential deformation at
centre.
 [61]
Surface defects in rolling and remedy

Improper Roll Surface / Slab surface - Cracks, shells, sand

patches and sharp edged seams are always considered defects

❑ Shot blasting, ❑ Grinding, ❑ Welding

 [62]
Welding/ Joining defects
• Weak joint,

• HAZ, Microstructural and Property variation at local scale,

• Cracking,

• Pick up of [H] or other gaseous elements,

• Dross entrapment inside weld pool, inclusion formation,

• General solidification related problems, cracking, segregation,

embrittlement,

• Residual stress,

• Brazing/Soldering – use of too high pressure/ temperature.

[63]
 [64]
Different Types of Weld Cracking and distortion
 [65]
Machining
• Mechanical – Shear stress, Heavy deformation and strain-
hardening. Cracking. Residual stress generation.

• Thermal – Laser, plasma, electron beam, gas cutting – HAZ

formation, melting and solidification related problems (cracking).

• Chemical – controlled surface dissolution using chemical. Careful

control is essential. Corrosion-fatigue.

• Localized softening.
 [66]
Indentation marking / Embossing / Engraving

• Too heavy load application,

• Marks can act as stress raisers and cause cracking.

• Strain-hardening,

• Too high chemical / electro-chemical attack, even at

microstructural features.

Cracking under dynamic (fatigue or impact) loading.

[67]
 [68]
Non-destructive evolution of defects
 [69]
Despatching
Installation [70]
On-site Inspection – Life Assessment [71]
 [72]

Fractography studies on metal failures

Debalay Chakrabarti
Professor
Department of Metallurgical & Materials Engineering
Indian Institute of Technology Kharagpur
February, 2023
 Strength vs. toughness [73]

Toughness

Ductility

Strength
 [74]

Shape of the fractured specimens for

different modes of fracture
 [75]
Cup and Cone
Ductile Fracture
Metallic Alloys

Flat and Shiny

Brittle Fracture
 [76]

Brittle
Ductile

Effect of specimen thickness on fracture mode

 [77]
Importance of Cleanliness

Elongated inclusions – Elongated inclusions –

Mechanical Fibering Mechanical Fibering
MnS Cerium modified Sulphide
 [78]
Importance of alloy cleanliness

Oxygen content Vol. fraction of 2nd phase

 [79]

Particle initiating void

Ductile fracture surface – coarse and fine dimples

 [80]

Crack initiating point

Ductile fracture surface: Charpy Brittle Cleavage fracture: Charpy

impact testing at Room Temperature impact tested at low temperature
 [81]

Void initiation Void growth Void coalescence

Ductile fracture mechanism

 [82]

Void initiation –
Inclusion cracking /
interface separation
 [83]
Cleavage fracture surface

Transgranular cleavage fracture

 [84]

Cleavage facets

Brittle particle

Cleavage facets with river lines: At lower shelf

 [85]

Facets

Micro-Voids

At transition regime: Micro-voids in thin fibrous

regions between cleavage facets
 [86]

Fibrous Cleavage

Change in fracture mechanism from fibrous to

cleavage in mild steel specimen.
 [87]

Pre-existing crack
inside TiN particle

Weakest Link Theory

 [88]

Hard and Brittle Particle (TiN) Initiated Cleavage Cracking

 [89]

Particle interface
Particle cracking separation

Twin-Particle
interaction

Cleavage cracking from TiN particles

 [90]

Fatigue Failure
 [91]

Fatigue Failures
 [92]

Fatigue Failures
 [93]

Fatigue Failures in Rotor Shaft

 [94]

Fatigue Fracture Surfaces

 [95]

Monotonic Cyclic

Fatigue Crack Initiation:

Intrusion and Extrusion
 [96]

Fatigue Crack Initiation

 [97]

Fatigue Striations
 [98]

Intergranular Fracture

Creep,
Environment Assisted
Cracking,
Embrittlement
 [99]

Intergranular fracture
 [100]

Creep Cavitation: Intergranular fracture

 [101]

Different fracture surfaces:

A summary
 [102]

Stress-corrosion cracking, Corrosion-Fatigue

 [103]

Stress-corrosion
cracking, Corrosion-
Fatigue
 [104]

Corrosion /
Oxidation
induced cracking
 [105]

[H]-induced cracking,
[H]-embrittlement

[H]-Flaking
 [106]

Quench Cracking
 [107]

Tempered Martensitic Embrittlement / Temper Embtlmnt

Temper embrittlement [108]

Key to Metals
 Temper embrittlement [109]

(400-600C)
Slow cooling or isothermal holding over the temperature range of 400-600C.

Reasons:
❑ Carbide precipitation during tempering at packet boundaries / prior-austenite grain
boundaries.
❑ Segregation of impurity elements such as, P, S, N, Sb and Sn.
Reduces the cohesive strength of the grain boundary and results
in intergranular fracture
Thank You