Morphological and compositional changes in Tiny Rolled in Scale due to BAF

annealing
Authors: Nikhil Ramakrishnan, S Dhara, MBN Raju
Team: USP, DK, KKO, TT, SKJ, SC, MA, AD
Depts : FPTG/SS/CRM
Background: Rolled in Scale is an HR surface defect. Smaller sized defects (<1mm) are barely visible
even during inspection at Recoiling lines. This leads to the defect being missed and subsequent customer
complaints.
Presently, this tiny Rolled in Scale is identified by porous, entrapped particles at defect location and the
presence of Oxygen detected by EDAX. However there have been some customer complaint samples (see
for example FP/SOUTH/MADS/ST/2011-2012/79) where only one or the other features have been
identified, leading to confusion about the nature of this defect. Little information was available on the
origin of the porosity regularly found on RIS particles.
Experiments:
The present work aimed at imaging the tiny RIS defect at FHCR stage and track the structural and
compositional changes of the defect after annealing in the 100% H2 (3-10ppm O2, and products of
reactions of hydrocarbons on strip surface with H2) environment. An attempt was made to determine the
origin of the porosity regularly found in the RIS particles and the degree of reduction on the defect
surface so as to correctly identify the defect in future.
Part I: FHCR
FHCR samples of skin panel coil 215614 MU04 (PABSY) were taken from TCM HE (ID). The samples
were identified visually as the defect Tiny RIS by TCM inspection crew as well as by RCL#3
inspectors.

The general view of the sample with surface defect is shown. Tiny line type marks are observed when
observed minutely (Fig. 1B). The defect was also observed under stereoscope. A shallow impression

mark was observed. The region was observed under SEM after ultrasonic cleaning. The observations are
shown in Fig. 3A and Fig. 3B. Small irregular shaped particles are observed over the surface. EDS
analysis on those particles show strong peaks of O and Fe along with occasional peaks of Al. Thus,
confirming presence of iron oxide particles at the defect region.

At one particular location (Fig 3c.), no particulate matter was found. This indicates the RIS particles are
being removed in the FHCR stage itself, leaving behind what appear to be contours of the defect on the
FH strip. The absence of RIS particles in complaint/RCL samples should not automatically disqualify it
from being a preexisting RIS defect.
Part II: After BAF defect samples
The defect samples were placed carefully within a BAF stack to replicate the actual conditions a defect
sample would face in regular production. The cycle chosen was HIFS720_690. Soaking time was
17hr04min, with total H2 consumption logged 369m3. No cycle abnormality was noted.
SEM examination:

The SEM observations are shown in Fig. 6B, Fig. 7B. Small irregular shaped particles porous in nature
were observed at higher magnification. The origin of the pores is thus established as being BAF
annealing.
EDS analysis on those particles shows peaks of Fe only:

Taken together, the porosity and lack of Oxygen in the annealed samples suggest that reduction of the
Iron oxide RIS particles in the BAF environment has occurred.
Conclusions:
1. Particles from the Tiny RIS defect are being removed in the FHCR stage itself

2. The defect in FHCR stage appears non porous and contains Oxygen (approx 30% by EDAX)
3. The defect after annealing in the BAF environment appears porous and with no Oxygen
suggesting complete reduction at surface