Journal of Magnetism and Magnetic Materials 491 (2019) 165578

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Journal of Magnetism and Magnetic Materials

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Research articles

Evaluation of electric and magnetic signals in heat-resistant HP alloys using T

scanning probe microscopy
⁎
M.P. Arenasa,b, C.J. Pachecoa, , A.B. Fonsecaa,b, F.S. Queirozb, M. Gaudencioa,b, C.B. Ecksteinc,
L. Nogueirac, L.H. De Almeidab, J.M.A. Rebellob, B. Nystend, G.R. Pereiraa,b
a
Non-destructive Testing, Corrosion and Welding Laboratory, LNDC/COPPE, Rio de Janeiro, Brazil
b
Metallurgical and Materials Engineering Program PEMM/COPPE, Federal University of Rio de Janeiro, Brazil
c
Petrobras, Rio de Janeiro, Brazil
d
Institute of Condensed Matter and Nanosciences – Bio and Soft Matter, Université Catholique de Louvain, Croix du Sud 1/L7.04.02, B-1348 Louvain-la-Neuve, Belgium

A R T I C LE I N FO A B S T R A C T

Keywords: HP steels are commonly used in steam reforming tubes, which are exposed to harsh operational conditions
Heat-resistant alloys causing microstructural changes. These microstructural changes cause variations in the magnetic properties,
Aging states which can be measured by different techniques. This work aims at the measurement of the magnetic and electric
Magnetic force microscopy variations in HP-Nb modified alloys with different chemical composition using scanning probe microscopy
Kelvin probe force microscopy
(SPM) techniques. The results show that, despite the microstructural change due to variation of chemical
Contact potential difference
composition, samples with aging state I exhibit a magnetic response at the carbides boundary, while for ad-
vanced aging states, the magnetic response is not evidenced.

1. Introduction tend to coalesce, and a secondary chromium precipitation is initiated at

the intradendritic region. In addition, for HP-Nb modified alloys, Nb
HP steels are commonly used in steam reforming tubes, which are carbides are partially transformed into G-phase [5,6]. By using SEM and
responsible for the production of hydrogen. These tubes operate in a SPM techniques, this study found that HP samples with same aging
condition where they are exposed to a gradient of temperature along state, but different chemical composition, present similar behavior
their length causing microstructural evolution which can be classified concerning to their magnetic response (all samples with aging state I
in different aging states [1,2]. Reforming furnaces are composed of presented magnetic response at the carbides boundaries). Thus, a cor-
hundreds of tubes, which chemical composition may vary slightly as relation between microstructural modifications and the variations of
they do not necessarily come from the same manufacturer. It is ex- the magnetic response [1,2,4,7,8], allow implementing reliable non-
tremely important to guarantee that these chemical composition var- destructive electromagnetic techniques for measuring the structural
iations do not affect their magnetic response, which ensures high re- condition of HP reformer tubes. This type of procedure allows to draw
liability of nondestructive inspections during the scheduled shutdowns. important conclusions for programming occasional replacements and/
Accordingly, this work aims at measuring the local magnetic response or components repair, avoiding major expenses with corrective main-
of HP-Nb modified alloys using scanning probe microscopy (SPM) tenance [9,10].
techniques with the objective of identifying if microstructural changes,
caused by variation in chemical composition, affect the magnetic re- 2. Samples and methods
sponse in samples with same aging state.
The microstructure morphological characterization of each aging 2.1. Sample description
states is well described by Le May et al. [3]. Therefore, this criterion
was used to classify the analyzed samples. Samples with aging state I or HP-Nb modified samples were extracted from three different steam-
in the as-cast condition present an austenitic matrix with interdendritic reforming tubes with different operating time and chemical composi-
chromium rich carbides and niobium carbides (NbC) [4]. As the ma- tion, regarding mainly the niobium and titanium content, as observed
terial is exposed to temperatures above 600 °C, the primary carbides in Table 1. The chemical composition was measured using a carbon and

⁎
Corresponding author.
E-mail address: [email protected] (C.J. Pacheco).

https://doi.org/10.1016/j.jmmm.2019.165578
Received 21 March 2019; Received in revised form 15 July 2019; Accepted 15 July 2019
Available online 22 July 2019
0304-8853/ © 2019 Elsevier B.V. All rights reserved.
M.P. Arenas, et al. Journal of Magnetism and Magnetic Materials 491 (2019) 165578

Table 1
Chemical composition (wt%) of HP-Nb modified austenitic stainless steel samples compared with the standard ASTM A608 [11].
Tube Ni Cr C Nb Ti Si Zr

ASTM A608 34–37 24–27 0.38–0.45 0.5–1.5 – 0.5–1.5 –

A 34.0 ± 0.1 26.1 ± 0.1 0.44 ± 0.01 0.92 ± 0.01 < 0.010 1.34 ± 0.01 0.016 ± 0.001
B 35.0 ± 0.1 25.5 ± 0.1 0.54 ± 0.04 1.13 ± 0.01 0.083 ± 0.001 1.60 ± 0.01 0.001 ± 0.0002
C 34.3 ± 0.1 26.1 ± 0.1 0.52 ± 0.03 1.26 ± 0.01 < 0.010 1.89 ± 0.01 < 0.001

sulfur analyzer, X-ray fluorescence and plasma atomic emission spec- Table 3
trometers. Imaging parameters used in MFM and KPFM modes.
Each tube was operated for different time of operation; the tube Image size 40 µm × 40 µm
length was exposed to different temperatures causing different aging Scan rate 3 s/line
states along its length. In order to analyze the magnetic response as a Resolution 256 points/line
function of the service temperature or aging state, three samples were Lift height (MFM) 100–150 nm
AC bias frequency (KPFM) 17 kHz
extracted from different positions along each steam reforming tube,
AC bias amplitude (KPFM) 4V
being characterized with different aging states according to the criteria
stated by Le May et al. [3]. Metallographic samples, extracted from the
cross-sectional tube, with dimension of 10 mm × 12.5 mm × 5 mm, electric potential map were thus acquired simultaneously. The main
were metallographic sanded and polished. At the center of each sample, parameters used for the MFM and KPFM analyses are given in Table 3.
two small marks (made with a wet ink pen) allowed to easily identify
the same region by SEM and MFM/KPFM. Sample description is given
in Table 2. 3. Results and discussion
The microstructural characterization of the samples was performed
using a scanning electron microscope FEI FEG Versa 3D Dual Beam, 3.1. SEM and EDS
coupled to an energy-dispersive X-ray spectrometer. The morphological
characteristics of the samples were analyzed in the backscattered SEM images obtained on all the samples in the back-scattered
electron mode and a semi-quantitative chemical analysis was measured electron mode are presented in Fig. 1. Phase identification was per-
using energy-dispersive X-ray spectroscopy (EDS). formed for all samples using semi-analytical EDS. Results obtained on
tube A are shown in Fig. 2 due to the presence of all the microstructural
phases (as described below). In addition, the observed phases for tubes
2.2. Scanning Probe Microscopy (SPM)
A, B and C are summarized in Table 4.
In the as-cast conditions and aging state I, HP-Nb modified alloys
The SPM characterization was performed using a Nanosurf Flex
present chromium carbides (dark, spot 2 in Fig. 2.a) and fragmented
AFM microscope. The magnetic and electric measurements were per-
MC carbides (where M = metal, mostly Nb, bright, spot 3 in Fig. 2.a),
formed by using the MFM and KPFM modes. A conductive silicon tip
also known as Chinese-script morphology [5,15–17]. Sample A is an
coated with cobalt (Si-Co) was used for the magnetic and the electrical
alloy with low niobium addition; the Chinese-script morphology is not
characterizations [7,12]. Before the analysis, the samples were placed
observed due to the presence of zirconium which inhibits the formation
on a permanent magnet in order to permanently magnetize the ferro-
of this morphology [5,15,18], Fig. 1.a. The chemical composition of
magnetic phases [7,13,14]. Afterward, the samples were placed in the
sample B presents a high niobium content with micro-addition of tita-
AFM and, based on the SEM micrographs previously obtained, the
nium. Small concentrations of titanium change the MC morphology
scanning was performed on the regions of interest. The MFM data were
from lamellar to blocky, since this element inhibits the formation of the
acquired in two steps (double pass). Initially, the topography of the
Chinese-script morphology [17], Fig. 1.d. On the other hand, sample C
sample was measured in the intermittent contact mode. Then, the probe
is an alloy with high niobium content and no micro-addition of titanium
was lifted to a constant distance between 100 and 150 nm above the
presenting the Chinese-script morphology in niobium carbides (white),
surface of the sample (lift mode). The KPFM measurements were ac-
Fig. 1.g.
quired in the amplitude modulation mode in single pass with the me-
For aging state III, primary chromium carbides (dark) become
chanical excitation of the cantilever at its resonance frequency and an
blocky and a secondary chromium carbide precipitation (small phases
AC electrical bias applied off-resonance. The topographic image and the
precipitated inside the γ-matrix) is observed. This secondary pre-
cipitation is more evident in Sample C, Fig. 1.h. It should also be noted
Table 2
that samples A-III and B-III present a partial phase transformation of
Description for each sample removed from tubes A, B and C showing time of
operation, wall thickness, approximated operating temperatures, and aging
NbC (white) into G-phase (gray, spot 4 in Fig. 2.b), Fig. 1.b. and
state. Fig. 1.e. As reported in literature [19–21], Nb carbides are not stable at
temperatures above 700 °C, being transformed into Nb-Ni-silicide,
Tube Time of Wall Sample Operating Aging state
known as G-phase. In addition, the transformation of G-phase also de-
operation (h) thickness name Temperature (°C)
(mm) pends on the concentration of Si and Ni. The formation of G-phase is
more likely to occur for higher concentrations of Si and Ni [22]. Thus,
A 107,000 11.0 A–I 550 I the NbC of sample C-III presents almost a full phase transformation into
A–III 750 III
G-phase due to the high Si content, Fig. 1.h.
A–VI 1000 VI
For samples with aging state V and VI, a morphological modification
B 90,000 13.0 B–I 550 I is observed in the primary carbides, which lose their lamellar structure
B–III 750 III
B–VI 1000 VI
and form coarser and more compact blocks. The secondary precipita-
tion coalesced, which makes the austenitic matrix cleaner. Sample A-VI
C 135,000 16.5 C–I 550 I
presents Cr-Ni-Nb-Si phase, identified as η-phase by different authors
C–III 750 III
C–V 950 V (spot 5 in Fig. 2.c) [23–25], Fig. 1.c. For sample B-VI, the NbC were
fully transformed into G-phase (gray) and the sample presents

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M.P. Arenas, et al. Journal of Magnetism and Magnetic Materials 491 (2019) 165578

Fig. 1. SEM micrographs in the back-scattered electron mode, revealing NbC, Cr23C6, G-phase, η-phase. Sample A: (a) A-I, (b) A-III and (c) A-VI. Sample B: (d) B-I, (e)
B-III and (f) B-VI. Sample C: (g) C-I, (h) C-III and (i) C-V.

exclusively chromium carbides and G-phase, as depicted in Fig. 1.f. step variation between the carbide and the γ-matrix without huge dip or
Finally, sample C-V presents chromium carbides and G-phase, Fig. 1.i. peak at the carbide boundary, Fig. 4.b. These results prove that the
MFM signal at the chromium carbide boundary is a real magnetic sig-
nature [7]. Moreover, the magnetic signal around the carbides detected
3.2. SPM
by MFM may be explained by the phase transformation or by the var-
iation of the chemical composition around this region.
3.2.1. Sample A
Sample A-III presents Cr carbides, Nb carbides, and G-phase, as
SEM image (Fig. 3.a) shows the presence of Cr-carbides and Nb-
shown in Fig. 3.d. The MFM image shows a weak contrast between the
carbides in age state I on tube A. The MFM image shows that the aus-
γ-matrix and the carbides or G-phase, Fig. 3.e. In contrast, the KPFM
tenitic matrix and the interior of the carbides presents a homogeneous
image presents various contrasts associated to each phase, as shown in
contrast, as shown in Fig. 3.b. However, a dark contrast is observed at
Fig. 3.f. The contact potential difference between the Cr-carbide/γ-
the chromium carbide boundary. In the KPFM measurement the contact
matrix is −36.3 ± 3.1 mV, that difference is higher between Nb-car-
potential difference (VCPD) detected between the Cr-carbide/γ-matrix
bide/γ-matrix (-52.5 ± 11.0 mV). The VCPD between G-phase/γ-matrix
and Nb-carbide/γ-matrix is −29.7 ± 11.0 mV and −56.7 ± 5.0 mV,
is 41.0 ± 4.5 mV. In the case of this sample, the weak contrast between
respectively. This variation of the VCPD resulting from the difference of
the γ-matrix and carbides or G-phase on the MFM image is most
work function between the austenitic matrix and the chromium or
probably not due to a magnetic signal but rather due to the difference of
niobium carbides is observed at the KPFM image, Fig. 3.c.
electrostatic force as suggested by the KPFM potential image.
In order to support if the signature around the carbide is due to real
The SEM micrograph of the sample A-VI presents Cr carbides and η-
magnetic signals, three profile lines were outlined from the interior of
phase, as depicted in Fig. 3.g. The MFM image presents a very homo-
the Cr-carbide to the γ-matrix in both MFM (red lines), Fig. 4.a, and
genous response where is not possible to distinguish any phase, Fig. 3.h.
KPFM (yellow lines), Fig. 4.b. The MFM profile lines present almost the
The KPFM potential image reveals again contact potential differences
same phase-shift inside the non-magnetic carbide and γ-matrix. The Cr-
between the different phases, Fig. 3.i. The contact potential differences
carbide boundary presents a huge variation of the MFM signal, as
between Cr-carbide/γ-matrix and η-phase/γ-matrix are
shown in Fig. 4.a. On the other hand, the KPFM line profiles present a

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M.P. Arenas, et al. Journal of Magnetism and Magnetic Materials 491 (2019) 165578

Fig. 2. SEM micrograph obtained in the backscattered electron mode on tube A. Samples: (a) A-I, (b) A-III and (c) A-VI. The EDS spectra of each spot marked on the
images are presented in the right column.

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M.P. Arenas, et al. Journal of Magnetism and Magnetic Materials 491 (2019) 165578

Table 4 potential image, it can again be attributed to a real magnetic signal.

Microstructural phases observed in tubes A, B and C based on the SEM-EDS For the aging state III, Cr and Nb carbides are observed as well as G-
analyses. phase, Fig. 5.d. In the MFM image a contrast is observed between the γ-
Aging state Tube A Tube B Tube C matrix and the carbides, Fig. 5.e, which may be attributed to electro-
static interactions induced by the differences of the contact potential
I Cr-carbide Cr-carbide Cr-carbide between them. In the KPFM analysis, Fig. 5.f, the VCPD between the Cr-
Nb-carbide Nb-carbide Nb-carbide
carbide/γ-matrix is −41.4 ± 8.6 mV and the contrast between G-
III Cr-carbide Cr-carbide Cr-carbide phase/γ-matrix is 25.8 ± 4.7 mV.
Nb-carbide Nb-carbide G-phase
The sample with aging state VI presents a complete transformation
G-phase G-phase η-phase
of the Nb carbides into G-phase, as shown in Fig. 5.g. In the MFM
V/VI Cr-carbide Cr-carbide Cr-carbide
image, no contrast is observed (Fig. 5.h), as in sample A-VI, not al-
η-phase G-phase G-phase
lowing the detection of the microstructural phases. However, the KPFM
potential image shows a contrast between γ-matrix and Cr-carbide of
−35.8 ± 6.9 mV and −46.0 ± 7.0 mV, respectively. −77.5 ± 10.0 mV, Fig. 5.i. In addition, the contrast between the γ-
matrix and G-Phase is almost the same with a small VCPD between both
phases (11.5 ± 7.1 mV)
3.2.2. Sample B
Sample B-I also presents Cr carbides and Nb carbides, as shown in
Fig. 5.a. The MFM image, Fig. 5.b, presents the MFM signal with a 3.2.3. Sample C
homogeneous contrast in the austenitic matrix and within the carbides. Sample C-I presented also Cr and Nb carbides, as observed in the
As in the case of sample A-I, a rather strong magnetic signal is observed SEM image Fig. 6.a. The MFM image presents magnetic response at the
around the chromium carbides, but also around the niobium carbides. carbide boundaries (Fig. 6.b), presenting the same behavior as samples
The KPFM image shows a VCPD at Cr-carbide/γ-matrix of A-I and B-I. The KPFM potential image presents a contact potential
33.6 ± 4.4 mV, instead for the NbC/γ-matrix is −10.6 ± 3.3 mV. This difference between the Cr-carbides and γ-matrix of −13.5 ± 5.2 mV,
variation is also represented by a contrast between the austenitic matrix Fig. 6.c.
and the carbides, as shown in Fig. 5.c. As the signal observed at the Sample C-III presents Cr carbides, G-phase, and η-phase, as observed
carbide boundary on the MFM image is not observed on the KPFM the Fig. 6.d. No evidence of NbC was observed in this mapped region.

Fig. 3. SEM micrographs (a,d,g), MFM phase-shift images (b,e,h) and KPFM potential images (c,f,i) of samples A-I (a-c), A-III (d-f), and A-VI (g-i).

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M.P. Arenas, et al. Journal of Magnetism and Magnetic Materials 491 (2019) 165578

Fig. 4. Sample A-I profile lines dashed from the interior of the Cr-carbide to the γ-matrix in (a) MFM image (red lines) and (b) KPFM image (yellow lines). (For
interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 5. SEM micrographs (a,d,g), MFM phase-shift images (b,e,h) and KPFM images (c,f,i) obtained on samples B-I (a-c), B-III (d-f) and B-VI (g-i).

The MFM image presents a very weak contrast between the micro- between the Cr carbide/γ-matrix and η-phase/γ-matrix is
structural phases and the γ-matrix (Fig. 6.e). This weak contrast may −52.7 ± 4.9 mV and −16.1 ± 5.1 mV, respectively. For the G-
not be due to magnetic interactions but rather to electrostatic interac- phase/γ-matrix the VCPD is 60.5 ± 9.6 mV and for the brighter region is
tions resulting from the differences in contact potential revealed in the 125.7 ± 42.0 mV. This variation of the VCPD is observed in the KPFM
KPFM potential image, Fig. 6.f. The contact potential difference image as an evident contrast between chromium carbide (dark), G-

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M.P. Arenas, et al. Journal of Magnetism and Magnetic Materials 491 (2019) 165578

Fig. 6. SEM micrographs (a,d,g), MFM phase-shift images (b,e,h) and KPFM potential images (c,f,i) for samples C-I (a-c), C-III (d-f) and C-V (g-i).

phase, η-phase, and γ-matrix. It is also observed that G-phase presents observed between carbides and γ-matrix was due to the difference of
two contrasts which may be attributed to different stoichiometry work function between them.
[15,26,27], resulting in a work function difference. Furthermore, as the
weak contrast observed in the MFM image is mainly constant, the sig- Acknowledgments
nificant difference of contact potential between the phases in the KPFM
analysis once again did not affect the signal detected by the MFM. The authors would like to thank the Brazilian research agencies
Finally, sample C-V presents Cr carbides and G-phase, as observed in CAPES, CNPq, and FAPERJ for the financial support and PETROBRAS
the SEM image, Fig. 6.g. The MFM image shows no contrast between for the samples supply. BN also thanks Wallonie Bruxelles International
the precipitates and the γ-matrix (Fig. 6.h). On the other hand, a clear (WBI) for the financial support.
contrast between these phases is observed in the KPFM image; where
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