Applied Surface Science 470 (2019) 870–881

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Applied Surface Science

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Full Length Article

Fractal and multifractal analysis of fracture surfaces caused by hydrogen T

embrittlement in high-Mn twinning/transformation-induced plasticity steels
Hao Fua, Wei Wanga, Xiaojun Chenb, , Giorgio Piac, Jinxu Lia,
⁎ ⁎

a
Corrosion and Protection Center, Key Laboratory for Environmental Fracture (MOE), University of Science and Technology Beijing, Beijing 100083, China
b
Key Laboratory of Tectonics and Petroleum Resources, Ministry of Education, China University of Geosciences ,Wuhan 430074, China
c
Dipartimento di Ingegneria Meccanica, Chimica e dei Materiali, Università degli Studi di Cagliari, via Marengo 2, 09123 Cagliari, Italy

ARTICLE INFO ABSTRACT

Keywords: A fracture surface is very important evidence in failure analysis after a material fractures under the combined
Fracture surfaces actions of load and environment. In this work, we used field-emission scanning electron microscopy to obtain the
Hydrogen embrittlement susceptibility (Eloss) morphology of fracture surfaces, which is ascribed to hydrogen embrittlement (HE) for high-Mn twinning/
High-Mn TWIP/TRIP steels transformation-induced plasticity (TWIP/TRIP) steels with various phase volume fractions of ε-martensite and
Fractal geometry
similar ultimate tensile strengths in the hydrogen-contained environment. The fracture surfaces were then
Multifractal and generalised fractals
quantitatively characterised by fractal and multifractal methods. The results indicate that HE fracture surfaces of
Hydrogen atoms
high-Mn TWIP/TRIP steels have obvious self-similar and multifractal characteristics. Moreover, the traditional
simple fractal is not appropriate for the complexity of HE fracture surfaces, but the multifractal spectrum f(α)-α
and generalised fractal D(q)-q curves show perfect performance in accurately depicting the roughness and
homogeneity of such complex fracture surfaces. The width of multifractal spectrum (Δα) and the ratio of gen-
eralised fractal dimension Dmin to Dmax (Dmin/Dmax) show a remarkable linear negative correlation with HE
susceptibility (Eloss). The internal reason was analysed in detail. It is important to note that two linear corre-
lations between the fractal parameters and Eloss give a good indicator for evaluation of the HE property based on
the morphology images of fracture surfaces without multi-step experiments and may be applied in on-site failure
analysis of high-Mn TWIP/TRIP steels.

1. Introduction structural materials to reduce the plasticity of material and leads to

The fracture surface of an engineering material formed during the
test or service process is important evidence in failure analysis. It re-
cords the irreversible deformation of the fracture and the crack pro-
pagation up to entire fracture under multiple effects of load and en-
vironment. Meanwhile, the morphologies of fracture surface [1,2] are
subject to diverse factors from material properties to environmental
media. So the morphologies characteristics of fracture surfaces are
comprehensive results and reflections of inherent mechanical proper-
ties and external fracture mechanism. Thus, the reasons for fracture and
mechanism analysis are of great significance to prevent the recurrence
of failure and economic losses or casualties. In practice, material failure
resulting from hydrogen embrittlement (HE) is one of the typical failure
modes of engineering materials, especially for high-strength steels.
Outside hydrogen atoms enter into the material during its manufacture,
processing and service [3–6]. Under the action of external loads, hy-
drogen atoms diffuses and accumulates inside the engineering
delayed fracture which is the most frequent dangerous low-stress brittle
fracture for metal materials [7–9], known as HE. Generally, the typical
fracture surfaces of HE is an intergranular fracture whose roughness,
however, strongly depends on the HE susceptibility (Eloss) [10–12].
Therefore, the analysis of fracture surfaces related to HE is of great
significance in understanding the relationship between fracture process
and inner composition and microstructure of material and providing
valuable suggestions for improving resistance to HE.
Generally, fracture surface analysis has mainly focused on qualita-
tive information about morphology. To gain insight into material
failure fracture, quantitative characterisation is urgently needed
through which a correlation could be established directly between
mechanical properties and failure mechanism. In this regard, fractal
geometry provides a powerful tool to quantitatively study the com-
plexity of fracture surfaces based on self-similar mechanisms of frac-
ture. Mandelbrot et al. [13] applied fractal geometry to materials sci-
ence for the first time. This evidence suggests that fractal geometry

⁎
Corresponding authors.
E-mail addresses: chenxj@cug.edu.cn (X. Chen), jxli65@ustb.edu.cn (J. Li).

https://doi.org/10.1016/j.apsusc.2018.11.179
Received 13 July 2018; Received in revised form 26 October 2018; Accepted 22 November 2018
Available online 23 November 2018
0169-4332/ © 2018 Elsevier B.V. All rights reserved.
H. Fu et al.
shows increasing power in characterising the irregularity and disorder
of fracture surface systems. Hence, there seems to be an inevitable trend
that a certain relationship between fracture morphology and material
mechanical properties should be established by fractal geometry for
material failure. However, inconsistency exists in this relationship in
previous studies. For example, Hiders et al. found that impact toughness
increases with increasing fractal dimension [14] and suggested that a
linear relationship exists between impact toughness and fractal di-
mension [15]. However, Mandelbrot et al. [13] found that impact
toughness decreases as fractal dimension increases. So far, no consensus
has been reached. It is worth noting that above fractal geometry studies
are based on traditional simple fractals. For the fracture surface com-
plexity, especially the high-strength steel fracture surface of HE due to
diffusion and enrichment of hydrogen atoms during fracture, a single
fractal may not be accurate enough to comprehensively analyse the
fracture surface [16]. However, multifractal and generalised fractal
theory provides a new avenue to characterise this complexity of irre-
gular surfaces. Recently, multifractal has been successfully applied in
many fields, such as geophysics [17,18], petroleum reservoir [19,20]
and heat transfer theory, etc. [21,22]. For material science, multi-
fractals are primarily used to characterise the surface roughness, het-
erogeneity of thin films [23–28] and the mechanical properties of
porous materials [29–31]. For material failure, multifractals have been
intensively used to describe the fracture surface complexity of polymer
materials and composites [32–34]. However, the fracture caused by HE
of high-strength steel is essentially the failure caused by the diffusion
and enrichment of hydrogen atoms in the steel and HE fracture surface
is the result of a natural evolution. Until now, few studies have been
carried out on HE of metal materials by the multifractal and general-
ised fractal approach [35–37]. Thus, this work attempts to quantita-
tively characterise the HE fracture of high-strength steel by this
method.
Recently, high-Mn TWIP/TRIP steels have been developed with high
work–hardening rates [38,39], high elongation [40,41], high ultimate
tensile strength [42,43] and the rate dependence of microstructure
evolution with various strain rates under impact loads [44–49] have
received enthusiastic attention in automotive, shipbuilding and energy
industry owing to their good properties. However, undesirable HE oc-
curs in high-Mn steels when it is serviced in seawater or other hy-
drogen-containing environments, even in humid air [50–53]. To gain
insight into the relationship between HE susceptibility (Eloss) and frac-
ture surfaces morphology of metal materials, fractal and multifractal
analysis are conducted for quantitative analysis of the fracture mor-
phology. Therefore, the primary object of this work was to establish a
quantitative relationship between Eloss and fractal parameters in high-
Mn steels to provide useful information for a better understanding of
the HE process in these new materials. This can give a new perspective
in predicting the failure of materials and provide reference values for
steel research and development in the automotive field.
2. Experiments and materials
The high-Mn TWIP/TWIP steels with nominal compositions of Fe-
18Mn-0.6C (in wt.%) were melted from pure elements in a vacuum
induction furnace under a protective argon atmosphere and were cast
into 21 kg ingots (900 × 100 × 40 mm3). The specific chemical com-
position is listed in Table 1. With an oxidation coating painted on the
surface, the ingots were hot-rolled to a 3 mm-thick plate after
Table 1
Chemical composition of investigated steel used in the present study (wt.%).
Mn C S P Fe
18.2 0.56 0.016 0.008 Balance
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Applied Surface Science 470 (2019) 870–881
homogenisation at 1475 K for 1.5 h: the hot rolling start temperature
was 1325 K and the final temperature was 1175 K. After surface des-
caling, the hot-rolled plates were cold-rolled to a 1.5 mm-thick sheet
with a thickness reduction of 50%. Then, part of the sheets was an-
nealed for 20 min at 1175 K in the air and then water-quenched to room
temperature. To obtain some flat test materials, rolling with slight re-
duction was carried out on the annealed sheets. Then, the test materials
were annealed at 1175 K for 10, 30 and 40 min respectively, finally
being water-quenched to room temperature again. These specimens
were conveniently labelled S10, S30 and S40 respectively. During the
annealing, surface decarburisation of specimens occurred and the ac-
companying thermal distortion induced ε-martensite transformation.
The decarburisation depth below the sheet surfaces varied with the
annealing conditions. Therefore, specimens with varying amounts of ε-
martensite were obtained. To obtain full austenitic microstructure
specimens, some of cold-rolled sheets were directly annealed at 1175 K
under a protective nitrogen atmosphere for 50 min and then water-
quenched to room temperature without rolling but with slight reduc-
tion. Distinctively, this specimen was labelled S0. To prevent the effect
of nitrogen on the surface composition of all specimens, the annealed
specimens were polished with sandpaper for subsequent testing. The
detailed preparation process for specimens is shown in Fig. 1.
The microstructure and phase volume fraction of ε-martensite
(PVFM) after annealing were examined using X-ray diffractometer
(XRD, Ultima IV) with a Cu-Kα target. The operating voltage for X-ray
diffractometry was 30 kV and the scanning range, rate and step size
were 40–100°, 2° min−1 and 0.02° respectively.
Two types of tensile tests were conducted in the present work: a
normal tensile test in air and a slow strain rate test (SSRT) in HE. In
both cases, the tensile specimens were machined along the rolling di-
rection with gauge dimensions of 20 mm long × 5 mm wide × 1.4 mm
thick. Grip sections on both ends were cut by spark erosion for the
annealed sheets. Those sheets were then mechanically polished by
using grit abrasive paper to reduce the thickness from 1.4 mm to
1.2 mm (wearing off both sides by 0.1 mm). Even if nitriding occurred,
the abraded thickness is much greater than the thickness of the ni-
triding layer. Therefore, the effect of nitriding on the specimen can be
completely ruled out in this work. The normal tensile test was carried
out at a strain rate of 1 × 10−4 s−1 in an ambient atmosphere. We
believe that the mechanical properties of specimen are not affected by
the strain rate in air when tensile test is carried out at a slower strain
rate than 1 × 10−4 s−1 according to previous researchers' works
[52,54–56]. The SSRT was performed at strain rates of 1 × 10−5 s−1,
5 × 10−6 s−1 and 1 × 10−6 s−1. Hydrogen was continuously in-
troduced into the specimens during the tensile tests by electro-chemical
charging in a 3% NaCl aqueous solution containing 3 g/L NH4SCN at
current density of 5 A/m2 at ambient temperature, as shown in Fig. 2.
During SSRT, a platinum wire was used as the anodic electrode and the
solution was continuously replenished to cover the gauge part of tensile
specimens. All the tensile tests were performed on a computer-con-
trolled tensile testing machine.
The fracture surfaces morphologies of tensile specimens were ob-
served using a field-emission scanning electron microscope (FE-SEM)
after SSRT. The operating voltage was 20 kV and working distance was
12–13 mm. SEM images of fracture surfaces of all specimens after SSRT
were obtained at a magnification of 500× (intergranular) and 1000×
(ductile) to obtain the morphology with a full view of the field.
3. Methodology
Fractured surfaces commonly have an undulating surface with a
height difference at the micron level at each point. With conventional
measurement methods, it is very challenging to obtain accurate eleva-
tion map data sets. The SEM image is a gray-scale image that provides a
good indirect method via colour intensity discrepancy in the whole
image. White indicates the raised area, which is the highest location.
H. Fu et al. Applied Surface Science 470 (2019) 870–881

Temp.
Solution
treatment
at 1423 K
(1.5 h) Hot rolling
(3 mm plate) Annealing
at 1173 K Annealing
1173 K at 1173 K
20 min 50 min (N2protection)
1323 K 10 min 30 min 40min

Wa ter que nc hin

Water q ue nc hi ng
Air
S0
S10

col
S30 S40

ling

g
Cold rolling
(1.5 mm plate)
Small reduction

Time
Fig. 1. Schematic diagram showing rolling and heat-treatment processes.

Black represents the recessed area, which is the lowest part. Grey re-
presents the height between the two levels. Therefore, grey value of
each point in the SEM image can approximate the relative elevation
value of each point in the range of 0–255, which is expressed by the
formula:
A (x , y , G )~A (x , y, H )
where A is the pixel of SEM image; x, y are the coordinates of this pixel
A; G is the grey value of this pixel; H is the relative height or elevation,
H = G. The original SEM images must be pre-processed and cropped. To
be continuously segmented by the box counting algorithm and projec-
tive covering method, each image should be cut into two different sizes
of 2 N and 2 N +1 pixels, specifically 256 pixels and 257 pixels (N = 8),
to obtain the maximum coarse information and to calculate the
multifractal and single-area dimensions. Since the selected calculation
area does not cover the entire field of view, therefore it becomes in-
creasingly important to determine the fractal parameters only after
multiple regions are selected in one SEM image, ensuring the accuracy
of fractal data. The original SEM images are rectangular (768 × 1024
pixels), thus six areas in one image are selected and cropped (upper-left,
(1)
upper-centre, upper-right, bottom-left, bottom-middle and bottom-
right). For example, Fig. 3 presents the upper-right and lower-left lo-
cations (corresponding pixel values of locations, X-axis: 177-689, Y-
axis: 2-514 (Fig. 3(b)); X-axis: 4-516, Y-axis: 511-1023 (Fig. 3(e)).
Xie et al. [57,58] proposed a single surface area-based fractal di-
mension Ds based on the projective covering algorithm (Fig. 4). Sym-
bols A and B represent the real fracture surface and the projection grid
covering plane respectively. When the rectangular grids a, b, c, d (a, b, c
Tensile direction

Upper grip

Connected negative electrode

Plastic container (-)

Sample
Connected positive electrode H
+
H+ H+ H
+

(+) H+ H+
3%NaCl+0.3g/LNH 4 SCN
H
+
H
+

H
+
H+ H
+

Counter electrode (Pt)

Tensile direction

Lower grip

Fig. 2. Schematic of the hydrogen charging set-up.

872
H. Fu et al. Applied Surface Science 470 (2019) 870–881

(a) c)
(b)

30μm 30μm
30μm

(d) (f)
(e)

30μm 30μm
30μm

Fig. 3. Image processing by digital image analysis: (a, d) the original SEM image for the fractured surface of steel caused by hydrogen embrittlement; (b, e) cutting of
(a) into 512 × 512 pixels for the calculation of fractal dimensions; (c, f) digital elevation image from (b, e).

and d are the four corners of the square) of the k-th sub-size δ × δ are N( )

selected, the points a, b, c and d of the rough surface height correspond AT ( ) = Ak ( )

k=1 (3)
to H1, H2, H3 and H4. The rough surface area Ak surrounded by the
projection grid a, b, c, d can be approximated by: where N(δ) is total number of boxes. In different sizes of boxes, there is
a power law expressed by:
Ak = S1 + S2 = p1 (p1 ab)(p1 ad )(p1 bd ) N( )
AT ( ) = Ak ( )~ 2 Ds
+ p2 (p2 bc )(p2 cd )(p2 bd )
k=1 (4)
P1 = (ab + ad + bd )/2; P2 = (bc + cd + bd )/2
As δ → 0, AT approaches the real surface area of fracture. Therefore,
ad = (x1 x2 )2 + (y1 y2 )2 + (H1 H2 )2 (2) the variation of surface area with the observation scale reflects the
roughness of fracture surface.
The total surface area AT is measured at the k-th measurement scale
As stated above, a single fractal Ds records the variation law of
by:
surface area of each box but does not consider the variation rule of the

Box size δ
b
A
a c

d
240
B 220
140
200
180
160
140 (x 4 ,y 4 ,H 4 )
120
ab
100 bc
80
S1 bd S
60 2
40
20 (x 3 ,y 3 ,H 3 )
0
(x 1 ,y 1 ,H 1 ) ad cd
(x 2 ,y 2 ,H 2 )
Fractured Surface

(a) (b)
Fig. 4. Schematic diagram of calculating surface fractal dimension Ds based on projective-covering method and calculating multifractal and generalized dimension
based on BC algorithm. (a) boxes with different sizes are projected on the fracture surface for calculating the surface area and height in each box. Red indicates a high
part of the fracture, green indicates a low fracture position; (b) the calculated area under each box, which equals to the area of the space quadrilateral enclosed by
four breaking vertices.

873
H. Fu et al. Applied Surface Science 470 (2019) 870–881

proportion of each box surface area. Therefore, it may not fully portray
the complexity of nature [59]. Real complex fracture systems not only
have surface-area-based self-similar characteristics but also have char-
acteristics based on mass or height proportion distribution. Multi-
fractals and generalised fractals are powerful in characterising this mass
or height proportion [60].
The generalised entropy Hq(δ) and generalised dimension Dq are
defined as [61]:
N q
ln i = 1 hi
Hq ( ) = 1 q

Dq = lim
0 ln
Hq ( )
=
(q)
q 1
; (q = 1, D 1 =
hi ln hi
ln ) (5)
where hi = Hi/Ht accounts for the ratio of the height value of the i-th
box and total height value of the surface of the fracture at a certain
scale (Here, we set the height of the lowest point of the fracture to zero
and the maximum is the colour value of 255). The variable q represents
the weight with a common range from qmin = −10 to qmax = 10 in Fig. 5. X-ray diffraction patterns of four annealed steels under different heat-
increments of 1. The variable τ(q) refers to the mass exponent, which is treatment conditions.
a function of the variable q. The convex-concave nature of the τ(q)-q
curve can be used to determine whether the complex state under in- Table 2
vestigation satisfies multifractal characteristics. Dq is also known as Calculation results for the ε-martensite phase volume fraction (PVFMs) for all
Renyi dimension. For single fractal patterns (strictly self-similar), all Dq tested steels in the present study.
values are equal to D0 (Eq. (5)). For the complex fractal, Dq char- Specimens S0 S10 S30 S40
acterises the fluctuation and unevenness of the multifractal sets. When
q = −10, Dmin is the minimum generalised dimension; for q = 0, D0 is ε-martensite PVFM (%) 0 15 38 55

the single box-fractal dimension; and when q = 1, D1 is the information

dimension; for q = 2, D2 is the correlation dimension; and for q = 10,
complexity of ε-martensite transformation based on multiple factors of
Dmax is the maximum generalised dimension. The multifractal spectrum
thermodynamics, kinetics and so on. Consequently, if the annealing
is expressed as:
time further increases, PVFM and grain size will increase correspond-
f( )= lim
In(N ( ))
ingly and the elongation and ultimate tensile strength of the tests steels
In( )
0
will be affected dramatically, resulting in the comparison of the HE
In(hi)
(q) = lim
(6) susceptibility in such case (typically, PVFM > 60%) being meaningless
0 In( )
and invalid. Thus, PVFM of 0, 15%, 38% and 55% were selected in the
where α(q) is the singularity exponent and f(α) represents the multi- present work.
fractal spectrum function. N (α) represents the integral value of α in Fig. 6(a) reveals the engineering stress-strain curves of all specimens
speed [α, α + dα]. Through the Legendre transform, f(α) and α(q) can with various PVFM after uniaxial tensile in air at room temperature. As
be given as follows: observed, S10 specimen exhibited the highest uniform elongation
(q ) (UE ≈ 88%) and ultimate tensile strength (UTS ≈ 1060 MPa). In addi-
(q ) = q tion, S40 specimen exhibited the lowest UE (≈76%) and UTS
f (q ) = (q ) q (q ) (7) (≈900 MPa). The specimens of S0 and S30 have same UE, while UTS of
S0 was higher than that of S30. It is worth noting that UTS of all spe-
By the definition of the function τ(q), Eq. (7) can be changed to:
cimens are approximately equal. The UTS discrepancy between the
(q) = lim In
1
µi In(hi ) highest and the lowest is within 10%. In general, the higher the UTS of
i
0
the steel, the more sensitive it is to HE. Therefore, all specimens can be
1
f (q) = lim In µIn(µi ) used to compare the HE susceptibility in this study.
0
i (8)
where the µi = i i .
The plot of f(α) vs. α represents the multi-
hiq/ hq
fractal spectrum curve [62]. Thus, Eq. (8) is used to calculate the 4.2. SSTR for the evaluation of hydrogen embrittlement
multifractal spectrum curve by using programming codes.
Generally, the properties of HE were analysed by the SSRT results.
4. Results and discussion Fig. 6(b–e) show the engineering stress-strain curves of all specimens
after SSRT. As shown, UE significantly deteriorates after hydrogen-
4.1. Phase volume fraction and mechanical properties of as-annealed charging. The HE susceptibility was quantified by the loss ratio of UE,
specimens which was determined by [64]:
EU (air) EU (H - charging)
XRD spectra of all cold-rolled specimens at different annealing times Eloss =
EU (air) (9)
are presented in Fig. 5. The red line shows the fully austenitic micro-
structure after specimens were annealed in a nitrogen-filled environ- where EU(air) and EU(H-charging) represent the UE of the hydrogen-free
ment. The other spectra suggest that the ε-martensite transformation and hydrogen-charging specimens, respectively. The calculated values
occurred during annealing in air. As the annealing time increases, the of Eloss were shown in Table 3, which indicates that Eloss increased with
intensity of peak at the same diffraction plane of ε-martensite increases. a decrease in strain rate during SSRT since more hydrogen atoms have
The PVFM was estimated by the calculation method of De et al. ac- enough time to diffuse inward from the surfaces of the specimens with
cording to X-ray diffraction [63]. Table 2 presents the calculated results the lower strain rate during SSRT by stress induction. The Eloss increased
of PVFM of as-annealed specimens, indicating that PVFM increases with with increasing PVFM through the whole range of strain rates,
the extension of annealing time without a linear law due to the 1 × 10−5 s−1 to 5 × 10−6 s−1, for specimens S10, S30 and S40.

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H. Fu et al. Applied Surface Science 470 (2019) 870–881

1200

Engineering stress (MPa)

(a)
1000

800

600

400 S0
S1 0
200 S3 0
S4 0
0
0 .1 0.2 0.3 0 .4 0 .5 0.6 0.7 0 .8 0 .9 1.0
Engineering strain

1200 1200

Engineering stress (MPa)

(c )S10
Engineering stress (MPa)

(b)S0
1000 1000

800 800

600 600
Air 1× 1 0-4 s-1
400 -6 -1 400 Ai r 1× 10
-4
s
-1

H-charging 1× 10 s -6 -1
H-ch a rg in g 1× 10 s
H-charging 5× 10-6 s-1 200 H-ch a rg in g 5× 10
-6
s
-1

200 -5 -1

H-charging 1× 10-5 s-1

H-ch a rg in g 1× 10 s

0 0
0 .1 0 .2 0 .3 0 .4 0 .5 0 .6 0 .7 0 .8 0 .9 0.1 0.2 0 .3 0 .4 0.5 0.6 0.7 0 .8 0.9 1.0

Engineering strain Engineering strain

1200 1000
(d)S30
Engineering stress (MPa)
Engineering stress (MPa)

(e)S40
1000
800
800
600
600
Air 1× 10-4 s-1 400
400 Air 1× 10 s
-4 -1
H-c harging 1× 10-6 s-1 -6 -1
-6 -1 H-charging 1× 10 s
H-c harging 5× 10 s
200 200 H-charging 5× 10-6 s-1
H-c harging 1× 10-5 s-1
H-charging 1× 10-5 s-1
0 0
0.1 0 .2 0 .3 0.4 0.5 0 .6 0 .7 0.8 0.9 0 .1 0.2 0.3 0.4 0 .5 0 .6 0.7 0.8
Engineering strain Engineering strain
Fig. 6. Engineering stress -strain curves (a) and SSRT cures of the different PVFM specimens (b–e): (b) S0, (c) S10 (d) S30 and (e) S40.

However, the Eloss of S0 specimen reached the highest value at strain
rate of 1 × 10−6 s−1 and then remained at steady state.
Fig. 7 gives typical fracture surfaces for part of specimens after SSRT
with different strain rates. As exhibited in Fig. 3, the fracture surfaces of
high-Mn TWIP/TRIP steels display a typical characteristic of HE during
SSRT, which includes intergranular fracture on the edges of specimens
(Fig. 7(a–f)) and ductile fracture in the centre of each specimen
(Fig. 7(g–l)) caused by continuous inward diffusion of hydrogen atoms
from the surface with a relatively slow strain rate. It is noteworthy that
for S40 specimen, the entire fracture surface is characterised by inter-
granular fracture and there is no ductile fracture zone at the strain rate
of 1 × 10−6 s−1.
We know that the most important factor determining the suscept-
ibility of metal materials to HE is the size of the intergranular area in
the entire fracture. The larger the intergranular area is, the higher the
value of Eloss. Therefore, the fractal dimension of fracture surface is
discussed on the basis of determining the area of the intergranular
fracture area in each fracture for each specimen. That is, we ensure that
the percentages of specimens in which the area of the intergranular area
accounts for the entire fracture area are similar, while Eloss is different.
Among these, the relationship between Eloss and fractal dimension is
studied. Hence, we calculate the ratio of intergranular fracture area to
the total fracture area (AI/E) as a percentage in the mean calculation of
the Eloss test material, as shown in Table 3. It can be seen from the

Table 3
Susceptibility to HE with various amounts of ε-martensite at different strain rates on H-charging.

875
H. Fu et al.
Fig. 7. Fracture surfaces of a part of the specimens after SSRT: (a–f) intergranular fracture surfaces (g–l) ductile fracture surfaces.
calculation results that when the Eloss is between 0.649 and 0.837, the
area percentage of the intergranular fracture zone is equivalent (≈0.5),
but when Eloss is between 0.871 and 0.946, the area is also equivalent
(all are greater than 0.79). Therefore, we will analyse these two parts
while discussing the relationship between Eloss and the fractal para-
meters.
4.3. Simple fractal analysis of fracture surfaces
The simple fractal dimensions (Ds) were calculated by the protective
covering method (PCM) and the results are shown in Table 4. The re-
lationship between the Ds and Eloss of intergranular fracture surfaces
shows that as Eloss increases, Ds increases first and then decreases,
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Applied Surface Science 470 (2019) 870–881
reaching a maximum value at 5 × 10−6 s−1 strain rate, which means
that Ds value is related to the strain rate for intergranular fracture
caused by HE, as shown in Fig. 8(a). For S0 specimen, the relationship
between Ds for ductile fracture and Eloss is shown by red line in the
Fig. 8(b). Here, the relationship between Ds and Eloss shows the same
tendency as that of the intergranular situation. The maximum value of
Ds appears at 5 × 10−6 s−1 strain rate. However, for S10 and S30
specimens, the relationship between Ds and Eloss shows the opposite
tendency with both the minimum values of Ds appearing at the
5 × 10−6 s−1 strain rate. For S40 specimen, since the incompatibility of
ε-martensitic deformation results into the fact that diffusible hydrogen
atoms have enough time to diffuse during SSRT at 1 × 10−6 s−1 strain
rate. So, there is no ductile fracture, instead there is a full intergranular
H. Fu et al. Applied Surface Science 470 (2019) 870–881

Table 4
The fractal and multifractal spectral parameters of fracture surfaces with var-
ious strain rates (Ds: simple fractal dimension; Δα: width of the singularity
exponent spectrum; IF: intergranular fracture; DF: ductile fracture).
Specimens Ds Δα Dmin/Dmax

IF DF IF DF IF DF

−5 −1
S0-1 × 10 s 2.450 2.455 1.804 1.837 1.814 1.807
S0-5 × 10−6 s−1 2.459 2.500 1.759 1.763 1.777 1.768
S0-1 × 10−6 s−1 2.467 2.465 1.699 1.639 1.715 1.684
S10-1 × 10−5 s−1 2.445 2.502 1.765 1.785 1.779 1.755
S10-5 × 10−6 s−1 2.474 2.477 1.752 1.728 1.763 1.737
S10-1 × 10−6 s−1 2.441 2.515 1.720 1.676 1.742 1.713
S30-1 × 10−5 s−1 2.419 2.482 1.765 1.748 1.773 1.754
S30-5 × 10−6 s−1 2.457 2.446 1.734 1.726 1.756 1.723
S30-1 × 10−6 s−1 2.410 2.505 1.709 1.652 1.718 1.689
S40-1 × 10−5 s−1 2.385 2.516 1.744 1.743 1.76 1.746
S40-5 × 10−6 s−1 2.395 2.460 1.723 1.696 1.735 1.709
Fig. 9. The curve of τ(q) versus q for fracture surfaces.
S40-1 × 10−6 s−1 2.381 1.708 1.72

reveals that Δα decreases with increasing values of Eloss and shows a

fracture. Moreover, the variation trend of Ds and Eloss for S10 specimen
is in agreement with S30 specimen.
The simple fractal analysis indicates that Ds and Eloss do not show a
clear correlation for both types of fracture surfaces. Additionally, the
variation trends between Ds and Eloss of dimple surfaces have a strong
inconsistency among specimens.
4.4. Relationship between multifractal spectra and Eloss
The simple fractal, which can provide only overall characterisation
of rough surfaces, ignores more comprehensive and finer local in-
formation due to the complexity of fracture surfaces related to HE.
However, the multifractal can make up for these limitations. As men-
tioned earlier, the convexity and concavity of τ(q)-q curve can be used
to determine whether the fracture surface satisfies the multifractal
characteristics. Fig. 9 reveals that curve of τ(q) versus q has a non-linear
relationship with an upwardly convex shape, indicating that the frac-
tured surface of high-Mn steels has typical multifractal features.
Fig. 10 gives the multifractal spectrum f(α)-α of all specimens, in
which Fig. 10(a) represents the intergranular fracture surfaces and
Fig. 10(b) manifests the ductile surfaces. Furthermore, the parameters
of multifractal spectra are also summarised in Table 4. From Fig. 10(a,
b), multifractal spectrum have a clear left-hook shape. At the same
time, the widths of the singularity exponent spectrum Δα
( = αmax − αmin) are obviously different among all specimens. This is
related to Eloss, as shown in Fig. 10(c, d). Fig. 10(c, d) give the re-
lationship between Δα and Eloss for all specimens. It should be noted
that two figures were divided into two regions with two colours and
data points in both regions possess similar area fractions of inter-
granular fracture. The pink area represents AI/E approximately 0.5 and
the light blue area shows values of AI/E that are no less than 0.79. This
remarkable linear negative correlation for intergranular fracture sur-
faces (R2 = 0.97774) and ductile fracture surfaces (R2 = 0.98886):
Intergranular: = 0.3433Eloss + 2.2025
Ductile: = 0.6838Eloss + 2.2868 (10)
For intergranular fracture surfaces, Δα reaches 1.804 when Eloss is
0.649 in S0 specimen at 1 × 10−5 s−1 strain rate and Δα falls to 1.699
when Eloss equals 0.946 in S0 specimen at 1 × 10−6 s−1 strain rate. This
means that the more severe the plasticity loss caused by HE, the more
uniform the grey-scale distribution is on the surface. From the reference
[33], since the size of the box δ ≤ 1, it shows that the smaller the value
of αmin, the larger the largest probability distribution is. In addition, the
larger the value of αmax, the smaller the smallest probability distribu-
tion is. That is to say, αmax represents the minimum grey value dis-
tribution probability and αmin represents the maximum. Therefore, Δα
can be applied to describe the range of probability. The larger the Δα,
the wider the range of probability distribution is, hence the greater the
difference is between the most probability subset and the least prob-
ability subset of grey value distribution and vice versa.
As mentioned before, black area represents the lower positions and
white stands for the higher positions in SEM image. Thus, Δα can be
further used to characterise the degree of undulation of fracture sur-
faces known as “fracture surface roughness”. The lower the Eloss, the
rougher and more inhomogeneous the fracture surface is. Thus, Δα
provides a good indicator for determining the degree of Eloss of high-Mn
steels based on SEM image analysis without experiments.
In intergranular fracture surfaces caused by HE, the black locations
stand for the secondary crack (yellow arrow) or a grain hole (red arrow)
in Fig. 7(a–f), while white or grey locations represent convex grains.
Hence, the value of Δα can also be used to describe the number of

2 .5 0 2.54
(a )Intergranular fracture surfaces (b) Dimple fracture surfaces
2.52
2 .4 5
2.50
2.48
Ds

2 .4 0
Ds

2.46
S0
2 .3 5 S1 0
2.44 S0
S10
S3 0
2.42 S30
S4 0
S40

0.6 0.7 0.8 0 .9 1.0 0.6 0 .7 0.8 0 .9 1.0

Eloss E loss

Fig. 8. The relationship between Eloss and Ds for: (a) intergranular fracture surfaces (b) ductile fracture surfaces.

877
H. Fu et al. Applied Surface Science 470 (2019) 870–881

Fig. 10. The multifractal spectra f(α) of fracture surfaces for all specimens (a, b) and the relationship between Eloss and Δα(c, d). (the data points of the two regions of
(c, d) possess similar area fractions of intergranular fracture AI/E).

secondary cracks or holes and their random distribution. The more
secondary cracks and the more random the distribution, the larger the
Δα value will be and vice versa. Fig. 11 shows the segmented maps with
threshold values of 80 in the fracture surface area (Fraction greater than
80 is green, while fraction less than 80 is blue), in which Fig. 11(a–c)
represent the intergranular fracture surfaces corresponding to Fig. 7(a),
(b) and (f), respectively and Fig. 11(d–f) represent ductile fracture
surfaces corresponding to Fig. 7(g), (j) and (h), respectively. The in-
tergranular surfaces are equivalent to a map with many randomly dis-
tributed “islands” in a “sea”, which lead to a relative roughness and a
larger Δα value compared with a relatively smooth plane. The raised
grains are similar to the islands and secondary cracks or holes of the

(a) (b) (c)

island island

island
sea sea
sea

(d) pit (e) (f)

pit
land

land
pit
land
pit

Fig. 11. Segmented maps with threshold gray-value of 80 in fracture surfaces: (a–c) intergranular fracture; (d–f) ductile fracture (the green color represents “island”
and “land”; the blue color stands for “ sea” and “pit”).

878
H. Fu et al.
grains are similar to the sea. For example, the secondary crack is ran-
domly distributed on the intergranular fracture for S0 specimen at the
1 × 10−5 s−1 strain rate. Its Δα value is 1.804, so it is rough as shown
in Fig. 11(a). The small and local non-uniform grains exist for S0 spe-
cimen with the relatively short annealing time, resulting into small
number of hydrogen atoms in the unit grain boundary [65]. Conse-
quently, hydrogen atoms are more likely to be enriched in the grain
boundary of larger grains under an internal stress gradient due to the
poor coordination of relatively larger grains during the deformation
with a relatively high strain rate [66] (1 × 10−5 s−1). Thus, these grain
boundaries are preferred locations for crack nucleation and smaller
grains are forced to crack to form holes with exterior stress due to stress
concentration at grain boundaries [65]. With the extension of the an-
nealing time, more ε-martensitic transformation occurs and austenite
grain size also increases and becomes uniform. Due to the tendency of
high-Mn TWIP/TRIP steels to form bimodal grains during annealing
[67], grains with same size are aggregated in a certain area and the
number of hydrogen atoms in the unit grain boundaries is also in-
creased with increasing grain size, resulting in the boundaries of large
grains preferentially nucleating cracks [67]. Thus, at the time of frac-
ture, small grains are forced to crack. That is, grains with the same size
crack together, so the number of secondary cracks is relatively few
[65,66]. In such case, the entire intergranular fracture surface is
equivalent to a whole “sea” with only a few locations as “islands”. For
instance, in the S10 specimen with 5 × 10−6 s−1 strain rate, its Δα
value is 1.752, so it is relatively rough, as shown in Fig. 11(b). With the
condition that the size of the secondary cracks is large and its location is
rather singular, the fracture surface resembles an “island” surrounded
by the “sea”. Such a fracture surface is not rough enough. Therefore, Δα
is lower compared to a significantly rough surface. For S40 specimen,
the secondary cracks are few on the intergranular fracture with
1 × 10−6 s−1 strain rate. Its Δα value is 1.720, which is relatively small
compared to the values shown in Fig. 11(a) and (b). Thus, it is smooth
as shown in Fig. 11(c).
In the same way, for ductile fracture surfaces, Δα can be used to
characterise the number, size and distribution of micro-voids (green
Fig. 12. The generalised fractal curves of fracture surfaces for all specimens (a, b) and the relationship between Eloss and Dmin/Dmax (c, d) (the data points of the two
regions of (c, d) possess a similar percentage of the area of intergranular fracture AI/E).
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Applied Surface Science 470 (2019) 870–881
arrow in Fig. 7(g–l)). The more micro-voids and random the distribu-
tion is, the greater the Δα. Once the main cracks have been nucleated,
the crack tip stress changes from the original single-face stress state to a
three-dimensional stress state. As second-phase particles or inclusions
do not exist in the solid solution state of high-Mn TWIP/TRIP steels in
our work, the deformation of the crack tip continues to expand along
the plane that parallels the maximum shear stress after local plastic
deformation. More dislocations quickly occur inside materials. The
elimination, aggregation and entanglement of dislocations lead to many
small nuclear micro-voids. With increasing time, the micro-voids grow
and eventually form larger micro-caverns. At fast strain rates, such as
1 × 10−5 s−1, the short tensile duration corresponds to the short dis-
tance that hydrogen atoms diffuse into the material. Thus, there are few
intergranular fracture zones and abundant ductile fracture zones. These
large amounts of micro-voids have an uneven distribution corre-
sponding to the large “pit” on the “land”, as shown in Fig. 11(d–f) re-
sulting into a relatively rough fracture surfaces. Hence, there is a large
Δα. For instance, the large micro-voids are unevenly distributed on the
ductile fracture for S0 specimen at the1 × 10−5 s−1 strain rate. Its Δα
value is 1.837, so it is rough as shown in Fig. 11(d).
Compared with the strain rate of 1 × 10−5 s−1, at a slow strain rate,
such as 1 × 10−6 s−1, the whole tensile duration is much longer. Thus,
the distance of hydrogen atom diffusion is greater, resulting in more
intergranular fracture regions with less ductile fracture area.
Additionally, when the external intergranular crack is nucleated and
the crack tip undergoes more serious plastic deformation, the ductile
fracture region with such a small area undergoes an increase in the
dislocation and the elimination and entanglement cannot form suffi-
ciently large micro-voids. These micro-caverns are evenly distributed
with a small number in the fracture surface of the ductile fracture re-
gion corresponding to small “pits” on the “land”, which has only a small
impact on the surface roughness. Thus, Δα has a respectively small
value. For example, at the small micro-voids evenly distributed on the
ductile fracture at a 1 × 10−6 s−1 strain rate for S0 specimen, the Δα
value is 1.639, so it is smooth, as shown in Fig. 11(f). Between
Fig. 11(d) and (f), there is a relatively rough or relatively smooth state,
H. Fu et al.
for example, the S30 specimen with strain rate of 5 × 10−6 s−1. Here,
its Δα value is 1.726, as shown in Fig. 11(e).
4.5. Relationship between generalized fractal spectra and Eloss
The generalised dimension spectrum curves q-D(q) were obtained in
the range of −10 ≤ q ≤ 10 (Fig. 12(a, b)). From the q-D(q) curves,
when q > 0, D(q) decreases gradually with increasing q, which de-
scribes the macrostructural characteristics of the fracture surfaces. In
addition, when q < 0, D(q) increases gradually with an increase in the
absolute value of q, which describes the characteristics of the gradual
subtle bump on the fracture surface.
Fig. 12(a, b) suggest that the values of D0, D1 and D2 are approxi-
mately the same in an intergranular fracture surface as well as a ductile
fracture surface. These three values do not change with Eloss. However,
it was found that the values of Dmax and Dmin show slight differences.
Therefore, we established the relationship between Dmin/Dmax and Eloss
using the ratio of Dmin/Dmax to expand the difference between Dmax and
Dmin. Fig. 12(c, d) reveal that Dmin/Dmax decreases with an increase in
Eloss and satisfies a good linear negative correlation in both fracture
surfaces (Intergranular: R2 = 0.98014, Ductile: R2 = 0.96643), which
can be expressed as:
Intergranular: Dmin / Dmax = 0.33448Eloss + 2.03147
Ductile: Dmin / Dmax = 0.41905Eloss + 2.07824 (11)
The two linear fitting plots were also separated into two regions
with different colours. The data points in both regions have a similar
fraction of intergranular fracture area; the pink area represents AI/E
approximately 0.5 and the light blue area shows AI/E equal to or greater
than 0.79, as shown in Fig. 12(c, d). When q = −10, the large prob-
ability subset plays a decisive role and for q = 10, the small probability
subset plays a decisive role. Thus, the ratio of Dmin/Dmax represents the
ratio of the small probability subset to the large probability subset
characterising the degree of surface roughness. The smaller the value of
Dmin/Dmax, the smaller the surface roughness is. For example, the Dmin/
Dmax value for the intergranular fracture of the S40 specimen is 1.720
with 1 × 10−6 s−1 strain rate, so it is smooth as shown in Fig. 7(f). In
contrast, the Dmin/Dmax value of the intergranular fracture of S0 spe-
cimen is 1.814 with 1 × 10−5 s−1 strain rate, so it is rough, as shown in
Fig. 7(a). As discussed above, the reason is the same as with multi-
fractals in the formation of HE fracture surfaces.
It is well-known that the HE of metal materials is an energy-ab-
sorbing process. The material also has different Eloss at the same fraction
of intergranular fracture. Hence, the multi-fractal and generalised
fractal features of the fracture surface play a crucial role in HE. The
larger the value of Δα and Dmin/Dmax, the rougher and the more non-
uniform is the fracture surface. This means that the materials need to
absorb more energy in the fracturing process. For instance, the Δα value
decreases from 1.759 to 1.723 (in detail, 1.759 → 1.752 → 1.734 →
1.723) and the Dmin/Dmax value decreases from 1.777 to 1.735 (in de-
tail, 1.777 → 1.763 → 1.756 → 1.735) for the intergranular fractures for
all specimens at the strain rate of 5 × 10−6 s−1. This indicates that as
the PVFMs increases in the high-Mn TWIP/TRIP steels, the smoother
the intergranular fracture surfaces by HE are and the lower the energy
is absorbed during the fracture process, suggesting the greater Eloss. In
contrast, the rougher the surface, the more energy it absorbs, indicating
a lower Eloss.
5. Conclusions
In this work, both fractal and multifractal methods have been ap-
plied to quantitatively characterise the fracture surfaces caused by HE
in high-Mn TWIP/TRIP steels with various PVFMs and the similar dif-
ferences in ultimate tensile strength. Simple fractal analysis is not ac-
cpetable to describe the complexity of HE fracture surfaces, i.e. Ds and
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Applied Surface Science 470 (2019) 870–881
Eloss do not satisfy a clear relationship. However, the results of multi-
fractal analysis show that the width of multifractal spectrum Δα and the
parameter Dmin/Dmax of the generalised fractal dimension can quanti-
tatively characterise the roughness and uniformity of the HE fracture
surface. Both parameters Δα, and Dmin/Dmax satisfy a good negative
linear correlation with Eloss, i.e. Δα = −0.3433Eloss + 2.202467 and
Dmin/Dmax = −0.33448Eloss + 2.02147 (for intergranular fracture),
which indicates that the greater the Eloss, the smaller the Δα and Dmin/
Dmax corresponding to a smoother fracture surface. This new method of
quantitative fracture morphology for the evaluation of mechanical
properties and the energy–absorption process during fracture gives in-
sight into studying and predicting the failure of materials.
Acknowledgements
This project was supported by the National Natural Science
Foundation of China under Grant Nos. 51571029, U1760203 and State
Key Laboratory of Development and Application Technology of
Automotive Steels (Baosteel Group).
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