materials

Article
Microstructure and Mechanical Properties of
34CrMo4 Steel for Gas Cylinders Formed by Hot
Drawing and Flow Forming
Yuebing Li 1,2 , Wei Fang 1 , Chuanyang Lu 1 , Zengliang Gao 1,2, * , Xiakang Ma 3 , Weiya Jin 1,2 ,
Yufeng Ye 4,5 and Fenghuai Wang 4,5
1 Institute of Process Equipment and Control Engineering, Zhejiang University of Technology,
Hangzhou 310032, China; ybli@zjut.edu.cn (Y.L.); 17857685226@163.com (W.F.); lvcykk@163.com (C.L.);
jinweiya@zjut.edu.cn (W.J.)
2 Engineering Research Center of Process Equipment and Remanufacturing, Ministry of Education,
Hangzhou 310032, China
3 Zhejiang Jindun Pressure Vessel Co. Ltd., Shaoxing 312300, China; maxiakang@126.com
4 Zhejiang Provincial Special Equipment Inspection and Research Institute, Hangzhou 310016, China;
13906536843@139.com (Y.Y.); wangfh@zjtj.org (F.W.)
5 Key Laboratory of Special Equipment Safety Testing Technology of Zhejiang Province,
Hangzhou 310016, China
* Correspondence: zlgao@zjut.edu.cn; Tel.: +86-571-8529-0402




Received: 19 March 2019; Accepted: 23 April 2019; Published: 25 April 2019


Abstract: An integral manufacturing process with hot drawing and cold flow forming was proposed
for large-diameter seamless steel gas cylinders. The main purpose of this study was to find out the
effects of the manufacturing process on the microstructure and mechanical properties of gas cylinders
made of 34CrMo4 steel. Two preformed cylinders were produced by hot drawing. One cylinder
was then further manufactured by cold flow forming. The experiments were carried out using
three types of material sample, namely, base material (BM), hot drawing cylinder (HD), and cold
flow-formed cylinder (CF). Tensile and impact tests were performed to examine the mechanical
properties of the cylinders in longitudinal and transverse directions. Microstructure evolution was
analyzed by scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) to reveal
the relation between the mechanical properties and the microstructure of the material. It is found
that the mechanical properties of the 34CrMo4 steel gas cylinders were significantly improved after
hot drawing and flow forming plus a designed heat treatment, compared with the base material.
The observations of microstructure features such as grain size, subgrain boundaries, and residual
strain support the increase in mechanical properties due to the proposed manufacturing process.

Keywords: flow forming; hot drawing; microstructure; mechanical properties; gas cylinder

1. Introduction
Gas cylinders are widely used to store and transport clean energy, such as compressed natural gas
cylinders on vehicles and tube trailers for the transportation of hydrogen. These cylinders containing
corrosive compressive gases are always operated under a high pressure over 20 MPa, which presents
fatality risk and challenges for the safety of the gas cylinders throughout their anticipated long service
life. Once the cylinders containing flammable gas rupture or leak, subsequent ignition is likely to occur,
which can result in fire fatality [1,2]. Good performance characteristics of gas cylinders should not
only ensure their safe operation, but also generate economic benefits. To optimize the performance
of gas cylinders, especially for lightweight and long-life ones, several research studies have been

Materials 2019, 12, 1351; doi:10.3390/ma12081351 www.mdpi.com/journal/materials

Materials 2019, 12, 1351 2 of 14

dedicated to raw materials and manufacturing processes. A brief patent review of steel alloys used
in the manufacture of gas cylinders was made by Nourani et al. [3]. Chromium-molybdenum steels
with an excellent strength-to-weight ratio are currently used. One of the authorized steels for gas
cylinders is 34CrMo4 (AISI 4130) steel which has superior corrosion resistance, mechanical properties,
hardenability, and deformation characteristics.
To achieve an optimal structure for the cylinder end, the hot drawing process is widely used to
fabricate gas cylinders [4,5]. The thermo-mechanical parameters of this process, such as temperature
and strain rate, have a direct effect on the microstructure and mechanical properties of the cylinder
material [3]. Rajan et al. [6] performed a study on the effect of heat treatment on the mechanical
properties of flow-formed AISI 4130 steel tubes, by comparing the microstructures of the preform and
finished flow-formed tubes using normalizing as well as hardening and tempering routes. The dynamic
recrystallization characteristics of 34CrMo4 steel were investigated by hot compression tests at a
temperature range of 900–1100 ◦ C, a strain rate range of 0.001–0.1 s−1 , and a strain of 0.9 [3,7]. For the
mechanical properties of 4130 steel, hardening behaviors until high strain rates of 103 s−1 and at
elevated temperatures up to 1000 ◦ C have been investigated by many researchers [8,9]. Recently,
the stress–strain curves at various strain rates for 4130 steel were described with the modified Lim–Huh
model, which includes the thermal softening effect [10] and the hyperbolic sine law in an Arrhenius-type
equation [11].
In order to improve the performance and the final product quality of gas cylinders, the authors
proposed an integral manufacturing process with a cold flow forming process for large-diameter
seamless steel gas cylinders [5]. The flow forming process is most widely used to produce thin-walled,
high-precision tubular products [12–14]. The effect of flow forming on material properties has also
been studied with the evolution of microstructure and texture [15–17]. Rajan and Narasimhan [18]
presented experimental observations of defects developed during flow forming of high-strength
steel tubes and gave some advice for the flow forming parameters. Podder et al. [19] showed that
variation in microstructural features and mechanical properties of the preforms due to heat treatments
could significantly affect the flow formability and the deformation homogeneity of the resultant
flow-formed tubes made of AISI 4340 steel. These research studies are usually limited to the laboratory
test results. However, limited research has been carried out on the effect of cold flow forming on
the material properties of the product cylinder. It is necessary to present the effects of the integral
manufacturing process with cold flow forming process on the performance of gas cylinders using
actual product materials.
This paper presents a systematic investigation of the effects of the manufacturing process proposed
in [5] on the performance of gas cylinders, especially the effect of the cold flow forming on the product
material properties. The mechanical properties of the gas cylinder materials before and after cold flow
forming were tested and compared with the requirements of the material standard. The variation of
the material with respect to microstructure, grain orientation, and boundary and local misorientation
following the manufacturing process was also investigated.

2. Materials and Methods

2.1. Materials and Cylinders

The billet used in this research was a block sample of 34CrMo4 steel. The chemical compositions
of the base material were measured using an ARL 4460 optical emission spectrometer (Thermo Fisher
Scientific, Waltham, MA, USA) and are given in Table 1, which satisfy the requirements of BS EN
10083-3: 2006 [20]. The base material is represented by “BM” in the rest of the paper. Two gas cylinders
with an inner diameter of 210 mm (see Figure 1) were used to investigate the effect of the forming
process on the material properties and the microstructures. The gas cylinder with a thickness of
7.94 mm was manufactured using the traditional process of hot drawing from the billet. This cylinder
is referred to as the hot drawing cylinder and is represented by “HD” in the rest of the paper. Another
Materials 2019, 12, 1351 3 of 14

Materials 2018, 11, x FOR PEER REVIEW 3 of 14

cylinder was initially manufactured using the HD process and further fabricated by cold flow forming
with aforming
flow final thickness reduced
with a final to 5 mm.
thickness This cylinder
reduced to 5 mm.isThis
referred to asisthe
cylinder cold flow-formed
referred to as the cold cylinder
flow-
and is represented
formed cylinder and byis“CF” in the rest
represented byof the paper.
“CF” TheofCF
in the rest thecylinder was CF
paper. The flow formedwas
cylinder withflowa thickness
formed
reduction
with of 37%reduction
a thickness by a single-pass
of 37% byforming. The roller
a single-pass feed
forming. rate
The andfeed
roller mandrel rotation
rate and mandrel speed were
rotation
controlled to be 1 mm/r and 180 r/min, respectively. In order to improve the toughness
speed were controlled to be 1 mm/r and 180 r/min, respectively. In order to improve the toughness of the cylinders,
a post
of heat treatment
the cylinders, a postwas
heatintroduced to both
treatment was HD andtoCF
introduced cylinders
both HD andafter deformation.
CF cylinders afterThe cylinders
deformation.
werecylinders
The 870 ◦heated
heated towere C for 45tomin
870 and water
°C for quenched,
45 min andquenched,
and water then tempered at 620
and then ◦ C for 1.5 h followed
tempered at 620 °C for
by water
1.5 cooling.
h followed To study
by water the performance
cooling. To study the differences
performancebefore and afterbefore
differences the forming process,
and after several
the forming
tests for several
process, mechanical
tests properties wereproperties
for mechanical carried out, including
were carried tensile tests, impact
out, including tensiletests,
tests,and hardness
impact tests,
tests.hardness
and In addition, microstructure
tests. In addition, was observed using
microstructure wasscanning
observed electron
using microscopy (SEM) and
scanning electron electron
microscopy
(SEM) and electron
backscatter backscatter
diffraction (EBSD). diffraction (EBSD).

Table 1. Chemical composition of 34CrMo4 steel (%, mass fraction).

Source
Source C C Si Si MnMn SS PP CrCr MoMo Ni Ni AlAl Fe
Fe
Measured
Measured 0.36 0.36 0.23 0.23 0.710.71 0.003
0.003 0.012
0.012 1.06
1.06 0.23
0.23 0.044
0.044 0.022
0.022 Balance
Balance
BS
BSEN
EN 10083-3
0.30–0.370.30– Max. 0.60–0.90
Max. 0.40 0.60– Max.Max.
0.035 Max.
Max. 0.025 0.90–
0.90–1.20 0.15–
0.15–0.30 -
10083-3 [20] - - - --
[20] 0.37 0.40 0.90 0.035 0.025 1.20 0.30

Figure 1. Gas
Figure 1. Gas cylinders
cylinders with
with aa diameter
diameter of
of 210
210 mm
mm used
used in
in this work, including
this work, including the
the hot drawing
hot drawing
cylinder
cylinder (HD)
(HD) and
and the
the cold
cold flow-formed cylinder (CF).
flow-formed cylinder (CF).

2.2. Tensile
2.2. Tensile Tests
Tests
Rectangular specimens
Rectangular specimensfor forthe
thetensile
tensiletest,
test,asas
shown
shown in in
Figure
Figure 2a,2a,
were extracted
were from
extracted the HD
from the and
HD
CF cylinders. A cylindrical coordinate system (L–R–T) was adopted to describe
and CF cylinders. A cylindrical coordinate system (L–R–T) was adopted to describe the sampling the sampling directions,
where the Lwhere
directions, direction
the Lcorresponds to the longitudinal
direction corresponds or axial direction,
to the longitudinal thedirection,
or axial R direction thecorresponds
R direction
to the radial direction,
corresponds and thedirection,
to the radial T direction andcorresponds to the transverse
the T direction correspondsor circumferential
to the transversedirection.
or
For both HD and CF cylinders, the tensile specimens for L and T directions were
circumferential direction. For both HD and CF cylinders, the tensile specimens for L and T directionsmachined to compare
the properties
were machinedintolongitudinal
compare theand transverse
properties directions, respectively.
in longitudinal and transverse The directions,
specimen sizes are shown
respectively. in
The
Figure 2b, sizes
specimen wherearetheshown
thickness t is equal
in Figure 2b, to the wall
where the thickness
thickness of t isthe cylinder.
equal to theItwall
should be noted
thickness of that
the
the T-direction specimens are nonplanar due to the curvature of the cylinders.
cylinder. It should be noted that the T-direction specimens are nonplanar due to the curvature of theTherefore, they were
flattened mechanically
cylinders. Therefore, theybefore
weretheflattened
test. Themechanically
tensile tests were carried
before out using
the test. an Instron
The tensile tests 8700
weremachine
carried
(Instron, Norwood, MA, USA) at ambient temperature under a loading rate
out using an Instron 8700 machine (Instron, Norwood, MA, USA) at ambient temperature under a of 0.2 mm/min.
loading rate of 0.2 mm/min.
Materials 2019, 12, 1351 4 of 14
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Materials 2018, 11, x FOR PEER REVIEW 4 of 14

(a)
(a)
5 15
R1 R

80
80

22.5
12.5

22.5
12.5
t
180 t
180

(b)
(b)
Figure
Figure 2. Specimens
2. Specimens forfor tensiletest,
tensile test,(a)
(a) Sampling
Sampling direction
direction(b)(b)
Specimen sizes.
Specimen sizes.
Figure 2. Specimens for tensile test, (a) Sampling direction (b) Specimen sizes.
2.3. Charpy Impact
2.3. Charpy TestsTests
Impact
2.3. Charpy Impact Tests
SimilarSimilar
to theto tensile
the tensile specimens,the
specimens, theimpact
impact test
test specimens
specimenswerewerealso extracted
also along
extracted L and
along T
L and T
SimilarFor
directions. to the
bothtensile
L- andspecimens, the
T-direction impact test
specimens, specimens
the werethickness
through-wall also extracted along
notchwas L and T
was machined
machined
directions. For
directions.
both L- and T-direction specimens, the through-wall thickness notch (see
(see FigureFor
3), both L- and
and the T-direction
specimen widthspecimens,
equal to the
the through-wall thickness notch
of thewas machined
Figure 3),Figure
(see and the3), specimen
and the specimen equalisisto
width iswidth the nominal
equal to the
nominal wall-thickness
wall-thickness
nominal of the
wall-thickness of the
cylinders.
cylinders.
cylinders.
The
TheThe
impact
impact tests were carried out on a ZBC-300A impact testing machine (MTS-SANS, Shanghai, China)
tests impact
were carried out
tests wereof on
carrieda out on a ZBC-300A impact testing machine (MTS-SANS, Shanghai, China) at a
ZBC-300A impact testing machine (MTS-SANS, Shanghai, China)
at a temperature ◦ −50 °C.
temperature of −50 of
at a temperature C.−50 °C.

Transverse Longitudinal
Transverse Longitudinal
specimen
specimen specimen
specimen
Charpy
Charpy
V-notch
V-notch
Charpy
Charpy
V-notch
V-notch
Figure 3. Specimens for impact test.
Figure3.3.Specimens
Figure forimpact
Specimens for impacttest.
test.
2.4. Hardness
2.4. Hardness Tests
TestsTests
2.4. Hardness
The hardness tests along the wall-thickness were carried out for both L- and T-direction
The hardness tests alongalong
The hardness the wall-thickness were carried out for both
for L- andL-T-direction specimens
specimens using thetests the wall-thickness
Vickers method, with a load of were carried
0.05 kgf out
and 10 both
s loading time. and T-direction
usingspecimens
the Vickers method,
using withmethod,
the Vickers a load of 0.05
with kgf and
a load 10 kgf
of 0.05 s loading
and 10 stime.
loading time.
2.5. Microstructure Tests
2.5. Microstructure Tests
2.5. Microstructure Tests
Samples for microstructure tests were extracted from both HD and CF cylinders, as shown in
Samples
Samples
Figure for for
4. Several microstructure
microstructure
samples testswere
were tests
made werethe
with extracted
extracted from
from
face in the both
both
normal HDHD and CF
and
direction CF
of L,cylinders,
and T, as
R,cylinders, shown in in
as shown
respectively.
Figure
FigureFor 4.
4. each Several
Several samples
samples
surface were
to be were made
made
observed, with
it with the face in the
the facegrinded
was initially normal
in the normal direction of
direction
to 1500 mesh L, R, and
of L, by
precision T,
R, andrespectively.
T, respectively.
sandpaper and
For
For each each
polished surface
surface tosurface
to be
to mirror be observed,
observed, it itwas
wasinitially
on a polishing initially
machine. grinded
grinded to
to1500
The samples 1500mesh
weremesh precision
then precision
etched by15
for sandpaper
bys in
sandpaperand and
a solution
polished
consisting to of
mirror
96% surface
ethanol on a polishing machine. The samples were then etched for 15 s in a(OM)
solution
polished to mirror surface on aand 4% HNO
polishing 3, then cleaned
machine. with alcohol.
The samples were Optical microscope
then etched for 15 s in a and
solution
consisting of 96% ethanol and 4% HNO3, then cleaned with alcohol. Optical microscope (OM) and
consisting of 96% ethanol and 4% HNO3 , then cleaned with alcohol. Optical microscope (OM) and SEM
analysis were performed using a Nova Nano SEM450 type field emission scanning electron microscope
(FEI Company, Hillsboro, OR, USA). Furthermore, after mechanical plus electrolytic polish of the L
Materials 12, 1351
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Materials 11, x FOR PEER REVIEW 5 of 145 of 14

Materials 2018, 11, x FOR PEER REVIEW 5 of 14

SEM analysis were performed using a Nova Nano SEM450 type field emission scanning electron
and R surfaces, (FEI
microscope an EBSD test was
Company, performedUSA).
Hillsboro, at a step size of 0.1 µm for both HD plusand CF samples,
SEM analysis were performed using a OR,
Nova NanoFurthermore,
SEM450 typeafter fieldmechanical
emission scanning electrolytic
electron
but 1polish
µm for
of the
the BM
L and samples.
R surfaces,The
an dimensions
EBSD test was of the scan
performed area
at a were
step sizeapproximately
of
microscope (FEI Company, Hillsboro, OR, USA). Furthermore, after mechanical plus electrolytic 0.1 µm for 57
both × 42and
HD µm for
CF
the HD samples,
andofCF
polish but 1
thesamples,µm for the BM
whereasan
L and R surfaces, samples.
they were
EBSD The
test570 dimensions
was×performed
420 µm for of the
at the scan
BM
a step area were
samples.
size of 0.1 µmapproximately
The
forworking
both HD and57 ×
distance
42 µm
was between for
CF samples, the
16 andHD and
but 117
µmmmCF samples,
andBM
for the whereas
thesamples. they
pixel binning were 570
used was
The dimensions × 420 µm
of 2the for
byscan the
2. Aarea BM samples.
scanning The working
electron microscope
were approximately 57 ×
distance
equipped forwas
42 µmwith between
a field
the HD and 16 samples,
emission
CF andtype
17 mm and the
electron
whereas gunpixel
they andbinning
were a570
TSL/OIM
× 420used was
µmEBSD 2 system
for the by
BM2.samples.
A (EDAX
scanning electron
TheInc., Mahwah,
working
microscope
distance equipped with a field emission typepixel
electron gunused
and awas TSL/OIM 2.EBSD system electron
(EDAX
NJ, USA) waswas used.between 16 and
The maximum 17accuracy
mm and ofthethe EBSDbinning
scanning system2 bywas A scanning
approximately 0.02 µm.
Inc., Mahwah,
microscope NJ,
equipped USA) was
with a was used. The maximum
fieldapproximately
emission type electron accuracy of the EBSD scanning system was
For the EBSD scans, the sample 65–70◦ gunfromand theahorizontal.
TSL/OIM EBSD The system
EBSD scan (EDAX control,
approximately
Inc., Mahwah, 0.02
NJ, µm. For
USA) was the EBSD
used. The scans,
maximum the sample
accuracy wasof approximately
the EBSD 65–70°
scanning from was
system the
data horizontal.
acquisition, and
The orientation
EBSD scanFor calibration
control, were all carried
data acquisition, out using the inbuilt software, TSL OIM
approximately 0.02 µm. the EBSD scans, the and orientation
sample calibration
was approximately were all carried
65–70° from outthe
Data using
Collection 5.0.
the inbuilt Data such
software, as average grain size and grain orientation difference angle of each view
horizontal. The EBSD scan TSL OIMdata
control, Dataacquisition,
Collection and
5.0. orientation
Data such as average grain
calibration were size and grain
all carried out
wereorientation
recorded. difference angle of each view were recorded.
using the inbuilt software, TSL OIM Data Collection 5.0. Data such as average grain size and grain
orientation difference angle of each view were recorded.
T
T
Face T
Face L L
Face RFace T
Face L L
Face R

R
Figure
Figure 4. 4.Specimens
Specimens for R and
for microstructure
microstructure texture
and test.
texture test.
Figure 4. Specimens for microstructure and texture test.
3. Results
3. Results
3. Results
3.1. Mechanical Properties
3.1. Mechanical Properties
3.1. Mechanical Properties
3.1.1.3.1.1. Tensile
Tensile Properties
Properties
3.1.1.The
The Tensile
basic Properties
basic mechanical
mechanical propertiesofofthe
properties the materials
materials were
wereobtained
obtained viavia
thethe
tensile tests,
tensile including
tests, including
yield strength,
yield strength, ultimate
ultimate
The basic tensile
tensile
mechanical strength,
strength,
properties and elongation.
andmaterials
of the elongation. Figure 5 shows
Figure 5via
were obtained the
shows stress–strain curves
the stress–strain
the tensile for
tests, including curves
the transverse
yield strength, specimens
ultimate (Figure
tensile 5a) and
strength, longitudinal
and elongation.specimens
Figure 5(Figure
shows 5b).
the The stress–strain
stress–strain curve
curves for
for the transverse specimens (Figure 5a) and longitudinal specimens (Figure 5b). The stress–strain
for the BM specimens is also included and in the figure. From Figure 5, the 34CrMo4The base material exhibits
curvethe
fortransverse specimens
the BM specimens (Figure
is also 5a)
included longitudinal specimens
in the figure. From (Figure
Figure 5b). stress–strain
5, the 34CrMo4 basecurve
material
good
for theductility
BM compared
specimens is alsowith the
included test
in results
the of
figure. the
From product
Figure materials.
5, the 34CrMo4Compared
base with the
material base
exhibits
exhibits good
material, ductility
the tensile compared
properties with
of the the test results of the product materials. Compared with the
good ductility compared with the testCF and HD
results of thematerials
productare obviously
materials. enhanced.
Compared Thethe
with tensile
base
base strength
material,ofthe tensile
thetensile properties
CF material of lower
is slightly the CFcompared
and HDwith materials of are
thatare the obviously
HD material enhanced.
for theThe The tensile
transverse
material, the properties of the CF and HD materials obviously enhanced. tensile
strength of the CF
specimens, material
while there is isnoslightly
obvious lower compared
difference for the with that of specimens.
longitudinal the HD material for the transverse
strength of the CF material is slightly lower compared with that of the HD material for the transverse
specimens, while
specimens, there
while is no
there is noobvious
obvious difference
differencefor for the
the longitudinal specimens.
longitudinal specimens.
1400
1400

1200
1400 1200
1400

1000
1200 1000
1200
(MPa)σ (MPa)

(MPa)σ (MPa)

800
1000 800
1000
HD-T
Stress, σStress,

HD-L
Stress, σStress,

600
800 600
800
CF-T
HD-T CF-L
400 BM 400 HD-L
600 600
CF-T BM
CF-L
200
400 BM 200
400
BM
0
200 0
200
0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Strain, ε (%) Strain, ε (%)
0 0
0 1 2 3 4(a) 5
Strain, ε (%)
6 7 8 9 10 0 1 2 3 4(b) 5 6 7 8 9 10
Strain, ε (%)

Figure 5. Stress–strain(a)
curve of 34CrMo4 for the (a) transverse (T) specimens (b)
and (b) longitudinal (L)
specimens.
FigureFigure 5. Stress–strain
5. Stress–strain curveofof34CrMo4
curve 34CrMo4 for
forthe
the(a)(a)
transverse (T) specimens
transverse and (b)
(T) specimens longitudinal
and (L)
(b) longitudinal
specimens.
(L) specimens.

The measured mechanical properties for all specimens are given in Table 2. The results of the
BM samples show that the strength and elongation satisfy the requirements of the standard [20].
Materials 2019, 12, 1351 6 of 14

The average yield strength and ultimate tensile strength of the CF and HD specimens are about 300
MPa higher than those of the base steel. The elongation of the HD and CF specimens is lower than
the BM specimens but it is still higher than the standard requirement of 12%. It can be concluded
that the mechanical properties of the product materials have changed after the manufacturing process
and heat treatment compared with the base steel but that they still satisfy the requirements of the
material standard.

Table 2. Tensile properties with average ± standard deviation.

Yield Strength Ultimate Tensile Strength Elongation

Specimen Name
(MPa) (MPa) (%)
BM 674 ± 4.5 913 ± 3.1 16.0 ± 0.4
HD-L 1142 ± 10.3 1214 ± 11.4 16.0 ± 0.5
HD-T 988 ± 25.4 1215 ± 17 13.0 ± 0.1
CF-L 1164 ± 3.3 1230 ± 0.4 15.5 ± 0.5
CF-T 975 ± 23.7 1207 ± 0.2 12.5 ± 0.2
BS EN 10083-3 [20] Min. 650 900–1100 12

For the average ultimate tensile strength of the formed components, small differences, namely,
16 MPa and −8 MPa in the longitudinal direction and transverse direction, respectively, are observed
between the CF and HD specimens. For the average yield strength, the differences of 22 MPa and
−13 MPa in longitudinal direction and transverse direction, respectively, are observed between the
CF and HD specimens. It is concluded that the subsequent cold flow forming process does not cause
significant changes in the mechanical properties of the material after heat treatment when compared
with the results of the HD specimens.
It is found that the yield strength in the transverse direction is obviously lower than that in
the longitudinal direction even in the same cylinder. The decrease is approximately 154 MPa and
189 MPa for the HD and CF specimens, respectively. In addition, there is a larger standard deviation in
the transverse direction for both HD and CF specimens, compared with the longitudinal direction.
This may be due to the amount of plastic deformation in the manufacturing process, which is different
in longitudinal and transverse directions.

3.1.2. Impact Properties

The impact test results for the two cylinders are shown in Table 3. It can be seen that the impact
toughness of the CF specimens is higher than that of the hot drawing one, in both transverse and
longitudinal directions. According to the results after cold flow forming, the average impact toughness
increases about 23%. However, considering the difference in specimen size used in the tests for the two
cylinders, this difference is insignificant. It can be concluded that the cold flow forming process does
not reduce the impact toughness.

Table 3. Impact properties with average ± standard deviation.

Specimen Width Depth Cross-Section Impact Energy Impact Toughness

Name (mm) (mm) Area (cm2 ) (J) (J/cm2 )
HD-L 25 8.05 2.01 85.3 ± 5.3 42.4 ± 2.6
HD-T 25 8.10 2.03 85.5 ± 5.5 42.2 ± 2.7
CF-L 25 4.95 1.24 69.6 ± 4.5 54.3 ± 1.8
CF-T 25 5.75 1.44 75.0 ± 4.8 50.4 ± 1.7

3.1.3. Hardness
Figure 6 shows the measured hardness along the radial direction from the inner to the outer
surface for the HD and CF specimens. It can be seen from the figure that the average value of hardness
Materials
Materials2018,
2018,11,
11,xxFOR
FOR PEER
PEERREVIEW
REVIEW 77 of
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14

3.1.3.
3.1.3. Hardness
Hardness
Figure
Figure 66 showsshows thethe measured
measured hardness
hardness along
along the
the radial
radial direction
direction fromfrom the the inner
inner toto the
the outer
outer
Materials 2019, 12, 1351 7 of 14
surface for the HD and CF specimens. It can be seen from the figure that the
surface for the HD and CF specimens. It can be seen from the figure that the average value of hardnessaverage value of hardness
in
in the
the whole
whole thickness
thicknessis is very
very close
closefor
for the
the HD
HDandand CF
CFsamples,
samples,as asshown
shown by by the
thedashed
dashed line
lineininFigure
Figure
in
6. the
6. Thewhole
The thickness
hardness
hardness values
valuesis very
are close
are uneven
unevenfor along
the HDthe
along andwall
the CF samples,
wall thickness,
thickness, as especially
shown
especiallyby thefordashed
for the CFline
the CF in Figure
samples.
samples. The
The 6.
The hardness
maximum values
hardness are uneven
values are along
located thein wall
the thickness,
mid-thickness especially
region for
maximum hardness values are located in the mid-thickness region and the maximum deviations of the
and CF
the samples.
maximum The maximum
deviations of
hardness
the
the average
averagevalues
values
values are located
in
in the in the mid-thickness
the whole
whole thickness
thickness are are region
48 HVand
48 HV andthe
and 56maximum
56 HV
HV forfor thedeviations
the HD
HD and andofCFthesamples,
CF average
samples,
values in the whole
respectively.
respectively. canthickness
ItIt can be
be concludedare 48 that
concluded HV
thatandthe 56
the HVflow
cold
cold for the
flow HD and
forming
forming CF samples,
process
process does
does not respectively.
not cause It can be
cause significant
significant
concluded
changes
changes in in that
hardnessthe cold
hardness of flow
of the
the forming
product
product processalthough
material,
material, does notthere
although causeis
there issignificant
aa difference
difference changes
in in hardness
in hardness
hardness of the
distribution
distribution
product
along
along the
thematerial, although there is a difference in hardness distribution along the wall-thickness.
wall-thickness.
wall-thickness.

440
440

420
420
HD
HD cylinder
cylinder
400
400
Hardness (HV)

380
380

360
360
CF
CF cylinder
cylinder
340
340

320
320

300
300
00 22 44 66 88
Distance
Distance from
from inner
inner surface
surface (mm)
(mm)
Figure
Figure 6.
6. Measured
Measured hardness
hardness along
hardness along the
the radial
radial direction
direction from
from the
the inner
inner to
to the
the outer
outer surface
surface for
for the
the HD
HD
and CF cylinders.
and CF cylinders.

3.2.
3.2. Microstructures
3.2. Microstructures
Microstructures
Figure
Figure 777 shows
Figure shows the
shows the metallographic
the metallographic structures
metallographic structures of
structures of the
of the different
the differentsamples.
different samples. There
samples. There is
There is an
an obvious
is an obvious
obvious
difference
difference between
difference between
between the the BM
the BM and
BM and the
and the formed
the formed cylinder
formed cylinder materials
cylinder materials
materials (HD (HD
(HD and and
and CF CF samples).
CF samples).
samples). For For
For thethe
the BM,
BM,
BM, aa
a large
large amount
amount of of lath
lath martensite
martensite can
can bebe found
found with
with aa small
small amount
amount of
of ferrite.
ferrite. The
The
large amount of lath martensite can be found with a small amount of ferrite. The microstructures are microstructures
microstructures are
are
tempered
tempered martensite
tempered martensite
martensite for for the
for the formed
the formed cylinder
formed cylinder materials
cylinder materials which
materials which have
which have been
have been heat
been heat treated
treated by
heat treated by quenching
by quenching
quenching
and
and tempering.
and tempering.
tempering. In In addition,
In addition, there
addition, there
there isis no
is no significant
no significant difference
significant difference
difference inin the
in the metallographic
the metallographic structure
metallographic structure between
structure between
between
HD
HD and
and CF
CF materials.
materials. AA similar
similar result
result can
can be
be found
found by
by SEM,
SEM, as
as shown
shown in
in Figure
Figure
HD and CF materials. A similar result can be found by SEM, as shown in Figure 8. The microstructure 8.
8. The
The microstructure
microstructure
of
of the
of the BM
the BM is
BM is martensite
martensite and
is martensite and ferrite
and ferrite and
ferrite and that
and thatof
that ofthe
of theformed
the formedcylinder
formed cylindermaterials
cylinder materialsis
materials istempered
is temperedmartensite.
tempered martensite.
martensite.

(a)
(a) (b)
(b) (c)
(c)

ferrite
ferrite

lath
lath martensite
martensite tempered
tempered martensite
martensite tempered
tempered martensite
martensite

Figure
Figure 7.
Figure 7. Optical
7. Optical microscope
microscope (OM)
(OM) images
images for
images for (a)
for (a) base
(a) base material
base material (BM),
material (BM), (b)
(BM), (b) HD,
(b) HD, and
HD, and (c)
and (c) CF
(c) CF materials.
CF materials.
materials.
Materials 2019, 12, 1351 8 of 14
Materials 2018,
Materials 11,11,
2018, x FOR PEER
x FOR PEERREVIEW
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8 of 14

(a)
(a) (b)
(b) (c)(c)
ferrite
ferrite

lath
lath martensite
martensite
tempered martensite
tempered martensite tempered martensite
tempered martensite

Figure 8. Scanningelectron
Scanning electron microscopy (SEM)
(SEM) images for (a) BM, (b) HD, and (c)(c)CF materials.
Figure
Figure 8.
8. Scanning electron microscopy
microscopy (SEM) images
images for
for (a)
(a) BM,
BM, (b)
(b) HD,
HD, and
and (c) CFCF materials.
materials.

TheThe fractographyof of tensile

tensile specimens for
forthe
thedifferent materials waswas
analyzed usingusing
SEM,SEM,
as
The fractography
fractography of tensile specimensfor
specimens the different
different materials
materials analyzed
was analyzed using SEM, as
as shown
shown in Figure
in Figure 9. The
9. Thefracture surface
fracture of
surface the BM is basically characterized of dimples (see Figure
shown in Figure 9. The fracture surface of theofBMtheisBM is basically
basically characterized
characterized of dimples
of dimples (see
(see Figure
9a), indicating
Figure a ductile
9a), indicating failure mode mode
a ductile in the BM. The voids
Theand cracks
andare found
aretofound
be adjacent to the
9a), indicating a ductile failurefailure
mode in the BM. in the BM.
The voids voids
and cracks cracks
are found to be adjacent
to be adjacent to the
to grain
the boundaries.
grain boundaries.The fracture
The surfaces
fracture of
surfacesthe HD
of and
the HD CF specimens
and CF are representative
specimens are of quasi-
representative of
grain boundaries. The fracture
cleavage characterized by the
surfaces
flat flat
of the
facets with
HD and
teartear
CF specimens
ridges, and
are representative
dimples, manifesting
of quasi-
a mixed
quasi-cleavage
cleavage characterized
characterized by the by the facets with ridges, and dimples, manifesting a mixed
brittle/ductile failure mode, as flat
shown facets with 9b–e.
in Figure tear ridges,
At the same and dimples,
time, the manifesting
serrated cracks a mixed
and
brittle/ductile
brittle/ductile failure
failure mode,
mode, as shown
as shown in Figure
in Figure 9b–e. At the same time, the serrated cracks and
discontinuous voids are located at the edges of the 9b–e. At the
flat facets. It cansame time, the
be inferred thatserrated
the voidscracks and
initially
discontinuous
discontinuous voids
voids are
are located
located at
at the
the edges
edges of
of the
the flat
flat facets.
facets. It
It can
can be
be inferred
inferred that
that the
the voids
voids initially
initially
nucleate at grain boundaries and then grow and coalesce to become cracks along the grain
nucleate
nucleate atatgrain
grainboundaries
boundaries andandthen then
grow growand coalesce
and in to become
coalesce cracks along the grain
alongboundaries,
boundaries, inducing a partial quasi-cleavage fracture the HD to andbecome cracks
CF tensile specimens. the grain
inducing a partial quasi-cleavage fracture in the HD and CF tensile
boundaries, inducing a partial quasi-cleavage fracture in the HD and CF tensile specimens. specimens.

(a) (b) (c)

(a) (b) (c)

(d) (e)
(d) (e)

Figure 9. The fractography of tensile specimens for (a) BM, (b) HD-L, (c) HD-T, (d) CF-L, and (e) CF-T.

Figure
Figure
Figure 10 fractography
9.9.The
The shows the orientation
fractography of
of tensile maps for for
tensile specimens
specimens the(a)
for BM
(a) BM,
BM, as(b)
well
(b) as the
HD-L,
HD-L, HD and
(c) HD-T,
(c) HD-T, (d)CF
(d) materials
CF-L,
CF-L, and(e)
and in both
(e)CF-T.
CF-T.
longitudinal and transverse directions obtained by EBSD. It can be observed that there are no distinct
Figure 10
Figure
orientations10ofshows
shows the
grainsthe orientation
orientation
in these maps for
three materials andtheinBMbothasLwellwell
and Tasasdirections.
the HD
the HD and
and
TheCF CF materials
materials
average grain inin both
both
sizes
longitudinal
longitudinal and transverse
of the BM, HD-L,
and transverse
HD-T, CF-L, directions
and CF-T
directions obtained
materials
obtained byare
by EBSD.
11.22,
EBSD. It1.02,
It can be
can be observed
observed
1.06, that
1.00, andthat there
1.07there are no
no distinct
distinct
µm, respectively.
are
The grain of
orientations
orientations size of thein
of grains
grains inBM is approximately
these
these three materials
three materials 11and
times
and in as
in large
both
both as those
LL and
and of the HD
TT directions.
directions. Theand CF materials
average in
sizes
grain sizes
bothBM,
of the
of longitudinal
HD-L, HD-T, and transverse
CF-L, anddirections. The total
CF-T materials are numbers
11.22, 1.02, of 1.06,
grains investigated
1.06, 1.00,
1.00, and
and 1.07 of
1.07µm,
µm,therespectively.
BM, HD-
respectively.
TheL, HD-T,
grain CF-L,
size of and
the CF-T
BM materials
is are
approximately 917, 1331,
11 times1280,
as 1540,
large and
as 1123,
those respectively.
of the
The grain size of the BM is approximately 11 times as large as those of the HD and CF materials in both HD and CF materials in
both longitudinal
longitudinal and transverse
and transverse directions.
directions. TheThe
totaltotal numbers
numbers of grains
of grains investigated
investigated of of
thethe BM,
BM, HD-
HD-L,
L, HD-T,
HD-T, CF-L,
CF-L, andand CF-T
CF-T materials
materials areare
917,917, 1331,
1331, 1280,1280, 1540,
1540, andand 1123,
1123, respectively.
respectively.
Materials 2019, 12, 1351 9 of 14
Materials 2018, 11, x FOR PEER REVIEW 9 of 14

(a) (b) (c)

(d) (e)
Figure 10. The
The orientation
orientation maps
maps for
for (a) BM, (b) HD-L, (c) HD-T, (d) CF-L, and (e) CF-T.
CF-T.

Figure
Figure 11
11 illustrates
illustrates the
the grain
grain boundary
boundary maps for the BM, HD, HD, and CF materials.
materials. InIn this
this figure,
figure,
high-angle grain boundaries (HAGBs) with misorientation of more than 15 ◦ and low-angle grain
high-angle grain boundaries (HAGBs) with misorientation of more than 15° and low-angle grain
boundaries
boundaries (LAGBs)
(LAGBs) with misorientation of 5–15°5–15◦ are
are shown
shown with
with black
blackand
andgreen
greenlines,
lines,respectively.
respectively.
The misorientation distributions of grain boundaries in different materials are shown
The misorientation distributions of grain boundaries in different materials are shown in Figure in Figure 12.
12.
The
The initial
initialmicrostructure
microstructure shows a high
shows percentage
a high (~86%) (~86%)
percentage of LAGBs,
of namely,
LAGBs,the subgrain
namely, theboundaries,
subgrain
in the BM, whereas
boundaries, in the BM, the percentages
whereas of the HAGBs
the percentages are relatively
of the HAGBs large (~40%)
are relatively in both
large (~40%) HD and
in both HD
CF materials.
and CF materials.

(a) (b) (c)

(d) (e)
Figure
Figure 11.
11. The
The grain
grain boundary
boundary maps
maps for
for (a)
(a) BM,
BM, (b)
(b) HD-L,
HD-L, (c)
(c) HD-T, (d) CF-L,
HD-T, (d) CF-L, and
and (e)
(e) CF-T.
CF-T.
Materials 2019, 12, 1351 10 of 14
Materials 2018, 11, x FOR PEER REVIEW 10 of 14

Materials
0.6 2018, 11, x FOR PEER REVIEW 0.5 10 of 14

0.50.6 0.5
0.4 HD-T
0.40.5 HD-L
0.4 HD-T
Frequency

Frequency
0.3
0.30.4 HD-L
Frequency

Frequency
0.3
0.2
0.20.3
0.2
0.10.2 0.1

0.1
00.1 0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60
0 Misorientation (°) 0 Misorientation (°)
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60
(a)
Misorientation (°) (b) (°)
Misorientation
(a) 0.5 (b)
0.5
0.4 CF-T
0.4 CF-T
CF-L
Frequency

0.3 CF-L
Frequency

0.3
0.2
0.2
0.1
0.1
0
0 0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60
0 4 8 12 16 20Misorientation
24 28 32 36 (°) 40 44 48 52 56 60
Misorientation (°)
(c)
(c)
Figure 12.
12.The
Figure12. Themisorientation
misorientation distributions of grain
distributions of grainboundaries for(a)(a)
boundariesfor
for (a) BM,
BM,
BM, (b)
(b)(b) HD,
HD,
HD, (c)
(c)(c) CF.
CF.CF.

The
The
Thelocal
local
local misorientation
misorientationmaps
misorientation mapscorresponding
maps corresponding
corresponding to to materials
tomaterials withdifferent
materialswith different
different processes
processes
processes areare
are shown
shown
shown in in
in
Figure
Figure 13.
13. It is clear that the residual
residual strain
strain is
is obviously
obviously larger
larger in
in the
the BM
BM than
than that
that in
in the
the
Figure 13. It is clear that the residual strain is obviously larger in the BM than that in the HD and CF HD
HD and
and CF
CF
materials.
materials.The
materials. concentrations
concentrations of
Theconcentrations of residual strain frequently
residual strain frequentlyoccurred
occurredatatthethegrain
grain
grain boundaries
boundaries
boundaries in in
in the
thethe
BM.
BM.
BM.There
There
Thereis still
isis stillaaacertain
still certainamount
certain amountof
amount ofgrains
of grains with little
with little
with residual
littleresidual strain
residualstrain adjacent
strainadjacent toto
adjacent to the
the
the grains
grains
grains with
with
with high
high
high
residual
residual strain
strain
residual strainin
ininthetheBM.
the BM.
BM.

(a) (b) (c)

(a) (b) (c)

(d) (e)
(d) (e)
Figure
Figure 13.The
13. Thelocal
localmisorientation
misorientation maps
maps for
for (a)
(a) BM,
BM,(b)
(b)HD-L,
HD-L,(c)
(c)HD-T,
HD-T,(d)
(d)CF-L,
CF-L,and (e)(e)
and CF-T.
CF-T.
Figure 13. The local misorientation maps for (a) BM, (b) HD-L, (c) HD-T, (d) CF-L, and (e) CF-T.
Materials 2019, 12, 1351 11 of 14

4. Discussion
The effect of sampling in tensile tests for the transverse specimens is first checked. Unlike the
longitude samples, the flattening introduces a pre-strain on the transverse specimens. With reference
to the cold-bending of steel plate to pipe [21], the strain ε(x) imparted due to flattening at a distance (x)
from the mid-thickness of the thickness t and outer diameter D can be related by the following equation:

2x
ε(x) = . (1)
D−t
The strain is negative from mid-thickness to outer surface and positive from mid-thickness to
inner surface. The compressive strain at the outer surface is about 3.6% for the transverse specimen
from the HD cylinder and 2.3% from the CF cylinder. During the flattening and the subsequent tension
test, the outer wall is subjected to compression–tension strains, which indicates the Bauschinger effect.
The Bauschinger effect results in a lower yield strength, which has been adopted to explain the decrease
in yield strength of linepipe steels under repeated tension and compression strains [22,23]. Meanwhile,
the process of flow forming brings about compressive strains in the cylinder transverse, which further
reduces the yield strength due to the Bauschinger effect. Then, it drops more for CF than for HD. To sum
up, the decrease in yield strength of the transverse specimens may result from the combination effect of
flow forming and specimen preparation. Nevertheless, the strength properties of the cylinder exceed
the minimum required high ultimate tensile strength (1200 MPa) and yield strength (900 MPa) [6].
From the microstructure view as shown in Figure 9, the non-distinct orientations of grains may
result from the fact that the differences in tensile strength are not apparent in these three materials and
in both L and T directions. HD and CF tested in the current work were heat treated after forming to
eliminate the significant elongated grains along the longitudinal direction and residual stress. During
the heat treatment of HD and CF, thermal recovery and recrystallization occurred, resulting in the
fine equiaxed grains present in the HD and subsequent CF materials. In this way, the anisotropic
characteristics in the HD and CF materials can be drastically alleviated, avoiding the extremely weak
properties in certain orientations of the materials.
The slight differences in tensile strength can be deduced from the grain sizes. As mentioned
above, the fine grains in the HD and CF materials were primarily caused by the heat treatment which
induced the thermal recovery and recrystallization of materials. The grain sizes in the transverse
direction are always larger than those in the longitudinal direction of both HD and CF materials,
attributing to the extension of the longitudinal length in the HD and CF processes. Additionally,
the grains of the HD material in the longitudinal direction are coarser than those of the CF material in
the same direction, whereas it was the opposite in the transverse direction of the HD and CF materials.
This phenomenon may be mainly attributed to the deformation mechanism of CF which reduced the
cross-section area to extend the longitudinal length of the gas cylinder by external pressure in the
radial direction. It should be noted that the volume of the gas cylinder was nearly constant during that
process. Therefore, extruding the cylinder in the radial direction would stretch the grains along the
longitudinal direction, leading to the growth of grain size in the transverse direction and the reduction
of grain size in the longitudinal direction. It was therefore inferred that the CF process exerted an effect
of refining grains in the longitudinal direction and coarsening grains in the transverse direction on CF
materials. Meanwhile, the mechanical strength is considered to be predominantly dependent on the
grain size according to the Hall–Petch relationship which can be expressed as follows [24]:

σs = σ0 + kd0.5 , (2)

where σ0 is the material strength, σ0 is the intrinsic strength of a metal, k is the Hall–Petch constant,
and d is the average grain size. Considering this, it is reasonable that the value of yield and ultimate
tensile strengths are maximum in the CF-L materials and minimum in the BM because the grains are
finest in the CF-L material and coarsest in the BM.
Materials 2019, 12, 1351 12 of 14

The impact property is also affected by the process of cold flow forming which results in the
change of microstructure and crystallographic textures [16,25]. However, the gas cylinder after cold
flow forming was heat treated. In consideration of the thermal recovery and recrystallization effects
generated by the heat treatment, the dislocation density was therefore decreased, leading to the decline
in the amount of subgrain boundaries appearing in the HD and CF materials. Although the ratio of
subgrain boundaries was decreased in the HD and CF materials, the grain sizes of HD and CF were
smaller than those of the BM, introducing a larger amount of grain boundaries per volume in the
HD and CF materials than that in the BM. The grain boundaries are regarded as the barriers to the
dislocation movements, which can produce a strain-hardening effect on the deformation and strength
of the materials. The refined grains possess a higher resistance to brittle cleavage fracture since grain
boundaries are effective barriers to the propagation of brittle fractures [26].
In general, the hardness affected by flow forming is reduced from the outer surface toward
the inner layers [27,28]. It should be noted that the gas cylinder after cold flow forming was heat
treated. Overall, this suggests that the appearance with respect to hardness is a combined effect of
deformation and heat treatment. This trend was also found for high-pressure steel cylinders treated by
quenching and tempering [29]. The explanation for that phenomenon may come from the samples’
microstructure [17]. The varied hardness indicates that the microstructures along the thickness are
varied, which can be further investigated.
An attempt to reveal the performance characteristic of the gas cylinders was also made using
the local misorientations. It has been stated that the local misorientation measured by EBSD can be a
function of geometrically necessary dislocation (GND) density as expressed below [30]:

2θ
ρGND = , (3)
µb

where ρGND is the GND density at the investigated point, θ is the local misorientation angle, µ is the unit
length of the point, and b is the Burger’s vector (~0.253 nm for steels [31]). Based on the relationship
between local misorientation and GND density, it can be concluded that there were significant
dispersions of dislocation density at the interfaces between high-residual-strain and low-residual-strain
grains in the BM, resulting in the preferential stress concentration produced at these interfaces in the
tensile and impact tests. It is therefore inferred that the voids and cracks would primarily initiate at the
aforementioned interfaces, leading to the low yield and ultimate tensile strengths of the BM specimens.
Due to the heat treatments after HD, thermal recovery was introduced to the HD material, dramatically
reducing the dislocation density and residual strain in the material. The local misorientation, namely
the residual strain, observed in Figure 13b,c is obviously lower in the HD materials than that in
the BM. In the HD and CF materials, as displayed in Figure 13b–e, the residual strains are mainly
aggregated at the subgrain boundaries, especially at the serrated boundaries and triple joints of grain
boundaries. Consequently, the voids and cracks can be initially induced at and propagated along those
sites during tensile and impact tests. This is in agreement with the inference from the fractography
of the tensile specimens as shown in Figure 9. There is no obvious difference in the distributions of
residual strain between the longitudinal and transverse directions of the HD and CF materials as
shown in Figure 13b–e.

5. Conclusions
(1) The mechanical properties of the product cylinder materials all satisfy the requirements of the
material standard. The tensile properties of the 34CrMo4 steel gas cylinders are obviously
improved after the hot drawing and cold flow forming processes plus heat treatment compared
with the base material. Therefore, the proposed manufacturing process and heat treatment used
in the manufacture of the gas cylinders are acceptable.
(2) The mechanical properties and the impact toughness of the cold flow-formed cylinder are very
similar to those of the hot drawing cylinder after heat treatment. Therefore, the cold forming
Materials 2019, 12, 1351 13 of 14

process would not cause a reduction of the material’s strength and the process parameters and
heat treatment plan are acceptable.
(3) The grain sizes of the HD and CF materials are significantly smaller than those of the BM, leading
to the increase in the mechanical properties of the HD and CF materials. The microstructures of
the HD and CF materials are very similar, including grain size, subgrain boundaries, and residual
strain. This confirms the correctness of the processing parameters and the heat treatment plan
used in the manufacture of the gas cylinders.
(4) The primary sites for voids and cracks during the mechanical tests of the BM are the interfaces with
large dispersion of dislocation density. Meanwhile, the voids and cracks should be preferentially
initiated at and propagated along the serrated boundaries and triple joints of the grain boundaries
in the HD and CF materials during the tensile and impact tests.

Author Contributions: Conceptualization, Z.G. and X.M.; Data curation, W.F. and C.L.; Formal analysis, C.L.;
Funding acquisition, Y.L.; Investigation, Y.L., W.F., W.J., Y.Y. and F.W.; Methodology, Z.G.; Supervision, Z.G. and
X.M.; Writing—original draft, Y.L.; Writing—review and editing, C.L. and W.J.
Funding: This research was funded by the National Natural Science Foundation of China, grant numbers 51605435
and 51575489.
Conflicts of Interest: The authors declare no conflict of interest.

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