Metal Science and Heat Treatment, Vol. 52, Nos. 11 12, March, 2011 (Russian Original Nos.

. 11 12, November December, 2010)

DISPERSION OF STRUCTURE
UDC 669.14.018

DISPERSION OF THE STRUCTURE OF STEEL 35Kh UP TO NANOLEVEL

WITH THE AIM OF CREATING A MATERIAL FOR PRESSURE VESSELS
Yu. N. Simonov,1 A. P. Nishta,1 S. S. Yugay,1 and A. S. Pertsev1
Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 11, pp. 7 12, November, 2010.

A comparative study of the structure and mechanical properties of sheet and tube preforms from steel 35Kh after heat refining, cold rolling, and wobble forming is performed. It is shown that wobble forming produces a
positive effect on formation of an a-phase with homogeneous and dispersed cellular substructure in the whole
of the cross section of tube preforms, which ensures a favorable combination of strength, ductility, and impact
toughness. It is recommended to subject the tube preforms to subsequent annealing in order to raise the parameters of ductility and impact toughness without lowering the strength.

Key words: wobble forming, dispersion of structure, mechanical properties of tube preforms.

positive feature of this kind of deformation is its high locality, which makes it possible to use conventional equipment
for deforming materials with elevated and high strength
level; the same microvolume of the metal can be deformed
repeatedly, which produces a homogeneous structure and
substructure in the cross section of the metallic preform.
It cannot be excluded that due to the locality and the repeated nature of the deformation in wobble forming (or any
other treatment of the kind) the actual strain is substantially

INTRODUCTION
Development and installation of advanced technologies
for increasing the output, reducing the consumption of materials, and simultaneously raising the service reliability of machine parts and structures remains an important task of mechanical engineering and materials science.
One such technology is deformation of a material by a
wobbling tool (we will call it wobble forming). According to
the idea of this method of pressure treatment, one of the tools
(the female die or the male die) performs a wobbling (precessional) motion created by a special drive, while the other tool
performs translational motion created by a conventional hydraulic drive (Fig. 1). This method of treatment is especially
effective for making tube preforms and articles like pressure
vessels and hydraulic cylinders. Today articles of this type
are primarily produced with the help of mechanical treatment
(drilling) or by bending and welding of initial sheet preforms
followed by hardening heat treatment.
Wobble forming (WF) makes it possible to lower the
consumption of metal and to simplify the process of manufacturing of tube preforms on the whole. In addition, results
of studies performed in the last decades show that forming of
this type raises the entire set of characteristics of mechanical
properties and thus the reliability of the articles. Another
1

P
3
2

q
1

Fig. 1. Scheme of deformation of a tube preform in a through wobbling facility: 1 ) precessional tool; 2 ) deformed tube preform;
3 ) arbor.

Perm State Engineering University, Perm, Russia (e-mail:

mto@pstu.ru).

517
0026-0673/11/1112-0517 2011 Springer Science + Business Media, Inc.

518

Yu. N. Simonov et al.

TABLE 1. Chemical Composition of Steel 35Kh

Content of elements, wt.%
Preform

12-mm-thick sheet
Tube with wall thickness of 12 mm

Cr

Mn

Si

Ni

Cu

0.34
0.35

0.96
0.92

0.64
0.63

0.23
0.27

0.03
0.04

0.05
0.07

0.009
0.014

0.019
0.022

higher than the design one. Thus, the method of wobble

forming is an example of commercial process that implements to this or that degree the mode of severe plastic deformation.
The aim of the given work was a comparative study of
the fine structure and properties of sheet and tube preforms
from steel 35Kh obtained by rolling and wobble forming and
development of a process for manufacturing a reliable material for pressure vessels.
METHODS OF STUDY
We studied sheet and tube preforms from steel 35Kh.
The chemical composition of the preforms is presented in
Table 1.
The sheet and tube preforms were heat treated in a mode
consisting of hardening from 860C (40 min) in water and
subsequent tempering at 570C for 1 h with water cooling.
After the heat refinement the preforms were subjected to
cold plastic deformation. The sheet preforms were deformed
by rolling with 30 and 60% shrinkage; the tube preforms
were wobble formed with 42 and 63% shrinkage. Then the
cold-deformed preforms were annealed in a temperature
range of 300 650C with 1-h and 2-h holds.
The sheets and the tubes was then cut into preforms with
a thickness of 0.4 0.5 mm in an electrospark discharge machine and subjected to an electron microscopic study. Then
the preforms were thinned mechanically against sand papers
to a thickness of 0.05 0.10 mm and polished electrically
using anode dissolution in a phosphorus-chromium electrolyte (860 ml orthophosphoric acid + 100 g chromic anhydride). The foils obtained were studied under an EM-12M
electron microscope at an accelerating voltage of 100 kV and
a JEM-200CX microscope at 160 kV. One structural state
was studied for at least 5 foils; the number of studied fields
for each foil was at least 10.
The images were computer processed and the longitudinal and transverse sizes of fragments of the a-phase (laths,
cells, or subgrains depending on the structural state) and of
the cementite carbides were measured. The number of measurements in every case was no less than 500. We used formulas of mathematical statistics for processing the metallographic images [1] and computed the mean longitudinal and
transverse sizes of the structural components, the variance,
the standard deviation, the confidence interval, and form factor of each component.

The characteristics of strength and ductility were determined in accordance with the GOST 149773 Standard for
short cylindrical specimens with initial diameter of 5 mm in
a 1231U-10A universal testing machine at a deformation rate
of 2 mm/min. The recorded stress-strain diagram was used
to compute the ultimate rupture strength sr , the yield strength
s0.2 , and the elongation d. The contraction y was evaluated
in therms of the change in the diameter of the specimen. No
less than 4 5 specimens were tested after each variant of
treatment.
The impact toughness was computed using the results of
the tests in an MK-30 impact machine in accordance with the
requirements of GOST 945478 for specimens of types 3 and
17. The tests were performed at a temperature ranging from
+ 20 to 60C. Negative temperatures were obtained by
mixing liquid nitrogen with ethyl alcohol. The temperature
was controlled by a preliminarily calibrated copper-constantan thermocouple connected to a digital millivoltmeter.
The static crack resistance was evaluated in terms of the
crack resistance limit Ic. Preparation of the specimens, conduction of the tests, and processing of the results were performed according to GOST 25.50685 for flat specimens
with a thickness of 5 mm, a side notch, and a crack in the
mode of three-point bending using an INSTRON 5882 machine at a deformation rate of 0.5 mm/min. The relative
length of a crack l determined in accordance with GOST
25.50685 as the ratio of the total length l of the notch and of
the fatigue crack grown from it to the width b of the specimen; in our tests l = 0.45 0.55.
The test error in determination of the mechanical characteristics did not exceed 5% in any case.
RESULTS AND DISCUSSION
Properties of Steel 35Kh in the Initial State
The structure obtained in the preforms after heat refinement may be classified as disperse tempered sorbite represented by elongated subgrains (or cells) of ferrite inherited
from the martensitic structure and cementite carbides segregated primarily over boundaries of ferrite subgrains. The dislocation density inside the subgrains is not high.
In addition to the disperse tempered sorbite the structure
bears microvolumes that have experienced secondary recrystallization. These microvolumes have a size of about 5 mm

Dispersion of the Structure of Steel 35Kh with the Aim of Creating a Material for Pressure Vessels

and their volume fraction does not exceed 10 15%. Cementite carbides are encountered inside such ferrite polyhedrons.
Statistical analysis of the structure parameters of the tube
preforms (Table 2) shows that the sizes of ferrite subgrains
and cementite carbides in similarly oriented layers over the
thickness of a tube preform remain virtually invariable. At
the same time, comparison of structure parameters in an internal horizontal layer and in an internal vertical layer shows
that the transverse size of ferrite subgrains in the tangential
direction is somewhat larger than in the radial one (layers 3
and 6 in Table 2).
The results of the tensile and impact toughness tests
show that the tube preforms in such condition have the following mechanical properties: rupture strength sr = 860 MPa,
yield strength s0.2 = 550 MPa, elongation d = 12%, contraction y = 65%, impact toughness KCU + 20 = 1.65 MJ/m2, and
KCU 60 = 1.28 MJ/m2. The sheet preforms in the initial
state have close parameters of structure and mechanical characteristics.
Structure and Properties of Preforms from Steel 35Kh
after Rolling and Wobble Forming
The structure of disperse tempered sorbite is preserved
on the whole both after rolling and after wobble forming.
The most substantial difference of this structure from the initial (high-tempered) one is the absence of microvolumes
with features of secondary recrystallization and the presence
of a developed cellular substructure in the a-phase with elevated dislocation density inside the cells.
The results of statistical analysis show that when the reduction ratio is increased, the sizes of the cells change inconsiderably (Table 3). The shape factor of the cells remains virtually constant, i.e., K1 = 2.5 2.8, which reflects considerable elongation of the cells.
In contrast to the cell substructure formed by rolling, the
cells formed due to wobble forming contain subgrains of a
polygonal type, which divide a cell additionally into several
segments (Fig. 2a ).
Statistical analysis shows that the sizes of the cell substructure after wobble forming are noticeably smaller than

519

200 nm

200 nm

Fig. 2. Fine structure of steel 35Kh after wobble forming with 63%
reduction (a) and subsequent annealing at 570C for 1 h (b ).

after rolling (Table 3) and the cells themselves are more

equiaxed; K1 = 1.6 1.9. In addition, the given cellular substructure is very homogeneous both over the section of the
tube preform and in various directions; the mean transverse
size of the cells measured in various layers d = 160
170 nm, and the mean longitudinal size l = 270 310 nm
(wobble forming with e = 42%, layers 1, 3, 6 in Table 3).
The sizes of the carbide particles after rolling and after
wobble forming differ inconsiderably. However, we should
note that the form factor of the particles after rolling
K2 = 3.0 3.7, whereas after wobble forming K2 1.85 2.0.
In other words, on the whole, wobble forming yields a more
dispersed and equiaxed substructure than rolling.
Mechanical properties of sheets and tube preforms after
rolling and after wobble forming are presented in Table 4. It

TABLE 2. Parameters of Structure of a Tube Preform in the Initial State

Layer in the cross section
of the tube*

d, nm

Sd , nm

l, nm

Sl , nm

a, nm

Sa , nm

Sc , nm

k1 , nm

k2, nm

1 (external surface)

500 30

300

2800 30

950

100 20

60

320 70

200

5.6

3.2

3 (middle layer over the

wall thickness)
6 (internal surface)

580 40

300

2950 30

1030

100 7

50

200 10

80

5.1

2.0

820 60

400

2700 40

1200

100 20

60

400 80

300

3.4

4.0

The parameters of structure of layers 2, 4, 5 in the longitudinal section are not given in Table 2.

Notations: d and l are the mean transverse and longitudinal sizes of ferrite subgrains, respectively; a and c are the mean transverse and longitudinal sizes of the carbides, respectively; d, l, a, and c are given with a confidence interval at confidence probability 0.95; k1 = l/d is the shape
factor of ferrite subgrains; k2 = c/a is the shape factor of carbides; S is the standard deviation of the structure parameters.

520

Yu. N. Simonov et al.

TABLE 3. Parameters of the Structure of Preforms from Steel 35Kh after Rolling and Wobble Forming after Subsequent Annealing
Layer*

d, nm

l, nm

a, nm

c, nm

k1, nm

k2, nm

Rolling, e = 60%

External

271 8

660 190

43 4

160 48

2.50

3.70

Rolling, e = 60% + annealing at 570C, 1 h

External

289 40

531 85

59 3

140 8

1.84

2.37

WF, e = 42%

160 10

310 30

55 4

170 16

1.90

3.10

WF, e = 42%

170 10

270 20

70 6

140 7

1.60

2.00

WF, e = 42%

160 10

290 20

100 10

200 20

1.80

2.00

WF, e = 63%

160 10

260 20

65 8

120 14

1.60

1.85

WF, e = 63% + annealing at 570C, 1 h

210 20

350 30

86 4

160 10

1.63

1.86

WF, e = 63% + annealing at 570C, 2 h

377 56

614 107

120 7

180 9

1.70

1.50

Treatment mode

In cross section of a tube (layers 1, 3, 6 ) or a sheet (external layer).

Notations: WF) wobble forming; the structural parameters are denoted as in Table 1.

TABLE 4. Characteristics of Mechanical Properties of Preforms from Steel 35Kh after Various Treatment Variants
Treatment

sr , MPa

s0.2 , MPa

d, %

y, %

KCU + 20,
MJ/m2

KCT + 20,
MJ/m2

KCU 60,
MJ/m2

KCT 60,
Ic + 20,
Ic 60,
MJ/m2 MPa m1/2 MPa m1/2

1.45
0.78

0.48
0.32

0.98
0.62

0.37
0.24

83.2
88.3

79.2
99.9

e = 30%

785
820

560
760

15
12

Rolling
62
56

e = 30% + annealing at 570C

630

540

17

56

0.96

0.38

0.71

95.1

88.0

e = 60%

965

830

10

56

0.53

0.20

0.43

0.18

85.5

79.3

e = 60% + annealing at 570C

670

585

19

53

0.85

0.33

0.77

0.28

85.0

80.7

Initial state
e = 42%

800
977

550
900

15
12

Wobble forming
65
1.65
65
1.60

0.67
0.60

1.28
1.20

0.48
0.45

80.4
101.2

77.2
98.7

e = 42% + annealing at 570C

825

700

18

0.57

1.77

106.4

98.7

e = 63%

1003

952

11

60

1.48

0.50

1.15

0.40

88.4

95.4

e = 63% + annealing at 570C

840

757

17

67

1.80

0.53

1.65

0.44

99.3

90.6

Initial state

can be seen that both rolling and wobble forming raise substantially the strength parameters of the preforms, whereas
the ductility decreases somewhat. It is important that the impact toughness of the specimens tested at room and minimum climatic temperatures both with a soft and a sharp concentrator is considerably higher after wobble forming than
after rolling.
The static crack resistance at room temperature after rolling and after wobble forming changes by a dependence with
a maximum due to deformation with 30 40% reduction.
The ultimate crack resistance after wobble forming with
mean reduction e = 42% is substantially higher than after
rolling with e = 30%, i.e., I c+ 20 = 101.2 and 88.3 MPa m1/2,
respectively. After testing at minimum climatic temperature
( 60C) the change in the ultimate crack resistance after
rolling is the same as at room temperature. After wobble
forming with reduction of 42% the ultimate crack resistance
increases with respect to the initial value; when the degree of

68

2.0

reduction is increased to 63%, it remains invariable at a level

of 95 MPa m1/2 in contrast to rolled preforms.
Thus, wobble forming with high enough reduction does
not cause substantial decrease in the characteristics of impact
toughness and static crack resistance in contrast to rolling.
These differences are especially obvious in dynamic tests.
Structure and Properties of Deformed Preforms
after Recrystallization Annealing
Electron microscopic analysis shows that post-deformation annealing yields a subgrain structure in the preforms
both after rolling and after wobble forming (Fig. 2b ). The
boundaries of the subgrains are thin and well manifested.
The dislocation density inside subgrains is not high. Quite
frequently, subgrain boundaries exhibit a characteristic striated contrast, which is a feature of high-angle off-orientation
of these subgrains. After annealing, the sizes of the subgrains
are somewhat larger than after the corresponding mode of

Dispersion of the Structure of Steel 35Kh with the Aim of Creating a Material for Pressure Vessels

TABLE 5. Comparative Analysis of the Requirements of OST

3-168680 and the Properties of Rube Preforms after Various Treatment Variants
Requirements of OST 3-168680 for tube-type articles
Strength category

s0.2 , MPa,
at least

d, %,
at least

y, %,
at least

KCU 20,
MJ/m2,
at least

sr ; s0,2 , P

s0.2 , MPa

d, %

y, %

KCU 20,
MJ/m2

WF, e = 42%

550
900

15
12

65
65

1.65
1.60

WF, e = 63%

952

11

60

1.48

1.9

WF, e = 42% + annealing

at 570C, 2 h

700

18

68

2.00

1.7

1.80

1.5

WF, e = 63% + annealing

at 570C, 2 h

757

17

67

Note. Initial state: heat refining (hardening from 860C in water +

2-h tempering at 570C).

sr

800

40

80

30

70

20

60

y
700

600
200

300

400

500

600

700

tan , C
KCU, J/m2

+ 20C

1.3

60C

1.1
0

pressure treatment, which is a sign of migration of subboundaries in the annealing process.

The main mass of the cementite-type carbides after annealing, just like after cold plastic deformation, is arranged
over the boundaries of the components of the substructure.
The mean sizes of the carbides after annealing are somewhat
larger than directly after deformation. However, it should be
noted that after annealing very fine carbide segregations are
observable inside subgrains, which are most probably a consequence of the occurrence of processes of strain aging. The
possibility of strain aging is confirmed indirectly by the results of statistical analysis of the sizes of carbide particles.
Comparison of the data presented in Tables 2 and 3 shows
that cold plastic deformation lowers the sizes of carbide particles, especially the longitudinal ones. This should be connected primarily with mechanical separation of carbide particles in the process of cold deformation, which does not, however, exclude dissolution of individual fragments of particles
due to the action of the deformation.
As an example, we present in Fig. 3a dependences of the
characteristics of strength and ductility of specimens of tube
preforms from steel 35Kh on the temperatures of annealing
performed after wobble forming with 63% reduction.
According to the results of the tests, the behavior of the
strength and of the ductility does not depend on the degree of
reduction. For example, after annealing at 300C the strength
characteristics increase and the elongation decreases somewhat. It should only be noted that after the deformation with
e = 63% the growth in the strength characteristics is higher

y, %

s0.2

900

0.66
0.60
0.44

Initial state

d, %

1000

KS55
550
12
45
KS70
700
9
45
KS100
1000
5
40
Experimental properties of tube preforms
Treatment mode

521

200

400

600

tan , C
Fig. 3. Dependences of the characteristics of strength, ductility (a),
and impact toughness (b ) of tube preforms from steel 35Kh on the
temperature of post-deformation annealing (t = 1 h). Initial state:
wobble forming with 63% reduction: a) test temperature is 20C;
b ) 20 and 60C (the numbers at the curves).

than due to reduction e = 42%; the yield strength increases

by 70 80 MPa and 40 50 MPa, respectively. This fact is
another confirmation of the occurrence of strain aging processes. When the annealing temperature is increased to
600C, the strength characteristics decrease and the ductility
characteristics increase; the strength of the specimens wobble formed with reduction of 63% is preserved at a higher
level.
The dependence of the impact toughness of a tube preform from steel 35Kh after wobble forming with reduction of
63% and subsequent annealing is presented in Fig. 3b. It can
be seen that independently of the test temperature the impact
toughness increases upon growth in the temperature from
300 to 600C. Even at the temperature of maximum manifestation of the effect of strain aging (300C) its level is quite
high, i.e., KCU = 1.6 and 1.5 MJ/m2 at test temperatures of
+ 20 and 60C, respectively.
Comparative analysis of the characteristics of mechanical properties of steel 35Kh (Table 5) shows that wobble
forming ensures a higher strength than rolling, as well as a
higher ductility, static crack resistance and, what is the most

522

substantial, a higher impact toughness including the case of

minimum climatic temperature.
Comparison of the requirements of the OST 3-168680
specification for tube articles and the characteristics of the
mechanical properties of tube preforms after various variants
of treatment (Table 5) shows that the tube preform subjected
to heat refining meets only the KS55 strength category. The
tube subjected to wobble forming with 43% reduction and
subsequent annealing at 300C has a strength level meeting
the KS100 category. The tube wobble formed with 63% reduction and then annealed at 570C has a strength level
meeting category KS700 and possesses an almost doubled
ductility margin and tripled margin of the impact toughness.
CONCLUSIONS
1. Wobble forming yields a more dispersed and equiaxed
substructure than rolling. The size of ferrite grains after rolling is 270 290 nm; that after wobble forming is 160
170 nm.

Yu. N. Simonov et al.

2. Post-deformation annealing at 570C results in formation of a homogeneous subgrain structure with primarily
high-angle off-orientations. The size of the subgrains after
wobble forming with 63% reduction and subsequent 1-h annealing at 570C amounts to 210 nm.
3. Wobble forming produces a higher level of strength
than rolling at a higher ductility, static crack resistance,
and, what is the most important, at a substantially higher impact toughness including that at the minimum climatic
temperature.
4. Comparison of the requirements of the OST 3-168680
specification for tube-type articles with the mechanical properties of tube preforms after various treatment variants has
shown that wobble forming yields a reliable material for fabricating pressure vessels.
REFERENCES
1. S. A. Saltykov, Stereometric Metallography [in Russian], Metallurgiya, Moscow (1976).