Influence of the plasma stream irradiation on the surface modification, structure and properties of materials
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Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2000
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| Cite this: | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials / V.I. Lapshin, I.M. Neklyudov, V.I. Tereshin // Вопросы атомной науки и техники. — 2000. — № 6. — С. 146-151. — Бібліогр.: 13 назв. — англ. |
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| author | Lapshin, V.I. Neklyudov, I.M. Tereshin, V.I. |
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| citation_txt | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials / V.I. Lapshin, I.M. Neklyudov, V.I. Tereshin // Вопросы атомной науки и техники. — 2000. — № 6. — С. 146-151. — Бібліогр.: 13 назв. — англ. |
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UDC 533.9
146 Problems of Atomic Science and Technology. 2000. № 6. Series: Plasma Physics (6). p.146-151
INFLUENCE OF THE PLASMA STREAM IRRADIATION ON THE
SURFACE MODIFICATION, STRUCTURE AND PROPERTIES OF
MATERIALS
V.I.Lapshin, I.M.Neklyudov, V.I.Tereshin
National Scientific Center “Kharkov Institute of Physics and Technology”
61108 Kharkov, Ukraine
1. Introduction
Investigation of processes of intensive pulsed fluxes
of particles and radiation influence on materials
properties is now of great interest. This is due to two
reasons at least. On the one hand, there is a necessity of
investigations of fusion reactor materials behaviour
under the irradiation by powerful pulsed plasma streams
[1-4]. On the other hand, there was shown the
possibility of material surfaces modification and
hardening by pulsed plasma streams irradiation [5-10].
For forecasting the behavior of the fusion reactor
materials irradiated by powerful plasma streams during
many years there were used data obtained in
investigations of materials behavior under their
irradiation with steady-state high-energy ion beams of
hydrogen and helium. In this case the influence of such
parameters, as wide energy spectrum of particles,
bombarding materials surfaces, and pulsed character of
irradiation, that are essential for conditions of fusion
reactor operation, was not taken into account.
As it was shown at the beginning of eightieth [11],
due to the spread of particles by energy one of the most
intensive factors of surface erosion, namely radiation
helium blistering, can be suppressed. This was the
reason for the verification of the conclusions about the
possibility of a number of materials using in fusion
reactor. As to the investigation of pulse surface loading,
this is appeared to be of importance when there was
shown that it is not possible to avoid such strong plasma
instabilities as current disruption and others, followed
by high power pulsed plasma flows (with power density
1-10 MW/cm2) to the surfaces. The first experiments,
carried out with pulsed plasma streams [1-3], have
shown that such pulse plasma surface loading
essentially influence the structure and mechanical
properties of metals and constructional steels.
2. Experimental installation and diagnostics
All experiments, described here, were carried out in
“Prosvet” device with the pulse plasma accelerator
(PPA) as a plasma source [12]. Coaxial plasma
accelerator with cathode 5 cm in diameter and 60 cm in
length, and outer anode 12 cm in diameter generated
plasma streams with the parameters as follows: plasma
density (1-2)x1014 cm-3, average ion energy up to 2 keV,
pulse duration (3-5) µs, the repetition rate 1 shot per 3-5
min. Plasma energy density was varied in the range of
(5-40) J/cm2. PPA operated with different working
gases. Hydrogen, nitrogen, helium, argon or their
mixtures were used in those experiments.
The samples of different geometry and materials
were used in these experiments. Among these there
were samples of vanadium, niobium and nickel [1-3],
copper and its alloys, stainless steels H16N15M3B and
H18N10T [4, 10], as candidates for the first wall or
inner elements of fusion reactor, as well as steels 40H,
12HN3A, ShH15, steel 45 and other steels and hard
alloys VK8, VK20 [6, 8, 9, 11]. The geometry of
samples was varied in dependence on type of
experiment. For investigations of mechanical properties
of materials samples of 200 µm in thickness with area
of surface 10x3.5 mm were in use. The surfaces of
annealed samples were chemically and electrolytically
polished before irradiation. Those samples were placed
in special supporting system providing good thermal
contact with metal substrate. The temperature of sample
surface was not controlled, but it could achieve the
melting point. For analysis of surface modification the
samples of (3-5) cm in diameter and 5 mm in thickness
were utilized.
Magnetic and electric probes, local calorimeters,
bolometers, spectroscopy and mass-energy analyzer
were used for measurements of plasma parameters. As
to the surface analysis, there were used microhardness-
meter, profilograph, optical and electron microscopes,
metallography, X-ray analysis and so on. Mechanical
properties of samples were defined by deformation
diagrams of sample tension.
3. Results of experiments and discussion
3.1. Vanadium and niobium
Vanadium and niobium samples were irradiated by
plasma streams up to the dose of 2.4x1018 ion/cm2
(around 400 shots). Analysis of sample surfaces with
scanning electron microscope has shown that very deep
cracks appeared at the boundary of grains of both
materials as a result of irradiation (Fig. 1).
It was possible to expect that such a strong
intergranular cracking between grains could influence
the mechanical properties of the whole sample.
Especially that under the irradiation the surface layer
(about (1-3) µm) microhardness was increased by 3-6
times (Fig. 2). Nevertheless, tension test of the
irradiated samples of vanadium and niobium had shown
that their mechanical properties were not essentially
changed.
As it was mentioned above, the temperature of the
sample surface layer could be essentially increased
under irradiation due to the high-energy deposition into
the sample. Increasing the sample temperature provides
drastic increase of the spread of hydrogen diffusion. As
147
Fig.1. Microphotography of sample surfaces, irradiated
by hydrogen plasma with fluence 1.8x1018 cm-2:
Up – niobium, down – vanadium;
a – common view, b – details of structure
the result, one part of hydrogen abandons the material,
but another one is accumulated in the region of inter-
grains boundaries, forming the gas-filled microcavities
and bubbles of high pressure. Besides, in the bulk of
material there are formed rather stable complexes of
hydrogen atoms with radiation-induced defects and
atoms of impurities that provides hardening of the
surface layer.
3.2. Copper and its alloys
Copper and its alloys are discussed as possible
structural materials of fusion reactor. As far as in the
case of FR copper materials should be influenced by
hydrogen, there was a necessity to exclude such of
copper alloys that have high “hydrogen brittleness”. The
most stable with respect to the “hydrogen brittleness”
were found the following materials: copper produced by
Fig.2. Dependencies of microhardness of vanadium
surface (ο, • ) and niobium one (∆,▲)
on the depth of indentor immersion in initial
(o, ∆) and irradiated (• , ▲)states
electron-beam melting (MVE) as well as types of
copper alloys developed in the NSC KIPT - copper
micro-alloyed by palladium (MVP), yttrium (MMVI),
scandium (MMVS), and zirconium (MMVC).
The irradiation of samples of these materials was
carried out under the plasma stream energy loading of
10 J/cm2.pulse up to the dose 1.5x1018 cm-2. Mechanical
properties of samples, examined under the room
temperature, are shown in Table 1.
One can see from this table that treatment of copper
materials by plasma leads to the increasing of the yield
point and to the ultimate strength as well as to the
decreasing of their plasticity. One need to note that the
maximum increase of yield point is observed for non-
alloyed copper produced by electron-beam melting
(about 270%). An increase of yield point of palladium-
alloyed copper and alloys of copper micro-alloyed by
chemically active dopants is around 90%.
3.3. Steels H18N10T and H16N15M3B
To avoid samples bending under the one side plasma
irradiation, the samples treatments were carried out
alternately on the front and back sides. Total dose of
irradiation was (6-7).1017 ion/cm2. Purely hydrogen and
helium plasmas, as well as their mixture (50% H + 50%
He) were used.
Table 1. Mechanical properties of copper and alloyed copper
before and after treatment
Type of
copper
Mechanical properties
Before plasma treatment After plasma treatment
σ0.2 σB δ, % Hµ σ0.2 σB δ, % Hµ
KG/mm2 kG/mm2 kG/mm2 kG/mm2 kG/mm2 kG/mm2
MVE 4.6 22 70 48 16.9 26 29 68
MVP 6.6 20 24 57 12.9 24 23 63
MMVI 4.4 22 72 51 8.2 23 46 67
MMVS 9.2 27 22 68 17.9 28 21 73
MMVC 7.0 20 38 61 12.0 20 32 72
148
Mechanical tests of as-received and being irradiated
samples were done under the room temperature. The
values of σ0.2, σB, and δ measured under different
experimental conditions are collected in Table 2.
Table 2. Mechanical properties of steels H18N10T
and H16N15M3B
Irradiation
conditions
Steel σ0.2,
kG/mm2
σB,
kG/mm2
δ, %
Before
irradiation
H16N15M3B
H18N10T
205
207
526
604
42
63
Hydrogen
plasma
H16N15M3B
H18N10T
352
357
540
632
17
27
Helium
plasma
H16N15M3B
H18N10T
369
394
561
564
18
23
Hydrogen-
helium
plasma
H16N15M3B
H18N10T
349
336
579
617
18
23
One can see from the data of Table 2 and sample
strain diagrams (Fig. 3) that mechanical properties of
samples were essentially changed under their irradiation
with pulsed plasma streams. As the result of irradiation,
yield point of steels was increased by 1.7-1.8 times and
the ultimate strength increased as much as 10 %. The
significant variation was observed for the value of
elongation. This value was decreased by 2 times for
steel H16N15M3B and by 2.5 times for steel H18N10T.
One need to note that even the high temperature
annealing of samples dose not take off completely their
hardened state. Etching from the both sides of sample
surfaces of material layers with thickness up to 20 µm
practically do not influenced the mechanical properties
of materials gained due to their irradiation. This was the
reason to conclude that achieved changing of the
mechanical properties of thin steel samples is the result
of structure-phase state variation in the whole sample
volume.
Fig.3. Diagram of H16N15M3B steel samples
stretching for initial state (1), after irradiation (2)
and after annealing of irradiated sample under 10500
C during 10 min
3.4. Electron-microscopic investigations of
material structure
Electron-microscopic investigation of structure of
stainless steel H16N15M3B samples had shown that it
has monophase face-centered cubic lattice structure,
equiaxial granes (with mean size of about 25 µm) with
large-angle boundaries and small number of annealing
twins. The second phase precipitates are presented by
niobium carbonitrides with sizes within (0.1-1) µm and
density ≈ 1012 cm-2. The density of dislocations was ≈
5x108 cm-2 (Fig. 4, a).
a b
Fig.4. Microstructure of H16N15M3B steel
surfaces: a) – initial sample, b) – sample irradiated with
helium plasma
The irradiation result is the essential changes of
surface layer microstructure. One can see in Fig. 4, b
that irradiation leads to shattering of grains by the
blocks. The cell structure is formed with cell size of
(0.15-0.25) µm. It was shown by electron diffractometry
and dark-field electron microscopy that boundaries of
blocks, seen at the surface of irradiated samples, are the
amorphous phase inter-layers.
Step by step etching of the sample surface, and the
electron microscopic analysis, had show that the cell
structure, formed by blocks of grains, separated by the
layers of quasi-amorphous phase, extended into a depth
of up to 10 µm. With further increase of a depth this
structure was gradually transformed into the cells,
separated by dislocation network, the density of which
was decreasing with the depth and disappeared at the
depth of 25 µm (Fig. 5). At the depth of more than 25
µm the niobium carbonitrides appearance was indicated.
Their absence at the upper layers of samples is the
evidence of very high temperature of upper layers under
the plasma irradiation.
The dislocation structure and shattering of grains by
blocks, appeared under the plasma irradiation, is
qualitatively similar to ones, appeared under the high
temperature thermo-mechanical steel treatment [13].
Due to the creation of such structures one can to explain
the variation of mechanical characteristics of austenite
steels observed under their irradiation with powerful
pulsed plasma streams.
3.5. Structural steels and alloys
One of the main aim of investigations of plasma streams
influence on the properties of structural steels and
alloys, widely used in different types of tools, is
analysis of possibility to modify their surfaces to
achieve their hardening. A number of materials were
used in these experiments, such as steels H40, 12HN3A,
H12, steel 45, steel 10, ShH15, 65G and so on. The
samples of these materials were irradiated by pulsed
streams of nitrogen, hydrogen, nitrogen-helium,
nitrogen-hydrogen and others plasmas.
149
Fig.5. Cell boundaries structure changes
in the irradiated steel in dependence on the depth
from the surface: a – 1 µm, b – 5 µm, c – 25 µm.
Magnification is 12x104
Surface layer formation. Optical and electron
microscopy were used for the analysis of structure of
material cross-sections, prepared by diamond saw. As
the result of surface irradiation by plasma streams with
plasma energy loading within (10-40) J/cm2, the melt
layer was formed (Fig. 6). Its thickness was of an order
12 µm for energy load around 15 J/cm2 and increased
with energy loading increasing, achieving 30 µm for
plasma energy density of 40 J/cm2. The material
structure changes were observed even in the bulk of
steels up to the depth of an order 70 µm (the grain
structure was changed and the number of bubbles was
essentially decreased).
← layer → ____
3 µm
Fig.6. Cross-section of the H40 steel sample,
irradiated with plasma, obtained by electron
microscope
Phase-structure analysis. The results of X-ray
surface analysis of H12 steel, both for irradiated and
non-treated materials are shown in table 3. Similar
results were obtained for other grades of steels.
Table 3. Results of X-ray analysis of steel H12
# 2Θ°, CuKα
I,
relative
d (Å) Phase
1 22.00 Weak 4.04 Cr2N
2 38.20 Weak 2.3559 Fe2N
3 42.10 Weak 2.1462 Fe4N
4 43.00 Middle 2.1034 Fe2N
5 44.80 Middle 2.0230 α-Fe
6 50.30 Strong 1.8139 γ-Fe
7 73.70 Weak 1.2854 γ-Fe
8 89.80 Middle 1.0921 Fe2N
One can see in this table, that the main phase at the
surface of initial (non-treated steels) is α-Fe one.
Besides the γ-Fe and Fе3С (cementite) phases are seen.
As the result of plasma irradiation (with the dose
l.5xl018cm-2) the main phase at the surface appeared to
be γ-Fe phase with preferred orientation in the direction
[100]. The lattice spacing of γ-Fe phase for H12 steel
irradiated with plasma was a=3.6256 Å that is
essentially higher than the parameter of crystal lattice of
common γ-Fe (a=3.5264 Å). One can assume that this
increase of lattice parameter for γ-Fe was due to the
effective nitrogen implantation into the crystal lattice. It
was shown in [10] that under the similar conditions in
the stainless steel H18N10T samples, a number of
implanted nitrogen could achieve 5% of the total dose
of irradiation.
Strong blurring of the diffraction reflections from
the surface of steel 40H, observed after its irradiation
with plasma, was the evidence of initial stage of surface
layer amorphization.
Surface microhardness. The surface microhardness
variation with increasing of the irradiation dose (number
of pulses) is shown, as an example, in Fig. 7 for three
kinds of steels and different plasmas.
200
600
1000
1400
0 20 40 60 80 100
***
*
*
+
+ + + +
O
O O O
N
H , kg/mmv
2
*+
+
O
a
H V ,kg/mm2
0 20 40 60 80 100
200
600
1000
1400
1800
N
b
Fig. 7. Dependence of microhardness on the number of
plasma pulses: + - 12HN3A; * - 40H; о - VK-20.
a - nitrogen plasma, b - hydrogen-nitrogen plasma
These dependencies of microhardness on the total
dose of samples treatment, in principal, are similar to all
irradiated materials. The maximum value of
microhardness was achieved for the exposure dose of
(5-10)⋅1017cm-2 (5-10 plasma shots). The relative
increase of microhardness of irradiated samples as
compare to the initial ones was varied in the region of
(1.4 -4) times in dependence on grade of steel an its
150
preliminary treatment. The absolute values of
microhardness for different steels and alloys both for
irradiated and not irradiated ones are shown in Table 4.
One need to note that essential increase of
microhardness was observed even for preliminary
thermally quenched steels.
Table 4. Microhardness of materials processed by
nitrogen plasma with energy density (15 - 20) J/cm2
Material НV, kg/mm2
Before
processing
НV, kg/mm2
After
processing
Steel 10 200 510
Steel 45 250 628
Steel 45, quenched 370 796
40H 252 751
40H,quenched 386 794
37Q-S4 352 742
SAE 1040 264 527
65G 350 560
12HN3A 236 630
12HN3A, quenched 387 715
H12 312 510
H12, quenched 553 593
WCo20 1000 1400
The observed increase of microhardness of different
steels and alloys is the result of phase-structure
changing in the surface layers of materials due to
mainly specific thermal influence and, only partly, due
to the process of surface nitration. Confirmation of this
conclusion follows from the practically identical
dependencies of both microhardness on the number of
pulses (Fig. 7) and microhardness distribution on the
depth (Fig. 8) of irradiated materials for samples treated
with the plasma streams of different gases.
0 10 20 30 40
100
200
300
400
500
H , kg/mmv
2
l, µ m
a
0 20 40 60
900
1000
1100
1200
1300
1400
H , kg/mmv
2
l, µ m
b
Fig. 8. Dependence of microhardness of different
materials on the depth from the surface irradiated by
nitrogen (×), hydrogen-helium ( ) and hydrogen-
nitrogen (∆) plasmas: a-12HN3A; b- WCo20
The depth of surface layer with increased
microhardness was varied in dependence on plasma
stream loading and achieved (20-30) µm for plasma
energy density (30-40) J/cm2 (for instance, Fig. 8).
One need to note that for all treated materials the
depth of layers with increased microhardness (Fig.2 and
Fig. 8) was essentially higher (more than 100 times) the
mean free path of plasma ions in materials.
Effect of "long-ranging" (hardening into the high
depth) takes place under the different types of solids
irradiation, both steady state and pulse influence by
high-energy beams of ions and neutrals, and has
different physical nature. As to our case, the main
reason for changing the structure and properties of
materials under plasma irradiation is, naturally, due to
the pulsed high temperature heating of the surfaces up
to the temperatures exceeding the melt ones under the
conditions of high shock pressure by plasma streams.
Wear resistance of steels irradiated by plasma
streams. Investigations of variation of steel surface
wear resistance under plasma streams irradiation was
carried out for many grades of steels (40H, ShH15, steel
45 and so on) both non quenched and previously
thermally quenched ones. The wear and tear of samples
surfaces was measured by pin-on-disk method described
in [9]. The speed of indentor sliding was 0.8 m/s under
the normal load of 7 kG/mm2. A friction path was
varied in the range of (1-10) km. These tests followed
by analysis of linear wear of sample surfaces, measured
by profilograph-profilometer. Some results of such
measurements are shown in diagram of Fig. 9 for
friction path of 1 km.
It follows from these measurements that wear
resistance of irradiated steels was increased up to 20
times (for 40H steel, 13 times for ShH15 steel and so
on). It was increased up to 4 times even for preliminary
quenched steels. Increase of friction path up to 20 km
did not lead to essential increase of linear wear. This
means that up to this friction path the wear and tear does
not exceed the thickness of modified layer. Wear
resistance tests carried out with using some other
methods (flat-on-flat, abrasive, and cavitation methods)
have shown also essential increase of wear resistance of
steel samples irradiated by plasma.
0
2
4
6
8
10
12
14
40H 40H
(quenched)
SHH15 12HN3A
(quenched)
Steel45
initial
processed
W
ea
r
de
pt
h
[µ µµµ
m
]
Fig.9. Linear wear of different steels for initial and
irradiated samples
One need to note that plasma irradiation of samples
leads to some increase of friction coefficient of their
surfaces. This is especially true for surface irradiation
by plasma with energy density more than 20 J/cm2. In
151
the latter case there was observed increase of surface
roughness also. For energy load of about (12-15) J/cm2
the roughness parameter RA was of an order (0.4-0.7)
µm. The latter result is good enough for many
machinery tools.
Conclusions
The obtained experimental results have shown that
irradiation of materials with powerful (1-10 MW/cm2)
pulsed plasma streams influence the properties of
different metals and alloys in different way. For
instance, in the case of pure vanadium and niobium such
irradiation essentially changes the microstructure of
their surfaces, but practically does not influence their
mechanical characteristics. On the contrary, such
irradiation of some austenite steels, H16N15M3B and
H18N10T, leads to the deterioration of their mechanical
properties. The most unfavorable factor of such plasma
influence, from the point of view of their behavior in
fusion reactor, is the drastic decrease of a plasticity of
the mentioned above structural steels. Nevertheless, one
need to note that experiments, described above, were
carried out with steel samples of small thickness (200
µrn). For those samples the structure changes, that leads
to changing of the sample mechanical characteristics,
achieve the depths that are comparable with sample
thickness. In the case of massive material samples effect
of formation of structures, penetrating into the
respectively small depth, can be insufficient for
noticeable influence on the mechanical properties of
steels. On the other hand, the conditions of our
experiments were not adequate to fusion reactor
conditions. In the latter case the pulses of plasma
streams irradiating the material surfaces under current
disruptions or other instabilities should be essentially
longer that can essentially increase effects discussed
above.
There was shown the possibility of essential surface
modification of different steels and alloys under their
irradiation by powerful pulsed nitrogen (or other gases)
plasma streams. The thickness of modified layer with
increased microhardness and wear resistance was
increased with plasma energy loading and achieved 30
µm for plasma energy density of 40 J/cm2. The wear
resistance increase was as much as by 10-20 times (by
pin-on-disk method of wear tests) and depended on the
grade of material and plasma energy loading. Wear
resistance was increased by several times even for
preliminary thermally quenched steels. Due to the
effects of long-range action the possibilities of essential
hardening in depth of materials and tools are in a
prospect.
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V.I.Lapshin, I.M.Neklyudov, V.I.Tereshin
61108 Kharkov, Ukraine
Conclusions
References
|
| id | nasplib_isofts_kiev_ua-123456789-78556 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1562-6016 |
| language | English |
| last_indexed | 2025-12-07T16:18:11Z |
| publishDate | 2000 |
| publisher | Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| record_format | dspace |
| spelling | Lapshin, V.I. Neklyudov, I.M. Tereshin, V.I. 2015-03-18T19:13:49Z 2015-03-18T19:13:49Z 2000 Influence of the plasma stream irradiation on the surface modification, structure and properties of materials / V.I. Lapshin, I.M. Neklyudov, V.I. Tereshin // Вопросы атомной науки и техники. — 2000. — № 6. — С. 146-151. — Бібліогр.: 13 назв. — англ. 1562-6016 https://nasplib.isofts.kiev.ua/handle/123456789/78556 533.9 en Національний науковий центр «Харківський фізико-технічний інститут» НАН України Вопросы атомной науки и техники Low temperature plasma and plasma technologies Influence of the plasma stream irradiation on the surface modification, structure and properties of materials Article published earlier |
| spellingShingle | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials Lapshin, V.I. Neklyudov, I.M. Tereshin, V.I. Low temperature plasma and plasma technologies |
| title | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials |
| title_full | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials |
| title_fullStr | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials |
| title_full_unstemmed | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials |
| title_short | Influence of the plasma stream irradiation on the surface modification, structure and properties of materials |
| title_sort | influence of the plasma stream irradiation on the surface modification, structure and properties of materials |
| topic | Low temperature plasma and plasma technologies |
| topic_facet | Low temperature plasma and plasma technologies |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/78556 |
| work_keys_str_mv | AT lapshinvi influenceoftheplasmastreamirradiationonthesurfacemodificationstructureandpropertiesofmaterials AT neklyudovim influenceoftheplasmastreamirradiationonthesurfacemodificationstructureandpropertiesofmaterials AT tereshinvi influenceoftheplasmastreamirradiationonthesurfacemodificationstructureandpropertiesofmaterials |