Nanocrystalline vacuum-arc nitride coatings
possess the totality of unique structural states and
properties (high hardness, wear resistance, oxidation
stability, etc.). The coatings of the Mo-N system
show a high hardness and low solubility of
nonferromagnetic materials, thereby attracting great
interest in their industrial use. Unfortunately, at
present there is an apparent lack of information on the
regularities of phase-structural state formation in the
Mo-N system.
When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/3535

Andreev, A.A.

Fil’chikov, V.E.

Grigoriev, S.N.

Sobol, O.V.

Stolbovoy, V.A.

Volosova, M.V.

Electronic Sumy State University Institutional Repository

Proceedings of the International Conference  Nanomaterials: Applications and Properties VOL. 2 NO 2, 02FNC19(3PP) (2013)   2304-1862/2013/2(2)02FNC19(3) 02FNC19-1  2013 Sumy State University Effect of Preparation Conditions in the Pressure Range of Atmospheric Nitrogen (2 ... 50) 10-4 Torr on the Structural and Phase State of the Vacuum-Arc Coatings of Mo-N  O.V. Sobol’1,*, A.A. Andreev2,†, V.A. Stolbovoy1, V.E. Fil’chikov1 S.N. Grigoriev3‡, M.V. Volosova3  1 National Technical University "Kharkiv Polytechnical Institute",21, Frunze Str., 61002 Kharkiv, Ukraine, 2 National Science Center “Kharkiv Institute of Physics & Technology”, 1, Akademicheskaya Str., 61108 Kharkiv, Ukraine 3 Moscow State Technological University "Stankin", 3a, Vadkovskij Line, 127055 Moscow, Russia  (Received 10 June 2013; published online 20 August 2013)  This work deals with the impact of the reactive atmosphere (N2) pressure and bias potential values on the phase-structural state of the coatings being formed. It has been found that at a low bias potential Ub  (0 … -40) V, and with pressure increase from 210-4 up to 510-3 Torr, phase formation takes place in the following sequence: supersaturated solid solution of nitrogen in the bcc lattice of Mo (Mo(N))  -Мо2N  -MoN phases with the NaCl-type lattice and with different degrees of octahedral interstitial site occupation with nitrogen. At Ub  (-40 … -100) V, the sequence of phase-structural states is as follows: Мо (Мо(N))  -Мо2N  -MoN (hexagonal lattice)  -МоN. At highest Ub (with a strong radiation factor ef-fect) values ranging between -150 V and -200 V and with pressure increase, the composition changes to Мо (Мо(N))  -Мо2N  -Мо2N  -MoN  -МоN.  Keywords: Vacuum-Arc coatings, Nanostructured, Mo-N system, Bias potential, X-ray diffraction.   PACS numbers: 81.07.Bc, 61.05.cp, 61.46.Hk, 81.15.Jj.                                                          *sool@kpi.kharkov.ua †aandreev@kipt.kharkov.ua ‡science@stankin.ru 1. INTRODUCTION  Nanocrystalline vacuum-arc nitride coatings possess the totality of unique structural states and properties (high hardness, wear resistance, oxidation stability, etc.) [1]. The coatings of the Mo-N system show a high hardness and low solubility of nonferromagnetic materials, thereby attracting great interest in their industrial use [2]. Unfortunately, at present there is an apparent lack of information on the regularities of phase-structural state formation in the Mo-N system. Mo-N coatings can be deposited by various techniques such as ion beam deposition stimulated, dc and r.f. magnetron sputtering, arc PVD-technique and ion implantation of nitrogen into the film-coated pure molybdenum. Among these techniques arc PVD is one of the most versatile processes due to the high degree of ionization and good adhesion properties of the coatings. Formation phases in Mo-N coatings is strongly dependent on process parameters. Currently there is a lack of information in the literature concerning the systematic investigation of relations between the parameters and deposition properties of the coatings Mo-N. For this system, characterized by two stable compounds: -MoN and Mo2N. Recently, the compound exists in two versions: the low-temperature – () and high (). The transformation    is a martensitic. Phase -MoN has a hexagonal lattice with parameters a  0.572 nm and c  0.560 nm (Fig. 1a). The homogeneity region Mo2N is (27.5 ... 30.1) at. N. Phase Mo2N has an fcc lattice with a structural type of NaCl (a  0.4137 nm at 27.5 atm. N, Fig. 1b). -Mo2N – an ordered tetragonal modification -Mo2N pseudo cell face centered tetragonal (a  0.4200 nm, c  0.4005 nm, Fig. 1c) [3].     a   b    c  Fig. 1 – Crystal structure of -MoN (a), -Mo2N (b) and -Mo2N (c)  O.V. SOBOL, , A.A. ANDREEV, V.A. STOLBOVOY, V.E. FIL’CHIKOV, ET AL. Proc. NAP 2, 02FNC19 (2013)   02FNC19-2  Also in the case of vacuum-plasma condensates in analogy to that described in [4] for coatings in the system Mo-N to form a nanostructured state can ex-pect the appearance of the crystallite space group P6/mmm, which for the nitrides was recorded in the system TaN. MoN phase with a hexagonal lattice of the space group P6/mmm, denoted by analogy with the phase of ε-TaN [5], as -MoN phase with a hex-agonal crystal structure shown in Fig. 2.    Fig. 2 – The crystal structure of TaN: a – the unit cell; b – its vertical section on AB [5]  An attempt to systematize the structural and phase state was first made in [6] for the system Mo-N at relatively high pressure reactive atmosphere (more than 210-3 Torr). However, studies have shown the mechanical properties of the vacuum-arc coating system Mo-N [7] to the highest mechanical properties of the system can be expected at lower pressures. Moreover, this pressure provides a tech-nological process, as proceeds at a net formation conditions. In this context, this paper attempts to summarize accumulated in this area by the authors of data for relatively low pressure range form (210-4-510-3) Torr.  It should be noted that the identification phase state compared with X-ray diffraction data given in [6] shows the possibility of using all of the phase states, and at a lower pressure, but increased inten-sity because of the use of the process nitride for-mation additional magnetic block [8], increases ioni-zation, and by improving the process of forming by supplying high-voltage pulse to the substrate bias potential. If we consider the sub-bands in the pres-sure range studied (210-4-510-3) Torr, in accordance with the characteristic of phase-structural state can be distinguished interval РN  (2 … 6)10-4 Torr. This interval is characterized by the formation of single-phase structural state of Mo phase with a bcc lattice. Constant flow of negative bias potential leads to the appearance of the texture of growth (110) (Fig. 3a). In the case of low value of the bias potential (-40 V) at a pressure of 810-4 Torr instead supersatu-rated on nitrogen atoms of molybdenum is formed -Mo2N (structural type NaCl) with a relatively low lattice period and texture (311), see Fig. 3b.  30 40 50 60 70 80 9002000400060008000100001200014000(220)Mo  I, arb. un.2, degr(110)Moa  30 40 50 60 70 80 900100020003000400050006000Mo2NMo2NMo2NMo2NI, arb. un.2, degr  b  Fig. 3 – X-ray diffraction spectrum from the coating produced by PN  810-4 Torr and Ub  -200 V (a) and spectrum from the Mo-N coatings obtained at Ub  -40 V and a nitrogen pressure of about 710-4 Torr at length storage at 10 seconds (radiation Cu-K, identification of the phase -Mo2N) (b)  Feeding of a higher amount of negative bias potential results in a phase with a low nitrogen content, even at relatively high pressure PN  210-3 Torr. In the two-phase coating stabilized condition in which, in addition to the solid solution of nitrogen in the bcc molybdenum nitride formed -Mo  N with very poor texture (311). The lattice periods of nitrides are close to the value of 0.416 nm. Apparently, this value corresponds to the peri-od of the stoichiometric composition of the phase Mo2N with NaCl-type lattice in which nitrogen occupies half of the possible places to fill the octahedral interstices. As the pressure decreases the value of a work environment macrodeformation from -1.92 at a pressure of 810-4 Torr (-40 V) up 0.53 at PN  210-3 Torr. Such a reduction in the stress-strain state with increasing pressure may be due to a significant loss of energy film-forming particles at high pressure. In the latter case, a phase according Mo «a-sin2»-method developed tensile strain value 0.28 (cor-responding to step macrostresses tension value 0.67 GPa). For coatings produced at a relatively high pressure ni-trogen PN  0.2 Pa, and a relatively small Ub  -40 V and -70 V at diffraction spectra also revealed the texture (311) (see Fig. 5), and the values were large periods and amounted to 0.4184 nm and 0.4189 nm, respectively. The value of macrodeformation was -0.97 for Ub  -40 V and -2.05 for Ub  -70 V. In this connection identified in the characteristic val-ues of two frames (close to 0,416 nm and 0,419 nm, re-spectively, Fig. 4) can be classified into two types of order-ing in the lattice structural type NaCl. In the first case corresponds to the ordering of the stoichiometry of -Mo2N, while the second - MoN with fcc metal sublattice. At higher pressure PN  (2 ... 6)10-3 Torr and Ub  (-150 ... -200) V occurs in the formation of ε-MoN phase  EFFECT OF PREPARATION CONDITIONS IN THE PRESSURE RANGE… Proc. NAP 2, 02FNC19 (2013)   02FNC19-3 with a hexagonal crystal structure (Fig. 5).  0,0 0,1 0,2 0,3 0,4 0,5 0,64,154,164,174,184,194,204,214,224,23423  a, 10-1, nmsin21  Fig. 4 – «a-sin2»-graphs for determining the macrodeformation in coatings Mo-N system, obtained at no bias potential supply (when "floating" potential) and a pressure PN  710-4 Torr (1), when the PN  1,310-3 Torr and Ub  -40 V(2), Ub  -70 V (3) and Ub  -200 V (4)  30 40 50 60 70 80400080001200016000(112)-MoN(220)-MoN(211)-MoN(300)-MoN(111)-MoN(101)-MoN(110)-MoN2  I, arb. un2degr1  Fig. 5 – X-ray diffraction spectra from the coating Mo-N system, obtained by pressure at PN  3*10-3 Torr, Ub  -200 V and and high-voltage pulse with an amplitude of stimulation: 1 – 1.2 kV, 2 – 2 kV  Thus, a generalized phase diagram coordinates P(N)–Ub for range pressures PN  (7 ... 50)10-4 Torr and Ub  (0 ...  200) V has the form shown in Fig. 6.    Fig. 6 – The phase diagram for vacuum plasma coatingMo-N system in the coordinates P(N)-Ub  It is seen that the vacuum plasma nanostructured coating of the Mo-N system with an increase in bias potential observed with the formation of phases disadvantage nitrogen atoms and a non-cubic crystal lattice type.     REFERENCES  1. N.A. Azarenkov, O.V. Sobol’, V.M. Beresnev, A.D. Pogrebnyak, S.V. Litovchenko, O.N. Ivanov. Materi-als science of nonequilibrium state of modified surface (Sumy, Sumy State University, 2012). 2. M.K. Kazmanli, M. Urgen, A.F. Cakir, Surf. Coat. Technol. 167, 77 (2003). 3.  F. Schank Structure of Binary Alloys (Moscow: Metallur-gy: 1973). 4.  S.I. Sadovnicov, A.A. Rempel, Solid State Physics 51 No11, 2237 (2009). 5. G.V. Samsonov, Nitrides (Kijev: Naukova Dumka: 1969). 6.  M.K. Kazmanli, M. Urgen, A.F. Cakir, Surf. Coat. Tech-nol. 167, 77 (2003). 7. O.V. Sobol, A.A. Andreev, V.A. Stolbovoi, V.E. Fil`chikov Technical Physics Letters 38 No2, 168 (2012). 8. A.A. Andreev,  S.N. Grigoriev, O.V. Sobol, V.F. Gorban, M.A. Volosova, V.A. Stolbovoy, I.V. Serduk, Hardening technology and coatings 85 No1, 14 (2012). 

Effect of Preparation Conditions in the Pressure Range of Atmospheric Nitrogen (2 ... 50) 10-4 Torr on the Structural and Phase State of the Vacuum-Arc Coatings of Mo-N

SocioEconomic Challenges Journal (Sumy State University)

Proceedings of the International Conference  
Nanomaterials: Applications and Properties 
VOL. 2 NO 2, 02FNC19(3PP) (2013) 
 
 
2304-1862/2013/2(2)02FNC19(3) 02FNC19-1  2013 Sumy State University 
Effect of Preparation Conditions in the Pressure Range of Atmospheric Nitrogen (2 ... 50) 10-4 
Torr on the Structural and Phase State of the Vacuum-Arc Coatings of Mo-N 
 
O.V. Sobol’1,*, A.A. Andreev2,†, V.A. Stolbovoy1, V.E. Fil’chikov1 S.N. Grigoriev3‡, M.V. Volosova3 
 
1 National Technical University "Kharkiv Polytechnical Institute",21, Frunze Str., 61002 Kharkiv, Ukraine, 
2 National Science Center “Kharkiv Institute of Physics & Technology”, 1, Akademicheskaya Str., 61108 Kharkiv, 
Ukraine 
3 Moscow State Technological University "Stankin", 3a, Vadkovskij Line, 127055 Moscow, Russia 
 
(Received 10 June 2013; published online 20 August 2013) 
 
This work deals with the impact of the reactive atmosphere (N2) pressure and bias potential values on 
the phase-structural state of the coatings being formed. It has been found that at a low bias potential 
Ub  (0 … -40) V, and with pressure increase from 210-4 up to 510-3 Torr, phase formation takes place in 
the following sequence: supersaturated solid solution of nitrogen in the bcc lattice of Mo (Mo(N))  -
Мо2N  -MoN phases with the NaCl-type lattice and with different degrees of octahedral interstitial site 
occupation with nitrogen. At Ub  (-40 … -100) V, the sequence of phase-structural states is as follows: Мо 
(Мо(N))  -Мо2N  -MoN (hexagonal lattice)  -МоN. At highest Ub (with a strong radiation factor ef-
fect) values ranging between -150 V and -200 V and with pressure increase, the composition changes to Мо 
(Мо(N))  -Мо2N  -Мо2N  -MoN  -МоN. 
 
Keywords: Vacuum-Arc coatings, Nanostructured, Mo-N system, Bias potential, X-ray diffraction. 
 
 PACS numbers: 81.07.Bc, 61.05.cp, 61.46.Hk, 
81.15.Jj. 
 
                                                        
*sool@kpi.kharkov.ua 
†aandreev@kipt.kharkov.ua 
‡science@stankin.ru 
1. INTRODUCTION 
 
Nanocrystalline vacuum-arc nitride coatings 
possess the totality of unique structural states and 
properties (high hardness, wear resistance, oxidation 
stability, etc.) [1]. The coatings of the Mo-N system 
show a high hardness and low solubility of 
nonferromagnetic materials, thereby attracting great 
interest in their industrial use [2]. Unfortunately, at 
present there is an apparent lack of information on the 
regularities of phase-structural state formation in the 
Mo-N system. 
Mo-N coatings can be deposited by various 
techniques such as ion beam deposition stimulated, dc 
and r.f. magnetron sputtering, arc PVD-technique and 
ion implantation of nitrogen into the film-coated pure 
molybdenum. Among these techniques arc PVD is one 
of the most versatile processes due to the high degree of 
ionization and good adhesion properties of the coatings. 
Formation phases in Mo-N coatings is strongly 
dependent on process parameters. Currently there is a 
lack of information in the literature concerning the 
systematic investigation of relations between the 
parameters and deposition properties of the coatings 
Mo-N. For this system, characterized by two stable 
compounds: -MoN and Mo2N. Recently, the compound 
exists in two versions: the low-temperature – () and 
high (). The transformation    is a martensitic. 
Phase -MoN has a hexagonal lattice with parameters 
a  0.572 nm and c  0.560 nm (Fig. 1a). The 
homogeneity region Mo2N is (27.5 ... 30.1) at. N. 
Phase Mo2N has an fcc lattice with a structural type of 
NaCl (a  0.4137 nm at 27.5 atm. N, Fig. 1b). -
Mo2N – an ordered tetragonal modification -Mo2N 
pseudo cell face centered tetragonal (a  0.4200 nm, 
c  0.4005 nm, Fig. 1c) [3]. 
 
  
 
a   b 
 
 
 
c 
 
Fig. 1 – Crystal structure of -MoN (a), -Mo2N (b) and -
Mo2N (c) 
 O.V. SOBOL, , A.A. ANDREEV, V.A. STOLBOVOY, V.E. FIL’CHIKOV, ET AL. Proc. NAP 2, 02FNC19 (2013) 
 
 
02FNC19-2 
 
Also in the case of vacuum-plasma condensates in 
analogy to that described in [4] for coatings in the 
system Mo-N to form a nanostructured state can ex-
pect the appearance of the crystallite space group 
P6/mmm, which for the nitrides was recorded in the 
system TaN. MoN phase with a hexagonal lattice of 
the space group P6/mmm, denoted by analogy with 
the phase of ε-TaN [5], as -MoN phase with a hex-
agonal crystal structure shown in Fig. 2. 
 
 
 
Fig. 2 – The crystal structure of TaN: a – the unit cell; b –
 its vertical section on AB [5] 
 
An attempt to systematize the structural and 
phase state was first made in [6] for the system Mo-
N at relatively high pressure reactive atmosphere 
(more than 210-3 Torr). However, studies have 
shown the mechanical properties of the vacuum-arc 
coating system Mo-N [7] to the highest mechanical 
properties of the system can be expected at lower 
pressures. Moreover, this pressure provides a tech-
nological process, as proceeds at a net formation 
conditions. In this context, this paper attempts to 
summarize accumulated in this area by the authors 
of data for relatively low pressure range form (210-4-
510-3) Torr.  
It should be noted that the identification phase 
state compared with X-ray diffraction data given in 
[6] shows the possibility of using all of the phase 
states, and at a lower pressure, but increased inten-
sity because of the use of the process nitride for-
mation additional magnetic block [8], increases ioni-
zation, and by improving the process of forming by 
supplying high-voltage pulse to the substrate bias 
potential. If we consider the sub-bands in the pres-
sure range studied (210-4-510-3) Torr, in accordance 
with the characteristic of phase-structural state can 
be distinguished interval РN  (2 … 6)10-4 Torr. This 
interval is characterized by the formation of single-
phase structural state of Mo phase with a bcc lattice. 
Constant flow of negative bias potential leads to the 
appearance of the texture of growth (110) (Fig. 3a). 
In the case of low value of the bias potential (-
40 V) at a pressure of 810-4 Torr instead supersatu-
rated on nitrogen atoms of molybdenum is formed -
Mo2N (structural type NaCl) with a relatively low 
lattice period and texture (311), see Fig. 3b. 
 
30 40 50 60 70 80 90
0
2000
4000
6000
8000
10000
12000
14000
(2
2
0
)M
o
 
 
I,
 a
rb
. 
u
n
.
2, degr
(1
1
0
)M
o
a
 
 
30 40 50 60 70 80 90
0
1000
2000
3000
4000
5000
6000
Mo2N





M
o
2
N





M
o
2
N





M
o
2
N
I,
 a
rb
. 
u
n
.
2, degr
 
 
b
 
 
Fig. 3 – X-ray diffraction spectrum from the coating produced 
by PN  810-4 Torr and Ub  -200 V (a) and spectrum from the 
Mo-N coatings obtained at Ub  -40 V and a nitrogen pressure 
of about 710-4 Torr at length storage at 10 seconds (radiation 
Cu-K, identification of the phase -Mo2N) (b) 
 
Feeding of a higher amount of negative bias potential 
results in a phase with a low nitrogen content, even at 
relatively high pressure PN  210-3 Torr. In the two-phase 
coating stabilized condition in which, in addition to the 
solid solution of nitrogen in the bcc molybdenum nitride 
formed -Mo  N with very poor texture (311). 
The lattice periods of nitrides are close to the value of 
0.416 nm. Apparently, this value corresponds to the peri-
od of the stoichiometric composition of the phase Mo2N 
with NaCl-type lattice in which nitrogen occupies half of 
the possible places to fill the octahedral interstices. As the 
pressure decreases the value of a work environment 
macrodeformation from -1.92 at a pressure of 810-4 Torr 
(-40 V) up 0.53 at PN  210-3 Torr. Such a reduction in 
the stress-strain state with increasing pressure may be 
due to a significant loss of energy film-forming particles at 
high pressure. In the latter case, a phase according Mo «a-
sin2»-method developed tensile strain value 0.28 (cor-
responding to step macrostresses tension value 0.67 GPa). 
For coatings produced at a relatively high pressure ni-
trogen PN  0.2 Pa, and a relatively small Ub  -40 V and -
70 V at diffraction spectra also revealed the texture (311) 
(see Fig. 5), and the values were large periods and 
amounted to 0.4184 nm and 0.4189 nm, respectively. The 
value of macrodeformation was -0.97 for Ub  -40 V and -
2.05 for Ub  -70 V. 
In this connection identified in the characteristic val-
ues of two frames (close to 0,416 nm and 0,419 nm, re-
spectively, Fig. 4) can be classified into two types of order-
ing in the lattice structural type NaCl. In the first case 
corresponds to the ordering of the stoichiometry of -
Mo2N, while the second - MoN with fcc metal sublattice. 
At higher pressure PN  (2 ... 6)10-3 Torr and Ub  (-
150 ... -200) V occurs in the formation of ε-MoN phase 
 EFFECT OF PREPARATION CONDITIONS IN THE PRESSURE RANGE… Proc. NAP 2, 02FNC19 (2013) 
 
 
02FNC19-3 
with a hexagonal crystal structure (Fig. 5). 
 
0,0 0,1 0,2 0,3 0,4 0,5 0,6
4,15
4,16
4,17
4,18
4,19
4,20
4,21
4,22
4,23
4
2
3
 
 
a,
 1
0
-1
, 
n
m
sin2
1
 
 
Fig. 4 – «a-sin2»-graphs for determining the macrodeformation 
in coatings Mo-N system, obtained at no bias potential supply 
(when "floating" potential) and a pressure PN  710-4 Torr (1), 
when the PN  1,310-3 Torr and Ub  -40 V(2), Ub  -70 V (3) and 
Ub  -200 V (4) 
 
30 40 50 60 70 80
4000
8000
12000
16000
(1
1
2
)
-M
o
N
(2
2
0
)
-M
o
N
(2
1
1
)
-M
o
N
(3
0
0
)
-M
o
N
(1
1
1
)
-M
o
N
(1
0
1
)
-M
o
N
(1
1
0
)
-M
o
N
2
 
 
I,
 a
rb
. 
u
n
2degr
1
 
 
Fig. 5 – X-ray diffraction spectra from the coating Mo-N system, 
obtained by pressure at PN  3*10-3 Torr, Ub  -200 V and and 
high-voltage pulse with an amplitude of stimulation: 1 – 1.2 kV, 
2 – 2 kV 
 
Thus, a generalized phase diagram coordinates 
P(N)–Ub for range pressures PN  (7 ... 50)10-4 Torr and 
Ub  (0 ...  200) V has the form shown in Fig. 6. 
 
 
 
Fig. 6 – The phase diagram for vacuum plasma coatingMo-N 
system in the coordinates P(N)-Ub 
 
It is seen that the vacuum plasma nanostructured 
coating of the Mo-N system with an increase in bias 
potential observed with the formation of phases 
disadvantage nitrogen atoms and a non-cubic crystal 
lattice type. 
 
 
 
 
REFERENCES 
 
1. N.A. Azarenkov, O.V. Sobol’, V.M. Beresnev, 
A.D. Pogrebnyak, S.V. Litovchenko, O.N. Ivanov. Materi-
als science of nonequilibrium state of modified surface 
(Sumy, Sumy State University, 2012). 
2. M.K. Kazmanli, M. Urgen, A.F. Cakir, Surf. Coat. Technol. 
167, 77 (2003). 
3.  F. Schank Structure of Binary Alloys (Moscow: Metallur-
gy: 1973). 
4.  S.I. Sadovnicov, A.A. Rempel, Solid State Physics 51 
No11, 2237 (2009). 
5. G.V. Samsonov, Nitrides (Kijev: Naukova Dumka: 1969). 
6.  M.K. Kazmanli, M. Urgen, A.F. Cakir, Surf. Coat. Tech-
nol. 167, 77 (2003). 
7. O.V. Sobol, A.A. Andreev, V.A. Stolbovoi, V.E. Fil`chikov 
Technical Physics Letters 38 No2, 168 (2012). 
8. A.A. Andreev,  S.N. Grigoriev, O.V. Sobol, V.F. Gorban, 
M.A. Volosova, V.A. Stolbovoy, I.V. Serduk, Hardening 
technology and coatings 85 No1, 14 (2012). 


English

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Effect of Preparation Conditions in the Pressure Range of Atmospheric Nitrogen (2 ... 50) 10-4 Torr on the Structural and Phase State of the Vacuum-Arc Coatings of Mo-N

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