Gas-Phase Synthesis of Film Structures of Ni—N System
As shown, the magnetron sputtering is effective for the synthesis of various nanostructured phases of nickel nitride (solid solution of nitrogen in nickel, Ni₄N, Ni₃N, and Ni₂N). The regularities of formation of globular or nanocolumnar film structures are determined, depending on the concentration...
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Інститут металофізики ім. Г.В. Курдюмова НАН України
2015
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irk-123456789-1118922017-01-16T03:03:16Z Gas-Phase Synthesis of Film Structures of Ni—N System Shalaev, R.V. Металлические поверхности и плёнки As shown, the magnetron sputtering is effective for the synthesis of various nanostructured phases of nickel nitride (solid solution of nitrogen in nickel, Ni₄N, Ni₃N, and Ni₂N). The regularities of formation of globular or nanocolumnar film structures are determined, depending on the concentration of nitrogen in the buffer gas. Показано, що магнетронне розпорошення є ефективним для синтези різноманітних наноструктурних фаз нітриду ніклю (твердий розчин Нітроґену у ніклі, Ni₄N, Ni₃N та Ni₂N). Визначено закономірності утворення наноколонарних або ґлобулярних плівкових структур системи Ni—N залежно від концентрації азоту у буферному газі. Показано, что магнетронное распыление эффективно для синтеза различных наноструктурных фаз нитрида никеля (твёрдый раствор азота в никеле, Ni₄N, Ni₃N и Ni₂N). Определены закономерности образования наноколонарных или глобулярных плёночных структур системы Ni—N в зависимости от концентрации азота в буферном газе. 2015 Article Gas-Phase Synthesis of Film Structures of Ni—N System / R. V. Shalaev // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 509-519. — Бібліогр.: 12 назв. — рос. 1024-1809 PACS: 52.40.Hf, 61.05.cp, 68.35.Dv, 68.37.Ps, 68.55.Nq, 81.07.Bc, 81.15.Gh http://dspace.nbuv.gov.ua/handle/123456789/111892 en Металлофизика и новейшие технологии Інститут металофізики ім. Г.В. Курдюмова НАН України |
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Металлические поверхности и плёнки Металлические поверхности и плёнки |
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Металлические поверхности и плёнки Металлические поверхности и плёнки Shalaev, R.V. Gas-Phase Synthesis of Film Structures of Ni—N System Металлофизика и новейшие технологии |
| description |
As shown, the magnetron sputtering is effective for the synthesis of various nanostructured phases of nickel nitride (solid solution of nitrogen in nickel, Ni₄N, Ni₃N, and Ni₂N). The regularities of formation of globular or nanocolumnar film structures are determined, depending on the concentration of nitrogen in the buffer gas. |
| format |
Article |
| author |
Shalaev, R.V. |
| author_facet |
Shalaev, R.V. |
| author_sort |
Shalaev, R.V. |
| title |
Gas-Phase Synthesis of Film Structures of Ni—N System |
| title_short |
Gas-Phase Synthesis of Film Structures of Ni—N System |
| title_full |
Gas-Phase Synthesis of Film Structures of Ni—N System |
| title_fullStr |
Gas-Phase Synthesis of Film Structures of Ni—N System |
| title_full_unstemmed |
Gas-Phase Synthesis of Film Structures of Ni—N System |
| title_sort |
gas-phase synthesis of film structures of ni—n system |
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Інститут металофізики ім. Г.В. Курдюмова НАН України |
| publishDate |
2015 |
| topic_facet |
Металлические поверхности и плёнки |
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http://dspace.nbuv.gov.ua/handle/123456789/111892 |
| citation_txt |
Gas-Phase Synthesis of Film Structures of Ni—N System / R. V. Shalaev // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 509-519. — Бібліогр.: 12 назв. — рос. |
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Металлофизика и новейшие технологии |
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AT shalaevrv gasphasesynthesisoffilmstructuresofninsystem |
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2025-07-08T02:51:36Z |
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2025-07-08T02:51:36Z |
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1837045485785841664 |
| fulltext |
509
PACS numbers:52.40.Hf, 61.05.cp,68.35.Dv,68.37.Ps,68.55.Nq,81.07.Bc, 81.15.Gh
Gas-Phase Synthesis of Film Structures of Ni—N System
R. V. Shalaev
O. O. Galkin Donetsk Physicotechnical Institute, N.A.S. of Ukraine,
72 Rosa Luksemburg Str.,
83114 Donetsk, Ukraine
As shown, the magnetron sputtering is effective for the synthesis of various
nanostructured phases of nickel nitride (solid solution of nitrogen in nickel,
Ni4N, Ni3N, and Ni2N). The regularities of formation of globular or nanoco-
lumnar film structures are determined, depending on the concentration of
nitrogen in the buffer gas.
Показано, що магнетронне розпорошення є ефективним для синтези різ-
номанітних наноструктурних фаз нітриду ніклю (твердий розчин Нітро-
ґену у ніклі, Ni4N, Ni3N та Ni2N). Визначено закономірності утворення
наноколонарних або ґлобулярних плівкових структур системи Ni—N за-
лежно від концентрації азоту у буферному газі.
Показано, что магнетронное распыление эффективно для синтеза различ-
ных наноструктурных фаз нитрида никеля (твёрдый раствор азота в ни-
келе, Ni4N, Ni3N и Ni2N). Определены закономерности образования нано-
колонарных или глобулярных плёночных структур системы Ni—N в зави-
симости от концентрации азота в буферном газе.
Key words: nickel nitride, nanocolumnars, globules, magnetron sputtering,
atomic force microscopy.
(Received January 14, 2015)
1. INTRODUCTION
Last years, nitrides of transition metals, such as Fe, Co, Ni, attract
major interest of the scientists because of their unique physical prop-
erties–mechanical, optical, electrical, and magnetic ones. These ma-
terials have a high potential of practical application in such fields of a
science and technique, as semiconductor technics, magnetooptics, sen-
Металлофиз. новейшие технол. / Metallofiz. Noveishie Tekhnol.
2015, т. 37, № 4, сс. 509—519
Оттиски доступны непосредственно от издателя
Фотокопирование разрешено только
в соответствии с лицензией
2015 ИМФ (Институт металлофизики
им. Г. В. Курдюмова НАН Украины)
Напечатано в Украине.
510 R. V. SHALAEV
sor devices, and magnetic devices of storing of information [1, 2]. As
known, a nitrogen introduction in structure of transition metals al-
lows to actively control their properties, in particular, magnetic ones
(coercivity, magnetic moment) [3]. Unfortunately, nitrides of such
metals as Ni and Co are frequently metastable and not all their phases
are uniquely identified, despite the complicated phase diagram. First,
it falls into nickel: nickel nitrides, in comparison with other nitrides of
metals, are insufficiently studied, their properties, and methods of
production are not well observed, until now the confirmed data for
some phases of Ni—N are absent.
At the same time, numerous experiments on synthesis of film nickel
nitrides have shown that the composition of films is an intermixture of
various nitride phases up to the pure nickel [4, 5], though there is an
obvious dependence on the nitrogen contents: the higher nitrogen con-
tent–the more nitrogen saturated nitride phases enter into the com-
position of film. During the gradual increase of the nitrogen content in
a material, pure nickel with the f.c.c. lattice sequentially transfers in
nickel nitride Ni4N (f.c.c.), further in Ni3N (h.c.p.) and at the maxi-
mum concentrations of nitrogen in Ni2N (body-centred tetragonal–
b.c.t.) [6]. All these phases under certain conditions exist in the mate-
rial simultaneously.
Nickel nitrides are usually produced by such methods as reactive
spraying and ion-beam implantation. Implantation of ions sometimes
is more preferable for the precise stoichiometry control and production
of various unstable phases of nickel nitride [7]; however, it usually
demands rather complicated procedures. Reactive magnetron spraying
is also one of the popular methods of metals nitrides films production.
For instance, Dorman and co-authors [5] produced nickel nitrides
(Ni4N, Ni3N and Ni2N) by the direct current reactive spraying at vari-
ous fractional pressure of nitrogen. Phase Ni3N can be produced at
nickel heating in a stream of ammonia NH3 at 781 K [8]; however, it is
not stoichiometrically pure. Ni3N is also produced using high pressure
(20 GPa) and temperatures (2000 K) from the intermixture of nickel
and sodium nitride NaN3 [9]. Besides, in the literature, there are men-
tions of such phases as Ni3N2 and NiN6 [10], which were not confirmed
in later works.
Thus, frequently contradictory information concerning diversiform
phases of nickel nitride and insufficiently studied behaviour of Ni—N
(in particular, in the form nanostructured films) demand the addition-
al investigations devoted to production of various phases of Ni—N sys-
tem.
In the present work, a number of phases of nickel nitride (Ni with a
nitrogen solid solution, Ni4N, Ni3N, and Ni2N) are synthesized by a
method of magnetron sprayings of a nickel target in an argon—nitric
intermixture, which is confirmed by the X-ray diffraction studies.
GAS-PHASE SYNTHESIS OF FILM STRUCTURES OF Ni—N SYSTEM 511
2. EXPERIMENT AND DISCUSSION
Process of magnetron sputtering allows to precipitate films of a wide
spectrum of materials with a variation of a thickness from tens nano-
metres to several micrometres. Magnetron spraying falls into the
methods of spraying of materials with the ionic bombing of a surface.
In the present work, films of nickel and nickel nitride are produced on
the VUP-5M installation with a standard magnetron direct current at-
tachment. Plasma is produced by means of a magnetron of a planar de-
sign with a flat cathode and an orificed anode. Power of discharge of
the magnetron did not exceed 20 W, a discharge current–40 mA. The
nickel (very high purity grade) target of 40 mm in diameter is fixed on
the cathode of the magnetron and sputtered on substrates from a cover
or quartz glass at the temperature of 240С in Ar atmosphere with
adding from 2% to 70% N2. Gas mixture is preliminary prepared in
external gas system and pumps down in vacuum volume through the
piezoelectric inlet valve. Pressure of gas in the chamber is controlled
by devices of the vacuum post and comprises 24 Pa. Substructures are
preliminary cleaned in an intermixture of solvents and their vapours.
The distance from the cathode to the substructure is 2.5 cm. Time of
growth of films was 20 minutes; the thickness thus varied from 0.2 to
0.5 micrometres (measurements were performed using MII-4 interfer-
ence microscope).
The X-ray diffraction analysis of the produced specimens is per-
formed using of DRON-3 diffractometer in CoK radiation, and also
using Panalytical X’Pert MPD 1 Bragg—Brentano diffractometer
equipped with the scintillation counter, in CuK radiation. Morpholo-
gy of a surface of films and their thickness is analysed by field emissive
scanning electron microscopy using JEOL JSM-6490 LV device, and an
atomic force microscopy (AFM) with the help of the Ntegra Aura probe
nanostation. Magnetic properties of the films are studied using induc-
tive-frequency installation [11]. X-ray diffraction patterns of Ni—N
system films produced with adding of 0—8 vol.% of nitrogen in a
growth atmosphere at CuK radiation are presented in Fig. 1. Identifi-
cation of the specified structure has been performed and the infor-
mation concerning phase composition of films is obtained (see Table 1).
The analysis of X-ray spectra of the specimens produced in nitrogen-
free atmosphere and at insignificant concentrations of nitrogen (less
than 2%), has shown the presence of lines, close to lines of the f.c.c.
lattice of nickel (see Fig. 1, а). Difference consists only in some broad-
ening and shift of lines towards smaller angles. Besides, in the speci-
men No. 252, the presence of traces of the ferromagnetic phase of Ni4N
nitride is observed. Shift of Bragg reflexes directly points to the in-
crease of f.c.c. lattice parameter of nickel that is indicative of nitrogen
solid-solution formation in nickel.
512 R. V. SHALAEV
Thus, at concentrations of nitrogen in the gas phase lower than 2%,
the films are made as the pure nickel phase or the nitrogen solid solu-
tion in nickel. The ferromagnetic phase of Ni4N nickel nitride (f.c.c.) is
sustainably formed at nitrogen concentrations in the growth atmos-
phere less than 2—4% (see Fig. 1, b) and, at the further increase of ni-
trogen content, is substituted by the Ni3N phase (h.c.p.). Intensive re-
flexes from (110) and (111) planes, in comparison with tabular etalon
Fig. 1. X-ray diffraction patterns (CoK radiation) of Ni—N films produced
with the contents of 0—2% N2 (a) and 4—8% N2 (b).
GAS-PHASE SYNTHESIS OF FILM STRUCTURES OF Ni—N SYSTEM 513
patterns for equioriented crystallites, allow to speak about preferen-
tial orientation of growing Ni3N crystallites in these two directions.
X-ray diffraction patterns of films of Ni—N system, produced with
adding of 27—70% of nitrogen in the growth atmosphere, at CuK ra-
diation are presented in Fig. 2. Identification has been made and the
information about phase composition of films is obtained (see Table 2).
As seen, at concentrations of nitrogen in a gas phase approximately
from 6% to 30% in growing structure only one Ni3N phase is observed,
that is unequivocally identified by a number of reflexes. Preferential
orientation of (110) and (111) planes is preserved. At the further ni-
trogen concentration increase, the appearance of a new phase reflexes
is observed (see Fig. 2, a, b and Table 2), which has been identified by
us as Ni2N (b.c.t.). This phase is mentioned in references in very rare
cases [5, 12] and by now is studied insufficiently. Intensity of its re-
flexes increases at the further increase of nitrogen concentration in
the growth atmosphere.
Nevertheless, the specimen produced at 70% of nitrogen still con-
tains a small amount of Ni3N phase, which is seen from the correspond-
TABLE 1. Phase composition of Ni—N films produced with the contents of 0—
8% vol. of N2 in the gas phase.
Number of specimen
and N2 content
2Qexp., deg. 2Qtab., deg. hkl Phase
No. 250
0% N2
52.17
61.04
91.79
52.17
61.01
91.76
111
200
220
Ni
Ni
Ni
No. 252
2% N2
49.28
52.15
61.05
91.8
48.92
52.17
61.01
91.76
111
111
200
220
Ni4N
Ni
Ni
Ni
No. 253
4% N2
45.62
49.39
52.13
57.18
45.54
48.92
52.15
57.15
110
111
111
200
Ni3N
Ni4N
Ni3N
Ni4N
No. 255
6% N2
45.62
49.14
52.18
69.21
84.29
45.54
49.316
52.178
69.16
84.293
110
002
111
112
300
Ni3N
Ni3N
Ni3N
Ni3N
Ni3N
No. 251
8% N2
45.6
49.12
52.16
69.2
84.31
45.54
49.316
52.15
69.16
84.29
110
002
111
112
300
Ni3N
Ni3N
Ni3N
Ni3N
Ni3N
514 R. V. SHALAEV
ing X-ray diffraction pattern (see Fig. 2, b). Hence, at concentrations
of nitrogen in a gas phase above 30%, heterophase system Ni3N Ni2N,
with a dominance of the last phase, is formed at the nitrogen concen-
tration increase.
Thus, as seen from the presented spectra and the tables, the pro-
duced specimens for the most part are heterophase, as several Ni—N
phases are present in their compositions simultaneously, and their ra-
tio varies with a change of specimens’ production conditions (change of
nitrogen concentration in the growth atmosphere). The X-ray struc-
tural analysis demonstrates for produced specimens successive transi-
Fig. 2. X-ray diffraction patterns (CuK radiation) of Ni—N films produced
with the N2contents of 27%, 45% (a) and 70% (b).
GAS-PHASE SYNTHESIS OF FILM STRUCTURES OF Ni—N SYSTEM 515
tion from formation of pure metal nickel (the cubic phase) and the ni-
trogen solid solution in nickel to the nickel nitrides of various stoichi-
ometry: Ni4N, Ni3N, and Ni2N at the increase of gaseous nitrogen con-
centration in the growth atmosphere from 0% to 70% (Figs. 1 and 2).
At concentrations of nitrogen in a gas phase above 50%, dominancy of
Ni2N phase in the structure of films (see Fig. 2) is observed.
The broadening of reflexes observed in produced spectra can indi-
cate a comparatively small size of crystallites from which the film is
built. The estimate of this size by the Scherrer formula provides ampli-
tude 10 times smaller than full thickness of produced films, i.e., ten
nanometres. Sizes of crystallites L (more exactly, coherent scattering
region–CSR) have been determined for all phases of the produced
specimens by maximally intensive reflexes. The diffraction reflection
TABLE 2. Phase composition of Ni—N films produced with the N2 contents of
27—70% in the gas phase.
Number of specimen
and N2 content
2Qexp., deg. 2Qtab., deg. hkl Phase
No. 233
7% N2
38.89
41.87
44.38
58.45
70.44
78.27
85.48
87.21
38.94
42.111
44.48
58.51
70.6
78.38
85.665
87.39
110
002
111
112
300
113
302
221
Ni3N
Ni3N
Ni3N
Ni3N
Ni3N
Ni3N
Ni3N
Ni3N
No. 234
45% N2
38.9
40.37
41.9
44.42
45.56
58.54
66.36
69.73
70.45
80.62
87.27
38.94
40.79
42.111
44.48
45.79
58.51
66.76
70.60
70.67
81.28
88.38
110
101
002
111
110
112
200
300
112
211
202
Ni3N
Ni2N
Ni3N
Ni3N
Ni2N
Ni3N
Ni2N
Ni3N
Ni2N
Ni2N
Ni2N
No. 237
70% N2
31.74
38.81
40.36
44.33
66.35
69.68
80.59
87.29
31.94
38.94
40.79
44.48
66.76
70.67
81.28
88.38
100
110
101
111
200
112
211
202
Ni2N
Ni3N
Ni2N
Ni3N
Ni2N
Ni2N
Ni2N
Ni2N
516 R. V. SHALAEV
peak width at half-height of the peak intensity and angles of diffrac-
tion for each phase of specimens are measured, and calculation is per-
formed by the Scherrer formula:
0.9
,
cos
L
B Q
where is wavelength of X-rays ( 1.7902 Å for CoK radiation,
1.54056 Å for CuK radiation), Q is diffraction angle, В is the width
of the diffraction reflection at half-height of the peak intensity. The
dependence of change of CSR of Ni3N crystallites calculated by reflex-
es of (111) orientation, depending on concentration of nitrogen in the
growth atmosphere in which specimens are grown, is presented in Fig.
3. The distinctive growth of crystallites sizes of Ni3N phase with
growth of nitrogen concentration is observed.
The complicated relief of a surface of grown nickel nitride speci-
mens is confirmed by the 3D-images obtained by the means of AFM. In
Figure 4, the 3D-images of a surface of films produced in the pure Ar
atmosphere (see Fig. 4, a) and in atmosphere with adding of 75% of
nitrogen (see Fig. 4, b) are presented. In Figure 4, a, the specimen is
represented by the film of pure nickel (with a small amount of the dis-
solved atoms of nitrogen). ‘Sharp’ needle structure formed by the sep-
arate thin nanocolumns is well seen. Heterophase Ni3N Ni2N film in
Fig. 4, b differs by smoother differences of a surface profile, typical
for globules.
Fig. 3. Dependence of the typical sizes of crystallites of Ni3N phase in the
films produced at various nitrogen concentrations in the growth atmosphere.
GAS-PHASE SYNTHESIS OF FILM STRUCTURES OF Ni—N SYSTEM 517
AFM data also correlate with high-resolution SEM investigation
(see Fig. 5). As seen, the films grown at low concentrations of nitrogen
(nitrogen solid solution in nickel and Ni4N phase) consist of close
packed nanocolumns with the effective diameter 50—70 nm (see Fig.
Fig. 4. AFM 3D-images of the surface of films of Ni—N system grown in 100%
Ar (a) and with adding of 75% N2 (b) in the growth atmosphere.
a
b
c
Fig. 5. SEM images of the surface of
films of Ni—N system grown with
adding of 2% N2 (a), 27% N2 (b) and
75% N2 (c) in the growth atmosphere.
518 R. V. SHALAEV
5, а and paper [11]). With growth of the nitrogen content in the gas
phase in the films containing Ni3N and Ni2N phases, appreciable struc-
tural change of films is observed (see Fig. 5). They have the typical
globular structure with the effective size of elements 20—40 nm, and
incorporation of separate globules in aggregates with a size lower than
400—500 nm (see Fig. 5, b, c). It correlates with AFM data. It should be
noted that the specimens produced at nitrogen concentrations of 2%
and 27% have predominantly metal type of conductivity. It is well seen
by the quality of the SEM image. At the same time, the specimen pro-
duced at 75% N2 (Ni2N major phase) is characterised by considerably
smaller conductivity. It is seen from SEM image deterioration (see
Fig. 5, c).
3. CONCLUSIONS
As shown in this work, the magnetron spraying is effective method of
synthesis of various nanostructured phases of Ni—N system. With
growth of nitrogen concentration in the growth atmosphere of magne-
tron plasma, consequent formation of phases Ni, Ni4N, Ni3N and Ni2N
(at present, the last phase is insufficiently investigated) on the sub-
strate is observed. The typical sizes of crystallites of nickel nitride
phases comprise tens nanometres. It is revealed that the films pro-
duced at high concentrations of nitrogen (Ni3N and Ni2N phases) have
the globular structure, whereas films of pure nickel and the nitrogen
solid solution in nickel with small additions of the Ni4N phase are
nanocolumnar. Thus, depending on growth parameters (in particular,
on nitrogen concentrations in a buffer gas), one of the processes is ob-
served: nucleation of nanocolumns growing perpendicularly to the
substrate surface or the films growth with the globular character, i.e.
processes of self-organising of substance on the substrate, provided by
the non-catalytic mechanism, take place.
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/HRV (Za stvaranje Adobe PDF dokumenata najpogodnijih za visokokvalitetni ispis prije tiskanja koristite ove postavke. Stvoreni PDF dokumenti mogu se otvoriti Acrobat i Adobe Reader 5.0 i kasnijim verzijama.)
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/NLD (Gebruik deze instellingen om Adobe PDF-documenten te maken die zijn geoptimaliseerd voor prepress-afdrukken van hoge kwaliteit. De gemaakte PDF-documenten kunnen worden geopend met Acrobat en Adobe Reader 5.0 en hoger.)
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/ENU (Use these settings to create Adobe PDF documents best suited for high-quality prepress printing. Created PDF documents can be opened with Acrobat and Adobe Reader 5.0 and later.)
>>
/Namespace [
(Adobe)
(Common)
(1.0)
]
/OtherNamespaces [
<<
/AsReaderSpreads false
/CropImagesToFrames true
/ErrorControl /WarnAndContinue
/FlattenerIgnoreSpreadOverrides false
/IncludeGuidesGrids false
/IncludeNonPrinting false
/IncludeSlug false
/Namespace [
(Adobe)
(InDesign)
(4.0)
]
/OmitPlacedBitmaps false
/OmitPlacedEPS false
/OmitPlacedPDF false
/SimulateOverprint /Legacy
>>
<<
/AddBleedMarks false
/AddColorBars false
/AddCropMarks false
/AddPageInfo false
/AddRegMarks false
/ConvertColors /ConvertToCMYK
/DestinationProfileName ()
/DestinationProfileSelector /DocumentCMYK
/Downsample16BitImages true
/FlattenerPreset <<
/PresetSelector /MediumResolution
>>
/FormElements false
/GenerateStructure false
/IncludeBookmarks false
/IncludeHyperlinks false
/IncludeInteractive false
/IncludeLayers false
/IncludeProfiles false
/MultimediaHandling /UseObjectSettings
/Namespace [
(Adobe)
(CreativeSuite)
(2.0)
]
/PDFXOutputIntentProfileSelector /DocumentCMYK
/PreserveEditing true
/UntaggedCMYKHandling /LeaveUntagged
/UntaggedRGBHandling /UseDocumentProfile
/UseDocumentBleed false
>>
]
>> setdistillerparams
<<
/HWResolution [2400 2400]
/PageSize [612.000 792.000]
>> setpagedevice
|