Handbook of Modern Coating Technologies

Application of nano- and microprobes for the analysis of nanomaterials and nanocomposites, including nitrides of high-entropy alloys

Many studies have shown the successful use of modern micro- and nanoprobes for analyzing diffusion segregation processes. Table 5.4 contains the most promising results of studies of nanomaterials and nanocomposites using proton microwaves for analysis using RBS, PIXE, etc., and positron beam microprobe.
Some of the studies mentioned in Table 5.4 have important scientific results and, there-fore, should be considered in greater detail.
In studies [134,203] it was shown that irradiation of a-Fe samples by a high-current elec-tron beam resulted in the formation of local regions with lowered electron density, aggre-gates of interstitial carbon atoms, vacancies, and their agglomerations (see Figs. 5—25 and
5— 26). Subsequent irradiation of these samples gave rise to the formation of "craters” and thereby markedly altered the morphology of polished samples ([134,203] and Fig. 5—26).
Another example of the successful application of nano- and microprobes is provided in a series of publications where seven methods were used to analyze the fatigue strength at the subatomic level in the course of studying the formation of dark spots [118,216,217], slip bands, and speeding up chemical reactions in nanobulk materials (steel), which are accom-panied by the appearance of high-temperature local regions [218—223].
Worthy of note is the contribution of Russian researchers, both theorists and experimen-talists, to the development of near-field microwave diagnostics of ferrites and superconduct-ing ceramics [224—226].
Microwave diagnostics is successfully used to detect tumors and biological objects [227] and to increase the probing depth up to a few millimeters or centimeters and the probing area up to square millimeters or centimeters. In such cases, the point is visualization of an object rather than nanodefects, individual cells, or microcircuits, that is, the depth and the area of analysis increase at the expense of object size resolution, which decreases from nan-ometers to millimeters or centimeters [228].
Table 5.4 Brief summary of nanomaterials and nanocomposites investigated by nano- and microprobes.
Positron beam
Material Method Parameters energy Properties References
a-Fe HCEB • E 5 6-20 keV W5 2.3-5.2 H V 5 69-106 [134,203]

• T 5 0.75 p,s J/cm2 kg/mm2
• p5100-1000
A/cm2
a-Fe HCEB • E5 6-20 keV W5 2.5-5.2 [47]

• T 5 0.8 p,s J/cm2
• p5100-1000
A/cm2
Ta-Fe and HighHCEB • E5 6-20 keV W5 2.3-5.2 H V 5 270-520 [204]

Mo-Fe • T 5 0.75-1.5 ^s J/cm2 kg/mm2
• p5100-1000
A/cm2
Mg and Ti LEHCPEB • E 5 10-40 keV W 5 0.5-40 J/cm2 • wr 5 2-8 X 102 [205]

• T 5 0.5-5 p,s mm3/min
• p5100-1000 • COF 5 0.24-0.27
A/cm2 • cr 5 0.07-0.75 g/cm2 h
Fe-Cr Intense pulsed • E5 14 keV W5 30-53 J/cm2 • HV54400 MPa [206]

electron beam • T 5 450 ^m • wr 5 1.6 X 1026 mm3/Nm
Fe-Cr-C Intense pulsed T 5 50-200 ^s W 5 10-30 J/cm2 [207]

electron beam
TiN HIPIMS • T 5 0.5 p,s — • H 5 34.8-38 GPa [208]

• U5 -400 V • COF 5 0.84-0.97
CrN Pulsed magnetron • P 5 0.3-0.35 mPa — • H 5 20-23 GPa [209]

sputtering • U 5 -90 V • E 5 160-220
Ti-Si-N Pulse high-frequency • I 5 90 A — • H 5 38-39 GPa [210]

sputtering • PN 5 0.3-0.7 Pa • E 5 356 GPa
• Ub 5 -50—200 V • wr 5 1.95-7.69 X 1025 mm3/nm
• COF 5 0.69-0.88
Al-Si-N Closed magnetic field dual • P 5 0-0.5 Pa — • H 5 15-25 GPa [211]

magnetron sputtering • l5 1 A • E 5 230-240 GPa
Ti-Cr-N ICP- assisted magnetron P 5 80 mTorr — H V > 5000 [212]

sputtering
Ti-Hf-Si-N Pulse high-frequency • PN 5 0.3-0.7 Pa W5 1-20 keV • H 5 37.4-48.6 GPa [213]

sputtering • Ub 5 -100—200 V • COF 5 0.12-0.6
Ti-Al-Si-N MPPMS • T 5 1000 p,s — • H 5 23.6-31.3 GPa [214]

• lp 5 62.2-138.2 A • H/E 5 0.079-0.091
• Vp 5 401-408 V • We 5 50.1%-57.4%
(Ti-Hf-Zr- Pulse high-frequency • PN 5 0.08-0.3 Pa — • COF 5 0.22-1.03 [215]

V-Nb)N sputtering • Ub 5 -40 200 V • wr 5 0.027 X 1025 mm3/Hmm
HCEB, High-current electron beam; HIPIMS, high power impulse magnetron sputtering; ICP, inductively coupled plasma; LEHCPEB, low-energy high- current pulsed electron beam; MPPMS, modulated pulsed power magnetron sputtering.

x 103

FIGURE 5-25 (Color image online.) Distribution of elements over a-Fe sample surface obtained with a microprobe (PIXE and RBS): (A) after irradiation by an electron beam (10 pulses), (B) the initial surface prior to irradiation, and (C) separated electron-irradiated region [47]. PIXE, Particle-induced X-ray emission; RBS, Rutherford backscattering.

The present review does not pretend to be a comprehensive description of new, promis-ing methods; their characteristics can be found in numerous papers and monographs. Our aim was to demonstrate the successful application of micro- and nanoprobes for diagnostics of materials at the subatomic level, bearing in mind that most of the relevant information is available only to researchers working in this specific field. The data included in the review may be of value for specialists interested in the analysis and development of new nanocom-posites, nanoconsolidates, and nanopolymers, as well as for those engaged in medico- biological research at the subatomic level. It is safe to predict the further development and application of analytic techniques, which promote the introduction of novel materials based on the better understanding of subatomic processes in them.
Fig. 5—27 shows the results of an elementary analysis obtained using the method of EDS and RBS. From Fig. 5—27A, the following distribution of concentrations can be seen: CTi« 55—60 at.%, CSi ^ 5 at.%, and CN « 35—40 at.%. Fig. 5—27B shows the distribution of element concentrations in this form: CTi« 44 at.%, CSi« 5.5 at.%, and CN « 50 at.%.
Based on the RBS data, the coating thickness was found to be 2.18 6 0.01 pm. EDS results (see Fig. 5—27C) confirm the RBS data. In the coating, the concentration of the elements has the following values: CTi« 40.69 at.%, CSi ^ 2.62 at.%, and CN « 55.92 at.%. Using XPS analysis, a Si—Nx bond was studied for another series of samples (with CSi $ 5.8 at.%). The results of the study showed the formation of the Si—Nx bond in this sample (this is indicated by a high peak at 101.9 eV). Also this study showed the presence of a small amount of Si—O (peak at 103.9 eV) as a result of annealing at 600°C for 30 min in air. The formation of SiN at the boundaries of TiN nanograins showed additional studies using the p-PIXE method.
(A) Positron penetration depth (pm)
0 0.02 0.24 0.46 0.74

(B) Positron penetration depth (pm)
0 0.08 0.26 0.49 0.78

FIGURE 5-26 (A) Ion backscattering (RBS) spectra obtained with the use of a microprobe from coarse-grained a-Fe-samples (grain size 2-3 mm): 1—before irradiation, 2—irradiation by an electron beam with an energy density of 2.5 J/cm2, 3—irradiation by a high-current beam, 3.5 J/cm2, and 4—irradiation by a high-current beam, 5.5 J/cm2. (B) Depth distribution of vacancy defects obtained using a slow beam of positrons implanted into a-Fe (positron microprobe) after irradiation by a high-current electron beam of different densities: 1—before irradiation (grains larger than 3 mm), 2-2.5, 3-3.5, 4-4.5, 5-5.2, and 6-5.5 J/cm2 [47]. RBS, Rutherford backscattering.

Fig. 5-28 shows the surface images of the coating before and after annealing for 30 min at a temperature of 600°C. Regardless of HF stimulation, flat "drops” of the molten phase can be observed. An analysis of the droplet fractions of which the plasma jet partially consists was not carried out. A round hole was cut through the thickness of the coating to normalize the depth of analysis of the slow positron beam and obtain the real thickness of the Ti-Si-N nanostructured coating. Fig. 5-28C shows that the coating thickness is 2.39 6 0.01 pm. Moreover, for Emax = 20 keV the calculated path of the positrons in the coat¬ing is 2.11 pm. The positron beam does not reach the interface between the substrate and 
FIGURE 5-27 Energy spectra of Ti—Si — N coatings: (A) nitrogen pressure PN 5 0.5 Pa and bias potential Us =-50 V (RBS) (the second curve corresponds to the SiW curve of the standard); (B) PN = 0.7 Pa and Us = -100 V (RBS); and (C) PN = 0.5 Pa and Us =-50 V (EDS) [210]. RBS, Rutherford backscattering. 
N509 SIMS mass spectrum with oxygen flooding 6x10 6 Torr

FIGURE 5-28 Topography of the surface of Ti —Si—N coating: (A) after deposition, (B) after annealing at 600°C, and (C) SEM analysis of the cross section in the shape of a circle prepared by the cutting using ion beam [210]. SEM, Scanning electron microscopic.

the coating even under the condition of the thermalized positrons diffusion (its length is ~100 nm). Therefore information on vacancy defects over the entire thickness of the Ti—Si—N coating is provided by profiles of the average penetration depth of the positron, although the interface between them is not reached.
In nanocrystalline materials, the method of the positron annihilation is one of the most reliable and effective techniques for analyzing free volumes (the defect analysis interval is in the range of 10_6/10_3 defects per atom) [215,229].
At the interface of three neighboring nanocrystals or at the interface between two adja¬cent nanograins, a part of positrons can be captured. Since the volume (length) of such boundaries affects the properties of nanocomposite coatings, this allows understanding the interface structure between nanograins, which is one of the most complex and interesting problems of nanomaterials [47,230—237].
The energy dependence of the S parameter is shown in Fig. 5—29. That is, in the Ti—Si—N coating, defect profiles are visible before (black and red curves are the defect pro-files prior and after thermal annealing for 30 min at 600°C, respectively). Considerable changes can be observed in the defective and electronic structure (Fig. 5—29). It is important that, at defects located at the nanograin boundaries, all positrons are localized and annihi-late, and that the concentration of defects increases over the entire thickness of the coating. The nanograin size is 12.8 6 0.3 nm, and the diffusion depth of thermalized positrons is « 100 nm;therefore, almost all positrons are captured at interface defects.
Approaching the interface between the coating and substrate, the S-parameter signifi-cantly increases, that is, defects also migrate to the interface between the coating and sub-strate due to thermal diffusion. The thickness of this transition layer of defects is no more than 250 nm. Calculation of vacancy defect concentration was done using the positron capture model with two types of vacancy defects [237], and it showed that defect concen-tration increases after annealing from 5 X1016 to 7.5 X 1017/cm3, increase in the
N509 GDMS depth profile analysis

Time (s) Time (s)
FIGURE 5-29 Energy dependence of the positron S-parameter microbeam (deposited coating is a black curve; annealed coating is a red curve) [210].

FIGURE 5-30 SIMS analysis data for the first series of Ti—Hf—Si — N samples (element concentration profiles in the coating). High concentration of Fe is observed in the substrate material (steel) [213]. SIMS, Secondary-ion mass spectrometry.

concentration of the thermally activated vacancies from 1 X 1016 to 5 X 1018/cm3 is also observed (red curve).
The advantage of this method is that it is nondestructive. A more sensitive analysis method is SIMS (detection accuracy is ~10—6 at.%) (Fig. 5—30). Therefore the comparison of the results collected by the RBS, SIMS, and GDMS methods gives a more realistic map of the distribution of the elemental composition through the thickness of the coating. This made it possible to determine the concentrations of uncontrolled carbon and oxygen impurities com-ing from the residual atmosphere of the chamber working medium and to analyze the film composition from the film-substrate interface to the surface of the film.
The energy dispersion spectra of the Ti—Hf—Si—N coating (series 1) are shown in Fig. 5—31A and B. Integral information from a 2 X 2 mm2 area is shown in Fig. 5—31A, and local analysis information is shown in Fig. 5—31B. The distribution of elements along the coating depth is uniform, since there is no particular difference between the spectra.
The relationship between S-parameters and the incident positron microbeam energy is shown in Fig. 5—32. According to stoichiometry (content) of elements and phase composi-tion, the significant differences in the depth profiles of vacancy defects in the coatings (series 2 [a] and series 3 [b]) are observed (Fig. 5—33). The curve behaviors differ drastically. For samples of series 2, a two-phase system is formed consisting of (Ti, Hi) N and a-Si3N4. It is characterized by the formation of two peaks (an increase in the S parameter) in the region of 20 keV (near the coating—substrate interface) and in the region of 10 keV. In the case of a series of samples 3, the S parameter is quite large for a single-phase (Ti, Hf) N solid solution, and is —0.492, and at the film—substrate interface it is 0.476 [238—241].
In the jet regime of a plasma flow without separation, non-textured polycrystalline coat-ings with a sufficiently high relative peak intensity are formed as shown in Fig. 5—33.
The deposited coatings had different textures during beam separation. A texture was obtained with [110] when a low bias potential (—100 V) was established on the substrate. Thus the structure of the coating consists of nontextured and textured crystallites. The volu-metric content of non-textured crystallites is ~60% of the total, and the lattice constant in comparison with textured crystallites is reduced. An uneven distribution of Hf atoms in the coating may be the most likely reason for the increase in the lattice constant of textured crys-tallites. Moreover, in the direction perpendicular to the growing surface, texturing results in the increase in the average crystallite size. So, the average size in the fraction of textured crystallites is 10.6 nm, and the size in the fraction of nontextured crystallites is much lower and is 6.7 nm. This type of coating has maximum values of nanohardness. In the case of using a separation scheme and increasing the voltage up to — 200 V during deposition, the formation of the coatings with an average crystallite size of ~5.0 nm and less than 20 vol.% fraction of textured crystallites is observed. The texture is formed in the [001] direction. Accelerating voltage (energy of the plasma stream) increases from —100 to —200 V during the formation of the textured fractions with the same spatial period. However, the lattice parameter in this case is 0.4337 nm and exceeds the non-textured fraction period, which can be obtained by applying to the substrate a low potential. According to the Vegard's rule for solid solutions, this period matches Hf concentration in the solid metal solution (Hf, Ti) of
(A) Energy (keV)
500 1000

(B) Depth (nm)
5 50 150 300 500 1000

FIGURE 5-31 Energy dispersive spectra from series 1 of Ti—Hf—Si — N coatings: (A) integrated information from the 2 x 2 mm2 region and (B) analysis from the local places [213].

~33 at.% [the following values of parameters were used for calculation: aHfN = 0.452534 nm (JCPDS 33—0592) and aTiN = 0, 424173 nm (JCPDS 38—1420)] [233,242].
The maps in element contrast obtained using the EDS shown in Fig. 5—34A indicate the distribution of the elements of (Ti—Hf—Zr—V—Nb)N coatings. The scan area of EDS analysis 
is 0.1 X 10 mm2. The concentration of elements in the sample is defined by color intensity. The droplet fraction appeared during the deposition process is seen on the surface of the coatings as dark round shaped spots. The results of EDS microanalysis of the as-deposited coatings obtained under different deposition conditions is presented in Fig. 5—34B and C, 

FIGURE 5-33 Images of structure areas of nanocomposite Ti—Hf—Si—N coating, obtained by TEM JEOL 2010 F: (A) structure of surface and (B) dark-field image of the nanograin structure [213]. TEM, Transmission electron microscope.

FIGURE 5-34 Results of EDS microanalysis of (Ti—Hf—Zr—V—Nb)N coatings: (A) elemental mapping at coating's surface; (B) EDS spectrum of the coating obtained at Ub =-100 V and PN = 2 x 10-0; (C) EDS spectrum of the coating obtained at Ub = -200 V and PN = 3 x 10-0; and (D) EDS spectrum of the sample at 873K [215].

while EDS microanalysis of the annealed sample at 873K during 30 min (the pressure in the chamber was 100 Pa) is shown in Fig. 5—34D.
According to obtained results the concentration of the constituent elements in experi-mental coatings obtained at gas pressure of 2 X 10-2 Pa in atomic percentage is N = 49.05, Ti = 22.92, V = 5.04, Zr = 6.84, Nb = 7.47, and Hf = 8.68 at pressure 2 X 10-2 Pa. The decrease of the concentration of nitrogen to 36.04 at.% (other elements' concentration are Ti = 20.13 at.%, V = 2.28 at.%, Zr = 17.12 at.%, Nb = 17.50 at.%, and Hf = 6.93 at.%) is observed at pressure lowering to 3 X 10-2 Pa. It indicates a significant nitrogen deficiency in the multicomponent systems obtained at low nitrogen pressure in comparison with coatings of stoichiometric composition.
The results of RBS and EDS analyses shown in Figs. 5—34 and 5—35 designate a notice-ably effect of the radiation factor related to the increase of negative bias potential on

0 100 200 300 400
Time of sputtering (min)
FIGURE 5-35 RBS spectra of (Ti-Hf-Zr-V-Nb)N coatings obtained at: (A) PN 5 8 x 10-0 Pa and Ub 5 -200 V (sample 512) and (B) PN 5 2 x 10-0 Pa and Ub 5-50 V (sample 510) [215]. RBS, Rutherford backscattering.

segregation processes occurring during the deposition process. That is, the contribution of the radiation factor can be enhanced by the energy of ion plasma flux increases due to the increase of the bias potential. There are two required terms that can ensure the formation of a two-phase nanostructured film. The first one is the increased rate of the diffusion of atoms along the grain boundaries. Another is the high temperature of the deposition process (873K) at which the process of spinodal segregation is completed [243-246].
According to the results of EDS microanalysis, ion bombardment (enhanced by increasing the substrate bias) exert the determining influence on the segregation processes while the coating formation. When the energy of ion flux increases, the contribution of ion bombard¬ment enhances, which suggests the increase of radiation-induced defect density [247].
The annealing of (Ti-Hf-Zr-V-Nb)N samples results in the formation of an oxide film on the surface of the coatings, presented by high-intense O peak at EDS spectrum (see Fig. 5-34D). The results of XRD analysis of annealed samples have also confirmed this state¬ment (see Fig. 5-36). The presence of Fe and Cr at EDS spectra occurs due to the diffusion of these elements from the steel substrate. The deviation of the concentration values of 
nitrogen in experimental samples is ~0.26 at.% for coatings with a nitrogen concentration of
49.5 at.% and not more than 0.18 at.% for coatings in which nitrogen concentration is less
36.5 at.%. According to the positron annihilation, the positrons are located well within the following areas of low electron density: vacancy-type defect divacancies, vacancy complexes, conglomerates of various vacancies, and interstitial defects of three or more atoms bonds [237,239,240]. The literature data [246,248—251] reported that in nanostructured materials, deposited using vacuum compaction, the grain boundaries are strong trapping centers for the positrons, which then annihilate with two or three components of the positron lifetime ті, T2, and T3. It is obviously related to positron annihilation at the grain boundaries, that is, the formation of the quasiamorphous phase for our samples.
The results presented at Fig. 5—37A and B clearly indicate that the defect profiles (S- parameter) vary significantly for different deposition conditions (see deposition conditions for samples 510 and 512). The temperature annealing at a high residual pressure of 100 Pa leads to the great changes of S-parameter over the depth of the coating. This way, S-parame- ter for sample 512 reduces from 0.58 to 0.56 (as-deposited) to 0.52 to 0.51 (annealed). However, when analyzing the energy of positrons 12.5—15 keV, it increases to 0.53. 
According to the curve of as-deposited sample 510 (see Fig. 5—37B), the positron-sensitive defects are almost absent within the depth scan line. Thus the positron annihilation has occurred mainly with the electrons from the defect-free areas.
The minimal value of the magnitude of S-parameter is 0.49. The significant increase of the magnitude of S-parameter to 0.53 is registered after thermal annealing of the coating at 
600°С. There is the dependence of S-parameter on the analyzing depth: it increases to the maximal value of 0.59 when the positron energy range changes from 14 to 17 keV [248].
It is important to mention that S-parameter depends on the concentration of vacancy defects at which positrons are captured and then annihilate in the areas of low electron den-sity and their type (dislocation, vacancy, and grain boundary) [246,248,249].
It is known that if the size grains in nanostructured coatings is smaller than the length of diffusion track of positrons in defect-free areas, all positrons can reach the grain surface and consequently their boundaries. Hence, obtained results, in this case, relate to the defects at the boundaries and triple or more bonds. Inasmuch as the grains size of experimental coat-ings changes from 40 to 60 nm, the volume fraction of the interfaces reaches the range of 30—35 vol.%, and the interfaces of triple bonds are ~5—10 vol.%, hence, almost all positrons will be bonded along the interfaces [246].
When the distance between the defects is essentially shorter the positron diffusion length, all positrons will be captured by defects, hence, the capture saturation is observed. The posi-tron lifetime spectrum will contain only one component in this case [246,248] and S-parame- ter of Doppler broadening will reach the maximum value.
The map of the element distribution of (Ti—Zr—Hf—V—Nb)N coating sample 512 (the analyzed area is 2.5 X 2.5 pm2 and scanning step is 0.5 pm) is presented in Fig. 5—38A. It is obvious that constituent elements are spread very evenly over the surface and bulkwise the coating. The thermal treatment of the samples at 873K during 30 min promotes the segrega-tion of impurities at the grain boundaries, which clearly can be observed at presented maps (see Fig. 5—38B). It is worthwhile to pay attention to the fact that almost all constituent ele-ments are detected, and only nitrogen is not revealed at the spectrum since PIXE method is not insensitive enough to light elements. The width of these grains interfaces is ~0.12 6 0.25 pm, and the size of large grains ranges from 0.3 to 0.8 pm. Considering the results obtained by XRD and p-PIXE, it can be concluded that the grains of microsize (0.3—0.8 pm) composed of fragmented nanograins (45—60 nm) are formed in the structure of

FIGURE 5-38 Maps of the element distribution of (Ti—Zr—Hf—V—Nb)N coating (sample 512) before (A) and after (B) thermal treatment. Analyzed area is 2.5 X 2.5 pm2, step size is 0.5 pm [215].

multielement (Ti—Zr—Hf—V— Nb)N coatings. The size of the grains was determined on the basis of XRD results. It is also established that the impurities segregated at the boundaries of large grains due to temperature stimulated diffusion, and result in the formation of the inter¬layer small grains.
According to the results obtained by TEM analysis, the structural phase state of experi-mental coatings, composed by different alloying elements (Si, B, and Al) in the TiN system even at high diffusion mobility of atoms, presented by two-phase textured grains structures. It is also established that grains of a submicron size (0.2—0.6 pm) are fragmented by the low- angle interfaces with the disorientation angles of 5 degrees and by nanograins of 20—30 nm in investigated coatings [252].
According to Fig. 5—38, the elements are distributed almost uniformly over the surface and in-depth of the experimental coatings. The thermal annealing of films at 600°С results in segregation of the impurities at the grain boundaries [247].
The mass spectra for multilayer (Ti-Hf-Zr-V-Nb)N coating (sample 509) obtained by SIMS method is presented in Fig. 5—39. It is obvious that there is a thin oxide film on the surface of the experimental coating. It is presented by ZrO, NbO, HfO, and ZrO2 phases and also contains a high concentration of titanium and vanadium elements.
The spectra (the depth profiles of elements) obtained by GDMS under different etching rates are shown in Fig. 5—40. It is obvious that all profiles have a similar distribution of con-stituent elements as well as the same thickness of the coating layer. However, the depth

Energy (keV)
FIGURE 5-39 SIMS spectra for multilayer (Ti—Hf—Zr—V—Nb)N coating (sample 509) [253]. SIMS, Secondary-ion mass spectrometry.

FIGURE 5-40 GDMS spectra for multilayer (Ti-Hf-Zr-V-Nb)N coating (sample 509) [247].

distribution of Fe and N elements differs due to different etching rates. But the profiles of elements with high concentration are similar. Thus the results obtained by RBS, SIMS, and GDMS give an insight on the element distribution of investigated coatings.
Experimental investigations show that positrons are concentrated in the regions with a low electron density, that is, vacancy-type defects divacancies, vacancies cluster, vacancy complexes with two or three interstitial atoms [246,254,255]. As it follows from literature data [236,249,250], the nanostructured materials deposited using vacuum compaction, act as traps for positrons, with the positron lifetime of т 1, T2, and T3. The positron lifetime т is presented as a function of the electron density at the annihilation size. When positrons are trapped in open-volume defects, the positron lifetime increases and related to the defect-free state of the sample. The intensity of the component with a long lifetime is directly related to the defect concentration. In [251] reported that the lifetime T1 is considered as the lifetime of positrons in vacancies of the grain interfaces, the annihilation of positrons in three-dimensional vacancy agglomerates (nanopores) is characterized by T2 and finally, T3 is pre-senter the large free volume the dimensions of which close to the crystallites size [236].
According to the results of EDS analyze for the sample 510 with lower elastic stress in the initial state than for other samples, two peaks are formed on the curve of S-parameter at the energy of the positron beam of 3/5 and 14/17 keV. This is explained by the intense diffusion process of N and O atoms in the near-surface region for this sample and indicates the forma-tion of new channels for the positrons annihilation, which are more actively pulled to defects at the interface. The new quasi-amorphous nitride phases are formed in this case. This con-clusion is also proved by the results of PIXE-p analysis, according to which, an oxide film has formed on the surface, and caused the increase of S-parameter. It is observed the redistribu¬tion of the elements along the coating depth and signals the end of the spinodal segregation process and the formation of new phases at nanograin interfaces [30-34]. It is worthwhile to note that the mechanism of structural relaxation is occurred due to the growth of the grains
during temperature annealing, and the segregation of nitrogen at the grain boundaries pre-vents the growth of nanosized crystals.
Acknowledgments
The authors are grateful to their colleagues: A.G. Ponomarev, A.P. Shypylenko, O.V. Sobol', A.A. Bagdasaryan, K.V. Smyrnova, et al. for assistance in the collaborative research. This work was supported by the Ukraine's state budget programs: “Implantation of low-energy and high-energy ions into multielement and multilayer coatings: microstructure and properties” (registration number 0119U100787);“Improved physical and mechanical properties multilayer protective coatings based on high-entropy alloy nitrides” (registration num¬ber 0120U100475).
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