By small angle X-ray scattering (SAXS) and atomic force microscopy characteristic sizes are deter-mined, structural features of thin iron films deposited by magnetron evaporation onto substrates  from  py-roceramics are established. It is shown that morphologically the film is characterized by disorder. It is 
formed from columnar nano crystallites that are oriented either perpendicular to the substrate or situated 
in its plane, which dictates polydispersity of those coatings. It is shown that SAXS may be thought of as 
nondestructive technique for analyzing structure and composition and conducting quality control of mag-netron films.
When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/3625

Chekadanov, A.S.

Chevyakov, L.M.

Dobromyslov, M.B.

Emelyanov, S.G.

Kuzmenko, A.P.

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 6 No 3, 03023(3pp) (2014) Том 6 № 3, 03023(3cc) (2014) 
 
 
The article was reported at the International Conference «The Advanced Technology, Equipment and Analytical Systems for Materials», Kursk, 13-14 May, 2014 
2077-6772/2014/6(3)03023(3) 03023-1  2014 Sumy State University 
Small Angle X-ray Scattering in Thin Iron Films 
 
A.S. Chekadanov1, A.P. Kuzmenko1, S.G. Emelyanov1, L.M. Chevyakov1, M.B. Dobromyslov2 
 
1 South-West State University, 94, 50 Let Oktyabrya St., 305040 Kursk, Russia 
2 Pacific National University, 136, Tikhookeanskaya St., 680035 Khabarovsk, Russia 
 
(Received 19 May 2013; published online 15 July 2014) 
 
By small angle X-ray scattering (SAXS) and atomic force microscopy characteristic sizes are deter-
mined, structural features of thin iron films deposited by magnetron evaporation onto substrates from py-
roceramics are established. It is shown that morphologically the film is characterized by disorder. It is 
formed from columnar nano crystallites that are oriented either perpendicular to the substrate or situated 
in its plane, which dictates polydispersity of those coatings. It is shown that SAXS may be thought of as 
nondestructive technique for analyzing structure and composition and conducting quality control of mag-
netron films. 
 
Keywords: Small angle X-ray scattering, Atomic force, Scanning electron, Digital holographic microscopy, 
Thin magnetron films. 
 
 PACS number: 61.10.Eq 
 
 
1. INTRODUCTION 
 
Thin-film materials that feature unique physico-
chemical properties, which are due in large part to di-
mensional effects and phenomena, find very broad ap-
plication in both nanomaterial science and micro- and 
nanoelectronics that are being developed most inten-
sively [1], including development of sensor devices, 
magnetic data carriers, protecting coatings, etc. Study 
of structural features of such entities presents a pro-
found scientific problem. Transmission electron micros-
copy (TEM), as a rule, does not provide validity of ob-
tained data any more. In this connection, small-angle 
X-ray scattering (SAXS) technique, which does not 
cause secondary effects due to X rays, can be success-
fully applied for studying the regularities of growth of 
thin-film materials, and the influence of their synthesis 
parameters on the structure and properties. The chief 
merit of this technique is that only this method, in fact, 
makes it possible to obtain statistical values of size, 
volume, surface area and forms of nanoparticles of sub-
stance. Unlike granulometric analysis, SAXS excludes 
the influence of human factors [2]. 
 
2. EXPERIMENTAL SECTION 
 
Magnetron iron films were evaporated with facility 
GENCO onto substrates from pyroceramics the size of 
40  60 mm, which provided high surface uniformity of 
films. Working pressure of argon in a chamber was 
1 Pa. Power of plasma discharge was not greater than 
400 W. These parameters of the facility are significantly 
distinct from those given in [3]. Topology of film surface 
and determination of an average size of the granular 
structure was investigated with scanning probe micro-
scope (SPM) SmartSPM (AIST NT). Morphological fea-
tures and changes in surface structure of materials 
studied were investigated with scanning electron micro-
scope (SEM) (JEOL JSM-6610LV) with a magnification 
of up to 100000x at an accelerating voltage of 20 kV. 
Morphology of film surface was also studied with digital 
holographic microscope (Lyncee tec) with a height 
measuring accuracy of 0.1 nm. 
Studies with SAXS were conducted with the help of 
facility SAXSessmc2 (Anton Paar) in the linear collima-
tion mode, which makes it possible to characterize 
structural features of objects with the size of 0.1 to 
100 nm. To this end a typical X-ray tube was used with 
copper anticathode and a monochromator with X-ray 
radiation of 0.154 nm K line.  
 
3. RESULTS AND DISCUSSION 
 
Typical scattering curve according to SAXS is given 
in a logarithmic scale in Fig. 1. 
 
 
 
Fig. 1 – SAXS curve of a magnetron iron film at the substrate 
from pyroceramics (logarithmic scale) 
 
Figure 2 shows SEM-image of an iron film with 
characteristic sizes of nanodimensional objects. It is seen 
some surface disorder when structures in both evapora-
tion plane and as usual perpendicular to it are observed 
[3-5] with the formation of columnar nano crystallites. 
Disorder of thin-film structure is attested by its profile 
along the line of 350 m length obtained with holograph-
ic microscope according to which the maximum height 
difference was 26.24 nm with an average roughness of 
not greater than 3.5 nm.  
The shape observed was of two types: elongated in 
the substrate plane and regular of a circle form, which 
was probably the tip of a columnar nanocrystal structure 
 A.S. CHEKADANOV, A.P. KUZMENKO, ET AL., J. NANO- ELECTRON. PHYS. 6, 03023 (2014) 
 
 
03023-2 
perpendicular to the substrate surface. Granulometric 
analysis of AFM-images revealed that coatings studied 
had clearly polydisperse structures (Fig. 2b). The given 
particles had sizes varied within broad ranges from sev-
eral tens to several hundredths of nm, among which 
prominent are formations of a cylindrical shape (up to 
360 nm) composed from individual likely disk-like blocks 
of order 20 nm. It should be noted that sizes obtained 
with AFM-images are, as a rule, laterally overestimated 
due to spherical form of a cantilever probe (R  15 nm). 
Real-world size form (Fig. 2) can be reduced by 30 %. 
 
 
 
 
 
Fig. 2 – Electron-microscopic and atomic-force image of the 
iron film 
 
As was noted, for studying disperse systems in such 
thin magnetron layers SAXS can be utilized. However, 
unlike the situation shown in [6] it is excluded in our 
case. Moreover, as AFM- and SEM-data reveal film 
magnetron layers on substrates from pyroceramics 
were formed from polydisperse nanoparticles and their 
agglomerates as columnar nano crystallites. 
Processing of SAXS data (Fig. 1) was made with the 
program GIFT (PCG Software Package), which made it 
possible to compute the volume size distribution of par-
ticles DV(r) (Fig. 3) in analogy with [7]. The average 
sizes of particles forming the magnetron films were 
found to be 6, 22, and 114 nm. Evaluation of normal-
ized number of various-size nanoparticles determined 
from the ration of their areas under their distribution 
reveals that particles with a radius of 11 nm take the 
large part of the volume in the film studied. Compari-
son of these sizes with data found with microscopic 
techniques suggests correspondence. 
The validity of this approach stems from the follow-
ing considerations. It is obviously that for monodis-
perse film there is a maximum size of nanoparticles 
that is determined from the distance distribution curve 
p(r) . The curve is computed from intensity of SAXS 
with the program of indirect Fourier transformation 
 
    
 
max
min
exp2
sin1
2
s
s s
sr
p r I s ds
sr

  .  
 
The length of the scattering vector – s (the vector 
equal to the difference between the vectors of scattered 
and incident waves) is determined from: 
 
 0
4 sin
2 sin
 


 s k ,  
 
where 2 is the, Iexp is experimentally observed intensi-
ty, and r is the distance between two scattering elec-
trons. Whereas for polydisperse system one can deter-
mine the function of volume size nanoparticle distribu-
tion from the integral equation: 
 
        
max
min
2
0
R
V
R
I s D R m R i sR dR    
 
Here Rmin, Rmax and R are maximum and minimum 
sizes and the particle size, i0(x) and m(R) are form-
factor of particle (the particle shape is set a priory) and 
its volume. In computing V(R) the value Rmin is taken 
equal to zero and the quantity Rmax is chosen individu-
ally for each specific case by the most appropriate fit-
ting. The function DV(R) may be thought of as appro-
priate if it does not provide negative spikes and ap-
proaches zero at a maximum value of R without a 
sharp fall-off, i.e. the computed scattering intensity 
curve coincides with the curve from experiment. 
 
 
 
Fig. 3 – Volume size distribution of particles in iron magnetron 
film at the substrate from pyroceramics 
 
4. CONCLUSIONS 
 
The given inference is also corroborated by similar 
studies with copper magnetron films when the formation 
of columnar nano crystallites is observed with aspect 
 SMALL ANGLE X-RAY SCATTERING IN THIN IRON FILMS J. NANO- ELECTRON. PHYS. 6, 03023 (2014) 
 
 
03023-3 
ratio L  l / d, whose value with characteristic magni-
tudes of diameter (d) and length (l) is 15-20. Such mag-
netron films also feature developed morphology; include 
columnar nanoparticles, which are oriented both per-
pendicular to the substrate and situated in its plane. 
This dictates polydispersity of those coatings and makes 
its analysis and examination difficult. In this connection, 
SAXS technique may be thought of as nondestructive 
technique for analyzing structure and composition and 
conducting quality control of magnetron films. 
 
 
REFERENCES 
 
1. R.P. Seisyan, Tech. Phys. 56 No 8, 1061 (2011). 
2. A.P. Kuzmenko, A.S. Chekadanov, E.Yu. Orlov, Nanothech-
nika No 4(36), 41 (2013). 
3. S.N. Saltykov, A.N. Kharin, A.M. Khoviv, Kondensiro-
vannye sredy I mezhfaznye granitsy 11, No 2, 147 (2009) 
[in Russian]. 
4. K. Nowakowska-Langier, K. Zdunek, R. Chodun, R. Nietubyc, 
R. Mirowski, J. Witkowski, Problems of atomic science and 
technology. Series: Plasma Physics 16, No 6, 159 (2010) [in 
Russian]. 
5. A.P. Kuzmenko, V.G. Zavodinsky, А.Е. Kuzko, D.I. Timakov, 
S.V. Nokolenko, S.A. Pyachin, M.A. Pugachevsky, Izvestiya 
YuZGU. Physics and chemistry serie 1, 37 (2011) [in Rus-
sian]. 
6. Y. Ito, K. Omote, J. Harada, International Centre for Dif-
fraction Data, Advances in X-ray Analysis 46, 56 (2003). 
7. A.P. Kuzmenko, A.S. Chekadanov, S.V. Zakhvalinsky, 
E.A. Pilyuk, M.B. Dobromyslov, J. Nano-Electron. Phys. 5 
No 4, 04025 (2013).  
 


Small Angle X-ray Scattering in Thin Iron Films

Electronic Sumy State University Institutional Repository

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ Vol. 6 No 3, 03023(3pp) (2014) Том 6 № 3, 03023(3cc) (2014)   The article was reported at the International Conference «The Advanced Technology, Equipment and Analytical Systems for Materials», Kursk, 13-14 May, 2014 2077-6772/2014/6(3)03023(3) 03023-1  2014 Sumy State University Small Angle X-ray Scattering in Thin Iron Films  A.S. Chekadanov1, A.P. Kuzmenko1, S.G. Emelyanov1, L.M. Chevyakov1, M.B. Dobromyslov2  1 South-West State University, 94, 50 Let Oktyabrya St., 305040 Kursk, Russia 2 Pacific National University, 136, Tikhookeanskaya St., 680035 Khabarovsk, Russia  (Received 19 May 2013; published online 15 July 2014)  By small angle X-ray scattering (SAXS) and atomic force microscopy characteristic sizes are deter-mined, structural features of thin iron films deposited by magnetron evaporation onto substrates from py-roceramics are established. It is shown that morphologically the film is characterized by disorder. It is formed from columnar nano crystallites that are oriented either perpendicular to the substrate or situated in its plane, which dictates polydispersity of those coatings. It is shown that SAXS may be thought of as nondestructive technique for analyzing structure and composition and conducting quality control of mag-netron films.  Keywords: Small angle X-ray scattering, Atomic force, Scanning electron, Digital holographic microscopy, Thin magnetron films.   PACS number: 61.10.Eq   1. INTRODUCTION  Thin-film materials that feature unique physico-chemical properties, which are due in large part to di-mensional effects and phenomena, find very broad ap-plication in both nanomaterial science and micro- and nanoelectronics that are being developed most inten-sively [1], including development of sensor devices, magnetic data carriers, protecting coatings, etc. Study of structural features of such entities presents a pro-found scientific problem. Transmission electron micros-copy (TEM), as a rule, does not provide validity of ob-tained data any more. In this connection, small-angle X-ray scattering (SAXS) technique, which does not cause secondary effects due to X rays, can be success-fully applied for studying the regularities of growth of thin-film materials, and the influence of their synthesis parameters on the structure and properties. The chief merit of this technique is that only this method, in fact, makes it possible to obtain statistical values of size, volume, surface area and forms of nanoparticles of sub-stance. Unlike granulometric analysis, SAXS excludes the influence of human factors [2].  2. EXPERIMENTAL SECTION  Magnetron iron films were evaporated with facility GENCO onto substrates from pyroceramics the size of 40  60 mm, which provided high surface uniformity of films. Working pressure of argon in a chamber was 1 Pa. Power of plasma discharge was not greater than 400 W. These parameters of the facility are significantly distinct from those given in [3]. Topology of film surface and determination of an average size of the granular structure was investigated with scanning probe micro-scope (SPM) SmartSPM (AIST NT). Morphological fea-tures and changes in surface structure of materials studied were investigated with scanning electron micro-scope (SEM) (JEOL JSM-6610LV) with a magnification of up to 100000x at an accelerating voltage of 20 kV. Morphology of film surface was also studied with digital holographic microscope (Lyncee tec) with a height measuring accuracy of 0.1 nm. Studies with SAXS were conducted with the help of facility SAXSessmc2 (Anton Paar) in the linear collima-tion mode, which makes it possible to characterize structural features of objects with the size of 0.1 to 100 nm. To this end a typical X-ray tube was used with copper anticathode and a monochromator with X-ray radiation of 0.154 nm K line.   3. RESULTS AND DISCUSSION  Typical scattering curve according to SAXS is given in a logarithmic scale in Fig. 1.    Fig. 1 – SAXS curve of a magnetron iron film at the substrate from pyroceramics (logarithmic scale)  Figure 2 shows SEM-image of an iron film with characteristic sizes of nanodimensional objects. It is seen some surface disorder when structures in both evapora-tion plane and as usual perpendicular to it are observed [3-5] with the formation of columnar nano crystallites. Disorder of thin-film structure is attested by its profile along the line of 350 m length obtained with holograph-ic microscope according to which the maximum height difference was 26.24 nm with an average roughness of not greater than 3.5 nm.  The shape observed was of two types: elongated in the substrate plane and regular of a circle form, which was probably the tip of a columnar nanocrystal structure  A.S. CHEKADANOV, A.P. KUZMENKO, ET AL., J. NANO- ELECTRON. PHYS. 6, 03023 (2014)   03023-2 perpendicular to the substrate surface. Granulometric analysis of AFM-images revealed that coatings studied had clearly polydisperse structures (Fig. 2b). The given particles had sizes varied within broad ranges from sev-eral tens to several hundredths of nm, among which prominent are formations of a cylindrical shape (up to 360 nm) composed from individual likely disk-like blocks of order 20 nm. It should be noted that sizes obtained with AFM-images are, as a rule, laterally overestimated due to spherical form of a cantilever probe (R  15 nm). Real-world size form (Fig. 2) can be reduced by 30 %.      Fig. 2 – Electron-microscopic and atomic-force image of the iron film  As was noted, for studying disperse systems in such thin magnetron layers SAXS can be utilized. However, unlike the situation shown in [6] it is excluded in our case. Moreover, as AFM- and SEM-data reveal film magnetron layers on substrates from pyroceramics were formed from polydisperse nanoparticles and their agglomerates as columnar nano crystallites. Processing of SAXS data (Fig. 1) was made with the program GIFT (PCG Software Package), which made it possible to compute the volume size distribution of par-ticles DV(r) (Fig. 3) in analogy with [7]. The average sizes of particles forming the magnetron films were found to be 6, 22, and 114 nm. Evaluation of normal-ized number of various-size nanoparticles determined from the ration of their areas under their distribution reveals that particles with a radius of 11 nm take the large part of the volume in the film studied. Compari-son of these sizes with data found with microscopic techniques suggests correspondence. The validity of this approach stems from the follow-ing considerations. It is obviously that for monodis-perse film there is a maximum size of nanoparticles that is determined from the distance distribution curve p(r) . The curve is computed from intensity of SAXS with the program of indirect Fourier transformation       maxminexp2sin12ss ssrp r I s dssr  .   The length of the scattering vector – s (the vector equal to the difference between the vectors of scattered and incident waves) is determined from:   04 sin2 sin  s k ,   where 2 is the, Iexp is experimentally observed intensi-ty, and r is the distance between two scattering elec-trons. Whereas for polydisperse system one can deter-mine the function of volume size nanoparticle distribu-tion from the integral equation:          maxmin20RVRI s D R m R i sR dR     Here Rmin, Rmax and R are maximum and minimum sizes and the particle size, i0(x) and m(R) are form-factor of particle (the particle shape is set a priory) and its volume. In computing V(R) the value Rmin is taken equal to zero and the quantity Rmax is chosen individu-ally for each specific case by the most appropriate fit-ting. The function DV(R) may be thought of as appro-priate if it does not provide negative spikes and ap-proaches zero at a maximum value of R without a sharp fall-off, i.e. the computed scattering intensity curve coincides with the curve from experiment.    Fig. 3 – Volume size distribution of particles in iron magnetron film at the substrate from pyroceramics  4. CONCLUSIONS  The given inference is also corroborated by similar studies with copper magnetron films when the formation of columnar nano crystallites is observed with aspect  SMALL ANGLE X-RAY SCATTERING IN THIN IRON FILMS J. NANO- ELECTRON. PHYS. 6, 03023 (2014)   03023-3 ratio L  l / d, whose value with characteristic magni-tudes of diameter (d) and length (l) is 15-20. Such mag-netron films also feature developed morphology; include columnar nanoparticles, which are oriented both per-pendicular to the substrate and situated in its plane. This dictates polydispersity of those coatings and makes its analysis and examination difficult. In this connection, SAXS technique may be thought of as nondestructive technique for analyzing structure and composition and conducting quality control of magnetron films.   REFERENCES  1. R.P. Seisyan, Tech. Phys. 56 No 8, 1061 (2011). 2. A.P. Kuzmenko, A.S. Chekadanov, E.Yu. Orlov, Nanothech-nika No 4(36), 41 (2013). 3. S.N. Saltykov, A.N. Kharin, A.M. Khoviv, Kondensiro-vannye sredy I mezhfaznye granitsy 11, No 2, 147 (2009) [in Russian]. 4. K. Nowakowska-Langier, K. Zdunek, R. Chodun, R. Nietubyc, R. Mirowski, J. Witkowski, Problems of atomic science and technology. Series: Plasma Physics 16, No 6, 159 (2010) [in Russian]. 5. A.P. Kuzmenko, V.G. Zavodinsky, А.Е. Kuzko, D.I. Timakov, S.V. Nokolenko, S.A. Pyachin, M.A. Pugachevsky, Izvestiya YuZGU. Physics and chemistry serie 1, 37 (2011) [in Rus-sian]. 6. Y. Ito, K. Omote, J. Harada, International Centre for Dif-fraction Data, Advances in X-ray Analysis 46, 56 (2003). 7. A.P. Kuzmenko, A.S. Chekadanov, S.V. Zakhvalinsky, E.A. Pilyuk, M.B. Dobromyslov, J. Nano-Electron. Phys. 5 No 4, 04025 (2013).   

https://essuir.sumdu.edu.ua/bitstream/123456789/36258/1/Small%20Angle%20X-ray%20Scattering%20in%20Thin%20Iron%20Films.pdf

Small Angle X-ray Scattering in Thin Iron Films

Abstract

Similar works

Full text

Available Versions

SocioEconomic Challenges Journal (Sumy State University)

Electronic Sumy State University Institutional Repository