ISSN 0027-1314, Moscow University Chemistry Bulletin, 2019, Vol. 74, No. 1, pp. 14–19. © Allerton Press, Inc.

, 2019.
Russian Text © N.N. Begletsova, O.A. Shinkarenko, E.I. Selifonova, O.Yu. Tsvetkova, A.J.K. Al-Alwani, A.M. Zakharevich, R.K. Chernova, E.G. Glukhovskoy, 2019, published
in Vestnik Moskovskogo Universiteta, Seriya 2: Khimiya, 2019, No. 1, pp. 19–26.

Synthesis of Copper Nanoparticles Using Hydrazine in Micellar

Solutions of Sodium Dodecyl Sulfate
N. N. Begletsovaa, b, *, O. A. Shinkarenkoa, b, E. I. Selifonovab, O. Yu. Tsvetkovab,
A. J. K. Al-Alwania, c, A. M. Zakharevichb, R. K. Chernovab, d, and E. G. Glukhovskoya, b
aDepartment
of Nano- and Biomedical Technologies, Saratov State University, Saratov, Russia
b
Education and Research Institute of Nanostructures and Biosystems, Saratov State University, Saratov, Russia
c
Babylon University, Babylon, Iraq
d
Institute of Chemistry, Saratov State University, Saratov, Russia
*e-mail: [email protected]
Received December 12, 2017

Abstract⎯The influence of the synthesis conditions and composition of the reaction medium on the size and
morphology of copper nanoparticles is studied for the Cu(II)—N2H4–sodium dodecyl sulphate systems. In
accordance with scanning electron microscopy, the nanoparticles size varies in the range of 30 to 90 nm at
the average diameter of 40 to 45 nm and spherical shape of copper nanoparticles. The dimensions of copper
nanoparticles are evaluated to be up to 400 nm. As shown via the spectrophotometry, the stabilization of cop-
per dispersions resistant to oxidation, as well as their aggregation and sedimentation, occurs at Cu(II) : N2H4
molar ratios of 1 : 100; 1 : 200, and 1 : 300 in sodium dodecyl sulphate micellar solutions. A hypsochromic
shift of the surface plasmon resonance absorption band of copper is established to occur in the range of
574 nm–568 nm–564 nm with a change of the Cu(II) : N2H4 molar ratio.

Keywords: copper nanoparticles, chemical reduction, hydrazine, sodium dodecyl sulphate

DOI: 10.3103/S0027131419010024

In the past decades, there has been a breakthrough ble colloidal dispersions of copper NPs, chemical
in the field of fabrication and characterization of reduction is the most extensively used method due to
nanomaterials. In connection with this, the synthesis its simplicity, economical efficiency, and ability to
of metal nanoparticles (NPs) is one of the main topics control and vary the size and shape of the NPs. How-
of modern research. Significant attention is paid to the ever, it also contains some shortcomings, such as the
production of copper NPs due to their unique proper- broad size distribution of the NPs and the aggregative
ties, such as catalytic action and antibacterial activity, instability of NPs solutions.
as well as the capability to exhibit high levels of heat Copper NPs were obtained using a system com-
and electric conductivity together with a low cost, posed of an aqueous copper(II) chloride solution, рН
making them promising and widely used materials in regulator (complexing ammonium agent), and reduc-
the electrotechnical industry (nanocircuits [1], flexi- ing agent (hydrazine) in the presence of surfactant
ble electronics and printing [2], lubricants [3]), anti- micelles of sodium dodecyl sulfate (SDS). The forma-
bacterial agents in medicine [4], and catalysts in tion of copper NPs in the redox reactions is a complex
chemistry. The properties of nanomaterials are known process depending on many factors, such as ther
to depend to a large extent on the characteristics of the nature and concentration of the reducing agent, dis-
constituent particles, i.e., the size, morphology, oxida- solvent, рН, and temperature, as well as the presence
tion rate, and the ability to aggregate. In this respect, the and type of stabilizers.
synthesis of NPs must take into account the factors that Copper NPs produced by the reduction of cop-
affect the parameters mentioned above. per(II) salts with hydrazine are known to be unstable
Copper nanoparticles can be produced via various in water with a propensity toward oxidation, aggrega-
methods, such as thermal decomposition [5], laser tion, and sedimentation after 24 h. The measurements
ablation [6], chemical vapor deposition [7, 8], bio- were made at a Cu(II) : N2H4 molar ratio of 1 : 10. The
chemical synthesis (green synthesis) [9–11], chemical ammonium copper and hydrazine concentrations
reduction of copper from its salts [12–14], thermal were varied in the range of 1 to 20 and 10 to 200 mM,
and sonochemical reduction [15], and radiolysis [16]. respectively [17]. Copper NPs are formed after 3 h and
Among this variety of routes for the production of sta- their polydispersed solutions remain resilient for 24 h.

14
 SYNTHESIS OF COPPER NANOPARTICLES USING HYDRAZINE 15

As is well known, the phenomena given above can be 2+

Cu 2 + + NH3 ↔ [Cu(NH3 )] ,
prevented by stabilizing copper NPs by various agents
2+
+ 2NH3 ↔ [Cu(NH3 )2 ] ,
2+
(high-molecular weight compounds, non-ionic and Cu
cationic surfactants, and others). However, the influence 2+
(1)
of anionic surfactants and high hydrazine concentrations Cu 2 + + 3NH3 ↔ [Cu(NH3 )3 ] ,
2+
was not studied in these systems. Cu 2 + + 4NH3 ↔ [Cu(NH3 )4 ] .
The present work aims to elucidate the effects of The effect of reducing the agent concentration in
the pH and the molar ratio of copper(II) and reducing copper salts reduced by hydrazine was explored at
agent (hydrazine) in a micellar medium of the anionic molar ratios of Сu2+ : N2H4 equal to 1 : 10, 1 : 20, and
surfactants on the size and shape of the forming NPs, 1 : 40 [17]. It is worth mentioning that the impact of
as well as on the stability toward aggregation and sedi- large reducing agent concentrations was not investi-
mentation of the produced copper dispersions. gated earlier. Since they may be different for salts in
various environments, the following Cu(II) : N2H4
molar concentrations were taken in this study: 1 : 10,
REAGENTS, FACILITIES, 1 : 100, 1 : 200, and 1 : 300. The concentration of the
AND CHARACTERIZATION METHODS surfactant solution was kept above the value of the
critical micelle concentration (CMC). The pH value
Reagents was adjusted to the required value by using NH3 · H2O
ammonium water.
Copper NPs solutions can be produced using sim-
ple Сu(II) salts as precursors, such as sulfates, nitrates,
and chlorides. In this study, the precursors were cop- Synthesis of Copper NPs
per(II) chloride [CuCl2 ⋅ 2H2O] (Mr = 171 g/mol), The first flask was filled with 0.136 g of CuCl2 ⋅ 2H2O
GOST (State Standard) 4167–74); sodium dodecyl and 20 mL of 0.01 M SDS, diluted with ammonium to
sulfate [СН3(СН2)11ОSO3Na] (Mr = 288.38 g/mol); achieve a pH value of 12 on obtaining an intense blue
hydrazine hydrate [N2H4 ⋅ H2O] (Mr = 50 g/mol) copper ammine solution. Other flasks contained 20 mL
(Vekton, GOST 19503–88, 100% aqueous solution) of 0.01 M SDS with successively added various vol-
and ammonia water [NH3 ⋅ H2O] UHP 25–5 (Vekton, umes of hydrazine hydrate (0.5; 5; 10 and 15 mL)
GOST 3760-79, 25% aqueous solution). None of the under constant stirring. Hence the molar ratios of
precursors were subjected to additional purification. Cu(II) : N2H4 were 1 : 10, 1 : 100, 1 : 200, and 1 : 300
The conductivity of distilled water (solvent) was 5 × were obtained. The dilution of hydrazine took place
10–6 S/cm. with the release of the heat and the solution remained
colorless. Mixing the two solutions (in the first and
second flasks) led to the color changing from dark blue
to light yellow. The obtained solution was heated to
Facilities 30°С and was continuously stirred for 1 h. During the
The surface morphology of copper-containing synthesis of the copper NPs, the solution gradually
changed color from light yellow to dark red (within
samples was examined on a TESCAN MIRA II LMU
30 min) and then became permanently brown (after 1 h).
scanning electron microscopy (SEM) in the secondary This color variation for the solution is typical for cop-
electron (SE) detection mode at an accelerating voltage per [10, 11].
of 30 kV and a pressure of P = 5.0–6.0 × 10–2 Pa in the
Before photometric measurements, the solutions
chamber. The surface plasmon resonance (SPR)
were diluted with distilled water in the same ratio (1 : 5)
absorption spectra of the solution with copper NPs because of their highly intense color.
products were recorded on a SHIMADZU UV-2550
spectrophotometer in the wavelength range of 500 to
750 nm. Solutions were stirred using an IKA RCT Preparation of the Solution for SEM Measurements
basic magnetic stirrer and centrifuged on an ELMI The scanning electron microscopy (SEM) analysis
СМ-70М facility. of solutions reveals that copper NPs cannot be visual-
ized due to the large amount of surfactants on the sub-
strate. In order to remove their excess, the obtained
The Procedure for Obtaining Copper NPs suspension was predecanted using the distilled water
solution. For this, 0.1 mL of distilled water was added
Solutions with copper NPs were obtained via the to 0.5 mL of the suspension in the Eppendorf-type test
chemical reduction of ammonium copper using hydra- tube; the solution was rinsed and then exposed to
zine in a 0.01 М aqueous solution. A precursor was the 15 min of centrifugation at 4000 rpm. The precipitated
complex copper salt—[Cu(NH3)4]2+—obtained in the copper NPs were applied to a silicon substrate and
excess of ammonium in accordance with reaction (1). heated to 100°С for 4 min.

MOSCOW UNIVERSITY CHEMISTRY BULLETIN Vol. 74 No. 1 2019

16 BEGLETSOVA et al.

RESULTS AND DISCUSSION 3

The effect of pH
Although hydrazine is known as a strong reducing

Absorbance, a.u.
1
agent, its redox potential depends to a large extent on the 2
рН value of the reactive medium [(Е°, V = –0.5(–1.15)
for рН of 3–14]. Besides the formation of copper NPs,
2
the reduction of copper(II) salts in the neutral pH
series leads to the emergence of dichlorohydrazine 1
cuprate(II) (2): 3
CuCl 2 + 2N2H4 + 2H2O
(2) 0
= [Cu(N2H4 )2Cl 2 ] ⋅ 2H2O(sediment). 500 600 700
Wavelength, nm
The reduction of copper(II) in an weak-alkaline
environment may cause the formation of Cu2О copper
oxide together with metallic copper (3): Fig. 1. UV–visible spectra of copper NPs solution at
([Cu(NH3)4]2+ : N2H4 molar ratio is 1 : 200); pH: 12 (1),
CuCl 2 + 4N2H4 + 2NH3 + H2O (3) 10 (2), 9 (3).
= Cu 2O + 3Cu + 2N2 + 2N2H5Cl + 2NH4Cl + 6HCl.
The reduction of ammonium copper in a strongly band to 564 nm (Fig. 2c). This circumstance means
alkaline medium yields the formation of copper NPs that hydrazine in the system is not only a reducing
and the release of nitrogen (4): agent but also interacts with copper NPs, affecting the
2CuCl 2 + 4NH3 + N2H4 = 2Cu + N2 + 4NH4Cl. (4) size of the forming particles. Furthermore, hydrazine
The influence of the alkalinity on the copper NP for- in the aqueous solution is present in the form of N2H5+
mation was studied at pH values of 9, 10, and 12 in a cop- and N2H62 + cations, and the negative charge of copper
per(II)—hydrazine—SDS system with [Cu(NH3)4]2+ : NPs makes their interplay with hydrazonium ions
N2H4 molar ratios of 1 : 10, 1 : 100, 1 : 200, and 1 : 300. probable. Meanwhile, the SEM images (Figs. 3a, 3b)
One example of these systems is given in Fig. 1. reveal the formation of polydispersed copper NPs
As follows from Fig. 1, the optimal pH value is (with sizes ranging from 30 to 80–90 nm), as well as
close to 12. The decreasing pH value leads to a similar the aggregates with dimensions up to 300–400 nm
decrease in the amount of NPs for systems with differ- after 3 days. It can appear that the fraction of copper
ent component ratios. NPs with sizes of 30 to 90 nm, forming at different
hydrazine contents in the reactive system, is not con-
The results coincide with the value of the redox stant; however, this fact invisible in the SEM images
potential of hydrazine, increase in an alkaline and necessitates other experimental facilities, e.g., a
medium, and are consistent with the data reported in Zetasizer Nano ZS particle size analyzer.
the literature. A further study was performed at the
optimal pH of 12.
The Influence of the Hydrazine Concentration
on the Stability of Copper NPs Dispersed
The Influence of the Hydrazine Concentration in SDS Solutions
on the Behavior of Copper NPs Forming in SDS solutions
A great deal of attention is being paid to the influ-
In accordance with a spectrophotometric study at ence of an excess of hydrazine on the aggregative sta-
Cu(II) : N2H4 molar ratios of 1 : 10, 1 : 100, 1 : 200, and bility of the dispersed copper NPs with time. Accord-
1 : 300 (and a constant SDS concentration of 0.01 M) in ing to a spectrophotometric analysis of the solutions
the wavelength range of λ = 500–750 nm, there are no obtained at [Cu(NH3)4]2+ : N2H4 molar ratios of 1 : 100,
copper NPs in the solution at a ratio of Сu (II) : N2H4 = 1 : 200, and 1 : 300 immediately after the synthesis of
1 : 10 because of a lack of the SPR absorption band copper NPs and then after 3 days, the absorption spec-
characteristic of copper NPs [18]. This testifies to the trum undergoes transformations with an increase of
fact that the amount of the reducing agent is inferior to the SPR band intensity (Figs. 2a–2c). This effect is
that of the precursor in this suspension. The spectrum due to the aggregation of the NPs with time and man-
at a Cu(II) : N2H4 ratio of 1 : 100 exhibits the SPR band ifests itself by the enhancing light scattering in the total
at a wavelength of 574 nm (Fig. 2a). The Cu(II) : N2H4 absorbance of the photometric solution. The exposure
ratio of 1 : 200 results in a hypsochromic shift in the of the solution for 11 days yields a successive decrease
SPR band to 568 nm (Fig. 2b). A further increase in in the absorbance of the solutions in the SPR spectra
the hydrazine concentration at a Cu(II) : N2H4 ratio of and a simultaneous increase in the sediment concen-
1 : 300 leads also to a hyprochromic shift of the SPR tration of the aggregated copper NPs. The process was

MOSCOW UNIVERSITY CHEMISTRY BULLETIN Vol. 74 No. 1 2019

 SYNTHESIS OF COPPER NANOPARTICLES USING HYDRAZINE 17

3 (a) (b)
574 3
2

Absorbance, a.u.

Absorbance, a.u.
2 2 2 568
1
1 1
1

0 0
500 600 700 500 600 700
Wavelength, nm Wavelength, nm
(c) 1.5

Absorbance, a.u.
3 1.0
564
2
Absorbance, a.u.

0.5
2
1
0
500 550 600 650 700 750
1 Wavelength, nm

0
500 600 700
Wavelength, nm

Fig. 2. UV–visible spectra of copper NPs solution recorded (1) immediately after experiments and (2) 3 days after synthesis
(pH of 12, [Cu(NH3)4]2+ and N2H4 molar ration is (a) 1 : 100; (b) 1 : 200; (c) 1 : 300).

(a) (b)

500 nm 500 nm

Fig. 3. SEM images of copper NPs (a) immediately after experiments and (b) within 3 days.

the slowest at a maximum hydrazine excess chloride in the previous case was 0.136 g) at a Cu(II) :
([Cu(NH3)4]2+ : N2H4 = 1 : 300). In this case, the SPR N2H4 molar ratio of 1 : 300. This enabled us to obtain
band is still observed even 11 days after the synthesis an emulsion which remained steady during 1 month
(insert in Fig. 2c). It is worth mentioning that the sta- (Fig. 4). The copper NPs aggregation was observed
bilization of copper NPs solutions depends on the within the next 2 months and was followed by the
excess hydrazine and also on the initial copper chlo- sedimentation of copper NPs that kept their dark
color light.
ride concentration. In this respect, a supplementary
study was performed in a similar system using 0.086 g The identical solution of copper NPs with copper
of a copper chloride sample (the weight of the copper nitrate (the salt sample weight was 0.1268 g) was also

MOSCOW UNIVERSITY CHEMISTRY BULLETIN Vol. 74 No. 1 2019

18 BEGLETSOVA et al.

2.0 of about 1.5–3.0 nm. The micellar number of aggrega-

tion for SDS in a spherical micelle is 60–70.
All measurements were made in the anionic surfac-
1.5 tant of SDS at the concentration of its micelle forma-
Absorbance, a.u.

570 tion. The micelles formed at these concentrations

1 exhibit a spherical shape (Fig. 5), whose external layer is
1.0 composed of negatively charged SO3− hydrophilic groups
2 3 and a hydrophobic core, including C12 hydrocarbon rad-
icals. The peculiar feature of these micelles is the pres-
0.5 ence of a shell of anti-ions, as shown in Fig. 5.
Micelles of the anionic surfactant metioned above
are electrically charged because of the dissociation of
0 polar sulfogroups. A large number of anti-ions (up to
500 600 700 80% or even more) are merged with a surface of this
Wavelength, nm micelle, forming a dense double electric layer (the
Fig. 4. UV–visible spectra of copper NPs solution at Stern layer) (Fig. 5). Other anti-ions compose a diffu-
[Cu(NH3)4]2+ : N2H4 molar ratio of 1 : 300; pH of 12; 0.01 M sive ion shell (the Gouy–Chapman layer). In accor-
SDS; m(СuCl2 ⋅ 2H2О) = 0.086 g ((1 and 2) 6 and 12 days dance with Stigter, the Stern layer on the micelle sur-
after synthesis; (3) 1 month after synthesis). face is on the order of 0.22 to 0.40 nm, which is com-
parable with the dimensions of polar SDS groups.
The lifetime of one-charge ions on the micelle sur-
obtained after more than 30 days at the same Cu(II) : face is 10–8 s and that of two-charge ones is 10–6 s (by
N2H4 molar ratio of 1 : 300 in a 0.01 M SDS. the example of SDS at I = 0). It is noticeable that the
These results illustrate that solutions stable to translated movements of anions on the ion micelle
aggregation can be produced within a month by the surface are almost an order of magnitude slower than
selection of the initial precursor concentrations at a in the aqueous solution. Anti-ions are associated with
high hydrazine content. a micelle due to the long-range electrostatic forces. At
the same time, the anti-ions remain hydrated. Most of
the hydrated anti-ions become cations. The surfactant
polar groups in the micelle are also always hydrated. In
The Role of Anionic Surfactant in the Studied System total, micelles of ion surfactants can be considered spe-
Sodium dodecyl sulfate represents the anionic sur- cific, coarse multicharge ions composed of 20–30 elec-
factant with hydrophilic sulfate groups and hydropho- tric charges [19].
bic hydrocarbon radicals composed of 12 carbon The complex copper ammoniates in the studied
atoms. The processes taking place in the studied sys- system, as well as hydrazine (5) and (6), are positively
tem in the presence of SDS micelles can be interpreted charged [20, 21]:
as follows. Spherical SDS micelles are compact for-
mations with a high degree of dispersion and a radius N2H4+ + H2O ↔ N2H5+ + OH− (pK = 6.5), (5)

Gouy–Chapman layer

Stern layer

Micelle core

1
2

Fig. 5. Schematic structure of SDS micelle in water: (1) SO3− ; (2) anti-ions [Cu(NH3)4]2+, N2H5+ .

MOSCOW UNIVERSITY CHEMISTRY BULLETIN Vol. 74 No. 1 2019

 SYNTHESIS OF COPPER NANOPARTICLES USING HYDRAZINE 19

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MOSCOW UNIVERSITY CHEMISTRY BULLETIN Vol. 74 No. 1 2019