Russian Journal of Applied Chemistry, 2013, Vol. 86, No. 6, pp. 928−932.
Pleiades Publishing, Ltd., 2013.
Original Russian Text © E.A. Venediktov, E.P. Rozhkova, 2013, published in Zhurnal Prikladnoi Khimii, 2013, Vol. 86, No. 6, pp. 987−991.
AND POLYMERIC MATERIALS
Kinetic Relationships of Metal Filling
of Epoxy Resin by in Situ Reduction of Silver Nitrate
E. A. Venediktov and E. P. Rozhkova
Institute of Solution Chemistry, Russian Academy of Sciences, Ivanovo, Russia
Received December 18, 2012
Abstract—The kinetics of metal ﬁ lling of ED-20 epoxy oligomer by its action on AgNO
in the temperature
interval 50–90°С was studied.
Silver-ﬁ lled epoxy resins are used as heat- and elec-
tricity-conducting materials and as functional polymeric
coatings in electrical engineering, electronics, and other
ﬁ elds [1–9].
Metal ﬁ lling of epoxy resins is performed by vacuum
sputtering of metals , dispersion of their particles
[3, 8], implantation of high-energy metal ions ,
thermolysis , and reduction of metal compounds in
the presence of organic or inorganiс reductants . It
was shown  that epoxy resin can be ﬁ lled with silver
particles by its action on silver nitrate.
In this study we examined the kinetic relationships of
ﬁ lling of ED-20 epoxy oligomer with silver nanoparticles
by in situ reduction of silver nitrate.
We used ED-20 commercial epoxy–4,4'-isoprop-
ylidenediphenol oligomer and AgNO
prepared by the
procedure described in .
Synthesis of silver particles was combined with spec-
trophotometric monitoring of their formation. Synthesis
of metal particles was performed in a square glass cell
1 cm thick and 2 cm high, arranged in the temperature-
controlled holder of the cell compartment of a Specord
M-40 double-beam spectrophotometer. The temperature
was maintained with an accuracy of ±1°C. To perform
the synthesis, 11 mg of ﬁ nely divided AgNO
on the cell bottom, and 1.5 ml of the epoxy oligomer
preheated to the required temperature was slowly poured
into the cell without stirring. After deﬁ nite time intervals,
the optical density of the resin in the range 400–700 nm
was measured using as reference the pure epoxy oligomer
at the same temperature. Because the reaction system
remains heterophase up to the end of the reaction, the
weighed portion of the salt was chosen so as not to pre-
vent the light transmission through the oligomer. Also,
because of the heterophase character of the process, the
epoxy oligomer over the salt was stirred for a short time
prior to measurements to ensure equal concentration of
silver nanoparticles throughout the height and volume
of the cell.
The size of the forming metal particles was exam-
ined by dynamic light scattering with a Zetasizer Nano
ZS Malvern instrument (excitation wavelength 633 nm,
detection angle 173°) in square glass cells 1 cm thick.
The averaged diameter was determined from the results
of three measurements at the sample thermostating time
of 90, 120, and 150 min.
Action of the hot epoxy oligomer on solid AgNO
results in bright yellow coloration of the oligomer. Visual
examination shows that the process starts at the phase
boundary and develops in the radial-frontal direction
throughout the height and volume of the solution. In
addition, a characteristic metal mirror ﬁ lm is formed on
the walls of the glass reactor near the phase boundary.