Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn
By modification of the highly dispersed silica surface with amino complexes of silver, copper and zinc from aqueous solution with further heat treatment, silica nanocomposites containing surface compounds of silver, copper and zinc were synthesized. The concentration of the silver in the samples was...
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Інститут хімії поверхні ім. О.О. Чуйка НАН України
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| Цитувати: | Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn / V.M. Bogatyrov, M.V. Galaburda, O.M. Zaichenko, K.S. Tsyganenko, Ya.I. Savchuk // Поверхность. — 2015. — Вип. 7 (22). — С. 119-125. — Бібліогр.: 34 назв. — англ. |
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irk-123456789-1484822019-02-19T01:25:54Z Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn Bogatyrov, V.M. Galaburda, M.V. Zaichenko, O.M. Tsyganenko, K.S. Savchuk, Ya.I. Физико-химия поверхностных явлений By modification of the highly dispersed silica surface with amino complexes of silver, copper and zinc from aqueous solution with further heat treatment, silica nanocomposites containing surface compounds of silver, copper and zinc were synthesized. The concentration of the silver in the samples was 1-2 wt%, and the copper and zinc - 1-5 wt%. Biocidal activity of the composites was tested against 18 different strains of micromycetes, phytopathogenic bacteria and algae. It was shown, that the highest efficiency is observed in the samples of silica modified with silver/copper and silver/zinc. Модифицированием поверхности высокодисперсного кремнезема амино-комплексами серебра, меди и цинка из водного раствора с последующей термообработкой, синтезированы кремнеземные нанокомпозиты, содержащие поверхностные соединения серебра, меди и цинка. Концентрация серебра в образцах составляла 1–2 %, а меди и цинка – 1–5 %. Биоцидная активность полученных композитов была изучена по отношению к 18 различным штаммам микромицетов, фитопатогенных бактерий и водорослей. Установлено, что наибольшая эффективность наблюдается в образцах кремнезема, модифицированного серебром/медью, а также серебром/цинком. Модифікуванням поверхні високодисперсного кремнезему аміно-комплексами срібла, міді та цинку з водного розчину з наступною термообробкою, синтезовано кремнеземні нанокомпозити, що містять поверхневі сполуки срібла, міді та цинку. Концентрація срібла в зразках становила 1–2 %, а міді та цинку – 1–5 %. Біоцидну активність одержаних композитів вивчали по відношенню до 18 різних штамів мікроміцетів, фітопатогенних бактерій і водоростей. Встановлено, що найбільша ефективність спостерігається в зразках кремнезему, модифікованого сріблом/міддю, а також сріблом/цинком. 2015 Article Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn / V.M. Bogatyrov, M.V. Galaburda, O.M. Zaichenko, K.S. Tsyganenko, Ya.I. Savchuk // Поверхность. — 2015. — Вип. 7 (22). — С. 119-125. — Бібліогр.: 34 назв. — англ. 2617-5975 http://dspace.nbuv.gov.ua/handle/123456789/148482 544.72+615.28 en Поверхность Інститут хімії поверхні ім. О.О. Чуйка НАН України |
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Физико-химия поверхностных явлений Физико-химия поверхностных явлений |
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Физико-химия поверхностных явлений Физико-химия поверхностных явлений Bogatyrov, V.M. Galaburda, M.V. Zaichenko, O.M. Tsyganenko, K.S. Savchuk, Ya.I. Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn Поверхность |
| description |
By modification of the highly dispersed silica surface with amino complexes of silver, copper and zinc from aqueous solution with further heat treatment, silica nanocomposites containing surface compounds of silver, copper and zinc were synthesized. The concentration of the silver in the samples was 1-2 wt%, and the copper and zinc - 1-5 wt%. Biocidal activity of the composites was tested against 18 different strains of micromycetes, phytopathogenic bacteria and algae. It was shown, that the highest efficiency is observed in the samples of silica modified with silver/copper and silver/zinc. |
| format |
Article |
| author |
Bogatyrov, V.M. Galaburda, M.V. Zaichenko, O.M. Tsyganenko, K.S. Savchuk, Ya.I. |
| author_facet |
Bogatyrov, V.M. Galaburda, M.V. Zaichenko, O.M. Tsyganenko, K.S. Savchuk, Ya.I. |
| author_sort |
Bogatyrov, V.M. |
| title |
Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn |
| title_short |
Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn |
| title_full |
Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn |
| title_fullStr |
Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn |
| title_full_unstemmed |
Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn |
| title_sort |
biocidal activity of the precipitated silica with surface compounds of ag, cu and zn |
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Інститут хімії поверхні ім. О.О. Чуйка НАН України |
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2015 |
| topic_facet |
Физико-химия поверхностных явлений |
| url |
http://dspace.nbuv.gov.ua/handle/123456789/148482 |
| citation_txt |
Biocidal activity of the precipitated silica with surface compounds of Ag, Cu and Zn / V.M. Bogatyrov, M.V. Galaburda, O.M. Zaichenko, K.S. Tsyganenko, Ya.I. Savchuk // Поверхность. — 2015. — Вип. 7 (22). — С. 119-125. — Бібліогр.: 34 назв. — англ. |
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Поверхность |
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2025-07-12T18:49:32Z |
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2025-07-12T18:49:32Z |
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1837468146129174528 |
| fulltext |
Поверхность. 2015. Вып. 7(22). С. 119–125 119
UDC 544.72+615.28
BIOCIDAL ACTIVITY OF THE PRECIPITATED SILICA
WITH SURFACE COMPOUNDS OF Ag, Cu AND Zn
V.M. Bogatyrov1, M.V. Galaburda1, O.M. Zaichenko2, K.S. Tsyganenko2,
Ya.I. Savchuk2
1Chuiko Institute of Surface Chemistry, National Academy of Sciences of Ukraine,
17 General Naumov Str., Kyiv 03164, Ukraine, e-mail: vbogat@ukr.net
2Zabolotny Institute of Microbiology and Virology, National Academy of Sciences of Ukraine,
154 Acad. Zabolotnoho Str., Kyiv 03143, Ukraine
By modification of the highly dispersed silica surface with amino complexes of silver, copper
and zinc from aqueous solution with further heat treatment, silica nanocomposites containing surface
compounds of silver, copper and zinc were synthesized. The concentration of the silver in the samples
was 1-2 wt%, and the copper and zinc - 1-5 wt%. Biocidal activity of the composites was tested
against 18 different strains of micromycetes, phytopathogenic bacteria and algae. It was shown, that
the highest efficiency is observed in the samples of silica modified with silver/copper and silver/zinc.
Introduction
It is known that microorganisms have both positive and negative effects on the
environment. In particular, there are many causative agents of many diseases in warm-
blooded animals and plants, species with toxigenic properties and corrosion activity in
different materials and buildings. A malignant bacteria causes significant damages to the
human health and therefore to the economics in general. The main tools to combat the
harmful actions of microorganisms are antibiotic compounds and chemical agents, including
composites those which contains silver, copper, zinc and etc. The biocidal activity of copper,
zinc and silver was well known even in ancient times. New directions in study of those
composites have appeared due to recent developments in the nanotechnology, which caused
an interest in investigation of the bioactivity of the metal and oxides nanoparticles for there
use in industry, biotechnology and medicine [1-9].
Special attention is paid to creation of new advanced materials and coatings, resistant
to the biodeteriorations or with biocidal activity against the microorganisms. In this regard, an
interesting approach is to utilize silica materials (silica gels, zeolites, aerogels, microspheres
and etc.) as substrate for bioactive nanoparticles deposition. The bioactivity of metallic silver
nanoparticles in various materials was widely studied; furthermore, the possibilities of
transformation of the silver nanoparticles into the oxide form on the silica surface and
influence of this process on the biocidal activities have been reported [10-16]. The
antimicrobial effect of the silica matrix modified with nanoparticles of metals or ions of
silver, copper, zinc has been reported [17-22]. Such materials can be used as the bioactive
adsorbent alone as well as a part of polymer composites and textile fabrics with biocide
properties.
Various methods of chemical modification of silica surface with silver, copper and
zinc, were previously reported. However, majority of the traditional methods are multi-stage
and involves the silver salt reduction to the zero valence state; formation of stabilized sol and
precipitating of the obtained nanoparticles in the pores or on the silica surface [23-25]. The
possibility of chemical modification of the silica surface with ammine complexes of silver,
copper and zinc is extremely perspective to obtain bioactive nanocomposites [26-32]. In case
of the fumed silica, this method is simple enough to obtain the composite powder with
nanoscale content of the biocidal metals.
120
The aim of this work was to synthesize a highly dispersed solid of the precipitated
silica modified with silver, copper and zinc, and to study their bioactive properties against the
wide range of microorganisms (micromycetes, algae and bacteria).
Materials and methods
Precipitated silica NewSil-125 (China), silver nitrate AgNO3 (GOST 1277-75, 99.7%),
copper acetate monohydrate Cu(Ac)2·H2O (GOST 5852-70, 98%), zinc acetate tetrahydrate
Zn(Ac)2·4H2O (GOST 5823-78 97%), and aqueous solution of ammonia 25%
(Chemlaborreaktiv Ltd, Ukraine) were used to prepare modified silica. All chemicals were
used without further purification.
Ammonia complexes of the metal salts were prepared by dissolving of metal salts in
distilled water with further addition of the ammonia solution. Initially, the metal hydroxides
precipitate, but with further addition of ammonia the insoluble hydroxide transforms into the
transparent solution of metal-ammine complex i.e. silver diammine, copper tetraammine and
zinc tetraammine complexes [30, 33].
Utilizing metal-ammine complexes to prepare the silica-based biocide composites
allows modification of the precipitated silica with two metals at the same time. In this case,
ammonia was added into solution of the two salts in distilled water until transparent solution
of metal-ammine complexes was formed.
In a typical preparation of the modified silica the ammonia complex of metal was
added to 3g of the precipitated silica under stirring at the room temperature in order to obtain
a homogeneous suspension. Then the suspension was aged for 0.5 h and placed into the
thermostatic oven at 200 °C for 2 hours to evaporate ammonia and to dry the sample.
The ratio of the initial components in the synthesis and the calculated content of the
metal content in the samples are given in Table 1.
Table 1. Composition and reagent consumption for the modification of 3 g of precipitated
silica*.
Sample Initial salt Salt
content,
mg
Water,
ml
Aqueous
solution of
ammonia,
ml
Metal
content,
wt%
№2 AgNO3 50 9 1 1
№3 AgNO3 100 9 1 2
№4 Cu(Ac)2·H2O 600 8 3 5
№5 Zn(Ac)2·4H2O 130 10 1 1
№6 Zn(Ac)2·4H2O 660 7 4 5
№7 AgNO3/Cu(Ac)2·H2O 100/120 10 1.5 2/1
№8 AgNO3/Zn(Ac)2·4H2O 100/130 10 1.8 2/1
№9 Cu(Ac)2·H2O/Zn(Ac)2·4H2O 120/130 8.5 1.5 1/1
*Sample №1 is the initial precipitated silica
NewSil-125 is a white powder with silica content over 98% and values of specific
surface area is about 110-140 m2/g. Surface silanol groups of the silica react with amino
complexes of the metals in the aqueous solution via ion exchange reaction with the formation
of the surface metal amino compounds. A thermal treatment at 200 °C leads to evaporation of
ammonia and the subsequent cooling in the ambient condition forms the hydroxo-complexes
or chemisorbed molecules of metal hydroxide on the silica surface [30-32]. Obtained samples
of silica modified with silver, copper and zinc were tested for biocidal activity against
micromycetes of phytopathogenic bacteria and algae. The pristine precipitated silica was used
as a blank test (sample №1).
121
In this research 12 cultures of microscopic funguses (8 of them with corrosion activity
(Penicillium funiculosum 16721, P. chrysogenum 16719, P. aurantiogriseum 16244,
Aspergillus terreus 16184, A. niger 73001, Aspergillus oryzae 16718, Paecilomyces variotii
16724 and Trichoderma viride16516) and 4 with toxic activity (P. urticae 811, Fusarium
oxysporum 220, Myrothecium verrucaria 324 and Stachybotrys chartarum 526)) were used to
test the biocidal properties of synthesized composites. Stachybotrys chartarum 526 is known
as the initiator of the so-called "sick building syndrome" appearance [34]. Along with this,
three strains of pathogenic bacteria and three strains of green algae were tested too. The
cultures of microscopic funguses and phytopathogenic bacteria are from Ukrainian Collection
of Microorganisms (UCM), and cultures of green algae are from National Herbarium of
Ukraine (NHU).
Biocidal activity was determined by the wells method in Petri dishes using appropriate
agar medium at 26 ± 1 °C. Test cultures were introduced into the molten broth (≈40°С) in
amounts of ×106, 1×106 and 1×102 cells/ml, for fungi, green algae and phytopathogenic
bacteria, respectively.
Nanocomposites (10 mg of the powder) were placed in holes on the agar surface in
Petri dish. All experiments were performed under sterile conditions and in triplicate. The
biocidal efficacy was assessed by measuring of the diameter of the zones of inhibition of
culture growth (bright zone) and expressed in mm as the average for three experiments (Table
2 and 3).
Results and discussion
According to the obtained data (Table 2), the highest inhibition effect on the
micromycetes growth has a silver/copper and silver/zinc nanocomposites (samples №№ 2, 3,
7, 8). It should be noted that nanocomposites with high concentration of zinc (sample № 6)
shows the selective activity against toxigenic strains of P. urticae 811 and M. verrucaria 324.
Moreover, those samples act equally according to the corrosion-active and to the toxigenic
strains. Slightly greater sensitivity in the investigated micromycetes was established for
Penicillium and Aspergillus. High sensitivity of Penicillium and Trichoderma strains as to
copper (sample №4) and zinc (sample№6) must be noted too.
Table 2. Antifungal activity of silica nanocomposites containing surface compounds of silver,
copper and zinc (diameter of the zones of inhibition, mm)
Sample
P
en
ic
il
li
um
fu
ni
cu
lo
su
m
1
67
21
P
. c
hr
ys
o-
ge
nu
m
1
67
19
P
. a
ur
an
ti
o-
gr
is
eu
m
1
62
44
A
sp
er
gi
ll
us
te
rr
eu
s
16
18
4
A
. n
ig
er
7
30
01
A
. o
ry
za
e
16
71
8
P
ae
ci
lo
m
yc
es
v
ar
io
ti
i 1
67
24
T
ri
ch
od
er
m
a
vi
ri
de
1
65
16
P
en
ic
il
li
um
u
rt
ic
ae
8
11
F
us
ar
iu
m
ox
ys
po
ru
m
2
20
M
yr
ot
he
ci
um
v
er
ru
ca
ri
a
32
4
St
ac
hy
bo
tr
ys
c
ha
rt
ar
um
5
26
№1 (silica) 0 0 0 0 0 0 0 0 0 0 0 0
№2 30 22 32 18 22 15 16 20 36 18 16 31
№3 33 20 46 26 26 16 19 22 32 28 18 30
№4 15 0 20 0 0 0 0 16 35 24 0 21
№5 0 0 0 0 0 0 0 0 0 0 0 0
№6 20 0 0 0 0 0 0 0 30 0 23 0
№7 52 45 51 28 30 25 30 30 49 23 28 39
№8 30 25 32 22 23 19 20 26 42 25 26 28
№9 0 0 0 0 20 0 0 0 28 0 0 0
122
The improved biocidal activities of the mix-metal samples can be explained by differ
in biostatic action. In particular, if the silver composites are characterized by biocidal activity,
the others have static activity. It has to be noted that, the active agents together with the
suppression of fungal growth inhibited sporogenesis. Using silver together with copper or
zinc compounds in the sample synthesis increases the biocidal activity of the final silica
composites. All these characteristics of active composites can be utilized in prospective
protective agents by incorporating of such composite within the building element structure or
into the anticorrosion coating. It opens a way to depress the growth of the Stachybotrys
chartarum fungus and to protect the buildings from the so-called "sick building syndrome" by
treatment with active nanocomposites.
High activity of nanocomposites was shown against to phytopathogenic bacteria and
green algae (Table 3), which also gives an opportunity to use them to treat the agricultural
crops diseases. A green algae overgrowth of the structures and communications within the
buildings at high humidity also can be averted by the active nanocomposites application.
Table 3. Biocidal activity of silica nanocomposites containing surface compounds of silver,
copper and zinc (diameter of the zones of inhibition, mm).
Sample
P
ec
to
ba
ct
er
iu
m
ca
ro
to
vo
ru
m
8
63
6
P
se
ud
om
on
as
s
yr
in
ga
e
pv
.
s
yr
in
ga
e
85
23
A
gr
ob
ac
te
ri
um
tu
m
ef
ac
ie
ns
8
62
8
C
hl
or
el
la
v
ul
ga
ri
s
1
90
C
. v
ul
ga
ri
s
1
91
C
. k
es
sl
er
i 2
00
№1 (silica) 0 0 0 0 0 0
№2 55 25 33 34 29 24
№3 32 25 31 40 38 25
№4 19 34 20 29 28 23
№5 26 33 14 0 0 0
№6 0 0 22 29 31 27
№7 54 35 41 48 45 42
№8 47 29 34 54 44 53
№9 26 24 19 22 20 18
In prospective this work needs additional studies, in particular extending the range of
test cultures and in development of technology of the nanocomposites application.
Conclusions
A high biocidal efficiency of the precipitated silica modified with silver, copper and
zinc has been shown. An increase in the biocidal activity of the modified silica when silver is
combined with copper or zinc was discovered.
The resulting material can be used as filling compounds for organic and inorganic
polymer coatings of the building constructions imparting a high bio-resistance.
Acknowledgments
VMB and MVG are grateful to European Community, Seventh Framework
Programme (FP7/2007–2013), Marie Curie International Research Staff Exchange Scheme
(IRSES grant No 612484) for partial financial support of this project.
123
The authors are grateful to Zabolotny Institute of Microbiology and Virology NAS of
Ukraine to Department of Physiology and Taxonomy of micromycetes for presented cultures
of micromycetes from their collections of microscopic funguses, and to Department of
Phytopathogenic Bacteria for presented cultures of phytopathogenic bacteria. We express our
gratitude to Department of Phycoogy from M.G. Kholodny Institute of Botany NAS of Ukraine
for presented cultures of green algae.
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БИОЦИДНАЯ АКТИВНОСТЬ ОСАЖДЕННОГО КРЕМНЕЗЕМА С
ПОВЕРХНОСНЫМИ СОЕДИНЕНИЯМИ Ag, Cu И Zn
В.М. Богатырев1, М.В. Галабурда1, А.М. Зайченко2,
Е.С. Цыганенко2, Я.И. Савчук2
1Институт химии поверхности им. А.А. Чуйко Национальной академии наук Украины
ул. Генерала Наумова 17, Киев, 03164, Украина, e-mail: vbogat@ukr.net
2Институт микробиологии и вирусологии Национальной академии наук Украины
ул. Академика Заболотного154, Киев, 03143, Украина
Модифицированием поверхности высокодисперсного кремнезема амино-
комплексами серебра, меди и цинка из водного раствора с последующей
термообработкой, синтезированы кремнеземные нанокомпозиты, содержащие
поверхностные соединения серебра, меди и цинка. Концентрация серебра в образцах
составляла 1–2 %, а меди и цинка – 1–5 %. Биоцидная активность полученных
композитов была изучена по отношению к 18 различным штаммам микромицетов,
фитопатогенных бактерий и водорослей. Установлено, что наибольшая
эффективность наблюдается в образцах кремнезема, модифицированного
серебром/медью, а также серебром/цинком.
БІОЦИДНА АКТИВНІСТЬ ОСАДЖЕНОГО КРЕМНЕЗЕМУ З ПОВЕРХНЕВИМИ
СПОЛУКАМИ Ag, Cu ТА Zn
В.М. Богатирьов1, М.В. Галабурда1, О.М. Зайченко2,
К.С. Циганенко2, Я.І. Савчук2
1Інститут хімії поверхні ім. О.О. Чуйка Національної академії наук України
вул. Генерала Наумова 17, Київ, 03164, Україна, e-mail: vbogat@ukr.net
2Інституту мікробіології і вірусології Національної академії наук України
вул. Академіка Заболотного 154, Київ, 03143, Україна
Модифікуванням поверхні високодисперсного кремнезему аміно-комплексами
срібла, міді та цинку з водного розчину з наступною термообробкою, синтезовано
кремнеземні нанокомпозити, що містять поверхневі сполуки срібла, міді та цинку.
Концентрація срібла в зразках становила 1–2 %, а міді та цинку – 1–5 %. Біоцидну
активність одержаних композитів вивчали по відношенню до 18 різних штамів
мікроміцетів, фітопатогенних бактерій і водоростей. Встановлено, що найбільша
ефективність спостерігається в зразках кремнезему, модифікованого сріблом/міддю, а
також сріблом/цинком.
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