In situ investigation of gold nanoclusters growth in polymer matrices
Polytetrafluoroethylene (PTFE) and polyparaphenylene sulphide (PPS) films were filled with gold (Au) nano-clusters by co-deposition in a vacuum. Multi-component film, filled simultaneously with Au and dye was deposited for the first time. Film formation was studied using optical absorption Плівки по...
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| Опубліковано в: : | Реєстрація, зберігання і обробка даних |
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| Дата: | 2004 |
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Інститут проблем реєстрації інформації НАН України
2004
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| Цитувати: | In situ investigation of gold nanoclusters growth in polymer matrices / K.P. Grytsenko, D.O. Grynko, M.V. Sopinskyy, S. Schrader // Реєстрація, зберігання і оброб. даних. — 2004. — Т. 6, № 1. — С. 3-11. — Бібліогр.: 25 назв. — англ. |
Репозитарії
Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860233052410609664 |
|---|---|
| author | Grytsenko, K.P Grynko, D.O. Sopinskyy, M.V. Schrader, S. |
| author_facet | Grytsenko, K.P Grynko, D.O. Sopinskyy, M.V. Schrader, S. |
| citation_txt | In situ investigation of gold nanoclusters growth in polymer matrices / K.P. Grytsenko, D.O. Grynko, M.V. Sopinskyy, S. Schrader // Реєстрація, зберігання і оброб. даних. — 2004. — Т. 6, № 1. — С. 3-11. — Бібліогр.: 25 назв. — англ. |
| collection | DSpace DC |
| container_title | Реєстрація, зберігання і обробка даних |
| description | Polytetrafluoroethylene (PTFE) and polyparaphenylene sulphide (PPS) films were filled with gold (Au) nano-clusters by co-deposition in a vacuum. Multi-component film, filled simultaneously with Au and dye was deposited for the first time. Film formation was studied using optical absorption
Плівки політетрафторетилену та поліпарафеніленсульфіду було наповнено нанокластерами золота та барвника методом сумісного випаровування в вакуумі. Формування плівок було досліджено, застосовуючи оптичну спектроскопію. Було знайдено значні перетворення оптичних спектрів у процесі росту плівок, які пов’язані з ростом кластерів золота та їх агрегатів. Обробка пари плазмою у процесі нанесення плівок призвела до формування менших, але більш агрегованих кластерів золота. В трикомпонентних плівках нанокластери золота виявили сферичну форму.
Пленки политетрафторетилена и полипарафениленсульфида были наполнены нанокластерами золота и красителя методом совместного испарения в вакууме. Формирование пленок было исследовано, используя оптическую спектроскопию. Были найдены значительные преобразования оптических спектров в процессе роста пленок, связанные с ростом кластеров золота и их агрегатов. Обработка пара плазмой в процессе нанесения пленок привела к формированию меньших, но более агрегированных кластеров золота. В трехкомпонентных пленках нанокластеры золота проявили сферическую форму.
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| first_indexed | 2025-12-07T18:22:05Z |
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Фізичні основи, принципи і методи
реєстрації даних
ISSN 1560-9189 Реєстрація, зберігання і обробка даних, 2004, Т. 6, № 4 3
UDC 681.327
K. P. Grytsenko1,2, D. O. Grynko1, M. V. Sopinskyy1, S. Schrader2
1 V.E. Lashkaryov Institute of Semiconductor Physics
45 Nauky pr., 03650 Kyiv, Ukraine
2 Institut fur Plasma/Laser/Optronic der TFH Wildau, Bahnhofstrabe,
15745, Wildau, Germany
In situ investigation of gold nanoclusters
growth in polymer matrices
Polytetrafluoroethylene (PTFE) and polyparaphenylene sulphide (PPS)
films were filled with gold (Au) nano-clusters by co-deposition in a vacuum.
Multi-component film, filled simultaneously with Au and dye was deposited
for the first time. Film formation was studied using optical absorption spec-
troscopy in situ. Electron microscopy and ellipsometry were used for film
characterisation. Au nano-cluster diameter is in 2–8 nm range in PTFE ma-
trix. At the film growth beginning small clusters with plasmon band about
480 nm were grown, than aggregation of clusters began, which made plas-
mon band shift to 520–550 nm, which is dependent on Au concentration.
Treatment with plasma led to formation of smaller, but aggregated Au clus-
ters. Ellipsometry showed that the part of clusters are elongated and stands
perpendicular to substrate. If PPS was used as a matrix, the growth kinetics
revealed two stepped mechanism. At the film growth beginning Au clusters
with plasmon band about 600 nm were formed, but with film thickness
growth intensity of band at 420 nm grows faster. The resulting film has most
strong band at 420 nm. But plasma treatment led to formation of Au aggre-
gates confined with PPS matrix with plasmon band at 620 nm.
Key words: nanocluster, gold, PTFE, PPS, optical spectra, plasma, plas-
mon.
Introduction
Metal nanoclusters are studied for applications in sensors [1, 2], photonics devices
and plasmonic structures [3], waveguides [4], films for photovoltaics [5], optical re-
cording of information [6–13], including high density near-field optical recording [14].
Several methods were used for deposition of metal-filled polymer film from a gas
phase. Methods include: magnetron sputtering of gold target in C2F3Cl [15, 16] or mix-
ture of CH4 and Ar gaseous media [17], co-sputtering of Econol and Au targets [18],
© K. P. Grytsenko, D. O. Grynko, M. V. Sopinskyy, S. Schrader
K. P. Grytsenko, D. O. Grynko, M. V. Sopinskyy, S. Schrader
4
vacuum co-deposition of metal and polymers, in particular, Au and PTFE [8] or ion co-
sputtering of these materials [19, 20]. Novel method to produce metal-containing poly-
mer film is the plasma enhanced chemical vapor deposition (PECVD) using organome-
tal precursors [9–14]. Te and Se compounds were used for composite film deposition by
PECVD, including the mixture of their diethyls. Later Sn, Sb and Pd filled composite
films were produced and the possibility of optical recording of information on these
films was shown.
The aim of this work is to research the growth kinetics and structure of the film ob-
tained by Au and polymer co-evaporation in a vacuum.
Experimental details
Films were deposited using VUP-5M installation equipped with computerised con-
trol system. Starting pressure in the chamber was 10–3 Pa. Control system assigns neces-
sary heating regimes for Au, dye and polymer evaporators. Data from quartz thickness
monitors with 6·10–8 kg/m2 sensitivity, chamber pressure, boat currents and tempera-
tures are displaying at computer screen. Rotating glass disc with attached Si, NaCl and
quartz slides were used as substrates. Spectrometer Polytec with optical fibres, intro-
duced through quartz window, was recording absorption spectra of film, growing on
rotating disc. Spectra were displayed at computer screen in situ. Spectra were recorded
using one beam scheme. Polymer films were deposited by two methods: 1 — thermal
evaporation for PPS, 2 — PTFE evaporation with vapor activation by electron cloud.
Polymer vapors can be additionally treated by 40,68 MHz 20–70 W plasma. Fig. 1 pre-
sents the scheme of the installation used for film deposition. Boat and electronic control
channel for the third component are not shown.
Fig. 1. Scheme of the deposition installation: 1 — vacuum chamber; 2 — substrates; 3 — system and 4
— motor for substrate rotation; 5 — shutter; 6 — evaporator-activator for polymer; 7 — evaporator for
metal; 8 — RF electrodes; 9 — quartz crystals; 10 — fibres; 11, 15, 16, 17 — controllers of quartz
monitors, motor, polymer and metal evaporators; 12 — RF generator; 13 — computer; 14 — optical
absorption spectrometer Polytec; 18 — digital-to-analogue and analogue-to-digital converters
In situ investigation of gold nanoclusters growth in polymer matrices
ISSN 1560-9189 Реєстрація, зберігання і обробка даних, 2004, Т. 6, № 4 5
Absorption spectra of the deposited films were recorded by Perkin-Elmer Lambda
16 spectrometer. Optical properties of films were studied by multiple angle ellipsometry
at 632 nm wavelength. Film thickness was controlled by ellipsometry and by atomic
force microscopy (AFM) on step. Both isotropic and anisotropic models were used for
ellipsometry calculations. Film structure was studied by transmission electron micro-
scope (TEM) JEM-100EX.
Results and discussion
Fig. 2 shows evolution of absorption spectra of Au-PTFE films, grown both with
and without plasma treatment. In Table 1 are summarised experimental data for Au-
filled PTFE films. Ellipsometry data presented in the Table 1 are obtained using iso-
tropic model.
Fig. 2. Evolution of absorption spectra of Au–
filled PTFE films, recorded during their growth:
Au12 and Au42 deposited without plasma treat-
ment, Au18– deposited with plasma treatment
For the film, containing 12 vol. % of Au and deposited without plasma treatment,
absorption band monotonously is shifting with film thickness growth from 480 nm to
520 nm. Plasmon band for the film deposited with 20 % of Au exhibits more sharp shift
K. P. Grytsenko, D. O. Grynko, M. V. Sopinskyy, S. Schrader
6
to certain film thickness — about 25 nm and further no changes. The behavior of plas-
mon band for the film containing 10 vol. % of Au and deposited with plasma treatment
is like the latter one. The shift of plasmon band can be caused by Au clusters aggrega-
tion.
Table 1. Preparation and characterization of Au-filled PTFE films
Deposition
parameters
Thickness,
nm
n k Au, vol. %
Average clus-
ter diameter,
nm
No
I, mA V, kV RF, W by
AFM
by ellipsometry quartz
moni-
tor
calculated
by
TEM
PTFE–2 7 1,2 0 – 212 1,36 0,003 0 – – –
PTFE–4 8 1,2 40 – 261 1,37 0,000 0 – – –
Au–12 3 1,2 0 56,7 57 1,78 0,078 12 10,8 5,4 4,5
Au–14 3,5 1,2 40 – 51 1,79 0,070 10 – – 4
Au–15 4,5 2,0 40 – 61 1,46 0,037 7 – – 5,5
Au–17 7 1,8 0 40 37 1,68 0,071 5 – – 3,5
Au–18 8 2,2 40 74 60 1,61 0,12 10 8,6 1,9 6,5
Au–42 7 2,0 0 60 60 1,80 0,228 20 21 5,5 4,4
Au-PTFE film parameters, calculated in the frame of isotropic and one-axis anisot-
ropic model, are shown in the Table 2. Comparison of data obtained using both iso-
tropic and uniaxial anisotropic models showed that the last one yields better approxima-
tion of experimental ellipsometric parameters and better correlation of film thickness
values, obtained by ellipsometry and AFM. As can be seen from Table 2, degree and
sign of birefringence and dichroism is dependent on thickness of the film and deposition
conditions.
Table 2. Properties of Au-filled PTFE films calculated by isotropic and uniaxial anisotropic models
using ellipsometry data
No h, nm n k no ne – no ko ke – ko
Au–12 57 1,78 0,078 1,803 –0,029 0,064 –0,01
Au–14 51–53 1,80 0,070 1,73 +0,050 0,15 –0,0075
Au–15 61–63 1,46 0,037 1,384 +0,0495 0,030 +0,028
Au–17 40–41 1,56 0,105 1,52 +0,097 0,66 -0,25
Au–18 74 1,61 0,12 1,605 +0,053 0,183 –0,072
Au–42 60 1,89 0,144 1,80 +0,057 0,228 –0,128
Fig. 3 presents TEM images of all Au-filled polymer films. Normal law describes
distribution of cluster size in the Au-PTFE film deposited without plasma. Cluster size
is in 2–8 nm range. Distribution of Au clusters in PTFE in film deposited with plasma
treatment are more wide. Smaller clusters were grown. But TEM image also revealed
aggregates up to 13 nm diameter made from these small clusters.
In situ investigation of gold nanoclusters growth in polymer matrices
ISSN 1560-9189 Реєстрація, зберігання і обробка даних, 2004, Т. 6, № 4 7
1 2
3 4 5
6 7
8 9 10
Fig. 3. TEM images of the Au-filled polymer films: 1 — Au12; 2 — Au18; 6 and 7 — their electron
diffraction patterns; 3 — thermal evaporation of PPS; 4 — thermal evaporation of PPS with plasma
treatment; 8 and 9 — their electron diffraction patterns; 5 and 10 — CoPc-Au-PTFE film.
Magnification: 500 000
K. P. Grytsenko, D. O. Grynko, M. V. Sopinskyy, S. Schrader
8
Au clusters have also been characterised using ellipsometry data. Maxwell-Garnett
theory was used for calculations [24]. Au clusters were considered as nanocrystals em-
bedded in PTFE matrix. The quasi-classical approximation [25] was used for the calcu-
lations of the dielectric constant as a function of the Au nanocrystals size. Volume frac-
tion of the Au clusters calculated using this approach is close to the value obtained with
quartz monitor. For the film deposited without plasma treatment calculated diameter of
Au clusters is close to average size obtained by TEM. For the film deposited with
plasma treatment calculated diameter of Au clusters is close to the minimal size ob-
tained by TEM. This points out to the aggregation of Au clusters in the film deposited
with plasma.
The difference in the film structure can be caused by: 1 — plasma can charge Au
clusters, which can lead to their repelling; 2 — more chemically active CxFy species fix
Au nuclei, increasing nuclei quantity but preventing their growth; 3 — cross-linked
PTFE matrix resists Au diffusion and suppresses cluster growth; 4 — due to 2 and 3, the
next layer of Au clusters is more favourable to grow onto already formed Au clusters.
Fig. 4 shows absorption spectra of Au-PPS films deposited with and without
plasma treatment. Spectra show different mechanism of formation of film, grown with-
out plasma treatment. At the film growth beginning plasmon band at 560 nm appeared.
At initial stage of film thickness increase this band is shifted to 575 nm. This is evi-
dence of formation of large Au clusters or aggregates. But with film thickness further
growth the relative intensity of the band 425 nm increases more rapidly, than intensity
of the band 575 nm. Final film spectrum has wide band at about 430 nm, but this can be
the superposition of 580 nm and new 420 nm bands. Chemical reaction of Au with S
can be suggested. In this case the formation of compound with new absorption band is
possible. Film growth with plasma treatment revealed initial plasmon band at about 620
nm and no changes in its position during film thickness increase. This is true for all
films studied with 5-30 Au vol. % concentration.
a b
Fig. 4. Evolution of absorption spectra of Au-PPS films: a — deposited without plasma treatment filled
with 18 % Au; b — deposited with plasma treatment filled with: 1 — 20, and 2 — 15 Au (vol. %)
In situ investigation of gold nanoclusters growth in polymer matrices
ISSN 1560-9189 Реєстрація, зберігання і обробка даних, 2004, Т. 6, № 4 9
TEM images showed large differences in the film structure (Fig. 3, 3,4). Film de-
posited without plasma is almost disordered mixture, while film deposited with plasma
contained large Au cluster aggregates clearly divided one from other by polymer matrix.
Electron diffraction patterns showed that in the former case film structure is far from the
Au cluster structure in PTFE matrix (Fig. 3, 7,8). For the latter film Au cluster structure
is almost the same as in PTFE matrix. The average diameter of Au clusters in PPS ma-
trix is smaller (3 nm and 5,5 nm) than in PTFE matrix for both cases.
This can be explained in the following way: in the first case Au-S interaction is
strong enough. So diffusion and cluster growth were suppressed. Au-S compound can
be formed. In the second case plasma treatment makes organic species more active,
therefore their interaction between them is stronger than with Au. But in the latter case
plasma also can lead to decomposition of monomer to smaller species, so resulted de-
posit is less like original PPS than if film was deposited without plasma treatment. In
both cases interaction of Au clusters with PPS decomposition products and matrix is
stronger than interaction with PTFE ones, so cluster growth is suppressed more
strongly.
Recently multi-component organic systems with Au nanoclusters attracted atten-
tion for various applications [4, 5]. But all these systems were deposited from solutions.
We deposited three-component dye-Au-PTFE film in a vacuum for the first time. Fig. 5
presents evolution of absorption spectrum during CoPc-Au-PTFE film growth. Film
composition Au:CoPc:PTFE (vol. %) is 6:44:50.
Fig. 5. Evolution of CoPc-Au-PTFE film spectrum
Spectrum represents superposition of Au plasmon band at 520 nm and CoPc ab-
sorption at 430, 610 and 670 nm. But 430 nm band of pure CoPc film is shifted to 420
nm in three-component film, intensity of 610 nm is weaker. The former effect may be
caused by the contribution of small Au cluster absorption in the 420 nm region. The lat-
ter one can be due to that the Au clusters prevent CoPc aggregation and crystallisation,
resulting in formation less organised CoPc clusters.
K. P. Grytsenko, D. O. Grynko, M. V. Sopinskyy, S. Schrader
10
TEM investigations showed Au clusters about 2–7 nm diameter, rarely distributed
in a matrix (Fig. 3,5) and only several aggregates. Most of clusters have perfect round
shape. The distribution of CoPc and PTFE phases may be not resolved due to their al-
most equal density. At least no large aggregates or crystals were formed. This is caused
by the fact that the each phase prevents the growth of another one. Electron diffraction
pattern shows weak point reflexes (Fig. 3,10). This points to formation of crystallites
with preferential orientation.
In summary we can make the conclusion that the use of optical spectroscopy in situ
for film growth studies allows to discover transformations with film thickness increase.
These investigations have to help to understand mechanism of the structure formation in
multi-component composite system.
Conclusions
1. PTFE and PPS films filled with Au nanoclusters were deposited by co-
evaporation in a vacuum.
2. Both PTFE and PPS based films showed nonlinear changes of optical spectrum
during film growth.
3. Treatment of vapor by RF discharge led to aggregation but of more small Au
clusters in the matrix.
4. Ellipsometry data showed that the films have anisotropy in optical properties,
especially for films deposited with plasma.
5. Three-component dye-Au-PTFE film was deposited in a vacuum. Au clusters
have round shape.
Acknowledgments
Deposition equipment was made in the frame of STCU Project 2348. Thanks to
DAAD for granting of Polytec spectrometer system. Thanks to Mr. A. Kotko for TEM
images.
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Received 15.11.2004.
Introduction
Experimental details
Results and discussion
Conclusions
Acknowledgments
|
| id | nasplib_isofts_kiev_ua-123456789-50698 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1560-9189 |
| language | English |
| last_indexed | 2025-12-07T18:22:05Z |
| publishDate | 2004 |
| publisher | Інститут проблем реєстрації інформації НАН України |
| record_format | dspace |
| spelling | Grytsenko, K.P Grynko, D.O. Sopinskyy, M.V. Schrader, S. 2013-10-28T18:59:41Z 2013-10-28T18:59:41Z 2004 In situ investigation of gold nanoclusters growth in polymer matrices / K.P. Grytsenko, D.O. Grynko, M.V. Sopinskyy, S. Schrader // Реєстрація, зберігання і оброб. даних. — 2004. — Т. 6, № 1. — С. 3-11. — Бібліогр.: 25 назв. — англ. 1560-9189 https://nasplib.isofts.kiev.ua/handle/123456789/50698 681.327 Polytetrafluoroethylene (PTFE) and polyparaphenylene sulphide (PPS) films were filled with gold (Au) nano-clusters by co-deposition in a vacuum. Multi-component film, filled simultaneously with Au and dye was deposited for the first time. Film formation was studied using optical absorption Плівки політетрафторетилену та поліпарафеніленсульфіду було наповнено нанокластерами золота та барвника методом сумісного випаровування в вакуумі. Формування плівок було досліджено, застосовуючи оптичну спектроскопію. Було знайдено значні перетворення оптичних спектрів у процесі росту плівок, які пов’язані з ростом кластерів золота та їх агрегатів. Обробка пари плазмою у процесі нанесення плівок призвела до формування менших, але більш агрегованих кластерів золота. В трикомпонентних плівках нанокластери золота виявили сферичну форму. Пленки политетрафторетилена и полипарафениленсульфида были наполнены нанокластерами золота и красителя методом совместного испарения в вакууме. Формирование пленок было исследовано, используя оптическую спектроскопию. Были найдены значительные преобразования оптических спектров в процессе роста пленок, связанные с ростом кластеров золота и их агрегатов. Обработка пара плазмой в процессе нанесения пленок привела к формированию меньших, но более агрегированных кластеров золота. В трехкомпонентных пленках нанокластеры золота проявили сферическую форму. Deposition equipment was made in the frame of STCU Project 2348. Thanks to DAAD for granting of Polytec spectrometer system. Thanks to Mr. A. Kotko for TEM images. en Інститут проблем реєстрації інформації НАН України Реєстрація, зберігання і обробка даних Фізичні основи, принципи та методи реєстрації даних In situ investigation of gold nanoclusters growth in polymer matrices In situ дослідження вирощування нанокластерів золота в полімерних матрицях In situ исследование выращивания нанокластеров золота в полимерных матрицах Article published earlier |
| spellingShingle | In situ investigation of gold nanoclusters growth in polymer matrices Grytsenko, K.P Grynko, D.O. Sopinskyy, M.V. Schrader, S. Фізичні основи, принципи та методи реєстрації даних |
| title | In situ investigation of gold nanoclusters growth in polymer matrices |
| title_alt | In situ дослідження вирощування нанокластерів золота в полімерних матрицях In situ исследование выращивания нанокластеров золота в полимерных матрицах |
| title_full | In situ investigation of gold nanoclusters growth in polymer matrices |
| title_fullStr | In situ investigation of gold nanoclusters growth in polymer matrices |
| title_full_unstemmed | In situ investigation of gold nanoclusters growth in polymer matrices |
| title_short | In situ investigation of gold nanoclusters growth in polymer matrices |
| title_sort | in situ investigation of gold nanoclusters growth in polymer matrices |
| topic | Фізичні основи, принципи та методи реєстрації даних |
| topic_facet | Фізичні основи, принципи та методи реєстрації даних |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/50698 |
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