Technische Universität Chemnitz, Center for ...Preparation of aspheric copper nanoparticles Scheme...
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Preparation of aspheric copper nanoparticles Scheme 1: Synthesis of copper nanoparticles by thermolysis of copper(I) carboxylate 1 [7]. • Preparation of copper nanoparticles by thermal decomposition of compound 1 in 1-hexadecylamine (precursor concentration: 10 mM, ϑ = 330 °C, t = 10 min) Figure 1: TEM images of aspheric copper nanoparticles. Figure 2: Particle size distribution from TEM of aspheric copper nanoparticles. 0-20 20-40 40-60 60-80 80-100 100-120 120-140 140-160 160-180 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 Frequency [%] d [nm] Preparation of gold nanoparticles Scheme 4: Synthesis of gold nanoparticles by thermolysis of copper(I) carboxylate 1 in the presence of HAuCl 4 . • Preparation of gold nanoparticles by thermal decomposition of compound 1 in 1-hexadecylamine in the presence of HAuCl 4 (precursor and Au 3+ concentration: 10 mM, ϑ = 330 °C, t = 10 min) Figure 4: TEM images (left, center) and electron diffraction pattern (right) of gold nanoparticles. Figure 5: Particle size distribution from TEM of gold nanoparticles. Synthesis concepts for metal nanoparticles in different shapes and their pyrene-supported linkage to SWCNTs A. Kossmann 1 , D. Adner 1 , S. Schulze 1 , T. Blaudeck 2 , S. Hermann 2 , C. Tegenkamp 1 , S. E. Schulz 2,3 and H. Lang 1 1 Technische Universität Chemnitz, Faculty of Natural Sciences, Chemnitz, Germany 2 Technische Universität Chemnitz, Center for Microtechnologies (ZfM), Chemnitz, Germany 3 Fraunhofer Institute for Electronic Nano Systems (ENAS), Chemnitz, Germany Motivation Metal nanoparticles attached to carbon-based nanostructured materials enable new applications in electrochemical energy storage (e.g. fuel cells) [1] as well as chemical detection [1,2,3] and optical sensing [2,3,4]. Requirements for electronic sensors are appropriate and versatile nanoelectronic transducers, the design of which can comprise the modification of the channel material of a nanoelectronic field-effect transistor, e.g. made from semiconducting single-walled carbon nanotubes (s-SWCNTs). In the ideal case, this component can be functionalized with nanoscopic building blocks in a modular manner that allows a selective response and tuning of the sensitivity. Field-effect transistors (FETs) using individualized SWCNTs have been proposed for this case as FET channel material with special properties regarding sensitivity and selectivity of resulting sensor devices [5,6]. Recently, we presented a scalable on-chip functionalization approach for SWCNTs between palladium electrodes in the geometry of a field-effect transistor with preformed gold nanoparticles [5]. This method is wafer-level compatible and comprises two stages of flow chemistry. In a new chemical approach, we are using pyrenylalkylthioates as linker molecules for non covalent functionalization of SWCNTs with metal nanoparticles which also enable debundling of CNT agglomerates. Summary • Preparation of aspheric copper nanoparticles by thermal decomposition of copper(I) carboxylates → Different shape (spheres, triangles, hexagons and ellipses) & size (19 to 162 nm size) • Template supported synthesis of gold nanoparticles by thermal decomposition of copper(I) carboxylates in the presence of HAuCl 4 → Different shape (spheres, triangles and ellipses) & size (13 to 75 nm size) • Pyrene derivatives with long alkyl chains and terminal thioacetate functionalization can be used for linkage of nanoparticles to CNTs by π-π-stacking and also enable debundling of CNT agglomerates. References [1] I. Capek, Adv. Colloid Interface Sci. 2009, 150, 63–89. [2] K. Yoshimura, C. Langhammer, B. Dam, Mat. Res. Soc. Bull. 2013, 38, 495–503. [3] R. D. Rodriguez, T. Blaudeck, J. Kalbacova, E. Sheremet, S. Schulze, D. Adner, S. Hermann, M. Hietschold, H. Lang, S. E. Schulz, D. R. T. Zahn, RSC Adv. 2016, 6, 15753–15758. [4] C.J. Zhou, S. Wang, J.L. Sun, N. Wie, L.-J. Yang, Z.Y. Zhang, J.H. Liao, L.-M. Peng, Appl. Phys. Lett. 2013, 102, 1031021–1031025. [5] T. Blaudeck, D. Adner, S. Hermann, H. Lang, T. Gessner, S. E. Schulz, Microelectron. Eng. 2015, 137, 135–140. [6] S. Mubeen, T. Zhang, B.Y. Yoo, M.A. Deshusses, N.V. Myung, J. Phys. Chem. C 2007, 111, 6321–6327. [7] D. Adner, M. Korb, S. Schulze, M. Hietschold, H. Lang, Chem. Commun. 2013, 49, 6855–6857. Linkage to CNTs Scheme 2: Synthesis protocol for the preparation of functionalized pyrene derivative 2. Scheme 3: Representation of linkage between the pyrene derivative and CNTs by π-π-stacking. Figure 3: UV-Vis-NIR spectrum of pyrene derivative 2 and SWCNTs. Acknowledgments We thank Viraj Madhiwala for UV-Vis-NIR measurements and we gratefully acknowledge generous financial support from the Deutsche Forschungsmemeinschaft (FOR 1713 SMINT). 0-10 10-20 20-30 30-40 40-50 50-60 60-70 70-80 80-90 90-100 0 2 4 6 8 10 12 14 16 18 20 22 24 Frequency [%] d [nm] d min = 13 nm d max = 75 nm d avg = 42 ± 15 nm d min = 019 nm d max = 162 nm d avg = 61 ± 28 nm
Transcript of Technische Universität Chemnitz, Center for ...Preparation of aspheric copper nanoparticles Scheme...
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Preparation of aspheric copper nanoparticles
Scheme 1: Synthesis of copper nanoparticles by thermolysis of copper(I) carboxylate 1 [7].
• Preparation of copper nanoparticles by thermal decomposition of compound 1 in
1-hexadecylamine (precursor concentration: 10 mM, ϑ = 330 °C, t = 10 min)
Figure 1: TEM images of aspheric copper nanoparticles.
Figure 2: Particle size distribution from TEM of aspheric copper nanoparticles.
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Preparation of gold nanoparticles
Scheme 4: Synthesis of gold nanoparticles by thermolysis of copper(I) carboxylate 1 in the
presence of HAuCl4.
• Preparation of gold nanoparticles by thermal decomposition of compound 1 in
1-hexadecylamine in the presence of HAuCl4 (precursor and Au3+ concentration: 10 mM,
ϑ = 330 °C, t = 10 min)
Figure 4: TEM images (left, center) and electron diffraction pattern (right) of gold
nanoparticles.
Figure 5: Particle size distribution from TEM of gold nanoparticles.
Synthesis concepts for metal nanoparticles in different
shapes and their pyrene-supported linkage to SWCNTsA. Kossmann1, D. Adner1, S. Schulze1, T. Blaudeck2, S. Hermann2,
C. Tegenkamp1, S. E. Schulz2,3 and H. Lang1
1Technische Universität Chemnitz, Faculty of Natural Sciences, Chemnitz, Germany2Technische Universität Chemnitz, Center for Microtechnologies (ZfM), Chemnitz, Germany
3Fraunhofer Institute for Electronic Nano Systems (ENAS), Chemnitz, Germany
MotivationMetal nanoparticles attached to carbon-based nanostructured materials enable new
applications in electrochemical energy storage (e.g. fuel cells) [1] as well as chemical
detection [1,2,3] and optical sensing [2,3,4]. Requirements for electronic sensors are
appropriate and versatile nanoelectronic transducers, the design of which can comprise
the modification of the channel material of a nanoelectronic field-effect transistor, e.g.
made from semiconducting single-walled carbon nanotubes (s-SWCNTs). In the ideal
case, this component can be functionalized with nanoscopic building blocks in a modular
manner that allows a selective response and tuning of the sensitivity. Field-effect
transistors (FETs) using individualized SWCNTs have been proposed for this case as FET
channel material with special properties regarding sensitivity and selectivity of resulting
sensor devices [5,6].
Recently, we presented a scalable on-chip functionalization approach for SWCNTs
between palladium electrodes in the geometry of a field-effect transistor with preformed
gold nanoparticles [5]. This method is wafer-level compatible and comprises two stages of
flow chemistry. In a new chemical approach, we are using pyrenylalkylthioates as linker
molecules for non covalent functionalization of SWCNTs with metal nanoparticles which
also enable debundling of CNT agglomerates.
Summary
• Preparation of aspheric copper nanoparticles by thermal decomposition of
copper(I) carboxylates
→ Different shape (spheres, triangles, hexagons and ellipses) & size (19 to
162 nm size)
• Template supported synthesis of gold nanoparticles by thermal decomposition
of copper(I) carboxylates in the presence of HAuCl4→ Different shape (spheres, triangles and ellipses) & size (13 to 75 nm size)
• Pyrene derivatives with long alkyl chains and terminal thioacetate
functionalization can be used for linkage of nanoparticles to CNTs by
π-π-stacking and also enable debundling of CNT agglomerates.
References [1] I. Capek, Adv. Colloid Interface Sci. 2009, 150, 63–89. [2] K. Yoshimura, C. Langhammer, B. Dam, Mat. Res. Soc. Bull. 2013, 38, 495–503. [3] R. D. Rodriguez, T. Blaudeck,
J. Kalbacova, E. Sheremet, S. Schulze, D. Adner, S. Hermann, M. Hietschold, H. Lang, S. E. Schulz, D. R. T. Zahn, RSC Adv. 2016, 6, 15753–15758. [4] C.J. Zhou, S. Wang, J.L. Sun,
N. Wie, L.-J. Yang, Z.Y. Zhang, J.H. Liao, L.-M. Peng, Appl. Phys. Lett. 2013, 102, 1031021–1031025. [5] T. Blaudeck, D. Adner, S. Hermann, H. Lang, T. Gessner, S. E. Schulz,
Microelectron. Eng. 2015, 137, 135–140. [6] S. Mubeen, T. Zhang, B.Y. Yoo, M.A. Deshusses, N.V. Myung, J. Phys. Chem. C 2007, 111, 6321–6327. [7] D. Adner, M. Korb, S. Schulze,
M. Hietschold, H. Lang, Chem. Commun. 2013, 49, 6855–6857.
Linkage to CNTs
Scheme 2: Synthesis protocol for the preparation of functionalized pyrene derivative 2.
Scheme 3: Representation of linkage
between the pyrene derivative and
CNTs by π-π-stacking.
Figure 3: UV-Vis-NIR spectrum of
pyrene derivative 2 and SWCNTs.
Acknowledgments
We thank Viraj Madhiwala for UV-Vis-NIR measurements and we gratefully acknowledge
generous financial support from the Deutsche Forschungsmemeinschaft (FOR 1713
SMINT).
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dmin = 13 nm
dmax = 75 nm
davg = 42 ± 15 nm
dmin = 019 nm
dmax = 162 nm
davg = 61 ± 28 nm
