Opt Quant Electron (2016) 48:490 DOI 10.1007/s11082-016-0758-9
Sensory properties of copper microstructures deposited from water-based solution upon laser irradiation at 532 nm Maxim S. Panov1 • Ilya I. Tumkin1 • Vasily S. Mironov1 Evgeniia M. Khairullina1 • Alexandra V. Smikhovskaia1 Sergey S. Ermakov1 • Vladimir A. Kochemirovsky1
• •
Received: 15 November 2015 / Accepted: 4 October 2016 Springer Science+Business Media New York 2016
Abstract The simple and cheap method for fabrication of micro-sized electrochemical electrodes was proposed. The porous copper microstructures synthesized by laser-induced metal deposition technique were used as an indicator electrode, whereas a bulk polycrystalline copper with similar geometric parameters was used as an etalon electrode. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. An analytical response of the fabricated copper electrode is 15 times higher than those observed for a pure bulk copper. A study of sensory characteristics for hydrogen peroxide and D-glucose detection showed that the value of Faraday current at the fabricated copper electrode is 2–2.5 orders of magnitude higher than for etalon one. Keywords Laser-induced deposition Copper Sensors Electrochemical electrodes Cyclic voltammetry Impedance spectroscopy
1 Introduction Laser-induced chemical liquid-phase deposition of metals (LCLD) is one of the promising and effective methods for patterning of the microelectronic devices. In LCLD metal reduction proceeds in local volume of solution within the laser beam focal point resulting
This article is part of the Topical Collection on Laser technologies and laser applications. Guest Edited by Jose´ Figueiredo, Jose´ Rodrigues, Nikolai A. Sobolev, Paulo Andre´ and Rui Guerra. & Maxim S. Panov
[email protected] 1
Saint Petersburg State University, 7/9 Universitetskaya nab., St. Petersburg 199034, Russia
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in the deposition of small-sized metal structures on the surface of dielectric substrate (Kochemirovsky et al. 2012, 2013, 2014; Tumkin et al. 2015). This approach is substantially simple, fast and precise. Many other similar techniques, for example, laser-induced chemical vapour deposition (LCVD), pulsed laser deposition (PLD) and laser-induced forward transfer (LIFT) have some serious disadvantages such as low adhesion of metal on dielectric surface, the presence of impurities, low deposition rate, complicity of the experimental setups, relatively low electrical conductivity of the obtained metal structures with respect to the pure bulk metal etc. In contrast, LCLD does not have these drawbacks and allows to produce porous metal structures (lines) with low electrical resistivity which is very close to those revealed by corresponding pure bulk metal (Panov et al. 2016). These structures, which have the developed surfaces and exhibit high electrical conductivity properties, can be applied for fabrication of extra small metallic conductors on dielectric surfaces without using photomask in contrast to photolithography (Kim and Choi 2013; Peng and Jiang 2012). The laser-induced deposition of series of metals was performed to date (Kordas et al. 2001; Shafeev 1993; Yokoyama et al. 1984). Here, copper attracts more attention among other metals due to its wide application in microelectronics; furthermore, copper deposited upon laser irradiation can be potentially used in fabrication of the nanoand micro-sized electrochemical sensors. It is known that electrochemical sensors are the most widely used group of devices, in which an analytical signal is provided by the electrochemical reaction that occurs in the near-electrode space. These sensors can be successfully used for qualitative and quantitative analysis of liquid and gaseous media (Clark 1956; Kordas et al. 2001; Updike and Hicks 1967). Electrochemical sensors are mainly used for determination of reactive (electroactive) substances, which can be electrochemically reduced or oxidized on an indicator electrode of the electrochemical cell where an analytic signal is generated (Kordas et al. 2001). Typically, the inert (platinum, palladium, gold, silver), chemically active (silicon, indium, tin) modified and ion selective electrodes are used as indicator electrodes. In turn, the liquid (aqueous solutions of potassium chloride, hydrogen sulfate and buffer solutions) and solid (zirconium oxide, aluminum oxide, hydrous antimony pentoxide) electrolytes as well as polyelectrolytes (Kordas et al. 2001) are used as background ones. The fabrication of electrochemical sensors based on nanomaterials has been intensively developing during last decade (Abad et al. 2009; Blaedel and Engstrom 1980; Jaraba et al. 1998; Miyamoto et al. 1991). Nanomaterials in electrochemical sensors can perform the functions of transducers, catalysts and signal labels. In all cases, the improvement of the catalytic, adsorption and electrochemical activity of these nano-sized structures compared to the corresponding bulk material is caused by the size effects and their individual properties (Barton et al. 2004). A special attention deserves the biosensors based on the use of electrodes modified with nanomaterials rather than electrodes, which use enzymes as sensory-active elements. Such modification results in facilitation of charge transfer, prevention of denaturation of enzymes on the surface of an electrode and increase of the electrode specific surface area. In this regard, the development of a new generation of electrochemical sensors based on nanomaterials is important for theoretical and experimental study of size effects as well as development of ideas allowing to predict properties of the fabricated sensors (Davis and Higson 2007). The analysis of the recently published articles reveals a great interest towards electrochemical sensors used for biomolecules detection and based on the nano-structured elements. According to our previous studies (Lozhkina et al. 2015; Kochemirovsky et al. 2015) the LCLD method allows to synthesize porous conductive micro-sized nano-structured electrodes, which can be applied for
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manufacturing of enzymeless biosensors with enhanced sensory activity, sensitivity and quick testing capabilities. Thus, the main aim of the current work is to obtain the conductive small-sized copper electrodes and study their sensory properties. In order to achieve this goal, we conducted the laser-induced synthesis of porous copper deposits using the LCLD technique and studied the sensory activity of these structures towards such well-known disease markers as glucose and hydrogen peroxide.
2 Experimental All chemicals used in this work were of analytical grade and purchased commercially (Sigma Aldrich). The detailed description of the experimental setup for the laser-induced copper deposition has been published elsewhere (Tver’yanovich et al. 2011). Briefly, the output from a continuous wave 532 nm diode-pumped solid-state Nd:YAG laser is split into two parts. The first part is focused on the boundary region between metal salt solution and dielectric substrate. Thus, the focused laser beam is moved along the substrate by the computer controlled motorized stage producing metal structures of given geometric sizes and shapes. The second one is sent to web-camera used for in situ monitoring and control of the laser-induced deposition process. As a result, laser-induced deposition of 1-cm-long copper lines from 0.5 mm thick solutions was performed at the laser power of 900 mW and the scanning speed of 2.5 lm s-1. Optical images of copper lines were obtained using an optical microscope with 409 magnification (MMN-2, LOMO). The topology of the deposited copper structures was observed by means of scanning electron microscopy (SEM). The atomic composition of these structures was studied using energy dispersion of X-ray spectroscopy (EDX). The EDX-system was coupled with a Zeiss Supra 40 VP scanning electron microscope equipped with X-ray attachment (Oxford Instruments INCA X-act). The quantitative and qualitative analysis of composition of the copper line surface was conducted using an Escalab 250Xi X-ray photoelectron spectrometer. The surface profile of the deposited copper structures was obtained using atomic force microscopy (AFM). The electrical conductivity properties of the deposited copper lines were studied with an impedance meter Z-2000 (Elins Co.) in the frequency band of 20 Hz to 2 MHz at the signal amplitude of 125 mV. The electrochemical properties of these structures were studied with an Autolab PGST 302 N Metrohm impedance meter. The measurements were carried out in a standard three-electrode cell using a platinum wire counter electrode, a Ag/AgCl reference electrode and an indicator electrode based on the deposited copper structures. The range of frequencies varied from 100 kHz to 1 MHz. The amplitude of the probe voltage was 1 mV and a constantly applied potential was 200 mV. The solution of 0.1 M H2SO4 used as a background electrolyte was argon purged to remove oxygen by bubbling argon through the solution for 45 min.The electrochemical properties of the obtained copper structures were also studied using a cyclic voltammetry (potentiostat, Elins P30I). The measurements were carried out in a standard three-electrode cell described above. The sweep speed of the potential was set at 50 mV s-1. The read speed was 50 points per second. The potential range was 8 V. The current sensitivity of the etalon copper and the fabricated copper electrodes was 10 and 1000 lA, respectively. The mixture of 0.1 M H2SO4, 0.1 M Na2SO4 (pH 9.8) and 0.1 M NaOH was used as a background solution. The D-glucose and hydrogen peroxide substrates were added to a background solution for the sensory activity studies.
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3 Results and discussion The composition of solutions used for laser-induced copper deposition is shown in Table 1. As a result, the copper lines of about a 100 lm wide, 6 lm thick and 1 cm long were produced using the LCLD technique. Figure 1 illustrates optical and SEM images of typical copper microstructures obtained in current work. Optical microscopy demonstrates that these deposits have a continuous structure with typical copper lustre and without any serious defects. In turn, a highly developed surface of these copper structures was observed by scanning electron microscopy. A study of the elemental composition of the deposited copper line using the EDX reveals that copper is the primary component. The electrical conductivity studies show that the deposited copper structures have very low level of electrical resistance. Thus, good topology and high electrical conductivity properties of the obtained copper deposits allow to use them in fabrication of micro-sized electrodes, which then can be checked on sensory properties.
Table 1 The composition of solutions used for laser-induced copper deposition Concentration, mM
pH
CuCl2
KNaC4H4O6 9 4H2O
NaOH
Reducing agent*
10
33
100
75
13
* Sorbitol, xylitol, glycerol, formaldehyde
Fig. 1 Optical microphotograph (a) and SEM images (b, c, d) of the copper structures produced by LCLD
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The cyclic voltammetry technique was applied to determine the effective electrochemical surface area of the fabricated copper electrode and a bulk polycrystalline copper with the same geometric parameters used as etalon electrode. The cyclic voltammograms (CV’s) obtained in 0.1 M H2SO4 (Fig. 2) show that the fabricated electrode exhibits much higher effective electrochemical surface area than those revealed by etalon electrode. In turn, the most effective surface area was revealed by the copper microstructures deposited from solution containing sorbitol used as reducing agent (Fig. 2). Therefore, here and after we discuss only results of the electrochemical studies on copper deposits obtained from sorbitol-containing solution. The sensitivity of these copper electrodes towards hydrogen peroxide was evaluated. Hydrogen peroxide is well-known as very effective substrate for testing electrodes including electrodes, which demonstrate even insignificant catalytic and sensory properties. Figures 3 and 4 illustrate the cyclic voltammograms obtained in the background solution and mixture of the background solution with substrate (hydrogen peroxide), respectively. These CV’s reveal changes in the magnitude of background currents depending on the square of the effective surface area as well as appearance of hydrogen peroxide peak at -240 mV. Figure 5 demonstrates the dependences of value of Faraday current (hydrogen current) on hydrogen peroxide concentration. These dependences have a linear character, i.e. the trend of the effective surface area-sensory properties is kept. This observation is consistent with recently published work on a study of sensory properties of an electrode based on nickel nano-sheets (Liu et al. 2015). Another widely used substrate for studying the sensory properties is D-glucose. Therefore, we also studied the sensory activity of copper electrode obtained in LCLD experiments towards this substrate. Figures 6 and 7 present CV’s of the fabricated and etalon electrodes recorded in the presence of different concentration of D-glucose. It was found that CV’s for the fabricated copper electrode exhibit the increase of the peak corresponding to oxidation of glucose. Here, as in the case of hydrogen peroxide, the dependence of Faraday current of oxidation reaction on concentration of D-glucose has a linear character; however, for the etalon electrode this dependence is quasi-parabolic. This behavior can be explained by diffusion difficulties
Fig. 2 The cyclic voltammograms of copper structures deposited from solutions containing various reducing agents and a pure bulk copper (etalon) recorded in 0.1 M H2SO4
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Fig. 3 The cyclic voltammograms of copper structures deposited from solutions containing various reducing agents and a pure bulk copper (etalon) recorded in the background solution (0.1 M Na2SO4)
Fig. 4 The cyclic voltammograms of copper structures deposited from solutions containing various reducing agents and a pure bulk copper (etalon) recorded in the mixture of the background solution (0.1 M Na2SO4) with hydrogen peroxide
experienced by the substrate when reaching the active sites at which oxidation occurs. On the other hand, the dependence exhibited by the etalon electrode suggests that the accessibility of the catalytic centers is higher but their number is significantly lower. Thus, the substrates consisting of large molecules aggregate in aqueous solution causing difficulties for diffusion inside the pores of the electrode. In order to support this idea the deposited copper structures were studied using X-ray photoelectron spectroscopy and atomic force microscopy. AFM experiment (Fig. 8) shows high roughness and heterogeneity of these copper structures (the fabricated electrode), which is considered to be a main reason of sensory properties. Photoelectron spectroscopy (Fig. 9; Table 2) reveals a significant
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LCLD (sorbitol) etalon LCLD (xylitol) LCLD (formaldehyde) LCLD (glycerol)
300 250
Current,µA
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200 150 100 50 0 0
20
40
60
80
100
Concentration,mM
40
0.1M NaOH
35
35
30
30
25
25
Current,µA
Current,µA
40
20 15 10
0.626mM D-Glucose+ 0.1M NaOH
20 15 10 5
5 0
0
-5
-5 0
200
400
600
0
800
200
400
600
800
Potential (mV vs Ag/AgCl)
Potential (mV vs Ag/AgCl) 50 50
1.24mM D-Glucose+ 0.1M NaOH
2.99 mM D-Glucose+ 0.1M NaOH
40 30
Current,µA
Current,µA
40
20 10 0
30 20 10 0
-10
-10 0
200
400
600
Potential (mV vs Ag/AgCl)
800
0
200
400
600
800
Potential (mV vs Ag/AgCl)
Fig. 6 The cyclic voltammograms of copper structures deposited from solutions containing various reducing agents recorded recorded in the presence of different concentration of D-glucose
amount of organic compounds on the surface of copper deposits and the presence of oxidized forms of copper. Ion etching of several areas of copper deposits and subsequent measurement of X-ray photoelectron spectra showed similar results (Fig. 10; Table 3). However, the high roughness of copper deposit and dielectric substrate does not allow to quantitatively estimate the etching depth. Therefore, the dependence of the active resistance on temperature (Fig. 11) was obtained for the qualitative characterization of the copper deposit. Moreover, it should be pointed out that the presented in Fig. 11 a linearly
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0.1M NaOH
80
120
0.666mM D-Glucose+ 0.1M NaOH
100 60
Current,µA
Current,µA
80 40 20 0
60 40 20 0
-20 0
200
400
600
-20
800
0
Potential (mV vs Ag/AgCl) 140
1.25mM D-Glucose+ 0.1M NaOH
140
120
400
600
800
2.87mM D-Glucose+ 0.1M NaOH
120
100
100
Current,µA
Current,µA
200
Potential (mV vs Ag/AgCl)
80 60 40 20
80 60 40 20
0
0
-20
-20 0
200
400
600
Potential (mV vs Ag/AgCl)
800
0
200
400
600
800
Potential (mV vs Ag/AgCl)
Fig. 7 The cyclic voltammograms of a pure bulk copper (etalon) recorded in the presence of different concentration of D-glucose
Fig. 8 The atomic force micrograph of the surface of copper structures deposited from solutions containing sorbitol
increasing dependence is typical for metals. Thus, based on the results previously discussed one can assume that the surface of copper deposits (electrode) is highly porous, in turn, the pores are coated with organic compounds and oxidation products of copper. Furthermore, we believe that some sort of nano-structured objects are inside the pores, which are
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100000
Fig. 9 The X-ray photoelectron spectrum of the deposited copper structures recorded without ion bean etching
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Cu2p3 Zn2p
Counts/s
80000
O1s Cl2p Si2p C1s
60000 40000 20000 0 1400
1200
1000
800
600
400
200
0
Binding energy,eV
Table 2 The composition of the surface of the deposited copper structures obtained by X-ray photoelectron spectroscopy without ion bean etching
Name
Peak BE
Atomic %
C1s
284.43
54.49
O1s
531.78
23.21
Si2p
101.9
9.45
Cl2p
198.78
6.95
Cu2p3
932.26
3.97
Zn2p
1022.11
1.93
Cu2p3
Fig. 10 The X-ray photoelectron spectrum of the deposited copper structures recorded using ion bean etching
200000 Zn2p
Counts/s
150000
Cl2p
100000 O1s C1s
50000
Si2p
0 1400
1200
1000
800
600
400
200
0
Binding energy,eV
Table 3 The composition of the surface of the deposited copper structures obtained by X-ray photoelectron spectroscopy using ion bean etching
Name
Peak BE
Atomic %
C1s
284.25
30.18
O1s
532.15
30.08
Si2p
102.92
14.38
Cu2p3
932.57
12.97
Cl2p
199.14
9.94
Zn2p
1022.46
2.45
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Fig. 11 The dependence of the active resistance of the deposited copper structures on temperature
R,Ohm
14,0 13,5 13,0 12,5 12,0 30
40
50
60
70
80
90
Temperature,°C
responsible for sensory activity. In addition, we also think that there is a core of monolithic copper in the depth of deposit, which is responsible for high electrical conductivity and the temperature dependence presented above. A similar model of the porous electrode was proposed and described in Levie (1967), Macdonald and Franceschetti (1987). The impedance spectroscopy was applied in order to confirm the porosity of the deposited copper microstructures. Figures 12 and 13 show the impedance hodographs of the fabricated and etalon electrodes obtained in aqueous solution of 0.1 M H2SO4. The hodographs reveal the significant difference between these electrodes in the radius of the semicircle formed by the resistance of the electrolyte solution, active resistance of the electrode and the capacitance of the electric double layer (EDL) at the electrode-solution border. This can be explained by the fact that the capacity of EDL depends on the effective area of the electrode and the dielectric permittivity of the electric double layer. As it was previously discussed the fabricated copper electrode has a higher effective electrochemical surface area than those observed for the etalon electrode. Moreover, one should remember that the copper deposit contains organic compounds on its surface. All together, this explains the large capacity of EDL and, therefore, larger radius of the semicircle demonstrated by the fabricated copper electrode. In addition, impedance spectra of both electrodes exhibit the Warburg impedance (Song et al. 1999), which characterizes the diffusion limitations for the charge carriers in solution within the low frequency region.
Fig. 12 The impedance hodograph of the deposited copper structures recorded in aqueous solution of 0.1 M H2SO4
-Z'' (Ohm)
3000
2000
1000
0 0
1000
2000
Z' (Ohm)
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Fig. 13 The impedance hodograph of a pure bulk copper (etalon) recorded in aqueous solution of 0.1 M H2SO4
Fig. 14 The equivalent electric circuit constructed for the deposited copper structures and a pure bulk copper (etalon). Here, W1 Warburg impedance; C1 the capacitor formed by EDL; R1 and R2 active resistance of solution and electrode, respectively
Based on the model of porous electrode behavior proposed in Levie (1967) and Macdonald and Franceschetti (1987), it was found out that there are three dispersions of pores with a range of characteristic sizes (diameters) varied from 50 to 50 lm. These calculations were performed in MathCAD 13. According to Levie (1967), Macdonald and Franceschetti (1987) and Song et al. (1999) as well as taking into account the aforementioned dispersion of pore sizes, one can construct the equivalent electric circuit of the electrochemical cell shown in Fig. 14 and calculate the values of the corresponding elements (Table 4) using proper software package (ZView2). The analysis of the obtained values (Table 4) indicates that the surface development of the fabricated copper electrode is higher compared with the etalon one. Furthermore, the obtained values of the Warburg impedance suggests that the fabricated electrode has more porous surface than that observed in the bulk polycrystalline copper (etalon electrode). Table 4 The values of the calculated elements of the constructed equivalent electric circuit for the deposited copper structures and pure bulk copper (etalon) The deposited copper structures
The pure bulk copper (etalon) 3.5 9 10-8
C1, F
4.2 9 10-6
R1, X
5
0.98
R1, X
156.5
9.12
W1, X
0.0011
2.1 9 10-6
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4 Conclusion The high conductive porous copper microstructures with a dispersion of pore size ranging from 50 nm to 50 lm were synthesized using laser-induced metal deposition method. These structures have a developed effective surface area, which is 30 times higher than that observed for a pure bulk copper with similar geometric parameters. The electrochemical studies revealed that an analytical response of the fabricated copper electrode is 15 times higher than those observed for a pure bulk copper. The sensory properties towards hydrogen peroxide and D-glucose showed that the value of Faraday current at the fabricated copper electrode is 2–2.5 orders of magnitude higher than for a pure bulk copper used as the etalon electrode. The overall results indicate that the laser-induced metal deposition technique is a good candidate for fabrication of small-sized electrochemical electrodes, which in turn can find application in design and production of new high efficient enzymeless biosensors. Acknowledgments I. I. T., M. S. P. and E. M. K. acknowledge the Russian Fund for Basic Research (Grants 15-03-05139). V. A. K., S. S. E. and A. V. S. acknowledge Saint Petersburg State University for a research Grants (2015–2017, 12.38.219.2015). The authors also express their gratitude to the SPbSU Nanotechnology Interdisciplinary Centre, Centre for Optical and Laser Materials Research, Centre for GeoEnvironmental Research and Modelling (GEOMODEL) and Center for Nanophotonics Research.
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