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3D printed low-cost spectroelectrochemical cell used for in situ Raman measurements Matheus Fernandes dos Santos, Vera Katic, Pãmyla Layene dos Santos, Bruno Morandi Pires, André Luiz Barboza Formiga, and Juliano A. Bonacin Anal. Chem., Just Accepted Manuscript • DOI: 10.1021/acs.analchem.9b01518 • Publication Date (Web): 17 Jul 2019 Downloaded from pubs.acs.org on July 18, 2019
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Analytical Chemistry
3D printed low-cost spectroelectrochemical cell used for in situ Raman measurements Matheus F. dos Santos, Vera Katic, Pãmyla L. dos Santos, Bruno M. Pires, André L. B. Formiga, Juliano A. Bonacin* Institute of Chemistry, University of Campinas, P. O. Box 6154, 13083-970, Campinas, SP, Brazil ABSTRACT: Raman spectroelectrochemistry is a powerful technique to characterize structural changes of materials during electrochemical reactions and investigate the mechanism of film deposition and adsorption processes on the surface of electrodes. Moreover, in situ measurements enable identification of catalytic sites and reaction intermediates, which facilitates the comprehension of reaction mechanisms. The limitations of this technique include the high-cost and the complexity of the experimental arrangement required by commercial spectroelectrochemical cells (SEC). Thus, 3D-printing technology emerges as an excellent alternative for production of SEC, with desirable shape, low-cost and robustness in a short period of time. In this work, a SEC and a 3D-printed working electrode were fabricated from acrylonitrile-butadiene-styrene (ABS) and conductive graphene polylactic acid (PLA) filaments, respectively. The proposed SEC and the 3D-printed electrode were printed within 3.5 hours with estimated cost of materials less than US$ 2. Then, the 3D-printed SEC and the electrode were used in the study of structural changes of Prussian blue according to different voltage bias. Keywords: 3D-printing technology, Raman spectroelectrochemistry, 3D-printed spectroelectrochemical cell, Prussian blue, 3Dprinted graphene electrodes Spectroelectrochemistry allows two measurements to be performed simultaneously, avoiding misinterpretation of electrochemical or spectroscopic results.1–3 With the possibility to control the applied potential, spectroscopic information such as electronic states and vibrational modes of molecules, related to in situ electrogenerated species can be obtained.3,4 Numerous spectroscopic methods coupled with electrochemical systems such as UV-Vis, infrared and Raman spectroelectrochemistry have been reported.5–8 Among them, Raman spectroelectrochemistry, a non-destructive tool with no sample preparation, emerges as a powerful technique for investigation of interfacial and surface phenomena. Therefore, this technique has been applied in elucidation of formation, corrosion and passivation of films under different experimental conditions.9 Since spectroelectrochemistry allows real-time monitoring of the surface of electrodes, kinetic studies of electrochemical reactions10 and adsorptiondesorption process11 can be performed. In addition, Raman spectroelectrochemistry has been extensively employed to identify reaction intermediates and to understand mechanism of electrocatalytic processes.12–15 In this sense, to perform spectroelectrochemical measurements, a proper spectroelectrochemical cell (SEC) should be used, and it is usually designed for specific equipment.16,17 Timm et al. have reported a robust Raman SEC, resistant to chemical reactants and solvents.17 However, the utilization of expensive materials such as quartz plate and platinum ring increase the cost of the SEC. Additionally, the fabrication process requires specialized technicians to operate subtractive manufacturing machines. To overcome this limitation, 3D-printing technologies emerge as an alternative tool for production of cheap, versatile and robust SEC. The multidisciplinary characteristic of this
technology comes from its simplicity and the possibility to design almost without boundaries using free available designing tools, and to generate 3D object.18,19 Generally, 3Dprinting technologies enable the production of any kind of device, either a part of the complex structures or the structure itself.20,21 The main advantages of this technology are the ability of fast prototyping, waste management and generation of low-cost products18,22. Because of this, 3D-printing technology has found applications in a variety of fields23–25, including fabrication of electrochemical devices, such as electrodes26, batteries27, microfluidic chips28 and electrochemical synthetic reactors.29 Recently, we have reported enhanced performance of 3D-printed graphene electrodes towards sensing of dopamine by applying a simple electrochemical pre-treatment.30 Cardoso et al. have reported a 3D-printed electrochemical cell for sensing of phenolic compounds, which allows the large-scale production, use in research and education purposes19. Herein, we report for the first time the production of a cheap and robust Raman spectroelectrochemical cell printed in a 3Dprinter. The dome-shaped SEC was fabricated using ABS filament. The proposed design was chosen to fit Raman objective lenses in the center of the cell, above the surface of a working electrode. Additionally, a screw shaped working electrode was printed using conductive graphene-based PLA filament. In order to evaluate the applicability of the cell, the working electrode was modified with Prussian blue, and structural changes were studied during its redox process
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EXPERIMENTAL SECTION Details about the design of the spectroelectrochemical cell and the working electrode, the description of the activation of the 3D printed electrode, the modification with Prussian blue and further experimental details are described in the Supporting Information. The cell design was divided in two parts: the cup and the cover, to optimize slicing and printing process, see the Figure 1A. Lateral view of assembled SEC can be seen Figure 1B. The cup is a cylinder with diameter of 60 mm, height of 10 mm and wall thickness of 2 mm (1, Figure 1A). A circular hole (outer and inner diameter of 14 mm and 8.5 mm, respectively) was introduced to allow coupling with a working electrode (3 in the Figure 1A). The working electrode consists of a circular base of 9.9 mm in diameter, and a strip of 2.0 mm coupled with screw thread. 3D-printed screw nut (4, Figure 1A) enables to pressure the head of working electrode against the O-ring to assemble the cell. This allows contact between the working electrode and solution without leakage. The strip was designed to allow the contact between the electrode and potentiostat by a crocodile clip. The cover is a spherical cap (base diameter of 60.0 mm and height of 19.3 mm) with three holes (2, Figure 1A). The centered hole with a diameter of 30.0 mm is the aperture for incident laser and the Raman lenses. The size and the dome-shape were defined to facilitate the entrance of Raman lenses (Figure 1C) in the interior of the cell to focus properly on the surface of the electrode and to prevent solution contamination. The other two holes (diameter of 10.0 mm each) were located with a maximum separation of 45.0 mm from each other with respect to their centers with an inclination of 22.5 degrees, in order to fit reference (Ag/AgCl 3 mol L-1) and counter electrodes (Pt). The diameters were designed according to the size of the electrodes. A support was printed to guarantee the cell immobility during the measurement. It consists of a 1 mm thick rectangular base (85 mm x 75 mm, part 6 from Figure 1A), which dimensions were defined according to Raman sample holder size. The support has a cylindrical cavity with a diameter 2 mm larger than the cup and depth of 1 mm inside a parallelepiped (thickness of 1 mm and square base of side 65 mm). In the center of support the circular hole was introduced to enable screw and electrode connection.
Figure 1. Photos of the proposed SEC: (A) Components of the 3D-printed cell: (1) cell cup, (2) cell cover, (3) graphene 3Dprinted screw-shaped working electrode (9.9 mm in diameter), (4) screw nut, (5) O-ring and (6) support for equipment, (B) the lateral view of the SEC, (C) 3D-printed cell coupled to Raman equipment, in the left orifice reference electrode and in the right the counter electrode.
Spectroelectrochemical measurements were performed according to the setup presented in Figure 1C, using the asprinted or activated 3DGrE modified with PB as working electrode, a Pt wire as counter electrode and Ag/AgCl (3.0 mol L-1) as reference electrode. Experimental procedures of the pre-treatment30 and modification of the electrodes31 can be found in the section S-1 of the Supporting Information. RESULTS AND DISCUSSION The presence of functional groups plays an important role in the modulation of the electrochemical properties of graphene. Recently, we have reported30 a simple electrochemical oxidation/reduction pre-treatment of 3D-printed graphene electrodes to improve their electrocatalytic properties. The detailed description of the Raman-assisted electrochemical functionalization of 3D-printed graphene electrode can be found in the Supporting Information. To evaluate the applicability of the 3D-printed graphene electrode and the spectroelectrochemical cell, PB was chosen as the electrode modifier due to its well-known redox properties.31 Structural changes of Prussian blue were monitored during electrochemical measurements. Figure S2 and S3 show the morphology of the surface of the activated 3DGrE before and after modification, indicating that the proposed electrode is a good support to anchor spherical and cubic particles of PB. The 3D-printed electrode exhibited a similar electrochemical behavior to the commercial glassy carbon electrode (GCE), as it can be seen in Figure S4. The cyclic voltammograms of the modified electrodes shows two redox processes at ca. +0.2 V and +0.9 vs. Ag/AgCl, AgCl assigned to the oxidation of Prussian White (PW) to Prussian blue (PB) and to oxidation of PB to Berlin Green (BG), respectively.32,33 In situ Raman spectra of PB on the 3D-printed graphene electrode are shown in Figure 2, obtained within a broad electrode potential window ranging from -0.4 V to +1.2 V vs. Ag/AgCl. The spectra have been normalized and limited between 2200 and 2000 cm-1 to investigate shift of the characteristic (CN) band of PB. Detailed discussion about Raman spectra of Prussian blue and the alterations of the frequencies of C≡N stretching band in function of the applied potential can be found in section S-5 of the Supporting Information.
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Analytical Chemistry
Figure 2. Raman spectra of PB modified 3D-printed graphene electrodes recorded at electrode potential ranging from -0.4 V to +1.2 V vs. Ag/AgCl, at excitation wavelength of 532 nm (25mW).
The first spectrum acquired, obtained under OCP conditions in solution, presents PB as predominate phase. The corresponding bands located at 2156 cm-1 and 2094 cm-1 corroborates with previously report by Mažeikienė et al., using 785 nm excitation.34 The in situ measurements started by applying negative potentials from -0.4 V to -0.1 V vs. Ag/AgCl. In this range of potentials, PW is the dominant phase. Due to the different chemical environment of the cyanide group in PW (FeII-CNFeII), the (CN) bands are shifted and appear approximately at 2140 cm-1 and 2110 cm-1 (Figure 2, Table S-1). With an increase in the applied potential, the band close to 2140 cm-1 shifts to higher frequencies due to the oxidation of FeII-CNFeII to FeII-CN-FeIII. Another indication of the formation of PB is the increase of the relative intensity between the higher frequency band (2140-2156 cm-1) and the lower frequency band (~2110 cm-1), as it can be seen in Figure 3. Two plateaus are observed in Figure 3, which means that in the ranges of 0.4 to -0.1 and +0.2 to +0.6, the composition of the electrode is predominantly PW and PB, respectively. In addition, the appearance of a shoulder assigned to A1g (CN) mode associated to Fe(II) in PB at ~2090 cm-1, upon application of +0.2 V, confirms the oxidation of PW to PB (see Figure 2). According to the cyclic voltammogram presented in Figure S4, PB oxidizes to BG at +0.9 V vs. Ag/AgCl. However, from Figure 3, the ratio between the bands at 2156 and at c.a. 2120 cm-1 starts to increase upon application of +0.7 V, probably due to oxidation of Fe(II) of PB by the oxygen presented in the electrolyte solution. In addition, the absence of the band at ~2120 cm-1 upon application of +0.9 V is an indicative of oxidation of PB to BG. Upon increasing of the applied potential, the band at 2090 cm-1 disappears, since Fe(III) is the main iron cations in BG. According to Samain et al., the complete oxidation of PB to BG is accompanied by a shift of the band at 2156 cm-1 to lower frequencies.35 However, due to the large area of the electrode, pure BG phase could be obtained if positive potential was applied for an interval of time higher than 20 minutes.
Figure 3. Relationship of the applied potential and the ratio between the intensities of the higher and lower frequency bands assigned to (CN).
CONCLUSION This work demonstrated limitlessness of 3D printing technology for in situ measurements. This powerful technique was used to print a simple, low-cost, robust 3D printed SEC and working electrode. In addition, the whole printing process can cost less than US$ 2. The SEC was produced using cheap, inert ABS filament, whereas working electrode was printed using conductive PLA/ graphene filament. The 3D-printed SEC was tested for in situ Raman measurements, with non-modified and PB modified working electrodes. It was possible to investigate the structural changes of PB during the redox process. In addition, from in situ electrochemical functionalization of graphene, a relationship between the level of structural disorders/defects and reaction time could be established. Therefore, in situ measurements facilitate the optimization of electrochemical parameters for obtention of electroactive surfaces. The reported SEC was designed intentionally for Raman measurements and its design was chosen to fit Raman lenses specifically. However, 3D printing is boundless when it comes to the shape and dimensions, therefore SECs for any kind of equipment can be easily produced. The 3D-printed SEC is adaptable from the point of views of the equipment, easy to print and cheap. These features open new possibilities to explore in situ reactions or operando. Supporting Information The Supporting Information is available free of charge on the ACS Publications website. Supplemental experimental section includes chemicals, design of the spectroelectrochemical cell, activation of 3D printed electrodes, modification with Prussian blue, microscopy and electrochemical characterization, and spectroelectrochemistry analysis; Raman-assisted electrochemical functionalization of 3Dprinted graphene electrode; Spectroelectrochemistry of Prussian blue modified 3D-printed electrode
AUTHOR INFORMATION Corresponding Author Prof. Juliano Alves Bonacin,*e-mail:
[email protected] ACS Paragon Plus Environment
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Phone: +55 (19) 3521 3103; www.bonacin.iqm.unicamp.br
Author Contributions
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The manuscript was written through contributions of all authors and all authors have given approval to the final version of the manuscript.
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Notes Any additional relevant notes should be placed here.
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ACKNOWLEDGMENT The authors acknowledge the financial support by CAPES, Fundo de Apoio ao Ensino, à Pesquisa e à Extensão - FAEPEXUNICAMP (grant#2824/17), CNPq (grant#459923/2014-5), São Paulo Research Foundation, FAPESP (grant#2013/22127-2 and grant# 2017/23960-0) and the National Institute of Science and Technology in Complex Functional Materials (CNPqMCT/FAPESP).
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