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A Triboelectric Closed-Loop Sensing System for Authenticity Identification of Paper-Based Artworks

Baodong Chen, Di Liu, Tao Jiang, Wei Tang, and Zhong Lin Wang*

DOI: 10.1002/admt.202000194

be developed. The results showed nano-generators (NGs) based on contact elec-trification effect might avoids to these limitations.[9–12] The first organic mate-rials-based triboelectric nanogenerator (TENG) was invented by Prof. Z. L. Wang in 2012,[13] which it’s not only a revolu-tionary energy harvesting technology, but also an innovative self-powered active sensing technology.[14,15] The fundamental and technological studies of TENG were experiencing a rapid development and its applications cover a wide range of fields for internet of things and artificial intel-ligence.[16–18] It could be used as active sensors, its application covers mechanical sensors,[19,20] physiological detection,[21,22] motion sensing,[23–25] touch and electronic skin.[26–28] The working principle of TENG is based on the contact electrification effect,[29–32] due to the surface states and energy levels of various tribo-materials are

generally distinct that its consequences lead to the capturing ability differences of charge.

Herein, we report a practical triboelectric closed-loop sensing system (TE-CLSS) by the contact electrification effect[33,34] and a conformable system,[35] that could be used to NDT for authenticity identification of paper-based artworks by detect the changes of triboelectric charge. This system was composed of a novel stethoscope-like triboelectric nanogenerator (SL-TENG) and a matched closed-loop feedback circuit. The electric output of SL-TENG was tested systematically for different tribo-materials. The performance of TE-CLSS was tested in the test conditions like different grayscale values, colored inks and oil paintings, and the influence factors were also discussed in detail. This study demonstrates a new type of portable NDT technology and it possesses fast response, high sensitivity, stable and reliable traits.

2. Results and Discussion

2.1. The Working Mechanism and Properties of the SL-TENG

Overall schematic of SL-TENG was shown in Figure 1a, it is composed of aluminum electrode and tribo-materials, acrylic sheet and 3D-printed structural frameworks. SL-TENG was made by sandwich structure, as detailly shown in Figure S1a,b in the Supporting Information. Also, the output performance of SL-TENG were tesed with different tribo-materials during this

Nondestructive testing (NDT) is crucial technology for authenticity identifica-tion of paper-based artworks. Emerging optical spectroscopy is an important technique of NDT at present, by which high-bightness light, electron beams, and rays could cause permanent damage to different types of paper-based artworks. Here, using only NDT technology, triboelectric closed-loop sensing system (TE-CLSS) is developed by contact electrification effect. It is composed of a stethoscope-like triboelectric nanogenerator (SL-TENG) and matched closed-loop feedback circuit (CLFC), that is capable of active sensing in a similar way to a stethoscope when it makes slight contact with the surface of object. The results report that the ΔV accuracy of TE-CLSS could achieve 0.01 V, with relative error of measurement within 3%, and average response time of 0.205 s. Furthermore, it could sense the area change of the test mate-rial layers that accurately reach millimeter level, by which different grayscale values, colored inks, and oil paintings are successfully identified. This work gives a new insight into the future NDT technologies suitable for the identifi-cation of cultural relics.

Prof. B. Chen, D. Liu, Prof. T. Jiang, Prof. W. Tang, Prof. Z. L. WangCAS Center for Excellence in NanoscienceBeijing Key Laboratory of Micro-nano Energy and SensorBeijing Institute of Nanoenergy and NanosystemsChinese Academy of SciencesBeijing 100083, P. R. ChinaE-mail: [email protected]. B. Chen, D. Liu, Prof. T. Jiang, Prof. W. Tang, Prof. Z. L. WangSchool of Nanoscience and TechnologyUniversity of Chinese Academy of SciencesBeijing 100049, P. R. ChinaProf. Z. L. WangSchool of Material Science and EngineeringGeorgia Institute of TechnologyAtlanta, GA 30332, USA

The ORCID identification number(s) for the author(s) of this article can be found under https://doi.org/10.1002/admt.202000194.

1. Introduction

Nondestructive testing (NDT) is essential for authenticity identification of paper-based artworks,[1–3] however, most con-ventional testing method is destructive at present, laborious and time-consuming, even if emerging optical spectroscopies is a NDT technology, which high-energy photons, electron beams, rays and or even camera’s flash could be permanent damage.[4–8] To satisfy the testing requirement and to overcome these bottlenecks, a new NDT technology is urgently needed to

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experiment, such as copper foil (Cu), aluminum foil (Al), poly-ethylene terephthalate (PET), polytetrafluoroethylene (PTFE), polyimide (PI), polyvinyl chloride (PVC), and fluorinated ethy-lene propylene (FEP). In addtion, the paper-based toners layer was printed by the same laser-printer, which is intended spe-cifically for experimentation and testing. Figure 1b represents the working mechanism of SL-TENG, the electricity genera-tion process including four typical states.[36–38] When PTFE film is used as the tribo-material layer, PTFE layer had nega-tive charges and the toners layer accumulated to positive charge due to the different surface electron affinities and band struc-ture of materials. Using the contact electrification effect cre-ated on the surfaces of two dissimilar materials when they are brought into physical contact, the contact-induced triboelectric

charges can generate a potential drop when the two surfaces are separated by a mechanical force, which can drive electrons to flow between the two electrodes built on the top and bottom surfaces of the two materials. At the initial state I, there was no current flow or potential difference. The amount of nega-tive charges on PTFE layer is equivalent as much as the posi-tive charges on the toners layer according to the law of charge conservation. So that, the surface potentials of the two layers at their initial state are equaled. As shown in state II, when the two layers separated with each other by an external force, the contact-inducted triboelectric charges can generate the potential difference, which can drive electrons to flow from ground to Al electrode. In equilibrium state III, the SL-TENG is fully sepa-rated where the potential difference and transferred charges

Figure 1. The working principle and output performance of stethoscope-like triboelectric nanogenerator (SL-TENG). a) Overall schematic and stracture of SL-TENG used in this study. b) Schematic diagram showing the working principle of SL-TENG. c) The numerically calculated electrical potentials distribution of SL-TENG based on PTFE film (thickness of ≈40 µm). d) The spider diagram showing the transfer charge quantity (Qsc), output short-circuit currents (Isc) and output open-circuit voltages (Voc) of SL-TENG. e) The Ring diagram showing the numerically calculated electrical potentials distribution of SL-TENG with different tribo-materials.





reached the maximum value, so that there is no charge flow. As shown in state IV, when the separation distance decreases as between the two layers, which lead the electrons to flow from electrode to ground simultaneously and generating a reverse current in the load because of the electrostatic induction effect. Figure S1 c–e in the Supporting Information shows the elec-trical output of SL-TENG, the charge transfer quantity (ΔQsc) of nearly 10.33 nC, the short-circuit current (Isc) of 2.81 µA and the open-circuit voltage (Voc) of 17.24 V in each cycle. Theoretically electrical potential distribution of SL-TENG were predicted by COMSOL simulation in each state, as shown in Figure 1c. At the starting point, the calculated electrical potential difference between the two electrodes was zero (state I), then, a potential was generated to keep the charge balance according to the sim-ulation (i.e., state II, state III, and state IV). COMSOL simula-tion has proved that the results are quite consistent with the working mechanism of SL-TENG with four typical states.

In order to uncover an optimal matching of contact electrifi-cation between various tribo-materials with paper-based toners layer, which suggested the existence of an optimal material in the electrical output for Cu, Al, PET, PTFE, PI, PVC, and FEP. The output performance of SL-TENG was investigated, as shown in Figure 1d,e and Figure S1f–h in the Supporting Information. The electrical output and COMSOL simulation were obtained with the various tribo-materials, a comparison between the experimental results proved that FEP material had excellent triboelectric and electric output properties. The max-imum values of ΔQsc, Isc, and Voc can reach up to nearly 31.42 nC, 2.87 µA, and 93.76 V, respectively (Figure S1f–h, Supporting Information). It is clear shown that the potential difference of various tribo-materials are consistent with experiment results, which reaches a maximum range of nearly −177.9 to 184.5 V on the FEP film (Figure S2, Supporting Information). Detailed material informations and testing process of SL-TENG were provide in the experimental section.

2.2. The Triboelectric Sensing Characteristics of SL-TENG

The triboelectric characteristics of SL-TENG based on FEP film were evaluated for different parallel stripes, patterns and con-tact areas on a size of 2 × 2 cm, as shown in Figure 2. The electric output of SL-TENG for different parallel stripes were tested, the ΔQsc, Isc, and Voc were decreased distinctly in com-parison to without stripe (white paper), as shown in Figure 2a–c (Figure S3a–f, Supporting Information). In this case, these have the same toners area between the different parallel stripes from 1 to 8. Figure 2d–f demonstrate the electrical output of SL-TENG for different patterns, the ΔQsc, Isc, and Voc were decreased with the increase area of toners layer (Figure S5a,b, Supporting Information). That is because the dielectric prop-erty of contact layers were changed with the increased area of toners layer, and the effect of contact electrification was weak-ened. The electrical output of SL-TENG for different contact areas were shown in Figure 2g–i, the ΔQsc, Isc and Voc were increased with the increased contact areas from 1 to 2500 mm2 (Figures S4 and S5c–f, Supporting Information). It is notable that the ΔQsc, Isc, and Voc of SL-TENG were obtained only at the contact area of 1 mm2, is as follows: 1.62 nC, 0.27 nA, and

4.88 V, respectively. Meanwhile, the electrical output of SL-TENG per unit area was revealed a horizontal trend with the contact area from 25 to 2500 mm2 (Figure 2i). The results indicate that SL-TENG could sensitively sense the area change of paper-based toners layer even if a tiny change, its accuracy could achieve millimeter level.

One the other hand, Figure 3 demonstrated that SL-TENG could be used to sense different grayscale values and iden-tify colored ink materials. The electrical output of SL-TENG increases with the increased grayscale values from 20 to 240, as shown in Figure 3a,b, the ΔQsc, Isc, and Voc were 6.82 nC, 1.97 nA, and 20.17 V at the grayscale value of 240, respectively (Figure S6 a–f, Supporting Information), which the toners content per unit area is decrease with the increased grayscale values. With the increased proportion of grayscale values (%, relative to the value of 255), the electric output of SL-TENG was increase almost linearly, as shown in Figure 3c. The measured curves have a significant linear correlation with the increased proportion of grayscale values. Figure 3d,e displays the electrical output of SL-TENG for seven colored ink mate-rials, while there was maximum values for the electric output of SL-TENG at the brown ink, were 9.63 nC, 1.87 nA, and 23.83 V respectively (i.e., RGB value of 88, 61, and 47), and the minimum value was obtained at the violet ink (Figure S6 g–l, Supporting Information). In addition, the definition of RGB value and testing process were provide in the Experimental Sec-tion and the Supporting Information. Figure 3f shows the FTIR spectrum of ink materials to identify the functional groups. There were infrared absorption characteristic peak at nearly 3300, 2900, 1700, 1300, and 1000 cm−1 wavelengths and each peak represented the presence of O-H, C-H, C = O, C–H/O–H and C–O–C bonding (Figure S7a–c,h and Table S1, Supporting Information). These bonding shows that there exist functional materials in colored ink materials, such as pigments, organic solvent, active diluent, water and viscous materials. Further-more, the DSC-TG curve of colored ink materials were shown in Figure 3g–i and Figure S7d–g (Supporting Information). The results revealed that there are three sequential stages in the process of thermal decomposition, in order the primary stage of 300–410 K, second stage of 410–520 K, and third stage of 520–670 K range. First, the adsorbed water and crystal water were lost on the primary stage, the thermal decomposition of the ink materials were proved during temperature rising on the second and third stage. Furthermore, the endothermic peak and weight loss of violet ink material is relatively large, and the rest of weight (11.08%) was minimal. Figure 3i shown the electrical output of SL-TENG can coincide with the rest of weight with different ink materials, that due to the water loss and pyrolysis. It is clearly that SL-TENG could sensitively sense the change of ink materials. As a result, that are one interesting and momentous, a wide potential application that SL-TENG as a triboelectric sensing device could be used NDT for paper-based paintings.

2.3. The NDT Applications of TE-CLSS Based on SL-TENG

Figure 4 demonstrates the struture and applications of TE-CLSS as a practical NDT technolgy, this system was developed by





contact electrification and conformable system which com-posed of a SL-TENG unit and a CLFC (Figure S8, Supporting Information). Figure 4a schematic diagram shown a working scenario of TE-CLSS. Operational block diagram of the system design was shown in Figure 4b, and Figure 4c shows the digital image of TE-CLSS. The CLFC is consisting of an integrated circuit amplifier (ICA), microcontroller unit (MCU), capac-itor, resistances, smapling controlers (SC-I, SC-II) and display

controler (DC-I), as shown in Figure 4d. The detail of circuit principle is shown in the Supporting Information (The circuit diagram of CLFC).

Figure 4e shows TE-CLSS as a NDT sensing technology to detect the printed toners layer. The curve marked with red wire is the output voltage (Vp) when TE-CLSS contact with the white paper, while the curve marked with blue wire is the output voltage (Vt) when TE-CLSS contact with toners layer (Figure S9,

Figure 2. The electrical output of SL-TENG. a) Sketch showing the parallel stripes of laser-printed toner. b) The output Qsc, Isc, and Voc of SL-TENG with different number of parallel stripes. c) The relationship between the electrical output of SL-TENG and number of parallel stripes. d) Sketch showing the patterns of laser-printed toner. e) The output Qsc, Isc, and Voc of SL-TENG with different patterns. f) The relationship between the electrical output of SL-TENG and area of patterns. g) Sketch showing the contact areas of laser-printed toner from 1 to 2500 mm2. h) The output Qsc, Isc, and Voc of SL-TENG with different contact areas. i) The change law of the output performance per unit area.





Supporting Information). The results shown that the Vp of 0.48 V is slightly higher than the Vt of 0.3 V (Figure 4f), with average response time of 0.205 sand it only around 0.018 s to drop to the half maximum voltage (half-peak width) was required (described in detail in the Supporting Information). It is clearly, there is an apparently difference between two output voltage, which this system means that the different of contacting materials can be identified by detecting voltage. In

addtion, Figure 4g presents the identification process of TE-CLSS, which the results are both exactly exact and correct at the forward and reverse process (Videos S1 and S2 and Figure S10, Supporting Information). The testing results shows that the ΔV measurement accuracy of TE-CLSS can achieved to about 0.01 V order of magnitude. So that, this system could accurately judge whether there are toners for any given testing regions, and there is a voltage difference between. More remarkable,

Figure 3. The electrical output of SL-TENG with different grayscale values and colored inks. a) Sketch showing the different grayscale values of laser-printed toner. b) The output Qsc, Isc, and Voc of SL-TENG with different grayscale values. c) The relationship between the grayscale value and the electrical output of SL-TENG. d) Sketch showing the different RGB values of colored inks. e) The output Qsc, Isc, and Voc of SL-TENG with different colored inks. f) The FTIR characteristic of colored inks. g) The DSC-TG characteristic of colored inks with temperature ranges of 300–650 K. h) The DSC-TG characteristic of colored inks with temperature ranges of 320–420 K. i) The relationship between the rest of weight (%) and the electrical output of SL-TENG.





Figure 4. A triboelectric closed-loop sensing system (TE-CLSS) and its applications. a) Schematic diagram showing the working scenario of TE-CLSS. b) Operational block diagram of the overall system design. c) Digital photographs of TE-CLSS. d) The circuit diagram of TE-CLSS. e) The output elec-trical signals of TE-CLSS for white paper and laser-printed toner (red curve correspond to the white paper and blue curve correspond to the laser-printed toners). f) The local amplified electrical signals of TE-CLSS. g) The identification process of TE-CLSS.





TE-CLSS has the significant advantage of being high portability, rapid dynamic response and simple in structure relative to con-ventional NDT instrument. These demonstration processes and the detail of software can be found in Experimental Section and Supporting Information.

To further explore the applications for the developed TE-CLSS, a practical demonstration that the identification pro-cess of oil paintings was presented in Figure 5. Figure 5a schematic diagram showing a testing scenario for two paper-based paintings (L-Art and R-Art), which one of them is hand-drawn or printed. First, three identified regions were random selected in oil paintings, as shown in Figure 5b, i.e., A, B and C. The peak voltages were recorded by TE-CLSS for the con-tact area of 25 cm2, as shown in Figure 5c. The results shown that the peak voltage of the coated paper is higher obviously than three identified regions of L-Art and R-Art. In addition, the peak voltage are obvious differences in the same identi-fied region of L-Art and R-Art, moreover, the differences of peak voltage at A region (ΔVA), B region (ΔVB), and C region (ΔVC) are 0.22, 0.10, and 0.19 V, respectively, as shown in Figure 5d. Furthermore, the experimental results indicated that higher precision and resolution can be achieved by this system, which the ΔV measurement accuracy of TE-CLSS can achieved 0.01 V and the relative error of measurement within 3%. Figure 5e demonstrates the NDT process of authenticity recognition for two paintings by the TE-CLSS. The results shown that the identification results of TE-CLSS for A, B and C regions were consistent, which the L-Art is printed and the R-Art is hand-drawn. The identification process for A, B and C regions can be captured in Supporting Informa-tion (Videos S3–S5 and Figures S11–S13, Supporting Infor-mation). Additionally, the surface morphology of A, B, and C regions were characterized by OM, as shown in Figure 5f,g. The surface morphologies of L-Art shown that has a com-pletely uniform distribution microstructure with the concavo-convex structure of fine and homogeneous, this is due to the thinner inks layer and the inherent feature of coated paper. The surface morphology of R-Art shown that it has a lot of acicular structure, distribution uniformity and some orien-tation, this is because the characteristic of oil materials and formed thicker layer, which the calligraphy direction of the brush may result in some orientation of surface morphology. The surface morphology of two paintings were great discrep-ancy, but them hardly recognized by eyes in the sight-distance range. However, the above results confirmed that we designed TE-CLSS effectively responds to the change of surface mor-phology and ink materials.

3. Conclusions

In summary, a practical TE-CLSS based on the SL-TENG was fabricated according to the mechanism of contact electrification and conformable system, which could be applied in NDT for the paper-based paintings or artworks. The results illustrate that the approach of using SL-TENG as an active sensing device can be effective for detected the change of triboelectric charges on material surface. Moreover, it was confirmed that higher preci-sion and resolution can be achieved by this system, that the ΔV

measurement accuracy to one-100th of a volt and the relative error of measurement within 3%. Finally, TE-CLSS was suc-cessfully applied to identify various grayscale values, different colored inks and paintings, owing to its numerous advantages like portability, sensitivity, rapid response and simple fabrica-tion process, while it only needs to be contacted once lightly in the testing process. In most cases, this may not require to entirely substituting conventional detection technology, but this system and our supporting demonstration studies pro-vide a new framework for multifunctional sensing suitable for the verification of cultural relics and offering alternatives to future NDT technologies.

4. Experimental SectionThe Fabrication of TE-CLSS Based on SL-TENG: In this experiment,

triboelectric closed-loop sensing system (TE-CLSS) was fabricated by contact electrification and conformable system, which composed of a stethoscope-like triboelectric nanogenerator (SL-TENG) unit and a matched closed-loop feedback circuit (CLFC), with the size of 60 × 60 × 90 mm. Figure S8a,b in the Supporting Information shows the structure of SL-TENG, which its exterior structural framework was fabracted by 3D-printing. It consists of aluminum (Al) electrode (the thickness of ≈60 µm), FEP membrane (the thickness of ≈50 µm), acrylic substrate (the thickness of ≈3 mm) and stick tape. First, one acrylic sheet was cut by laser cutter into square (the size was 60 × 60 mm). Then, Al electrode was adhered to the acrylic sheets. Next, the FEP film was adhered to Al electrode with acrylic sheet as tribo-material layer. The wire from Al electrode connects to the ICA and output the electrical signals. The paper-based toners layer was printed by a laser-printer. Figure S8c in the Supporting Information shows the structure and components of TE-CLSS in detail.

The Composition of Closed-Loop Feedback Circuit (CLFC): The TLV2455 (TI) amplifier with low noise and high sensitivity was used to convert the current into voltage and amplifies it. The amplifier’s consumption was low with 23 µA per channel while offering 220 kHz of gain-bandwidth. A 12-bit analog-digital module with high conversion accuracy was used to convert the analog signal into digital. The voltage amplified was connected to the AD sample pins (P 9.0) of MSP430FR6989 launchpad. Besides, the oscillator’s frequency on the board was 32.768 kHz. In addition, three mechanical keys are connected to the P 2.2, P 2.3, P 2.4 pins as input of MCU. Two leds are connected to the P 3.1, P 3.3 pins as output of MCU, which the detail of circuit principle is shown in the Supporting Information the PDF file (The circuit diagram of CLFC). Figure S8d in the Supporting Information shows the structure and components of TE-CLSS in detail, the working principle of CLFC as shown in the Supporting Information.

The Design Principle of Software: The output voltage adjusted was input to the AD pins of MSP430 to achieve converting the analog signal into digital. The AD module operates on repeat-single-channel mode with oscillation frequency 32.768 kHz. The sample rate was set around 122 Hz which means the module can complete a sample once in 0.008 s. It can be adjusted to smaller to complete more times samples in one output voltage signal. In sample process, a gate voltage of 0.1 V was set in order to eliminate the disturb of noise. It can sample more than 10 times in one voltage signal on that situation. After 10 times samples, the average of input voltage was calculated and stored in MSP’s memory recording as the input voltage value (Vp and Vt). Then the relevant led will be lighted. In identification process, the AD module sample like previous again and stores the current voltage value. The CPU compares voltage value with Vp and Vt to judge which one was closer to current voltage value and light its led.

Data Processing: There was an industrial-frequency noise of 50 Hz existing in measuring instrument, the data sampled by 6517 voltage preamplifier and NI 6356 was processed by 50 Hz low pass FFT filter.





Figure 5. TE-CLSS apply to the identification of paper-based oil paintings. a) Schematic diagram showing a testing scenario of TE-CLSS. b) Oil painting and selecting three identified regions (A, B, and C). c)The peak voltages (Vmax) of TE-CLSS for A, B, and C regions. d) The difference of the peak voltages (ΔV) for A, B, and C regions. e) The identification process of TE-CLSS be used for on the paper-based oil painting. (This system can quickly “know” which one of L-Art and R-Art is hand-drawn or printed.). f–h) The optical images of L-Art and R-Art A, B, and C regions.





The MCU launchpad has less industrial-frequency noise, because it was powered by DC power with some filter capacitors in addition.

Electrical Measurements: To investigate the output performance of SL-TENG quantitatively, a linear motor was used to control the displacement, frequency, and produce the uniform contact. The output electrical signals were measured by a Keithley 6517 voltage preamplifier, a Data Acquisition Card and oscilloscope (Agilent, DSO-X 2014A). The software platform was constructed based on LabVIEW, which can realize real-time data acquisition control and analysis. The potential distribution in the SL-TENG was calculated from a finite-element simulation using COMSOL software. Constant laser-printing toners were taken and the same printer in each sample, in which the gray value of Red-Green-Blue (RGB) color was 255, 255, and 255, respectively, while a linear motor was used to drive the SL-TENG.

Characterization: The surface morphologies of ink materials were analyzed using an optical (OM). The Fourier-transform infrared spectroscopy (FTIR, Nicolet IS10) was utilized to binding analysis of ink materials. Thermal Gravimetric and Differential Scanning Calorimetry (TG-DSC) was utilized to pyrolysis behavior analysis of ink materials.

Supporting InformationSupporting Information is available from the Wiley Online Library or from the author.

AcknowledgementsB.C. and D.L. contributed equally to this work. The authors acknowledge the support from Beijing Natural Science Foundation (Grant No. 2192062), supported by National Natural Science Foundation of China (Grant Nos. 51502147, 51462026, 51672136, 61405131, 51432005, 51561145021, 51702018, and 11704032). The research was sponsored by the National Key R & D Project from Minister of Science and Technology (2016YFA0202704) and the Beijing Municipal Science and Technology Commission (Z171100002017017, Z181100003818016, and Y3993113DF). At the same time, authors thank for the oil painting that was provided from Wen-xin Chen (six-year-olds, Class 2, Grade1, Beijing NO.2 Experimental Primary School).

Conflict of InterestThe authors declare no conflict of interest.

Keywordscontact electrification, nanogenerators, nondestructive testing, triboelectric sensing

Received: March 6, 2020Revised: June 7, 2020

Published online:

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