ZnO nanorods patterned-textile using a novel hydrothermal method for sandwich structured-piezoelectric nanogenerator for human energy harvesting

Accepted Manuscript ZnO nanorods patterned-textile using a novel hydrothermal method for sandwich structured-piezoelectric nanogenerator for humam energy harvesting Zhi Zhang, Ying Chen, Jiansheng Guo PII:

S1386-9477(18)30870-1

DOI:

10.1016/j.physe.2018.09.007

Reference:

PHYSE 13281

To appear in:

Physica E: Low-dimensional Systems and Nanostructures

Received Date: 10 June 2018 Revised Date:

4 September 2018

Accepted Date: 10 September 2018

Please cite this article as: Z. Zhang, Y. Chen, J. Guo, ZnO nanorods patterned-textile using a novel hydrothermal method for sandwich structured-piezoelectric nanogenerator for humam energy harvesting, Physica E: Low-dimensional Systems and Nanostructures (2018), doi: 10.1016/ j.physe.2018.09.007. This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

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ZnO Nanorods Patterned-Textile Using a Novel Hydrothermal Method for Sandwich Structured-Piezoelectric Nanogenerator for Humam Energy Harvesting

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Zhi Zhang, Ying Chen, Jiansheng Guo∗

Key Laboratory of Textile Science and Technology, Ministry of Education, College of

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Textiles, Donghua University, Shanghai 201620, People’s Republic of China.

Abstract: With the development of wearable and flexible electronics, PENGs based on ZnO

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nanorod arrays patterned-textile have aroused great interests. Nevertheless, the currently used hydrothermal method to fabricate ZnO nanorods and the performance of ZnO strucures prepared at present still need to be further improved. Hence, ZnO nanorods patterned textile

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based-PENG (ZnO-T-PENG) has been developed in this paper, which consists of vertically arranged ZnO nanorod arrays sandwiched between two symmetrically layers of silver (Ag) coated-fabrics. A facile screen printing method was utilized to plate Ag paste on the fabric

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surface as electrodes. In particular, a novel hydrothermal method which requires single

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precursor solution was employed to synthesize ZnO nanorod arrays. Results reveal ZnO nanorod arrays which are uniformly, densely, and vertically arranged on the surface of Ag coated-fabric, have been synthesized successfully. Atomic force microscope (AFM) analysis proves the ZnO nanorods possess excellent coupled piezoelectric and semiconducting properties. This PENG can harvest the energy from human bodies with output voltages of 4 V,

∗

Corresponding author. E-mail address: E-mail addresses: [email protected] (J. Guo) 1

ACCEPTED MANUSCRIPT 0.8 V and output currents of 20 nA, 5 nA for palm clapping and finger bending respectively. This kind of ZnO-T-PENG exhibits superior flexibility and wearability with the capability of powering for micro electronic devices, which can promote the development of wearable

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electronics. Keywords: piezoelectric nanogenerator (PENG), ZnO nanorod, semiconductor, textile,

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wearable electronics

1. Introduction

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Piezoelectric nanogenerators (PENGs) [1] have aroused great interest for their capability of converting nano-energy [2] from our living environment into electricity, which involve great potential and prospects for the large-scale supply of power as alternative sources. The mechanism of PENG relies on the coupled piezoelectric and semiconducting properties of

semiconductors,

ZnO

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one-dimensional zinc oxide (ZnO), BaTiO3, CdS, GaN, etc [3-5]. Compared to other shows

exceptional

piezoelectric

properties

owing

to

its

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non-centrosymmetric crystal structure, especially the occurrence of anharmonic phonons that are responsible for piezoelectronic features [6]. Accordingly, ZnO has been extensively used

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to pursue designing PENGs [7]. However, the hydrothermal method, as the most commonly used method to synthesize ZnO nanorods, always uses different seed and growth solutions [8-11], which may be troublesome and lavish. Therefore a further optimization to the currently used hydrothermal method is urgently needed. On the other hand, PENGs currently researched usually utilized conventional rigid materials as the substrates, among which silicon (Si) [12-15], glass [16, 17] and titanium (Ti) foil [18] have been widely used. However, these materials exhibit poor flexibility and 2

ACCEPTED MANUSCRIPT deformation, above which PENGs are facing a challenge of practical applications. Especially in recent years, with the development of wearable and flexible electronics, PENGs with flexibility and stretchability play an increasingly important role as alternative energy sources

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[19]. Therefore there has been rapid progress on fabricating flexible or stretchable PENGs

based on ZnO nanowires or nanorods. The commonly used flexible substrates are paper [20-22], PU sponge [23], Poly-ethylene terephthalate (PET) [24-27], flexible plastic [11] and

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so forth. Nevertheless, these substrate materials above are unable to meet wearable

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requirements due to their limited wearing properties and poor integrity with clothing. Compared with these materials above, textile materials possess superiorities of intrinsically mechanical flexibility, lightweight and low cost, and most importantly, the feasibility for integration into various areas such as clothing, shoes and clothing accessories

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[28]. To make full use of the merits of fabrics, some researches have been carried out to apply fabric into PENGs. For typical examples, Khan et al. have finished a series of researches on PENGs by synthesizing one-dimensional ZnO structures on conductive textile fabric

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substrate using aqueous chemical growth (ACG) method [29-32]. Likewise, Liao et al.

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presented a novel, low-cost approach to fabricate flexible piezoelectric nanogenerators (NGs) consisting of ZnO nanowires (NWs) on carbon fibers and foldable Au-coated ZnO NWs on paper [8]. Nevertheless, the performance of the PENGs and ZnO strucures prepared on fabric surface at present need to be further improved to meet the needs of wearable electronics. Because textile materials present widespread prospects in flexible PENGs, ZnO nanorods patterned textile-based PENG (ZnO-T-PENG) has been developed using a novel hydrothermal method in this paper. The ZnO-T-PENG is composed of two layers of silver 3

ACCEPTED MANUSCRIPT (Ag) coated-nylon fabric which is located symmetrically on the top and bottom of ZnO nanorod arrays. A facile screen printing method was used to coat the surface of nylon fabric with Ag paste as the electrodes. Remarkably, a novel hydrothermal method using single

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solution instead of different seed and growth solution was employed to synthesize ZnO nanorod arrays. By controlling the concentration of reaction precursor solution, content of aqueous ammonia, reaction temperature and time and so forth, the ZnO nanorod arrays which

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are uniformly, densely, and vertically arranged on the surface of Ag coated-fabric, have been

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synthesized successfully. Atomic force microscope (AFM) analysis proves the ZnO nanorods possess excellent coupled piezoelectric and semiconducting properties, providing stable working mechanism for PENG. To harvest mechanical energy from human body, the as-fabricated PENG device is attached to human fingers and palms. By connecting the PENG

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device with test instrument, this PENG can harvest the energy from human bodies with output voltages of 4 V, 0.8 V and output currents of 20 nA, 5 nA for palm clapping and finger bending respectively. Besides, the ZnO-T-PENG possesses good stability and can provide

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electricity to micro-electronic devices. This kind of PENG exhibits superior flexibility and

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wearability which can promote the development of wearable electronics.

2. Experimental

2.1. Synthesis of ZnO nanorods patterned-textile The vertically-aligned ZnO nanorods were prepared by a novel hydrothermal method. Remarkably, this method requires only one precursor solution which differs from conventional hydrothermal method using different seed solution and growth solution [8-11],

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ACCEPTED MANUSCRIPT making it more convenient. Firstly, the precursor solution was prepared by dissolving hexamethylenetetramine (HMTA (C6H12N4), 99 wt%, AR, Aladdin) and zinc acetate dihydrate (Zn(CH3COO)2·2H2O, 99 wt%, AR, Aladdin) with equimolar concentration of 30

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mM in deionized water. Specifically, 395.12 mg Zn(CH3COO)2·2H2O and 252.4 mg HMTA were dissolved in 120 mL and stirred at room temperature for 30 min to ensure a sufficient dissolution. Then 6.7 mL ammonia solution (28-30%, Aladdin) was mixed dropwise into the

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solution which is crucial to control the aspect ratio and growing rate of ZnO nanorods [10,

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33]. This is ascribe to that an appropriate amount of ammonia solution can inhibit the homogeneous nucleation and promote heterogeneous nucleation in the precursor solution,

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then ZnO nanorods with higher aspect ratio can be prepared.

Fig. 1. Schematic diagram of the preparation process. (a) Screen printing method was used to coat the surface of fabric as the electrode. (b) Ag coated-weave fabric. (c) Ag coated-fabric was fixed on a customed PTFE holder. (d) Hydrothermal growth of ZnO nanorod arrays. (e) ZnO naorods vertically arrayed on the surface of Ag coated-fabric. 5

ACCEPTED MANUSCRIPT Prior to the synthesis of ZnO nanorods, the nylon fabric piece (2 cm × 1.5 cm) was firstly cleaned ultrasonically by acetone, alcohol and deionized water for 10 min, 10 min and 5 min respectively. Then, a facile screen printing method [34] was used to coated the surface of

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fabric with silver (Ag) paste as an electrode, followed by heating at 120℃ for 20 min, as shown in Fig. 1(a) and (b). To synthesize ZnO nanorod arrays vertically on the surface of Ag coated-fabric, the Ag coated-fabric was fixed on a customed PTFE holder (Fig. 1(c)).

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Subsequently, the PTFE holder with fabric was immersed in the precursor solution in

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water-bath at 35℃ for 5 min, followed by pulling out gently and annealing at 120℃ for 30 min. Then a uniform ZnO seed layer was formed on the surface of Ag coated-fabric, which provide a basic condition of lattice matching for the growth of ZnO nanorods. Afterwards, the PTFE holder was submerged in the precursor solution again, and the beaker containing fabric

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vertically was sealed and kept in the water-bath at 90℃ for 4 h. Finally the fabric was taken out from the beaker, rinsed by deionized water and annealed at 120℃ for several times, after which the ZnO nanorod arrays have well arrayed on the surface of Ag coated fabric with

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hexagonal cross section, as diagramed in Fig. 1(e).

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2.2. Characterization and Measurements The surface morphological observations of fabric, Ag coated-fabric and ZnO nanorod arrays were performed by a field emission scanning electron microscope (FE-SEM, Hitachi S-4800, Japan). Atomic force microscope (AFM, Agilent 5500, America) were used to observe surface topography and a conductive probe was used to get the surface current diagram and current-voltage curves. The crystal structures of Ag coated-fabric and ZnO nanorod arrays were analyzed by X-ray diffraction (XRD) using Cu Kα radiation (λ = 1.5406 6

ACCEPTED MANUSCRIPT Å). The electrical signals were acquired using an oscilloscope (ZDS 2022 Plus, China) and a programmable electrometer (Keithley Model 6514, America).

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3. Results and Discussions 3.1. Structure of ZnO-T-PENG

The structure of the ZnO-T-PENG is shown in Fig. 2, which consists of vertically

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arranged ZnO nanorod arrays sandwiched between two symmetrically layers of Ag coated-fabrics. The unique sandwich-like PENG not only provides good Schottky contact

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between ZnO nanorods and Ag electrodes but also forms a stable working mechanism, where

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the external fabrics are as substrate materials and protect the ZnO nanorods as well.

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Fig. 2. (a) The structure of PENG. (b) Schematic diagram of PENG constitution.

3.2. Morphology and crystal structure The surface morphologies of fabric before and after coated with Ag are shown in Fig. 3(a) and 3(b). Fig. 3(a) exhibits the nylon fabric with a plain weave structure, interweaving of wefts and warps. After coated with Ag paste, the surface is smooth which provides excellent condition for the growth of ZnO nanorods, as displayed in Fig. 3(b). It can be found that the Ag layer covered the fabric surface uniformly, because after coated with Ag, no Ag peaks 7

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Fig. 3. Surface morphologies of the fabric before (a) and after (b) coated with Ag. (c) XRD pattern of nylon fabric. (d) XRD pattern of Ag coated-fabric.

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have been observed in the XRD pattern, by comparing the XRD patterns of fabric before (Fig. 3(c)) and after (Fig. 3(d)) coated with Ag.

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The FE-SEM images in Fig. 4(a) to (c) show the morphologies of ZnO nanorods, and Fig. 4(c) shows the optical photo of the ZnO nanorods arrayed fabric. It can be seen from Fig. 4(a)

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and (b) that ZnO nanorods arrayed uniformly, vertically and with high density on the surface of Ag coated-fabric. The space homogeneity of ZnO nanorods is presented in Fig. 4 (b) by observing them in an oblique direction. It demenstrates that the ZnO nanorods have a resonable space uniformity. To indicate the length of ZnO nanorods accurately, a stripping method was utilized and corresponding FE-SEM image is shown in the insert picture in Fig. 4(c). The result indicates the average length of ZnO nanorods is about 4 µm. Besides, the diameter of ZnO nanorods is about 100 nm as shown in the insert of Fig. 4(d). Thus the 8

ACCEPTED MANUSCRIPT as-fabricated ZnO nanorod possesses a high length-diameter ratio (aspect ratio) of 40: 1, which can promote the piezoelectric effect. To characterize the crystal structures of ZnO nanorods, XRD pattern of ZnO nanorods was performed and shown in Fig. 4(d). Compared

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with the standard card (JCPDS card No. 36-1451), we can see that all the diffraction peaks can be indexed to hexagonal wurtzite structure of ZnO [35, 36]. The XRD results reveal that the ZnO nanorods have a typical wurtzite structure and grow along the (002) direction which

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indicate ZnO nanorods are well c-axis oriented. Two peaks of assigned Ag layer are also

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observed, which exists in the gap between adjacent ZnO nanorods.

Fig. 4. (a) Overlooking surface morphologies of ZnO nanorod arrays under lower magnification and optical picture of ZnO nanorods arrayed fabric (Upper right corner picture). (b) Oblique surface topographies showing space homogeneity of ZnO nanorods. (c) Overlooking surface morphologies and longitudinal surface of ZnO nanorod arrays under higher magnification. (d) XRD pattern and cross section of ZnO nanorod arrays. 9

ACCEPTED MANUSCRIPT 3.3. AFM analysis To analyze the coupled piezoelectric and semiconducting properties of ZnO nanorods, the measurements were performed using the AFM and the results are shown in Fig. 5. Fig. 5(a)

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shows the surface morphology under scanning by a conductive probe, which presents that the

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ZnO nanorods grow well on the surface of Ag coated-fabric. At the same time, the surface

Fig. 5. AFM measurements of ZnO nanorods. (a) Surface morphology of ZnO nanorods. (b) Surface

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current of ZnO nanorods coated-conductive fabric. (c) I-V curve of non-ZnO nanorods region. (d) I-V

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curve of single ZnO nanorod. (e) Repeatability measurement of I-V curve for one ZnO nanorod.

current diagram was obtained as depicted in Fig. 5(b). Besides, the current-voltage (I-V) characteristics of the as-fabricated PENG device are shown in Fig. 5(c) to (e), wherein the scanning voltage was kept from -2 V to 2 V. When the conductive probe contact the surface without ZnO nanorods, the I-V curve is shown in Fig. 5(c), when the probe contact the surface of single ZnO nanorod, the I-V curve is shown in Fig. 5(d). From the I-V curves we can find that ZnO nanorods possess excellent semiconductor characteristics and Schottky 10

ACCEPTED MANUSCRIPT contact is formed at the interface between Ag and ZnO nanorods. The nearly symmetrical nonlinear current-voltage characteristic curve obtained under forward and reverse bias mainly result from the impact of a pair of back to back Schottky barriers. One barrier is located at the

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interface of ZnO nanorod and Ag electrode, and the other exists at the interface of conductive probe and ZnO nanorod. Thus the measured curve does not show the corresponding features of I-V characteristic of the single Schottky diode [23, 24, 37]. Multiple curves in Fig. 5(e)

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confirm the repeatability of ZnO nanorods in the continuous contact and separation for 15

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times.

Fig. 6. Electricity generation mechanism of the NM-TENG. (a) Pressing. The electrons flow from the upper electrode to lower electrode and the ammeter deflect. (b) Pressed. No electrons flow. (c) Releasing. The electrons flow reversely and ammeter deflect reversely. (d) Released. No electrons flow.

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ACCEPTED MANUSCRIPT 3.4. Working mechanism of ZnO-T-PENG A cycle of electricity generation process of the PENG is shown in Fig. 6, which is based on the coupling of the piezoelectric and semiconducting properties of one-dimensional ZnO

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[1, 11, 38]. The preferred c-axis alignment of the ZnO nanorod arrays lead to the strong piezoelectric alignment with regard to the external force [39, 40]. With a force applied vertically, the strains of piezoelectric crystals occur along the length direction of ZnO

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nanorods, leading to the polarization of vertically arrayed ZnO naorods. Therefore, when a

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vertical force applied, equal amount of negative and positive piezoelectric potential are generated on the top and bottom side of ZnO nanorods respectively, as shown in Fig. 6(a). At this time, in order to neutralize the electric field formed along ZnO nanorods, electrons will flow from the upper electrode to the lower electrode to form a current in the external circuit.

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With the increase of the applied force, the strain of ZnO nanorod increase. As is shown in the Fig. 6(b), The electrons stop flowing until a potential balance forms. And then with the force withdrawing from the ZnO nanorods, the strain of ZnO nanords begin to recovery which

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result in the diminution of piezoelectric potential, at the same time, the electrons flow

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reversely (Fig. 6(c)). When the strains of ZnO nanorods recover absolutely, the electrons stop flowing where almost all of the piezoelectric charges are screened (Fig. 6(d)).

3.5. Output performance and possible applications of ZnO-T-PENG for harvesting human energy To validate the capability of the PENG for harvesting energy from human body, the as-fabricated device was connected with test instrument and measured by finger bending and palm clapping, as shown in Fig. 7(a). It can be seen from Fig. 7(b) and (c), by palm clapping 12

ACCEPTED MANUSCRIPT and finger bending, the output voltages and currents are about 4 V, 20 nA, and 0.8 V, 5 nA respectively. Besides, one cycle of the output voltage and current are displayed in Fig. 7(d) and (e). To investigate output stability, which is an important concern for the ZnO-T-PENG in

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real application, the output signals were measured and compared before and after 1000 cycles under the same stimulating force. According to Fig. 8, the output voltage shows an acceptable degradation in the beginning 200 cycles, especially the first 100 cycles. It is ascribed to the

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lodging of ZnO nanorods under external force. While the values of output voltage stay stable

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in the following cycles until 1000 cycles, indicating a good durability of the fabricated PENG

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device.

Fig. 7. Output performance of PENG. (a) Schematic diagram of test system. Output voltages (b) and currents (c) by finger bending and palm clapping. One cycle of output voltages (d) and currents (e) by finger bending and palm clapping. 13

ACCEPTED MANUSCRIPT Additionally, the capability of the ZnO-T-PENG for human energy harvesting and to power micro electronics were demonstrated. A 5 cm × 5cm size ZnO-T-PENG device was fabricated and fixed on PET plates. By colltcting energy from palm clapping, the

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ZnO-T-PENG can provide electricity for miniature display screens, as shown in Fig. 9(a).

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Fig. 8. Electric output stability test of the ZnO-T-PENG.

Fig. 9. Applications of the ZnO-T-PENG. (a) Photograph of ZnO-T-PENG powering a miniature display screen by palm pressing. (b) Photograph of ZnO-T-PENG lighting several LEDs by foot stepping. 14

ACCEPTED MANUSCRIPT Likewise, several Light Emitting Diodes (LEDs) LEDs can be light by foot stepping, as shown in Fig. 9(b). As mentioned above, this kind of ZnO-T-PENG possess the ability to harvest the energy

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from human bodies and power for micro-electronic devices, such as miniature display and LEDs. Most importantly, this kind of ZnO-T-PENG combines the advantages of textile

promoting the development of wearable electronics.

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4. Conclusion

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materials, such flexibility, elasticity, wear comfort and so on, and the function of PENG,

In summary, we have fabricated a flexible ZnO-T-PENG which consists of vertically arranged ZnO nanorod arrays sandwiched between two symmetrically layers of Ag coated-fabrics. A facile screen printing method was used to coat the surface of nylon fabric

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with silver paste, and a novel hydrothermal method which need single precursor solution was employed to synthesize ZnO nanorod arrays. By controlling the concentration of reaction

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precursor solution, content of ammonia solution, reaction temperature and time and so on, the ZnO nanorod arrays which are uniformly, densely, and vertically arranged on the surface of

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Ag coated-fabric, have been synthesized successfully. To harvest mechanical energy from human body, the as-fabricated PENG device is attached to human fingers and palms. By converting the energy from palm clapping and finger bending, this PENG can produce output voltages and currents as high as 4 V and 20 nA , 0.8 V and 5 nA respectively. The ZnO-T-PENG can power for micro-electronic devices by harvesting energy from human body. This kind of PENG exhibits superior flexibility and wearability which can promote the development of wearable electronics. 15

ACCEPTED MANUSCRIPT Conflict of Interest The authors declare no conflict of interest.

Acknowledgments

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This study was supported by grants from Donghua University (101-02-000120).

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S. N. Cha, J. S. Seo, S. M. Kim, H. J. Kim, Y. J. Park, S. W. Kim, J. M. Kim, Sound-driven piezoelectric nanowire-based nanogenerators, Adv. Mater. 22 (2010) 4726–4730. R. Yang, Y. Qin, C. Li, G. Zhu, Z. L. Wang, Converting biomechanical energy into electricity

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by a muscle-movement-driven nanogenerator, Nano Lett. 9 (2009) 1201-1205.

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ACCEPTED MANUSCRIPT Highlights： ·ZnO nanorods arrayed uniformly, vertically and with high density on the surface of Ag coated-fabric has been synthesized using novel method.

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· Coupled piezoelectric and semiconducting properties of ZnO nanorods are characterized using AFM analysis.

·Sandwich structured ZnO nanorods patterned textile-based PENG (ZnO-T-PENG)

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and detailed working mechanism.

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·This kind of ZnO-T-PENG possesses the ability to harvest energy from human

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bodies, promoting the development of wearable electronics.