Isotropic Paper Directly from Anisotropic Wood: Top-down Green

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Isotropic Paper Directly from Anisotropic Wood: Top-down Green Transparent Substrate Toward Biodegradable Electronics Mingwei Zhu, Chao Jia, Yilin Wang, Zhiqiang Fang, Jiaqi Dai, Lisha Xu, Dafang Huang, Jiayang Wu, Yongfeng Li, Jianwei Song, Yonggang Yao, Emily Hitz, Yanbin Wang, and Liangbing Hu ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b08055 • Publication Date (Web): 01 Aug 2018 Downloaded from http://pubs.acs.org on August 2, 2018

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ACS Applied Materials & Interfaces

Isotropic Paper Directly from Anisotropic Wood: Top-down Green Transparent Substrate Toward Biodegradable Electronics Mingwei Zhu,1,2 (a)* Chao Jia,2 (a) Yilin Wang,2 (a) Zhiqiang Fang,2 Jiaqi Dai,2 Lisha Xu,2 Dafang Huang,1 Jiayang Wu,1 Yongfeng Li,2 Jianwei Song,2 Yonggang Yao,2 Emily Hitz,2 Yanbin Wang,2 Liangbing Hu2,* 1

National Laboratory of Solid State Microstructures & College of Engineering and Applied Sciences, Nanjing University, Nanjing 210093, China 2

Department of Materials Science and Engineering, University of Maryland, College Park, Maryland, 20742, USA Email: [email protected]; * [email protected] (a) Equally contributed

Keywords: Wood, Isotropic, Transparent paper, Cellulose nanofibers, Green electronics

ACS Paragon Plus Environment

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ABSTRACT Flexible electronics have found useful applications in both the scientific and industrial communities. However, substrates traditionally used for flexible electronics, such as plastic, cause many environmental issues. Therefore, a transparent substrate made from natural materials provides a promising alternative, since it can be degraded in nature. The traditional bottom-up fabrication method for transparent paper is expensive, environmentally unfriendly, and time consuming. In this work, for the first time, we developed a top-down method to fabricate isotropic, transparent paper directly from anisotropic wood. The top-down method includes two steps: a delignification process to bleach the wood by lignin removal; and a pressing process for removing light-reflecting and -scattering sources. The resulting isotropic, transparent paper has high transmittance of about 90% and high haze over 80%, demonstrated as a nature-disposable substrate for electronic/optical devices. Adjusting the pressing ratio used changes the density of the resulting paper, which tunes the microstructure-related properties of the isotropic, transparent paper. This top-down method is simple, fast, environmentally friendly and cost-effective, which can greatly promote the development of paper-based green optical and electronic devices.


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1. INTRODUCTION Recently, flexible electronics have garnered tremendous attention in both scientific and industrial communities. Flexible electronics are fabricated on a substrate typically made of plastic film, flexible glass, or metal foil. Among them, plastic film is the most common. However, as the growing consumption and rapid life-cycle shrinkage of electronic devices occurs, a large amount of plastic waste from electronics has been produced, having serious implications for environmental and human health. Transparent paper, made of natural cellulose fibers, is one of the most attractive and sustainable candidates to replace traditional substrate materials.1–10 It has many advantages, such as high transparency, mechanical flexibility, high strength and heat resistance. 9,11–18 More importantly, it can be returned to nature without causing environmental problems. Recently, transparent paper has been demonstrated as an excellent transparent and flexible substrate for optoelectronic devices.19–28 Transparent paper can be manufactured by (1) simply impregnating ordinary paper with transparent materials (epoxy resin, acrylic resin, oil, wax etc.); (2) immersing opaque paper into various solvents, such as sulfuric acid, ionic liquids, etc., to dissolve portions of the cellulose on the surface of cellulose fibers; (3) using molecular cellulose, cellulose nanofibers (CNC, CNF, bacterial cellulose nanofiber, etc.) as building units. Traditionally, transparent paper is fabricated by a bottom-up method, which mainly includes two

steps: mechanical or chemical disintegration of cellulose nanofibers from wood; and

formation of a cellulose nanofiber network by different manufacturing techniques (Figure 1, iiv).1 The key technology in the bottom-up fabrication method is to disintegrate the natural cellulose microfibers into nanofibers to eliminate apparent light scattering.10,12,29 However, the separation, rinsing, and concentration of nanofibers cause the traditional bottom-up method to be


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very low efficiency, high cost and environmentally unfriendly. Therefore, a revolutionary fabrication approach is highly demanded. Here, we develop a top-down method for fabricating transparent paper that eliminates the need for disintegration of the cellulose nanofibers from the wood. The top-down method includes two straightforward steps: the colorful lignin is removed to eliminate light absorption (Figure 1, Step 1); then, the delignified wood slice is pressed to remove most of the light reflecting and scattering sources (Figure 1, Step 2), becoming optically uniform and transparent.30 This topdown fabrication eliminates the complicated and time-consuming process of nanofiber fabrication and separation required in the traditional bottom-up approach (Figure 1, Step i-iv). As a result, it consumes much less chemicals, water and time. The top-down method introduces a new way to fabricate transparent paper in a simple, efficient and environmentally friendly way.


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Figure 1. Comparison of transparent paper fabrication methods: our newly-developed top-down method vs. the traditional bottom-up method. (1)-(2) The top-down method including two steps. Step (1) involves the removal of lignin from the wood while preserving the cellulose framework. Step (2) includes mechanically pressing the anisotropic wood, and the anisotropic wood turns to the isotropic, transparent paper. (i)-(iv) The traditional bottom-up process, showing only the main steps. Step (i) is a delignification process; Step (ii) is a chemical process to obtain microsized cellulose fibers; Step (iii) is a mechanical process to reduce the fibers to nanometer-scale diameter; and Step (iv) is the process to filter and press the nanofibers, producing transparent paper.

2. EXPERIMENTAL SECTION


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Materials and Chemicals. Basswood was used with a size of 2 inches by 2 inches. The sodium hypochlorite solution was from SIGMA-ALDRICH (reagent grade, available chlorine 10-15 %) for removing lignin contents from wood. The polyethylene oxide (PEO, Mw = 100,000) and LiClO4 were from SIGMA-ALDRICH. Isotropic Paper Fabrication. The wood slices were immersed in the sodium hypochlorite solution for 2-4 hours (wood:NaClO = 1:40wt). After the wood slices turned to white, they were washed by water and ethanol mixtures (1:1wt) for three times. Then the lignin removed wood slices were covered with microporous filtering film and filter paper, respectively. Finally, they were put in a pressing machine (VHP-5T-4, MTI) at room temperature and pressed at different pressure for about 0.5-3 hours to obtain transparent paper. It should be noted that the pressure is gradually applied to make sure that water can be expelled from the paper. The final pressure values are about 0.3, 1.0 and 5.0 MPa for press ratio of about 3.3, 7.3 and 10.5, respectively. The densities of the resulted paper are about 0.5, 1.0 and 1.4 g/cm3, respectively. Electrolyte-Gated Graphite Transistor. Firstly, the Graphite flakes are transferred to the isotropic paper. Then, the Au contact electrodes about 50nm in thickness are fabricated by a shadow mask method with standard lithography processes. The electrolyte consisting of LiClO4 and PEO is prepared in the weight ratio 0.12:1. The electrolyte was mixed with methanol and then stirred overnight at room temperature. Measurements and Characterizations. The morphologies of wood were characterized by a scanning electron microscope (SEM, Hitachi SU-70). To improve image quality, AuPd coating was performed at 0.13 Torr Ar atmosphere with 10 mA current for 100-150 seconds (Anatech Hummer X magnetron sputtering machine) before SEM imaging. The surface morphology was characterized by an Asylum Research Cypher-ES atomic force microscope (AFM). The


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transmittance spectrum and haze were measured with a UV-Vis Spectrometer Lambda 35 (PerkInElmer, USA.). XRD were collected using multi-layered films on a Rigaku RAPID II equipped with a curved detector manufactured by Rigaku Americas Corp (operating tube voltage at 40 kV, tube current at 30 mA, CuKα, λ = 0.1541 nm). The performance of the transistor is measured by Keithley 2400. A fixed gate voltage and a fixed source-drain voltage are applied, source-drain current is measured continuously before and after adding the electrolyte. The mechanic properties are performed using a Tinius Olsen H5KT testing machine.

3. RESULTS AND DISCUSSION The fabrication of transparent paper directly from wood is facile and effective (Figure 2). First, a wood block is sliced perpendicular to the wood growth direction with a preset thickness (Figure 2a and Figure S1). A delignification is used to remove most of the lignin. After delignification, while the basic framework of the wood slice is preserved without destroying its basic framework (Figure S2).30 This partially frees the cellulose nanofibers, allowing them to shift during pressing. Finally, the wood slice is transformed to a transparent paper by pressing (Figure 2d). The resulted isotropic, transparent paper is dense and uniform with strong tensile strength of about 150 MPa. It shows both high transmittance and high haze. The characters underneath the isotropic, transparent paper can be clearly seen only when they are in close contact with the paper (Figure 2d). The sharp change in appearance is indicative of the considerable difference in microstructure between the original porous wood slice (Figure 2b), and the very dense paper that results after pressing (Figure 2e). The high density is achieved by a reduction in thickness of the sample, leading to significantly suppressed light scattering in the


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paper compared to the original wood slice. As a result, most of the light passes through and the paper exhibits high transparency. The original wood slice is naturally anisotropic with well aligned micro-channels i.e. lumen (Figure 2b). Most of the cellulose nanofibers and molecular chains are also aligned inherently,31 which is proved by the XRD pattern in inset of Figure 2b and Figure 2c. The isotropic paper can only be obtained by pressing the anisotropic wood slice along the lumen axis direction. If the applied press force deviates from the lumen axis, an anisotropic paper with aligned cellulose fibers will be obtained.32 The isotropy of the paper is proven by the XRD pattern (inset in Figure 2e), where high intensity diffractions form a circle, indicating the random distribution of cellulose molecules chains in the transparent paper. The isotropy of the paper is also directly observed by the atomic force microscopy (AFM) image shown in Figure 2f. The cellulose nanofibers are randomly stacked in paper. All the above results show that the isotropic paper can be directly made from anisotropic wood by the top-down fabrication method.


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Figure 2. Morphology and microstructure transformation from anisotropic wood to isotropic, transparent paper. (a) Photo and (b) SEM images of the natural wood slice. (c) SEM image of anisotropic wood cellulose nanofibers. (d) and (e) Photo and SEM images of transparent paper, respectively. (f) AFM image of the transparent paper isotropic nanofibers. SEM images of (b) and (e) show that the microstructure and thickness change from the anisotropic wood slice to the isotropic, transparent paper. The X-Ray diffraction patterns in (b) and (e) insets show the anisotropic and isotropic arrangements of cellulose molecules in natural wood slice and transparent paper, respectively.

The top-down method allows convenient tuning of the density of the resulting paper through a simple adjustment of the press ratio (Figure 3a), where press ratio is defined as a ratio of the thickness of the raw wood slice over the thickness of the resulted paper. The isotropic papers with press ratios of 3.3, 7.3 and 10.5 were fabricated, as shown in Figures 3b-3d. All papers have relatively flat surfaces. With higher press ratios, the thicknesses are gradually reduced. Isotropic papers with different press ratios display different optical properties corresponding to their microstructure changes. As shown in Figure 3e, the lower press ratio results in lower total transmittance. However, with a press ratio of 7.3, the total transmittance reaches a maximum value of about 90%. Notably, the total transmittance does not increase further for higher press ratios, as confirmed by the 90% transmittance value for the paper with press ratio of 10.5. Nevertheless, the haze measurement results show a different tendency. The haze continually decreases as the press ratio is increased (Figure 3f). All of these properties originate from the microstructure differences in the resulting paper. Lower density paper contains more tiny spaces among the fibers and thus more refractive index inhomogeneity, with


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each interface acting as a light scattering source. More scattering sources lead to higher haze and lower transmittance. Modulation of a paper’s pressing conditions provides a facile way to tune structure-dependent properties such as the optical haze and transmittance.

Figure 3. Tuning of isotropic paper via different press ratios. (a) Lignin-removed wood is pressed with different ratios of PR = 3.3, 7.3 and 10.5. The resulting isotropic paper samples are shown in the SEM images of (b), (c) and (d), respectively. (e) Diffused transmittance of the isotropic papers with different press ratios. The inset shows the relationship between the transmittance and the press ratio. Total transmittance tends to increase with higher press ratios


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until a press ratio of about 7.3, after which point the transmittance changes very little. (f) Diffused transmittance haze of the isotropic papers with different press ratios. The inset shows dependence of the haze of the resulting paper on the press ratio. The higher the press ratio, the lower the haze value.

The resulting isotropic, transparent paper is an ideal biodegradable substrate for electronic and optical devices, which can be disposable without causing many environmental problems. Here, we demonstrate a fabrication of a graphene transistor on the isotropic, transparent paper substrate, as shown in Figure 4a. The device relies on the principle of electrolyte gating, which causes an electrical double layer to form at the electrolyte/graphene interface, tuning the carrier density in the graphene flake and thus its conductivity. The thin graphene flake is obtained by mechanical exfoliation (Scotch tape method) on the isotropic paper and the electrical contacts are defined with shadow mask. The source-drain current Isd and the source-drain voltage Vsd exhibit a linear relationship, showing a typical Ohmic contact (Figure 4b). After adding the electrolyte (PEO/LiClO4), as shown in Figure 4c, the source-drain current changes as a function of the gate voltage, showing bipolar transistor behavior. The results demonstrate that the isotropic transparent paper can serve well as the substrate for flexible electronic devices, competitive with other common substrates such as SiO2 on a silicon wafer.


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The device fabricated on the isotropic, transparent paper is biodegradable. As a demonstration, the device is placed in soil and left exposed to the elements in nature (Figure 4d). Originally, the electrode structure has perfectly-defined conductive lines and the device is intact (Figure 4d). After 6 days, the electrode structure is destroyed and loses its function because of the broken of the conductive lines (Figure 4e). The paper slowly breaks down and is returned to nature, illustrating the small environmental effect such biodegradable devices will cause.

Figure 4. Demonstration of isotropic paper as the substrate for electronic device and its transient property. (a) Optical image of a graphene transistor device. Isotropic paper is used as the substrate, and the electrodes are fabricated on the surface of the isotropic paper. (b) Experimental result of the source-drain current as a function of the source-drain voltage, showing a typical Ohmic contact. (c) Experimental result of the source-drain current as a function of the gate voltage at a source-drain voltage of 10 mV, showing bipolar transistor behavior. (d) Schematic of


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the device deposited in nature and (inset and right) zoomed-in optical images of the original device. (e) The device is environmentally degraded after exposing it in nature for 6 days, which will have a minimum effect on the environment.

The new top-down method exhibits many superior characteristics: the process is much simpler, more environmentally friendly, and more cost-effective compared to the traditional bottom-up method (Figure 5). The traditional approach is extremely time-consuming, often requiring days to complete33 due to the many low efficiency fabrication steps involved, such as the nanofiber fabrication, filtration process (separating nanofibers from solvent) and drying process (separating residual solvent from nanofibers). In contrast, our top-down method is much more efficient and can be finished in less than five hours. Our procedure also boasts an improved environmental impact and cost savings over conventional methods due to its use of several times less water, energy, and chemicals (Figure 5c).


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Figure 5. Comparison of the top-down method and the bottom-up method for fabricating the isotropic, transparent paper. (a) The top-down method, which adopts two simple steps and uses only one kind of chemical. (b) The bottom-up method, which uses many chemicals and complicated instruments. (c) Comparison of estimated consumptions of time, chemicals, water and energy in the top-down method and the bottom-up method.

4. CONCLUSIONS Transparent paper made of natural cellulose nanofibers was a potential replacement material for plastic film. It is both environmentally friendly and can decompose in nature. However, transparent paper made by the traditional method is too expensive to be widely used. For the first time, we demonstrated that isotropic, transparent paper can be directly obtained from anisotropic wood. A top-down method including two steps, delignification and pressing, is developed. The resulting isotropic, transparent paper has high transmittance (~90%) and high haze (over 80%),


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and proves to be an excellent substrate for disposable electronic and optical devices without causing environmental problems. This work provides a simple, environmentally friendly and cost-effective method for fabricating the transparent paper, which will promote the development of environmentally conscious optical and electronic devices.


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ASSOCIATED CONTENT Supporting Information. The detailed fabrication processes, structure changes during the fabrication, mechanical property, flexibility, paper made from beech wood are in the contents of the material supplied as Supporting Information.

ACKNOWLEDGEMENT We acknowledge the financial support from National Key Research and Development Program of China (No. 2018YFB1105400).

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Table of Content (TOC) Figure:

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Figure 1 177x117mm (300 x 300 DPI)


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Figure 2 177x90mm (300 x 300 DPI)



Figure 3 177x124mm (300 x 300 DPI)


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Figure 4 177x106mm (300 x 300 DPI)



Figure 5 177x98mm (300 x 300 DPI)


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Isotropic Paper Directly from Anisotropic Wood: Top-down Green

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