Recent Advances in Controlling the Depositing Morphologies of

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Recent Advances in Controlling the Depositing Morphologies of Inkjet Droplets Jiazhen Sun, Bin Bao, Min He, Haihua Zhou, and Yanlin Song ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.5b07006 • Publication Date (Web): 07 Dec 2015 Downloaded from http://pubs.acs.org on December 12, 2015

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ACS Applied Materials & Interfaces

Recent Advances in Controlling the Depositing Morphologies of Inkjet Droplets Jiazhen Sun,† Bin Bao,‡ Min He,‡ Haihua Zhou,‡ and Yanlin Song*,†,‡ †

School of Chemistry and Environment, Beihang University, Beijing 100191, China

‡

Key Laboratory of Green Printing, Institute of Chemistry, Chinese Academy of Sciences,

Beijing Engineering Research Center of Nanomaterials for Green Printing Technology, Beijing National Laboratory for Molecular Sciences, Beijing 100190, China KEYWORDS: depositing morphology, inkjet droplets, coffee ring effect, wettability, pattern, droplets coalescence

ABSTRACT

Inkjet printing has been widely used in functional material patterning for fabrication of optical/electrical devices. The depositing morphologies of inkjet droplets are critical to the resolution and performance of resulted functional patterns. This review summarizes various strategies to control the depositing morphologies of inkjet droplets, including suppressing and utilizing coffee-ring effect, employing liquid substrates, developing patterned substrates and controlling droplets coalescence. Moreover, the remaining challenges in controlling inkjet droplets are presented, and the broad research and application prospects of controlling nanomaterial patterning by inkjet printing are proposed.

ACS Paragon Plus Environment

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Introduction Patterning functional materials has aroused wide attention due to its promising applications in

optic/electronic devices,1-3 sensors,4,5 biochips,6,7 displays8,9and other devices. Comparing with the conventional patterning technologies, such as lithographic printing,10,11 nano-imprinting12,13 and micro-contact printing14-16, inkjet printing is a direct depositing technique using the liquid phase materials.17-19 By virtue of its low-cost, convenience, flexibility and speediness, inkjet printing has attracted great attention for fabricating high-quality patterns.20-22 In recent years, with the high-resolution pattern fabrication,23,24 inkjet printing has made important progress in green-platemaking technology,25 transparent conducting film,26 organic semiconductor,27 light-emitting diode,28 solar cell,29 biochip,30 RFID antenna,31 sensor,32-35 etc. As the depositing morphologies of inkjet droplets directly influence the resolution and performance of printed patterns, it is of great significance to control the depositing morphologies of inkjet droplets, which are affected by complex factors, such as substrate wettability, ink rheology, printing apparatus and external field. So far, it is still a tough process to precisely control the inkjet droplets to form desired morphologies. In this paper, we review various strategies to control the depositing morphologies of inkjet droplets. Firstly, the depositing morphologies of droplets based on suppressing and utilizing coffee ring effect are discussed. Then the behavior of inkjet droplets on liquid substrates, such as slippery substrate and viscoelastic substrate, is introduced. Furthermore, the inkjet printed morphologies on patterned substrates are described. Moreover, the coalescence of inkjet droplets for constructing lines, films and 3D structures is discussed. Finally, the remaining challenges in controlling inkjet droplets are presented, and the broad research and application prospects of controlling nanomaterial patterning by inkjet printing are proposed.


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The depositing morphologies of inkjet droplets based on coffee ring effect When one droplet dries on a substrate, the inside solutes prefer depositing along the periphery

and leaving a ring-like deposit.36,37 This phenomenon is known as coffee ring effect, which is commonly observed during inkjet printing process and influences the depositing morphologies of inkjet droplets.38 In recent years, many high performance devices have been fabricated by inkjet printing technology based on suppressing or utilizing coffee ring effect. Here we will discuss the forming mechanism of coffee ring effect as well as how to suppress or utilize it in inkjet printing. 2.1 Forming mechanism of coffee ring effect In the past few decades, researchers have made great progress in revealing the forming mechanism of coffee ring effect. As the specific surface area at every point of evaporating droplets is different, the height reduced by the evaporation flux is non-uniform, and the evaporated volume in the central area is smaller than the volume in the edge area. When one droplet has a pinned three phase contact line (TCL), the excess solvent lost at the edge is replenished by solvent in the center, leading to a radial capillary flow. The capillary flow carries the solutes in evaporating droplet towards the pinned TCL, thus the ring-like morphology is formed (Figure 1a).39 The actual motion of evaporating droplet to maintain an equilibrium shape is shown in Figure 1b. With depinned TCL, the boundary of droplet shrinks due to the non-uniformity of evaporating droplet. As the evaporation removes the hashed layer, the interface will move from the solid line to the dashed line, and the contact line will move from A to B (Figure 1b (i)). With pinned TCL, the retreat from A to B is impossible, and there must be a flow that replenishes the lost fluid (Figure 1b (ii)).40,41 Therefore, the outward capillary flow occurs with the non-uniformity of evaporating droplet and the pinned TCL.


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Figure 1. The forming process of “coffee ring” effect. (a) The non-uniformity of evaporating droplet, the shaded annular region represents the evaporated volume in the central area is smaller than the volume in the edge area. Thus liquid flows outwards to supply the deficit volume (left) and the microsphere migration of a 2-cm-diameter drying drop was observed in a video micro-scope, the solute driven to the edge by evaporation flux (right). Reproduced with permission from ref 39. Copyright 1997 Macmillan Publishers Ltd. (b) The optical image of one ring-shaped depositing morphology, the diameter of deposit is approximate 5 cm (left) and the actual motion of droplet with depinned TCL (i) or pinned TCL (ii) (right). Reproduced with permission from ref 41. Copyright 2000 American Physical Society. 2.2 Depositing morphologies via suppressing coffee ring effect 2.2.1 Weakening Outward Capillary Flow When an evaporating droplet contacts substrate with pinned TCL, the non-uniformity of evaporating droplet happens. Then the outward capillary flow carries the solutes to the edge of evaporating droplet and induce a ring-like deposit. Therefore, many methods were investigated to weaken the outward capillary flow for suppressing coffee ring effect. Firstly, regulating the


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condition of solvent evaporation can reduce the influence of outward capillary flow, such as employing the cooled substrate, raising the ambient humidity or reducing the droplet scale. Soltman et al. found that the evaporation rate was more retarded at the droplet edge than that in the center on a cooled substrate, which decreased the non-uniformity of evaporating droplets.42 Though Marangoni recirculation would occur from edge to center, the effect of capillary flow was generally greater than the Marangoni recirculation in this case. Therefore, the cooled substrate weakened the coffee ring effect. Tokito et al. reported that the cross-sectional profile of printed pattern could be controlled from concave to convex by increasing ambient humidity.43 The higher humidity level would reduce the solvent evaporation rate. According to the Peclet number: Pe=J0L/D, the solvent evaporation rate (J0), the size of the droplet (L) and the diffusion coefficient (D) influence the final shape of the film. A larger value D leads to a convex shape, because the diffusion tends to homogenize the concentration field contrary to the outward flow. When the Peclet number < 1, the diffusion is strong and uniform profiles are expected, while the Peclet number > 1, the non-uniform profiles are a result.44,45 The high humidity level did not influence D but did J0. Thus the cross-sectional profile of printed pattern was convex in high humidity level. Wong et al. studied the influence of droplet scale to the depositing morphology.46 As the solvent evaporation rate was much faster than the solute movement rate, the time competition between solvent evaporation and solute movement in droplet would influence the depositing morphology of inkjet droplet. With droplet size shrinking, the solvent was dried out rapidly and there was not enough time for transferring the solute to the edge of droplet. Thus the coffee ring effect was inhibited. Secondly, the interactions among particles can influence the depositing behavior of solutes in drying droplets, which can be used to weaken the outward capillary flow.47,48 Yodh et al. found that anisotropic particles could suppress the coffee ring


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effect effectively.49 The outward capillary flow carried the ellipsoids to air-water interface, the strong long-ranged attractions between ellipsoids would be generated.50,51 The loosely packed structures in the air-water interface could prevent the suspended particles from reaching the droplet edge (Figure 2a). Song et al. prepared monodispersed core-shell latex spheres consisting of a hydrophobic polystyrene core and a hydrophilic poly (methyl methacrylate)/poly acrylic acid shell. The soft shell provided a strong assembling force by hydrogen bonding among particles to resist the influence of outward capillary. Then a large-area high quality multi-stopbands photonic crystal (PC) was fabricated (Figure 2b).52 Besides, sol-gel transition and depletion flocculation are effective strategies to weaken the outward capillary flow and influence the distribution of particles in a drying droplet.53,54 Jaeger et al. found when the monodispersed dodecanethiol-ligated gold nanocrystals were transferred on the liquid-air interface in toluene droplet, a highly ordered monolayer structure would generate and prevented the nanocrystal from reaching the droplet edge (Figure 2 c).55 Thirdly, introducing responsive materials with corresponding external fields can also be used to limit the outward capillary flow. Baigl et al. inkjet printed the ink contained photosensitive cationic surfactant, the photosensitive droplets offered reliable modulation of depositing morphologies. When droplet was applied a UV illumination, particle stickiness was optically controlled, sticky particles were trapped at the air-liquid interface during evaporation and homogeneous disk-shaped deposit was formed (Figure 2 d).56,57 Besides, temperature is another common external field for inhibiting the coffee ring effect with thermal responsive materials.58


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Figure 2. Controllable morphologies by weakening outward capillary flow. (a) Up: Outward flows carried elliptical particles from the inside of droplet to the air-water interface. Reproduced with permission from ref 50. Copyright 2013, American Physical Society. Down: Distribution images of ellipsoids and spheres after evaporation. Insets show the particle shapes. Reproduced with permission from ref 49. Copyright 2011, Macmillan Publishers Ltd. (b) UP: TEM image of latex spheres, scale bar: 100 nm and scheme of ‘‘paint on’’ effect among soft shells of latex spheres. Down: High-ordered structure with the monodispersed core-shell latex spheres and photograph of the multi-stopbands PC, scale bar: 1cm. Reproduced with permission from ref 52. Copyright 2009, Royal Society of Chemistry. (c) UP: Micrograph of a drop-casted monolayer with solution of dodecanethiol-ligated gold nanocrystals onto a Si3N4 substrate. The inset shows arrangement of two neighboring nanocrystals (left). Top view of the fully formed, compact nanocrystal monolayer (right). Down: Schematic diagram of self-assembly process during drying


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stages, showing how nanocrystals were captured by a quickly receding air-liquid interface. Reproduced with permission from ref 55. Copyright 2011, Macmillan Publishers Ltd. (d) Scheme shows the formation of a disk-shaped deposit from individual evaporation drop with light control. The photographs of the resulting pattern after complete evaporation of all the droplets illuminating for 5 minutes. Magnified image showing a disk-shaped and a ring-shaped deposit with exposing to UV light or protecting from UV light. Reproduced with permission from ref 57. Copyright 2014 Wiley. 2.2.2 Increasing Inward Marangoni Flow In 1865, C. Marangoni found that high surface tension liquid has a larger pull force on surrounding fluid than low surface tension liquid. The concentration or temperature gradient along the droplet surface can induce a surface-tension gradient, then a recirculatory flow will occur by a shear stress at the surface due to the surface tension gradient needs to be balanced by a velocity gradient in the bulk. The flow carries the particles that are near the surface to the top of droplet, which is called Marangoni Flow.59 The Marangoni flow is generally contrary to the direction of capillary flow and transports the solute to the center rather than the edge of droplet. So regulating the Marangoni flow in a drying droplet can control the evaporation-driven depositing and functional materials assembling. Hu et al. confirmed one Marangoni flow driven by surface-tension gradient produced with latent heat of evaporation, and the deposition occurred preferentially at the center of the droplet.60 In previous work, researchers have reported some methods to produce a Marangoni flow with the concentration gradient by adding compositional solvent. Moon et al. inkjet printed the homogeneous conductive patterns by adding high boiling point and low surface tension ethylene glycol (EG) to the water-based Ag conductive ink. The unbalanced evaporation induced a concentration gradient of EG, then an additional Marangoni


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flow was formed from the outer rim to the center to improve film morphology (Figure 3 a).61 Similarly, the fast responsive PC microdots were prepared by the compositional solvents.62 Cho et al. added high boiling point and low surface tension dodecane to a chlorobenzene ink. The solvent compositions resulted in a Marangoni flow to fabricate the self-aligned crystals (Figure 3 b).63 Besides, introducing a solvent surrounding is another way to produce a concentration gradient on droplet surface. Pasquali et al. obtained uniform deposition of nanoparticles in aqueous suspensions by drying the aqueous nanoparticle droplet in an ethanol vapor atmosphere. The absorption of ethanol from the saturated ethanol environment generated a surface tension gradient, and a strong recirculating flow was produced to induce a homogenous deposit (Figure 3 c).64 Moreover, surfactants also can be used to induce the Marangoni flow in a drying droplet.65 Still et al. demonstrated that ionic surfactant sodium dodecyl sulfate added to colloidal droplets could lead to a uniform depositing morphology. The outward capillary flow drew the surfactant to the edge of droplet, and the surface-tension gradient was produced to induce a stable Marangoni eddy.66 Sempels et al. discovered that a living bacterial system auto-produced surfactants to create a homogeneous deposition. The Marangoni flow was induced by the surfactant concentration gradient, and the coffee ring effect was effectively inhibited. In this way, the bacteria was prevented from depositing at the drop perimeter and the survivability was improved (Figure 3 d).67 In addition to increasing inward Marangoni flow by the concentration gradient,68 research on temperature gradient maybe also a significant strategy to control the depositing behavior of inkjet droplet.


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Figure 3. Controllable morphologies by increasing inward Marangoni flow. (a) Confocal laser scattering microscopic three-dimensional images for the depositing morphologies of single inkjet droplet with varying solvent compositions and the corresponding two-dimensional profiles. Reproduced with permission from ref 61. Copyright 2006, American Institute of Physics. (b) Up: The polarized images of inkjet droplets with chlorobenzene (left) and mixed-dodecane (right). Down: Schematic diagrams of the evaporating flows in drying droplet with compositional solvents. Reproduced with permission from ref 63. Copyright 2008 Wiley. (c) Up: Motion of particles in droplet with standard ambient. The outward capillary flow drove the particles to the edge, leading to a coffee ring structure. Down: Motion of particles in droplet with saturated ethanol environment. A higher surface tension generated at the top of droplet, and a Marangoni flow produced from the contact line to the top of droplet. The recirculating flow led to a uniform deposition. Reproduced with permission from ref 64. Copyright 2012 American Chemical


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Society. (d) The optical images of the corresponding bacteria distribution, and schematic diagrams of capillary flow and Marangoni flow without surfactants (up) and with surfactants (down). Reproduced with permission from ref 67. Copyright 2013 Macmillan Publishers Ltd. 2.2.3 Sliding of Three Phase Contact Line With the non-uniformity of evaporating droplet, the TCL of droplet will slide to maintain a balance on the depinned substrate.69,70 In this case, it is difficult for the solute in droplet to deposit at the edge with the depinned TCL, thus coffee ring effect can be avoided effectively. The influence of substrates to the self-assembled structure and spatial extent of colloidal silica in a drying droplet was shown in Figure 4a. A hemispherical assembly with ordered nanoparticle structure was fabricated on a hydrophobic surface.71 Similarly, the well-defined polymer structures were obtained on a hydrophobic perfluorinated substrate.72 The depinned TCL not only eliminates the formation of ring stains, but also provides a facile approach to fabricate high ordered structure of nanoparticles. Song et al. prepared substrates with different receding contact angles to study the depositing behavior of inkjet droplets. They found that the sliding TCL could help particles to move inwards and assemble into high height-to-diameter ratio PC domes (Figure 4 b).73 With the high ordered nanoparticles structure, surface enhanced Raman scattering-active spots were fabricated.74 Moreover, they inkjet printed silver nanoparticle arrays on a flexible hydrophobic substrate.75 The printed pattern could serve as the contacts of nanoscale circuits to fabricate flexible transparent conductive film with a sandwich structure of the patterned substrate, building blocks and a hydrophobic cover plate.76 Tsao et al. demonstrated the depositing behavior of small solutes or polymers on various contact angle hysteresis substrates. The concentrated stain was formed on substrate with weak contact angle hysteresis (Figure 4 c).77,78 Moreover, the depositing behavior of solutes in different drying


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stages can be used to control the final depositing morphologies. For example, Fairhurst et al. investigated the tall central pillars forming mechanism with sessile droplets of poly(ethylene oxide) during a 4-stage drying process.79,80 Theoretical analyses based on Peclet and Capillary numbers provide a strong support to study the influence of evaporation rate, diffusion and viscosity to the depositing morphologies of inkjet droplets.

Figure 4. Control of the depositing morphologies by the sliding three phase contact line. (a) Schematic diagram of assembling process and SEM images of depositing morphologies on different wettability surfaces, the low contact angle (up) and high contact angle (down). Reproduced with permission from ref 71. Copyright 2004 American Chemical Society. (b) Up: Scheme illustrates the assembling process of nanoparticles with the sliding TCL, nanoparticles in the droplet moving inwards and spontaneously assembling into PC domes. Down: images of printed dots with low receding contact angle (left) and high receding contact angle (right). The insets are the corresponding receding contact angles. Reproduced with permission from ref 73. Copyright 2014 Wiley. (c) The side view and top view images of solute in droplet forming a


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concentrated stain on the weak contact angle hysteresis substrate. Reproduced with permission from ref 77. Copyright 2013 American Chemical Society. 2.3 Depositing morphologies via utilizing coffee ring effect In additional to studying how to inhibit coffee ring effect in drying droplets, utilizing coffee ring effect has also been investigated for functional structure fabricating,81-85 nanoscale patterning,86,87 3D patterning,88 hybrid film fabricating,89 protein detecting90,91 and particle-size selecting92. The outward capillary flow can carry solute to the edge of evaporating droplet, which is an effective way to realize material patterning. In recent research, lots of complex structures have been achieved with the coffee ring effect by inkjet printing technology. Magdassi et al. inkjet printed the silver nanoparticle ink to form 150 µm diameter rings with width and height less than 10 µm and 300 nm respectively, the printed array of interconnected rings could be directly used as transparent conductive patterns (Figure 5 a).93 Then they fabricated a flexible transparent conductive pattern with the connecting carbon nanotube rings.94 Similarly, the detective device and transistor were directly obtained with the coffee ring effect.95,96 The coffee ring effect not only can be used for material enrichment, it also can be used for material transport. For example, Liu et al. inkjet printed N, N-dimethylformamide (DMF) on a polyacrylonitrile (PAN) coated substrate. The PAN on the substrate would be transported to the edge of droplet by DMF, then holes with a narrow interval were fabricated for patterning a graphene electrode pair with narrow channel (Figure 5 b).97,98 Magdassi et al. used the similar method to fabricate holes on a thin film composed of metal nanoparticles. The inkjet printed liquid pushed the metal nanoparticles away by the outward capillary flow, and a transparent film with a network of conductive materials was fabricated.99 The inkjet printing technology can easily manipulate droplets to fabricate lines and more complex patterns. Therefore, the motion of


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Ag nanoparticles in continuous droplets with pinned TCL was researched by Song’s group. They found that the capillary flow could drive the nanoparticles to the TCLs and help to form two parallel lines with 5-10 µm line width (Figure 5 c).100,101 Singler et al. also obtained twin continuous nanoparticle lines with the pinned TCL of consecutive drops.102 The printed polydopamine nanoparticle lines were used to fabricate patterns of high conductivity at near room temperature by electroless plating.103,104

Figure 5. Controllable morphologies by utilizing the coffee ring effect. (a) Up: SEM images of the whole printed ring and the rim, and the height profile graph of ring. Down: Transparent conductive film fabricated by the ring arrays. Reproduced with permission from ref 93. Copyright 2009 American Chemical Society. (b) Left: The schemes of fabricating details. 1. Spin coating the mask layer. 2. Dissolving the mask layer with inkjet printed pure solvent. 3. Patterned mask layer generated on the substrate. 4. Depositing graphene oxide layer. 5.


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Fabricating PS strengthening layer. 6. Peeling off the mask layer and the strengthening layer. Right: SEM images of the obtained conductive graphene electrodes with channel lengths of 1–2 µm under optimized conditions. Reproduced with permission from ref 97. Copyright 2012 Wiley. (c) Left: Schematic illustration of inkjet printing silver-nanoparticle lines based on coffee-ring effect. Right: Transmittance and optical image of the reticular conductive pattern on glass substrate. Reproduced with permission from ref 100. Copyright 2013 Wiley. 3.

The depositing morphologies of inkjet droplets on liquid substrates When droplet contacts with an immiscible liquid substrate, its wetting behavior is greatly

affected by the slippery or viscoelastic property of substrate.105 Aizenberg et al. developed an oil-infused slippery surface, in which the low-surface-energy fluoride silicone oil could restrict the permeation of most liquid.106 The dynamic dewettability and slippery property of liquid-solid composite substrate have been applied in many important domains, such as anti-fouling,107 anti-icing108 and fluid transportation109. Therefore, the liquid substrate offers a special surface to control the depositing behavior of inkjet droplets. Song et al. studied the wetting behavior of inkjet droplet on the liquid-solid composite substrate.110 They found that printed magnetic droplets could deform from hemispherical to pillared microstructure with droplet edge retracing under magnetic guiding, and a sequence of multiple microstructures, including hat, cone, pillar and spindle, were fabricated on the substrate (Figure 6a). The viscoelasticity is another characteristic of liquid substrate, which is different from the property of rigid solid substrate. When inkjet droplet impacts on viscoelastic liquid surface, the substrate can be used to wrap the droplet with the fluidity.111,112 Song et al. found that inkjet droplet could induce viscoelastic liquid PDMS surface to deform.113 With appropriate precuring degree, the high precision structure could be embedded in the substrate by inkjet printing. Then the concave


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microstructures were fabricated after solidifying the PDMS substrate and rinsing the polymer solute (Figure 6b). Furthermore, they studied the morphology of completely wrapped inkjet droplet in liquid substrate.114 The Rayleigh instability of inkjet droplet in liquid substrate was inhibited by adopting ink with viscosity sensitive to temperature. With the inkjet printed liquid template, microchannels could be conveniently fabricated (Figure 6c).

Figure 6. Control the printing morphology of inkjet droplet on liquid substrate. (a) Up: Schematic of inkjet printing 3D microstructure on slippery liquid-solid surface under magnet; Mid: Construction of the slippery surface by swelling PDMS with silicone oil. Illustration of the droplet deformation and retracting process. Down: Fabricating hat, cone, pillar and spindle microstructures with increased receding angles. Reproduced with permission from ref 110. Copyright 2015 Wiley. (b) Up: Schematic illustrations of three typical scenarios with the various


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precuring degree of PDMS substrates. Mid: Schematic illustrations of fabricating concave microstructure. Down: SEM images of the microdots and the microwells. Inserts are amplified images of dot and well, respectively. Reproduced with permission from ref 113. Copyright 2015 Wiley. (c) Left: Scheme for fabricating process of Y-shape microchannel. Right: Optical image of the microchannel. Insert: SEM images of cross and longitudinal section. Scale bar: 100 µm; (up) Optical image of branch-shape microchannel, scale bar: 50 µm; (down) Reproduced with permission from ref 114. Copyright 2015, Royal Society of Chemistry. 4.

The depositing morphologies of inkjet droplets on patterned substrates As patterned substrates can adjust the spreading and wetting of droplets with inhomogeneous

chemical or physical surfaces, many desired morphologies have been directly fabricated by inkjet printing on such patterned substrates. Firstly, the patterned substrate was considered to control the resolution and precision of inkjet printed pattern, which is generally determined by the size of single droplet and the interaction between droplet and substrate.115 Lam et al. employed the hydrophilic-hydrophobic patterned surface as the substrate in inkjet printing. They found the large wetting contrast between the hydrophilic area and the hydrophobic area provided a huge surface energy barrier to restrict the droplet spreading, and the resolution and accuracy of printed patterns were improved (Figure 7 a).116 Similarly, the uniform silver lines with 5-15µm width were fabricated on physical patterned substrate by confining the spreading droplets with capillary forces.117 List et al. inkjet printed an aqueous dispersion of nanospheres on a soft embossed polymer substrate. By interacting with the spheres and the undulated surface, a self-assembly process was triggered and a nanostructure was constructed.118 As two neighboring droplets tend to coalesce and release surface energy,119,120 it is difficult to achieve close patterns with small distance with direct inkjet printing. Then the patterned substrate was developed to


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solve this problem. With a narrow, repelling, hydrophobic polyimide line to confine the spreading of droplet on hydrophilic substrate, Sirringhaus et al. fabricated channels with 5 micrometers length by dewetting PEDOT/PSS water-based inkjet droplet on the patterned surface.121 With the high resolution hydrophobic line on the hydrophilic substrate, the conductive pattern with 500 nm length channel was achieved by the surface-energy-assisted inkjet printing (Figure 7 b).122 Furthermore, they reported a two-step inkjet printing methods: the first inkjet droplet was modified as a template by CF4-plasma treatment, then the second droplet was repelled to result in a sub-100 nm gap.123,124 Zhu et al. inkjet printed one droplet in situ formed a hydrophobic boundary without any intermediate treatment, which could repel subsequently deposited droplet to a consistent distance.125 This “double-shot” inkjet printing process provides a new way to fabricate functional materials.126,127 Moreover, the depositing morphologies of inkjet droplets are usually uniform on the homogeneous surface. To fabricate varying morphology with single inkjet droplet, Song et al. inkjet printed nanoparticles contained droplets on a hydrophobic-hydrophilic patterned substrate. The patterned substrate could induce asymmetric dewetting of inkjet droplet, and various morphologies with closely packed structures were obtained by assembling the nanoparticles (Figure 7 c).128 The controllable morphology of colloidal crystal can be served as multi-information carriers with multiple optical, location and morphology information. Comparing to the traditional methods, this work provides a facial method for fabricating 3D microstructures.129-131


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Figure 7. Control the printing morphology of inkjet droplet on patterned substrate. (a) Left: Fabricating flow of hydrophilic-hydrophobic patterned PET film. Right: Printed features with the patterned substrate (50 µm width, 100 µm spacing). Inkjet droplets spread on hydrophilic areas while non-wetted on hydrophobic areas. Reproduced with permission from ref 116. Copyright 2014 American Chemical Society. (b) Left: Schematic to illustrate PEDOT/PSS droplet dewetting with a FDTS/SiO2 mesa. Right: Photograph of depositing morphology of the dewetted PEDOT/PSS droplet. Reproduced with permission from ref 122. Copyright 2004 Macmillan Publishers Ltd. (c) Up: Schematic illustration of manipulating 3D morphology of droplet by asymmetric dewetting with a hydrophilic-hydrophobic silicon wafer. Down: SEM images of the assembled colloidal crystal structure. Mechanism scheme of nanoparticle assembly on the patterned surface. Reproduced with permission from ref 128. Copyright 2014 Willy.


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The depositing morphologies of coalesced inkjet droplets In recent years, there have been extensive reports on coalescing behavior between inkjet

droplets.132,133 The depositing morphologies of coalesced inkjet droplets can be controlled by regulating a dynamic balance between the forces driving shape relaxation and an opposing force for fabricating complex structures.134,135 The depositing morphologies of coalesced inkjet droplets are very important to fabricate lines, films and 3D structures. Generally, varying the droplet distance can directly achieve the inkjet printed line with the morphologies of individual, scalloped, uniform, bulging and stacked coins.136 Sun et al. analyzed the influence of droplet spacing and jetting delay to the interplay of drop spreading, evaporation, capillary relaxation and particle assembly processes with two consecutively printed colloidal droplets. They found that the depositing morphologies could be controlled by the droplet spacing and jetting delay.137 Riegler et al. investigated the coalescing behavior between miscible liquids with different surface tensions, and found that the induced Marangoni flow could delay the coalescing behavior of two droplets.138,139 Schubert et al. demonstrated that when the surface energy of substrate was low enough to limit the wetting of silver nanoparticle suspension, but high enough to prevent line bulging, the narrow conductive tracks could be obtained.140 Song et al. inkjet printed controllable footprint lines by regulating droplets’ surface tension and the nanoparticle concentration. The straight line could be obtained with appropriate surface tension difference (Figure 8 a).141 Recently, inkjet printing technology has been used to deposit film for optoelectronic devices.142-144 Schubert et al. investigated the influence of solvent mass ratio, print head velocity, dot spacing and multilevel printing method to obtain homogeneous polymer films. The results showed that the mixing solvent, decreasing the print head velocity, appropriate dot spacing and multilevel matrix deposition resulted in regular and smooth film (Figure 8 b).145 Furtherly, they


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studied structure and property of the inkjet printed films for preparing organic solar cells.146 Lee et al. demonstrated that morphology of organic nanocomposite structure can be controlled by droplet coalescence. They suggested the extent of droplet coalescence could vary solvent evaporation, supersaturation of solutes, and nucleation density of precipitating organic crystals.147 In addition, layer-by-layer depositing behavior of inkjet droplet coalescence is of significance for 3D structure fabrication.148-150 Brugger et al. demonstrated soft matter printing capabilities by characterizing and optimizing the spreading and gelation behavior of an individual microdroplet.151 Using alginate as a model system, the viable cells and branched microvasculature could be printed with suitable bio-ink and adapted 3D printing strategy in future. To fabricate 2D and 3D structures with sub-micrometer feature sizes, Poulikakos et al. employed dielectrophoresis-assisted on-demand printing of dielectric liquid-based gold nanoparticles.152 They found that uniform particle deposit could be obtained by filling up an initial ring-like deposit with the following droplet. The 3D structures could be controlled by introducing appropriate time-scales to adjust particle diffusion. Furthermore, they manufactured the 3D gold nanostructures by the electrohydrodynamic inkjet printing.153 The large aspect ratio nanostructures were fabricated by governing electrostatic field, the origin electrode structure could create strong electric-field gradients for focusing the incoming droplets to grow at a homogeneous diameter (Figure 8 c). This work provides an effective strategy to fabricate nanoscale device by inkjet printing technology, which is difficult to achieve by traditional inkjet printing technology.


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Figure 8. Control the depositing morphologies by coalescence of inkjet droplets. (a) Left: Schematic illustration of three types of coalescing inkjet droplets with spherical cap, line, and dumbbell structure, respectively. Right: Optical microscope images of printed PC lines. The lines showed vivid structure color with well-ordered nanoparticle assembly. Reproduced with permission from ref 141. Copyright 2014 American Chemical Society. (b) Up: Schematic illustration of multilevel matrix deposition with the order A1, A2, A3, B1, B2, etc. Down: Confocal scanning microscopy images and the corresponding profile graphs of inkjet printed polystyrene films. Reproduced with permission from ref 145. Copyright 2006 Royal Society of


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Chemistry. (c) Up: Schematic illustration of growing liquid meniscus and subsequent ejection of inkjet droplets from its apex applying a direct current voltage. The sharp structure consisting of dispersed nanoparticles has the ability to attract approaching charged droplets. Down: SEM images of the growth process of depositing pattern (scale bar: 150 nm). Reproduced with permission from ref 153. Copyright 2012 Macmillan Publishers Ltd. 6.

Conclusion and outlook In this paper, recent advances in precisely controlling the inkjet droplets to deposit desired

morphologies for fabricating high-performance devices have been summarized. Based on suppressing and utilizing the coffee ring effect, various depositing morphologies of inkjet droplets have been fabricated. To control the depositing behavior of inkjet droplets, liquid substrates and patterned substrates were employed. Besides, the coalescence of inkjet droplets was discussed to fabricate fine lines, films or 3D structures. Finally, the remaining challenges in controlling inkjet droplets are presented, and the broad research and application prospects of controlling nanomaterial patterning by inkjet printing are proposed. Despite a plenty of research devoted to the depositing morphologies of inkjet droplets, there are still many challenges to control the inkjet droplets. With detailed studies of the interactions between the droplets and the substrate,154 introducing external fields155,156 and special printing apparatuses155 will enhanced the controllability of inkjet droplet. Moreover, theoretical research on the solute distribution in the coalesced droplets is necessary for printing precise hetero-structure156 or 3D structure157. The movement of solute in one evaporating droplet is influenced by many complex factors, such as evaporation flux, diffusion flux and viscosity. Therefore, the quantitative relationship of the factors should be further clarified to accurately control the solute distribution. For the device fabricating process, there are still many challenges,


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such as to fabricate continuous lines with sharp edges and appropriate height-width ratio, as well as homogenous films with flat surface and adjustable thickness. Moreover, the resolution of inkjet printed pattern is usually limited to tens of micrometers, it is still a challenge to print high resolution patterns for fabricating micro/nano devices. In recent years, researchers have made good progress in this field by controlling the droplet with the sliding TCL69,73 and improving equipments160,161. In recent years, research on nanomaterials has become an advanced research hotspot in the field of new materials and devices. Nanomaterials have unique optical, electrical, thermal, catalytic and mechanical properties, enabling their promising applications in high performance devices. Recently, great progress has been made in patterning and applications of nanomaterial based inkjet inks,162 though it is still a challenge to disperse nanomaterials stably in ink. As an alternative, in-situ reactive inkjet printing has been proposed to fabricate the functional patterns that cannot be directly inkjet printed.69,126 Moreover, the controllable assembly of nanomaterials during the evaporating process of inkjet droplets provides a route to fabricate functional nanomaterial patterns in large-scale. It will be of great significance for practical applications such as electronic skins,163 wearable devices164 and stretchable conductors165. Due to the excellent performances of nanomaterial patterns, the promising applications in functional device fabrication and 3D printing technology could be foreseen in the near future.

AUTHOR INFORMATION Corresponding Author E-mail: [email protected]


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ACKNOWLEDGEMENTS We gratefully acknowledge financial support from the National Natural Science Foundation of China (Nos. 51173190, 51473173, 21303218, 21121001), the National Basic Research Program of China (973 Program) (No.2013CB933004), and the "Strategic Priority Research Program" of the Chinese Academy of Sciences (No. XDA09020000).

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Recent Advances in Controlling the Depositing Morphologies of Inkjet Droplets Jiazhen Sun,† Bin Bao,‡ Min He,‡ Haihua Zhou,‡ and Yanlin Song*,†,‡


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Recent Advances in Controlling the Depositing Morphologies of

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