WO2016076563A1 - Procédé d'impression de nanomotif de graphène, et appareil et encre utilisés à cet effet - Google Patents

Procédé d'impression de nanomotif de graphène, et appareil et encre utilisés à cet effet Download PDF

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Publication number
WO2016076563A1
WO2016076563A1 PCT/KR2015/011627 KR2015011627W WO2016076563A1 WO 2016076563 A1 WO2016076563 A1 WO 2016076563A1 KR 2015011627 W KR2015011627 W KR 2015011627W WO 2016076563 A1 WO2016076563 A1 WO 2016076563A1
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Prior art keywords
pattern
nano
graphene oxide
nozzle
printing
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PCT/KR2015/011627
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English (en)
Korean (ko)
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설승권
김정현
김대호
장원석
이건웅
한중탁
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한국전기연구원
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Priority to CN201580061448.7A priority Critical patent/CN107249858B/zh
Publication of WO2016076563A1 publication Critical patent/WO2016076563A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing

Definitions

  • the present invention relates to a method for printing a graphene nano pattern.
  • Graphene is one of the carbon allotropes composed of carbon atoms.
  • graphene refers to a two-dimensional single sheet composed of sp 2 hybrids of carbon and has a large surface area, and has excellent mechanical, thermal, optical and electrical properties, and flexibility and transparency. As a result, it has been in the spotlight as a candidate material for implementing next-generation flexible electric devices.
  • next-generation graphene-based flexible devices requires three-dimensional patterning technology that can produce nanometer-sized graphene three-dimensional structures in desired positions.
  • Printed electronics technology uses a variety of functional ink materials in direct printing process to produce digital appliances such as smartphones, digital cameras, digital versatile discs (DVDs) and liquid crystal displays (LCDs), as well as electronic paper and flexible physical and chemical sensors. It is a technology that can manufacture various next generation flexible electronic devices. Manufacturing an electronic device through a printing process may have various advantages over the existing process. First of all, various processes are possible without expensive manufacturing process, which can drastically lower the process cost, and also increase the process speed through the continuous process. In addition, it is environmentally friendly by reducing the consumption of various energy such as electricity used to maintain the process, and it is possible to minimize the discharge of unnecessary chemical waste since it is possible to selectively manufacture the electronic device only to the desired part. In addition, the printed electronic technology has a very high process compatibility with the flexible electronic device technology that many ink materials can be processed at a low temperature to implement the electronic device on a flexible plastic substrate.
  • Printed electronic technology includes a three-dimensional printing method capable of manufacturing a three-dimensional pattern in addition to a method of manufacturing an electronic device in a form of scanning, copying, and outputting a planar two-dimensional object.
  • Three-dimensional printing technology is based on three-dimensional design data based on materials such as insulators such as rubber, nylon, and plastic, stainless steel, and metals such as titanium. Can be shaped.
  • These two-dimensional and three-dimensional printing techniques are used in the field of printed electronics, which have been limitedly applied to some areas such as circuits of printed circuit boards, photomasks of semiconductors, and color filters of displays. It plays a role as a catalyst to grow into a new area while developing and converging.
  • 3D printing technology can provide a revolutionary direction in manufacturing new types of electronic devices and components.
  • materials such as carbon nanotubes and graphene can be filled into a matrix such as plastic as a filler to produce a structure having a size of at least tens of micrometers. You can't make three-dimensional nanostructures purely composed of graphene.
  • an object of the present invention is to provide a graphene oxide pattern and a method of printing a graphene pattern having a nano size of less than 1 micron.
  • an object of the present invention is to provide a printing method of the graphene nano pattern that can maintain the structure of the pattern by the bonding force between the graphene sheets.
  • Another object of the present invention is to provide a printing method of a flexible graphene electronic device.
  • the present invention comprises the steps of supplying an ink in which the graphene oxide sheets dispersed in a solvent to the nozzle; Positioning the nozzle at a point on the substrate; And printing the graphene oxide nanopattern corresponding to the movement path of the nozzle by moving the nozzle along a predetermined path on the substrate while discharging the ink from the nozzle.
  • the nano-pattern is printed with graphene oxide sheets laminated by evaporation of a solvent in a meniscus formed by the ink ejected from the nozzle between the nozzle and the substrate.
  • a method of printing a pattern is provided.
  • the concentration of the graphene oxide sheet is preferably 1g / L to 10g / L.
  • the moving speed of the nozzle is 0.1 ⁇ m / sec to 200 ⁇ m / sec, and the diameter of the nozzle is 0.1 ⁇ m to 50 ⁇ m.
  • the solvent is preferably at least one selected from the group of polar solvents consisting of water, alcohol, acetone and dichloromethane.
  • the present invention comprises the steps of supplying an ink in which a graphene oxide sheet dispersed in a solvent to the nozzle; Contacting the nozzle to the substrate; Separating the nozzle from the substrate by a predetermined distance such that a meniscus is formed between the substrate and the nozzle; And laminating graphene oxide sheets by solvent evaporation in the meniscus, printing the graphene oxide pattern by moving the nozzle relative to the substrate to induce the continuous graphene oxide deposition.
  • the evaporation of the solvent may be carried out below the boiling point of the solvent, in particular may be carried out at room temperature.
  • the laminated graphene oxide sheet in the present invention is characterized in that bonded by van der Waals force.
  • the size of the stacked graphene oxide nano pattern in the present invention is characterized in that it is controlled by inducing a change in the size of the meniscus through a change in the pulling speed of the nozzle.
  • the present invention provides a graphene oxide nano-pattern prepared by the above method in order to achieve the other technical problem; And it provides a graphene nano-pattern printing method comprising the step of printing the graphene nano-pattern by reducing the graphene oxide nano-pattern.
  • the reduction process may be performed by heat treatment in a vacuum or non-oxidizing atmosphere or by hydrazine treatment.
  • the present invention provides graphene oxide sheets; It provides a graphene oxide pattern printing ink, characterized in that the graphene sheets contain a dispersed solvent, and does not include a binder for molding the graphene oxide sheets. At this time, it is preferable that the said solvent has a boiling point of 100 degrees C or less.
  • the present invention comprises the steps of supplying an ink comprising a graphene oxide sheet and a solvent to the nozzle; Contacting the nozzle to a substrate; And discharging the ink to the nozzle to move the position of the nozzle with respect to the substrate without interruption of the ejected ink to form a meniscus by the ink between the nozzle and the substrate, And printing a nano-pattern in which the sheets are stacked by evaporation, wherein the nano-pattern is bonded by van der Waals forces between graphene oxide sheets.
  • the nano-pattern may include wrinkles formed by rolling or crumpling the graphene oxide sheets.
  • the graphene oxide sheet constituting the nano-pattern in the present invention may be aligned such that the normal direction of the sheet surface is substantially perpendicular to the moving direction of the nozzle. .
  • the ink is preferably at least one selected from the group of polar solvents consisting of water, alcohol, acetone and dichloromethane as a solvent.
  • the ink may not include a binder.
  • the present invention may further comprise the step of reducing the nano-pattern.
  • the present invention provides a method that can produce a nano-pattern consisting of graphene without undergoing a complicated process. This may be used as a printing technology for implementing flexible and transparent next-generation graphene-based electronic devices.
  • FIG. 1 is a view for schematically explaining a printing technique according to an embodiment of the present invention.
  • FIG. 2 is a conceptual diagram illustrating an operation process of the printing pen 110 for printing the graphene oxide pattern according to an embodiment of the present invention in more detail.
  • FIG. 3 is a diagram illustrating an example of a pattern printing method according to an embodiment of the present invention.
  • FIG. 4 is a view schematically showing a graphene nano pattern printing apparatus according to an embodiment of the present invention.
  • Figure 5 is a graph plotting the change in the size of the graphene oxide (GO) wire according to the nozzle pulling speed of the graphene nano wire prepared according to this embodiment.
  • Figure 6 is a photograph showing a change in the nozzle pulling speed, graphene oxide size and the diameter of the nanowires of the graphene nanowires prepared according to an embodiment of the present invention.
  • Figure 7 is a photograph showing the electrical, mechanical properties of the graphene wire prepared in one embodiment of the present invention.
  • FIG. 8 is a view showing an application example of the stretch interconnect and the gas sensing transducer of the graphene nano pattern according to an embodiment of the present invention.
  • FIG. 9 is a photograph showing various types of application patterns manufactured according to the present invention.
  • nano means a size of less than 1 micrometer, that is, several to several hundred nanometers in a conventional sense
  • nano pattern refers to a pattern having a line width of the pattern is nano size.
  • the pattern is a structure that functions as an electric element, including not only two-dimensional but also three-dimensional structures, for example, includes both structures in the form of wire stacked in a direction parallel to the substrate surface or extending in a direction perpendicular to the substrate. .
  • FIG. 1 is a view for schematically explaining a printing technique of the present invention.
  • the graphene oxide ink in which the graphene oxide sheet is dispersed at a predetermined concentration is maintained in the printing pen 110.
  • v a predetermined speed
  • W a predetermined flow rate
  • Ink discharged near the nozzle at the tip of the pen forms a meniscus (B) by surface tension.
  • the solvent of the ink evaporates from the meniscus surface, leaving a pure graphene oxide sheet stack (A) on the substrate.
  • the surface tension by the meniscus B formed at the tip of the nozzle allows the solution to be discharged out of the nozzle without interruption.
  • the solution in the nozzle is continuously discharged as the nozzle moves, and the laminated structure A of the graphene oxide sheet is printed on the evaporation site close to the substrate, while the meniscus B is formed on the nozzle side. A continuous process occurs.
  • a predetermined graphene oxide lamination pattern corresponding to the movement trajectory of the nozzle may be printed on the substrate.
  • FIG. 2 (a) to (c) is a conceptual diagram showing in more detail the operation of the printing pen 110 for printing the graphene oxide pattern according to an embodiment of the present invention.
  • FIG. 2A illustrates an initial state in which the nozzle of the pen 110 contacts the substrate 10 and the nozzle.
  • an ink including a graphene oxide sheet 22 and a dispersion medium 24 for dispersing the graphene oxide sheet is stored.
  • the graphene oxide pattern printed in the present invention is composed of a plurality of graphene oxide sheets.
  • the laminated pattern is supported by a bonding force resulting from the graphene oxide sheet itself, such as van der Waals force, and does not require a separate binder or a bonding matrix to bond between the sheets.
  • the width of the meniscus is maintained within an appropriate range to provide a high specific surface area for evaporation of the solvent.
  • the width of the meniscus in the present invention depends on the aperture of the nozzle and the speed of movement of the nozzle.
  • the line width of the resulting graphene oxide lamination pattern has a value equal to or smaller than the width d of the meniscus.
  • the meniscus has a width d of a predetermined size.
  • the width of the meniscus has a smaller value. This relationship can be expressed by the following formula called the law of material balance.
  • the graphene oxide nanopattern printed by the method of the present invention can be reduced to the graphene nanopattern in an appropriate manner.
  • a heat treatment process in a vacuum or non-oxidizing atmosphere may be performed.
  • the heat treatment temperature and time can be appropriately designed in consideration of the heat resistance of the device printed on the substrate and the neighboring device.
  • the reduction process may be performed by chemical treatment such as hydrazine.
  • the reduction process in the present invention may be performed by performing a heat treatment and a chemical treatment in parallel.
  • the graphene oxide nano pattern printing method of the present invention is applicable to various types of patterns.
  • FIG. 3 is a diagram illustrating an example of a pattern printing method according to the present invention.
  • the print pen 110 may move in a direction parallel to the substrate. Even in this case, the formation of the local meniscus, the evaporation of the solution and the production of the graphene oxide nanopattern can proceed with the same mechanism as described above. In addition, such a pattern may be applied to print a pattern of two-dimensional plane shape.
  • the print pen 110 is moved in a direction perpendicular to the substrate, thereby enabling the manufacture of a freestanding wire pattern in the direction perpendicular to the substrate.
  • wire bonding may be enabled in three-dimensional space by appropriately combining movements in two directions.
  • FIG. 4 is a view schematically showing a graphene nano-pattern printing apparatus according to an embodiment of the present invention.
  • the graphene nano pattern printing apparatus 100 of the present invention may include a printing pen 110, a substrate stage 120, and a position controller 140.
  • the printing pen 110 has a loading space for containing the graphene oxide ink 20 therein, and discharges the graphene oxide ink 20 through a nozzle provided at the tip portion.
  • the cross section of the printing pen 110 nozzle in the present invention may have a variety of shapes, such as circular, sand, hexagon.
  • the nozzle has a predetermined aperture.
  • the line width of the pattern printed by the movement of the nozzle depends on the movement speed of the nozzle.
  • the nano-size apertures are not required to obtain nano-sized patterns.
  • the diameter of the nozzle in the present invention is preferably 0.1 ⁇ m ⁇ 50 ⁇ m.
  • the diameter of the nozzle is 50 ⁇ m or more, the specific surface area of the meniscus formed is small, and printing of the laminated structure is not easy.
  • the nozzle size is less than 0.1 ⁇ m may block the nozzle.
  • An ink supply tank (not shown) and an ink supply valve (not shown) may be connected to the printing pen 110.
  • the ink supply valve may interrupt the flow of ink flowing into the printing pen 110.
  • the printing pen 110 may be attached to a transfer mechanism, for example, a transfer arm for three-axis transfer, the transfer arm may transfer the printing pen 110 in the X, Y, Z axis direction.
  • the substrate stage 110 may include an integrated means for holding a substrate to be printed.
  • the substrate stage 120 may include a transfer mechanism (not shown) that is movable in three axes.
  • the position controller 140 controls the position of at least one of the printing pen 110 and the substrate stage 120.
  • a three-dimensional relative position of the printing pen 110 and the substrate stage 120 may be controlled by driving the transfer mechanisms of the printing pen 110 and the substrate stage 120.
  • the position control unit 140 controls the relative movement speed of the printing pen 110 with respect to the substrate.
  • the moving speed of the nozzle for pattern printing is designed in consideration of the solution evaporation rate in the meniscus and the surface tension of the solution.
  • the moving speed of the nozzle is preferably in the range of 0.1 ⁇ m / sec to 200 ⁇ m / sec. At a moving speed of less than 0.1 ⁇ m / sec, the nozzle is blocked by rapid evaporation. And breakage of the pattern occurs at a moving speed of 200 ⁇ m / sec or more.
  • the position controller 120 may control the positions of the printing pen 110 and / or the substrate holder 120 by referring to the shape of the unit structure obtained through the CCD camera 142.
  • the position controller 140 may control the growth direction of the structure by controlling the shape of the meniscus 113 formed between the printing pen 110 and the substrate 120.
  • the ink supplied as a raw material of the graphene nano pattern printing apparatus 100 preferably has the following characteristics.
  • the ink is composed of a solvent (or dispersion medium) and a graphene oxide sheet dispersed in the solvent.
  • the solvent does not produce a residue after evaporation.
  • a polar inorganic solvent or an organic solvent may be used as the solvent.
  • the inorganic solvent may be water
  • the organic solvent may be alcohol, dichloromethane and acetone.
  • evaporation of the solvent and printing of the pattern should occur substantially in situ. Therefore, in the present invention, the solvent has a boiling point temperature equal to or lower than that of water, and preferably 100 ° C. or lower.
  • the graphene oxide sheet is dispersed in the solvent.
  • the concentration of the graphene oxide sheet in the ink is preferably in the range of 1g / L to 10g / L. At lower concentrations, the concentration of the graphene oxide sheet is low so that the structure is not manufactured during printing. At a concentration above this, the graphene oxide sheet may block the opening of the nozzle as the solvent evaporates.
  • the average size of the graphene oxide sheet may have a larger value than the aperture of the nozzle.
  • the graphene oxide sheet has a high flexibility, and even if a graphene oxide sheet larger than the nozzle aperture size is used, the graphene oxide sheet can pass through the nozzle while being bent or dried while passing through the nozzle.
  • graphene oxide sheets having an average size of 10 times larger than the nozzle size are not preferable because they can block the nozzle size.
  • the graphene oxide sheet was prepared by a modified Hummer method from natural graphite, Alfa Aesar (purity 99.999%, 200 mesh or less). Specifically, 20 g of graphite and 460 mL of H 2 SO 4 were mixed in a flask, and 60 g of KMnO 4 was slowly added in a cold water bath for at least 1 hour. Subsequently, the mixed solution was stirred vigorously at room temperature for 3 days, then 920 mL of deionized water was added and stirred for 10 minutes.
  • Graphite oxide sheets were prepared by exfoliating graphite oxide with ultrasonic waves.
  • An aqueous sample was prepared by dispersing the prepared graphene oxide sheet in water at a concentration of 1 g / L. At this time, the graphene oxide sheet using the average size of 1, 3, 5 ⁇ m each to prepare a separate aqueous sample.
  • Graphene nanowires were prepared using the prepared graphene oxide aqueous solution samples. A glass micro-pippet was used as the nozzle, and two nozzle diameters of 1.3 ⁇ m and 2.6 ⁇ m were used.
  • Free standing graphene oxide wire was printed on a gold coated silicon substrate.
  • Graphene oxide ink was supplied through the rear end of the pipette (pen) and was discharged from the tip without adding pressure other than capillary force.
  • the position and pull speed of the micropipette were precisely controlled with a position accuracy of 250 nm with a three-axis stepping motor.
  • the graphene nanowires (GO) prepared were heat-treated for 1 hour at 400 ° C. in a vacuum atmosphere to prepare reduced graphene nanowires (rGO).
  • Figure 5 is a graph plotting the size change of the graphene oxide (GO) wire according to the pulling speed of the graphene nano wire prepared according to this embodiment.
  • the nozzle diameter used was 1.3 ⁇ m, the ink in which the graphene oxide sheet having a size of 1, 3, 5 ⁇ m respectively dispersed.
  • the radius of the wire decreased from 625 nm to 150 nm.
  • the graphene wire produced in the present invention it can be seen that the graphene pattern shows a variety of surface structure according to the pulling speed.
  • the individual graphene nanosheets constituting the graphene nanowires at low pulling speed (c) are curled, wrinkled, and severely deformed.
  • Many wrinkles are formed on the surface of the graphene nanopattern due to wrinkles or entanglement between the graphene nanosheets.
  • wrinkles on the surface of the graphene nanopatterns tend to decrease gradually.
  • the arrangement of the graphene oxide sheet is such that the face of the graphene sheet is aligned in the direction of pulling the nozzle from the random arrangement (ie, the normal vector of the graphene sheet is aligned substantially perpendicular to the nozzle pulling direction). It shows a tendency. Since the electrons exhibit low resistance when moving along the surface of the graphene, when the surfaces of the graphene sheets are aligned in the nozzle direction, the path having the lower resistance increases, thereby improving the conductivity of the graphene structure.
  • Figure 6 is a photograph showing the change in the nozzle pulling speed, graphene oxide size and the line width of the nanowires of the graphene nanowires prepared according to this embodiment.
  • an interconnect connecting two electrodes was prepared by printing a graphene oxide nanowire on a gold electrode having a gap of 10 ⁇ m. Reduction of graphene oxide to graphene was carried out in a vacuum heat treatment (1 hour at 400 °C).
  • Figure 7 (a) is a graph plotting the current-voltage characteristics of the prepared graphene nano interconnect.
  • Figure 7 (b) is a photograph showing the mechanical properties of the prepared graphene nano interconnect. 7 (b) shows that the wire deformed by the stress is restored by removing the stress.
  • FIG. 8 (a) shows an application example of the flexible wiring electrode.
  • an interconnect connecting the two electrodes was manufactured by printing a graphene nanowire on a gold electrode having a 30 ⁇ m gap on the PDMS.
  • reduction of graphene oxide to graphene was performed by hydrazine treatment (12 hours at 120 ° C).
  • the interconnect showed no change in resistance even with 340% strain and stable characteristics without change in resistance with 120 repeated strains between 25% and 150%.
  • Figure 8 (b) shows an application example of the gas sensing transducer.
  • Printed Five graphene nanowires connected in parallel with a platinum pattern having a 10 ⁇ m interval were printed transducers for gas sensors. Nanowire transducers react linearly to varying concentrations of carbon dioxide injected at room temperature from 0.25% to 5%.
  • FIG. 9 is a photograph showing various types of wire patterns printed according to an example of the present invention.
  • Figure 9 (a) is an arrangement of free standing wire
  • Figure 9 (b) is a zigzag-shaped nano arch
  • Figure 9 (c) is a chain structure wire
  • Figure 9 (d) is a letter 'KERI'
  • 9 (e) shows the weave structure.
  • Graphene wire of the present invention can be a pattern of a variety of shapes, it is applicable to three-dimensional printed electronic technology, such as wire bonding, stretchable interconnect.

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Abstract

L'invention concerne un procédé d'impression d'un nanomotif de graphène. La présente invention concerne un procédé d'impression d'un nanomotif de graphène oxydé, qui comprend les étapes consistant à : fournir de l'encre à une buse, l'encre comportant des feuilles de graphène oxydé dispersées dans celle-ci par un solvant ; positionner la buse en un certain point sur un substrat ; imprimer un nanomotif de graphène oxydé correspondant au trajet de déplacement de la buse en déplaçant la buse le long d'un trajet prédéterminé sur le substrat tout en éjectant l'encre hors de la buse ; et mettre en oeuvre un traitement de réduction thermochimique du nanomotif de graphène oxydé imprimé. A l'étape d'impression du nanomotif de graphène oxydé, le nano-motif est imprimé en tant que feuilles de graphène oxydé qui sont stratifiées par l'évaporation du solvant dans le ménisque formé entre la buse et le substrat par l'encre éjectée par la buse, et la taille du nanomotif de graphène oxydé imprimé est réglée par un réglage de la vitesse de traînée de la buse. La présente invention permet d'imprimer un motif de graphène oxydé ou un motif de graphène nanométrique d'une taille inférieure à 1 micromètre sans matrice afin de maintenir la forme du graphène.
PCT/KR2015/011627 2014-11-11 2015-11-02 Procédé d'impression de nanomotif de graphène, et appareil et encre utilisés à cet effet WO2016076563A1 (fr)

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CN201580061448.7A CN107249858B (zh) 2014-11-11 2015-11-02 石墨烯纳米图案的印刷方法及用于其的装置和墨水

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KR1020140156361A KR102242028B1 (ko) 2014-11-11 2014-11-11 그래핀 나노 패턴 인쇄 방법，그에 사용되는 장치 및 잉크
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KR20220064078A (ko) * 2020-11-11 2022-05-18 한국전기연구원 구조색상 구조체 및 그 제조방법
US12024423B2 (en) 2021-02-01 2024-07-02 POSTECH Research and Business Development Foundation Method for fabricating micro- or nanowire at predetermined position of object using micro- or nanopipette
US11911983B2 (en) * 2021-02-01 2024-02-27 POSTECH Research and Business Development Foundation Method of forming micro- or nanowires at predetermined positions of an object using a micro- or nanopipette

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