KR101769023B1 - Flexible nanogenerator and preparing method of the same - Google Patents
Flexible nanogenerator and preparing method of the same Download PDFInfo
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- KR101769023B1 KR101769023B1 KR1020150074275A KR20150074275A KR101769023B1 KR 101769023 B1 KR101769023 B1 KR 101769023B1 KR 1020150074275 A KR1020150074275 A KR 1020150074275A KR 20150074275 A KR20150074275 A KR 20150074275A KR 101769023 B1 KR101769023 B1 KR 101769023B1
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-
- H01L41/22—
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
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Abstract
materials; A lower electrode comprising a metal pattern layer formed on the substrate and a two-dimensional nanomaterial layer formed on the metal pattern layer; A ferroelectric layer formed on the lower electrode; And an upper electrode formed on the ferroelectric layer, and a method of manufacturing the flexible nano-generator.
Description
The present invention relates to a flexible nano-generator and a method of manufacturing the flexible nano-generator.
Recently, the development of nanotechnology has made it possible to easily manufacture nano-sized devices. However, the battery that occupies most of the current power has a disadvantage that it occupies a larger area than the nano device and limits the performance and the independent driving of the nano device due to the limited lifetime.
In the conventional transparent nanogenerator, graphene is mainly used as an electrode. Graphene has attracted attention as a next generation material with high charge mobility, flexibility and transparency, but it has a limitation in device performance due to its high resistance. In addition, methods such as photolithography, stamping, or inkjet printing are mainly used in fabricating a metal grid pattern used as a transparent electrode, and these methods have a problem in that a complicated process and a vacuum state are required and high cost is incurred.
On the other hand, Korean Patent No. 10-1207075 discloses a flexible nano-generator manufacturing method and a flexible nano-generator produced thereby.
The present invention provides a flexible nano-generator including a metal pattern layer and a method of manufacturing the flexible nano-generator.
However, the problems to be solved by the present invention are not limited to the above-mentioned problems, and other problems not mentioned can be clearly understood by those skilled in the art from the following description.
One aspect of the invention provides a substrate, comprising: a substrate; A lower electrode comprising a metal pattern layer formed on the substrate and a two-dimensional nanomaterial layer formed on the metal pattern layer; A ferroelectric layer formed on the lower electrode; And an upper electrode formed on the ferroelectric layer.
According to another aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: forming a metal pattern layer on a substrate; Forming a lower electrode by forming a two-dimensional nanomaterial layer on the metal pattern layer; Forming a ferroelectric layer on the lower electrode; And forming an upper electrode on the ferroelectric layer. The present invention also provides a method of manufacturing a flexible nano-generator.
According to one embodiment of the present invention, a flexible nano-generator including a metal pattern layer and a method of manufacturing the flexible nano-generator can be provided. The flexible nano-generator according to the present invention can be used for a two-dimensional nanomaterial and a metal pattern It is possible to provide a high-performance and high-efficiency nano generator improved in resistance of a two-dimensional nanomaterial while maintaining flexibility and transparency. In addition, the nanosgenerator according to one embodiment of the present invention is transparent and flexible and can be applied to any living environment such as portable electronic devices, sensors, and medical science.
According to an embodiment of the present invention, large-area lines and lattice patterns can be easily fabricated using the flow coating method, and the resistance of the two-dimensional nanomaterial can be lowered by using the pattern.
1 is a cross-sectional view illustrating the structure of a flexible nano-generator according to one embodiment of the present invention.
Figure 2 illustrates a metal pattern layer according to one embodiment of the present invention.
3 (a) and 3 (b) are structural diagrams of a flexible nano-generator according to an embodiment of the present invention.
4A and 4B are graphs showing voltage characteristics and current characteristics of the lower electrode according to various metal pattern shapes in one embodiment of the present invention.
5 (a) shows a process of forming a metal grid pattern using a flow coating method in one embodiment of the present invention, and FIG. 5 (b) shows a process of forming a metal grid pattern according to one embodiment of the present invention It is an optical image of a grid pattern.
6 is a graph showing the transmittance of the Ag metal grid electrode according to the AgNP solution concentration in one embodiment of the present invention.
7 is a graph showing sheet resistance and light transmittance according to the line width of a metal grid in one embodiment of the present invention.
8 is a graph showing an output voltage and an output current density according to bending strain of a flexible nano generator in one embodiment of the present invention.
9 is a graph showing an output voltage and an output current density of a flexible nano generator according to an applied strain in the embodiment of the present invention.
Figure 10 shows the stability of a flexible nano-generator during a bending cycle of 0.18% strain, in one embodiment of the invention.
11 is an image showing driving of a light-emitting diode (LED) using a flexible nano-generator in one embodiment of the present invention.
Figures 12 (a) - (d) are pictorial image, perspective, schematic, and stage moving velocity graphs over time for a flow coating in one embodiment of the present invention.
13 (a) and 13 (b) are optical microscope images before and after the thermal sintering treatment of the metal pattern produced by the flow coating, in one embodiment of the present invention.
14A and 14B are graphs showing changes in AgNP line width according to AgNP solution concentration and resistance of a single AgNP sintered according to AgNP solution concentration in the embodiment of the present invention .
15 is an atomic force microscope image (height mode) of a line pattern, in one embodiment of the present invention.
16 is a graph showing the optical transmittance of the metal pattern electrode according to the AgNP solution concentration in one embodiment of the present invention.
17 is an optical microscope image of a pattern produced by various movement distances of a polymer blade, in one embodiment of the present invention.
18 (a) and 18 (b) are surface and cross-sectional scanning electron microscope images of the ferroelectric layer in one embodiment of the present invention.
Figure 19 shows the elements of the bend test of a flexible nano-generator device in one embodiment of the present invention.
Hereinafter, embodiments and examples of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains. It should be understood, however, that the present invention may be embodied in many different forms and is not limited to the embodiments and examples described herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.
Throughout this specification, when a part is referred to as being "connected" to another part, it is not limited to a case where it is "directly connected" but also includes the case where it is "electrically connected" do.
Throughout this specification, when a member is "on " another member, it includes not only when the member is in contact with the other member, but also when there is another member between the two members.
Throughout this specification, when an element is referred to as "including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise.
As used herein, the terms "about," " substantially, "and the like are used herein to refer to or approximate the numerical value of manufacturing and material tolerances inherent in the stated sense, Accurate or absolute numbers are used to prevent unauthorized exploitation by unauthorized intruders of the mentioned disclosure.
The term " step " or " step of ~ " as used throughout the specification does not imply " step for.
Throughout this specification, the term "combination (s) thereof " included in the expression of the machine form means a mixture or combination of one or more elements selected from the group consisting of the constituents described in the expression of the form of a marker, Quot; means at least one selected from the group consisting of the above-mentioned elements.
Throughout this specification, the description of "A and / or B" means "A or B, or A and B".
Throughout this specification, the term "graphene " means that a plurality of carbon atoms are linked together by a covalent bond to form a polycyclic aromatic molecule, wherein the carbon atoms linked by the covalent bond are 6-membered rings A 5-membered ring, and / or a 7-membered ring. Thus, the sheet formed by graphene can be seen as a single layer of carbon atoms covalently bonded to each other, but is not limited thereto. The sheet formed by the graphene may have various structures, and the structure may vary depending on the content of the 5-membered ring and / or the 7-membered ring which may be contained in the graphene. When the sheet formed by the graphene is a single layer, they may be laminated to form a plurality of layers, and the side end portion of the graphene sheet may be saturated with hydrogen atoms, but the present invention is not limited thereto.
Throughout the specification, the term "graphene oxide" is also referred to as graphene oxide and may be abbreviated as "GO ". But not limited to, a structure in which a functional group containing oxygen such as a carboxyl group, a hydroxyl group, or an epoxy group is bonded on a single layer graphene.
Hereinafter, embodiments of the present invention are described in detail, but the present invention is not limited thereto.
1 is a cross-sectional view showing a structure of a flexible nano-generator according to an embodiment of the present invention.
One aspect of the present invention provides a lithographic apparatus comprising: a substrate; A
The flexible nano-generator includes a
In one embodiment of the invention, the
The
In one embodiment of the present invention, the
In one embodiment of the present invention, the
In one embodiment of the present invention, the
In one embodiment of the invention, the pattern may include, but is not limited to, an interval of about 30 [mu] m to about 1,000 [mu] m. For example, the spacing may be from about 30 탆 to about 1,000 탆, from about 50 탆 to about 1,000 탆, from about 100 탆 to about 1,000 탆, from about 200 탆 to about 1,000 탆, from about 300 탆 to about 1,000 탆, From about 500 μm to about 1,000 μm, from about 600 μm to about 1,000 μm, from about 700 μm to about 1,000 μm, from about 800 μm to about 1,000 μm, from about 900 μm to about 1,000 μm, from about 30 μm to about From about 30 占 퐉 to about 300 占 퐉, from about 30 占 퐉 to about 200 占 퐉, from about 30 占 퐉 to about 800 占 퐉, from about 30 占 퐉 to about 700 占 퐉, from about 30 占 퐉 to about 600 占 퐉, , About 30 [mu] m to about 100 [mu] m, or about 30 [mu] m to about 50 [mu] m.
In one embodiment of the invention, the line width of the pattern may range from about 1 [mu] m to about 20 [mu] m, but is not limited thereto. For example, the line width of the pattern may be from about 1 [mu] m to about 20 [mu] m, from about 2 [mu] m to about 20 [mu] m, from about 3 [ From about 6 탆 to about 20 탆, from about 7 탆 to about 20 탆, from about 8 탆 to about 20 탆, from about 9 탆 to about 20 탆, from about 10 탆 to about 20 탆, from about 12 탆 to about 20 탆, from about 1 μm to about 17 μm, from about 1 μm to about 15 μm, from about 1 μm to about 20 μm, from about 20 μm to about 20 μm, from about 16 μm to about 20 μm, from about 18 μm to about 20 μm, From about 1 탆 to about 7 탆, from about 1 탆 to about 5 탆, or from about 1 탆 to about 3 탆, It is not.
In one embodiment of the present invention, the two-dimensional nanomaterial layer 220 may be any two-dimensional nanomaterial showing conductivity, and may be used without limitation, for example, graphene; Graphene oxide; Transition metal chalcogenide, for example, SnSe 2 , MoS 2 , TiS 2 , VS 2 , WS 2 , MoSe 2 , TiSe 2 , MoTe 2 , or TiTe 2 ; But are not limited to, those selected from the group consisting of, and combinations thereof. In addition, the two-dimensional nanomaterial layer 220 may be formed of one layer or a plurality of layers, but is not limited thereto.
In one embodiment of the present invention, the resistance of the
A
In one embodiment of the present invention, the
In one embodiment of the present invention, the
In one embodiment of the present invention, the flexible nano-generator may generate a voltage of about 1.5 V to about 6 V, but is not limited thereto. For example, the voltage may range from about 1.5 V to about 6 V, from about 2 V to about 6 V, from about 3 V to about 6 V, from about 4 V to about 6 V, from about 5 V to about 6 V, To about 5.6 V, from about 2 V to about 5.2 V, from about 3 V to about 4.8 V, or from about 4 V to about 4.4 V, for example.
An
In one embodiment of the present invention, the
In one embodiment of the invention, the flexible nano-generator may be transparent, but is not limited thereto. The flexible nano generator according to the present invention includes a two-dimensional nanomaterial layer 220 and a
According to another aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: forming a metal pattern layer on a substrate; Forming a lower electrode by forming a two-dimensional nanomaterial layer on the metal pattern layer; Forming a ferroelectric layer on the lower electrode; And forming an upper electrode on the ferroelectric layer. The present invention also provides a method of manufacturing a flexible nano-generator.
In the method of manufacturing a flexible nano-generator according to another aspect of the present invention, a detailed description of parts overlapping with those described for the flexible nano-generator according to one aspect of the present invention is omitted, Can be applied.
In one embodiment of the invention, the substrate may be transparent and flexible, but is not limited thereto. For example, the substrate may be, but is not limited to, polyethylene naphthalate (PEN), polyethersulfone (PES), or polycarbonate (PC).
In one embodiment of the present invention, the metal pattern layer may be formed by flow coating, photolithography, stamping, or inkjet printing, but is not limited thereto. The metal pattern layer may be formed by flow coating desirable. The flow coating method utilizes the evaporation characteristics of the solution. As the solvent evaporates rapidly at the edge portion of the solution containing the metal nanoparticles between the polymer blade and the substrate as shown in FIG. 5 (a) A flow occurs in the solution, and metal nanoparticles present in the solution migrate to and accumulate on the edge of the solution where the rapid evaporation takes place to form a single line. The plurality of line patterns can be formed by repeatedly patterning the lines in the same manner as above after having the stopping time of about 0.1 second to about 10 seconds and then moving the substrate by a pre-programmed distance. The lattice pattern can be obtained by rotating the substrate by about 90 占 and patterning it in the same manner as described above. By repeating the above process, a plurality of lines and / or grid patterns can be manufactured simply and inexpensively.
In one embodiment of the present invention, the metal nanoparticle solution is selected from the group consisting of Ag, Au, Pt, Al, Cu, Cr, V, And a metal selected from the group consisting of Mg, Ti, Sn, Pb, Pd, W, Ni, and combinations thereof. But is not limited thereto. In addition, the metal nanoparticle solution may include a solvent. For example, the solvent may include, but is not limited to, chlorobenzene, chloroform, toluene, or hexane.
In one embodiment of the present invention, the step of forming the metal pattern layer may include, but is not limited to, sintering the metal pattern layer at a temperature ranging from about 100 ° C to about 200 ° C. For example, the sintering temperature may range from about 100 ° C to about 200 ° C, from about 110 ° C to about 200 ° C, from about 120 ° C to about 200 ° C, from about 130 ° C to about 200 ° C, About 190 占 폚 to about 190 占 폚, about 110 占 폚 to about 200 占 폚, about 160 占 폚 to about 200 占 폚, about 170 占 폚 to about 200 占 폚, about 180 占 폚 to about 200 占 폚, About 180 ° C, about 120 ° C to about 170 ° C, about 130 ° C to about 160 ° C, or about 140 ° C to about 150 ° C.
In one embodiment of the present invention, the metal pattern layer may include a shape selected from the group consisting of engraved, embossed, and combinations thereof, but is not limited thereto.
In one embodiment of the present invention, the metal pattern layer may include a plurality of line patterns or a lattice pattern, but the present invention is not limited thereto. In addition, the pattern may be a regular pattern having a regular arrangement or an irregular pattern having an irregular arrangement, but the present invention is not limited thereto.
In one embodiment of the invention, the pattern may include, but is not limited to, a spacing of about 30 [mu] m to about 1,000 [mu] from about 500 탆 to about 1000 탆, from about 600 탆 to about 1000 탆, from about 100 탆 to about 1,000 탆, from about 200 탆 to about 1,000 탆, from about 300 탆 to about 1,000 탆, From about 800 탆 to about 1000 탆, from about 900 탆 to about 1,000 탆, from about 30 탆 to about 900 탆, from about 30 탆 to about 800 탆, from about 30 탆 to about 700 about 30 μm to about 100 μm, about 30 μm to about 50 μm, about 30 μm to about 600 μm, about 30 μm to about 500 μm, about 30 μm to about 300 μm, about 30 μm to about 200 μm, But is not limited thereto.
In one embodiment, the line width of the pattern may range from about 1 μm to about 20 μm, but the present invention is not limited thereto, and the line width may be adjusted according to the concentration of the metal nanoparticle solution . For example, the line width of the pattern may be from about 1 [mu] m to about 20 [mu] m, from about 2 [mu] m to about 20 [mu] m, from about 3 [ From about 6 탆 to about 20 탆, from about 7 탆 to about 20 탆, from about 8 탆 to about 20 탆, from about 9 탆 to about 20 탆, from about 10 탆 to about 20 탆, from about 12 탆 to about 20 탆, from about 1 μm to about 17 μm, from about 1 μm to about 15 μm, from about 1 μm to about 20 μm, from about 20 μm to about 20 μm, from about 16 μm to about 20 μm, from about 18 μm to about 20 μm, From about 1 탆 to about 7 탆, from about 1 탆 to about 5 탆, or from about 1 탆 to about 3 탆, It is not.
In one embodiment of the present invention, the metal pattern layer is formed of a metal such as Ag, Au, Pt, Al, Cu, Cr, V, Mg, Ti, Sn, Pb, Pd, W, Ni, and combinations thereof. But is not limited thereto.
In one embodiment of the invention, the formation of the two-dimensional nanomaterial layer may include but is not limited to being performed by chemical vapor deposition. For example, the chemical vapor deposition may be performed by thermal chemical vapor deposition (TCVD), rapid thermal chemical vapor deposition (RTCVD), inductively coupled plasma-chemical vapor deposition (ICP-CVD), low pressure chemical vapor deposition (LPCVD), atmospheric pressure chemical vapor deposition (APCVD), metal organic chemical vapor deposition Plasma-enhanced chemical vapor deposition (PECVD), and the like.
In one embodiment of the present invention, the two-dimensional nanomaterial layer can be used without limitations as long as it is a two-dimensional nanomaterial showing conductivity, for example, graphene; Graphene oxide; Transition metal chalcogenides such as SnSe 2 , MoS 2 , TiS 2 , VS 2 , WS 2 , MoSe 2 , WSe 2 , MoTe 2 , or TiTe 2 ; But are not limited to, those selected from the group consisting of, and combinations thereof. In addition, the two-dimensional nanomaterial layer may be formed of one layer or a plurality of layers, but is not limited thereto.
In one embodiment of the present invention, the formation of the ferroelectric layer may include, but is not limited to, being performed by spin coating. Further, in one embodiment of the present invention, the ferroelectric layer may further be spin-coated and then annealed at a temperature ranging from about 100 ° C to about 150 ° C. However, the present invention is not limited thereto, The treatment may be performed for crystallization of the ferroelectric layer. For example, the annealing temperature may range from about 100 ° C to about 150 ° C, from about 110 ° C to about 150 ° C, from about 120 ° C to about 150 ° C, from about 130 ° C to about 150 ° C, But is not limited to, from about 100 캜 to about 140 캜, from about 100 캜 to about 130 캜, from about 100 캜 to about 120 캜, or from about 100 캜 to about 110 캜.
In one embodiment of the present invention, the ferroelectric layer can be any transparent ferroelectric material, and can be used without limitation, for example, poly (vinylidene fluoride-co-trifluoroethylene) ], PZT [Pb (Zr, Ti) O 3], SBT (
In one embodiment of the invention, the ferroelectric layer may have a thickness in the range of about 4 μm to about 6 μm, but is not limited thereto. For example, the thickness of the ferroelectric layer may range from about 4 탆 to about 6 탆, from about 4.2 탆 to about 6 탆, from about 4.4 탆 to about 6 탆, from about 4.6 탆 to about 6 탆, From about 5 .mu.m to about 6 .mu.m, from about 5.2 .mu.m to about 6 .mu.m, from about 5.4 .mu.m to about 6 .mu.m, from about 5.6 .mu.m to about 6 .mu.m, to about 5 占 퐉, or from about 4 占 퐉 to about 4.5 占 퐉.
In one embodiment of the present invention, the upper electrode is not particularly limited as long as it is a conductive material. For example, the upper electrode may be transparent, but is not limited thereto. The
Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
[ Example ]
A metal grid pattern was formed on a PEN (polyethylene naphthalate) substrate by a flow coating method (Figs. 1, 2, and 5 (a) and 5 (b)). One layer of graphene was formed on the substrate having the metal grid pattern to prepare a lower electrode. Thereafter, a ferroelectric layer was formed on the lower electrode using P (VDF-TrFE), and then an upper electrode was formed on the ferroelectric layer using silver (Ag) to produce a flexible nano-generator (A) and (b) of FIG.
Specifically, the silver nanoparticles (AgNP) (Nanopaste, Harima Chemicals groups, Inc.), which had been previously purchased, were dissolved in toluene at various concentrations, and then the sheet resistance of 7 mg / mL The silver nanoparticle solution was selected (Figs. 6, 7, and 14 (a) and 14 (b)).
The silver nanoparticle solution of 7 mg / mL was injected between the PEN substrate and the polymer blade using a flow coating method and then passed through a programmed instrument (piezo nanopositioner, physic instrumente (PI) GmbH & Co) Ag pattern was formed and then Ag was sintered through heat treatment. Thereafter, the PEN substrate was rotated by 90 degrees to prepare an Ag wire in the same manner. As a result, a grid-shaped Ag grid was produced.
Then, poly (methyl methacrylate) (poly (methyl methacrylate)) was added to graphene grown by chemical vapor deposition on copper. PMMA] was coated and the copper was dissolved. After transferring the graphene onto an Ag grid, the PMMA was removed to obtain a substrate (Ag grid / graphene) having a structure in which graphene was formed on the Ag grid pattern.
Thereafter, P (VDF-TrFE) was coated on the Ag grid / graphene by spin coating and then heat-treated at 140 ° C for 3 hours and subjected to an electric poling process.
Finally, silver was deposited through a thermal evaporator to form the upper electrode.
[ Example One]
1. Manufacture of silver electrode
Ag nanoparticles (Nanopaste, NPS-J, Harima Chemicals Group, Inc., Japan) were dissolved in toluene to prepare silver nanoparticle solutions at various concentrations ranging from 1 mg / mL to 10 mg / mL. The particle size was about 10 nm. The solution was stirred for 24 hours to allow AgNP to disperse homogeneously. Polyethylene naphthalate (PEN) substrate was sequentially washed with acetone, 2-propanol, and deionized water, and then dried with nitrogen gas.
The preparation of the flow coating is carried out by using an angular polymer blade attached to a vertical translation stage and a piezo nanopositioner (Fig. Physics Instrumente (PI) GmbH & Co., KG]. A 75 micron thick polyethylene terephthalate (PET) blade was obtained 1.2 mm from the edge to make a hinge. The PET blade was fixed at an angle of 40 ° to the vertical moving stage and moved in contact with the substrate. 6 [mu] L of the AgNP solution having the concentration of 1 mg / mL to 10 mg / mL was injected between the PET blade and the substrate, and the AgNP solution was collected by a capillary force under the blade. The linear moving stage was programmed to move at a constant speed of 1.5 mm / s while periodically stopping for 1 second so that the moving distance was 50 μm to 250 μm. The AgNP wire pattern was formed on a PEN substrate, and then sintered by heating in a 150 DEG C chamber for 1 hour under a nitrogen atmosphere. After rotating the stage at 90 degrees, the second set of AgNP lines, such as the thermally sintered AgNP, was patterned.
2. Flexible Piezoelectricity Of the nano generator Produce
Poly (vinylidenefluoride-co-trifluoroethylene); poly (vinylidene fluoride-co-trifluoroethylene); P (VDF-TrFE)] was purchased from PIEZOTECH. The P (VDF-TrFE) copolymer (20 wt%) was dissolved in dimethylformamide (DMF) and the solution was stirred for at least 24 hours. A 5.5 μm thick P (VDF-TrFE) layer was spin-coated onto an Ag metal grid and a single-layer graphene (SLG) electrode. SLGs were synthesized by thermal CVD and transferred onto Ag metal grid electrodes using poly (methyl methacrylate) (PMMA) layer. The spin-coated P (VDF- TrFE) layer was crystallized by annealing for 3 hours at 140 DEG C. A thick Ag top electrode of 100 nm was evaporated by heat through a shadow mask at 10 <" 7 > Torr. Electrical poling was performed by dipole alignment And the crystallization of the P (VDF-TrFE) β phase was improved by application of an electric field of 100 MVm -1 for 30 minutes.
3 (a) and 3 (b) show the structure of a nano generator using Ag grid and graphene. In FIGS. 3 (a) and 3 (b), the lower end shows the movement of electrons when the nano- It is.
3. Flow Formation of metal pattern by coating
In the present embodiment, the linear pattern was formed during the flow coating process through a conventionally known " coffee-ring effect ". The ring strain was caused by the capillary flow during the droplet drying. The three-phase (liquid-solid-gas) contact line of the droplet tended to be congested as the volume of the droplet decreased due to solvent evaporation. The volume of the droplet evaporated from the edge of the droplet decreased and replenished from the inside thereof, so that the flow of the edge ward carried the non-volatile element in the solution to the droplet edge. The contact angle of the droplet was lowered below the critical angle, so that the solution was out of the contact line and fixed to the new contact line. The contact line was continuously switched between the fixed state and the non-fixed state.
The flow coating method adopted in this embodiment (Fig. 12 (a)) performed the adjustment to the contact line at the liquid-solid-gas interface using the polymer blade attached to the vertical movement stage. The method enabled regular adjustment of the formation of a plurality of periodic lines. The AgNP solution was injected between the polymer blade and the substrate and trapped by the capillary force. The substrate attached to the linear moving stage remained stationary for a period of time so that the non-volatile AgNP in the toluene solution migrated to the contact line during toluene evaporation, as shown in Figure 12 (b) , A line of AgNP was deposited. The polymer blades were moved at regular intervals and the meniscus was pulled until the contact angle fell below a critical lower limit angle. The capillary force exceeded a pinning force and the contact line moved to a new point. As a result, the contact angle was restored to its initial value leaving a new AgNP line. As mentioned above, the above steps were repeated and parallel lines of AgNP were obtained (Fig. 12 (c)). The interval between movements of the linear moving stage between the periodic stopping times (1 second) was varied from 50 μm to 250 μm, and the moving speed thereof was 1.5 mm / s (FIG. 12 (d)). In the present embodiment, the widths and intervals of the lines were adjusted by varying the solution concentration and the moving distance, respectively.
[ Experimental Example ]
The light transmittance of the Ag metal grid electrode was characterized by UV-vis spectrophotometry (Agilent 8453) and sheet resistance was measured using a four-point probe technique using Keithley 2182A and Keithley 6221 units Respectively. The output voltage and output current density of the piezoelectric nanosgenerators based on Ag metal grid electrodes were measured using a nanovoltmeter (Keithley 2182A) and a picoammeter (Keithley 6475), respectively.
1. Line width control of metal pattern according to metal solution concentration
In this embodiment, the line width of the AgNP pattern was systematically adjusted by varying the concentration of AgNP in the solution to 1 mg / mL to 10 mg / mL. 13 (a) shows an optical microscope image of the AgNP line pattern, which shows that the line width increased with the AgNP concentration. For example, concentrations of 1 mg / mL and 10 mg / mL AgNP produced line widths of 2.7 μm and 13.1 μm, respectively. The line width was plotted as a function of AgNP concentration in Figure 14 (a). This tendency can be understood qualitatively in terms of the fact that a higher concentration has resulted in a wider line by further feeding AgNP towards the edge of the meniscus. It was noted that the thickness (or height) of the Ag line remained constant because the fixed height was induced by the strong interlaminar force between the obtained polymer blade and the substrate (FIG. 15).
2. Characterization of metal pattern by metal solution concentration
At higher AgNP concentrations above 7 mg / mL, AgNP clusters were obtained in the region between the lines, which dramatically reduced the optical transmittance of the line electrodes (FIG. 16). Unnecessary AgNP clusters may have formed in solutions above the critical concentration since the AgNP can not move perfectly to the later position during the movement of the linear moving stage.
As shown in Fig. 13 (b), the AgNP wire pattern produced by the flow coating was sintered by heat at 150 캜 for 1 hour. It was confirmed that the line width was finely decreased after thermal sintering (Fig. 14 (a)). The AgNP line fabricated in this pattern contained organic ligand molecules between the AgNPs. During thermal sintering, the above molecules were degraded and gradually the distance between AgNPs decreased. The AgNP completely removed the ligand molecules and finally formed contact with other AgNPs. As shown in Fig. 14 (b), the resistivity of a single Ag wire after heat sintering was measured. The Ag line prepared using AgNP solution of 5 mg / mL or less was not conductive because the Ag lines were not connected. On the other hand, when the AgNP concentration was further increased, a highly conductive Ag wire was obtained after thermal sintering. The resistivity of the single Ag line was decreased by increasing the concentration of AgNP in the solution. The higher concentration produced a wider line, which reduced the resistivity of the Ag line.
3. Analysis of characteristics of metal pattern by controlling line width and line spacing
In addition, the line spacing could be controlled by various travel distances (50 [mu] m to 250 [mu] m) between the periodic stopping times of the polymer blades. The AgNP concentration and the polymer blade velocity were fixed at 7 mg / mL and 1.5 mm / s, respectively. The patterned AgNP line spacing was associated with the programmed travel distance (Figure 17). Figure 17 is an optical microscopy (OM) image of an AgNP line pattern fabricated with various movement distances (50, 100, 150, and 250 [mu] m) between the periodic stopping times of the polymer blades.
As shown in Fig. 5 (a), in this embodiment, a transparent flexible Ag grid electrode was fabricated. The first AgNP wire was patterned on the PEN substrate through a flow coating and sintered by heat in a chamber to prevent dissolution of the AgNP during the patterning of the second AgNP wire. The stage was rotated at 90 degrees. The second AgNP wire was patterned and sintered. Figure 5 (b) shows OM and photographic images of a large area Ag grid electrode with a grid width of 8 [mu] m and a grid spacing of 200 [mu] m produced by flow coating on a PEN substrate. Optical transmittance and sheet resistance were controlled by various AgNP concentrations. The optical transmittance over the range of 300 nm to 1,000 nm decreased with the value of the solution concentration (Fig. 6). The about 407 nm absorption peak was due to local surface plasmon resonance (30 nm to 40 nm) of AgNP clusters in the region between the lines. The peak suddenly increased at AgNP concentrations above 7 mg / mL. As shown in FIG. 7, the sheet resistance of the Ag grid electrodes prepared using various AgNP concentrations (6 mg / mL, 7 mg / mL, 8 mg / mL, 9 mg / mL, and 10 mg / mL) Optical transmittance (at 550 nm) is summarized. Both optical transmittance and sheet resistance decreased with increasing grid width. For example, grid widths of 7.5 μm and 10.6 μm produced sheet resistance (optical transmittance) of 332 Ω / sq (88%) and 132 Ω / sq (70%), respectively.
Flexible transparent Ag electrodes were successfully prepared using a flow coating method and used as an electrode of a flexible piezoelectric nano-generator (Fig. 3). The characteristics of the Ag grid pattern formed from the 7 mg / mL AgNP solution were optimized using the process described above for use as a bottom electrode in a piezoelectric nano generator: the movement speed of the polymer blades and the periodic stopping times were 1.5 mm / s and 1 sec, respectively. The width, spacing, and thickness of the grid were 8 [mu] m, 200 [mu] m, and 60 nm, respectively. The final Ag grid electrodes exhibited a sheet resistance of 174? / Sq and 86% of the optical transmittance at 550 nm. In this embodiment, P (VDF-TrFE) was used as a piezoelectric active material. The most stable phase of PVDF under ambient temperature and pressure is the? Phase, which is nonpolar and paraelectric due to the centrosymmetry of the unit cell, but the specific molar ratio (VDF content is Copolymerization with trifluoroethylene (TrFE) at 50% to 80% yielded piezoelectric crystalline beta phase. The introduction of the third fluorine component into the TrFE monomer increased the steric hindrance and preferred the all-trans structure, which led to the formation of the piezoelectric beta phase.
Prior to the spin coating of the P (VDF-TrFE) layer, a single-layer graphene (SLG) film grown by CVD is first transferred onto the patterned Ag electrodes so that the charges induced by the nano- Lt; RTI ID = 0.0 > and / or < / RTI > The P (VDF-TrFE) was spin coated on the Ag pattern and the SLG electrode, and then annealed by heat at 140 캜 for 3 hours to improve the orientation of the crystalline phase. The surface morphology and cross section of the P (VDF-TrFE) layer are shown in Fig. After deposition of the top Ag electrode by thermal evaporation, the electropolishing process was applied to the development of highly oriented molecular dipoles in the P (VDF-TrFE) layer.
4. Analysis of the characteristics of metal patterns
FIGS. 3A and 3B are structural diagrams of a flexible nano-generator manufactured according to the above-described embodiment. FIGS. 4A and 4B show a case where only graphene is used as a lower electrode, FIG. 5 is a graph showing a voltage characteristic and a current characteristic for a case including a pattern, a case including a longitudinal line pattern, and a case including a lattice pattern. The nano-generator manufactured according to the present embodiment generated a voltage of about 4.8 V, which was about four times higher than that of using only graphene as the lower electrode (1.2 V or lower). Specifically, Figures 4 (a) and 4 (b) show typical output voltage and current densities of a series flexible piezoelectric nano-generator fabricated from four different lower electrodes and following a strain of 0.18%. The results using only the SLG for comparison with the Ag line -SLG (red) in the horizontal (longitudinal) direction, the Ag line -SLG (green) in the vertical (transverse direction), and the Ag grid- ). The nanosgenerators fabricated using the SLG bottom electrode obtained the lowest output voltage of 1.2 V because the SLG sheet resistance (964 OMEGA / sq) was higher than that obtained from other electrodes. Higher output voltages (2 V) were observed in a piezoelectric nano-generator based on both the horizontal Ag line-SLG bottom electrode and the vertical Ag line-SLG bottom electrode. Importantly, the nanosgenerator produced using the Ag Grid-SLG exhibited a much higher output voltage in excess of 4.8 V, which can be described as follows. First, the grid-SLG patterns obtained a much lower sheet resistance than the linearly patterned electrodes. Second, the contact area between the Ag grid pattern and the P (VDF-TrFE) layer was twice the contact area of the linearly patterned electrodes and was more effective when contacting the charge produced by the strain-induced piezoelectric potential . Similarly, the current density of the nano-generator produced by the different lower electrodes showed the same tendency as the output voltage (Fig. 4 (b)).
5. Of the nano generator Bending property
The mechanism by which the piezoelectric nano-generator generates power can be described as follows. In the piezoelectric nano-generator, the aligned negative dipoles (V - ) push out the electrons and capture the holes in the lower Ag pattern / SLG electrode while the aligned dipoles (V + ) Pushes holes and catches electrons in the upper electrode (bottom of FIGS. 3 (a) and 3 (b)). When compressive strain was applied to the nanosgenerator, the enhanced piezoelectric potential was immediately transferred from the lower Ag pattern / SLG electrode to the upper Ag electrode via external circuits neutralized by holes present in the upper electrode. Positive output voltage and output current density. Electrons (holes) have accumulated at the interface between the upper (lower) electrode and P (VDF-TrFE) due to the excellent insulating property of P (VDF-TrFE). As a result of the strain being released, the piezoelectric potential immediately disappeared, and the accumulated electrons flowed back through the external circuit and neutralized by accumulating holes in the lower electrode. This process caused the output voltage and output current density of the cathode. Thus, the repeated compression and decoupling processes formed periodic AC output voltage and output current density.
The bending stability of the flexible nano-generator manufactured according to this embodiment was characterized. Fig. 3 (b) shows the bent nano generator. 8 to 10 are graphs showing electrical characteristics and cycle characteristics according to the degree of bending of the flexible nano-generator according to the present embodiment. When the device was bent and evaluated for 3,000 times, no performance degradation was observed, and the device stability was excellent.
Specifically, the output signal of the flexible piezoelectric nano-generator manufactured using the Ag grid / SLG upper electrode was examined as a function of the applied strain. As shown in the inset of FIG. 8, a strain of 0.10% to 0.18% was applied to the nanosgenerator. The applied strain? Y was calculated as? Y = h / 2R, where h is the thickness of the PEN substrate and R is the radius of curvature (Fig. 19). Figure 8 shows the output pulse signals under different strains: 0.10% (black), 0.12% (red), 0.14% (green), 0.16% (blue), and 0.18% (gray). The current density increased from 0.27 μA / cm 2 to 0.51 μA / cm 2 while the output voltage gradually increased from 2.7 V to 4.8 V as the strain increased. The statistical output signals under different strains are shown in Fig. A large strain induced a higher piezoelectric potential within the nanogenerator, which increased the output pulse signal. The durability of the nano-generator was tested as 3,000 cycles (FIG. 10). The highest and most stable output voltage with alternating anode and cathode bias was measured in a durability test. Finally, as shown in FIG. 11, it has been shown that the nanocrystals fabricated successfully can operate ordinary LEDs successfully. Therefore, the nano-generator according to the present invention is expected to be applicable to various applications such as portable electronic devices, sensors, and medical science because it is transparent and flexible.
In this embodiment, a metal grid pattern is formed on a transparent and flexible substrate, and one layer of graphene is placed thereon to form a lower electrode of a metal grid-graphene hybrid structure. In addition, through this process, a high-performance nano-generator can be realized as compared with the conventional graphene nano-generator. The metal lattice structure can be manufactured by a method such as photolithography, stamping, or inkjet printing, but has disadvantages such as a high cost and complicated process. Accordingly, in this embodiment, lines and lattice patterns were produced using the evaporation characteristics of a solution called flow coating, and metal patterns could be formed more simply and inexpensively.
It will be understood by those of ordinary skill in the art that the foregoing description of the embodiments is for illustrative purposes and that those skilled in the art can easily modify the invention without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. For example, each component described as a single entity may be distributed and implemented, and components described as being distributed may also be implemented in a combined form.
The scope of the present invention is defined by the appended claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be interpreted as being included in the scope of the present invention .
100: substrate 200: lower electrode
210: metal pattern layer 220: two-dimensional nanomaterial layer
300: ferroelectric layer 400: upper electrode
Claims (17)
A lower electrode comprising a metal pattern layer formed on the substrate and a two-dimensional nanomaterial layer formed on the metal pattern layer;
A ferroelectric layer formed on the lower electrode; And
And an upper electrode formed on the ferroelectric layer,
Wherein the lower electrode has a resistance lowered by the metal pattern layer,
Wherein the metal pattern layer comprises a metal selected from the group consisting of Ag, Au, Pt, Al, Cu, Cr, V, Mg, Ti, Sn, Pb, Pd, W, Ni,
Wherein the two-dimensional nanomaterial layer is formed from a group consisting of graphene, graphene oxide, SnSe 2 , MoS 2 , TiS 2 , VS 2 , WS 2 , MoSe 2 , WSe 2 , MoTe 2 , TiTe 2 , A flexible nano generator that is selected.
Wherein the substrate is transparent and flexible.
Wherein the metal pattern layer comprises a shape selected from the group consisting of engraved, embossed, and combinations thereof.
Wherein the metal pattern layer includes a plurality of line patterns or a lattice pattern.
The ferroelectric layer is poly (vinylidene fluoride-co-ethylene trifluoroacetate), poly (vinylidene fluoride), Pb (Zr, Ti) O 3, SrBi 2 Ti 2 O 9, Bi (La, Ti) O 3, Pb (La, Zr) TiO 3, Bi (Sr, Ti) O 3, and which is to made up of a combination thereof is selected from the group including a ferroelectric, a flexible nano-generator.
Wherein the upper electrode comprises a material selected from the group consisting of Ag, Au, Pt, Al, Cu, Cr, V, Mg, Ti, Sn, Pb, Pd, W, Ni, alloys thereof, A flexible nano generator.
Wherein the flexible nano generator generates a voltage of 1.5 V to 6 V.
Wherein the flexible nano-generator is transparent.
Forming a lower electrode by forming a two-dimensional nanomaterial layer on the metal pattern layer;
Forming a ferroelectric layer on the lower electrode; And
Forming an upper electrode on the ferroelectric layer
, ≪ / RTI &
Wherein the lower electrode has a resistance lowered by the metal pattern layer,
Wherein the metal pattern layer comprises a metal selected from the group consisting of Ag, Au, Pt, Al, Cu, Cr, V, Mg, Ti, Sn, Pb, Pd, W, Ni,
Wherein the two-dimensional nanomaterial layer is formed from a group consisting of graphene, graphene oxide, SnSe 2 , MoS 2 , TiS 2 , VS 2 , WS 2 , MoSe 2 , WSe 2 , MoTe 2 , TiTe 2 , Wherein the method comprises the steps of:
Wherein the metal pattern layer is formed by flow coating, photolithography, stamping, or inkjet printing.
Wherein the metal pattern layer comprises a shape selected from the group consisting of engraved, embossed, and combinations thereof. ≪ RTI ID = 0.0 > 21. < / RTI >
Wherein the metal pattern layer includes a plurality of line patterns or a lattice pattern.
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