KR20170026729A - Light sintering apparatus of metal nano particle composition and method for manufacturing conductive substrate using the same - Google Patents
Light sintering apparatus of metal nano particle composition and method for manufacturing conductive substrate using the same Download PDFInfo
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- KR20170026729A KR20170026729A KR1020150120785A KR20150120785A KR20170026729A KR 20170026729 A KR20170026729 A KR 20170026729A KR 1020150120785 A KR1020150120785 A KR 1020150120785A KR 20150120785 A KR20150120785 A KR 20150120785A KR 20170026729 A KR20170026729 A KR 20170026729A
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- sintering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0033—Apparatus or processes specially adapted for manufacturing conductors or cables by electrostatic coating
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21K—NON-ELECTRIC LIGHT SOURCES USING LUMINESCENCE; LIGHT SOURCES USING ELECTROCHEMILUMINESCENCE; LIGHT SOURCES USING CHARGES OF COMBUSTIBLE MATERIAL; LIGHT SOURCES USING SEMICONDUCTOR DEVICES AS LIGHT-GENERATING ELEMENTS; LIGHT SOURCES NOT OTHERWISE PROVIDED FOR
- F21K9/00—Light sources using semiconductor devices as light-generating elements, e.g. using light-emitting diodes [LED] or lasers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The present invention relates to a photo-sintering apparatus for a metal nanoparticle composition and a method of manufacturing a conductive substrate using the same, wherein a metal nanoparticle composition coated on a substrate is coated and then photo-sintered to form a conductive layer having good electrical and physical properties . The light sintering apparatus according to the present invention includes a substrate mounting portion and a dual light sintered portion. The substrate mounting part has a substrate on which a coating layer is formed by applying a metal nanoparticle composition containing copper nanoparticles on an upper surface, and an opening is formed to expose the lower part of the substrate. The dual light sintered portion is provided on the upper portion of the substrate mounting portion and below the opening portion of the substrate mounting portion, and is irradiated with light to the upper and lower portions of the substrate to photo-sinter the coating layer to form a conductive layer.
Description
The present invention relates to a light sintering apparatus and method, and more particularly, to a light sintering apparatus for a metal nanoparticle composition which forms a conductive layer by applying light scattering to a metal nanoparticle composition coated on a substrate, And a method for producing the same.
Light sintering has been used as a method for producing a conductive substrate (film) including a conductive layer using a composition containing metal nanoparticles such as copper nanoparticles (hereinafter referred to as a 'metal nanoparticle composition').
In the conventional light sintering method, the metal nanoparticle composition is prepared in the form of an ink or a paste, and then coated on the substrate to form a coating layer. Then, the conductive layer is formed by photo-sintering the coating layer on the substrate by light irradiation. At this time, a xenon lamp is mainly used as a light irradiation means.
In the conventional light sintering method, when the coating layer is thick, the light sintering is performed well at the surface portion of the coating layer, but the light sintering portion at the portion contacting the substrate has a disadvantage that the light sintering is not performed well. That is, when the coating layer is thick, the light irradiated at the time of photo-sintering may not affect the lower portion of the coating layer. In this case, the lower portion of the coating layer, that is, the portion contacting the substrate, may not be sintered well.
On the contrary, even if the thickness of the coating layer is thin, the adhesion force with the substrate is insufficient, and peeling phenomenon in which the conductive layer is separated from the substrate after light sintering may easily occur. That is, even if the thickness of the coating layer is thin, the light sintering increases the resistance in the vertical direction from the top of the conductive layer toward the substrate, because the top of the coating layer is made better than the bottom. This may cause a problem that the adhesive force between the substrate and the conductive layer is reduced and the conductive layer is separated from the substrate.
When the substrate is a flexible substrate having a small thickness, the substrate may easily bend due to the high energy of the light to be irradiated. That is, the light output from the xenon lamp for irradiating the coating layer includes ultraviolet light, visible light and infrared light as white light. The ultraviolet light and the visible light contained in the light output from the xenon lamp are absorbed by the metal nanoparticles, but the infrared part is absorbed by the substrate, which causes the substrate to warp.
Accordingly, an object of the present invention is to provide a photo-sintering apparatus for metal nano-particle composition capable of photo-sintering the entire coating layer even if the thickness of the coating layer is thick, and a method for manufacturing a conductive substrate using the same.
Another object of the present invention is to provide a photo-sintering apparatus for a metal nano-particle composition capable of maintaining a good adhesive force between a conductive layer and a substrate after photo-sintering, and a method of manufacturing a conductive substrate using the same.
Still another object of the present invention is to provide a light sintering apparatus for a metal nano-particle composition capable of suppressing the phenomenon that a substrate is bent by light sintering even if the substrate is a thin flexible substrate, and a method for manufacturing a conductive substrate using the same .
In order to achieve the above object, the present invention provides a method of manufacturing a metal nanoparticle composition, comprising: forming a coating layer by applying a metal nanoparticle composition containing copper nanoparticles on a substrate; drying the coating layer; And a step of photo-sintering the coating layer by irradiating light to a lower portion to form a conductive layer. The present invention also provides a method of manufacturing a conductive substrate using light sintering.
In the method of manufacturing a conductive substrate according to the present invention, in the step of forming the conductive layer, white pulsed light is irradiated onto the upper part of the coating layer using a xenon lamp, and ultraviolet to visible light band The LED light of at least one band can be irradiated to the lower portion of the coating layer.
In the method of manufacturing a conductive substrate according to the present invention, in the step of forming the conductive layer, white pulsed light is irradiated onto the upper part of the coating layer using a xenon lamp, white light is irradiated onto the lower part of the coating layer .
In the method of manufacturing a conductive substrate according to the present invention, in the step of forming the conductive layer, the white pulsed light has a pulse width of 100 to 5000 us, an output voltage of 100 to 900 V, a pulse number of 1 to 10, J / cm2 to 60 J / cm < 2 >.
The present invention also provides a light sintering apparatus for a metal nanoparticle composition comprising a substrate mounting part and a dual light sintered part. The substrate mounting part includes a substrate on which a coating layer is formed by applying a metal nanoparticle composition containing copper nanoparticles on an upper surface thereof, and an opening is formed to expose a lower portion of the substrate. The dual light sintered part is provided on the upper part of the substrate mounting part and the opening part of the substrate mounting part, and the upper layer and the lower part of the substrate are irradiated with light to photo-sinter the coating layer to form a conductive layer.
In the light sintering apparatus of the present invention according to the present invention, the dual light sintering unit may include a xenon lamp unit and an LED module. The xenon lamp unit is installed on the upper part of the substrate mounting part and irradiates the upper part of the coating layer with white pulsed light. The LED module is installed below the open part of the substrate mounting part and irradiates the coating layer with LED light of at least one of the ultraviolet to visible light band through the lower part of the substrate.
In the light sintering apparatus of the present invention according to the present invention, the dual light sintering unit may include a xenon lamp unit and a halogen lamp. The xenon lamp unit is installed on the upper part of the substrate mounting part and irradiates the upper part of the coating layer with white pulsed light. The halogen lamp is installed below the opening of the substrate loading part and irradiates white light through the lower part of the substrate.
According to the present invention, since the dual light sintered part forms a conductive layer by uniformly sintering the entire coating layer by irradiating light from above and below a coating layer formed by applying a metal nanoparticle composition containing copper nanoparticles on a substrate, Even if the thickness of the coating layer is thick, the entire coating layer can be uniformly photo-sintered.
Also, since the conductive layer is formed by uniformly sintering the entire coating layer by irradiating light from the upper and lower portions of the coating layer through the dual light sintered portion, resistance variation in the vertical direction of the conductive layer is reduced, Good adhesion can be maintained.
In addition, since the substrate on which the coating layer is formed is uniformly irradiated with light uniformly over a short period of time through the dual light sintered portion to perform light sintering, compared to a method in which light is irradiated and sintered only at the upper portion of the existing coating layer, The problem of bending can be suppressed. That is, when light sintering is performed, white pulsed light is irradiated to the upper portion of the coating layer using a xenon lamp. Infrared rays included in white pulsed light are absorbed by the substrate, which is a major cause of bending the substrate. In the present invention, since the light is irradiated from the top and bottom of the substrate, the light energy of the xenon lamp irradiated at the top of the substrate can be lowered, and the problem of warping of the substrate can be suppressed.
1 is a view showing a photo-sintering apparatus for a metal nanoparticle composition according to an embodiment of the present invention.
2 is a graph showing the spectrum of a xenon lamp used in light sintering.
3 is a graph showing absorption spectra of copper nanoparticles contained in the metal nanoparticle composition.
4 is a graph showing the wavelength band of light emitted from the LED module of FIG.
5 is a flowchart illustrating a method of manufacturing a conductive substrate using the light sintering apparatus of FIG.
6 to 10 are views showing respective steps of the method of manufacturing the conductive substrate of FIG.
11 is a SEM photograph of the conductive layer manufactured by the manufacturing method according to the comparative example.
12 is a SEM photograph of the conductive layer manufactured by the manufacturing method according to the embodiment.
In the following description, only parts necessary for understanding embodiments of the present invention will be described, and descriptions of other parts will be omitted to the extent that they do not disturb the gist of the present invention.
The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary meanings and the inventor is not limited to the meaning of the terms in order to describe his invention in the best way. It should be interpreted as meaning and concept consistent with the technical idea of the present invention. Therefore, the embodiments described in the present specification and the configurations shown in the drawings are merely preferred embodiments of the present invention, and are not intended to represent all of the technical ideas of the present invention, so that various equivalents And variations are possible.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
1 is a view showing a photo-sintering apparatus for a metal nanoparticle composition according to an embodiment of the present invention. 10 is a cross-sectional view showing a conductive substrate manufactured by the light sintering apparatus of FIG.
Referring to FIGS. 1 and 10, the
The
The dual optical
At this time, the
The light sintering refers to a series of processes in which metal particles are necked and then metallized by irradiating the
The reason why the white pulse light 45 generated from the
When a flexible substrate is used for the production of a conductive substrate, the
If the pulse width of the white pulsed light 45 is larger than 5000 mu s, the incident energy per unit time is reduced and the light sintering efficiency may be lowered.
If the pulse gap is greater than 1 ms or the number of pulses is greater than 10, the
In addition, when the pulse gap is less than 0.01 ms or the intensity of the white pulse light 45 is more than 60 J / cm 2, the damage or the life of the
In addition, when the intensity of the white pulse light 45 is 1 J / cm 2 or less, the reduction reaction for reducing the copper oxide film of the copper nanoparticles to copper is weak, so that the electrical resistance characteristic of the
On the contrary, when the intensity of the
The
In this embodiment, an
The reason for using the
Referring to FIG. 2, the spectrum of the
The absorption spectrum of the copper nanoparticles contained in the metal nanoparticle composition is shown in FIG. 8 shows an absorption spectrum when the size of the copper nanoparticles is 100 nm and the thickness of the copper oxide film of the copper nanoparticles is 7 nm. The size of copper nanoparticles and the thickness of copper oxide film change. The absorption spectrum of the surface changes, but copper nanoparticles generally absorb ultraviolet to visible light.
As a result, the metal nanoparticle composition containing the copper nanoparticles is coated on the
Also, when the
Therefore, in this embodiment, the
For example, as shown in FIG. 4, an
On the other hand, FIG. 4 shows an example of using the
In this embodiment, the
As described above, according to the present embodiment, the dual light-sintered
Since the
In addition, since light is uniformly irradiated to the
A method of manufacturing the
First, as shown in Fig. 6, a
The metal nanoparticle composition for forming the
The metal nanoparticles may further include silver nanoparticles in addition to copper nanoparticles, silver powder in the form of flakes, and the like.
Copper nanoparticles on which copper oxide film is formed are non-conductive but converted into copper particles having conductivity by light sintering to be used as a conductor source. The copper nanoparticles may be core-shell type particles, and the copper oxide film on the surface may be formed to a thickness of 50 nm or less. At this time, copper nanoparticles having a thickness of 50 nm or less are used for the copper oxide film because if the thickness of the copper oxide film is more than 50 nm, a part of the copper oxide film may not be reduced to copper by light irradiation to be. The copper nanoparticles may have a D 50 of 900 nm or less and a D max of 2 μm or less.
The reducing agent reduces the copper oxide film of the copper nanoparticles to copper by light irradiation. Examples of the reducing agent include an aldehyde-based compound, an acid including ascorbic acid, a phosphorus-containing compound, a metal-based reducing agent, p-benzoquinone, hydroquinone or anthraquinone.
For example, formaldehyde, acetaldehyde, etc. may be used as the aldehyde compound used as a reducing agent.
Examples of the acid used as the reducing agent include oxalic acid, formic acid, ascorbic acid, sulfonic acid, dodecyl benzene sulfonic acid, maleic acid, Hexamic acid, phosphoric acid, O-phthalic acid, acrylic acid, and the like can be used.
Phosphites, hypophosphites and phosphorous acid may be used as the phosphorus compound used as a reducing agent. The phosphorus compounds in the reducing agent are hydrogenphosphonates (acid phosphites) containing H2 (O) 2 OH - groups such as NH 4 HP (O) 2 OH containing PO 3 3- groups, H2P 2 O 5 2- Phosphites including HPO 3 2- such as diphosphites, (NH 4 ) 2 HPO 3 O H 2 O, CuHPO 3 O H 2 O, SnHPO 3 , and Al 2 (HPO 3 ) 3 O 4 H 2 O, (RO) phosphite ester, Hypophosphite ( H 2 PO 2 -) , such as 3 P, phosphatidylcholine, triphenylphosphate, cyclophosphamide , parathion, Sarin (phosphinate), Glyphosate (phosphonate), fosfomycin (phosphonate), zoledronic acid (phosphonate), and Glufosinate (phosphinate) organic phosphines such as Organophosphorus, triphenylphosphine, etc. (PR 3), triphenylphosphine oxide such as Phosphine oxide (OPR 3), ( CH 3 O) Phosphonite (P (OR) R 2) , such as 2 PPh, Phosphonite (P (OR) 2 R), Phosphinate (OP (OR) R 2 ), organic phosphonates (OP (OR) 2 R), Phosphate (PO 4 3- ), parathion, malathion, methyl parathion, chlorpyrifos , organophosphate (OP (OR) 3 ) such as diazinon, dichlorvos, phosmet, fenitrothion, tetrachlorvinphos, azamethiphos, azinphos methyl and the like.
As the metal reducing agent, lithium aluminum hydride (LiAlH 4 ), diisobutylaluminum hydride (DIBAL-H) and Lindlar catalyst can be used.
By including the reducing agent as a catalyst of the metal nanoparticle composition, it is possible to perform sintering through light irradiation, thereby suppressing damage such as warpage or shrinkage of the
In the metal nanoparticle composition according to the present embodiment, the reducing agent is preferably added in an amount of 0.1 to 5 parts by weight based on 100 parts by weight of the metal nanoparticles. If the addition amount of the reducing agent is more than 5 parts by weight, there may arise a problem of lowering the dispersibility in the metal nanoparticle composition and lowering the homogeneity due to lowering of the compatibility. On the contrary, if the amount of the reducing agent is less than 0.1 part by weight, a problem of not being smoothly reduced and sintered by light irradiation may occur.
The dispersing agent uniformly disperses the metal nanoparticles including the copper nanoparticles in the metal nanoparticle composition to suppress the generation of pores in the
Examples of the dispersing agent include an amine-based polymer dispersing agent such as polyethyleneimine and polyvinylpyrrolidone; a hydrocarbon-based polymer dispersing agent having a carboxylic acid group in the molecule such as polyacrylic acid and carboxymethylcellulose; a polyvinyl alcohol-based resin such as POVAL (polyvinyl alcohol) A polymer dispersant having a polar group such as a copolymer, an olefin-maleic acid copolymer, or a copolymer having a polyethyleneimine moiety and a polyethylene oxide moiety in one molecule may be used, but is not limited thereto.
The binder functions as a material that binds metal nanoparticles when the
Examples of such binders include PVP, PVA and PVC, cellulose resins, polyvinyl chloride resins, copolymer resins, polyvinyl alcohol resins, polyvinyl pyrrolidone resins, acrylic resins, vinyl acetate- An alkyd resin, an epoxy resin, a phenol resin, a rosin ester resin, a polyester resin, or silicone may be used, but is not limited thereto.
For example, a mixed resin of an epoxy acrylate, a polyvinyl acetal, and a phenol resin may be used as the binder. By using the above-mentioned mixed resin as a binder, thermal curing can be performed at a temperature of about 150 ° C. (a three-dimensional network structure can be formed to form a thermally highly stable structure), whereby the heat resistance of the metal nanoparticle composition can be improved have.
Next, as shown in FIG. 7, a
Next, as shown in FIG. 8, the
Then, photo-sintering is performed on the dried
The
The copper nanoparticles of the
The characteristics of the
In
The paste containing copper nanoparticles was printed on a PET film with a screen printer to form a
In the case of the
Referring to FIG. 11, in the comparative example in which only the xenon lamp was irradiated, it can be confirmed that the lower part of the conductive layer was not sintered.
On the other hand, referring to FIG. 12, in the case of Example 1 in which a xenon lamp and an LED module are used together, it can be confirmed that light sintering is well performed to a lower portion of the conductive layer. That is, it can be confirmed that the conductive layer is uniformly photo-sintered as a whole.
In the case of sheet resistance, the conductive layer of the comparative example without irradiation with LED light was 0.2? / ?, and the conductive layer of Example 1 in which LED light irradiation was simultaneously performed was 0.03? / ?. That is, it can be confirmed that the conductive layer of Example 1 has better electric conductivity than the comparative example.
It should be noted that the embodiments disclosed in the present specification and drawings are only illustrative of specific examples for the purpose of understanding, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that other modifications based on the technical idea of the present invention are possible in addition to the embodiments disclosed herein.
10: Conductive substrate
12: substrate
14: Coating layer
16: conductive layer
20: Light sintering device
30: Substrate mounting part
31:
40: Xenon lamp part
41: Xenon lamp
43: Reflector
45: White pulsed light
50: LED module
51: LED substrate
53: LED element
55: LED light
Claims (6)
Drying the coating layer;
Forming a conductive layer by photo-sintering the coating layer by irradiating light to upper and lower portions of the coating layer dried around the substrate;
Wherein the light-sintering is performed by using a light source.
Wherein the coating layer is irradiated with white pulsed light by using a xenon lamp and the LED light of at least one of ultraviolet to visible light bands is irradiated to the lower part of the coating layer by using an LED module Wherein the conductive substrate is made of a conductive material.
Wherein the white light is irradiated to the top of the coating layer using a xenon lamp and the white light is irradiated to the bottom of the coating layer using a halogen lamp.
Wherein the white pulsed light has a pulse width of 100 to 5000 占 퐏, an output voltage of 100 to 900 V, a pulse number of 1 to 10, and an intensity of 1 J / cm2 to 60 J / cm2. Way.
A dual light sintered portion provided on an upper portion of the substrate mounting portion and an opening portion of the substrate mounting portion to optically sinter the coating layer by irradiating light to upper and lower portions of the substrate to form a conductive layer;
Wherein the metal nanoparticle composition is a metal.
A xenon lamp part provided on the substrate mounting part and irradiating white pulsed light on the coating layer;
An LED module installed below the open part of the substrate loading part and irradiating the coating layer with LED light of at least one of the ultraviolet to visible light band through a lower part of the substrate;
Wherein the metal nanoparticle composition is a sintered body.
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Cited By (1)
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KR20190036211A (en) * | 2017-09-27 | 2019-04-04 | 한국화학연구원 | Light sintering conductive electrode, and method of manufacturing the same |
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KR20140044743A (en) | 2012-10-04 | 2014-04-15 | 한양대학교 산학협력단 | Conductive hybrid cu ink and light sintering method using the same |
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KR20140044743A (en) | 2012-10-04 | 2014-04-15 | 한양대학교 산학협력단 | Conductive hybrid cu ink and light sintering method using the same |
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KR20190036211A (en) * | 2017-09-27 | 2019-04-04 | 한국화학연구원 | Light sintering conductive electrode, and method of manufacturing the same |
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