KR101583304B1 - Conductive metal ion ink composition and method of making the same - Google Patents
Conductive metal ion ink composition and method of making the same Download PDFInfo
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- KR101583304B1 KR101583304B1 KR1020090007737A KR20090007737A KR101583304B1 KR 101583304 B1 KR101583304 B1 KR 101583304B1 KR 1020090007737 A KR1020090007737 A KR 1020090007737A KR 20090007737 A KR20090007737 A KR 20090007737A KR 101583304 B1 KR101583304 B1 KR 101583304B1
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Abstract
There is provided a uniform and oxidation stable metal ion ink composition including a conductive metal or conductive metal precursor, a metal ion generator, a metal ion stabilizer and a solvent, and a method for producing the same.
Ink, conductive metal, metal ion generator, metal ion stabilizer
Description
The present disclosure relates to conductive metal ion ink compositions and methods of making the same.
Inkjet technology is a new type of manufacturing process that realizes this at a time when we are pursuing productivity, cost reduction and creation of new industrial field by enlargement of display industry and process simplification. In particular, inkjet printing technology is a non-contact technology that prints a pattern with jetting ink from the nozzles of the printhead. In such inkjet printing technology, the printhead technology has matured somewhat in industry, but ink design remains a challenge.
In order to achieve optimum driving conditions, durability of the printing system, and the best printing pattern, the ink must meet the demanding physico-chemical characteristics, and in the case of ink, uniformity and stability must be given priority. In addition, in order to be applied to flexible display or RFID substrate or various materials, which have recently been highlighted, the firing temperature after patterning should be low.
As the conductive ink for ink jet, metal nanoparticles having a particle size of several to several tens of nanometers are mainly used as a material for forming fine conductive lines and conductive films. In recent years, studies have been made to fabricate metal ink using nanoparticles and then to form fine wires by inkjet technology. However, due to the high production cost due to the use of silver nanoparticles, there are many restrictions on industrial applications. Therefore, the necessity of copper nanoparticles having a relatively high conductivity while being a low-cost raw material is constantly mentioned, but it is difficult to manufacture stable copper nanoparticles due to low stability of copper, that is, high oxidation.
On the other hand, it is difficult to produce nanoparticles having uniform particle size and stable at the time of nanoparticle production, and dispersion stability in ink is important. Therefore, in order to improve the dispersibility of nanoparticles in the ink, dispersion of nanoparticles is attempted using a dispersant of mainly organic or polymer having a high molecular weight. However, in the case of such a dispersant, there is a problem that the decomposition temperature is generally high and the firing temperature must be increased.
In addition, the techniques related to the conventional ink production are characterized by using a metal compound having environmental pollution and danger after particle production. In addition, it is an industrial disadvantage in that an additional process is required to remove various compounds and ions which are residues that cause deterioration of characteristics after production.
One embodiment of the present invention is to provide a conductive metal ion ink composition that is uniform and stable to oxidation.
Another embodiment of the present invention is to provide a method of manufacturing a conductive metal ion ink composition that is environmentally friendly, economical, and safe, and can be usefully applied to a wide variety of industrial fields.
One embodiment of the present invention provides a conductive metal ion ink composition comprising a conductive metal or conductive metal precursor, a metal ion generator, a metal ion stabilizer and a solvent.
The conductive metal may be a transition metal or a rare earth metal. The conductive metal precursor may be represented by the following formula (1).
[Chemical Formula 1]
M (X) n
In Formula 1,
M is a transition metal or a rare earth metal,
X is a group selected from the group consisting of hydrogen, a hydroxyl group, a halogen group, a cyano group, a cyanate group, a carbonate group, a nitrate group (NO 3 ), a nitrite group (NO 2 ), a sulfate group, a phosphate group, a thiocyanate group, A substituent selected from the group consisting of perfluoro, perfluoro, perfluoro, perfluoro, perfluoro, perfluoro, perfluoro, perfluoro, perfluoro,
and n is determined according to the valence of M.
The metal ion generator may be a carboxylic acid. The carboxylic acid may be represented by the following formula (2), and more specifically, a carboxylic acid selected from the group consisting of formic acid, citric acid, malic acid, lactic acid, malic acid, tartaric acid, and combinations thereof may be used.
(2)
In Formula 2,
R 1 is hydrogen or an alkyl group having 1 to 20 carbon atoms when a is 0 and an alkylene group having 1 to 20 carbon atoms when a is 1 or 2,
a is an integer of 0 to 2,
b is an integer of 1 to 3;
The metal ion stabilizer may be selected from the group consisting of an amine compound, a thiol compound, and a combination thereof. More specifically, the metal ion stabilizer may be selected from the group consisting of compounds represented by the following formulas (3) and (4).
(3)
NR 2 3
[Chemical Formula 4]
R 3 SH
In the above formulas (3) and (4)
R 2 and R 3 are the same or different and each independently selected from the group consisting of hydrogen and an alkyl group having 1 to 20 carbon atoms.
The conductive metal ion ink composition may comprise a metal ion derived from the conductive metal or conductive metal precursor relative to the total amount of the conductive metal ion ink composition 0.1 to 30% by weight, a metal ion generating agent 0.1 to 50% by weight, a metal ion stabilizer 0.1 to 50% by weight, and the balance solvent. The conductive metal ion ink composition preferably contains a metal ion generator and a metal ion stabilizer in a weight ratio of 1: 0.1 to 5.
The conductive metal ion ink composition may further include a functional additive selected from the group consisting of a dispersant, a binder resin, a reducing agent, a surfactant, a wetting agent, a viscoelasticity modifier, a leveling agent, and a combination thereof.
Another embodiment of the present invention is a method for preparing a metal ion-stabilizing agent, comprising: a step of introducing and dissolving a metal ion generator and a metal ion stabilizer into a solvent; And a step of disposing an electrode including a conductive metal in the solution, wherein the step of ionizing the conductive metal in the solution by the electric energy generated by the AC voltage or the DC voltage applied to the electrode and the metal ion generator The present invention provides a method for producing a conductive metal ion ink composition.
Other details of the embodiments of the present invention are included in the following detailed description.
The conductive metal ion ink composition according to one embodiment of the present invention and its manufacturing method are environmentally friendly, economical, and safe, and can be applied not only to ink technology such as inkjet but also to a wide variety of industrial fields.
Hereinafter, embodiments of the present invention will be described in detail. However, it should be understood that the present invention is not limited thereto, and the present invention is only defined by the scope of the following claims.
One embodiment of the present invention provides a conductive metal ion ink composition comprising a conductive metal or conductive metal precursor, a metal ion generator, a metal ion stabilizer, and a solvent.
The conductive metal is a metal included in the conductive metal ion ink composition in order to impart conductivity. The kind of the conductive metal is not particularly limited, but more specifically, a transition metal or an arsenic metal may be used. Particularly, as the conductive metal, a transition metal of
In addition, the conductive metal precursor can easily generate metal ions by the metal ion generator, and organic metal compounds, metal salts, and the like can be used. More specifically, the conductive metal precursor may be represented by the following general formula (1).
[Chemical Formula 1]
M (X) n
In Formula 1,
M is a transition metal or a rare earth metal,
X is a group selected from the group consisting of hydrogen, a hydroxyl group, a halogen group, a cyano group, a cyanate group, a carbonate group, a nitrate group (NO 3 ), a nitrite group (NO 2 ), a sulfate group, a phosphate group, a thiocyanate group, A substituent selected from the group consisting of an alkyl group, a perchlorate group, a tetrafluoroborate group, an acetylacetonate group, a mercapto group, an amide group, an alkoxide group, a carboxylate group and combinations thereof, and n is determined depending on the valence of M . The carbonate group, amide group, alkoxide group or carboxylate group may contain alkyl having 1 to 10 carbon atoms.
In the above formula (1), M is a transition metal or a rare earth metal, and more specific examples of the transition metal and the rare earth metal are as described while describing the conductive metal.
The conductive metal ion ink composition according to an embodiment of the present invention may contain the metal ion derived from the conductive metal or the conductive metal precursor in an amount of 0.1 to 30% by weight based on the total amount of the conductive metal ion ink composition. More specifically, the metal ion derived from the conductive metal or the conductive metal precursor may be included in the range of 5 to 30% by weight. When the conductive metal ion ink composition according to an embodiment of the present invention contains a metal ion derived from a conductive metal or a conductive metal precursor in the above range, an effect of easily controlling the thickness can be obtained.
The metal ion generator may be a carboxylic acid. The carboxylic acid represented by the following formula (2) may be used.
(2)
In the formula (2)
R 1 is hydrogen or an alkyl group having 1 to 20 carbon atoms when a is 0 and an alkylene group having 1 to 20 carbon atoms when a is 1 or 2,
a is an integer of 0 to 2,
b is an integer of 1 to 3;
More specifically, the metal ion generator may be selected from the group consisting of formic acid, citric acid, malic acid, lactic acid, malic acid, tartaric acid, and combinations thereof.
The conductive metal ion ink composition according to an embodiment of the present invention may contain the metal ion generating agent in an amount of 0.1 to 50% by weight based on the total amount of the conductive metal ion ink composition. More specifically, the metal ion generator may be included in the range of 10 to 35% by weight. When the conductive metal ion ink composition according to an embodiment of the present invention contains a metal ion generator in the above-mentioned range, the reaction rate for forming metal ions is fast and the metal ions are stably dispersed in the ink, It is possible to obtain an effect that a conductive film can be produced with pure metal without being precipitated as a solid.
The metal ion stabilizer may be selected from the group consisting of an amine compound, a thiol compound, and a combination thereof. More specifically, the metal ion stabilizer may be selected from the group consisting of the compounds represented by the following formulas (3) and (4) to improve the solubility by uniformly and stably dispersing the conductive metal ion.
(3)
NR 2 3
[Chemical Formula 4]
R 3 SH
In the above formulas (3) and (4)
R 2 and R 3 are the same or different and each independently selected from the group consisting of hydrogen and an alkyl group having 1 to 20 carbon atoms.
More specifically, as the metal ion stabilizer, it is preferable to use an ammonia or ammonia aqueous solution capable of improving the binding ability with the conductive metal ion.
The metal ion stabilizer may be added in a liquid state or may be put into a conductive metal ion ink composition by a bubbling method in a gaseous state. For example, in the case of ammonia, the liquid state of ammonia water or bubbling of ammonia gas can be input.
The conductive metal ion ink composition according to an embodiment of the present invention may contain the metal ion stabilizer in an amount of 0.1 to 50% by weight based on the total amount of the conductive metal ion ink composition. More specifically, the metal ion stabilizer may be included in the range of 3 to 30% by weight. When the conductive metal ion ink composition according to an embodiment of the present invention contains a metal ion stabilizer in the above range, the metal ion can be uniformly and stably produced to improve solubility.
When the metal ion generator and the metal ion stabilizer are contained in a weight ratio of 1: 0.1 to 5, the dispersion stability and the oxidation stability of the conductive metal ion can be improved by controlling the content thereof.
The solvent may be used in an amount of the remainder, and may be adjusted to an appropriate range in order to control the viscosity of the ink composition or to form a smooth film. Such a solvent is not particularly limited as long as it can use both an aqueous solvent and a non-aqueous solvent. More specifically, examples of the solvent include water, alcohols such as methanol, ethanol, isopropanol, 1-methoxypropanol, butanol, ethylhexyl alcohol and terpineol; Glycols such as ethylene glycol and glycerin; Acetates such as ethyl acetate, butyl acetate, methoxypropyl acetate, carbitol acetate, ethyl carbitol acetate; Ethers such as methyl cellosolve, butyl cellosolve, diethyl ether, tetrahydrofuran and dioxane; Ketones such as methyl ethyl ketone, acetone, dimethyl formamide and 1-methyl-2-pyrrolidone; Hydrocarbon solvents such as hexane, heptane, dodecane, paraffin oil and the like; Aromatic solvents such as benzene, toluene and xylene; Halogen-substituted solvents such as chloroform, methylene chloride and carbon tetrachloride; Acetonitrile; Dimethyl sulfoxide; And a combination of these may be used.
In addition, the conductive metal ion ink composition according to an embodiment of the present invention includes a dispersing agent, a binder resin, a reducing agent, a surfactant, a wetting agent, a thixotropic agent, a leveling agent, ≪ / RTI > Each of these additives is generally used in the art, and the kind thereof is not particularly limited, but more specifically, the following additives can be used.
The dispersant may be necessary to smoothly disperse the conductive metal or conductive metal precursor when present in the form of particles or flakes. More specifically, the 4000 series of EFKA, the Disperbyk series of BYK, the Solsperse series of Avecia, the TEGO Dispers of Deguessa, Series, the Disperse-AYD series from Elementsys, and the JONCRYL series from Johnson Polymers.
Examples of the binder resin include acrylic resins such as polyacrylic acid or polyacrylic acid esters, cellulose resins such as ethyl cellulose, cellulose ester, cellulose nitrate, aliphatic or copolymerized polyester resins, polyvinyl butyral, polyvinyl acetate, Polyolefin resins such as polyamide resins, polyether resins and urea resins, alkyd resins, silicone resins, fluororesins, olefin resins such as polyethylene and polystyrene, thermoplastic resins such as petroleum resins and rosin resins Based resin, an epoxy resin, an unsaturated or vinyl polyester resin, a diallyl phthalate resin, a phenol resin, an oxetane resin, an oxazine resin, a bismaleimide resin, a silicone epoxy or a silicone poly Modified silicone resins such as esters, melamine resins and the like Thermosetting resins, ultraviolet or electron beam acrylic resins of various structures of curing, and ethylene may be used together with a butadiene rubber (SBR), starch, and natural polymers such as gelatin, select one or more categories - propylene rubber (EPR), styrene. In addition to the above-mentioned organic resin binders, inorganic binders such as glass resin and glass frit, silane coupling agents such as trimethoxypropyl silane and vinyl triethoxy silane, or titanium-based, zirconium-based and aluminum- The system can be used.
In order to facilitate the calcination, a reducing agent may be added. For example, hydrazine, acetic hydrazide, sodium or potassium borohydride, triosodium citrate, and methyldiethanolamine, dimethylamine borane, , Metal salts such as iron chloride, ferrous lactate, hydrogen, hydrogen iodide, carbon monoxide, formaldehyde, aldehyde compounds such as acetaldehyde, glucose, ascorbic acid, salicylic acid, tannic acid, (pyrogallol), and hydroquinone.
Surfactants include anionic surfactants such as sodium lauryl sulfate, nonyl phenoxy-polyethoxyethanol, and bees such as FSN from DuPont (Dupont) Cationic surfactants such as lauryl benzyl ammonium chloride and amphoteric surfactants such as lauryl betaine and cocobetain can be used.
As wetting or wetting dispersants there may be used compounds such as polyethylene glycol, Surfynol series from Air Products, and TEGO Wet series from Deguessa.
Viscoelasticity modifiers or leveling agents include the BYK series of BYK, the Glide series of Degussa, the EFKA 3000 series of EFKA, the DSX of Cognis, (DSX) series can be used.
The method of preparing a conductive metal ion ink composition containing a conductive metal ion ink composition according to an embodiment of the present invention is not particularly limited as long as it is a method generally used in the art, have.
In another embodiment of the present invention, there is provided a method for preparing a metal ion-stabilizing agent, comprising: a step of adding a metal ion generator and a metal ion stabilizer to a solvent and dissolving the same; And a step of disposing an electrode including a conductive metal in the solution, wherein the step of ionizing the conductive metal in the solution by the electric energy generated by the AC voltage or the DC voltage applied to the electrode and the metal ion generator The present invention provides a method for producing a conductive metal ion ink composition.
At this time, the kind and content of the conductive metal, the metal ion generating agent and the metal ion stabilizer are the same as those described in the description of the conductive metal ion ink composition according to one embodiment of the present invention.
In addition, the conductive metal ion ink composition prepared by controlling the applied AC voltage or DC voltage and controlling the electric energy may be applied with a conductive film to provide a conductive film having conductive metal of various components.
The method for producing the conductive metal ion ink composition according to one embodiment of the present invention will be described in more detail with reference to the
A solution in which the metal ion generator and the metal ion stabilizer are dissolved in water is fed into the
When the electric energy generated by the AC voltage or the DC voltage is applied to the electrode through the
At this time, the solution may be supplied to the
The conductive metal ion ink composition according to an embodiment of the present invention can easily form a thin film or a pattern through a coating or printing process using various substrates. For example, a thin film can be produced by coating on a substrate such as metal, glass, silicon wafer, ceramic, plastic film such as polyester or polyimide, rubber sheet, fiber, wood, Such a substrate may be used after being washed, degreased, or specifically pretreated. Examples of the pretreatment method include plasma, ion beam, corona, oxidation or reduction, heat, etching, ultraviolet (UV) ) Treatment. The thin film manufacturing and printing methods may be selected from the group consisting of spin coating, roll coating, spray coating, dip coating, flow coating, doctor blade, and dispensing such as printing, dispensing, inkjet printing, offset printing, screen printing, pad printing, gravure printing, flexography printing, stencil printing, imprinting, xerography, lithography, It is possible to select and use.
The pattern thus obtained may undergo an annealing process to improve the thin film characteristics such as conductivity and adhesion. In the case of the heat treatment, it may be carried out under a reducing atmosphere such as a mixed gas of hydrogen and nitrogen, an inert gas atmosphere of nitrogen gas and argon, or an air condition at a temperature of 400 DEG C or less, more specifically 140 to 300 DEG C. The conductive metal ion ink composition according to an embodiment of the present invention is advantageous in that it can be applied to a substrate made of glass or plastic having a thermally weak characteristic because the conductive metal ion ink composition according to the present invention can be heat-treated at the low temperature as described above.
The metal pattern forming method that can be used in the present invention may be used for replacing a sputter layer of a flexible display or a flat panel display, or may be used for a CMP-free damping processing (CMP- free damascene processing) and a PR-free ITO layer.
The conductive metal ion ink composition according to an embodiment of the present invention can provide a conductive metal ion ink composition that is uniform and stable even when baked at a low temperature using only a small amount of an additive. By using the conductive metal ion ink composition according to one embodiment of the present invention, it is possible to improve the electrical conductivity of printed fine wires and conductive films.
In addition, the method of producing a conductive metal ion ink composition according to another embodiment of the present invention is economical because it does not require expensive electrolytes and does not require any additional steps such as synthesis, filtration and washing of metal particles. As a result, it can be produced quickly by a simple method, and the process itself is environmentally friendly, economical and safe, and thus can be used in a wide range of industrial fields such as inkjet ink technology.
Hereinafter, specific embodiments of the present invention will be described. However, the embodiments described below are only intended to illustrate or explain the present invention, and thus the present invention should not be limited thereto.
In addition, contents not described here can be inferred sufficiently technically if they are skilled in the art, and a description thereof will be omitted.
Example 1
Aqueous solution of 40 mM citric acid and 30 ml of ammonia water (NH 3 [aq]) was added to 570 ml of pure water (DI-water) at room temperature. 600 ml of the above aqueous solution is fed into the
A general AC voltage of 110 V is applied to the
Comparative Example 1
An aqueous solution to which 40 mM of citric acid was added to 600 ml of pure water (DI-water) at room temperature was prepared, and the solution was supplied to the
According to the comparative example 1, it is confirmed that a large amount of copper hydroxide precipitates from the anode at the same time as the electrical energy is applied to the
Example 2
A copper hydroxide ink composition is prepared by dissolving a copper hydroxide powder, a metal ion generator and a metal ion stabilizer in an aqueous ammonia solution. In the copper ion ink composition, 20 g of copper hydroxide powder was added to 27 g of an aqueous ammonia solution, and 22 g of formic acid and 4 g of citric acid were added to completely dissolve the powder. This makes it possible to produce a copper ion ink composition at a concentration of about 17.8% by weight without using an evaporator.
Example 3
A copper ion ink composition was prepared in the same manner as in Example 2, except that 20 g of the copper hydroxide powder was added to 27 g of the aqueous ammonia solution, and 22 g of formic acid and 4 g of malic acid were added to completely dissolve the powder. A composition is prepared.
Example 4
A copper ion ink composition was prepared in the same manner as in Example 2 except that 18.4 g of 1-buthanethiol was used instead of 27 g of the aqueous ammonia solution as the copper ion ink composition.
The ink composition according to Examples 1 to 4 was pattern printed on a polyimide substrate by an inkjet method and fired at 140 占 폚 in an argon gas atmosphere to prepare a patterned conductive film. An electron micrograph of the conductive film according to Example 1 is shown in FIG. Referring to FIG. 2, it can be seen that the conductive film forms a uniform pattern having a line width of about 80 μm.
As a result of X-ray diffraction (XRD) analysis of the conductive film formed from the ink composition according to Example 1, it can be confirmed that pure copper metal free from oxides and impurities exists as shown in FIG. This is a characteristic that is well suited to the required characteristics of the ink for ink jet, and the copper ion ink composition thus prepared is likely to be suitably applied to the ink for ink jet.
As a result of X-ray diffraction (XRD) analysis of the conductive film formed from the ink composition according to Example 2, it can be confirmed that pure copper metal free from oxides and impurities exists as shown in FIG.
As a result of X-ray diffraction (XRD) analysis of the patterned conductive film formed from the ink composition according to Example 3, it can be confirmed that pure copper metal free from oxides and impurities exists as shown in FIG.
According to this embodiment, the ink composition prepared by a simple process can be uniformly and stably dispersed to provide a conductive film made of a pure metal, including a conductive metal or a conductive metal precursor, a metal ion generator, a metal ion stabilizer and a solvent .
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
1 is a schematic diagram of an apparatus for producing a conductive metal ion ink composition according to an embodiment of the present invention.
2 is an electron micrograph of the conductive film pattern prepared in Example 1. Fig.
FIG. 3 is a graph showing the X-ray diffraction analysis results of the conductive film pattern prepared in Example 1. FIG.
FIG. 4 is a graph showing the X-ray diffraction analysis results of the conductive film pattern prepared in Example 2. FIG.
FIG. 5 is a graph showing the X-ray diffraction analysis results of the conductive film pattern prepared in Example 3. FIG.
Description of the Related Art
1: Manufacturing device 2: Feeder
3: mixer 4: power supply
5: Thermometer 6: Temperature controller
8: Pump
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| CN103347965B (en) * | 2011-02-08 | 2016-01-13 | Lg化学株式会社 | Printing composition for ink and use the printing process of this composition for ink |
| KR101401571B1 (en) * | 2012-08-27 | 2014-06-05 | 한국과학기술연구원 | Conductive metal ion ink composition, method of preparing the same and prerparing method of highly conductive metal pattern or film using the same |
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| JP2003261798A (en) | 2002-03-07 | 2003-09-19 | Brother Ind Ltd | Ink jet recording water-based ink |
| KR100820038B1 (en) * | 2007-01-08 | 2008-04-07 | 한양대학교 산학협력단 | Fabrication of copper nano particle for metal ink on ink-jet technology |
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| WO2008018718A1 (en) * | 2006-08-07 | 2008-02-14 | Inktec Co., Ltd. | Process for preparation of silver nanoparticles, and the compositions of silver ink containing the same |
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| JP2003261798A (en) | 2002-03-07 | 2003-09-19 | Brother Ind Ltd | Ink jet recording water-based ink |
| KR100820038B1 (en) * | 2007-01-08 | 2008-04-07 | 한양대학교 산학협력단 | Fabrication of copper nano particle for metal ink on ink-jet technology |
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