CN102666745A - Conductive ink composition without forming particles and method for producing same - Google Patents
Conductive ink composition without forming particles and method for producing same Download PDFInfo
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- CN102666745A CN102666745A CN2010800531941A CN201080053194A CN102666745A CN 102666745 A CN102666745 A CN 102666745A CN 2010800531941 A CN2010800531941 A CN 2010800531941A CN 201080053194 A CN201080053194 A CN 201080053194A CN 102666745 A CN102666745 A CN 102666745A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
The present invention relates to a conductive ink composition which does not form particles and a method for producing the same, and more particularly, to a conductive ink composition which comprises a metal compound obtained by adding a mixture of a fatty acid having 10 to 22 carbon atoms and a fatty acid having 2 to 9 carbon atoms and ammonia to a metal precursor aqueous solution, an amine compound, and a solvent, and which can avoid aggregation of particles without forming particles, has a high metal content without adding additional nanoparticles, and can be used for various applications at heat treatment temperatures.
Description
Technical field
The present invention relates to not form particle and the conductive ink composition that under various temperature, can heat-treat and method of manufacture thereof.
Background technology
Use the nano ink of the metallics of nanometer size to have high conductivity, can carry out simple process and low-temperature heat treatment, therefore in multiple field, use.Particularly, receive more concern applicable to low resistive metal distribution, tellite (PCB), flexible circuit board (FPC), RFID tag (RFID Tag) with antenna, the metal wiring of flat panel displaying element (Flat Display Panel) and the nano ink of electrode.
Nanoparticle as the core material of nano ink utilizes several different methods such as drying process, damp process to make.In order to prevent the cohesion of nanoparticle, nano ink is used with the dispersion agent is main various additives, or when making nano ink via the other dispersion step of utilizing UW etc.However, the size of particle is more little, and the specific surface area of particle increases more, and the surfactivity of particle increases thus, and interparticle gravitation also increases, and therefore in fact can not prevent the cohesion of nanoparticle fully.
Under can not fully decentralized situation in nano ink, nanoparticle condenses and in nano ink, produces throw out, and because of the particle of growth can't be heat-treated at low temperatures, and specific conductivity also descends.
On the other hand, too much use under the situation of dispersion agent, also can produce the problem that specific conductivity descends and thermal treatment temp rises that causes by dispersion agent for the cohesion that prevents nanoparticle.Under the too much situation of dispersion step, also can in nano ink composition, produce unexpected side reaction, the performance of printing ink descends greatly, and can not become basic solution.
In order fundamentally to solve such problem, proposed not form the conductive ink of particle, such conductive ink utilizes ammonium carbamate or volatile salt to make typically.The major part of the metallic compound in the conductive ink of having developed at present is confined to silver metallized compound, because the ink stability of lower concentration is high, existing conductive ink mainly is made into the low low viscosity ink of viscosity own.But, when making, produce the problem of the stability decreases of printing ink with high density, therefore, in the operation that in fact requires high density, mix and use other nano silver particles.
Conductive ink is heat-treated under various temperature according to the purposes that is suitable for.For example, be applicable under the situation of RFID tag with the conductive ink of antenna, need under about about 150 ℃, heat-treating, under the situation of the metal wiring of flat panel displaying element, need heat-treat more than 350 ℃.At high temperature under the situation of thermal treatment low temperature with conductive ink, produce the coacervation of mf, on film surface, produce hole, perhaps produce Ling Qiu, uneven thereby the surface becomes, when forming electrode, even possibly break.In contrast, handle at low temperatures under the situation of high temperature with conductive ink, can not carry out thermal reduction, can't have electroconductibility, thereby can not be used as electrode.At present, known multiple low temperature is with conductive ink and method for making thereof, but very little with the exploitation of conductive ink and the conductive ink that can under various temperature, freely heat-treat to high temperature.
Summary of the invention
Technical problem
Therefore; The object of the present invention is to provide the cohesion that does not form particle and can avoid nanoparticle; The density of electrode is high when forming electrode, metal content is high but can not produce broken string and need not drop into other nanoparticle, and can be used in the conductive ink composition and the method for manufacture thereof of the purposes of multiple thermal treatment temp.
The means of dealing with problems
In order to achieve the above object; The present invention provides a kind of conductive ink composition, and it comprises carbonatoms is that lipid acid and the carbonatoms of 10-22 is that the mixture and the ammonia of the individual lipid acid of 2-9 adds metallic compound, amine compound and the solvent that obtains in the metal precursor aqueous solution to.
In addition, the present invention provides the method for manufacture of conductive ink composition, and it comprises: (1) is dissolved in metal precursor in the water and makes the step of the metal precursor aqueous solution; (2) be that lipid acid and the carbonatoms of 10-22 is that the mixture and the ammonia of the individual lipid acid of 2-9 adds the step that obtains metallic compound in the said metal precursor aqueous solution to carbonatoms; (3) with said metallic compound washing and exsiccant step; And (4) are dissolved in the step in the solvent with said dried metallic compound and amine compound.
The invention effect
Conductive ink composition of the present invention has following advantage: the first, owing to containing the lipid acid more than 2 kinds is mixed the metallic compound that obtains, thereby heat decomposition temperature is easy to adjust, and can be as the suitable conductive ink that is suitable for use; The second, be not limited in silver, can utilize multiple metallic element manufacturing not form the conductive ink of particle; The 3rd, owing to do not form particle, thereby do not need other dispersion step.
Embodiment
According to conductive ink composition of the present invention; It is characterized in that comprising carbonatoms is that lipid acid and the carbonatoms of 10-22 is that the mixture and the ammonia of the individual lipid acid of 2-9 adds metallic compound, amine compound and the solvent that obtains in the metal precursor aqueous solution to.
It is said metallic compound, amine compound and the solvent that benchmark is respectively 30～70 weight %, 20～50 weight % and 10～50 weight % that compsn of the present invention can preferably comprise in the composition total weight.
Conductive ink composition according to the present invention is made through following steps: (1) is dissolved in metal precursor the step of making the metal precursor aqueous solution in the water; (2) be that lipid acid and the carbonatoms of 10-22 is that the mixture and the ammonia of the individual lipid acid of 2-9 adds the step that obtains metallic compound in the said metal precursor aqueous solution to carbonatoms; (3) with said metallic compound washing and exsiccant step; And (4) are dissolved in the step in the solvent with said dried metallic compound and amine compound.
The metal of the metal precursor that can in above-mentioned steps (1), use is not special to be limited; But preferred the use is selected from the metal more than a kind in I family, IIA family, IIIA family, IVA family and the VIIIB families such as gold and silver, copper, aluminium, nickel, tin, palladium, platinum, zinc, iron, indium and magnesium, more preferably uses gold and silver, copper, aluminium, zinc, palladium, tin, nickel or their mixture.
Particularly; Above-mentioned metal can come suitably to mix to use as required; Can be in the above-mentioned metal of enumerating; As the principal constituent metal, and the metal except that selected principal constituent metal of selecting more than one uses principal constituent metal and ancillary component metal mixed as the ancillary component metal with a kind of metal.
At this moment, as the blending ratio of metal, with respect to 1 mole on principal constituent metal, the ancillary component metal can use with 0.001～0.5 mol ratio.If in above-mentioned scope, determine the blending ratio of metal, then can keep the characteristic of principal constituent metal, and come selectivity to give desirable function through the ancillary component metal.With respect to the principal constituent metal with situation less than 0.001 mixed in molar ratio ancillary component metal under, bring variation can not for the characteristic of principal constituent metal, and if surpass 0.5 mol ratio, then the ancillary component metal is too much, the natural characteristics of principal constituent metal disappears.For example, under the situation of silver,, has the problem of the electrode broken string that causes because of electromigration (electromigration) phenomenon though resistivity is low.At this moment, if in above-mentioned scope, use copper, then can prevent the electromigratory resistivity of keeping simultaneously.But, depart from above-mentioned scope and when not enough, can not prevent the electromigration of silver at the content of copper.On the contrary, if too much add copper, then because of copper forms sull, and resistivity sharply rises.
Be used as under the situation of ancillary component metal, the characteristic of each metal is following.
With regard to copper and palladium, they make the viscosity degradation of conductive ink, are suitable for the hydrophobicity substrate, and have electro migration resistance.When making conductive ink, be fit to use when desire reduces viscosity under the situation that does not change metal content, solvent etc., be used for suitable with the silver of electromigration difference, aluminium etc.Particularly, copper is low owing to its resistivity, thereby can be effective to the manufacturing of low resistance electrode.
With regard to aluminum and zinc, they rise the viscosity of conductive ink, are suitable for hydrophilic substrates.Therefore, when the viscosity that makes printing ink rises, be used for suitable.Form easily at the principal constituent metal under the situation of sull,, then generate electroconductive zinc oxide, and have the effect that the resistance that prevents to be caused by sull rises if add zinc.
With regard to tin, it is effective to improving with the bonding force of substrate, and is particularly, effective to improving with the bonding force of glass substrate.
With regard to nickel, the avidity of itself and Sauerstoffatom generates sull greatly and easily, if when needs generate the electroconductibility sull, add, can be more prone to generate the electroconductibility sull.
With regard to gold and silver, they rise viscosity, and resistivity is low.If the resistivity height at the principal constituent metal adds when perhaps electroconductibility is bad, the effect that reduces resistivity is arranged then.
So,, and add in the principal constituent metal, then can make the conductive ink that meets multiple condition and purpose if consider the characteristic of each metallic element when the ancillary component metal.
For above-mentioned metal precursor, as inorganic salt, can use nitrate salt, vitriol, acetate, phosphoric acid salt, silicate, hydrochloride etc., can use separately or use mixing more than 2 kinds.
Solvent as being used for the dissolution of metals precursor makes water, and this is because water is high for the solvency power of metal precursor, makes the separating of the metallic compound of separating out with fatty acid response, cleaning, drying become easy.
Spendable lipid acid is the unsaturated or sfas with carboxyl in the above-mentioned steps (2); Not special the qualification; As sfas; Propionic acid, butyric acid, isopropylformic acid, valeric acid, PIVALIC ACID CRUDE (25), enanthic acid, 2 ethyl hexanoic acid, caproic acid, capric acid, neodecanoic acid and LAURIC ACID 99 MIN can be enumerated,, undecylenic acid, oleic acid, Zoomeric acid, ricinoleate acid, Semen Myristicae oleic acid and erucic acid can be enumerated as unsaturated fatty acids.In the present invention; The carbonatoms that can be lipid acid and 0.2～9 molar equivalent of 10-22 with the carbonatoms of 1 molar equivalent is that 2-9 lipid acid mixes and uses, and carbonatoms is that 10-22 lipid acid and carbonatoms is 2-9 lipid acid selection more than a kind from the concrete example of above-mentioned saturated and unsaturated fatty acids respectively.
If to mix carbonatoms less than the amount of 0.2 molar equivalent is the individual lipid acid of 2-9, the metal content of the metallic compound that is then produced sharply reduces, and resistivity can rise to the degree that is difficult to as conductive ink.In addition, the thermolysis of metallic compound needs the high temperature more than 400 ℃, therefore, in fact, might be difficult to be applicable to conductive ink.In addition; If to mix carbonatoms greater than the amount of 9 molar equivalents is the individual lipid acid of 2-9; The advantage that resistivity decreased is then arranged, but the thermostability of the metallic compound that is produced reduces, and therefore makes under the situation of conductive ink with this metallic compound; Carry out reduction reaction in normal temperature, the problem that metallics is separated out takes place.
In above-mentioned scope, under the situation of mixed fatty acid, can suitably regulate the effect of heat decomposition temperature when having the stability of guaranteeing conductive ink as required.
Above-mentioned lipid acid is non-water soluble substance, thus not with step (1) in used water mix, formation is separated, and can't generate metallic compound.Therefore, in step (2), if use with ammonia, then lipid acid carries out amidation and might be dissolved in the aqueous solution, and pH in the regulator solution, promotes the generation of metallic compound.In the present invention, be benchmark in the lipid acid (fatty acid mixt) that is mixed with more than 2 kinds of 1 molar equivalent, ammonia can use 0.5～4 molar equivalent.
Under the situation of the ammonia that uses less than 0.5 molar equivalent, there is not amidated lipid acid in a large number, lipid acid is not dissolved in the aqueous solution, therefore produces and being separated of metal precursor solutions, and can't obtain the metal target compound smoothly.In addition, if use the ammonia that surpasses 4 molar equivalents, then can temporarily generate metallic compound; But along with reaction continues to carry out, the metallic element of metallic compound combines with ammonia, and remaining composition is reduced into lipid acid again; Generation is separated, and also can't obtain the metal target compound smoothly.
At this moment, be benchmark in the lipid acid that is mixed with more than 2 kinds of 1 molar equivalent, metal precursor can use 0.25～4 molar equivalent.
In step (3), utilize water or ethanol, after the metallic compound cleaning that generates in the above-mentioned steps (2) 2～3 times, drying obtains fine powdery metal compound thus.
Then, in step (4), above-mentioned exsiccant metallic compound is dissolved in the appropriate solvent with amine compound, thus the manufacturing objective conductive ink composition.In the composition total weight is benchmark, and above-mentioned metallic compound, amine compound and solvent can use 30～70 weight %, 20～50 weight % and 10～50 weight % respectively.At this moment, except above-mentioned metallic compound with the amine compound, can be as required add in the solvent additive usually used in this field is extra.
Used solvent must be can divide easily to spread or the dissolution of metals compound, regulate the viscosity of conductive ink and successfully film forming solvent easily in the step (4).As such solvent, can water, alcohols, glycols and organic solvent be used separately or use mixing more than 2 kinds, and be mixed together use with amine compound.The amine compound performance promotes the dissolved effect of above-mentioned metallic compound.
As alcohols, can use methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, 2-butanols, octanol, 2-Ethylhexyl Alcohol, amylalcohol, benzylalcohol, hexanol, 2-hexanol, hexalin, Terpineol 350, nonyl alcohol etc.
As glycols, can use methylene glycol, terepthaloyl moietie, butyleneglycol, Diethylene Glycol, triethylene glycol, TEG etc.
As organic solvent, can use toluene, YLENE, methylcarbonate, diethyl carbonate, 1-Methoxy-2-propyl acetate, ethyl lactate, 2-methoxy ethyl acetic ester, propylene glycol monomethyl ether, N-N-methyl-2-2-pyrrolidone N-, N-methylacetamide etc.
As amine compound; Can use quadrol, tn, tetramethylenediamine, 1; 3-tn, 1; 4-tetramethylenediamine, 1; 3-diaminobutane, 2; 3-diaminobutane, 1; 5-pentamethylene diamine, 2; 4-diamino-pentane, trimethylammonium quadrol, N-ethylethylenediamine, triethyl quadrol, NSC 446, Triethylenetetramine (TETA), tetren, N-Mono Methyl Ethanol Amine, N-ehtylethanolamine, N-propyl group thanomin, N-butylethanolamine, diethylolamine, trolamine, N methyldiethanol amine, N-ethyldiethanolamine, Yi Bingchunan, HSDB 338, tri-isopropanolamine, N-methyl isopropyl hydramine, N-ethyl Yi Bingchunan, N-propyl group Yi Bingchunan, 2-amino-1-propyl alcohol, N-methyl-2-amino-1-propyl alcohol, N-ethyl-2-amino-1-propyl alcohol, 1-amino-3-propyl alcohol, N-methyl isophthalic acid-amino-3-propyl alcohol, N-ethyl-1-amino-3-propyl alcohol, 1-amino-2-butanols, N-methyl isophthalic acid-amino-2-butanols, N-ethyl-1-amino-2-butanols, 2-amino-1-butanols, N-methyl-2-amino-1-butanols, N-ethyl-2-amino-1-butanols, 3-amino-1-butanols, N-methyl-3-amino-1-butanols, N-ethyl-3-amino-1-butanols, 1-amino-4-butanols, N-methyl isophthalic acid-amino-4-butanols, N-ethyl-1-amino-4-butanols, 1-amino-2-methyl-2-propyl alcohol, 2-amino-2-methyl-1-propanol, 1-amino-4-amylalcohol, 2-amino-4-methyl-1-pentene alcohol, 2-is amino-1-hexanol, 3-amino-4-enanthol, 1-amino-sec-n-octyl alcohol, 5-amino-4-octanol, 1-amino-2; Ammediol, 2-amino-1; Ammediol, three (methylol) aminomethane, 1; 2-diamino--3-propyl alcohol, 1,3-diamino--2-propyl alcohol, 2-(2-amino ethoxy) ethanol and their mixture.
The conductive ink composition of so making of the present invention does not form particle and can avoid the cohesion of particle, and metal content is high and need not drop into other nanoparticle, and can be used in the purposes of multiple thermal treatment temp.
Below, in order to help understand the present invention, enumerate preferred embodiment, but the following embodiment the present invention that has been illustration, scope of the present invention is not limited to following embodiment.
[embodiment]
Embodiment 1
Silver Nitrate 34.0g is dissolved among the water 0.5L and obtains silver nitrate aqueous solution.Oleic acid 28.2g, caproic acid 11.6g and 29 weight % ammonia soln 41.0g are mixed and stirred 30 minutes, add to then in the silver nitrate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate white powder, the white powder that is generated is cleaned 2-3 time with ultrapure water after, with the mixed solution cleaning of ultrapure water and methyl alcohol 1 time.In 40 ℃ of drying machines,, obtain the metal compound powders of 60.0g with the powder for drying after cleaning 8 hours.In the powder 30g of above-mentioned gained, add ethanol 12.0g and quadrol 10.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 350 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 5.6 μ Ω .cm.
Embodiment 2
Oleic acid and caproic acid are used 18.8g respectively, and caproic acid uses 15.5g, obtain metallic compound 54.6g, in addition, carry out the method identical, obtain conductive ink with embodiment 1.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 280 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.8 μ Ω .cm.
Embodiment 3
Silver Nitrate 34.0g is dissolved among the water 0.5L and obtains silver nitrate aqueous solution.Oleic acid 11.3g, caproic acid 9.3g, butyric acid 7.0g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the silver nitrate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate white powder, the white powder that is generated is cleaned 2-3 time with ultrapure water after, with the mixed solution cleaning of ultrapure water and methyl alcohol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 47.8g.In the powder 30g of above-mentioned gained, add ethanol 12.0g and quadrol 10.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 250 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.5 μ Ω .cm.
Embodiment 4
Oleic acid, caproic acid and butyric acid are used 8.1g, 6.6g and 10.1g respectively, obtain metallic compound 45.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 3.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.1 μ Ω .cm.
Embodiment 5
Silver Nitrate 33.7g is dissolved among the water 0.5L with cupric nitrate 479mg, obtains the metal precursor aqueous solution.Oleic acid 8.1g, caproic acid 6.6g, butyric acid 10.1g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the metal precursor aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with the mixed solution cleaning of ultrapure water and methyl alcohol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 45.0g.In the powder 30g of above-mentioned gained, add ethanol 12.0g and quadrol 10.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.3 μ Ω .cm.
Embodiment 6
Silver Nitrate, cupric nitrate, aluminum nitrate are used 33.3g, 475mg, 735mg respectively, obtain metallic compound 44.3g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 5.1 μ Ω .cm.
Embodiment 7
Silver Nitrate, cupric nitrate, Palladous nitrate are used 33.5g, 477mg, 270mg respectively, obtain metallic compound 45.3g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 5.3 μ Ω .cm.
Embodiment 8
Silver Nitrate, cupric nitrate, zinc acetate are used 33.3g, 474mg, 431mg respectively, obtain metallic compound 45.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 5.1 μ Ω .cm.
Embodiment 9
Silver Nitrate, aluminum nitrate are used 33.7g, 743mg respectively, obtain metallic compound 44.8g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 5.4 μ Ω .cm.
Embodiment 10
Silver Nitrate, aluminum nitrate, Palladous nitrate are used 33.5g, 739mg, 270mg respectively, obtain metallic compound 44.9g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 6.3 μ Ω .cm.
Embodiment 11
Silver Nitrate, Palladous nitrate are used 33.9g, 109mg respectively, obtain metallic compound 44.9g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.8 μ Ω .cm.
Embodiment 12
Silver Nitrate, zinc acetate are used 24.3g, 12.6g respectively, obtain metallic compound 42.3g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.5 μ Ω .cm.
Embodiment 13
Silver Nitrate, zinc acetate, nickelous nitrate are used 28.3g, 7.3g, 36mg respectively, obtain metallic compound 43.5g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.9 μ Ω .cm.
Embodiment 14
Silver Nitrate, zinc acetate, gold trichloride are used 30.9g, 4.0g, 112mg respectively, obtain metallic compound 44.8g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.4 μ Ω .cm.
Embodiment 15
Silver Nitrate, Palladous nitrate, gold trichloride are used 33.9g, 109mg, 123mg respectively, obtain metallic compound 45.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 4.9 μ Ω .cm.
Embodiment 16
Silver Nitrate, cupric nitrate, tin chloride are used 33.6g, 479mg, 69mg respectively, obtain metallic compound 45.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 6.2 μ Ω .cm.
Embodiment 17
Silver Nitrate, cupric nitrate, aluminum nitrate, tin chloride are used 33.3g, 474mg, 735mg, 69mg respectively, obtain metallic compound 45.3g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 6.5 μ Ω .cm.
Embodiment 18
Silver Nitrate, cupric nitrate, Palladous nitrate, tin chloride are used 33.6g, 478mg, 108mg, 69mg respectively, obtain metallic compound 45.7g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 7.2 μ Ω .cm.
Embodiment 19
Silver Nitrate, zinc acetate, tin chloride are used 28.3g, 7.3g, 59mg respectively, obtain metallic compound 43.2g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 6.1 μ Ω .cm.
Embodiment 20
Silver Nitrate, zinc acetate, tin chloride, nickelous nitrate are used 28.3g, 7.3g, 59mg, 35mg respectively, obtain metallic compound 43.4g, in addition, carry out the method identical, obtain conductive ink with embodiment 5.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 6.6 μ Ω .cm.
Embodiment 21
Cupric nitrate 48.4g is dissolved among the water 0.5L, obtains copper nitrate aqueous solution.Neodecanoic acid 17.2g, 2 ethyl hexanoic acid 14.4g and 29 weight % ammonia soln 41.0g are mixed and stirred 30 minutes, add to then in the copper nitrate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate the cyan powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metallic compound of 43.8g.In the powder 30g of above-mentioned gained, add Virahol 10.0g and NSC 446 6.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 280 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 6.0 μ Ω .cm.
Embodiment 22
Neodecanoic acid and 2 ethyl hexanoic acid are used 11.5g and 19.2g respectively, obtain metallic compound 43.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 21.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 250 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 5.8 μ Ω .cm.
Embodiment 23
Cupric nitrate 48.4g is dissolved among the water 0.5L, obtains copper nitrate aqueous solution.Neodecanoic acid 6.9g, 2 ethyl hexanoic acid 11.5g, propionic acid 5.9g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the copper nitrate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate the cyan powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 36.3g.In the powder 30g of above-mentioned gained, add Virahol 10.0g and NSC 446 6.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 220 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 5.6 μ Ω .cm.
Embodiment 24
Neodecanoic acid, 2 ethyl hexanoic acid and propionic acid are used 4.9g, 8.2g and 8.5g respectively, obtain metallic compound 34.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 23.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 5.5 μ Ω .cm.
Embodiment 25
Cupric nitrate 32.3g is dissolved among the water 0.5L with Silver Nitrate 11.3g, obtains the metal precursor aqueous solution.Neodecanoic acid 4.9g, 2 ethyl hexanoic acid 8.2g, propionic acid 8.5g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the metal precursor aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 36.8g.In the powder 30g of above-mentioned gained, add Virahol 10.0g and NSC 446 6.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 4.4 μ Ω .cm.
Embodiment 26
Cupric nitrate, Silver Nitrate, Palladous nitrate are used 34.3g, 9.6g, 389mg respectively, obtain metallic compound 36.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 4.9 μ Ω .cm.
Embodiment 27
Cupric nitrate, Silver Nitrate, aluminum nitrate are used 32.3g, 4.5g, 15.0g respectively, obtain metallic compound 33.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 5.3 μ Ω .cm.
Embodiment 28
Cupric nitrate, Silver Nitrate, aluminum nitrate, Palladous nitrate are used 34.5g, 4.9g, 10.7g, 78mg respectively, obtain metallic compound 34.2g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 5.2 μ Ω .cm.
Embodiment 29
Cupric nitrate, Silver Nitrate, aluminum nitrate, zinc acetate are used 34.6g, 4.9g, 5.4g, 3.1g respectively, obtain metallic compound 34.4g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 4.9 μ Ω .cm.
Embodiment 30
Cupric nitrate, Silver Nitrate, Palladous nitrate, zinc acetate are used 37.2g, 5.2g, 42mg, 3.4g respectively, obtain metallic compound 35.1g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 5.1 μ Ω .cm.
Embodiment 31
Cupric nitrate, Silver Nitrate, zinc acetate, gold trichloride are used 37.2g, 2.6g, 6.8g, 63mg respectively, obtain metallic compound 34.2g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 4.8 μ Ω .cm.
Embodiment 32
Cupric nitrate, Silver Nitrate, gold trichloride, tin chloride are used 43.9g, 3.1g, 149mg, 64mg respectively, obtain metallic compound 33.8g, in addition, carry out the method identical, obtain conductive ink with embodiment 25.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃, thermal treatment 10 minutes under vacuum state, result, the resistivity of the printing ink of being measured were 6.3 μ Ω .cm.
Embodiment 33
Aluminum nitrate 75.0g is dissolved among the water 1L, obtains aluminum nitrate aqueous solution.LAURIC ACID 99 MIN 20.0g, valeric acid 10.2g and 29 weight % ammonia soln 41.0g are mixed and stirred 30 minutes, add to then in the aluminum nitrate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate white powder, the powder that is generated is cleaned 3-4 time with ultrapure water.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 34.0g.In the powder 30g of above-mentioned gained, add methylene glycol 10.0g and tn 10.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 380 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 10.4 μ Ω .cm.
Embodiment 34
LAURIC ACID 99 MIN and valeric acid are used 13.3g and 13.6g respectively, obtain metallic compound 32.0g, in addition, carry out the method identical, obtain conductive ink with embodiment 33.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 350 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 9.8 μ Ω .cm.
Embodiment 35
Aluminum nitrate 75.0g is dissolved among the water 1L, obtains aluminum nitrate aqueous solution.LAURIC ACID 99 MIN 8.0g, valeric acid 8.2g, isopropylformic acid 7.0g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the aluminum nitrate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate white powder, the powder that is generated is cleaned 3-4 time with ultrapure water.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 28.2g.In the powder 20g of above-mentioned gained, add methylene glycol 6.7g and tn 6.7g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 300 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 8.7 μ Ω .cm.
Embodiment 36
LAURIC ACID 99 MIN, valeric acid and isopropylformic acid are used 8.0g, 8.2g and 7.0g respectively, obtain metallic compound 26.5g, in addition, carry out the method identical, obtain conductive ink with embodiment 35.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 250 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 8.1 μ Ω .cm.
Embodiment 37
Gold trichloride 82.4g is dissolved among the water 1L, obtains the gold trichloride aqueous solution.Zoomeric acid 25.4g, enanthic acid 13.0g and 29 weight % ammonia soln 41.0g are mixed and stirred 30 minutes, add to then in the gold trichloride aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 75.6g.In the powder 30g of above-mentioned gained, add Virahol 25.0g and Triethylenetetramine (TETA) 15.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 300 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 7.8 μ Ω .cm.
Embodiment 38
Zoomeric acid and enanthic acid are used 16.9g and 17.3g respectively, obtain metallic compound 71.5g, in addition, carry out the method identical, obtain conductive ink with embodiment 37.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 250 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 7.1 μ Ω .cm.
Embodiment 39
Gold trichloride 82.4g is dissolved among the water 1L, obtains the gold trichloride aqueous solution.Zoomeric acid 10.2g, enanthic acid 10.4g, propionic acid 5.9g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the gold trichloride aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 65.1g.In the powder 30g of above-mentioned gained, add Virahol 25.0g and Triethylenetetramine (TETA) 15.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 6.7 μ Ω .cm.
Embodiment 40
Zoomeric acid, enanthic acid and propionic acid are used 7.3g, 7.4g and 8.5g respectively, obtain metallic compound 62.3g, in addition, carry out the method identical, obtain conductive ink with embodiment 39.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 180 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 5.9 μ Ω .cm.
Embodiment 41
Palladous nitrate 54.8g is dissolved among the water 1L, obtains palladium nitrate aqueous solution.Semen Myristicae oleic acid 22.6g, PIVALIC ACID CRUDE (25) 10.2g and 29 weight % ammonia soln 41.0g are mixed and stirred 30 minutes, add to then in the palladium nitrate aqueous solution, 40 ℃ of reactions 1 hour down; At this moment; Generate brown powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 52.7g.In the powder 30g of above-mentioned gained, add Terpineol 350 20.0g and N-propyl group Yi Bingchunan 15.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 380 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 20.9 μ Ω .cm.
Embodiment 42
Semen Myristicae oleic acid and PIVALIC ACID CRUDE (25) are used 15.1g and 17.3g respectively, obtain metallic compound 48.8g, in addition, carry out the method identical, obtain conductive ink with embodiment 41.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 350 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 19.2 μ Ω .cm.
Embodiment 43
Palladous nitrate 54.8g is dissolved among the water 1L, obtains palladium nitrate aqueous solution.Semen Myristicae oleic acid 9.0g, PIVALIC ACID CRUDE (25) 10.4g, isopropylformic acid 7.0g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes; Add in the palladium nitrate aqueous solution then; Reacted 1 hour down at 40 ℃, at this moment, generate brown powder; After the powder that is generated cleaned 2-3 time with ultrapure water, with washed with methanol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 44.8g.In the powder 30g of above-mentioned gained, add Terpineol 350 20.0g and N-propyl group Yi Bingchunan 15.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 300 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 19.1 μ Ω .cm.
Embodiment 44
Semen Myristicae oleic acid, PIVALIC ACID CRUDE (25) and isopropylformic acid are used 6.5g, 7.4g and 10.1g respectively, obtain metallic compound 43.2g, in addition, carry out the method identical, obtain conductive ink with embodiment 43.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 250 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 18.3 μ Ω .cm.
Embodiment 45
Zinc acetate 44.0g is dissolved among the water 0.5L, obtains zinc acetate aqueous solution.Erucic acid 33.9g, butyric acid 8.8g and 29 weight % ammonia soln 41.0g are mixed and stirred 30 minutes, add to then in the zinc acetate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate white powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with the mixing solutions cleaning of ultrapure water and methyl alcohol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 53.7g.In the powder 30g of above-mentioned gained, add methylcarbonate 10.0g and diethylolamine 10.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 350 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 16.0 μ Ω .cm.
Embodiment 46
Erucic acid and butyric acid are used 22.6g and 11.7g respectively, obtain metallic compound 46.8g, in addition, carry out the method identical, obtain conductive ink with embodiment 45.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 300 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 15.2 μ Ω .cm.
Embodiment 47
Zinc acetate 44.0g is dissolved among the water 0.5L, obtains zinc acetate aqueous solution.Erucic acid 13.6g, butyric acid 7.0g, propionic acid 5.9g and 29 weight % ammonia soln 17.6g are mixed and stirred 30 minutes, add to then in the zinc acetate aqueous solution, in normal-temperature reaction 1 hour.At this moment, generate white powder, the powder that is generated is cleaned 2-3 time with ultrapure water after, with the mixing solutions cleaning of ultrapure water and methyl alcohol 1 time.With the powder after cleaning in 40 ℃ of drying machines dry 8 hours, obtain the metal compound powders of 38.6g.In the powder 30g of above-mentioned gained, add methylcarbonate 10.0g and diethylolamine 10.0g, stirred 2 hours, obtain conductive ink.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 250 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 14.3 μ Ω .cm.
Embodiment 48
Erucic acid, butyric acid and propionic acid are used 9.7g, 5.0g and 8.5g respectively, obtain metallic compound 35.8g, in addition, carry out the method identical, obtain conductive ink with embodiment 47.
After the conductive ink of above-mentioned manufacturing was coated on glass substrate, 200 ℃ of following thermal treatments 10 minutes, result, the resistivity of the printing ink of being measured were 13.8 μ Ω .cm.
Industrial applicibility
Conductive ink composition of the present invention has following advantage: the first, owing to containing the lipid acid more than 2 kinds is mixed the metallic compound that obtains, thereby heat decomposition temperature is easy to adjust, and can be as the suitable conductive ink that is suitable for use; The second, be not limited in silver, can utilize multiple metallic element manufacturing not form the conductive ink of particle; The 3rd, owing to do not form particle, thereby do not need other dispersion step.
Claims (13)
1. conductive ink composition; It is characterized in that comprising carbonatoms is that lipid acid and the carbonatoms of 10-22 is that the mixture and the ammonia of the individual lipid acid of 2-9 adds metallic compound, amine compound and the solvent that obtains in the metal precursor aqueous solution to.
2. conductive ink composition according to claim 1 is characterized in that, is benchmark in the composition total weight, and said metallic compound, amine compound and solvent contain 30～70 weight %, 20～50 weight % and 10～50 weight % respectively.
3. conductive ink composition according to claim 1 is characterized in that, said fatty acid mixt is that the carbonatoms by 1 molar equivalent is that the carbonatoms of 10-22 lipid acid and 0.2～9 molar equivalent is that 2-9 lipid acid mixes.
4. conductive ink composition according to claim 1 is characterized in that, said lipid acid is the unsaturated or sfas with carboxyl.
5. conductive ink composition according to claim 4; It is characterized in that said lipid acid is selected from the group of being made up of propionic acid, butyric acid, isopropylformic acid, valeric acid, PIVALIC ACID CRUDE (25), enanthic acid, 2 ethyl hexanoic acid, caproic acid, capric acid, neodecanoic acid, LAURIC ACID 99 MIN, undecylenic acid, oleic acid, Zoomeric acid, ricinoleate acid, Semen Myristicae oleic acid, erucic acid and their mixture.
6. conductive ink composition according to claim 1 is characterized in that, is benchmark in the fatty acid mixt of 1 molar equivalent, and said ammonia uses 0.5～4 molar equivalent.
7. conductive ink composition according to claim 1 is characterized in that, said metal precursor comprises the metal more than a kind that is selected from the group of being made up of gold and silver, copper, aluminium, nickel, tin, palladium, platinum, zinc, iron, indium and magnesium.
8. conductive ink composition according to claim 7 is characterized in that, said metal is the mixture of a kind of principal constituent metal and the ancillary component metal except that said principal constituent metal more than a kind.
9. conductive ink composition according to claim 8 is characterized in that, with respect to 1 mole of said principal constituent metal, said ancillary component metal uses 0.001～0.5 mol ratio.
10. conductive ink composition according to claim 1 is characterized in that, is benchmark in the fatty acid mixt of 1 molar equivalent, and said metal precursor uses 0.25～4 molar equivalent.
11. conductive ink composition according to claim 1 is characterized in that, said solvent is water, alcohols, glycols, organic solvent or their mixture.
12. conductive ink composition according to claim 1; It is characterized in that; Said amine compound is selected from by quadrol, tn, tetramethylenediamine, 1; 3-tn, 1; 4-tetramethylenediamine, 1; 3-diaminobutane, 2; 3-diaminobutane, 1; 5-pentamethylene diamine, 2; 4-diamino-pentane, trimethylammonium quadrol, N-ethylethylenediamine, triethyl quadrol, NSC 446, Triethylenetetramine (TETA), tetren, N-Mono Methyl Ethanol Amine, N-ehtylethanolamine, N-propyl group thanomin, N-butylethanolamine, diethylolamine, trolamine, N methyldiethanol amine, N-ethyldiethanolamine, Yi Bingchunan, HSDB 338, tri-isopropanolamine, N-methyl isopropyl hydramine, N-ethyl Yi Bingchunan, N-propyl group Yi Bingchunan, 2-amino-1-propyl alcohol, N-methyl-2-amino-1-propyl alcohol, N-ethyl-2-amino-1-propyl alcohol, 1-amino-3-propyl alcohol, N-methyl isophthalic acid-amino-3-propyl alcohol, N-ethyl-1-amino-3-propyl alcohol, 1-amino-2-butanols, N-methyl isophthalic acid-amino-2-butanols, N-ethyl-1-amino-2-butanols, 2-amino-1-butanols, N-methyl-2-amino-1-butanols, N-ethyl-2-amino-1-butanols, 3-amino-1-butanols, N-methyl-3-amino-1-butanols, N-ethyl-3-amino-1-butanols, 1-amino-4-butanols, N-methyl isophthalic acid-amino-4-butanols, N-ethyl-1-amino-4-butanols, 1-amino-2-methyl-2-propyl alcohol, 2-amino-2-methyl-1-propanol, 1-amino-4-amylalcohol, 2-amino-4-methyl-1-pentene alcohol, 2-is amino-1-hexanol, 3-amino-4-enanthol, 1-amino-sec-n-octyl alcohol, 5-amino-4-octanol, 1-amino-2; Ammediol, 2-amino-1; Ammediol, three (methylol) aminomethane, 1; 2-diamino--3-propyl alcohol, 1, the group that 3-diamino--2-propyl alcohol, 2-(2-amino ethoxy) ethanol and their mixture are formed.
13. the method for manufacture of each described conductive ink composition in the claim 1～12, it comprises: (1) is dissolved in metal precursor in the water and makes the step of the metal precursor aqueous solution; (2) be that lipid acid and the carbonatoms of 10-22 is that the mixture and the ammonia of the individual lipid acid of 2-9 adds the step that obtains metallic compound in the said metal precursor aqueous solution to carbonatoms; (3) with said metallic compound washing and exsiccant step; And (4) are dissolved in the step in the solvent with said dried metallic compound and amine compound.
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| KR1020090115054A KR101681046B1 (en) | 2009-11-26 | 2009-11-26 | Conductive ink composition which does not form a particle and preparation thereof |
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| PCT/KR2010/008234 WO2011065709A2 (en) | 2009-11-26 | 2010-11-22 | Conductive ink composition that does not form particles, and method for manufacturing same |
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| EP2795627B1 (en) * | 2011-12-23 | 2019-03-13 | The Board of Trustees of the University of Illionis | Ink composition for making a conductive silver structure |
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| US9982154B2 (en) | 2014-04-17 | 2018-05-29 | Electroninks Incorporated | Solid ink composition |
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| CN105339446A (en) * | 2013-07-01 | 2016-02-17 | 汉高知识产权控股有限责任公司 | Nanoparticle ink compositions, process and applications |
| CN107533879A (en) * | 2015-06-12 | 2018-01-02 | 日油株式会社 | Cover copper filler material, its preparation method and conductive composition in surface |
| CN107533879B (en) * | 2015-06-12 | 2019-04-19 | 日油株式会社 | Cover copper filler material, preparation method and conductive composition in surface |
| CN107614164A (en) * | 2015-06-15 | 2018-01-19 | 株式会社大阪曹达 | Metallic nano-particle manufacture composition |
| CN104946022A (en) * | 2015-07-10 | 2015-09-30 | 东北大学 | High-stability particle free type silver-based conductive ink and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102666745B (en) | 2015-03-25 |
| WO2011065709A2 (en) | 2011-06-03 |
| TW201129646A (en) | 2011-09-01 |
| TWI509032B (en) | 2015-11-21 |
| KR20110058307A (en) | 2011-06-01 |
| KR101681046B1 (en) | 2016-11-30 |
| WO2011065709A3 (en) | 2011-11-10 |
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