CN102321402A - Agranular transparent conductive ink and its preparation method - Google Patents
Agranular transparent conductive ink and its preparation method Download PDFInfo
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Abstract
The invention discloses an agranular transparent conductive ink which can sinter at low temperature and has good stability, and a preparation method thereof. The conductive ink mainly consists of a solvent organic amine or ammonia water and an organic silver salt. During preparation, one of the solvent organic amine or ammonia water or more than one of other solvents are only needed to be mixed well, then an effective quantity of the organic silver salt is added, and after complete dissolution and dispersion, the conductive ink can be obtained. The conductive ink can form a pattern or a wet film by means of printing or coating, wherein, the organic silver part can be reduced to silver particles in the following heat treatment process so as to form a conductive pattern or conductive film. The conductive ink obtained through the method of the invention can has high stability without adding an extra protective agent. The preparation method put forward in the method has the advantages of simple process, mild reaction condition, short reaction time and low preparation cost.
Description
Technical field
The present invention relates to the conductive ink technical field, specifically a kind of high stability that contains solvent organic amine or ammoniacal liquor and organic salt, low temperature sintering agranular type electrically conducting transparent ink and preparation method thereof.
Background technology
Conductive ink can be applied in the aspects such as intelligent wireless identification (RFID) electronic tag, printed substrate (PCB), flexible printed circuit board (FPCB), electromagnetic shielding material, solar-energy photo-voltaic cell and show electrode of high speed development.With respect to traditional thin film electronic complete processing, use conductive ink to print, can stop waste of material, simplify manufacturing procedure, both improved economic benefit, reduced production cost, also reduced the environmental pollution in the manufacturing processed.
Conductive ink in the existing research is divided into two types substantially: one type is the granule type conductive ink; One type is the agranular type conductive ink.The granule type conductive ink mainly is made up of conductive particle, solvent, dispersion stabilizer, tensio-active agent and other auxiliary agents, its essence is the dispersion system of conductive particle.Common conductive particle has graphite, metal etc., and graphitic conductive is relatively poor, generally is not used in to make low-resistance electro-conductive material, so uses more in the conductive ink to be the metallic conduction particle, mainly to comprise gold and silver, copper, platinum etc.Wherein, owing to costing an arm and a leg of gold and platinum, its application in industry is subject to many limitations; Though and copper all takes advantage on electroconductibility and cost, its chemical property is comparatively active, is easy to oxidizedly, and its application in industry has certain limitation equally; Therefore, comprehensive many factor is considered, the argent good conductivity, and unreactiveness is stronger, is difficult for oxidizedly, and it receives much concern in the research of conductive ink.For the granule type conductive ink, the factor that influences its sintering temperature mainly is the height of various auxiliary agents decomposition and evaporable complexity and metallic particles fusing point.The fusing point of metal reduces and reduces with its particle diameter, and when reaching nano level, because small-size effect, its fusing point can sharply descend.For argent, according to relevant bibliographical information, when its particle diameter is reduced to 50nm when following, fusing point just can be lower than 200 ℃.
The agranular type conductive ink mainly is made up of precursor compound, solvent, tensio-active agent and other auxiliary agents of conducting polymer or conducting metal, and essence is the solution of conducting polymer or conducting metal precursor compound.Compare with the granule type conductive ink; There is not the agglomeration traits of conductive particle in the agranular type conductive ink, therefore need not to add dispersion stabilizer, can realize advantages of higher stability; And do dispersion agent owing to need not add the high molecular polymer that is difficult to decompose and vapors away; In the mf that in the end forms, residual non-conducting portion is less than the metallic membrane that the granule type conductive ink forms far away, thereby helps obtaining the lower conductive film of resistance.And from the demand to high conductivity pattern and conductive film, the relatively poor application of polymer in this field of electroconductibility receives certain restriction, and the conducting metal precursor compound then enjoys favor.In principle, the agranular type conductive ink mainly utilizes metallic compound at high temperature to decompose or is reduced into metal simple-substance and forms conducting film, so the character of metal precursor is one of principal element that influences its pyrochemistry behavior.
Conductive ink is printed onto after the printed substrate, needs through certain processing, and the wet film of non-conductive or poorly conductive is converted into the satisfactory dry film of electroconductibility.Mainly be to handle through heat-agglomerating to obtain at present.In general, sintering temperature is high more, and the electroconductibility of dry film is good more, but high temperature sintering is comparatively harsh for the requirement of printed substrate, and qualitative variation at high temperature takes place some base material easily, influences its use.Therefore, exploitation is sintering and obtain the conductive ink of the low dry film of resistance at a lower temperature, widens the scope of conductive ink applicable base materials, not only the conductive ink industry itself is had significance, and can promote the development of each relevant with it industry.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of low temperature sintering conductive ink is provided, the preparation method is simple; Raw material is easy to get, and sintering temperature is low, the time is short, and stability is high; Be easy to deposit, and can be applied to multiple mode of printing and coating method, the printed substrate limitation is little.
Technical purpose of the present invention is achieved through following technical proposals:
A kind of low temperature sintering agranular type electrically conducting transparent ink is made up of solvent organic amine or ammoniacal liquor and organic salt, and wherein, solvent organic amine or ammoniacal liquor provide solvent environment, and organic salt provides conductive component.
Solvent organic amine of the present invention is the substituted one-level aliphatic amide of alkyl, secondary aliphatic amine or acid amides; Like methylamine, ethamine, propylamine, butylamine, hexylamine, stearylamine, quadrol, 1,5-dimethylhexylamine, 1,6-hexanediamine, 1; 2-tn, 1; 3-tn, 1, the substituted one-level aliphatic amides of alkyl such as 4-tetramethylenediamine, 1, triethylenediamine, vulkacit H; The substituted secondary aliphatic amines of alkyl such as n n dimetylaniline, dipropyl amine, Diisopropylamine, diisobutylamine, distearyl amine; Methane amide, ethanamide, propionic acid amide, yulocrotine, acrylic amide, hexanolactam, N, acid amides such as dinethylformamide, DMAC N,N.
It is of the present invention that the organic salt of conductive component can be provided is the silver aliphatic carboxylate that contains 1～22 carbon atom with 1～3 carboxyl; Like Silver monoacetate, silver citrate, silver tartrate, vinylformic acid silver, trifluoroacetic acid is silver-colored, ROHM is silver-colored, Succinic Acid is silver-colored, valeric acid is silver-colored, caproic acid is silver-colored, oleic acid is silver-colored, oxysuccinic acid is silver-colored, mountain Yu acid silver, silver stearate etc.; Silver content is the 1wt%～40wt% of whole ink massfractions in the conductive ink; Preferred 5wt%～40wt% is more preferably 20wt%～40wt%.
Organic salt of the present invention can prepare through following non-limiting method: organic acid and aqueous sodium hydroxide solution reaction that earlier will be corresponding with organic acid silver; Adding silver nitrate aqueous solution again mixes; 20 ℃ are stirred 1h, suction filtration, and de-ionized washing, ethanol are washed; The normal temperature lucifuge is dry, promptly gets said organic acid silver.
Preparing method of the present invention, earlier with solvent organic amine or ammoniacal liquor with one or more other solvent even after, add the organic salt of significant quantity again, treat can make conductive ink after it dissolves dispersion fully.Organic salt can release of heat in dissolution process, for reducing the unstable that organic salt decomposes or reduction in this process bring, is preferably under room temperature or the lower temperature and carries out, and is preferably 5 ℃～25 ℃.
Among the present invention, can be through adding viscosity and surface tension a kind of or that more than one other material is regulated ink, to adapt to concrete request for utilization.Described material can be non-polar organic solvents such as water or the Fatty Alcohol(C12-C14 and C12-C18) that contains 1～12 carbon atom with 1～3 hydroxy functional group, sulfoxide class isopolarity organic solvent or hydro carbons, ethers, ester class; Its add-on is the 0.01wt%～90wt% of whole ink massfractions, preferred 5wt%～40wt%.Can add one or more tensio-active agent according to the affinity of ink and printed substrate and wettability, its add-on is the 0.01wt%～5wt% of whole ink massfractions, preferred 0.05wt%～3wt%; Also can according in the use to conducting film and printed substrate close-burning requirement add one or more tackiness agent, its add-on is the 0.1wt%～10wt% of whole ink massfractions, preferred 1wt%～6wt%.
Tensio-active agent of the present invention is made up of in AS, cats product or the amphoterics one or more; Said tackiness agent is made up of in polyvinyl butyral acetal, PVP K120, ROHM, ZX-I, Walocel MT 20.000PV, Z 150PH, gum arabic, peach gum, PVA, the XG 550 etc. one or more.
Conductive ink prepared according to the methods of the invention is the electrically conducting transparent ink, and is colourless or have very shallow color, and do not have any particle, therefore can blockage phenomenon, can better be applicable to multiple mode of printing, especially spray ink Printing.
Conductive ink prepared according to the methods of the invention has superior stability, and room temperature (25 ℃) is preserved and do not occurred deposition in 1 month, and refrigerator cold-storage can be preserved and not occur any variation in 6 months.
The viscosity of conductive ink prepared according to the methods of the invention can be adjusted in the scope of broad, according to preparation method and concrete use and change, is preferably 1cP～1500cP.The ink that viscosity is lower is fit to ink jet printing; The higher ink of viscosity then can be applied to multiple mode of printings such as intaglio printing, silk screen printing.
Conductive ink prepared according to the methods of the invention, sintering temperature is minimum can be preferably 100 ℃～150 ℃ to 80 ℃.Therefore the range of choice broad of its printed substrate can be resin, glass, pottery, paper, silicon etc.
Conductive ink according to the invention can obtain the conducting film of electroconductibility and cohesiveness excellence again through such as coating method such as the coating of silk rod, scraper coating, rotary coating, spraying, roller coat, dip-coating, flow coat or such as mode of printing film forming on multiple base material such as ink jet printing, silk screen printing, intaglio printing, letterpress, lithographys through processing such as heat-agglomeratings.
Conductive ink prepared according to the methods of the invention can be applied in a plurality of fields such as intelligent wireless identification (RFID) electronic tag, printed substrate (PCB), flexible printed circuit board (FPCB), electromagnetic shielding material, solar-energy photo-voltaic cell and show electrode of high speed development.
Compare with existing conductive ink and preparation method thereof, the present invention has following outstanding feature:
1, is applicable to the multiple mode of printing that comprises ink jet printing;
2, sintering temperature is low, the time is short, and printed substrate is extensive;
3, preparation cost is low, and process is simple, and required starting material conveniently are easy to get;
4, transparent, the no particle of ink proterties, stability is high.
Description of drawings
Fig. 1 is the XRD figure spectrum of the Silver monoacetate for preparing among the present invention.
Fig. 2 is the TG/DSC curve of the silver citrate for preparing among the present invention.
Fig. 3 is the SEM picture of ink behind the ink jet printing sintering in the embodiment of the invention 2.
Fig. 4 is that ink in the embodiment of the invention 1 is at the square resistance of 150 ℃ of following sintering different times.
Embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.The viscosity of ink when using U.S. Brookfield DV-II+Pro viscosity tester to record 25 ℃ uses Germany's
DSA-20 dynamic contact angle survey meter to record ink surface tension.The square resistance that uses GuangZhou, China four point probe science and technology RTS-9 four point probe tester to record.
Embodiment one
The 30g Trisodium Citrate is dissolved in the 100ml water, and the 52g Silver Nitrate is dissolved in the 150ml water, then; The silver nitrate aqueous solution of gained is slowly joined in the aqueous solution of Trisodium Citrate, and stirring at room was filtered after one hour; De-ionized washing 3 times; Ethanol is washed 1 time, places 30 ℃ darkroom to dry naturally, promptly gets the silver citrate white powder.
5ml methyl alcohol, 2ml 1,2-tn and 3ml Virahol mix, constant temperature to 5 ℃; Add the 2.0g silver citrate again; Stir down 1h at 5 ℃, after the filtering membrane of colourless, the clear solution that obtains through 0.45 μ m filtered, promptly get Hydrocerol A money base ink jet printing conductive ink.
The viscosity of ink is 5.27cP when using Brookfield DV-II+Pro viscosity tester to record 25 ℃, uses
It is 26mNm that DSA-20 dynamic contact angle survey meter records ink surface tension
-1, preserve under the room temperature and had only light discolouration in 1 month, and do not precipitate, preserve in the refrigerator and do not have any variation in 6 months.Use the piezoelectric ink jet printer prints after on the PET film, handle the regular hours for 150 ℃, the square resistance that uses RTS-9 four point probe tester to record is seen Figure of description 4.
Embodiment two
The preparation method of silver citrate among the preparation method of Silver monoacetate pressed powder such as the embodiment one.
The 4.0g Silver monoacetate is dissolved in the mixed solvent that 3ml ethanol, 4ml quadrol and 3ml terepthaloyl moietie forms, and 5 ℃ are stirred 1h down, obtain having a little yellow, transparent solution, and it through behind the filtering membrane of 0.45 μ m, is promptly got acetic acid money base conductive ink.The viscosity that records ink in the time of 25 ℃ is 30cP, and surface tension is 38mNm
-1, use the intaglio printing proof press to be printed on the EPSON printing paper, handle 10min for 130 ℃, it is 0.06 Ω/ that the four point probe resistance meter records square resistance, the SEM photo of gained conductive pattern is seen Figure of description 3.
Embodiment three
2ml propyl carbinol, 6ml quadrol and 2ml terepthaloyl moietie mix; Constant temperature to 5 ℃ adds the 17g silver citrate again, and constant temperature stirs 2h; The viscosity of gained ink is 1500cP; Use screen printer print on ceramic plate, handle 2min for 200 ℃, the square resistance of gained conductive pattern is 0.005 Ω/ (square resistance unit).
Embodiment four
The preparation method of silver citrate among the preparation method of Succinic Acid silver pressed powder such as the embodiment one.
4ml ethanol, 2ml diethylamine, 1ml methane amide and 3ml terepthaloyl moietie mix all and, constant temperature to 5 ℃, and adding 10g Succinic Acid is silver-colored; Constant temperature stirs 1h, treat that it dissolves fully after, add the 0.5g polyvinyl butyral acetal again; Continue to stir 0.5h, can make Succinic Acid silver base conductive ink, with it through behind the filtering membrane of 0.45 μ m; The viscosity of gained water white transparency conductive ink is 25cP, and surface tension is 39mNm
-1, use the excellent spreader of silk to be coated on the sheet glass, handle 15min for 90 ℃, the square resistance of gained conductive pattern is 0.7 Ω/ (square resistance unit).
Embodiment five
After the ammoniacal liquor of 2ml water, the 5ml trimethyl carbinol and 3ml 25% mixed, constant temperature to 15 ℃ added the 0.9g silver citrate; Constant temperature stirs 0.5h, treat that it dissolves fully after, add the 0.003g X 2073; Continue to stir 0.5h, can make Hydrocerol A money base conductive ink, with it through behind the filtering membrane of 0.45 μ m; The viscosity of gained water white transparency conductive ink is 1cP, and surface tension is 45mNm
-1, use the piezoelectric ink jet printer prints on ceramic plate, handle 10min for 160 ℃, the square resistance of gained conductive pattern is 45 Ω/ (square resistance unit).
Embodiment six
After 2ml ethylene glycol monobutyl ether, 3ml DMSO 99.8MIN. and 5ml octodrine mixed, constant temperature to 20 ℃ added the 0.16g Silver monoacetate; Constant temperature stirs 20min, can make acetic acid money base conductive ink, with it through behind the filtering membrane of 0.45 μ m; Recording its viscosity is 5cP, and surface tension is 32mNm
-1, use the mode of dip-coating to be coated on the PI film, handle 2min for 190 ℃, the square resistance of gained conductive pattern is 300 Ω/ (square resistance unit).
Embodiment seven
The preparation method of silver citrate among the preparation method of LAURIC ACID 99 MIN silver pressed powder such as the embodiment one.
After 2ml propyl carbinol, 6ml n-Butyl Amine 99 and 2ml USP Kosher mixed, constant temperature to 15 ℃ added 3g LAURIC ACID 99 MIN silver; Constant temperature stirs 0.5h, can make LAURIC ACID 99 MIN silver base conductive ink, with it through behind the filtering membrane of 0.45 μ m; Recording its viscosity is 18cP, and surface tension is 35mNm
-1, use the intaglio printing proof press to be printed on the PI film, handle 10min for 160 ℃, the square resistance of gained conductive pattern is 65 Ω/ (square resistance unit).
Embodiment eight
After 3ml water, 3ml terepthaloyl moietie and 4ml octodrine mixed, constant temperature to 20 ℃ added the 1.5g Silver monoacetate; Constant temperature stirs 20min, treat that it dissolves fully after, add the 0.6g PVP K120; Continue to stir 15min, can make acetic acid money base conductive ink, with it through behind the filtering membrane of 0.45 μ m; Recording its viscosity is 12cP, and surface tension is 37mNm
-1, use printing of inkjet printer on the PI film, handle 20min for 140 ℃, the square resistance of gained conductive pattern is 5.9 Ω/ (square resistance unit).
Embodiment nine
After 2ml methyl alcohol, 3ml terepthaloyl moietie and 5ml normal hexyl Amine mixed, constant temperature to 20 ℃ added 1.8g Succinic Acid silver; Constant temperature stirs 20min, can make Succinic Acid silver base conductive ink, with it through behind the filtering membrane of 0.45 μ m; The viscosity that records conductive ink is 7cP, and surface tension is 37mNm
-1, use printing of inkjet printer on platinum printing paper, handle 20min for 130 ℃, the square resistance of gained conductive pattern is 15.9 Ω/ (square resistance unit).
Embodiment ten
3ml water, 5ml isopropylcarbinol and 2ml 1, after the 3-tn mixes, constant temperature to 15 ℃; Add the 2.0g silver citrate, constant temperature stirs 20min, treat that it dissolves fully after; Add the 0.006g TX10, continue to stir 15min, can make Hydrocerol A money base conductive ink; Through behind the filtering membrane of 0.45 μ m, recording its viscosity is 6cP with it, and surface tension is 43mNm
-1, use printing of inkjet printer on the PI film, handle 15min for 140 ℃, the square resistance of gained conductive pattern is 6.9 Ω/ (square resistance unit).
More than the present invention has been done exemplary description; Should be noted that; Under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (10)
1. an agranular type electrically conducting transparent ink is characterized in that, is made up of solvent organic amine or ammoniacal liquor and organic salt, and wherein, solvent organic amine or ammoniacal liquor provide solvent environment, and organic salt provides conductive component
Described solvent organic amine is the substituted one-level aliphatic amide of alkyl, secondary aliphatic amine or acid amides; Like methylamine, ethamine, propylamine, butylamine, hexylamine, stearylamine, quadrol, 1,5-dimethylhexylamine, 1,6-hexanediamine, 1; 2-tn, 1; 3-tn, 1, the substituted one-level aliphatic amides of alkyl such as 4-tetramethylenediamine, 1, triethylenediamine, vulkacit H; The substituted secondary aliphatic amines of alkyl such as n n dimetylaniline, dipropyl amine, Diisopropylamine, diisobutylamine, distearyl amine; Methane amide, ethanamide, propionic acid amide, yulocrotine, acrylic amide, hexanolactam, N, acid amides such as dinethylformamide, DMAC N,N
It is described that the organic salt of conductive component can be provided is the silver aliphatic carboxylate that contains 1～22 carbon atom with 1～3 carboxyl; Like Silver monoacetate, silver citrate, silver tartrate, vinylformic acid silver, trifluoroacetic acid is silver-colored, ROHM is silver-colored, Succinic Acid is silver-colored, valeric acid is silver-colored, caproic acid is silver-colored, oleic acid is silver-colored, oxysuccinic acid is silver-colored, mountain Yu acid silver, silver stearate etc., silver content is the 1wt%～40wt% of whole ink massfractions in the conductive ink.
2. a kind of agranular type electrically conducting transparent ink according to claim 1 is characterized in that silver content is the 5wt%～40wt% of whole ink massfractions in the conductive ink.
3. a kind of agranular type electrically conducting transparent ink according to claim 1 is characterized in that silver content is the 20wt%～40wt% of whole ink massfractions in the conductive ink.
4. a kind of agranular type electrically conducting transparent ink according to claim 1; It is characterized in that; Through adding viscosity and surface tension a kind of or that more than one other material is regulated ink; To adapt to concrete request for utilization; Described other materials can be non-polar organic solvents such as water or the Fatty Alcohol(C12-C14 and C12-C18) that contains 1～12 carbon atom with 1～3 hydroxy functional group, sulfoxide class isopolarity organic solvent or hydro carbons, ethers, ester class, and its add-on is the 0.01wt%～90wt% of whole ink massfractions, preferred 5wt%～40wt%.
5. a kind of agranular type electrically conducting transparent ink according to claim 1; It is characterized in that; Add one or more tensio-active agent according to the affinity of ink and printed substrate and wettability; Its add-on is the 0.01wt%～5wt% of whole ink massfractions, and described tensio-active agent is made up of in AS, cats product or the amphoterics one or more, preferred 0.05wt%～3wt%.
6. a kind of agranular type electrically conducting transparent ink according to claim 1; It is characterized in that; According in the use to conducting film and printed substrate close-burning requirement add one or more tackiness agent; Its add-on is the 0.1wt%～10wt% of whole ink massfractions; Preferred 1wt%～6wt%, said tackiness agent is made up of in polyvinyl butyral acetal, PVP K120, ROHM, ZX-I, Walocel MT 20.000PV, Z 150PH, gum arabic, peach gum, PVA, the XG 550 etc. one or more.
7. one kind prepares the method for weighing 1 described a kind of agranular type electrically conducting transparent ink, it is characterized in that organic acid and aqueous sodium hydroxide solution reaction that earlier will be corresponding with organic acid silver; Adding silver nitrate aqueous solution again mixes; 20 ℃ are stirred 1h, suction filtration, and de-ionized washing, ethanol are washed; The normal temperature lucifuge is dry, promptly gets said organic acid silver;
Then with solvent organic amine or ammoniacal liquor and one or more other solvent evenly after, add the organic salt of significant quantity again, treat can make conductive ink after it dissolves dispersion fully.
8. preparation method according to claim 7 is characterized in that, for reducing the unstable that organic salt decomposes or reduction in this process bring, under room temperature or lower temperature, prepares, and is preferably 5 ℃～25 ℃.
9. the method for the right to use 1 a described a kind of agranular type electrically conducting transparent ink; It is characterized in that; Through such as coating method such as the coating of silk rod, scraper coating, rotary coating, spraying, roller coat, dip-coating, flow coat or such as mode of printing film forming on multiple base material such as ink jet printing, silk screen printing, intaglio printing, letterpress, lithographys; Obtain electroconductibility and the excellent conducting film of cohesiveness through processing such as heat-agglomeratings again; The range of choice broad of said printed substrate can be resin, glass, pottery, paper, silicon etc.
10. according to power 9 described method of use, it is characterized in that selecting viscosity in the use is the conductive ink of 1cP～1500cP, sintering temperature is minimum can be preferably 100 ℃～150 ℃ to 80 ℃.
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