CN104817891A - Write-through nano-silver conductive ink and preparation method thereof - Google Patents
Write-through nano-silver conductive ink and preparation method thereof Download PDFInfo
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- CN104817891A CN104817891A CN201510170700.XA CN201510170700A CN104817891A CN 104817891 A CN104817891 A CN 104817891A CN 201510170700 A CN201510170700 A CN 201510170700A CN 104817891 A CN104817891 A CN 104817891A
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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
- C09D11/30—Inkjet printing 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
- C09D11/00—Inks
- C09D11/16—Writing 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
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Inks, Pencil-Leads, Or Crayons (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses white-through nano-silver conductive ink which comprises, by weight, 5-60% of silver nanoparticles coated with an anionic surfactant and 40-95% of an ink solvent. The ink solvent is composed of a solid A and a solid B according to the mass ratio of 1: (0.01-0.001), wherein the solid A is selected from at least one of 1,2-propylene glycol, triethanolamine, oleic acid and deionized water; and the solid B is selected from at least one of benzotriazol, 2,2-dibromo-2-cyanoacetamide and hydroxyethyl cellulose. A preparation method of the white-through nano-silver conductive ink is simple and easy to operate. Viscosity of the white-through nano-silver conductive ink at 20 DEG C is 100-500 mPa.s, and surface tension of the white-through nano-silver conductive ink at 20 DEG C is 30-50 mN.m<-1>. A circuit prepared by the use of the white-through nano-silver conductive ink has excellent conductivity and adhesiveness. The conductive ink can be applied to a flexible substrate. Thus, range of application of the conductive ink to printed electronics is broadened.
Description
Technical field
The invention belongs to printed electronics field, be specifically related to a kind of write-through nano silver conductive ink and preparation method thereof.
Background technology
Along with printing technology is to future developments such as flexibility, portable, wearable and low costs, using flexible materialss such as plastics, paper, clothes as the circuit requirements of substrate also in continuous increase.Except the printed circuit methods of routine, copy ballpoint pen to carry out simple straight write circuit preparation, especially the means of flexible circuit connection easily.
In early days, Janpanese Printing Co., Ltd adopts felt tip pen (JP07276878A), pours into silver-colored ink to prepare circuit, but the felt tip pen of similar writing brush, ink amount is not easy to control, and fineness is also poor, and circuit box resistance prepared by its electrically conductive ink adopted is up to 30M Ω/.(Xu, the L.Y. such as Xu, Yang, G.Y., Jing, H.Y., Wei, J., Han, Y.D.Pressure-assisted low-temperature sintering for paper-based writing electronics.Nanotechnology2013, 24, 355204.) silver nano-grain of preparation is dispersed in ethanol, in the mixed solution of ethylene glycol and glycerine, prepare silver-colored ink, then sign pen core is injected, photo papers draws pattern, through 120 DEG C, 25MPa hot pressed sintering is after 15 minutes, the resistivity of the conducting wire of preparation is 14.3 μ Ω cm, be about 9 times of block silver resistivity, but the use of hot-press sintering equipment, seriously limit the range of application of this conductive stylus.(Magdassi, the S. such as Magdassi; Grouchko, M.; Berezin, O.; Kamyshny, A.Triggering the Sintering of Silver Nanoparticles at Room Temperature.ACS Nano2010,4,1943-1948.) method of chemically sintered Argent grain is proposed, the plastic-substrates of soaking diallyl dimethyl ammoniumchloride (PDAC) solution prints Argent grain ink to prepare silver-colored conducting wire, but substrate first need be soaked in the solution, process is more loaded down with trivial details, can destroy the substrates such as paper simultaneously.
On the one hand, the method improving metallic conduction stability of ink realizes by adding protective material.The macromolecule dispersant added in metal nanoparticle preparation or metallic conduction ink preparation process and metal nanoparticle interact and are coated on metal nanoparticle surface; thus prevent the contact between particle and particle, improve the stability of metallic conduction ink.But on the other hand; the surface coated protective material of metal nanoparticle, often affects the transmission of electronics in the coating between metal nanoparticle, prints the circuit after writing; a last handling process (such as heating) must be had to promote particles sintering, improve the electroconductibility of circuit.Picture macromolecule dispersant polyvinylpyrrolidone, be conducive to the stability improving ink, but its post-processing temperature is up to 200 DEG C, limits its application in the flexible substrates such as plastics and paper; Picture lower alkyl amine protective material, although post-processing temperature at 140 DEG C, because the reactive force between this protective material and metal nanoparticle is more weak, can make again the bad stability of this ink.
Summary of the invention
Technical problem to be solved by this invention is, for the deficiencies in the prior art, a kind of write-through nano silver conductive ink and simple preparation method thereof are provided, this nano silver conductive ink can adopt spray ink Printing, the medium direct writing means of the injection shaft of a writing brush prepares circuit in the flexible substrates such as plastics, paper, and this circuit can obtain the good conducting channel of electric property without the need to aftertreatments such as sintering.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of write-through nano silver conductive ink, its mass percent composition comprises: Surface coating has the silver nano-grain 5 ~ 60% of anion surfactant, ink solvent 40 ~ 95%, described ink solvent by category-A liquid and category-B solid by 1:(0.01-0.001) mass ratio form, described category-A liquid is selected from least one in 1,2-PD, trolamine, oleic acid and deionized water; Described category-B solid is selected from least one in benzotriazole, DBNPA and Natvosol.
Category-A liquid is selected from least one in 1,2-PD, trolamine, oleic acid and deionized water, and wherein, 1,2-PD, trolamine and oleic acid are oily liquid, and the flowing being conducive to ink is smooth and easy stable, and deionized water meets the requirement of environmental protection.Category-B solid is selected from benzotriazole, 2, at least one in 2-dibromo-2-cyanoacetamide and Natvosol, wherein, benzotriazole and DBNPA are electrophilic monomer, in the ink curing processes write out, the anion surfactant on electrophilic monomer and silver nano-grain surface neutralizes, and then induce reunion, the sintering of silver nano-grain, Natvosol can change the viscosity of ink, to meet the use needs in different application field.
The particle diameter of described silver nano-grain is less than 60nm.
In above-mentioned write-through nano silver conductive ink, described anion surfactant be selected from polyglutamic acid, polyacrylic acid, polymethyl acrylic acid, polyoxypropylene, fatty alcohol-polyoxyethylene ether and polyxyethylated alkylphenol one or both.Polyglutamic acid, polyacrylic acid anion surfactant can make silver nano-grain surface band negative electricity, and between silver nano-grain, the interaction of electrostatic repulsion makes conductive ink performance more stable.
A preparation method for above-mentioned write-through nano silver conductive ink, comprises the following steps:
(1) category-A liquid and category-B solid are pressed 1:(0.01-0.001) mass ratio mixing, stir obtain ink solvent;
(2) in ink solvent, add the silver nano-grain that Surface coating has anion surfactant, obtain mixing solutions;
(3) mixing solutions is carried out stirring 1-4 hour, obtain the write-through nano silver conductive ink of stable performance.
In the preparation method of above-mentioned write-through nano silver conductive ink, described anion surfactant be selected from polyglutamic acid, polyacrylic acid, polymethyl acrylic acid, polyoxypropylene, fatty alcohol-polyoxyethylene ether and polyxyethylated alkylphenol one or both.
Compared with prior art, the invention has the advantages that: the invention discloses a kind of write-through nano silver conductive ink, its preparation method is simple, easy to operate; The viscosity of write-through nano silver conductive ink of the present invention 20 DEG C time is 100-500mPas, and surface tension is 30-50mNm
-1.Suitable ink viscosity and surface tension are conducive to the spray ink Printing of ink or inject the shaft of a writing brush and directly write and be unlikely to generation and be difficult to ejection or the counter productive such as to leak; Write-through nano silver conductive ink of the present invention can adopt spray ink Printing, the medium direct writing means of the injection shaft of a writing brush prepares circuit in the flexible substrates such as plastics, paper, and this circuit can obtain the good conducting channel of electric property without the need to aftertreatments such as sintering; The circuit adopting write-through nano silver conductive ink of the present invention to prepare has excellent electroconductibility and adhesivity, can be applicable to flexible substrates, expands the range of application of conductive ink on printed electronic.
Accompanying drawing explanation
Fig. 1 is the optical morphology figure writing circuit utilizing the write-through nano silver conductive ink of embodiment 1 on A4 printer paper;
Fig. 2 is the optical morphology figure writing circuit utilizing the write-through nano silver conductive ink of embodiment 1 in polyethylene terephthalate (PET) plastic-substrates;
Fig. 3 a, 3b, 3c be utilize the write-through nano silver conductive ink of embodiment 1 on carton paper write circuit dried scanning electron microscope diagram under room temperature, 100 DEG C/10 minutes, 150 DEG C/10 minutes conditions respectively;
Fig. 4 is the graph of relation between the rate of drying of the circuit that the write-through nano silver conductive ink of embodiment 1 is write out and resistance;
Fig. 5 is the resistance change situation adopting conducting wire in 3M tape adhesion 10000 processes.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
The preparation method of the write-through nano silver conductive ink of embodiment 1 is:
(1) by 0.06g benzotriazole, 0.04g DBNPA and 0.5g Natvosol join 5.2g 1,2-propylene glycol, 0.22g trolamine, in 0.16g oleic acid and 53.82g deionized water, stirring and dissolving obtains ink solvent, and quality is 60g;
(2) in ink solvent, add the silver nano-grain 40g that Surface coating has anion surfactant, obtain mixing solutions;
(3) mixing solutions is carried out stirring 3 hours, obtain the write-through nano silver conductive ink of stable performance.
Above-mentioned obtained write-through nano silver conductive ink is injected the clean pen core that written diameter of the steel ball is 380 μm, obtains conductive ink water-color paintbrush.
Utilize this conductive ink water-color paintbrush to draw conducting wire on common A4 printer paper, the optics picture of drawn conducting wire as shown in Figure 1.The section thickness of the rete utilizing four probe method to be formed in conjunction with sweep electron microscopic measure conductive ink, the resistivity calculating this conducting wire is 14.2 μ Ω cm.
Utilize this conductive ink water-color paintbrush to draw conducting wire in polyethylene terephthalate (PET) plastic-substrates, the optics picture of drawn conducting wire as shown in Figure 2.The section thickness of the rete utilizing four probe method to be formed in conjunction with sweep electron microscopic measure conductive ink, the resistivity calculating this conducting wire is 16.7 μ Ω cm.
Four probe method measures the principle of metal pattern: the needle point of four point probe touches metal pattern surface simultaneously, and two, the outside probe constant current source of four point probe is connected, and two, the inner side probe of four point probe is connected on voltmeter.When electric current flows through two probes in outside of four point probe from constant current source, the voltage flowing through metal pattern generation can read from voltmeter.The resistivity calculation formula of metal pattern is:
Wherein, ρ is the resistivity of metal pattern; I is the electric current flowing through metal pattern, is provided by constant current source; V is the voltage that electric current produces when flowing through metal pattern print, is read by voltmeter; D is the thickness of metal pattern, can be drawn by scanning electron microscope.
In order to further illustrate the room temperature writing effect of write-through nano silver conductive ink, this conductive ink water-color paintbrush is utilized to draw conducting wire on carton paper, then by drawn conducting wire dry under room temperature, 100 DEG C/10 minutes, 150 DEG C/10 minutes conditions or sintering respectively, the scanning electron microscopic picture of dried conducting wire is respectively as shown in Fig. 3 a, Fig. 3 b and Fig. 3 c.As can be seen from Fig. 3 a, Fig. 3 b, Fig. 3 c, along with the rising of sintering temperature, the morphology change of silver nano-grain is less, illustrates that the conducting wire adopting nano silver conductive ink of the present invention to prepare has excellent adhesivity and stability, record its corresponding resistivity in addition and be followed successively by 15.2 μ Ω cm, 14.8 μ Ω cm, 14.2 μ Ω cm, change less, the impact of visible sintering temperature on write-through nano silver conductive ink electric conductivity of the present invention is very little, even if illustrate without sintering step, the conducting wire adopting nano silver conductive ink of the present invention to prepare still has good electric conductivity, Fig. 4 is the graph of relation between the circuit rate of drying write out of the write-through nano silver conductive ink of embodiment 1 and resistance, illustrate that the circuit rate of drying that write-through nano silver conductive ink is write out is fast, be 260000 Ω during dry 1 minute of its resistance, and resistance drops to 193 Ω after dry 30 minutes.
Adopt 3M adhesive tape to test the adhesivity directly writing on suprabasil silver-colored conducting wire, measure the resistance (R-R of silver-colored conducting wire
0)/R
0along with the change adhering to number of times, wherein R is for adhering to rear conducting wire resistance, R
0for conducting wire initial resistance.Fig. 5 is the resistance change situation adopting conducting wire in 3M tape adhesion 10000 processes, as can be seen from Figure 5, even if adopt 3M tape adhesion 10000 times, the resistance change of conducting wire prepared by nano silver conductive ink of the present invention is only 2.5%, illustrate that the adhesive power of conducting wire and substrate is strong, substantially do not come off.
Therefore, write-through nano silver conductive ink of the present invention at room temperature has good writing effect, and the circuit adopting write-through nano silver conductive ink of the present invention to prepare has excellent electroconductibility, adhesivity and stability, can be applicable to various flexible substrates.
The preparation method of the write-through nano silver conductive ink of embodiment 2 is:
(1) by 0.05g benzotriazole, 0.02g DBNPA and 0.02g Natvosol join 26g 1,2-propylene glycol, 1.1g trolamine, in 0.8g oleic acid and 67.01g deionized water, stirring and dissolving obtains ink solvent, and quality is 95g;
(2) in ink solvent, add the silver nano-grain 5g that Surface coating has anion surfactant, obtain mixing solutions;
(3) mixing solutions is carried out stirring 4 hours, obtain the write-through nano silver conductive ink of stable performance.
The preparation method of the write-through nano silver conductive ink of embodiment 3 is:
(1) by 0.03g benzotriazole, 0.01g DBNPA and 0.01g Natvosol join 30g 1,2-propylene glycol, 2g trolamine, in 1g oleic acid and 36.01g deionized water, stirring and dissolving obtains ink solvent, and quality is 70g;
(2) in ink solvent, add the silver nano-grain 30g that Surface coating has anion surfactant, obtain mixing solutions;
(3) mixing solutions is carried out stirring 1 hour, obtain the write-through nano silver conductive ink of stable performance.
Surface coating used in above-described embodiment has the preparation of the silver nano-grain of anion surfactant, and the publication number can declared with reference to the applicant is the method recorded in the patent of invention of CN102816462A.
Claims (5)
1. a write-through nano silver conductive ink, it is characterized in that, its mass percent composition comprises: Surface coating has the silver nano-grain 5 ~ 60% of anion surfactant, ink solvent 40 ~ 95%, described ink solvent by category-A liquid and category-B solid by 1:(0.01-0.001) mass ratio form, described category-A liquid is selected from least one in 1,2-PD, trolamine, oleic acid and deionized water; Described category-B solid is selected from least one in benzotriazole, DBNPA and Natvosol.
2. a kind of write-through nano silver conductive ink according to claim 1, is characterized in that the particle diameter of described silver nano-grain is less than 60nm.
3. a kind of write-through nano silver conductive ink according to claim 1 and 2, it is characterized in that described anion surfactant is selected from polyglutamic acid, polyacrylic acid, polymethyl acrylic acid, polyoxypropylene, fatty alcohol-polyoxyethylene ether and polyxyethylated alkylphenol one or both.
4. a preparation method for the write-through nano silver conductive ink described in claim 1 or 2, is characterized in that comprising the following steps:
(1) category-A liquid and category-B solid are pressed 1:(0.01-0.001) mass ratio mixing, stir obtain ink solvent;
(2) in ink solvent, add the silver nano-grain that Surface coating has anion surfactant, obtain mixing solutions;
(3) mixing solutions is carried out stirring 1-4 hour, obtain the write-through nano silver conductive ink of stable performance.
5. the preparation method of a kind of write-through nano silver conductive ink according to claim 4, it is characterized in that described anion surfactant is selected from polyglutamic acid, polyacrylic acid, polymethyl acrylic acid, polyoxypropylene, fatty alcohol-polyoxyethylene ether and polyxyethylated alkylphenol one or both.
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| CN201510170700.XA CN104817891B (en) | 2015-04-13 | 2015-04-13 | Write-through nano-silver conductive ink and preparation method thereof |
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| CN201510170700.XA CN104817891B (en) | 2015-04-13 | 2015-04-13 | Write-through nano-silver conductive ink and preparation method thereof |
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| CN104817891B CN104817891B (en) | 2017-03-22 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106634220A (en) * | 2016-09-13 | 2017-05-10 | 江南大学 | Environmental friendly nano silver conductive ink and preparation method and printing application thereof |
| CN106752365A (en) * | 2016-12-02 | 2017-05-31 | 曲阜师范大学 | A kind of water-proof environmental protection prepared Chinese ink and preparation method thereof |
| CN108707369A (en) * | 2017-04-03 | 2018-10-26 | 纳米及先进材料研发院有限公司 | The water-base conductive ink of swift electron device prototype for that can write |
| CN108847359A (en) * | 2018-06-27 | 2018-11-20 | 暨南大学 | A kind of preparation method and application of direct write CNT/Ag flexible super capacitor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07319165A (en) * | 1994-03-31 | 1995-12-08 | Mitsubishi Paper Mills Ltd | Planographic printing plate and processing method for the same |
| CN102504647A (en) * | 2011-10-31 | 2012-06-20 | 天津大学 | Conductive ink based on nano metal and application thereof in different jet printing methods and photographic paper |
| CN102816462A (en) * | 2012-08-13 | 2012-12-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method for nano-silver particles coated with organic protection agent on surfaces |
| CN103194117A (en) * | 2013-04-08 | 2013-07-10 | 电子科技大学 | Preparation method and application of sintering-free ultrafine silver nanometer printing ink |
-
2015
- 2015-04-13 CN CN201510170700.XA patent/CN104817891B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07319165A (en) * | 1994-03-31 | 1995-12-08 | Mitsubishi Paper Mills Ltd | Planographic printing plate and processing method for the same |
| CN102504647A (en) * | 2011-10-31 | 2012-06-20 | 天津大学 | Conductive ink based on nano metal and application thereof in different jet printing methods and photographic paper |
| CN102816462A (en) * | 2012-08-13 | 2012-12-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method for nano-silver particles coated with organic protection agent on surfaces |
| CN103194117A (en) * | 2013-04-08 | 2013-07-10 | 电子科技大学 | Preparation method and application of sintering-free ultrafine silver nanometer printing ink |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106634220A (en) * | 2016-09-13 | 2017-05-10 | 江南大学 | Environmental friendly nano silver conductive ink and preparation method and printing application thereof |
| CN106752365A (en) * | 2016-12-02 | 2017-05-31 | 曲阜师范大学 | A kind of water-proof environmental protection prepared Chinese ink and preparation method thereof |
| CN108707369A (en) * | 2017-04-03 | 2018-10-26 | 纳米及先进材料研发院有限公司 | The water-base conductive ink of swift electron device prototype for that can write |
| CN108707369B (en) * | 2017-04-03 | 2021-04-30 | 纳米及先进材料研发院有限公司 | Water-based conductive ink for writable rapid electronic device prototypes |
| CN108847359A (en) * | 2018-06-27 | 2018-11-20 | 暨南大学 | A kind of preparation method and application of direct write CNT/Ag flexible super capacitor |
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| CN104817891B (en) | 2017-03-22 |
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