CN111393910A - Composite nano-copper conductive ink, preparation method thereof and conductive device - Google Patents
Composite nano-copper conductive ink, preparation method thereof and conductive device Download PDFInfo
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- 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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- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The invention relates to the technical field of printed electronics, in particular to composite nano-copper conductive ink, a preparation method thereof and a conductive device. The composite nano-copper conductive ink provided by the invention comprises, by mass, 50-60 wt.% of a solvent, 5-10 wt.% of a dispersant, 0-1 wt.% of an antioxidant and 34-39 wt.% of a conductive filler; the conductive filler includes nano copper powder and nano carbon material. The composite nano-copper conductive ink provided by the invention has excellent conductivity, and compared with the existing metal ink, the production cost is obviously reduced. The embodiment result shows that the conductivity of the composite nano-copper conductive ink provided by the invention is far higher than that of the ink only added with nano-copper powder as a conductive filler.
Description
Technical Field
The invention relates to the technical field of printed electronics, in particular to composite nano-copper conductive ink, a preparation method thereof and a conductive device.
Background
To date, most conductive inks in the field of printed electronics are made using metal nanomaterials, such as gold nanomaterials, silver nanomaterials, and copper nanomaterials, because of their higher conductivity. However, the material cost of gold and silver is high, and the material cost of copper is low, but the preparation process of the copper nano material is complex and expensive, so the production cost is high. Carbon nanomaterials such as graphene and carbon nanotubes have also been used for preparing conductive ink due to their advantages such as high mechanical strength and strong heat and electrical conductivity, but the conductive patterns prepared based on the carbon nanotube conductive ink have much lower electrical conductivity than metal ink.
Disclosure of Invention
The invention aims to provide composite nano-copper conductive ink, a preparation method thereof and a conductive device.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides composite nano-copper conductive ink which comprises, by mass, 50-60 wt.% of a solvent, 5-10 wt.% of a dispersant, 0-1 wt.% of an antioxidant and not 0, and 34-39 wt.% of a conductive filler; the conductive filler includes nano copper powder and nano carbon material.
Preferably, the boiling point of the solvent is 180-220 ℃.
Preferably, the dispersant comprises polyacrylic acid, polyvinyl alcohol, polyvinylpyrrolidone, gelatin, sodium lauryl sulfate, polyethylene glycol octylphenyl ether, cetyltrimethylammonium bromide, sodium diisooctyl succinate sulfonate, di (2-ethylhexyl) phosphoric acid, oleic acid or dodecylamine.
Preferably, the antioxidant is a saturated monocarboxylic acid.
Preferably, the particle size of the nano-copper powder is 30-60 nm.
Preferably, the mass of the nano carbon material accounts for 1-6% of the total mass of the composite nano copper conductive ink.
Preferably, the nanocarbon material comprises graphene or carbon nanotubes; the size of the graphene is 5-40 mu m, and the thickness of the graphene is 1-10 nm; the length of the carbon nano tube is 20-40 mu m, and the outer diameter of the carbon nano tube is 8-15 nm.
The invention provides a preparation method of the composite nano-copper conductive ink in the technical scheme, which comprises the following steps:
(1) mixing a solvent, a dispersant, an antioxidant and nano copper powder to obtain mixed slurry;
(2) and mixing the mixed slurry with a nano carbon material to obtain the composite nano copper conductive ink.
Preferably, the mixing in step (1) is ball milling.
The invention also provides a conductive device, which comprises a flexible substrate and a conductive layer arranged on the surface of the flexible substrate; the conducting layer is obtained by sintering and curing the composite nano-copper conducting ink prepared by the scheme or the composite nano-copper conducting ink prepared by the preparation method of the scheme.
The invention provides composite nano-copper conductive ink which comprises, by mass, 50-60 wt.% of a solvent, 5-10 wt.% of a dispersant, 0-1 wt.% of an antioxidant and not 0, and 34-39 wt.% of a conductive filler; the conductive filler includes nano copper powder and nano carbon material. In the invention, the addition amount of the dispersing agent is controlled, so that the dispersing agent is partially coated on the surfaces of the nano copper powder and the nano carbon material, the contact among particles is not hindered, and the conductive filler can be stably dispersed in the conductive ink; the antioxidant can prevent the oxidation of the nano-copper powder, and the conductive filler adopts the nano-copper powder and the nano-carbon material, so that the charge mobility of the conductive layer can be greatly improved under the condition of reducing the charge density of the conductive layer as little as possible, and meanwhile, the generation of cracks in the conductive layer is inhibited, and the conductive performance and the fatigue resistance of the ink are further improved; furthermore, the charge density and the charge transfer rate of the conductive layer are balanced by controlling the addition amount of the carbon nano material, so that the conductive performance of the conductive layer is improved; meanwhile, compared with the existing metal printing ink, the production cost is obviously reduced. The embodiment result shows that the conductivity of the composite nano-copper conductive ink provided by the invention is far higher than that of the ink only added with nano-copper powder as conductive filler, and the conductive layer formed by adopting the composite nano-copper conductive ink provided by the invention has excellent bending resistance.
Drawings
FIG. 1 is a schematic view of a bending fatigue testing machine according to a test example of the present invention.
Detailed Description
The invention provides composite nano-copper conductive ink which comprises, by mass, 50-60 wt.% of a solvent, 5-10 wt.% of a dispersant, 0-1 wt.% of an antioxidant and 34-39 wt.% of a conductive filler; the conductive filler includes nano copper powder and nano carbon material.
The composite nano-copper conductive ink comprises 50-60 wt% of solvent, preferably 52-57 wt%. In the invention, the boiling point of the solvent is preferably 180-220 ℃; the solvent is preferably one or more of toluene, cyclohexane, n-heptane, isooctane, methanol, ethanol, ethylene glycol, diethylene glycol and diethylene glycol. In a specific embodiment of the present invention, the solvent is diethylene glycol and ethanol, and the mass ratio of the diethylene glycol to the ethanol is preferably 52: 5. The high boiling point solvent is adopted in the invention to reduce the volatilization speed of the ink solvent and prevent the ink from being cured in advance in the long-time coating process, thereby influencing the coating uniformity of the conductive ink or the adhesive force between the conductive layer and the substrate after sintering.
The composite nano-copper conductive ink comprises 5-10 wt% of dispersing agent, preferably 6-8 wt%. In the present invention, the dispersant preferably includes polyacrylic acid, polyvinyl alcohol, polyvinyl pyrrolidone, gelatin, sodium lauryl sulfate, polyethylene glycol octylphenyl ether, cetyltrimethylammonium bromide, sodium diisooctyl succinate sulfonate, di (2-ethylhexyl) phosphoric acid, oleic acid, or dodecylamine. According to the invention, the dispersant can be partially coated on the surfaces of the nano copper powder and the nano carbon material by controlling the dosage of the dispersant, the Zeta potential of the ink is measured to obtain the dispersibility of the nano particles, the coating ratio is indirectly reflected, the coating ratio is preferably 50%, the contact among the particles is not hindered under the partial coating effect, the conductive filler can be stably dispersed in the conductive ink, and the conductivity and the fatigue resistance of the ink are further improved.
The composite nano-copper conductive ink comprises 0-1 wt.% of antioxidant, preferably 1 wt.%. According to the invention, the content of the antioxidant is controlled to be less than 1 wt.%, so that the adverse effect of the excessive content of the antioxidant on the conductivity of the sintered and cured conductive layer can be avoided. In the present invention, the antioxidant is preferably a saturated monocarboxylic acid, and particularly preferably formic acid, acetic acid or propionic acid. In the invention, the antioxidant can prevent the oxidation of the nano copper particles, so that the conductive ink can be sintered and cured in an atmospheric atmosphere.
The composite nano-copper conductive ink comprises, by mass, 34-39 wt.% of conductive filler, preferably 35-37%; the conductive filler includes nano copper powder and nano carbon material. In the invention, the nano carbon material preferably accounts for 1-6%, more preferably 4-5% of the total mass of the composite nano copper conductive ink. According to the invention, the nano copper powder and the nano carbon material are compounded, so that cracks in the conductive layer can be effectively reduced, the charge density of the conductive layer is not influenced, the charge migration rate of the conductive layer is improved, and the conductivity and the fatigue resistance of the ink are further improved.
In the invention, the particle size of the nano-copper powder is preferably 30-60 nm, and more preferably 40-50 nm. In the present invention, the nanocarbon material preferably includes graphene or carbon nanotubes; the size of the graphene is preferably 5-40 μm, and more preferably 20-30 μm; the size of the graphene refers to the length/width of the graphene sheet layer; the thickness of the graphene is preferably 1-10 nm, and more preferably 4-5 nm; the length of the carbon nano tube is preferably 20-40 μm, and more preferably 20-30 μm; the outer diameter of the carbon nano tube is preferably 8-15 nm, and more preferably 10-12 nm. In the present invention, the nanocarbon material is graphene or carbon nanotubes. The invention limits the size of the nano-copper powder and the nano-carbon material to be in the range, and can limit the volume fraction ratio of the nano-copper and the nano-carbon material in the conducting layer.
The invention provides a preparation method of the composite nano-copper conductive ink in the technical scheme, which comprises the following steps:
(1) mixing a solvent, a dispersant, an antioxidant and nano copper powder to obtain mixed slurry;
(2) and mixing the mixed slurry with a nano carbon material to obtain the composite nano copper conductive ink.
The solvent, the dispersant, the antioxidant and the nano-copper powder are mixed to obtain the mixed slurry. In the invention, the mixing is preferably ball milling mixing, and the milling beads for ball milling mixing are preferably agate balls; the diameter of the grinding bead is preferably 2 mm; the ball-material ratio of the ball-milling mixing is preferably 2: 1; the equipment adopted for ball milling and mixing is preferably a planetary ball mill; the rotation speed of ball milling mixing is preferably 300-400 r/min; the time for ball milling and mixing is preferably 8-10 h. The invention adopts ball milling mixing to ensure that the dispersing agent is uniformly coated on the nano-copper particles as much as possible.
After the mixed slurry is obtained, the mixed slurry is mixed with the nano carbon material to obtain the composite nano copper conductive ink. In the invention, the mixing of the mixed slurry and the nano-carbon material is preferably carried out in an ultrasonic cell crusher, the mixing is preferably ultrasonic mixing, and the time of the ultrasonic mixing is preferably 10-15 min. According to the invention, the solvent, the dispersant, the antioxidant and the nano-copper powder are mixed firstly, and then the nano-carbon material is added and mixed, so that the nano-carbon material can be prevented from being damaged in structure during ball milling and mixing, and the performance of the nano-carbon material is prevented from being influenced.
The invention also provides a conductive device, which comprises a flexible substrate and a conductive layer arranged on the surface of the flexible substrate; the conducting layer is obtained by sintering and curing the composite nano-copper conducting ink in the technical scheme or the composite nano-copper conducting ink prepared by the preparation method in the scheme. In the present invention, the flexible substrate is preferably a polyimide substrate or a polyester film. In the present invention, the thickness of the conductive layer is preferably 10 to 30 μm, and more preferably 20 μm. The invention has no special requirement on the sintering and curing atmosphere and can be used in the atmosphere. In the invention, the solvent is volatilized in the sintering and curing process; the dispersant is cracked and remained in the conductive layer; the antioxidant decomposes into nonconductive impurities; melting and growing the nano copper particles into a whole; the structure of the nano carbon material is basically unchanged and is wrapped by the copper nanoparticles. In the invention, the sintering and curing temperature is preferably 200-270 ℃, and more preferably 230 ℃; the sintering and curing time is preferably 0.5-2 h, and more preferably 1 h.
In a specific embodiment of the present invention, the method for manufacturing the conductive device preferably includes the steps of: and (3) printing the composite nano-copper conductive ink or the composite nano-copper conductive ink prepared by the preparation method of the above technical scheme on the surface of a flexible substrate by using a screen printing technology, and then sintering and curing to obtain the conductive device. The invention has no special requirements on the specific process parameters of the screen printing technology, and the screen printing technology which is well known by the technicians in the field can be adopted; the sintering and curing process parameters are the same as those in the foregoing, and are not described in detail here. In the present invention, the surface of the conductive device is preferably a patterned conductive layer.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The composite nano-copper conductive ink comprises the following components in percentage by mass: 60 wt% of solvent ethylene glycol, 1 wt% of antioxidant formic acid, 5 wt% of dispersant polyvinylpyrrolidone, 33 wt% of conductive filler nano-copper powder and 1 wt% of conductive filler graphene; the particle size of the nano copper powder is 30-60 nm, the graphene is No. 2 of commercial ink, the size of the graphene is 5-40 mu m, and the thickness of the graphene is 1-10 nm.
The preparation method comprises the following steps:
(1) according to the proportion, putting ethylene glycol, polyvinylpyrrolidone, formic acid and nano copper powder into a ball milling tank, and then adding agate ball milling beads with the diameter of 2mm, wherein the ball-to-material ratio is 2: 1; putting the mixture into a planetary ball mill, and stirring and mixing the mixture for 8 hours at the rotating speed of 300r/min to obtain mixed slurry;
(2) and placing the mixed slurry and graphene in a beaker, primarily stirring by using a glass rod, then placing in an ultrasonic cell crusher, and performing ultrasonic dispersion for 10min to obtain the composite nano-copper conductive ink.
Example 2
The composite nano-copper conductive ink comprises the following components in percentage by mass: 55 wt% of diethylene glycol serving as a solvent, 1 wt% of acetic acid serving as an antioxidant, 10 wt% of sodium dodecyl sulfate serving as a dispersant, 30 wt% of nano copper powder serving as a conductive filler and 4 wt% of graphene serving as a conductive filler; the particle size of the nano-copper powder is 30-60 nm, the size of the graphene is 5-40 mu m, and the thickness of the graphene is 1-10 nm.
The preparation method comprises the following steps:
(1) according to the proportion, diethylene glycol, sodium dodecyl sulfate, acetic acid and nano copper powder are placed in a ball milling tank, and then agate grinding balls with the diameter of 2mm are added, wherein the ball-material ratio is 2: 1; putting the mixture into a planetary ball mill, and stirring and mixing the mixture for 9 hours at the rotating speed of 300r/min to obtain mixed slurry;
(2) and placing the mixed slurry and graphene in a beaker, primarily stirring by using a glass rod, then placing in an ultrasonic cell crusher, and performing ultrasonic dispersion for 15min to obtain the composite nano-copper conductive ink.
Example 3
The composite nano-copper conductive ink comprises the following components in percentage by mass: 52 wt.% of diethylene glycol serving as a solvent, 5 wt.% of ethanol serving as a solvent, 1 wt.% of propionic acid serving as an antioxidant, 8 wt.% of cetyltrimethylammonium bromide serving as a dispersant, 30 wt.% of nano-copper powder serving as a conductive filler and 4 wt.% of carbon nano-tubes serving as a conductive filler; the particle size of the nano-copper powder is 30-60 nm, the length of the carbon nano-tube is 20-40 mu m, and the outer diameter of the carbon nano-tube is 8-15 nm.
The preparation method comprises the following steps:
(1) putting diethylene glycol, ethanol, hexadecyl trimethyl ammonium bromide, propionic acid and nano copper powder into a ball milling tank according to the proportion, and then adding agate ball milling beads with the diameter of 2mm, wherein the ball-to-material ratio is 2: 1; putting the mixture into a planetary ball mill, and stirring and mixing the mixture for 10 hours at the rotating speed of 400r/min to obtain mixed slurry;
(2) and placing the mixed slurry and graphene in a beaker, primarily stirring by using a glass rod, then placing in an ultrasonic cell crusher, and performing ultrasonic dispersion for 15min to obtain the composite nano-copper conductive ink.
Example 4
The composite nano-copper conductive ink prepared in the example 1 is printed on the surface of a polyimide substrate by using a screen printing technology, then the printed substrate is placed in a tube furnace, and is sintered and cured for 1 hour at the temperature of 230 ℃, and the composite nano-copper conductive ink forms a conductive layer on the surface of the polyimide substrate, so that a conductive device is obtained.
Example 5
The composite nano-copper conductive ink prepared in the example 2 is printed on the surface of a polyimide substrate by using a screen printing technology, then the printed substrate is placed in a tube furnace, and is sintered and cured for 1 hour at the temperature of 230 ℃, and the composite nano-copper conductive ink forms a conductive layer on the surface of the polyimide substrate, so that a conductive device is obtained.
Example 6
And (2) printing the composite nano-copper conductive ink prepared in the embodiment 3 on the surface of a polyimide substrate by using a screen printing technology, then placing the printed substrate in a tubular furnace, and sintering and curing for 1h at 230 ℃, wherein the composite nano-copper conductive ink forms a conductive layer on the surface of the polyimide substrate to obtain the conductive device.
Comparative example 1
The conductive ink comprises the following components in percentage by mass: 60 wt.% of solvent ethylene glycol, 5 wt.% of dispersant polyvinylpyrrolidone and 35 wt.% of conductive filler nano-copper powder; the particle size of the nano-copper powder is 30-60 nm.
The preparation method comprises the following steps: according to the proportion, putting ethylene glycol, polyvinylpyrrolidone and nano copper powder into a ball milling tank, and then adding agate ball milling beads with the diameter of 2mm, wherein the ball-material ratio is 2: 1; and putting the mixture into a planetary ball mill, and stirring and mixing the mixture for 8 hours at the rotating speed of 300r/min to obtain the conductive ink.
And printing patterns on the surface of the polyimide substrate by using the prepared conductive ink by using a screen printing technology, putting the printed substrate into a tube furnace, sintering and curing for 1h at 230 ℃ in an inert atmosphere, and forming a conductive layer on the surface of the polyimide substrate by using the conductive ink to obtain the conductive device.
Test example
Carrying out resistivity detection on the conductive devices prepared in the embodiments 4-6 and the comparative example 1 to test the conductivity of the conductive layer on the surface of the polyimide substrate; the conductivity test performed by the embodiment of the invention is performed according to the GB/T26074-2010 germanium single crystal resistivity direct-current four-probe measurement method standard;
conducting mechanical fatigue performance tests on the conductive devices prepared in examples 4-6 and comparative example 1 by adopting a repeated tensile loading (external bending) test; the bending fatigue testing machine shown in figure 1 is adopted for testing, and consists of a fixing clamp and an axial displacement part driven by a motor, and the fixing clamp and the axial displacement part are respectively used for fixing and bending the polyimide substrate; the fatigue test was carried out at a frequency of 1Hz, and the change in resistivity was measured every 250 cycles up to 1000 cycles, and the results are shown in table 1.
TABLE 1 test results of conductivity and bending fatigue properties
| 0 period of bending | Bending 250 period | Bending 500 cycles | Bending period 750 | Bending 1000 cycles | |
| Example 4 | 5.39μΩ·cm | 14.53μΩ·cm | 26.41μΩ·cm | 37.37μΩ·cm | 60.37μΩ·cm |
| Example 5 | 6.48μΩ·cm | 14.91μΩ·cm | 29.81μΩ·cm | 44.06μΩ·cm | 68.04μΩ·cm |
| Example 6 | 7.86μΩ·cm | 19.65μΩ·cm | 35.37μΩ·cm | 51.09μΩ·cm | 80.17μΩ·cm |
| Comparative example 1 | 11.50μΩ·cm | 64.4μΩ·cm | 227.7μΩ·cm | 729.1μΩ·cm | 1509.95μΩ·cm |
As can be seen from table 1, the conductive properties and bending fatigue properties of the conductive pattern prepared by the ink added with the nano carbon material are much higher than those of the ink using only the nano copper powder as the conductive filler. The composite nano-copper conductive ink provided by the invention can be directly sintered and cured in the atmosphere, does not need vacuum or inert atmosphere, has low requirements on preparation process and is easier to operate.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The composite nano-copper conductive ink comprises, by mass, 50-60 wt.% of a solvent, 5-10 wt.% of a dispersant, 0-1 wt.% but not 0 of an antioxidant, and 34-39 wt.% of a conductive filler; the conductive filler includes nano copper powder and nano carbon material.
2. The composite nano-copper conductive ink as claimed in claim 1, wherein the solvent has a boiling point of 180-220 ℃.
3. The composite nano-copper conductive ink according to claim 1, wherein the dispersant comprises polyacrylic acid, polyvinyl alcohol, polyvinylpyrrolidone, gelatin, sodium dodecyl sulfate, polyethylene glycol octyl phenyl ether, cetyl trimethylammonium bromide, sodium diisooctyl succinate sulfonate, di (2-ethylhexyl) phosphoric acid, oleic acid, or dodecylamine.
4. The composite nano-copper conductive ink according to claim 1, wherein the antioxidant is a saturated monocarboxylic acid.
5. The composite nano-copper conductive ink according to claim 1, wherein the nano-copper powder has a particle size of 30 to 60 nm.
6. The composite nano-copper conductive ink according to claim 1, wherein the nano-carbon material accounts for 1-6% of the total mass of the composite nano-copper conductive ink.
7. The composite nano-copper conductive ink according to claim 1 or 6, wherein the nano-carbon material comprises graphene or carbon nanotubes; the size of the graphene is 5-40 mu m, and the thickness of the graphene is 1-10 nm; the length of the carbon nano tube is 20-40 mu m, and the outer diameter of the carbon nano tube is 8-15 nm.
8. The preparation method of the composite nano-copper conductive ink as claimed in any one of claims 1 to 7, comprising the following steps:
(1) mixing a solvent, a dispersant, an antioxidant and nano copper powder to obtain mixed slurry;
(2) and mixing the mixed slurry with a nano carbon material to obtain the composite nano copper conductive ink.
9. The method of claim 8, wherein the mixing of step (1) is ball milling.
10. A conductive device comprises a flexible substrate and a conductive layer arranged on the surface of the flexible substrate, and is characterized in that the conductive layer is obtained by sintering and curing the composite nano-copper conductive ink as defined in any one of claims 1 to 7 or the composite nano-copper conductive ink prepared by the preparation method as defined in any one of claims 8 to 9.
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Application publication date: 20200710 |