CN110655831A - Preparation method of nano silver carbon nanotube composite conductive ink - Google Patents
Preparation method of nano silver carbon nanotube composite conductive ink Download PDFInfo
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- CN110655831A CN110655831A CN201911120080.3A CN201911120080A CN110655831A CN 110655831 A CN110655831 A CN 110655831A CN 201911120080 A CN201911120080 A CN 201911120080A CN 110655831 A CN110655831 A CN 110655831A
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
Abstract
The invention discloses a preparation method of nano silver carbon nanotube composite conductive ink, and relates to the technical field of ink preparation. Introducing polar groups on the surface of the carbon nano tube, and ultrasonically dispersing the polar groups in ethanol to prepare a carbon nano tube ethanol solution; reducing and loading nano silver on the prepared carbon nano tube to prepare a nano silver carbon nano tube conductive composite filler; and compounding the conductive filler, the flaky nano silver, the polyurethane acrylate, the epoxy acrylate, the acrylate monomer and the auxiliary agent to prepare the nano silver-carbon nanotube composite conductive ink. The nano silver is adopted to modify the carbon nano tubes, so that the van der Waals effect among the carbon nano tubes is reduced, and the agglomeration of the carbon nano tubes is limited; the modified carbon nano tube plays a role in stably dispersing the nano silver in the components, and inhibits the agglomeration and flocculation of the nano silver; meanwhile, the conductivity of the ink is improved by adding the nano silver carbon nano tube composite conductive filler, and the comprehensive performance of the ink is improved.
Description
Technical Field
The invention belongs to the technical field of ink preparation, and particularly relates to a preparation method of nano silver carbon nanotube composite conductive ink.
Background
With the development of electronic information technology, the traditional printing technology can not meet the requirements, and more electronic printing technologies are combined with the electronic information technology, so that the development and innovation of the printing technology are promoted. The conductive ink is a core part of the electronic printing technology and determines the quality of the electronic printing technology. The conductive ink on the market at present mainly comprises water-based conductive ink and solvent-based conductive ink, the two inks are used after being sintered and cured, the time required by sintering and curing is long, and the solvent is released in the curing process, so that the environment-friendly concept is not facilitated. The patent CN 104668575A discloses that a weak solvent is used to replace an organic solvent to prepare nano-silver conductive ink, and solves the problem of the volatilization of a large amount of organic solvent in the traditional solvent conductive ink. But the solvent still volatilizes, the UV conductive ink does not need to be sintered and cured, the UV conductive ink is cured for more than ten seconds under the irradiation of an ultraviolet lamp, the diluted monomer in the conductive ink is an active monomer and participates in reaction in the curing process, and the little solvent is released.
The conductive filler is the core part of the conductive ink and mainly comprises metal conductive filler, nonmetal conductive filler, conductive polymer conductive filler and composite conductive filler. At present, metallic conductive fillers and composite conductive fillers are researched more. The carbon nano tube has excellent mechanical property, electrical property and structural property, and is widely applied to the electronic field. The carbon nano tube has the characteristics of high length-diameter ratio, high conductivity, nano-scale diameter, tunnel effect and the like, and is high in strength and not easy to damage under the action of external force. However, the carbon nanotube belongs to a carbon system, and the contact resistance of the carbon nanotube itself is large, which is not favorable for the application of the carbon nanotube in electronic products. The carbon nano tube can be modified by nano metal, so that the contact resistance can be greatly reduced.
According to the invention, the nano-silver modified carbon nano-tube and the flaky nano-silver are used as conductive fillers, and the nano-silver carbon nano-tube can fill the gap, so that the electron flow is promoted, and the conductivity is improved. And the addition of the carbon nano tube can improve the comprehensive performance of the ink and expand the application field of the ink.
Disclosure of Invention
The invention aims to provide a preparation method of nano silver carbon nanotube composite conductive ink, and the prepared ink has the advantages of good stability, quick drying and curing, good adhesive force and excellent conductivity.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a preparation method of nano silver carbon nanotube composite conductive ink, which comprises the following steps:
step 1, introducing polar groups on the surface of a carbon nano tube, and ultrasonically dispersing the polar groups in ethanol to prepare a carbon nano tube ethanol solution;
step 2, reducing and loading the nano silver on the carbon nano tube prepared in the step 1 to prepare the nano silver carbon nano tube conductive composite filler;
and 3, compounding the conductive filler, the flaky nano silver, the polyurethane acrylate, the epoxy acrylate, the acrylate monomer and the auxiliary agent to prepare the nano silver-carbon nanotube composite conductive ink.
Further, the step 1 specifically includes:
adding carbon nano tubes into mixed acid of concentrated nitric acid and concentrated sulfuric acid, heating in a water bath at 50-60 ℃, and stirring for 2-4 h; then washing and centrifuging by using deionized water until the supernatant is neutral, taking the lower-layer precipitate, placing the precipitate in a vacuum oven at 50 ℃ and drying to constant weight to obtain the ultrasonic wave;
wherein the dosage ratio of the carbon nano tube to the concentrated nitric acid is as follows: (0.5-1): (13-25);
wherein the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid in the mixed acid is 1: 3;
wherein the mass ratio of the carbon nano tube to the ethanol is 1: 20-35.
Further, the polar group includes a hydroxyl group, a carboxyl group.
Further, the preparation of the nano silver carbon nanotube conductive composite filler comprises the following steps:
dissolving 0.5-3 parts of silver nitrate in 50 parts of deionized water to prepare a silver nitrate solution, adding 0.7-3 parts of polyvinylpyrrolidone, adding 10-20mL of acidified carbon nanotube ethanol solution, stirring at 40-60 ℃ for 20-30min, and uniformly dispersing to obtain solution A; dissolving 1.5-4.5 parts of hydrazine hydrate in 50 parts of deionized water, and marking as liquid B; dripping 5-15mL of solution B into solution A at a rate of 5-15 drops per minute, and stirring for 20-50 min; and washing and centrifuging for 3-5 times by using absolute ethyl alcohol after stirring is finished, and drying the sediment at the lower layer until the weight is constant to obtain the nano silver carbon nano tube conductive composite filler.
Further, the step 3 comprises:
adding 10-20 parts of urethane acrylate, 5-10 parts of epoxy acrylate, 5-15 parts of nano silver carbon nanotube composite conductive filler, 45-55 parts of flaky nano silver and 5-10 parts of acrylate monomer into a stirring barrel, and stirring for 30-60 minutes at the stirring speed of 700-; transferring the obtained liquid into a grinding machine, and grinding for 1-3 times; transferring the ground liquid into a stirring barrel, adding 1-5 parts of photoinitiator and 1-5 parts of auxiliary agent, and stirring for 30-60 minutes at the stirring speed of 700-.
Further, the acrylate monomer is selected from one or a mixture of butyl acrylate, methyl methacrylate, styrene, acrylic acid and hydroxyethyl acrylate.
Further, the photoinitiator is selected from one or a mixture of 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, 2,4, 6-trimethylbenzoyl phenyl ethyl phosphonate and 2-hydroxy-2-methyl-1-phenyl acetone.
Further, the auxiliary agent comprises one or more of a defoaming agent, a thickening agent, a polymerization inhibitor, a flatting agent, a dispersing agent and an antibacterial agent.
The invention has the following beneficial effects:
1. the conductive ink prepared by the invention has excellent conductivity, and can be applied to the fields of flexible screens, conductive films, solar cells and the like.
2. The nano silver is adopted to modify the carbon nano tubes, so that the van der Waals effect among the carbon nano tubes is reduced, and the agglomeration of the carbon nano tubes is limited; the modified carbon nano tube has the effect of stably dispersing the nano silver in the components, and inhibits the agglomeration and flocculation of the nano silver.
3. The addition of the nano silver carbon nanotube composite conductive filler improves the conductivity of the ink and improves the comprehensive performance of the ink.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Detailed Description
The invention is further illustrated by the following examples, without thereby limiting the invention to the scope of the described embodiments. 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 method comprises the following specific steps
(1) Acidizing the carbon nano tube:
adding 0.5 part of carbon nano tube into a mixed solution of 13 parts of concentrated nitric acid and 39 parts of concentrated sulfuric acid, and heating and stirring in a water bath at 50-60 ℃ for 2.5 hours; and then washing and centrifuging by using deionized water until the supernatant is neutral, taking the precipitate at the lower layer, placing the precipitate in a vacuum oven at 50 ℃ for drying until the weight is constant, and ultrasonically dispersing in an ethanol solution for later use.
(2) Synthesizing the nano silver carbon nanotube composite conductive filler:
taking 0.8 part of silver nitrate into 50 parts of deionized water to prepare a silver nitrate solution, adding 1.2 parts of polyvinylpyrrolidone, adding 10mL of acidified carbon nanotube ethanol solution, stirring at 40-60 ℃ for 20-30min, and uniformly dispersing to obtain solution A; dissolving 1.5 parts of hydrazine hydrate in 50 parts of deionized water, and marking as liquid B; 5mL of the solution B is dripped into the solution A at a rate of 5 drops per minute, and stirring is continued for 20-50min after dripping is finished; washing with anhydrous ethanol and centrifuging for 3-5 times after stirring, and dispersing the lower layer precipitate in anhydrous ethanol for storage.
(3) Synthesizing the nano silver carbon nanotube composite conductive ink:
adding 15 parts of urethane acrylate, 7 parts of epoxy acrylate, 10 parts of nano silver carbon nanotube composite conductive filler, 50 parts of flaky nano silver and 6 parts of acrylate monomer into a stirring barrel, and stirring for 30-60 minutes at the stirring speed of 700 plus materials and 1000 rpm; transferring the pre-dispersed liquid into a grinder, and grinding for 1-3 times; transferring the ground liquid into a stirring barrel, adding 3 parts of photoinitiator and 2 parts of auxiliary agent, and stirring for 30-60 minutes at the stirring speed of 700-1000rpm to obtain the nano silver-carbon nanotube composite conductive ink.
Example 2
The method comprises the following specific steps
(1) Acidizing the carbon nano tube:
adding 0.7 part of carbon nano tube into a mixed solution of 18 parts of concentrated nitric acid and 54 parts of concentrated sulfuric acid, and heating and stirring in a water bath at 50-60 ℃ for 2.5 hours; and then washing and centrifuging by using deionized water until the supernatant is neutral, taking the precipitate at the lower layer, placing the precipitate in a vacuum oven at 50 ℃ for drying until the weight is constant, and ultrasonically dispersing in an ethanol solution for later use.
(2) Synthesizing the nano silver carbon nanotube composite conductive filler:
taking 1.5 parts of silver nitrate into 50 parts of deionized water to prepare a silver nitrate solution, adding 2 parts of polyvinylpyrrolidone, adding 15mL of acidified carbon nanotube ethanol solution, stirring at 40-60 ℃ for 20-30min, and uniformly dispersing to obtain solution A; dissolving 2.5 parts of hydrazine hydrate in 50 parts of deionized water, and marking as liquid B; dripping 5mL of solution B into solution A at a rate of 6 drops per minute, and stirring for 20-50 min; washing with anhydrous ethanol and centrifuging for 3-5 times after stirring, and dispersing the lower layer precipitate in anhydrous ethanol for storage.
(3) Synthesizing the nano silver carbon nanotube composite conductive ink:
adding 18 parts of urethane acrylate, 7 parts of epoxy acrylate, 12 parts of nano silver carbon nanotube composite conductive filler, 48 parts of flaky nano silver and 7 parts of acrylate monomer into a stirring barrel, and stirring for 30-60 minutes at the stirring speed of 700 plus materials and 1000 rpm; transferring the pre-dispersed liquid into a grinder, and grinding for 1-3 times; transferring the ground liquid into a stirring barrel, adding 2 parts of photoinitiator and 2 parts of auxiliary agent, and stirring for 30-60 minutes at the stirring speed of 700-1000rpm to obtain the nano silver-carbon nanotube composite conductive ink.
Example 3
The method comprises the following specific steps
(1) Acidizing the carbon nano tube:
adding 1 part of carbon nano tube into a mixed solution of 25 parts of concentrated nitric acid and 75 parts of concentrated sulfuric acid, heating in a water bath at 50-60 ℃, and stirring for 2.5 hours; and then washing and centrifuging by using deionized water until the supernatant is neutral, taking the precipitate at the lower layer, placing the precipitate in a vacuum oven at 50 ℃ for drying until the weight is constant, and ultrasonically dispersing in an ethanol solution for later use.
(2) Synthesizing the nano silver carbon nanotube composite conductive filler:
preparing silver nitrate solution by taking 2 parts of silver nitrate in 50 parts of deionized water, adding 2.5 parts of polyvinylpyrrolidone, adding 10mL of acidified carbon nanotube ethanol solution, stirring at 40-60 ℃ for 20-30min, and uniformly dispersing to obtain solution A; dissolving 3.7 parts of hydrazine hydrate in 50 parts of deionized water, and marking as liquid B; 5mL of the solution B is dripped into the solution A at a rate of 7 drops per minute, and stirring is continued for 20-50min after dripping is finished; washing with anhydrous ethanol and centrifuging for 3-5 times after stirring, and dispersing the lower layer precipitate in anhydrous ethanol for storage.
(3) Synthesizing the nano silver carbon nanotube composite conductive ink:
adding 20 parts of urethane acrylate, 7 parts of epoxy acrylate, 8 parts of nano silver carbon nanotube composite conductive filler, 52 parts of flaky nano silver and 6 parts of acrylate monomer into a stirring barrel, and stirring for 30-60 minutes at the stirring speed of 700 plus materials and 1000 rpm; transferring the pre-dispersed liquid into a grinder, and grinding for 1-3 times; transferring the ground liquid into a stirring barrel, adding 3 parts of photoinitiator and 2 parts of auxiliary agent, and stirring for 30-60 minutes at the stirring speed of 700-1000rpm to obtain the nano silver-carbon nanotube composite conductive ink.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A preparation method of nano silver carbon nanotube composite conductive ink is characterized by comprising the following steps:
step 1, introducing polar groups on the surface of a carbon nano tube, and ultrasonically dispersing the polar groups in ethanol to prepare a carbon nano tube ethanol solution;
step 2, reducing and loading the nano silver on the carbon nano tube prepared in the step 1 to prepare the nano silver carbon nano tube conductive composite filler;
and 3, compounding the conductive filler, the flaky nano silver, the polyurethane acrylate, the epoxy acrylate, the acrylate monomer and the auxiliary agent to prepare the nano silver-carbon nanotube composite conductive ink.
2. The method for preparing nano silver carbon nanotube composite conductive ink according to claim 1, wherein the step 1 specifically comprises:
adding carbon nano tubes into mixed acid of concentrated nitric acid and concentrated sulfuric acid, heating in a water bath at 50-60 ℃, and stirring for 2-4 h; then washing and centrifuging by using deionized water until the supernatant is neutral, taking the lower-layer precipitate, placing the precipitate in a vacuum oven at 50 ℃ and drying to constant weight to obtain the ultrasonic wave;
wherein the dosage ratio of the carbon nano tube to the concentrated nitric acid is as follows: (0.5-1): (13-25);
wherein the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid in the mixed acid is 1: 3;
wherein the mass ratio of the carbon nano tube to the ethanol is 1: 20-35.
3. The method for preparing nano silver carbon nanotube composite conductive ink as claimed in claim 1, wherein the polar group comprises hydroxyl group and carboxyl group.
4. The method for preparing nano silver carbon nanotube composite conductive ink as claimed in claim 1, wherein the preparing of nano silver carbon nanotube conductive composite filler comprises:
dissolving 0.5-3 parts of silver nitrate in 50 parts of deionized water to prepare a silver nitrate solution, adding 0.7-3 parts of polyvinylpyrrolidone, adding 10-20mL of acidified carbon nanotube ethanol solution, stirring at 40-60 ℃ for 20-30min, and uniformly dispersing to obtain solution A; dissolving 1.5-4.5 parts of hydrazine hydrate in 50 parts of deionized water, and marking as liquid B; dripping 5-15mL of solution B into solution A at a rate of 5-15 drops per minute, and stirring for 20-50 min; and washing and centrifuging for 3-5 times by using absolute ethyl alcohol after stirring is finished, and drying the sediment at the lower layer until the weight is constant to obtain the nano silver carbon nano tube conductive composite filler.
5. The method for preparing nano silver carbon nanotube composite conductive ink as claimed in claim 1, wherein the step 3 comprises:
adding 10-20 parts of urethane acrylate, 5-10 parts of epoxy acrylate, 5-15 parts of nano silver carbon nanotube composite conductive filler, 45-55 parts of flaky nano silver and 5-10 parts of acrylate monomer into a stirring barrel, and stirring for 30-60 minutes at the stirring speed of 700-; transferring the obtained liquid into a grinding machine, and grinding for 1-3 times; transferring the ground liquid into a stirring barrel, adding 1-5 parts of photoinitiator and 1-5 parts of auxiliary agent, and stirring for 30-60 minutes at the stirring speed of 700-.
6. The method for preparing nano silver carbon nanotube composite conductive ink as claimed in claim 5, wherein the acrylate monomer is selected from one or more of butyl acrylate, methyl methacrylate, styrene, acrylic acid and hydroxyethyl acrylate.
7. The method for preparing nano silver carbon nanotube composite conductive ink as claimed in claim 5, wherein the photoinitiator is selected from one or more of 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, ethyl 2,4, 6-trimethylbenzoylphenylphosphonate, and 2-hydroxy-2-methyl-1-phenylpropanone.
8. The method for preparing nano silver carbon nanotube composite conductive ink according to claim 5, wherein the auxiliary agent comprises one or more of defoaming agent, thickening agent, polymerization inhibitor, leveling agent, dispersing agent and antibacterial agent.
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| CN112375432A (en) * | 2020-11-17 | 2021-02-19 | 安徽理工大学 | Carbon nanotube nano-silver conductive ink |
| CN113105776A (en) * | 2021-04-14 | 2021-07-13 | 深圳清华大学研究院 | Anti-fingerprint antibacterial glass |
| WO2022174244A1 (en) * | 2021-02-11 | 2022-08-18 | Yazaki Corporation | Conductive carbon nanotube-silver composite ink composition |
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