CN110894381A - Preparation method of nano-silver ink - Google Patents
Preparation method of nano-silver ink Download PDFInfo
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- CN110894381A CN110894381A CN201911317148.7A CN201911317148A CN110894381A CN 110894381 A CN110894381 A CN 110894381A CN 201911317148 A CN201911317148 A CN 201911317148A CN 110894381 A CN110894381 A CN 110894381A
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- 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
Abstract
The invention discloses a preparation method of nano-silver ink, which comprises the following steps: uniformly mixing a dispersing agent and a solvent to obtain a solution; and adding nano silver particles until the nano silver particles are uniformly dispersed, adding the tourmaline powder after heat treatment until the nano silver particles are uniformly dispersed, adding a conductive active agent and a conductive activating agent until the conductive active agent and the conductive activating agent are uniformly dispersed, adding a pH regulator, a surface tension regulator and a viscosity regulator until the conductive active agent, the surface tension regulator and the viscosity regulator are uniformly dispersed, and finally adding an adhesive and a defoaming agent until the adhesive and the defoaming agent are uniformly mixed to obtain the nano silver ink. The method assists silver to transmit electrons by adding tourmaline, and the capability of the tourmaline for transmitting electrons can be effectively enhanced by heat treatment and the action of a conductive active agent, so that the conductivity of a wire circuit is improved; the tourmaline and the conductive active agent have good improvement effect on the evaporation of the line solvent, and can effectively prevent the circuit from cracking and forming micropores; the conductive activator has excellent conductivity, and can improve the dispersion stability of ink and enhance the toughness and strength of the circuit.
Description
Technical Field
The invention relates to the field of nano materials and droplet jetting 3D printing, in particular to a preparation method of nano silver ink.
Background
Additive manufacturing technology, also known as 3D printing technology, is a technology for forming three-dimensional solid parts by using CAD software and a numerical control system to build up a special material layer by layer and cure it layer by layer. Droplet ejection is also a technique and method in 3D printing, which is a non-contact, non-pressure, non-plate digital formation technique. With the rapid development of electronic products in the direction of ultra-light weight, high flexibility and low resistance, the traditional printing mode can not meet the current requirements. Compared with the traditional printing mode, the droplet ejection method has the advantages of high material utilization rate, short manufacturing period, high processing flexibility and the like, is applied to the fields of radio frequency tags, flexible display devices, solar cells, printed circuit boards, sensors and the like at present, and has very wide application prospects.
The conductive ink as a key material of the conductive pattern is a bottleneck in the development of printed electronic technology, and directly influences the performance and quality of electronic products. The current research on nano conductive ink technology has made a lot of progress, but there are some limitations in some aspects. The document of application No. 201810448265.6 discloses a conductive ink and a method for preparing the same, in which nanocellulose is added to a carbon material conductive ink to enable good dispersion of the ink and improve film forming property, but the ink does not provide a solution pH condition, and an acid-base environment has different influences on solution components, a nozzle and a substrate. The document of application No. 201410751794.5 discloses a method for preparing a nano silver conductive ink for inkjet printing, which uses hydroxycellulose as a stabilizer and a binder, and the prepared silver nanoparticle dispersion liquid is distilled under reduced pressure to control the silver content, but the process is difficult to control precisely, the process is complicated, and the operation is difficult. The document of application No. 201710559121.3 discloses a method for preparing conductive silver ink, which uses nano tourmaline as ink pH regulator to effectively improve the stability of ink and increase silver content, but does not use conductive activator and conductive activator to enhance the conductive property, nor does it describe the mechanical properties of the circuit.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of nano-silver ink.
The technical scheme for solving the technical problem is to provide a preparation method of nano-silver ink, which is characterized by comprising the following steps:
1) preparation of the solution: uniformly mixing 0.1-0.5 part by mass of a dispersant and 10-20 parts by mass of a solvent to obtain a solution;
2) preparation of silver ink aqueous dispersion: mixing 1-20 parts by mass of nano silver particles with the solution obtained in the step 1) until the nano silver particles are uniformly dispersed to obtain a silver ink aqueous dispersion;
3) preparing mixed conductive ink: performing heat treatment on 0.1-1 part by mass of tourmaline powder at the temperature of 700-900 ℃ for 10-120min, and mixing with the silver ink aqueous dispersion obtained in the step 2) until the tourmaline powder is uniformly dispersed to obtain mixed conductive ink;
4) preparing nano silver ink: adding 0.01-5 parts by mass of conductive active agent and 0.01-5 parts by mass of conductive activating agent into the mixed conductive ink obtained in the step 3) to uniformly disperse the conductive active agent and the conductive activating agent; then adding 0.05-5 parts by mass of pH regulator, 0.1-1 part by mass of surface tension regulator and 0.1-1.5 part by mass of viscosity regulator, and mixing uniformly; and finally, adding 0.01-0.5 part by mass of adhesive and 0.01-0.5 part by mass of defoaming agent, and uniformly mixing to obtain the nano silver ink.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method assists silver to transmit electrons by adding tourmaline, and the capability of the tourmaline for transmitting electrons can be effectively enhanced by heat treatment and the action of a conductive active agent, so that the conductivity of a wire circuit is improved; the tourmaline and the conductive active agent have good improvement effect on the evaporation of the line solvent, and can effectively prevent the circuit from cracking and forming micropores; the conductive activator has excellent conductivity, and can improve the dispersion stability of ink and enhance the toughness and strength of the circuit.
(2) The volume of the tourmaline unit cell after heat treatment is spontaneously reduced, the center of the crystal structure is relatively displaced, and the inherent electric dipole moment is increased, so that the electric polarity is enhanced; the heat treatment also enhances the capability of the tourmaline in a permanent electric field, can absorb and release charges more quickly, and better assists the electron transmission among the nano silver, thereby improving the conductivity.
(3) The conductive active agent can enhance the ability of the tourmaline to absorb and release electrons, improve the far infrared ray radiation performance of the tourmaline, and avoid the problems of cracking, porosity, uneven surface and the like in the process of circuit evaporation. In view of the characteristics of excellent conductivity, good strength and toughness and a nanosheet structure of graphene, the graphene is selected as a conductive activator, so that the bending strength of the conductive circuit can be increased, the flexibility of the conductive wire is improved and the fracture phenomenon is not easy to occur under the condition that the conductive circuit meets high conductivity.
(4) The pH regulator is added to regulate the pH of the solution, so that the influence of acid-base environment on the components of the solution, the spray head and the substrate is overcome.
(5) The method has the advantages of simple process, stability, easy control, no involvement of any complex equipment, good stability of the ink prepared at room temperature, long preservation time and low curing temperature.
Detailed Description
Specific examples of the present invention are given below. The specific examples are only intended to illustrate the invention in further detail and do not limit the scope of protection of the claims of the present application.
The invention provides a preparation method (method for short) of nano-silver ink, which is characterized by comprising the following steps:
1) preparation of the solution: adding 0.1-0.5 part by mass of a dispersing agent into 10-20 parts by mass of a solvent, and stirring for 3-5min by using a glass rod or a magnetic stirrer until the dispersing agent and the solvent are fully and uniformly mixed to obtain a solution;
in the step 1), the dispersant is at least one of polyvinylpyrrolidone, sodium citrate, polyvinyl alcohol, glycerol, polyamide, dodecylamine, sodium polyacrylate, potassium tripolyphosphate or potassium pyrophosphate.
In the step 1), the solvent is at least one of deionized water, methanol, ethanol, isopropanol, propanol, n-propanol, isobutanol, butanol, n-hexanol, ethylene glycol, acetone, toluene or xylene.
2) Preparation of silver ink aqueous dispersion: under the condition of ultrasonic dispersion, adding 1-20 parts by mass of nano silver particles into the solution obtained in the step 1), and performing ultrasonic oscillation for 30-60min until the nano silver particles are uniformly dispersed to obtain a silver ink aqueous dispersion;
in the step 2), the nano silver particles are sphere-like nano silver particles, and the particle size is 20-1000 nm.
3) Preparing mixed conductive ink: performing heat treatment on 0.1-1 part by mass of tourmaline powder at the temperature of 700-900 ℃ for 10-120min, and then adding the tourmaline powder into the silver ink dispersion liquid obtained in the step 2) to perform ultrasonic oscillation for 10-30min until the tourmaline powder is uniformly dispersed to obtain mixed conductive ink;
in the step 3), the tourmaline powder is nano tourmaline particles with the particle size of 10-2000 nm; the tourmaline is at least one of lithium tourmaline, schorl, dravite, chromium-magnesium tourmaline, bragmelin, iron-magnesium tourmaline, rock-magnesium tourmaline, calcium-lithium tourmaline, calcium-magnesium tourmaline, alkali-free lithium tourmaline or alkali-free iron tourmaline.
4) Preparing nano silver ink: adding 0.01-5 parts by mass of conductive active agent and 0.01-5 parts by mass of conductive activating agent into the mixed conductive ink obtained in the step 3), so that the conductive active agent and the conductive activating agent are fully and uniformly dispersed; according to the requirement of droplet spraying, sequentially adding 0.05-5 parts by mass of pH regulator, 0.1-1 part by mass of surface tension regulator and 0.1-1.5 part by mass of viscosity regulator, stirring for 5-10min until uniformly mixing, and controlling the pH value to be 7-9, the surface tension to be 28-32mN/m and the viscosity to be 5-15 mP.s; and finally, sequentially adding 0.01-0.5 part by mass of the adhesive and 0.01-0.5 part by mass of the defoaming agent, and carrying out ultrasonic oscillation for 3-5min until the mixture is uniformly mixed to obtain the nano-silver ink.
In the step 4), the conductive active agent is at least one of cerium oxide, cerium hydroxide, titanium oxide, titanium hydroxide, praseodymium oxide, praseodymium hydroxide, germanium oxide or germanium hydroxide, and cerium oxide or titanium dioxide is preferred.
In the step 4), the conductive activating agent is a graphene material and is selected from at least one of single-layer graphene, double-layer graphene, multi-layer graphene, graphene oxide, reduced graphene oxide or modified graphene; the radial size of the graphene sheet layer is 0.5-3 mu m, and the thickness is 0.5-10 nm.
In the step 4), the pH regulator is at least one of hydrochloric acid, acetic acid, ammonia water or ethanolamine.
In the step 4), the surface tension regulator is at least one of polyacrylamide, polyacrylate, sodium dodecyl sulfate or triethanolamine.
In the step 4), the viscosity regulator is at least one of glycerol, terpineol or methyl nylon acid.
In the step 4), the defoaming agent is at least one of diethyl ethanol, isooctyl alcohol or isoamyl alcohol.
In the step 4), the adhesive is at least one of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, acrylic resin, polyvinyl alcohol, phenolic resin, acrylic resin, epoxy resin, alkyd resin, polyester resin or polyurethane resin.
Example 1
1) Preparation of the solution: adding 1g of polyvinylpyrrolidone into 50g of deionized water, and stirring for 5min by using a magnetic stirrer until the polyvinylpyrrolidone and the deionized water are fully and uniformly mixed to obtain a solution;
2) preparation of silver ink aqueous dispersion: under the condition of ultrasonic dispersion, adding 10g of nano silver powder with the particle size of 50nm into the solution obtained in the step 1), and uniformly dispersing by ultrasonic oscillation for 40min to obtain a silver ink aqueous dispersion;
3) preparing mixed conductive ink: carrying out heat treatment on 1g of black tourmaline powder with the particle size of 30nm at the temperature of 700 ℃ for 20min, and then adding the black tourmaline powder into the silver ink dispersion liquid obtained in the step 2) to carry out ultrasonic oscillation for 30min to uniformly disperse the black tourmaline powder and the silver ink dispersion liquid to obtain mixed conductive ink;
4) preparing nano silver ink: adding 0.01g of cerium oxide and 0.1g of graphene into the mixed conductive ink obtained in the step 3), so that the cerium oxide and the graphene are fully and uniformly dispersed; according to the requirement of droplet spraying, 0.05g of ammonia water, 0.2 g of polyacrylamide and 0.5g of terpineol are added into the mixture in sequence, the mixture is stirred for 10min until the mixture is uniformly mixed, the pH value is controlled to be 8, the surface tension is 30.1mN/m, and the viscosity is 8.9mP & s; and finally, sequentially adding 0.1g of hydroxymethyl cellulose and 0.05g of isooctanol, and carrying out ultrasonic oscillation for 5min until the mixture is uniformly mixed to obtain the nano-silver ink.
The nano silver ink can be stored for more than 120 days at normal temperature. Compared with the common ink, the conductivity of the ink printed into a conductive circuit on the flexible substrate (sintered and formed after heat treatment at 180 ℃ for 30 min) is improved by 35%. The flexible substrate with the conductive circuit is bent to be nearly 90 degrees and repeated for 500 times, the conductivity change rate of the ink is 12 percent lower than that of the common ink, and therefore the bending resistance is improved by 12 percent.
The conductivity of the ink is characterized by the reciprocal of resistivity, the resistivity is obtained by a four-point probe method and a voltammetry method, and a four-probe resistance tester and a digital multimeter are adopted as experimental instruments.
Example 2
1) Preparation of the solution: adding 1g of sodium citrate into a mixed solvent of 20g of deionized water and 30g of ethanol, and stirring for 5min by using a magnetic stirrer until the sodium citrate and the mixed solvent are fully and uniformly mixed to obtain a solution;
2) preparation of silver ink aqueous dispersion: under the condition of ultrasonic dispersion, adding 10g of nano silver powder with the particle size of 50nm into the solution obtained in the step 1), and uniformly dispersing by ultrasonic oscillation for 40min to obtain a silver ink aqueous dispersion;
3) preparing mixed conductive ink: carrying out heat treatment on 1g of magnesium tourmaline powder with the particle size of 30nm for 20min at the temperature of 700 ℃, adding the magnesium tourmaline powder into the silver ink dispersion liquid obtained in the step 2), and carrying out ultrasonic oscillation for 30min to uniformly disperse the magnesium tourmaline powder to obtain mixed conductive ink;
4) preparing nano silver ink: adding 0.01g of cerium oxide and 0.1g of graphene into the mixed conductive ink obtained in the step 3), so that the cerium oxide and the graphene are fully and uniformly dispersed; according to the requirement of droplet spraying, 0.05g of ammonia water, 0.2 g of polyacrylamide and 0.5g of terpineol are added into the mixture in sequence, the mixture is stirred for 10min until the mixture is uniformly mixed, the pH value is controlled to be 8, the surface tension is 29.2mN/m, and the viscosity is 6.3mP & s; and finally, sequentially adding 0.1g of hydroxymethyl cellulose and 0.05g of isooctanol, and carrying out ultrasonic oscillation for 5min until the mixture is uniformly mixed to obtain the nano-silver ink.
The nano silver ink can be stored for more than 100 days at normal temperature. Compared with the common ink, the conductivity of the ink printed into the conductive circuit on the flexible substrate is improved by 38%. The flexible substrate with the conductive circuit is bent to be nearly 90 degrees and repeated for 500 times, the conductivity change rate of the ink is 16 percent lower than that of the common ink, and therefore the bending resistance is improved by 16 percent.
Example 3
1) Preparation of the solution: adding 1g of polyvinylpyrrolidone into 50g of ethanol, and stirring for 5min by using a magnetic stirrer until the polyvinylpyrrolidone and the ethanol are fully and uniformly mixed to obtain a solution;
2) preparation of silver ink aqueous dispersion: under the condition of ultrasonic dispersion, adding 10g of nano silver powder with the particle size of 30nm into the solution obtained in the step 1), and uniformly dispersing by ultrasonic oscillation for 40min to obtain a silver ink aqueous dispersion;
3) preparing mixed conductive ink: carrying out heat treatment on 1g of lithium tourmaline powder with the particle size of 30nm for 20min at the temperature of 750 ℃, adding the lithium tourmaline powder into the silver ink dispersion liquid obtained in the step 2), and carrying out ultrasonic oscillation for 30min to uniformly disperse the lithium tourmaline powder to obtain mixed conductive ink;
4) preparing nano silver ink: adding 0.01g of cerium oxide and 0.1g of graphene into the mixed conductive ink obtained in the step 3), so that the cerium oxide and the graphene are fully and uniformly dispersed; according to the requirement of droplet spraying, 0.05g of ammonia water, 0.2 g of polyacrylamide and 0.5g of terpineol are added into the mixture in sequence, the mixture is stirred for 10min until the mixture is uniformly mixed, the pH value is controlled to be 8, the surface tension is 29.6mN/m, and the viscosity is 5.3mP & s; and finally, sequentially adding 0.1g of hydroxymethyl cellulose and 0.05g of isooctanol, and carrying out ultrasonic oscillation for 5min until the mixture is uniformly mixed to obtain the nano-silver ink.
The nano silver ink can be stored for more than 60 days at normal temperature. Compared with the common ink, the conductivity of the conductive circuit printed on the flexible substrate by the ink is improved by 41%. The flexible substrate with the conductive circuit is bent to be nearly 90 degrees and repeated for 500 times, the conductivity change rate of the ink is 18 percent lower than that of the common ink, and therefore the bending resistance is improved by 18 percent.
Example 4
1) Preparation of the solution: adding 1g of polyvinyl alcohol into a mixed solvent of 30g of methanol and 20g of ethanol, and stirring for 5min by using a magnetic stirrer until the polyvinyl alcohol and the mixed solvent are fully and uniformly mixed to obtain a solution;
2) preparation of silver ink aqueous dispersion: under the condition of ultrasonic dispersion, adding 10g of nano silver powder with the particle size of 50nm into the solution obtained in the step 1), and uniformly dispersing by ultrasonic oscillation for 40min to obtain a silver ink aqueous dispersion;
3) preparing mixed conductive ink: carrying out heat treatment on 1g of chromium-magnesium tourmaline powder with the particle size of 30nm at the temperature of 800 ℃ for 20min, and then adding the chromium-magnesium tourmaline powder into the silver ink dispersion liquid obtained in the step 2) to carry out ultrasonic oscillation for 30min to uniformly disperse the mixture to obtain mixed conductive ink;
4) preparing nano silver ink: adding 0.01g of cerium oxide and 0.1g of graphene into the mixed conductive ink obtained in the step 3), so that the cerium oxide and the graphene are fully and uniformly dispersed; according to the requirement of droplet spraying, 0.05g of ammonia water, 0.2 g of polyacrylamide and 0.5g of terpineol are added into the mixture in sequence, the mixture is stirred for 10min until the mixture is uniformly mixed, the pH value is controlled to be 8, the surface tension is 28.9mN/m, and the viscosity is 7.8mP & s; and finally, sequentially adding 0.1g of acrylic resin and 0.05g of isooctanol, and carrying out ultrasonic oscillation for 5min until the mixture is uniformly mixed to obtain the nano-silver ink.
The nano silver ink can be stored for more than 180 days at normal temperature. Compared with the common ink, the conductivity of the conductive circuit printed on the flexible substrate by the ink is improved by 30%. The flexible substrate with the conductive circuit is bent to be nearly 90 degrees and repeated for 500 times, the conductivity change rate of the ink is 15 percent lower than that of the common ink, and therefore the bending resistance is improved by 15 percent.
Nothing in this specification is said to apply to the prior art.
Claims (10)
1. A preparation method of nano-silver ink is characterized by comprising the following steps:
1) preparation of the solution: uniformly mixing 0.1-0.5 part by mass of a dispersant and 10-20 parts by mass of a solvent to obtain a solution;
2) preparation of silver ink aqueous dispersion: mixing 1-20 parts by mass of nano silver particles with the solution obtained in the step 1) until the nano silver particles are uniformly dispersed to obtain a silver ink aqueous dispersion;
3) preparing mixed conductive ink: performing heat treatment on 0.1-1 part by mass of tourmaline powder at the temperature of 700-900 ℃ for 10-120min, and mixing with the silver ink aqueous dispersion obtained in the step 2) until the tourmaline powder is uniformly dispersed to obtain mixed conductive ink;
4) preparing nano silver ink: adding 0.01-5 parts by mass of conductive active agent and 0.01-5 parts by mass of conductive activating agent into the mixed conductive ink obtained in the step 3) to uniformly disperse the conductive active agent and the conductive activating agent; then adding 0.05-5 parts by mass of pH regulator, 0.1-1 part by mass of surface tension regulator and 0.1-1.5 part by mass of viscosity regulator, and mixing uniformly; and finally, adding 0.01-0.5 part by mass of adhesive and 0.01-0.5 part by mass of defoaming agent, and uniformly mixing to obtain the nano silver ink.
2. The method of claim 1, wherein in the step 1), the dispersant is at least one of polyvinylpyrrolidone, sodium citrate, polyvinyl alcohol, glycerol, polyamide, dodecylamine, sodium polyacrylate, potassium tripolyphosphate, and potassium pyrophosphate.
3. The method for preparing nano silver ink according to claim 1, wherein in the step 1), the solvent is at least one of deionized water, methanol, ethanol, isopropanol, propanol, n-propanol, isobutanol, butanol, n-hexanol, ethylene glycol, acetone, toluene or xylene.
4. The method for preparing nano silver ink according to claim 1, wherein in the step 2), the nano silver particles are sphere-like nano silver particles, and the particle size is 20-1000 nm.
5. The method for preparing nano-silver ink according to claim 1, wherein in the step 3), the tourmaline powder is tourmaline with a particle size of 10-2000 nm; the tourmaline is at least one of lithium tourmaline, schorl, dravite, chromium-magnesium tourmaline, bragmelin, iron-magnesium tourmaline, rock-magnesium tourmaline, calcium-lithium tourmaline, calcium-magnesium tourmaline, alkali-free lithium tourmaline or alkali-free iron tourmaline.
6. The method for preparing nano silver ink according to claim 1, wherein 0.05 to 5 parts by mass of the pH adjusting agent, 0.1 to 1 part by mass of the surface tension adjusting agent, and 0.1 to 1.5 parts by mass of the viscosity adjusting agent are sequentially added in step 4) to be uniformly mixed, and the pH value is controlled to be 7 to 9, the surface tension is 28 to 32mN/m, and the viscosity is controlled to be 5 to 15mP · s.
7. The method for preparing nano silver ink according to claim 1, wherein in the step 4), 0.01 to 0.5 parts by mass of the binder and 0.01 to 0.5 parts by mass of the defoaming agent are added in sequence until the mixture is uniformly mixed.
8. The method for preparing nano silver ink according to claim 1, wherein in the step 4), the conductive active agent is at least one of cerium oxide, cerium hydroxide, titanium oxide, titanium hydroxide, praseodymium oxide, praseodymium hydroxide, germanium oxide or germanium hydroxide; the conductive activator is graphene, the radial size of a graphene sheet layer is 0.5-3 mu m, and the thickness of the graphene sheet layer is 0.5-10 nm.
9. The method for preparing nano silver ink according to claim 1, wherein in the step 4), the pH regulator is at least one of hydrochloric acid, acetic acid, ammonia water or ethanolamine; the surface tension regulator is at least one of polyacrylamide, polyacrylate, sodium dodecyl sulfate or triethanolamine; the viscosity regulator is at least one of glycerol, terpineol or methyl nylon acid.
10. The method for preparing nano silver ink according to claim 1, wherein in the step 4), the binder is at least one of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, acrylic resin, polyvinyl alcohol, phenolic resin, acrylic resin, epoxy resin, alkyd resin, polyester resin or polyurethane resin; the defoaming agent is at least one of diethyl ethanol, isooctyl alcohol or isoamyl alcohol.
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