CN111180107A - Preparation method for electric field driven injection of micro-nano 3D printing nano silver paste - Google Patents
Preparation method for electric field driven injection of micro-nano 3D printing nano silver paste Download PDFInfo
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Abstract
The invention provides a preparation method for electric field driven spraying of micro-nano 3D printing nano silver paste, belonging to the technical field of conductive silver paste and micro-nano 3D printing, wherein the nano silver paste is composed of modified nano silver powder, an organic carrier and high polymer resin; the weight ratio of each component is modified nano silver powder: organic carrier: 55-75% of polymer resin: 15-40: 1-10; the organic carrier is composed of an organic solvent, a thickening agent, a plasticizer, a surfactant, a dispersing agent, a flatting agent and an additive, wherein the organic carrier comprises the following components in percentage by weight: thickening agent: plasticizer: surfactant (b): dispersing agent: leveling agent: 60-90% of additive: 2-10: 3-10: 1-8: 1-10: 1-10; 1-10; through modification of the nano silver powder and adjustment of each component, the viscosity of the nano silver powder is matched with that of electric field driven jet micro-nano 3D printing, the manufacturing of the conductive pattern with ultra-fineness, large height-to-width ratio and high performance is realized, the excellent adhesive force and the excellent conductive performance are finally realized, and particularly, the problem of unstable use performance caused by aggregation of the nano silver material is solved.
Description
Technical Field
The invention belongs to the technical field of conductive silver paste and micro-nano 3D printing, and particularly relates to a preparation method for electric field driven spraying of micro-nano 3D printing nano silver paste.
Background
The electric field driven jet micro-nano 3D printing is a brand new micro-nano 3D printing and micro-nano additive manufacturing technology which appears in recent years, utilizes electrohydrodynamic jet and charge induction self-alignment based on a self-excited electrostatic field, combines three printing working modes of pulse cone jet, continuous cone jet and micro-extrusion, realizes high-efficiency and low-cost batch manufacturing of large-area complex three-dimensional micro-nano structures, and particularly has unique advantages and potentials in multi-material multi-scale 3D printing and macro/micro cross-scale 3D printing. The organic electroluminescent material is applied to the fields of flexible electronics, transparent electrodes (conducting films), tissue engineering, biomedical treatment, solar cells, OLEDs, 3D structure electronics, paper-based electronics, micro-nano optics, transparent electric heating, electromagnetic shielding and the like, and shows wide industrial application prospects. Especially, the organic electroluminescent display panel has a huge commercial application prospect in industries such as transparent electrodes, transparent conductive films, flexible electronics, OLEDs, 3D structural electronics and the like. The printing material (nanometer conductive ink) is one of three core process elements (printing equipment, printing material and printing process) of electric field driven jet micro-nano 3D printing, and has decisive influence on the performance (line width, aspect ratio, geometric morphology, electrical performance, optical performance, adhesion performance with a base material and the like) of the printed conductive pattern. At present, various conductive inks such as nano silver paste, nano silver ink, nano silver wire conductive ink, graphene conductive ink, carbon nanotube conductive ink, conductive polymer PEDOT: PSS and the like have been developed in domestic and foreign industrial and academic circles, the existing research results and industrial application prove that the nano silver paste is the most ideal conductive material for electric field driven jet micro-nano 3D printing, however, the existing nano silver paste (ink) mainly faces to the fields such as silk screen printing, aerosol jet printing, ink jet printing, nano imprinting and the like, the performances (rheological property, printing property, physical property and the like) required by the electric field driven jet micro-nano 3D printing are greatly different, and especially the electric field driven jet micro-nano 3D printing has strict requirements on various physicochemical performances (dielectric constant, viscosity, surface tension, silver content, rheological property and the like) of the used nano silver paste, and the optimal process window is also relatively narrow.
In order to solve the problems that the existing nano silver paste is not suitable for electric field driven jet micro-nano 3D printing, especially the silver content is insufficient, the resolution ratio of a printed pattern is low, the adhesion with a substrate is poor, and multilayer printing is difficult, the development of novel nano conductive silver paste suitable for electric field driven jet micro-nano 3D printing is urgently needed, the high-efficiency low-cost manufacturing of high-performance ultra-fine micro-nano conductive patterns based on electric field driven jet micro-nano 3D printing is realized, and the requirements of industrial application (excellent printing performance, high pattern resolution ratio, stable long-time storage, low cost, good environmental protection performance and the like) are met.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method suitable for electric field driven spraying of micro-nano 3D printing nano silver paste, so as to solve the problems that the existing nano silver paste is difficult to meet the requirements of an electric field driven spraying micro-nano 3D printing process, is difficult to realize manufacturing of conductive patterns with ultra-thinness, large height-to-width ratio and high performance, and especially solves the problem that the service performance is unstable due to aggregation of nano silver materials.
In order to solve the technical problems, the first aspect of the invention provides a preparation method for electric field driven injection of micro-nano 3D printing nano silver paste, which comprises the following steps:
a preparation method for electric field driven injection of micro-nano 3D printing nano silver paste is characterized by comprising the following steps: the nano silver paste is composed of modified nano silver powder, an organic carrier and high polymer resin; the weight ratio of each component is modified nano silver powder: organic carrier: 55-75% of polymer resin: 15-40: 1-10;
the organic carrier is composed of an organic solvent, a thickening agent, a plasticizer, a surfactant, a dispersing agent, a flatting agent and an additive, wherein the organic carrier comprises the following components in percentage by weight: thickening agent: plasticizer: surfactant (b): dispersing agent: leveling agent: 60-90% of additive: 2-10: 3-10: 1-8: 1-10: 1-10; 1-10;
the preparation method of the nano silver paste comprises the following steps:
(1) preparing modified nano silver powder: weighing a certain proportion of succinic acid and PVP, respectively dissolving in an ethanol solution to obtain a succinic acid-ethanol solution, and recording the succinic acid-ethanol solution as a solution I and the PVP-ethanol solution as a solution II; weighing corresponding silver powder according to the mass ratio of 1:1 of succinic acid to silver powder, pouring the silver powder into the prepared solution I, placing the solution I on a magnetic stirrer, stirring for 30-60min, standing for layering, and pouring out supernatant; adding the prepared solution II, performing ultrasonic treatment for 30-60min, stirring while performing ultrasonic treatment, centrifuging by using a centrifuge at 3600-4200r/min for 10-20min after the ultrasonic stirring is finished, removing the upper liquid, and drying the silver powder obtained by treatment in a vacuum drying oven at 50-100 ℃;
(2) preparation of organic vehicle: weighing an organic solvent according to a certain proportion, placing the organic solvent in a beaker, weighing a corresponding thickening agent, placing the weighed organic solvent in a constant-temperature water bath kettle for heating in a water bath at 50-80 ℃, simultaneously carrying out mechanical stirring at a stirring speed of 400-600r/min, slowly adding the thickening agent in the stirring process, placing the beaker containing a thickening agent solution in an ultrasonic processor for ultrasonic treatment after the thickening agent is completely dissolved in the organic solvent, and sequentially adding a plasticizer, a surfactant, a dispersing agent, a leveling agent and an additive according to the corresponding component proportion; in the ultrasonic treatment process, simultaneously carrying out mechanical stirring at the stirring speed of 600-800r/min, taking down the beaker after full dissolution, and cooling to obtain a prepared organic carrier;
(3) firstly, weighing modified nano silver powder, an organic carrier and resin according to a proportion, stirring and mixing the organic carrier and the resin, heating to 40-50 ℃, finally slowly adding the modified nano silver powder, carrying out ultrasonic stirring for 100-120min at a constant temperature, and then carrying out ball milling treatment for more than 48 hours by utilizing a ball mill to obtain the nano silver paste.
The organic solvent is one or more of terpineol, ethanol, isopropanol, ethylene glycol, propylene glycol, butyl carbitol, dibasic ester and polyethylene glycol 40000.
The thickening agent is selected from one or more of the following materials: ethyl cellulose, polyacrylate copolymer emulsion, triton X-100, sodium carboxymethylcellulose and methyl cellulose.
The plasticizer is selected from one or more of the following materials: dibutyl phthalate, polyester phthalate, polymethyl methacrylate and polymethyl styrene.
The surfactant is selected from one or more of the following materials: polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, lecithin and span-85.
The dispersing agent is selected from one or more of the following materials: methyl amyl alcohol, sodium hexametaphosphate, sorbitan monooleate and cellulose derivatives.
The leveling agent is selected from one or more of the following materials: furoic acid, terephthalic acid, dimethyl siloxane, ethylene glycol dibutyl ether and modified polysiloxane.
The additive is one or two of a silane coupling agent KH570 and hydrogenated castor oil.
The polymer resin is selected from one or more of the following materials: epoxy resin, acrylic resin, polyurethane resin, polyamide resin, polyester resin, alkyd resin.
Preferably, the organic solvent: thickening agent: plasticizer: surfactant (b): dispersing agent: leveling agent: 75-90% of additive: 6-8: 3-10: 1-8: 1-6: 1-8: 1-8.
The particle size of the nano silver powder is preferably 200-500nm, and more preferably 300 nm.
The second aspect of the invention provides the nano silver paste prepared by the preparation method, wherein the viscosity of the nano silver paste is 30000-60000mPa · s, and the adhesive force of the nano silver paste is 3B-5B.
The third aspect of the invention provides application of the nano silver paste in electric field driven jet micro-nano 3D printing.
The invention has the beneficial effects that:
(1) according to the invention, the silver powder is pretreated in the process of preparing the nano silver paste by adopting the preparation method, namely the surface of the nano silver particles is modified, so that the nano silver particles are kept uniformly dispersed in a liquid phase system for a long time, the stability of the prepared nano silver paste is ensured, and the prepared nano silver paste has good dispersibility and conductivity.
(2) The nano silver paste for the electric field driven injection micro-nano 3D printing, which is prepared by the invention, has excellent printing performance and can be suitable for printing of different substrates (glass, PET and photographic paper).
(3) According to the invention, through the optimization of the component ratio, the nano silver paste has a better leveling state in different stages, and the phenomenon of sedimentation and layering of the nano silver paste caused by solvent volatilization is avoided by combining the optimized selection of preparation parameters.
(4) The preparation method provided by the invention is simple and feasible, economic and environment-friendly, short in production period and low in cost, and meets strict environment-friendly standards.
Drawings
Fig. 1 is a process flow chart of the preparation of the nano silver paste for the electric field driven jet micro-nano 3D printing technology.
Fig. 2 shows the microstructure morphology of the nano silver paste prepared by the invention.
Fig. 3 shows the printing results of different graphic structures of the nano silver paste prepared by the invention in the electric field driving jetting micro-nano 3D printing technology with glass as the substrate.
Fig. 4 shows a line width variable printing result of the nano silver paste prepared by the invention in an electric field driving jetting micro-nano 3D printing technology by using glass as a substrate.
Fig. 5 is a line width variable printing result diagram of the nano silver paste prepared by the invention with PET as a substrate in the electric field driving jetting micro-nano 3D printing technology.
Fig. 6 is a line width variable printing result diagram of the nano silver paste prepared by the invention in an electric field driving jetting micro-nano 3D printing technology by taking photographic paper as a substrate.
Fig. 7 shows the electrical heating performance of the electrodes with different periods of grid structures printed by the nano silver paste prepared by the invention by using the electric field-driven jet micro-nano 3D printing technology and using glass as a substrate.
Detailed Description
The invention will be better understood by reference to the following detailed description of specific embodiments.
Example 1
A nanometer silver paste for an electric field driven jet micro-nano 3D printing technology comprises the following components in parts by weight: 55 wt% of modified nano silver powder, 39 wt% of organic carrier, 3 wt% of polyurethane resin, 3 wt% of epoxy resin and spherical-like silver powder with the particle size of 300 nm.
The preparation process comprises the following steps:
(1) preparing modified nano silver powder: weighing a certain proportion of succinic acid and PVP, respectively dissolving in an ethanol solution to obtain a succinic acid-ethanol solution, and recording the succinic acid-ethanol solution as a solution I and the PVP-ethanol solution as a solution II; weighing corresponding silver powder according to the mass ratio of 1:1 of succinic acid to silver powder, slowly adding the weighed silver powder into the solution I, placing the solution I on a magnetic stirrer to stir for 30min, standing for layering, pouring out supernatant, adding the prepared solution II, performing ultrasonic treatment for 60min, stirring simultaneously in the ultrasonic process, performing centrifugal treatment by using a centrifugal machine after the ultrasonic stirring is completed, rotating speed 4000r/min for 15min to remove supernatant liquid, placing the silver powder obtained by treatment in a vacuum drying oven for drying treatment at 80 ℃, removing redundant solvent, and ensuring that the silver powder is not coagulated into blocks for later use.
And a second process: preparing an organic carrier: the organic carrier comprises the following components in percentage by mass: 54 wt% of terpineol, 20 wt% of ethanol, 400005 wt% of polyethylene glycol, 4 wt% of ethyl cellulose, 6 wt% of dibutyl phthalate, 2 wt% of polyvinylpyrrolidone, 1 wt% of sorbitan monooleate, 1 wt% of dimethyl siloxane, KH5702 wt% of a silane coupling agent and 5 wt% of hydrogenated castor oil.
Weighing organic solvent and ethyl cellulose in proportion, placing the weighed organic solvent in a beaker into a constant temperature water bath kettle, heating in 60 ℃ water bath, simultaneously mechanically stirring at the stirring speed of 500r/min, slowly adding ethyl cellulose in the stirring process, after the ethyl cellulose is completely and fully dissolved in the organic solvent solution, placing the beaker containing the ethyl cellulose solution in an ultrasonic processor for ultrasonic treatment, and sequentially adding dibutyl phthalate, polyvinylpyrrolidone, sorbitan monooleate, dimethyl siloxane, a silane coupling agent KH570 and hydrogenated castor oil according to corresponding component proportions, and in the ultrasonic treatment process, simultaneously carrying out mechanical stirring at the stirring speed of 800r/min to fully dissolve and uniformly mix the mixture in the beaker, taking down the beaker, and cooling to finally obtain the prepared organic carrier.
The third process: the preparation method comprises the steps of firstly weighing modified nano silver powder, an organic carrier, polyurethane resin and epoxy resin according to a proportion, carrying out ultrasonic stirring and mixing on the organic carrier, the polyurethane resin and the epoxy resin, heating to 45 ℃, finally slowly adding the modified nano silver powder, carrying out ultrasonic stirring for 120min at a constant temperature, and carrying out ball milling treatment for 48 hours by using a ball mill to obtain the nano silver paste.
Example 2
The nanometer silver paste for the electric field driven jet micro-nano 3D printing technology comprises the following components in parts by weight: 65 wt% of nano modified silver powder, 27 wt% of organic carrier, 4 wt% of alkyd resin, 4 wt% of epoxy resin and 300nm of silver powder particle size.
The preparation process comprises the following steps:
the first process is as follows: preparing nano modified silver powder: weighing a certain proportion of succinic acid and PVP, respectively dissolving in an ethanol solution to obtain a succinic acid-ethanol solution, and recording the succinic acid-ethanol solution as a solution I and the PVP-ethanol solution as a solution II; weighing corresponding silver powder according to the mass ratio of 1:1 of succinic acid to silver powder, slowly adding the weighed silver powder into the solution I, placing the solution I on a magnetic stirrer to stir for 30min, standing for layering, pouring out supernatant, adding the prepared solution II, performing ultrasonic treatment for 60min, stirring simultaneously in the ultrasonic process, performing centrifugal treatment by using a centrifugal machine after the ultrasonic stirring is completed, rotating speed 4000r/min for 15min to remove supernatant liquid, placing the silver powder obtained by treatment in a vacuum drying oven for drying treatment at 80 ℃, removing redundant solvent, and ensuring that the silver powder is not coagulated into blocks for later use.
And a second process: and (4) preparing an organic carrier. The organic carrier comprises the following components in percentage by mass: 50 wt% of terpineol, 10 wt% of ethylene glycol, 20 wt% of ethanol, 400003 wt% of polyethylene glycol, 5 wt% of ethyl cellulose, 5 wt% of dibutyl phthalate, 2 wt% of polyvinylpyrrolidone, 1 wt% of sorbitan monooleate, 1 wt% of dimethyl siloxane and 3 wt% of hydrogenated castor oil.
Weighing organic solvent and ethyl cellulose in proportion, placing the weighed organic solvent in a beaker into a constant temperature water bath kettle for heating in a 60 ℃ water bath, simultaneously carrying out mechanical stirring at the stirring speed of 500r/mim, slowly adding ethyl cellulose in the stirring process, after the ethyl cellulose is completely and fully dissolved in the organic solvent solution, placing the beaker containing the ethyl cellulose solution in an ultrasonic processor for ultrasonic treatment, and sequentially adding dibutyl phthalate, polyvinylpyrrolidone, sorbitan monooleate, dimethyl siloxane and hydrogenated castor oil according to corresponding component proportion, and in the ultrasonic treatment process, simultaneously carrying out mechanical stirring at the stirring speed of 800r/min to fully dissolve and uniformly mix the mixture in the beaker, taking down the beaker, and cooling to finally obtain the prepared organic carrier.
The third process: the preparation method comprises the steps of firstly weighing modified nano silver powder, an organic carrier, alkyd resin and epoxy resin according to a proportion, carrying out ultrasonic stirring and mixing on the organic carrier, the alkyd resin and the epoxy resin, heating to 45 ℃, finally slowly adding the modified nano silver powder, carrying out ultrasonic stirring for 120min at a constant temperature, and carrying out ball milling treatment for 48 hours by using a ball mill to obtain the nano silver paste.
Example 3
The nanometer silver paste for the electric field driven jet micro-nano 3D printing technology comprises the following components in parts by weight: 75 wt% of silver powder, 19 wt% of organic carrier, 3 wt% of alkyd resin and 3 wt% of epoxy resin, and the silver powder is similar to spherical silver powder with the particle size of 300 nm.
The preparation process comprises the following steps:
the first process is as follows: preparing modified nano silver powder: weighing a certain proportion of succinic acid and PVP, respectively dissolving in an ethanol solution to obtain a succinic acid-ethanol solution, and recording the succinic acid-ethanol solution as a solution I and the PVP-ethanol solution as a solution II; weighing corresponding silver powder according to the mass ratio of 1:1 of succinic acid to silver powder, slowly adding the weighed silver powder into the solution I, placing the solution I on a magnetic stirrer to stir for 30min, standing and layering, pouring out supernatant, pouring the prepared solution II into a beaker of the solution I containing the silver powder, carrying out ultrasonic treatment for 60min, simultaneously stirring in the ultrasonic process, carrying out centrifugal treatment by using a centrifugal machine after the ultrasonic stirring is finished, rotating at the speed of 4000r/min for 15min to remove supernatant liquid, placing the silver powder obtained by treatment in a vacuum drying oven to carry out drying treatment at the temperature of 80 ℃, removing redundant solvent, and ensuring that the silver powder is not coagulated into blocks to be used for later use.
And a second process: preparing an organic carrier: the organic carrier comprises the following components in percentage by mass: 46 wt% of terpineol, 8 wt% of ethylene glycol, 10 wt% of ethanol, 10 wt% of dibasic ester, 400008 wt% of polyethylene glycol, 6 wt% of ethyl cellulose, 6 wt% of triton X-1002 wt%, 4 wt% of dibutyl phthalate, 4 wt% of span-852 wt%, 1 wt% of sorbitan monooleate, 1 wt% of dimethyl siloxane and 1 wt% of silane coupling agent KH5702 wt%.
Weighing an organic solvent and ethyl cellulose according to a proportion, placing the weighed organic solvent in a beaker in a constant-temperature water bath kettle for 60 ℃ water bath heating, simultaneously carrying out mechanical stirring at a stirring speed of 500r/mim, slowly adding the ethyl cellulose and triton X-100 in the stirring process, placing the beaker containing a thickening agent solution in an ultrasonic processor for ultrasonic treatment after the ethyl cellulose and the triton X-100 are fully dissolved in the organic solvent solution, sequentially adding dibutyl phthalate, span-85, sorbitan monooleate, dimethyl siloxane and a silane coupling agent KH570 according to corresponding component proportions, simultaneously carrying out mechanical stirring in the ultrasonic treatment process at a stirring speed of 800r/min so that the mixture in the beaker is fully dissolved and uniformly mixed, taking off the beaker, and finally obtaining the prepared organic carrier after cooling the organic carrier.
The third process: the preparation method comprises the steps of firstly weighing modified nano silver powder, an organic carrier, alkyd resin and epoxy resin according to a proportion, carrying out ultrasonic stirring and mixing on the organic carrier, the alkyd resin and the epoxy resin, heating to 45 ℃, finally slowly adding the modified nano silver powder, carrying out ultrasonic stirring for 120min at a constant temperature, and carrying out ball milling treatment for 48 hours by using a ball mill to obtain the nano silver paste.
Various performance tests were performed on the three types of nano silver pastes prepared above, and the results are shown in table 1.
Table 1 comparison of properties of nano silver paste in different examples
COMSOL Multiphysics numerical simulation analysis is carried out on the formation process of the Taylor cone in the printing process of the prepared nano silver paste, and the simulation result shows that the prepared nano silver paste can form stable Taylor cone jet flow under the action of a self-excitation single potential electric field, other process parameters are kept unchanged under the condition of meeting the stable voltage value of the Taylor cone jet flow, and the moving speed of a printing platform is only changed, so that the printed graph size with excellent appearance quality is obtained.
The nano silver paste prepared by the invention is printed with different patterns on different substrates such as glass, PET and photographic paper by an electric field driving injection micro-nano 3D printing technology, the printed line type and line appearance are good, the preparation of the ultra-fine high-performance conductive pattern with a large height-width ratio can be realized, the problem of unstable service performance caused by easy agglomeration of nano silver materials is solved, and the practicability is very strong.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation method for electric field driven injection of micro-nano 3D printing nano silver paste is characterized by comprising the following steps: the nano silver paste is composed of modified nano silver powder, an organic carrier and high polymer resin; the weight ratio of each component is modified nano silver powder: organic carrier: 55-75% of polymer resin: 15-40: 1-10;
the organic carrier is composed of an organic solvent, a thickening agent, a plasticizer, a surfactant, a dispersing agent, a flatting agent and an additive, wherein the organic carrier comprises the following components in percentage by weight: thickening agent: plasticizer: surfactant (b): dispersing agent: leveling agent: 60-90% of additive: 2-10: 3-10: 1-8: 1-10: 1-10; 1-10;
the preparation method of the nano silver paste comprises the following steps:
(1) preparing modified nano silver powder: weighing a certain proportion of succinic acid and PVP, respectively dissolving in an ethanol solution to obtain a succinic acid-ethanol solution, and recording the succinic acid-ethanol solution as a solution I and the PVP-ethanol solution as a solution II; weighing corresponding silver powder according to the mass ratio of 1:1 of succinic acid to silver powder, pouring the silver powder into the prepared solution I, placing the solution I on a magnetic stirrer, stirring for 30-60min, standing for layering, and pouring out supernatant; adding the prepared solution II, performing ultrasonic treatment for 30-60min, stirring while performing ultrasonic treatment, centrifuging by using a centrifuge at 3600-4200r/min for 10-20min after the ultrasonic stirring is finished, removing the upper liquid, and drying the silver powder obtained by treatment in a vacuum drying oven at 50-100 ℃;
(2) preparation of organic vehicle: weighing an organic solvent according to a certain proportion, placing the organic solvent in a beaker, weighing a corresponding thickening agent, placing the weighed organic solvent in a constant-temperature water bath kettle for heating in a water bath at 50-80 ℃, simultaneously carrying out mechanical stirring at a stirring speed of 400-600r/min, slowly adding the thickening agent in the stirring process, placing the beaker containing a thickening agent solution in an ultrasonic processor for ultrasonic treatment after the thickening agent is completely dissolved in the organic solvent, and sequentially adding a plasticizer, a surfactant, a dispersing agent, a leveling agent and an additive according to the corresponding component proportion; in the ultrasonic treatment process, simultaneously carrying out mechanical stirring at the stirring speed of 600-800r/min, taking down the beaker after full dissolution, and cooling to obtain a prepared organic carrier;
(3) firstly, weighing modified nano silver powder, an organic carrier and resin according to a proportion, stirring and mixing the organic carrier and the resin, heating to 40-50 ℃, finally slowly adding the modified nano silver powder, carrying out ultrasonic stirring for 100-120min at a constant temperature, and then carrying out ball milling treatment for more than 48 hours by utilizing a ball mill to obtain the nano silver paste.
2. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the organic solvent is one or more of terpineol, ethanol, isopropanol, ethylene glycol, propylene glycol, butyl carbitol, dibasic ester and polyethylene glycol 40000.
3. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the thickening agent is selected from one or more of the following materials: ethyl cellulose, polyacrylate copolymer emulsion, triton X-100, sodium carboxymethyl cellulose, and methyl cellulose, preferably at least one of ethyl cellulose and triton X-100.
4. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the plasticizer is selected from one or more of the following materials: dibutyl phthalate, polyester phthalate, polymethyl methacrylate and polymethyl styrene.
5. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the surfactant is selected from one or more of the following materials: polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, lecithin and span-85.
6. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the dispersing agent is selected from one or more of the following materials: methylpentanol, sodium hexametaphosphate, sorbitan monooleate, cellulose derivatives, preferably sorbitan monooleate.
7. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the leveling agent is selected from one or more of the following materials: furoic acid, terephthalic acid, dimethyl siloxane, ethylene glycol dibutyl ether and modified polysiloxane.
8. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the additive is one or two of a silane coupling agent KH570 and hydrogenated castor oil; the polymer resin is selected from one or more of the following materials: epoxy resin, acrylic resin, polyurethane resin, polyamide resin, polyester resin, alkyd resin.
9. The preparation method for the electric field driven spraying of the micro-nano 3D printing nano silver paste according to claim 1 is characterized by comprising the following steps: the particle size of the nano silver powder is preferably 200-500nm, and more preferably 300 nm.
10. The nano silver paste prepared by the preparation method for the electric field driven jet micro-nano 3D printing nano silver paste according to any one of claims 1 to 8 has the viscosity of 30000 to 60000 mPa-s and the adhesive force of 3B to 5B.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111132448A (en) * | 2019-12-30 | 2020-05-08 | 广德新三联电子有限公司 | Silver paste multilayer board for monitoring operation of generator set and preparation process thereof |
| CN112038099A (en) * | 2020-08-27 | 2020-12-04 | 中南大学 | Preparation method of aluminum electrolytic capacitor anode foil based on 3D printing technology |
| CN112275034A (en) * | 2020-09-27 | 2021-01-29 | 华南理工大学 | Electrofluid printing-based silver filter element and preparation method and application thereof |
| CN116230290A (en) * | 2023-03-15 | 2023-06-06 | 西安汇创贵金属新材料研究院有限公司 | Photocuring silver paste for additive manufacturing and preparation method thereof |
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| CN112038099A (en) * | 2020-08-27 | 2020-12-04 | 中南大学 | Preparation method of aluminum electrolytic capacitor anode foil based on 3D printing technology |
| CN112038099B (en) * | 2020-08-27 | 2022-03-01 | 湖南艾华集团股份有限公司 | Preparation method of aluminum electrolytic capacitor anode foil based on 3D printing technology |
| CN112275034A (en) * | 2020-09-27 | 2021-01-29 | 华南理工大学 | Electrofluid printing-based silver filter element and preparation method and application thereof |
| CN112275034B (en) * | 2020-09-27 | 2021-08-10 | 华南理工大学 | Electrofluid printing-based silver filter element and preparation method and application thereof |
| CN116230290A (en) * | 2023-03-15 | 2023-06-06 | 西安汇创贵金属新材料研究院有限公司 | Photocuring silver paste for additive manufacturing and preparation method thereof |
| CN118039460A (en) * | 2024-04-15 | 2024-05-14 | 绵阳新能智造科技有限公司 | Method for thickening silicon wafer |
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