CN110875100A - Nano silver wire conductive ink sintered film based on sodium chloride hot-pressing sintering and preparation method and application thereof - Google Patents
Nano silver wire conductive ink sintered film based on sodium chloride hot-pressing sintering and preparation method and application thereof Download PDFInfo
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- CN110875100A CN110875100A CN201810991885.4A CN201810991885A CN110875100A CN 110875100 A CN110875100 A CN 110875100A CN 201810991885 A CN201810991885 A CN 201810991885A CN 110875100 A CN110875100 A CN 110875100A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/006—Thin film resistors
Abstract
The invention discloses a method for sintering a nano silver wire at a low temperature, which comprises the steps of preparing the nano silver wire with a large length-diameter ratio, preparing isopropanol conductive ink for the nano silver wire, dispersing the nano silver wire in an isopropanol solvent, and ultrasonically dispersing to prepare the nano silver wire conductive ink with the silver content of 3 g/L. The mixture is injected into a clean pen core by a syringe, and a square resistor is coated on the Epson photographic paper. Firstly, NaCl solution is adopted for chemical sintering, then the mixture is placed on a sintering table, and hot-pressed sintering is carried out for 30min at the temperature of 150 ℃ and under the pressure of 3.0 x 104 Pa. The resistance values of all the square resistors were measured by a four-probe resistance measurement method. According to the invention, the nano silver wire conductive ink is subjected to low-temperature NaCl-hot pressing sintering, the optimal technological parameters of the low-temperature sintering of the nano silver wire are explored, so that the defects of high sintering temperature and serious damage to the substrate of the traditional thermal sintering nano silver wire conductive ink are overcome, and the technological parameters of the nano silver wire conductive ink which is low in sintering temperature, short in sintering temperature and excellent in conductivity after sintering are set.
Description
Technical Field
The invention relates to the technical field of conductive materials, in particular to a nano silver wire conductive ink sintered film based on sodium chloride hot-pressing sintering and a preparation method and application thereof.
Background
The rapid development of technology and the continuous improvement of human living standards have promoted the development of electronic display devices. The development of electronic touch screens in electronic displays and the appearance of transparent conductive films have led us to enter a new electronic technology era. The performance of the transparent conductive film, which is used as a key link of all products in the display field, directly affects the efficacy of the final product. Among them, flexible electronic devices are one of the directions in which electronic devices will be developed in the future, and therefore, excellent flexible conductive films are required. The nano silver wire has better mechanical stability, no toxicity and low cost, and can be subjected to roll-to-roll continuous production, so that the nano silver wire becomes a preferred material for replacing the traditional Indium Tin Oxide (ITO). The conductivity of the conductive film of the nano silver wires can be influenced by the node resistance among the nano silver wires, and the sintering of the nano silver wires with the length of 20-40 mu m is carried out, so that the node resistance is reduced, and the conductivity of the conductive film is improved.
To achieve the above object, firstly, a nano silver wire conductive ink with better performance is prepared, and the obtained conductive ink is sintered. In the traditional thermal sintering of the nano silver wire, because PVP organic matter is attached to the surface of the nano silver wire, the PVP attached to the surface of the nano silver wire is removed in the process of heating, so that the nano silver wire is lapped, and the resistance of the conductive film is reduced. When the temperature rises, the ends of the nano silver wires are sintered, and effective conductive paths are formed among the nano silver wires. However, the sintering requires a high temperature, which may damage the substrate of the conductive film and reduce the mechanical properties of the film.
Disclosure of Invention
The invention aims to provide a nano silver wire conductive ink sintered film based on sodium chloride hot-pressing sintering and a preparation method and application thereof, wherein NaCl-hot-pressing sintering is used for replacing hot sintering, NaCl is used for carrying out chemical sintering, organic matters on the surface of a nano silver wire are removed, pressure is applied, and added load is increased, so that the sintering driving force of the nano silver wire is increased, the sintering temperature of the nano silver wire is reduced, the conductivity of the film is improved, the damage to the film substrate is reduced, the nano silver wire can obtain a better silver wire joint at a low temperature, the node resistance between the nano silver wires is reduced, the conductivity of the nano silver wire film is improved, and the mechanical property of the film substrate is reserved.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a nano silver wire conductive ink sintered film is prepared according to the following method:
step 1, dispersing the nano silver wires in isopropanol to obtain nano silver wire ink with the concentration of the nano silver wires being 3-6 g/L;
step 2, writing the nano silver wire ink on Epson photographic paper to obtain a square resistor;
step 3, soaking the square resistor in 0.5-2.0mol/L NaCl solution for 20-40min, then rinsing with distilled water to remove residual NaCl, and drying;
step 4, drying the square resistor at 160 ℃ of 140 DEG to 2.5-3.5 × 104And (3) carrying out hot-pressing sintering for 20-40min under the Pa condition to obtain the nano silver wire conductive ink sintered film.
In the technical scheme, the drying mode in the step 3 is to blow the fabric at the temperature of 30-50 ℃ by using a blower.
In the technical scheme, the nano silver wire is prepared by a polyol method, and specifically comprises the following steps:
adding 1.2-1.5g PVP-K30 to 0.13-0.18mmol/L FeCl3Uniformly dispersing in ethylene glycol solution to obtain PVP-FeCl3-ethylene glycol solution to the PVP-FeCl340-60ml of AgNO prepared by adding 0.13-0.19mol/L of AgNO dropwise into the ethylene glycol solution3After the ethylene glycol solution is uniformly dispersed, the reaction system reacts for 2-3h at the temperature of 130-170 ℃, after the reaction is finished, the reaction system is naturally cooled to the room temperature of 20-25 ℃, and then acetone and absolute ethyl alcohol are used for washing, so that the nano silver wire is obtained.
In the technical scheme, the concentration of the NaCl solution in the step 3 is 1.0 mol/L.
In the above technical solution, the temperature of the hot pressing sintering in the step 4 is 150 ℃, and the pressure is 3.0 × 104Pa, time 30 min.
In another aspect of the present invention, the method for preparing the nano silver wire conductive ink sintered film comprises the following steps:
step 1, dispersing the nano silver wires in isopropanol to obtain nano silver wire ink with the concentration of the nano silver wires being 3-6 g/L;
step 2, writing the nano silver wire ink on Epson photographic paper to obtain a square resistor;
step 3, soaking the square resistor in 0.5-2.0mol/L NaCl solution for 20-40min, then rinsing with distilled water to remove residual NaCl, and drying;
step 4, drying the square resistor at 160 ℃ of 140 DEG to 2.5-3.5 × 104And (3) carrying out hot-pressing sintering for 20-40min under the Pa condition to obtain the nano silver wire conductive ink sintered film.
In the technical scheme, the nano silver wire is prepared by a polyol method, and specifically comprises the following steps:
adding 1.2-1.5g PVP-K30 to 0.13-0.18mmol/L FeCl3Uniformly dispersing in ethylene glycol solution to obtain PVP-FeCl3-ethylene glycol solution to the PVP-FeCl340-60ml of AgNO prepared by adding 0.13-0.19mol/L of AgNO dropwise into the ethylene glycol solution3Glycol solution of (2), dispersingAnd after the reaction is uniform, reacting the reaction system for 2-3h at the temperature of 130-170 ℃, naturally cooling to the room temperature of 20-25 ℃ after the reaction is finished, and then washing by using acetone and absolute ethyl alcohol to obtain the nano silver wire.
In the above technical solution, the concentration of the NaCl solution in the step 3 is 1.0mol/L, the temperature of the hot pressing sintering in the step 4 is 150 ℃, and the pressure is 3.0 × 104Pa, time 30 min.
In another aspect of the invention, the application of the nano silver wire conductive ink sintered film in a flexible resistor is also included, and the resistance of the sintered film is 0.7-0.9 Ω/sq.
In the above technical scheme, when the concentration of NaCl in the step 3 is 1.0mol/L and the temperature of the hot-pressing sintering in the step 4 is 150 ℃, the pressure is 3.0 multiplied by 104When Pa and time are 30min, the resistance of the nano silver wire conductive ink sintering film is 0.8 omega/sq.
Compared with the prior art, the invention has the beneficial effects that:
1. the sintering driving force of the nano silver wire is increased by using an external load, and the sintering temperature of the nano silver wire is reduced, so that the nano silver wire can be connected at a low temperature, and the damage to a film substrate caused by the high temperature required by the thermal sintering of the nano silver wire is compensated. Finally, under proper pressure, the sintering process of the nano silver wire conductive ink with low sintering temperature, good contact and good conductivity after sintering is obtained.
2. The NaCl is used for cleaning, organic matters on the surface of the nano silver wire can be removed, the NaCl plays a role in chemical sintering, the PVP content on the surface of the nano silver wire is reduced, the contact between the nano silver wires is facilitated, and the sintering temperature of the nano silver wire is reduced.
Drawings
FIG. 1 is an SEM image of a silver nanowire conductive ink of comparative example 1 after direct writing and conventional thermal sintering;
FIG. 2 shows the conductive ink of silver nanowire of comparative example 2, which is directly written at 150 deg.C and 3.0 × 104SEM picture after Pa hot pressing sintering;
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preparing nano silver wire ink:
1. 13mg of FeCl was weighed using a precision balance3Adding into 50ml of ethylene glycol solution to prepare FeCl with the concentration of 0.16mmol/L3-a glycol solution.
2. 1.39g of PVP-K30 was weighed and added to FeCl under magnetic stirring3In ethylene glycol solution to obtain PVP-FeCl with PVP concentration of 0.25mol/L3And (3) ethylene glycol solution.
3. 0.85g of silver nitrate is weighed by a precision balance and added into 50ml of ethylene glycol under the action of magnetic stirring to obtain 0.1mol/L AgNO3-a glycol solution.
4. AgNO is added under the condition of magnetic stirring3Adding the ethylene glycol solution into the PVP-FeCl 3-ethylene glycol solution in a syringe or a rubber head dropper within 1min, and magnetically stirring for 15 min.
5. The final solution was poured into the reaction kettle and oil-bathed at 160 ℃ for 2.5 h.
6. After the reaction is finished, the solution is naturally cooled, the reaction solution is transferred to a centrifugal tube, acetone which is 5-10 times of the reaction solution is added, the mixture is ultrasonically stirred uniformly, then the mixture is centrifuged at the rotating speed of 3000rpm, supernatant liquid is removed, and then absolute ethyl alcohol is used for ultrasonic centrifugal washing. The above centrifugation washing was repeated 3 times.
7. And dispersing the obtained final precipitate in anhydrous isopropanol to obtain 3g/L of nano silver wire ink.
Comparative example 1
The square resistance is obtained by the method of straight writing by using the nano silver wire ink.
Controlling the sintering table, controlling the sintering temperature at 150 ℃ respectively, and heating the square resistor at 150 ℃ for 30 min. Finally obtaining the sintered nano silver wire film, and measuring the resistance of the film by a four-probe method to be 2.23 omega/sq.
Comparative example 2
The square resistance is obtained by the method of straight writing by using the nano silver wire ink.
The temperature of the sintering table was controlled to 150 ℃ and 3.0X 10 square resistance was applied4And applying an external load of Pa, and performing hot-pressing sintering for 30 min. Finally obtaining the sintered nano silver wire film, and measuring the resistance of the film by a four-point probe method to be 1.6 omega/sq.
Example 1
1. NaCl solutions with the concentrations of 0.5mol/L, 1.0mol/L and 2.0mol/L are respectively prepared;
2. soaking the dried square resistors in NaCl solutions with different concentrations for 30min respectively;
3. rinsing the soaked square resistor with distilled water for 3 times, removing residual NaCl, and drying by using a blower;
4. at 150 ℃ and 3.0X 104Hot-pressing and sintering for 30min under Pa;
5. the resistance was measured using a four point probe method. When the concentration of NaCl was 1.0mol/L, the resistance was 0.8. omega./sq.
Fig. 1 is an SEM image of a silver nanowire thin film obtained by the 150 ℃ thermal sintering in comparative example 1, in which the nano silver wires are subjected to the 150 ℃ thermal sintering, and a partial connection is formed between the silver wires to form a sintering neck through which an effective conductive path is formed. It has been found that sintering of the nanosilver particles is primarily relied upon to promote the formation of connections between nanosilver wires, forming conductive pathways.
FIG. 2 is an SEM photograph of a silver nanowire thin film obtained by hot press sintering in comparative example 2, in which a silver nanowire is subjected to 150 ℃ and 3.0X 104And (6) Pa hot-pressing sintering. It was found that an effective connection between the silver nanowires was formed, and that primarily the connection between the silver wires formed a more effective conductive path.
After NaCl is adopted for chemical sintering, PVP organic matter is reduced, and contact between the nano silver wires is promoted. After hot-press sintering is adopted, as can be seen from the figure, the sintering nodes among the nano silver wires are increased, so that the conductive paths of the nano silver wires are increased, and the joints among the nano silver wires are sintered more fully, so that the conductive performance is better.
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 nano silver wire conductive ink sintered film is characterized by being prepared according to the following method:
step 1, dispersing the nano silver wires in isopropanol to obtain nano silver wire ink with the concentration of the nano silver wires being 3-6 g/L;
step 2, writing the nano silver wire ink on Epson photographic paper to obtain a square resistor;
step 3, soaking the square resistor in 0.5-2.0mol/L NaCl solution for 20-40min, then rinsing with distilled water to remove residual NaCl, and drying;
step 4, drying the square resistor at 160 ℃ of 140 DEG to 2.5-3.5 × 104And (3) carrying out hot-pressing sintering for 20-40min under the Pa condition to obtain the nano silver wire conductive ink sintered film.
2. The sintered film of silver nanowire conductive ink as claimed in claim 1, wherein the drying manner in step 3 is drying at a temperature of 30-50 ℃ by a blower.
3. The silver nanowire conductive ink sintered film of claim 1, wherein the silver nanowire is prepared by a polyol method, and specifically comprises the following steps:
adding 1.2-1.5g PVP-K30 to 0.13-0.18mmol/L FeCl3Uniformly dispersing in ethylene glycol solution to obtain PVP-FeCl3-ethylene glycol solution to the PVP-FeCl340-60ml of AgNO prepared by adding 0.13-0.19mol/L of AgNO dropwise into the ethylene glycol solution3After the ethylene glycol solution is uniformly dispersed, the reaction system reacts for 2-3h at the temperature of 130-170 ℃, after the reaction is finished, the reaction system is naturally cooled to the room temperature of 20-25 ℃, and then acetone and absolute ethyl alcohol are used for washing, so that the nano silver wire is obtained.
4. The silver nanowire conductive ink sintered film of claim 1, wherein the concentration of the NaCl solution in the step 3 is 1.0 mol/L.
5. The silver nanowire conductive ink sintered film as claimed in claim 1, wherein the temperature of the hot press sintering in the step 4 is 150 ℃ and the pressure is 3.0 x 104Pa, time 30 min.
6. The use of the sintered film of silver nanowires conductive ink as claimed in claim 1, wherein the resistance of the sintered film is 0.7-0.9 Ω/sq.
7. The use according to claim 6, wherein the pressure is 3.0X 10 when the NaCl concentration in step 3 is 1.0mol/L and the temperature of the hot press sintering in step 4 is 150 ℃ and the pressure is 3.0X 104When Pa and time are 30min, the resistance of the nano silver wire conductive ink sintering film is 0.8 omega/sq.
8. A preparation method of a nano silver wire conductive ink sintered film is characterized by comprising the following steps:
step 1, dispersing the nano silver wires in isopropanol to obtain nano silver wire ink with the concentration of the nano silver wires being 3-6 g/L;
step 2, writing the nano silver wire ink on Epson photographic paper to obtain a square resistor;
step 3, soaking the square resistor in 0.5-2.0mol/L NaCl solution for 20-40min, then rinsing with distilled water to remove residual NaCl, and drying;
step 4, drying the square resistor at 160 ℃ of 140 DEG to 2.5-3.5 × 104And (3) carrying out hot-pressing sintering for 20-40min under the Pa condition to obtain the nano silver wire conductive ink sintered film.
9. The method according to claim 8, wherein the silver nanowires are prepared by a polyol method, specifically comprising the steps of:
mixing 1.2-1.5g ofPVP-K30 was added to 0.13-0.18mmol/L FeCl3Uniformly dispersing in ethylene glycol solution to obtain PVP-FeCl3-ethylene glycol solution to the PVP-FeCl340-60ml of AgNO prepared by adding 0.13-0.19mol/L of AgNO dropwise into the ethylene glycol solution3After the ethylene glycol solution is uniformly dispersed, the reaction system reacts for 2-3h at the temperature of 130-170 ℃, after the reaction is finished, the reaction system is naturally cooled to the room temperature of 20-25 ℃, and then acetone and absolute ethyl alcohol are used for washing, so that the nano silver wire is obtained.
10. The method according to claim 8, wherein the NaCl solution concentration in the step 3 is 1.0mol/L, the temperature of the hot press sintering in the step 4 is 150 ℃ and the pressure is 3.0X 104Pa, time 30 min.
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Application publication date: 20200310 |