CN114749587A - Silver nanowire welding interconnection method - Google Patents
Silver nanowire welding interconnection method Download PDFInfo
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- CN114749587A CN114749587A CN202210401448.9A CN202210401448A CN114749587A CN 114749587 A CN114749587 A CN 114749587A CN 202210401448 A CN202210401448 A CN 202210401448A CN 114749587 A CN114749587 A CN 114749587A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21F—WORKING OR PROCESSING OF METAL WIRE
- B21F15/00—Connecting wire to wire or other metallic material or objects; Connecting parts by means of wire
- B21F15/02—Connecting wire to wire or other metallic material or objects; Connecting parts by means of wire wire with wire
- B21F15/06—Connecting wire to wire or other metallic material or objects; Connecting parts by means of wire wire with wire with additional connecting elements or material
- B21F15/08—Connecting wire to wire or other metallic material or objects; Connecting parts by means of wire wire with wire with additional connecting elements or material making use of soldering or welding
Abstract
The invention provides a silver nanowire welding interconnection method, and belongs to the technical field of nano materials. The welding interconnection method comprises the following specific processes: and at normal temperature, completely soaking the solid carrier with the silver nanowires attached to the surface in the nano interconnection welding mixed solution for 10s and 300s, and thus completing the welding interconnection of the silver nanowires. The nano welding mixed liquid comprises ascorbic acid as one component and inorganic acid or organic acid with etched metal silver, such as nitric acid, 1,2,3, 4-butanetetracarboxylic acid, acrylic acid and the like as the other component. The method of the invention can promote the silver nanowires to be firmly welded and interconnected, the appearance and the structure are not easy to be damaged, the welding condition is mild, the process is easy to operate and control, and the special conditions of hot melting, high pressure, vacuum and the like are avoided. The invention is suitable for the preparation of flexible transparent conductors in the field of flexible electronics and the field of other advanced functional materials.
Description
Technical Field
The invention belongs to the field of nanotechnology, and particularly relates to a silver nanowire welding interconnection method.
Background
Currently, flexible electronics are receiving great attention due to their unique flexibility characteristics and efficient, low-cost manufacturing processes. As a core material for constructing various flexible electronic components and equipment such as flexible display screens, flexible solar cells, flexible light-emitting diodes and the like, the flexible transparent conductor is very important for developing flexible electronics. Therefore, flexible transparent conductors are one of the current multidisciplinary frontier research fields.
Silver nanowire-based flexible transparent conductors are the most widely studied and promising class of flexible transparent conductors, and can be prepared by compounding flexible silver nanowires on the surface of a flexible transparent polymer substrate (Haifei Lu, Xilingang Ren, Dan Ouyang, Wallace C H Choy. electronic novel metals for photonic applications. Small,2018, 1703140. 20153180; Jun Wang, jinding Jiu, Masaya Nogi, Tohru Sugahara, Shijo NAgao, Hirotaka Koga, Peng He, Katsuki Suganma. A high purity and flexible sensing sensor with electric wires and electronic monitoring wires 2932, 2932). The development of high-performance silver nanowire flexible transparent conductors has been a target problem that the academia and the industry try to solve. Electrical conductivity, optical transparency, haze are key properties of flexible transparent conductors, they are mutually constrained and influenced by many parties. In order to meet the requirements of high light transmission and low haze, the low-density silver nanowires are required to be used for preparing the silver nanowire flexible transparent conductor. The conductivity of the transparent conductor under this condition is mainly determined by the contact resistance at the silver nanowire lap (Hwansu Sim, Shingyu Bok, Bongsung Kim, Minka Kim, Guh Hwan Lim, Sung Min Cho, Byungkwon Lim. organic-stable-free polyol synthesis of silver nanoviruses for electrode applications. Angew. chem. int. Ed.,2016,55, 11814-one 11818). Since the silver nanowires are loosely lapped on the surface of the flexible transparent conductor, and a thin layer of macromolecules is adhered to the surface of the flexible transparent conductor, the contact resistance between the nanowires is high, and thus the low electrical conductivity of the prepared flexible transparent conductor of the silver nanowires is caused. In addition, the loosely lapped silver nanowires are easy to slip, wander and agglomerate in long-term service, which not only affects the conductivity stability of the flexible transparent conductor of the silver nanowires, but also causes uneven and unstable light transmission and haze. Therefore, the problem that the lap-joint looseness of the silver nanowires becomes a key problem for developing high-performance silver nanowire flexible transparent conductors is solved.
Disclosure of Invention
The invention provides a silver nanowire welding interconnection method aiming at the key problem of loose lapping of silver nanowires in the preparation process of a flexible transparent conductor, and the silver nanowires are enabled to be firmly welded and interconnected.
The invention provides a silver nanowire welding interconnection method, which comprises the following specific steps:
(1) pouring the silver nanowire dispersion liquid on the surface of a solid carrier, volatilizing a solvent at normal temperature, and drying; the solid carrier is inorganic, organic or high molecular material.
(2) Preparing a nano welding mixed solution containing two types of components of reducing property and non-reducing property at normal temperature;
the reducing component of the nano welding mixed solution is ascorbic acid, and the concentration of the ascorbic acid is 0.010.5M; the non-reducing component of the nano welding mixed solution is single or mixed inorganic or organic acid, and the concentration of hydrogen ions in the acid is 0.05M 3M.
(3) And (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the step (1) in the nano welding mixed solution prepared in the step (2) at normal temperature, and reacting for 10s and 300s to complete the welding and interconnection of the silver nanowires.
Further, the solid carrier in the step (1) is glass, silicon wafer, polyurethane, polyester or silicon rubber.
Further, the inorganic acid in the step (2) is nitric acid.
Further, the organic acid in the step (2) is 1,2,3, 4-butanetetracarboxylic acid or acrylic acid.
The scientific principle of the invention is that the interconnection of the silver nanowires is realized by in-situ etching/reduction welding, namely, one non-reducing acid in welding liquid is used for in-situ etching the silver nanowires to release metal ions, meanwhile, another reducing acid is used for reducing the released silver ions to form silver atoms, and the diffusion and deposition on the lapping interface of the silver nanowires in the generation of the silver atoms are used for realizing the firm welding and interconnection of the silver nanowires. The process can be completed under the cooperation of two types of acids (non-reducing acid and reducing acid), and the silver nanowires cannot be firmly welded and interconnected by using the non-reducing acid or the reducing acid alone. Taking the welding and interconnection of silver nanowires in the mixed solution of nitric acid and ascorbic acid as an example, the specific process is illustrated with reference to fig. 1 of the accompanying drawings.
Compared with the prior art, the invention has the following technical effects:
(1) the silver nanowires are firmly welded and interconnected, but the appearance and the structure are not easily damaged.
(2) The welding interconnection condition is mild, the process is easy to operate and control, the special conditions of hot melting, high pressure, vacuum and the like are avoided, and the method is beneficial to large scale.
(3) The conductivity can be increased 3.25.3 times after welding.
Drawings
FIG. 1 is a schematic diagram of in-situ etching/reduction welding of silver nanowires;
as shown in fig. 1, when the silver nanowires are in the mixed solution of nitric acid and ascorbic acid for welding, the nitric acid will make the surfaces of the silver nanowires (including the lapping interface) be etched continuously to release Ag in situ+Simultaneously, the reducing agent ascorbic acid continuously and rapidly reduces Ag+Silver atoms are generated. During the generation process, the silver atoms can continuously diffuse, migrate and deposit between the lapping interfaces. The circulation, repeated etching and reduction reaction can promote the welding and interconnection of the silver nanowires at the lap joint. Due to Ag+Is not added additionally but is generated by in-situ etching, and is rapidly reduced in situ when being slowly released, so that the appearance of the silver nanowire at the non-lap joint part is basically not damaged. If, realize that silver nano-wire is at the welded interconnection of overlap joint, non-overlap joint is intact.
FIG. 2 is a typical scanning electron microscope image of silver nanowires in example 1 after interconnection by soldering;
as shown in fig. 2, the nano-welding method of the present invention can promote the lap joint to be welded and interconnected firmly, and the shapes of the nano-silver wires at the lap joint are kept intact except for the fact that the welding diameter of the nano-silver wires at the lap joint is slightly reduced.
Detailed Description
The present invention will be described in detail below with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
(1) Dispersing the silver nanowires into ethanol, pouring the silver nanowires on the surface of a silicon rubber carrier, volatilizing the ethanol at normal temperature, and drying.
(2) Preparing a nano welding mixed solution containing two components of reducing property and non-reducing property at normal temperature.
One reducing component of the nano welding mixed solution is ascorbic acid, and the concentration of the ascorbic acid is 0.015M;
the other non-reducing component of the nano welding mixed liquid is nitric acid with the concentration of 0.5M.
(3) And (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the nano interconnection welding mixed solution in the step (2) at normal temperature, and reacting for 60s to complete the welding and interconnection of the silver nanowires.
The conductivity after welding is increased by 5.3 times compared with that before welding.
Example 2
(1) Dispersing silver nanowires into ethanol, pouring the silver nanowires on the surface of a polyurethane carrier, volatilizing the ethanol at normal temperature, and drying.
(2) Preparing a nano welding mixed solution containing two components of reducing property and non-reducing property at normal temperature.
The nano welding mixed solution comprises a reducing component ascorbic acid with the concentration of 0.5M;
the other non-reducing component of the nano welding mixed solution is acrylic acid with the concentration of 3M.
(3) And (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the nano interconnection welding mixed solution in the step (2) at normal temperature, and reacting for 60s to complete the welding and interconnection of the silver nanowires.
The conductivity after welding is increased by 4.8 times compared with that before welding.
Example 3
(1) Dispersing silver nanowires into ethanol, pouring the silver nanowires on the surface of a silicon wafer, volatilizing the ethanol at normal temperature, and drying.
(2) Preparing a nano welding mixed solution containing two components of reducing property and non-reducing property at normal temperature.
The nano welding mixed solution comprises a reducing component ascorbic acid with the concentration of 0.01M;
another non-reducing component of the nano-soldering mixed liquid is 1,2,3, 4-butanetetracarboxylic acid with the concentration of 0.5M.
(3) And (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the nano interconnection welding mixed solution in the step (2) at normal temperature, and reacting for 10s to complete the welding and interconnection of the silver nanowires.
The conductivity after welding is increased by 3.2 times compared with that before welding.
Example 4
(1) Dispersing the silver nanowires into ethanol, pouring the ethanol on the surface of glass, volatilizing the ethanol at normal temperature, and drying.
(2) Preparing a nano welding mixed solution containing two components of reducing property and non-reducing property at normal temperature.
One reducing component of the nano welding mixed solution is ascorbic acid, and the concentration of the ascorbic acid is 0.3M;
another non-reducing component of the nano-welding mixed liquid is nitric acid with the concentration of 1M.
(3) And (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the nano interconnection welding mixed solution in the step (2) at normal temperature, and reacting for 60s to complete the welding and interconnection of the silver nanowires.
The conductivity after welding was increased by 4.9 times compared to before welding.
Example 5
(1) Dispersing the silver nanowires into ethanol, pouring the silver nanowires on the surface of the silicon rubber, volatilizing the ethanol at normal temperature, and drying.
(2) Preparing a nano welding mixed solution containing two components of reducing property and non-reducing property at normal temperature.
One reducing component of the nano welding mixed solution is ascorbic acid, and the concentration of the ascorbic acid is 0.1M;
the other non-reducing component of the nano welding mixed liquid is nitric acid with the concentration of 0.5M.
(3) And (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the nano interconnection welding mixed solution in the step (2) at normal temperature, and reacting for 300s to complete the welding and interconnection of the silver nanowires.
The conductivity after welding is increased by 4.6 times compared with that before welding.
Claims (4)
1. A silver nanowire soldering interconnection method, characterized by comprising the steps of:
(1) pouring the silver nanowire dispersion liquid on the surface of a solid carrier, volatilizing a solvent at normal temperature, and drying; the solid carrier is an inorganic, organic or high molecular material;
(2) preparing a nano welding mixed solution containing two types of components of reducing property and non-reducing property at normal temperature;
the reducing component of the nano welding mixed solution is ascorbic acid, and the concentration of the ascorbic acid is 0.010.5M; the non-reducing component of the nano welding mixed solution is single or mixed inorganic or organic acid, and the concentration of hydrogen ions in the acid is 0.05M 3M;
(3) and (3) completely soaking the solid carrier with the silver nanowires attached to the surface in the step (1) in the nano welding mixed solution prepared in the step (2) at normal temperature, and reacting for 10s and 300s to complete the welding and interconnection of the silver nanowires.
2. The silver nanowire soldering interconnection method of claim 1, wherein the solid carrier in step (1) is glass, silicon wafer, polyurethane, polyester or silicone rubber.
3. The silver nanowire soldering interconnection method of claim 1, wherein the inorganic acid in the step (2) is nitric acid.
4. The silver nanowire soldering interconnection method of claim 1, wherein the organic acid of step (2) is 1,2,3, 4-butanetetracarboxylic acid or acrylic acid.
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