CN109473197B - High-resolution conductive silver paste containing silver-supermolecule organogel and preparation method thereof - Google Patents
High-resolution conductive silver paste containing silver-supermolecule organogel and preparation method thereof Download PDFInfo
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- CN109473197B CN109473197B CN201811351475.XA CN201811351475A CN109473197B CN 109473197 B CN109473197 B CN 109473197B CN 201811351475 A CN201811351475 A CN 201811351475A CN 109473197 B CN109473197 B CN 109473197B
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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- H01B1/20—Conductive material dispersed in non-conductive organic material
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Abstract
The invention provides a high-resolution conductive silver paste containing silver-supramolecular organogel and a preparation method thereof, wherein the conductive silver paste comprises the following raw materials in parts by weight: 55-70 parts of silver powder, 1-3 parts of low-melting-point glass powder and 30-50 parts of silver-supramolecular organogel. The silver-containing-supermolecule organogel is used for preparing the conductive silver paste, on one hand, the silver-containing organogel can be gathered into a small 1-2nm fiber unit in a paste system, and then self-assembled to form a large number of strip-shaped fiber bundles of 10-20nm which are mutually wound, so that the system can easily and quickly form a stable gel system once shearing force is removed, high-fineness printing is realized, on the other hand, nano silver formed by silver decomposition in the silver-containing organogel during silver paste sintering is uniformly dispersed in the silver paste system, and the problem that the nano silver is difficult to disperse by directly adding the nano silver is solved, so that the problems that the existing conductive silver paste is poor in conductivity, low in printing resolution, insufficient in stability and the like are well solved.
Description
Technical Field
The invention belongs to the technical field of silver paste preparation, and particularly relates to high-resolution conductive silver paste containing silver-supermolecule organogel and a preparation method thereof.
Background
The conductive silver paste is a paste consisting of silver powder, an organic or inorganic binder, a solvent and an additive, and is mainly used for forming a conductive film through printing and sintering to conduct current. The conductive silver paste needs to have the following characteristics: good conductivity, strong adhesion and excellent printing adaptability. The conductive paste is the basis for developing electronic components, and the silver-based electronic paste becomes a key functional material for producing various electronic component products by virtue of mechanical properties such as high conductivity, excellent adhesion property, weldability and the like, and has no replaceable function in the electronic industry. The trend of high-speed transmission and miniaturization and intellectualization in the electronic information industry requires higher performance and smaller size of components, so that the conductive silver paste used must have higher conductivity, higher printing fine resolution and uniformity.
At present, the main method for preparing the conductive paste to improve the conductivity is to add part of nano silver powder with the size to promote sintering, so as to form a compact conductive network, but the common nano silver particles are prepared by a physical method or a chemical method (mainly adopting a liquid phase reduction method), and the methods are used after pure nano silver particles are obtained. One method is that the silver paste is directly added into formula mixed liquid containing surfactant and the like, viscosity is adjusted to obtain silver paste, and in the preparation process, nano silver particles are not wrapped by the surfactant, and because the nano silver particles have high surface activity, agglomeration is easy to occur, the nano sintering advantage of the silver particles is reduced, and the purpose of improving conductivity is not achieved; the other method is to coat the nano silver powder with a large amount of organic matters, so that the dispersibility of the nano silver powder in a silver paste system can be improved, but the large amount of organic matters cannot be completely decomposed in the sintering process, so that residual carbon is generated, voids are caused, and the electric conductivity is influenced.
On the other hand, for the performance improvement of high printing resolution and high stability, the traditional method mainly adjusts the thixotropic property of the conductive silver paste by using a macromolecular thixotropic agent such as polyamide wax or an inorganic thixotropic agent such as bentonite and fumed silica, and improves the printing fineness, however, most of the paste is silver powder and a solvent, meanwhile, the external response speed and the system network structure recovery of the macromolecular thixotropic agent are slow, the improvement of the printing resolution by adding a small amount of thixotropic agent is limited and cannot meet the market requirement, and the conductive performance is influenced by using a non-conductive thixotropic inorganic substance agent.
In order to expand the application field of the silver paste and meet the requirement of the electronic industry on the high performance of the silver paste, the development of the silver paste with high conductivity, high resolution and high stability consistency is imperative.
The silver-containing supermolecule organogel is adopted to prepare the conductive silver paste, so that the problems can be well solved. On one hand, the silver-containing organic gel can be gathered into a fine 1-2nm fiber unit in a slurry system by taking intermolecular hydrogen bond, hydrophobic effect and the like as driving forces, and then self-assembled to form a large number of mutually-wound ribbon fiber bundles of about 10-20nm on the basis, so that the viscosity of the system is reduced when a shearing force is applied, the system can easily and quickly form a stable gel system once the shearing force is removed, high-fineness and high-resolution printing can be realized, solid particles can be better stabilized, and the stable consistency of products is kept; on the other hand, the nano silver formed by decomposing the silver in the silver-containing organogel is uniformly dispersed in the silver paste system when the silver paste is sintered, so that the problem that the nano silver is difficult to disperse by directly adding the nano silver is solved, and the conductivity and the uniformity of the silver paste are improved, therefore, the silver paste disclosed by the invention has high conductivity and excellent printing precision, can meet more use occasions, and has a wider application range and a wider market prospect.
Disclosure of Invention
The invention aims to solve the problems of poor conductivity, low printing resolution and poor stability of the conventional conductive silver paste.
In order to solve the technical problems, the invention adopts the following technical scheme:
the high-resolution conductive silver paste containing the silver-supramolecular organogel is characterized by comprising the following raw materials in parts by weight:
55-70 parts of silver powder;
1-3 parts of low-melting-point glass powder;
30-50 parts of silver-containing supramolecular organogel;
the silver powder is silver powder subjected to surface treatment by oleic acid amide or lauric acid amide, and the average particle size of the silver powder is 200-500 nm;
the low-melting-point glass powder is Bi2O3-B2O3-SiO2-Al2O3-CuO system with softening point of 460-650 deg.C and particle size of 2-4 μm;
the preparation method of the silver-containing supramolecular organogel comprises the following steps:
(1) under the protection of nitrogen and the heating condition of 50 ℃, dissolving 1-3 parts of phenylalanine in 2-5 parts of tetrahydrofuran, gradually adding 2-5 parts of bis (trichloromethyl) carbonate until the solution becomes transparent, reacting for 3 hours, and carrying out vacuum drying and recrystallization on the product to obtain white crystals;
(2) and (2) placing 15-30 parts of the white crystal obtained in the step (1), 1-5 parts of dichloromethane and 3-5 parts of silver alkyl amino acid in a container, reacting at 40-60 ℃ for 12-36h, putting the mixture into ether to separate out a precipitate, and drying at room temperature for 8h to obtain the silver-containing phenylpropylamino oligomer.
(3) And (3) adding 1 part of the phenylpropylamino oligomer obtained in the step (3) into 3-6 parts of an organic solvent, heating to 40 ℃, stirring and mixing for 30min until the oligomer is dissolved, and cooling to room temperature to obtain the silver-supramolecular organogel.
Further, the structure of the alkyl amino acid silver is as follows:
H2N-R--COOAg
r represents an alkyl group (CH)2)12-(CH2)18Further, the silver-containing styrene-acrylic amino oligomer has the following structure:
wherein n is 5-8; r represents an alkyl group (CH)2)12-(CH2)18(ii) a Ph represents a benzene ring
Further, the organic solvent is one or a mixture of more of sandalwood 803, alcohol ester dodeca and terpineol
Furthermore, the preparation method of the conductive silver paste is characterized by comprising the following process steps:
(1) uniformly mixing silver powder and low-melting-point glass powder by using an air flow mill;
(2) adding the mixture obtained in the step (1) into silver-supramolecular organogel, and stirring the mixture in a double-planet mixing stirrer at the speed of 50-80rmp for 1-2 hours;
(3) and dispersing and mixing the mixture uniformly, and then carrying out three-roll grinding, wherein the rolling fineness is less than 10 mu m, thus obtaining the conductive silver paste.
The invention has the following beneficial effects:
a. for the performance improvement of high printing resolution and high stability, the traditional method mainly adjusts the thixotropic property of the conductive silver paste by using a macromolecular thixotropic agent such as polyamide wax or an inorganic thixotropic agent such as bentonite and fumed silica, and improves the printing fineness, but the macromolecular thixotropic agent has a slow response speed to the outside and a slow recovery of a system network structure, the improvement of the printing resolution by adding a small amount of the thixotropic agent is limited and cannot meet the market requirement, and the use of the non-conductive inorganic thixotropic agent can influence the conductivity. The conductive silver paste prepared by the invention uses silver-containing-supramolecular organogel, can be aggregated into a fine 1-2nm fiber unit by taking intermolecular hydrogen bond, hydrophobic effect and the like as driving forces in a paste system, and then self-assembles to form a large number of strip-shaped fiber bundles which are mutually wound and are about 10-20nm on the basis, so that the viscosity of the system is reduced when a shearing force is applied, the system can easily and quickly form a stable gel system once the shearing force is removed, the fine line printing performance of the paste is excellent, the shaping capability is good, the printing with high fineness and high resolution can be realized, meanwhile, solid particles can be better stabilized, and the stable consistency of products is kept;
b. the silver paste prepared by the invention has the advantages that silver-containing-supermolecule organogel is in a homogeneous phase in the system, and is decomposed into nano silver which can be uniformly dispersed in the silver paste system during sintering, so that the problem of difficult dispersion of the directly added nano silver is solved, the uniformity and the stability of the silver paste are improved, the sintering activity of the silver paste is improved, the densification of a sintered silver layer is promoted, and the conductivity is improved.
Drawings
FIG. 1 is a schematic view of supramolecular gel formation
FIG. 2 is SEM image of intertwined fiber bundles in silver-containing supramolecular gel system
Fig. 3 is a schematic view of the quick recovery of silver paste containing silver supramolecular organogel under stress.
The invention will be better understood by reference to the following examples, which are included to illustrate but not to limit the scope of the invention.
Example 1
Preparing silver-containing supermolecule organogel, wherein the following proportions are calculated by weight:
(1) under the protection of nitrogen and the heating condition of 50 ℃, dissolving 1 part of phenylalanine in 3 parts of tetrahydrofuran, gradually adding 3 parts of bis (trichloromethyl) carbonate into the solution until the solution becomes transparent, reacting for 3 hours, and carrying out vacuum drying and recrystallization on the product to obtain white crystals;
(2) 15 parts of the white crystals obtained in step (1), 1 part of methylene chloride and 3 parts of silver alkyl amino acid H2N--(CH2)12placing-COOAg in a container, reacting at 40 deg.C for 24 hr, adding ether to precipitate, vacuum drying at room temperature for 8 hr to obtain Ag-containing phenylpropylamino oligomer
。
(3) And (3) adding 1 part of the phenylpropylamino oligomer obtained in the step (3) into 3 parts of sandalwood 803, heating to 40 ℃, stirring and mixing for 30min until the oligomer is dissolved, and cooling to room temperature to obtain a transparent gel, namely the silver-supramolecular organogel.
Preparing conductive silver paste according to the following proportions by weight:
(1) 55 parts of silver powder and 1 part of Bi2O3-B2O3-SiO2-Al2O3And (4) uniformly mixing the-CuO system low-melting-point glass powder by using an airflow mill. Wherein the softening point of the glass powder is 500 ℃, and the average grain diameter is 1.5 mu m; the average grain diameter of the silver powder is 200 nanometers, and the surface of the silver powder is modified by oleamide.
(2) Adding the mixture obtained in the step (1) into 44 parts of silver-supramolecular organogel, and stirring for 3min at a speed of 100rmp in a planetary gravity mixer;
(3) and dispersing and mixing the mixture uniformly, and then carrying out three-roll grinding, wherein the rolling fineness is less than 10 mu m, thus obtaining the conductive silver paste.
Example 2
Preparing silver-containing supermolecule organogel, wherein the following proportions are calculated by weight:
(1) under the protection of nitrogen and the heating condition of 50 ℃,3 parts of phenylalanine are dissolved in 5 parts of tetrahydrofuran, 5 parts of bis (trichloromethyl) carbonate is gradually added into the tetrahydrofuran until the solution becomes transparent, the reaction is carried out for 3 hours, and the product is dried in vacuum and recrystallized to obtain white crystals;
(2) 30 parts of the white crystals obtained in step (1), 5 parts of methylene chloride and 5 parts of silver alkyl amino acid H2N--(CH2)18placing-COOAg in a container, reacting at 60 deg.C for 30 hr, adding ether to precipitate, vacuum drying at room temperature for 8 hr to obtain Ag-containing phenylpropylamino oligomer
。
(3) And (3) adding 1 part of the phenylpropylamino oligomer obtained in the step (3) into 5 parts of mixed solution of sandalwood 803 and alcohol ester twelve in a ratio of 1:3, heating to 40 ℃, stirring and mixing for 30min until the solution is dissolved, and cooling to room temperature to obtain transparent gel, namely the silver-supramolecular organogel.
Preparing conductive silver paste according to the following proportions by weight:
(1) 70 parts of silver powder and 3 parts of Bi2O3-B2O3-SiO2-Al2O3And (4) uniformly mixing the-CuO system low-melting-point glass powder by using an airflow mill. Wherein the softening point of the glass powder is 600 ℃, and the average grain diameter is 3 mu m; the average grain diameter of the silver powder is 500 nanometers, and the surface of the silver powder is modified by lauric acid amide.
(2) Adding the mixture obtained in the step (1) into 27 parts of silver-supramolecular organogel, and stirring for 1min at 2000rmp speed in a planetary gravity mixer;
(3) and dispersing and mixing the mixture uniformly, and then carrying out three-roll grinding, wherein the rolling fineness is less than 10 mu m, thus obtaining the conductive silver paste.
Example 3
Preparing silver-containing supermolecule organogel, wherein the following proportions are calculated by weight:
(1) under the protection of nitrogen and the heating condition of 50 ℃, dissolving 2 parts of phenylalanine in 4 parts of tetrahydrofuran, gradually adding 4 parts of bis (trichloromethyl) carbonate into the tetrahydrofuran until the solution becomes transparent, reacting for 3 hours, and carrying out vacuum drying and recrystallization on the product to obtain white crystals;
(2) 21 parts of the white crystals obtained in step (1), 3 parts of methylene chloride and 4 parts of silver alkyl amino acid H2N--(CH2)16placing-COOAg in a container, reacting at 50 deg.C for 24 hr, adding ether to precipitate, vacuum drying at room temperature for 8 hr to obtain Ag-containing phenylpropylamino oligomer
。
(3) And (3) adding 1 part of the phenylpropylamino oligomer obtained in the step (3) into 4 parts of mixed solution of sandalwood 803, alcohol ester dodeca and terpineol according to the proportion of 1:2 and 2, heating to 40 ℃, stirring and mixing for 30min until the solution is dissolved, and cooling to room temperature to obtain transparent gel, namely the silver-supramolecular organogel.
Preparing conductive silver paste according to the following proportions by weight:
(1) 62 parts of silver powder and 2 parts of Bi2O3-B2O3-SiO2-Al2O3And (4) uniformly mixing the-CuO system low-melting-point glass powder by using an airflow mill. Wherein the softening point of the glass powder is 650 ℃, and the average grain diameter is 2 μm; the average grain diameter of the silver powder is 300 nanometers, and the surface of the silver powder is modified by oleamide.
(2) Adding the mixture obtained in the step (1) into 36 parts of silver-supramolecular organogel, and stirring for 2min at the speed of 1000rmp in a planetary gravity mixer;
(3) and dispersing and mixing the mixture uniformly, and then carrying out three-roll grinding, wherein the rolling fineness is less than 10 mu m, thus obtaining the conductive silver paste.
Comparative example 1
The supramolecular gel in example 1 was replaced with a conventional organic vehicle prepared from ethylcellulose; 0.7% of polyamide wax is added into the conductive silver paste to be used as a thixotropic agent; a conductive silver paste was prepared in the same manner as in example 1, except that 1% of 30nm silver powder was simultaneously added instead of nanoparticles generated by decomposition of silver in the silver-containing supramolecular gel.
Comparative example 2
The supramolecular gel in example 2 was replaced with a conventional organic vehicle prepared from ethylcellulose; 1% of fumed silica is added into the conductive silver paste to be used as a thixotropic agent; conductive silver paste was prepared in the same manner as in example 2, except that 3% of 50nm silver powder was simultaneously added instead of nanoparticles generated by decomposition of silver in the silver-containing supramolecular gel.
And (3) performance testing:
the conductive silver pastes prepared in examples 1,2,3 and comparative examples 1,2 were subjected to characteristic evaluation in the following operating conditions.
i) Printing on a 20cmX 20cm alumina substrate by a screen printing method;
ii) drying in a drying oven at 120 ℃ for 15 minutes;
iii) maintaining the temperature at 850 ℃ for 15 minutes by using a sintering furnace;
iv) testing the sheet resistance by using a four-probe instrument;
v) observing the printing resolution with a high power microscope;
vi) measuring the thickness of the film layer by using a scanning electron microscope.
Resistivity = sheet resistance vs film thickness
From the above results, it can be seen that: under the same condition, the silver paste prepared by the silver-supermolecule organogel has high resolution and good conductivity compared with the comparative example.
The silver paste prepared by the invention expands the application field of the silver paste, meets the requirement of the electronic industry on the high performance of the silver paste, and has wide market application prospect. The technical indexes of the silver electrode reach the level of batch production from the aspects of printing precision, conductivity and performance indexes of the silver electrode.
Claims (5)
1. The high-resolution conductive silver paste containing the silver-supramolecular organogel is characterized by comprising the following raw materials in parts by weight:
55-70 parts of silver powder;
1-3 parts of low-melting-point glass powder;
30-50 parts of silver-supramolecular organogel;
the silver powder is silver powder subjected to surface treatment by oleic acid amide or lauric acid amide, and the average particle size of the silver powder is 200-500 nm; the low-melting-point glass powder is a Bi2O3-B2O3-SiO2-Al2O3-CuO system, the softening point is 460-650 ℃, and the particle size is 2-4 mu m;
the preparation method of the silver-supramolecular organogel comprises the following steps:
(1) under the protection of nitrogen and the heating condition of 50 ℃, dissolving 1-3 parts of phenylalanine in 2-5 parts of tetrahydrofuran, gradually adding 2-5 parts of bis (trichloromethyl) carbonate until the solution becomes transparent, reacting for 3 hours, and carrying out vacuum drying and recrystallization on the product to obtain white crystals;
(2) putting 15-30 parts of white crystal obtained in the step (1), 1-5 parts of dichloromethane and 3-5 parts of silver alkyl amino acid into a container, reacting at 40-60 ℃ for 12-36h, putting into ether to separate out a precipitate, and vacuum drying at room temperature for 8h to obtain a silver-containing phenylpropylamino oligomer;
(3) and (3) adding 1 part of the phenylpropylamino oligomer obtained in the step (2) into 3-6 parts of an organic solvent, heating to 40 ℃, stirring and mixing for 30min until the oligomer is dissolved, and cooling to room temperature to obtain a transparent gel, namely the silver-supramolecular organogel.
2. The high resolution conductive silver paste comprising silver-supramolecular organogel according to claim 1, wherein said silver alkyl amino acid has the following structure:
H2N-R--COOAg
r represents an alkyl group (CH)2)12-(CH2)18。
3. The high resolution conductive silver paste containing silver-supramolecular organogel according to claim 1, wherein the silver-containing phenylpropylamino oligomer has the following structure:
wherein n is 5-8; r represents an alkyl group (CH)2)12-(CH2)18(ii) a Ph represents a benzene ring.
4. The high resolution conductive silver paste containing silver-supramolecular organogel according to claim 1, wherein the solvent is one or more of sandalwood 803, alcohol ester dodeca, and terpineol.
5. The method for preparing conductive silver paste according to claim 1, characterized by the following process steps: 1) Uniformly mixing silver powder and low-melting-point glass powder by using an air flow mill; 2) Adding the mixture obtained in the step 1) into silver-supramolecular organogel, and stirring the mixture for 1 to 3min at the speed of 1000 to 2000rmp in a planetary gravity mixing stirrer; 3) and (3) uniformly dispersing and mixing the mixture obtained in the step 2), and then carrying out three-roll grinding, wherein the rolling fineness is less than 10 mu m, so as to obtain the conductive silver paste.
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| CN112768113B (en) * | 2020-12-31 | 2023-06-27 | 合肥工业大学 | Preparation method of responsive nanocomposite polymer conductive film |
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Address after: 210015 No.5, jinchuanmenwai, Gulou District, Nanjing City, Jiangsu Province Patentee after: Nanjing University of Technology Optoelectronic Materials Research Institute Co.,Ltd. Patentee after: NANJING YUQUN MATERIAL TECHNOLOGY Co.,Ltd. Address before: 210015 No.5, jinchuanmenwai, Gulou District, Nanjing City, Jiangsu Province Patentee before: LIGHT INDUSTRY DEPARTMENT THE Research Institute OF NANJING ELECTRIC LIGHT SOURCE MATERIALS Patentee before: NANJING YUQUN MATERIAL TECHNOLOGY Co.,Ltd. |