CN111063488B - Processing method of conductive paste with excellent acid resistance - Google Patents
Processing method of conductive paste with excellent acid resistance Download PDFInfo
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- CN111063488B CN111063488B CN201910952101.1A CN201910952101A CN111063488B CN 111063488 B CN111063488 B CN 111063488B CN 201910952101 A CN201910952101 A CN 201910952101A CN 111063488 B CN111063488 B CN 111063488B
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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
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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
- H01B13/0003—Apparatus or processes specially adapted for manufacturing conductors or cables for feeding conductors or cables
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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
- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
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Abstract
The invention provides a processing method of conductive paste with excellent acid resistance, which adopts a mode of preparing conductive silver powder by nitrate, adds specific monovalent oxide and divalent oxide in the preparation process, and has more excellent acid resistance when the conductive paste is coated on a carbon foil, thereby being suitable for worse use environment.
Description
Technical Field
The invention relates to the field of conductive paste processing, in particular to a processing method of conductive paste with excellent acid resistance.
Background
The conductive paste is mainly used for processing a surface coating of a carbon foil of a lithium ion battery, the better the conductivity is the main measurement standard of the performance, but the optimized performance is acid resistance, the acid resistance of the conductive paste determines the limitation of the service life and the service environment of the carbon foil of the battery, the research on the optimized performance of the acid resistance by the conventional conductive paste is few, the invention provides the conductive paste with the excellent acid resistance, which can effectively expand the service environment and occasions of the lithium ion battery and simultaneously prolong the service life of the lithium ion battery, and the market demand on the aspect is high, so the economic benefit is excellent, and the invention provides the conductive paste processing method with the excellent acid resistance.
Disclosure of Invention
Aiming at the technical problems, the invention provides a processing method of conductive paste with excellent acid resistance,
the method comprises the following steps:
firstly, preparing conductive silver powder, taking a silver nitrate solution as a raw material to perform chemical reduction reaction, adding a reducing agent, a defoaming agent and a dispersing agent, and depositing and drying to obtain the conductive silver powder with the particle diameter of 0.8-1.19 microns; and secondly, mixing 15 parts of conductive silver powder and 5 parts of inorganic glass powder with absolute ethyl alcohol for at least 20min to obtain a first mixture for later use, mixing 3 parts of divalent oxide with an organic solvent for 5-15 min to obtain a second mixture for later use, mixing the first mixture, the second mixture and the monovalent oxide according to a mass ratio of 3: 1: 1, uniformly mixing and stirring to obtain a powder mixed solution; step three, taking the powder mixed solution, and grinding and rolling by using a three-roll grinder; fourthly, preparing the ground powder mixed solution into a silver film by adopting a screen printing process; fifthly, placing the silver film in a sintering furnace for sintering, setting the temperature to be more than 700 ℃, and adopting a water pressurization mode during sintering to keep the pressure to be more than 2.5Mpa to form a silver film compact body; and sixthly, smashing and grinding the silver film compact body into superfine conductive powder with the granularity of more than 600 meshes, adding an adhesive and a vehicle, adding 20 parts of the adhesive and 3 parts of the vehicle into every 10 parts of the superfine conductive powder, uniformly mixing and stirring, wherein the stirring time is at least 2 hours, and finally obtaining the conductive slurry, wherein the divalent oxide is any one of magnesium oxide, strontium oxide and baria, and the monovalent oxide is any one of lithium oxide and rubidium oxide.
Preferably, the first mixture is prepared while adding 1 part of boron oxide.
Preferably, the second mixture is prepared by adding 2 parts of zirconia simultaneously.
Has the advantages that:
1. the finished silver powder is not directly used, but the conductive silver powder is prepared by adopting the reduced silver nitrate, so that the pH value and the particle diameter of the prepared silver powder can be effectively controlled.
2. When the silver powder is prepared and molded, a coating film can be formed on the surface of the powder particles when the powder particles are not nucleated, so that the acid resistance of the silver powder is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a processing method of conductive paste with excellent acid resistance, which comprises the following steps:
firstly, preparing conductive silver powder, taking a silver nitrate solution as a raw material to perform chemical reduction reaction, adding a reducing agent, a defoaming agent and a dispersing agent, and depositing and drying to obtain the conductive silver powder with the particle diameter of 0.8-1.19 microns;
and secondly, mixing 15 parts of conductive silver powder and 5 parts of inorganic glass powder with absolute ethyl alcohol for at least 20min to obtain a first mixture for later use, mixing 3 parts of divalent oxide with an organic solvent for 5-15 min to obtain a second mixture for later use, mixing the first mixture, the second mixture and the monovalent oxide according to a mass ratio of 3: 1: 1, uniformly mixing and stirring to obtain a powder mixed solution;
step three, taking the powder mixed solution, and grinding and rolling by using a three-roll grinder;
fourthly, preparing the ground powder mixed solution into a silver film by adopting a screen printing process;
fifthly, placing the silver film in a sintering furnace for sintering, setting the temperature to be more than 700 ℃, and adopting a water pressurization mode during sintering to keep the pressure to be more than 2.5Mpa to form a silver film compact body;
and sixthly, smashing the silver film compact body, grinding the silver film compact body into superfine conductive powder with the granularity of more than 600 meshes, adding an adhesive and a vehicle, adding 20 parts of the adhesive and 3 parts of the vehicle into every 10 parts of the superfine conductive powder, mixing and stirring uniformly for at least 2 hours, and finally obtaining the conductive slurry.
The divalent oxide in the present invention may be any one of magnesium oxide, strontium oxide, and barium oxide, the monovalent oxide in the present invention may be any one of lithium oxide and rubidium oxide, 1 part of boron oxide is simultaneously added in the preparation of the mixture I, and 2 parts of zirconium oxide is simultaneously added in the preparation of the mixture II. The viscosity of the conductive silver powder in the powder mixed solution obtained after the boron oxide and the zirconium oxide are added is effectively improved, and according to the Ruita-Fred experiment, the content of the conductive silver powder has direct influence on the conductivity of the finally produced conductive paste. The invention improves the acid resistance of the conductive silver powder by a chemical coating method.
The invention designs an acid resistance test experiment, compares the acid resistance of the conductive paste processed by the invention with the acid resistance of common conductive paste on the market at the temperature of 20 ℃, and adopts the method of dripping 5% hydrochloric acid HCl on the surface of the battery carbon foil coated with different sample conductive pastes to test the foaming time, and the shorter the bubble time is, the faster the reaction speed is, and the worse the acid resistance is.
Experimental group 1: coating the surface of the carbon foil with the acid-resistant conductive slurry with the thickness of 0.06mm at the temperature of 20 ℃;
experimental group 2: coating the surface of the carbon foil with the acid-resistant conductive slurry with the thickness of 0.12mm at the temperature of 20 ℃;
experimental group 3: coating the surface of the carbon foil with the acid-resistant conductive slurry with the thickness of 0.16mm at the temperature of 20 ℃;
experimental group 4: coating common conductive slurry with the thickness of 0.06mm on the surface of the carbon foil at the temperature of 20 ℃;
experimental group 5: coating common conductive slurry with the thickness of 0.12mm on the surface of the carbon foil at the temperature of 20 ℃;
experiment group 6; coating common conductive slurry with the thickness of 0.16mm on the surface of the carbon foil at the temperature of 20 ℃;
control group 1: at 20 ℃, the surface of the carbon foil is not coated with any conductive paste.
The experimental data are shown in the following table:
| group of | Type of slurry | Ambient temperature deg.C | Coating thickness mm | Hydrochloric acid concentration | Bubble time h |
| Control group 1 | Is free of | 20 | 0 | 5％ | 1.8 |
| Experimental group 1 | Acid resistance | 20 | 0.06 | 5％ | 15 |
| Experimental group 2 | Acid resistance | 20 | 0.12 | 5％ | 31 |
| Experimental group 3 | Acid resistance | 20 | 0.16 | 5％ | 70 |
| Experimental group 4 | General | 20 | 0.06 | 5％ | 3 |
| Experimental group 5 | General | 20 | 0.12 | 5％ | 21 |
| Experimental group 6 | General | 20 | 0.16 | 5％ | 39 |
TABLE 1
The conductive paste with excellent acid resistance prepared by the invention has the longest bubble time and better acid resistance when 5% hydrochloric acid acts at 20 ℃.
Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
Claims (3)
1. A processing method of conductive paste with excellent acid resistance is characterized by comprising the following steps: firstly, preparing conductive silver powder, taking a silver nitrate solution as a raw material to perform chemical reduction reaction, adding a reducing agent, a defoaming agent and a dispersing agent, and depositing and drying to obtain the conductive silver powder with the particle diameter of 0.8-1.19 microns; and secondly, mixing 15 parts of conductive silver powder and 5 parts of inorganic glass powder with absolute ethyl alcohol for at least 20min to obtain a first mixture for later use, mixing 3 parts of divalent oxide with an organic solvent for 5-15 min to obtain a second mixture for later use, mixing the first mixture, the second mixture and the monovalent oxide according to a mass ratio of 3: 1: 1, uniformly mixing and stirring to obtain a powder mixed solution; step three, taking the powder mixed solution, and grinding and rolling by using a three-roll grinder; fourthly, preparing the ground powder mixed solution into a silver film by adopting a screen printing process; fifthly, placing the silver film in a sintering furnace for sintering, setting the temperature to be more than 700 ℃, and adopting a water pressurization mode during sintering to keep the pressure to be more than 2.5Mpa to form a silver film compact body; and sixthly, smashing and grinding the silver film compact body into superfine conductive powder with the granularity of more than 600 meshes, adding an adhesive and a vehicle, adding 20 parts of the adhesive and 3 parts of the vehicle into every 10 parts of the superfine conductive powder, uniformly mixing and stirring, wherein the stirring time is at least 2 hours, and finally obtaining the conductive slurry, wherein the divalent oxide is any one of magnesium oxide, strontium oxide and baria, and the monovalent oxide is any one of lithium oxide and rubidium oxide.
2. The method as claimed in claim 1, wherein the conductive paste has excellent acid resistance, and further comprises: the first mixture was prepared while adding 1 part of boron oxide.
3. The method as claimed in claim 1, wherein the conductive paste has excellent acid resistance, and further comprises: the second mixture was prepared by adding 2 parts of zirconia simultaneously.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910952101.1A CN111063488B (en) | 2019-10-09 | 2019-10-09 | Processing method of conductive paste with excellent acid resistance |
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| CN201910952101.1A CN111063488B (en) | 2019-10-09 | 2019-10-09 | Processing method of conductive paste with excellent acid resistance |
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| CN111063488B true CN111063488B (en) | 2021-08-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004179139A (en) * | 2002-09-30 | 2004-06-24 | Sumitomo Osaka Cement Co Ltd | Conductive particles and conductive adhesive material containing it and paint for forming transparent conductive film, and transparent conductive film as well as display device using it |
| MX2011009643A (en) * | 2009-03-24 | 2011-09-28 | Basf Se | Preparation of shaped metal particles and their uses. |
| CN101513675B (en) * | 2009-04-03 | 2010-12-01 | 中南大学 | Preparation method of ultrafine copper powder for conductive paste |
| KR101311098B1 (en) * | 2010-04-07 | 2013-09-25 | 오꾸노 케미칼 인더스트리즈 컴파니,리미티드 | Conductive paste and conductive pattern |
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