CN113903494A - High-performance graphene composite silver paste and preparation method thereof - Google Patents
High-performance graphene composite silver paste and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of silver paste, in particular to high-performance graphene composite silver paste. The graphene composite silver paste comprises the following raw materials in percentage by mass: 5-20% of graphite powder, 50-65% of nano silver paste, 3-5% of glass powder, 0.5-2% of dendritic organic molecules and 8-41.5% of organic solvent. Meanwhile, the invention also discloses a preparation method of the graphene composite silver paste. The inventor finds that the dendritic organic molecule not only utilizes the steric hindrance effect of the three-dimensional topological structure of the dendritic organic molecule to uniformly disperse graphene, but also forms a complex of the dendritic organic molecule with the nano silver particles by rich active sites provided by the terminal group functional groups of the dendritic organic molecule, so that the silver particles are uniformly attached to the two-dimensional graphene nanosheet, the compatibility of two phases is improved, and the interface energy is remarkably reduced. The obtained graphene composite silver paste can greatly reduce the content of silver powder in the existing commercial silver paste, greatly reduce the material cost and simultaneously keep the ultrahigh conductivity of the composite silver paste.
Description
Technical Field
The invention relates to the field of solar cell materials, in particular to high-performance graphene composite silver paste and a preparation method thereof.
Background
The conductive silver paste is widely used for the production of various electronic elements, such as integrated circuits and electric heating films, and particularly in the preparation of photovoltaic solar cells and the assembly of cells into power generation components for photoelectric conversion, the conductive silver paste becomes one of the key materials for the photovoltaic solar energy scale-up by virtue of excellent conductivity, printability and strong combination with a substrate. Therefore, the cost of the conductive silver paste is reduced, and the conductive silver paste has decisive significance for reducing the cost of the whole product, realizing the large-scale production and wider application of the solar cell.
The content of silver in the conductive silver paste is reduced, and the high conductivity of the conductive silver paste is kept, so that the cost of the silver paste is effectively reduced, and the development of the novel composite silver paste is not slow. As a novel two-dimensional material, graphene has high theoretical conductivity (10)6S/cm), high mechanical strength, good light transmission and the like, the hybrid orbit can provide electrostatic adsorption for silver particles, and the unique properties of the two enable the graphene/nano silver composite ink to arouse the interest of a plurality of researchers. The ingenious compounding not only reduces the silver content, but also effectively hinders the secondary stacking of the graphene. For example, the low-content nano silver conductive paste and the preparation method thereof disclosed in the chinese patent publication No. CN 1437200a, the nano silver particles with narrow particle size distribution are prepared by the microemulsion method, and the silver content of the conductive silver paste prepared from the nano silver particles is reduced to 20% while the good conductivity is maintained. The disclosure of the patent application publication No. CN 102136301A discloses a graphene nano conductive composite material and a preparation method thereof, and a silver graphene composite material is successfully prepared by adopting a one-step reduction method. The conductive composite silver paste prepared by the two patents uses nano metal particles and a new conductive material, so that the cost of the silver paste is reduced, and a new problem is brought simultaneously: (1) the redox graphene has a large number of structural defects, the high conductivity characteristic of the graphene is seriously reduced, and although the content of silver is reduced, the conductivity of the composite silver paste is also reduced; (2) the process is complex and not easy to repeat, the performance of the silver paste after sintering is not stable enough, the electrical performance of the electrode is greatly restricted, and the wide popularization and application are not facilitated.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-performance graphene composite silver paste.
The invention aims to solve another technical problem of providing a preparation method for preparing high-performance graphene-silver paste by one-step stripping of graphene and synchronous compounding of graphene and silver paste.
In order to solve the problems, the high-performance graphene composite silver paste provided by the invention comprises the following raw materials in percentage by mass: 5-20% of graphite powder, 50-65% of nano silver paste, 3-5% of glass powder, 0.5-2% of dendritic organic molecules and 8-41.5% of organic solvent.
Further, the solid content of the nano silver paste is 70-80%, and the particle size is 10 nm-1 μm.
Further, the glass powder is one or more of silicon dioxide, aluminum oxide, sodium oxide and titanium dioxide.
Further, the organic solvent is one or more of ethylene glycol, glycerol, terpineol, turpentine and diethylene glycol butyl ether.
Further, the dendritic organic molecules are one or more of polyamide-amine, polyethylene glycol-polyamide-amine, lysine-polyamide-amine, maleic amide, ammonium chloride, and ethylenediamine-polyamide-amine.
The preparation method of the high-performance graphene composite silver paste comprises the following steps:
s1, sequentially weighing graphite powder, nano silver paste, glass powder, dendritic organic molecules and an organic solvent according to the proportion;
s2, mixing the dendritic organic molecules and graphite powder in an organic solvent, uniformly stirring, and then stripping at a high speed to obtain a graphene organic solution;
s3, adding glass powder into the graphene organic solution, stirring, performing pulse ultrasonic treatment, and concentrating to obtain graphene slurry;
and S4, mixing the graphene slurry with the nano silver paste, and continuously stirring for 12 hours to obtain the graphene composite silver paste.
Further, the high-speed peeling conditions in S2 were: stripping at 3000r/min for 6h at normal temperature and pressure.
Further, in S3, the stirring condition was 1000rpm for 3 hours, and the pulse sonication time was 5 min.
Furthermore, the solid content of the graphene composite silver paste in S3 is 180-210 mg/mL, the sheet diameter is 3-10 μm, and the sheet thickness is 0.5-3 nm.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, graphene is selected as high-concentration graphene organic raw stock obtained under the steric hindrance effect and the interface friction effect of the three-dimensional topological structure dendritic polymer, and the completeness and high conductivity of graphene crystal lattices are ensured by a physical stripping method. The dendritic organic molecules are inserted in the middle of the graphene nanosheets by virtue of steric hindrance, and meanwhile, the three-dimensional topological structure of the dendritic organic molecules provides physical and surface chemical environments for uniform compounding of other organic carriers, inorganic carriers and graphene.
2. According to the invention, the adopted nano silver particles and the dendritic organic molecular chain terminal functional group are compounded under the weak interaction to form a complex of the dendritic molecular terminal functional group and the nano silver particles, and the nano silver is uniformly and tightly attached to the graphene nanosheet with excellent conductivity, so that the graphene stacking is inhibited, and meanwhile, the higher electron transfer rate is provided. The obtained graphene composite silver paste has the advantages of high conductivity, good substrate adhesion, good film flexibility and the like.
3. The preparation method of the high-performance graphene composite silver paste is simple and convenient in process, and does not relate to a harsh reaction process required by redox reaction, long reaction time and complex post-treatment for preparing the composite silver paste. The topological structure, the end group functional group and the interface effect of physical grinding of the dendritic molecules are ingeniously utilized, and the organic assembly of the nano silver particles and the graphene nanosheets is realized, so that the prepared graphene composite silver paste is high in graphene filling amount, the conductivity and the nano silver paste are in the same order of magnitude, and the method is a simple and convenient method for preparing the graphene composite silver paste with low cost, high conductivity and stable performance in a large scale.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are further described below.
The embodiment of the invention provides a preparation method of high-performance graphene composite silver paste, which mainly comprises the following steps:
s1, sequentially weighing graphite powder, nano silver paste, glass powder, dendritic organic molecules and an organic solvent according to the proportion; wherein, graphite powder is 5-20%, nano silver paste is 50-65%, glass powder is 3-5%, dendritic organic molecules are 0.5-2%, and organic solvent is 8-41.5%; under the induction and driving of dendritic organic molecular functional groups, graphene and nano glass powder are macroscopically assembled to form a point-plane combined composite system in which zero-dimensional silver nano particles are uniformly distributed on the surface of a two-dimensional graphene nanosheet;
s2, mixing the dendritic organic molecules and graphite powder in an organic solvent, stirring uniformly, adding mechanical high-speed stripping equipment, continuously shearing and stripping at high density for 6h under the conditions of 3000r/min of rotating speed and normal temperature and pressure, overcoming the van der Waals force effect between graphite flake layers under the steric hindrance effect and the interface friction effect of the three-dimensional topological structure of the dendritic organic molecules, and performing covalent bonding or weak interaction such as static electricity on the abundant functional groups at the starting end of the dendritic organic molecules to play a role in uniformly dispersing and stabilizing high-energy-state graphene so as to finally obtain a high-quality graphene organic solution which is assisted by dendritic polymers and has a complete crystal structure and has the sheet diameter size of less than 10 mu m;
s3, adding glass powder in a certain ratio into the graphene organic solution, continuously stirring for 3 hours at 1000rpm, and then performing pulse ultrasound for 5 minutes to enable the glass powder to be inserted between graphene layers, so that two-dimensional lamellar graphene is isolated and stabilized by cooperating with dendritic organic molecules through steric hindrance and interface action;
s4, concentrating the graphene organic solution until the solid content is 180-210 mg/mL, and obtaining high-concentration graphene slurry with the surface of the graphene nanosheet modified by the dendritic organic molecules; the sheet diameter of the graphene slurry is 3-10 mu m, and the thickness of the sheet layer is 0.5-3 nm;
s5, mixing the graphene slurry and the nano silver paste according to a certain proportion, continuously stirring for 12h, providing rich active sites with the help of a branch terminal functional group of a dendritic organic molecule, forming a silver particle complex of the dendritic organic molecule through weak interaction with silver nanoparticles, and enabling the nano silver particles to be uniformly attached to the graphene nanosheets through macroscopic assembly under the drive of induction and weak interaction of the dendritic molecules to obtain the high-conductivity composite silver paste inlaid with the zero-dimensional nano silver particles and the two-dimensional graphene nanosheets and assisted by the topological dendritic molecules.
< example 1>
The high-performance graphene composite silver paste comprises the following raw materials in percentage by mass: 20% of graphite powder, 65% of nano silver paste, 5% of glass powder, 2% of dendritic organic molecules and 8% of organic solvent.
Wherein: the dendritic organic molecule is a polyamidoamine.
The glass powder is silicon dioxide.
The organic solvent is ethylene glycol: the glycerol is mixed according to the mass ratio of 1:1 to form a mixture.
A preparation method of high-performance graphene composite silver paste comprises the following steps:
weighing graphite powder, nano silver paste, silicon dioxide, polyamide-amine and an organic solvent in sequence according to the proportion;
mixing polyamide-amine and graphite powder in an organic solvent, uniformly stirring, adding mechanical high-speed stripping equipment, and continuously shearing and stripping at a rotating speed of 3000r/min and under normal temperature and pressure for 6h at a high density to finally obtain a polyamide-amine-assisted high-quality graphene organic solution with a complete crystal structure and a sheet diameter of less than 10 microns;
thirdly, adding silicon dioxide into the graphene organic solution, continuously stirring for 3 hours at 1000rpm, and then performing pulse ultrasound for 5 minutes.
And fourthly, evaporating and concentrating the graphene organic solution until the solid concentration is 180-210 mg/mL, and obtaining high-concentration graphene slurry.
And fifthly, mixing the graphene slurry with the nano silver paste, continuously stirring for 12h, and compounding rich active sites provided by the terminal group functional groups of the dendritic organic molecules with the nano silver particles to form the complex of the dendritic organic molecules, so that the silver particles are uniformly attached to the graphene nanosheets, and the high-conductivity composite silver paste which is low in interfacial energy and compatible with the two-dimensional graphene sheets and assisted by the topological dendritic molecules is obtained.
< example 2>
The high-performance graphene composite silver paste comprises the following raw materials in percentage by mass: 15% of graphite powder, 55% of nano silver paste, 4% of glass powder, 1.5% of dendritic organic molecules and 24.5% of organic solvent.
Wherein: the dendritic organic molecule is polyethylene glycol-polyamide-amine.
The glass powder is alumina.
The organic solvent is glycerol: terpineol: the turpentine is mixed according to the mass ratio of 2:1:1 to form a mixture.
A preparation method of high-performance graphene composite silver paste comprises the following steps:
weighing graphite powder, nano silver paste, silicon dioxide, polyamide-amine and an organic solvent in sequence according to the proportion;
mixing polyethylene glycol-polyamide-amine and graphite powder in an organic solvent, uniformly stirring, adding mechanical high-speed stripping equipment, and continuously shearing and stripping at a high density for 6 hours at a rotating speed of 3000r/min under normal temperature and pressure to finally obtain a polyethylene glycol-polyamide-amine-assisted high-quality graphene organic solution with a complete crystal structure and a sheet diameter size of less than 10 microns;
thirdly, adding alumina into the graphene organic solution, continuously stirring for 3 hours at 1000rpm, and then performing pulse ultrasound for 5 min;
fourthly, evaporating and concentrating the graphene organic solution until the solid concentration is 180-210 mg/mL, and obtaining high-concentration graphene slurry;
and fifthly, mixing the graphene slurry with the nano silver paste, continuously stirring for 12h, and compounding rich active sites provided by the terminal group functional groups of the dendritic organic molecules with the nano silver particles to form the complex of the dendritic organic molecules, so that the silver particles are uniformly attached to the graphene nanosheets, and the high-conductivity composite silver paste which is low in interfacial energy and compatible with the two-dimensional graphene sheets and assisted by the topological dendritic molecules is obtained.
< example 3>
The high-performance graphene composite silver paste comprises the following raw materials in percentage by mass: 10% of graphite powder, 60% of nano silver paste, 3% of glass powder, 1% of nano organic molecular crystal or cluster and 26% of organic solvent.
Wherein: the dendritic organic molecules are lysine modified polyamide-amine.
The glass powder is titanium dioxide.
The organic solvent is terpineol: turpentine oil: diethylene glycol was mixed at a mass ratio of 2:1: 1.
The preparation method of the high-performance graphene composite silver paste comprises the following steps:
the method comprises the steps of weighing graphite powder, nano silver paste, glass powder, dendritic organic molecules and an organic solvent in sequence according to a ratio;
mixing the lysine modified polyamide-amine and graphite powder in an organic solvent, uniformly stirring, adding mechanical high-speed stripping equipment, and continuously shearing and stripping at a rotating speed of 3000r/min and under normal temperature and pressure for 6h at a high density to finally obtain a high-quality graphene organic solution which is assisted by the lysine modified polyamide-amine and has a complete crystal structure and a sheet diameter size of less than 10 mu m;
thirdly, adding titanium dioxide into the graphene organic solution, continuously stirring for 3 hours at 1000rpm, and then performing pulse ultrasound for 5 minutes;
fourthly, evaporating and concentrating the graphene organic solution until the solid concentration is 180-210 mg/mL, and obtaining high-concentration graphene slurry;
and fifthly, mixing the graphene slurry with the nano silver paste, continuously stirring for 12h, and compounding rich active sites provided by the terminal group functional groups of the dendritic organic molecules with the nano silver particles to form the complex of the dendritic organic molecules, so that the silver particles are uniformly attached to the graphene nanosheets, and the high-conductivity composite silver paste which is low in interfacial energy and compatible with the two-dimensional graphene sheets and assisted by the topological dendritic molecules is obtained.
< example 4>
The high-performance graphene composite silver paste comprises the following raw materials in percentage by mass: 5% of graphite powder, 50% of nano silver paste, 3% of glass powder, 0.5% of dendritic organic molecules and 41.5% of organic solvent.
Wherein: the dendritic organic molecule is ethylenediamine-polyamidoamine.
The glass powder is sodium oxide.
The organic solvent is ethylene glycol: glycerol: the terpineol is mixed according to the mass ratio of 2:1:1 to form a mixture.
The preparation method of the high-performance graphene composite silver paste comprises the following steps:
the method comprises the steps of weighing graphite powder, nano silver paste, glass powder, dendritic organic molecules and an organic solvent in sequence according to a ratio;
mixing ethylenediamine-polyamide-amine and graphite powder in an organic solvent, uniformly stirring, adding mechanical high-speed stripping equipment, and continuously shearing and stripping at a rotating speed of 3000r/min and under normal temperature and pressure for 6h at a high density to finally obtain an ethylenediamine-polyamide-amine-assisted high-quality graphene organic solution with a complete crystal structure and a sheet diameter of less than 10 microns;
thirdly, adding sodium oxide into the graphene organic solution, continuously stirring for 3 hours at 1000rpm, and then performing pulse ultrasound for 5 minutes.
And fourthly, evaporating and concentrating the graphene organic solution until the solid concentration is 180-210 mg/mL, and obtaining high-concentration graphene slurry.
And fifthly, mixing the graphene slurry with the nano silver paste, continuously stirring for 12h, and compounding rich active sites provided by the terminal group functional groups of the dendritic organic molecules with the nano silver particles to form the complex of the dendritic organic molecules, so that the silver particles are uniformly attached to the graphene nanosheets, and the high-conductivity composite silver paste which is low in interfacial energy and compatible with the two-dimensional graphene sheets and assisted by the topological dendritic molecules is obtained.
< comparative example 1>
The high-performance graphene composite silver paste comprises the following raw materials in percentage by mass: 5% of graphite powder, 65% of nano silver paste, 5% of glass powder, 0.5% of ethyl cellulose and 24.5% of organic solvent.
Wherein: the glass powder is sodium oxide.
The organic solvent is ethylene glycol: glycerol: the terpineol is mixed according to the mass ratio of 2:1:1 to form a mixture.
The preparation method of the high-performance graphene composite silver paste comprises the following steps:
weighing in proportion;
mixing ethyl cellulose and graphite powder in an organic solvent, uniformly stirring, adding mechanical high-speed stripping equipment, and continuously shearing and stripping at a rotating speed of 3000r/min and under normal temperature and pressure for 6h at a high density to finally obtain a graphene organic solution with dispersed ethyl cellulose;
thirdly, adding sodium oxide into the graphene organic solution, continuously stirring for 3 hours at 1000rpm, and then performing pulse ultrasound for 5 minutes;
fourthly, evaporating and concentrating the graphene organic solution until the solid concentration is 180-210 mg/mL, and obtaining high-concentration graphene slurry;
and fifthly, mixing the graphene slurry with the nano silver paste, continuously stirring for 12h, and obtaining the graphene composite silver paste by means of the dispersion effect of the traditional dispersant ethyl cellulose.
< comparative example 2>
The comparison sample is prepared from a viscous conductive silver paste (purchased from Aus Banbury Limited, Shenzhen) which is purchased from the market and consists of metal silver particles, a binder, a solvent and an auxiliary agent, and has high purity and solid content of 65%.
The graphene composite silver paste and the conductive silver paste obtained in the examples 1 to 4 and the comparative examples 1 to 2 are spread on the substrates such as PI, high temperature resistant glass sheets and silicon wafers under the drying conditions of 50 ℃, 100 ℃, 150 ℃, 200 ℃, 250 ℃ and 300 ℃ respectively for 1 hour, and finally the graphene composite silver paste film with the thickness of about 15 μm is obtained. Selecting a film coated with the graphene composite silver paste on the PI substrate as a test object, and comparing the test object with the conductive silver paste, wherein the test result is shown in Table 1:
TABLE 1
As can be seen from table 1, compared with the conductive silver paste prepared in comparative example 2, the high-performance graphene composite silver paste prepared in the invention maintains its high conductivity while reducing the content of silver in the conductive silver paste, and the test sheet resistance of the high-performance graphene composite silver paste is almost close to that of a nano silver paste. Meanwhile, due to the three-dimensional topological space provided by the dendritic organic molecules and the compounding of the organic molecule functional groups and the silver particles, the nano silver complex of the dendritic organic molecules is formed, and finally, the composite structure with the silver particles uniformly dispersed on the surface of the graphene two-dimensional sheet layer is obtained. The adhesive force of the coating obtained under the optimal experimental conditions can reach 4B level, and the total area of the coating falling off is less than 5 percent, which is superior to the adhesive force of the nano silver paste coating in a comparison sample. In addition, compared with the traditional graphene composite silver paste obtained by the assistance of single component ethyl cellulose (comparative example 1), the high-conductivity composite silver paste with the synergistic structure of the zero-dimensional silver particles assisted by the topological dendritic polymer and the two-dimensional graphene sheet layers, which is obtained by the invention, has an obvious conductivity advantage.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes, without departing from the technical spirit of the present invention, and any simple modification, equivalent change and change made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the technical spirit of the present invention.
Claims (9)
1. The high-performance graphene composite silver paste is characterized by comprising the following raw materials in percentage by mass: 5-20% of graphite powder, 50-65% of nano silver paste, 3-5% of glass powder, 0.5-2% of dendritic organic molecules and 8-41.5% of organic solvent.
2. The high-performance graphene composite silver paste according to claim 1, wherein the solid content of the nano silver paste is 70-80%, and the particle size is 10 nm-1 μm.
3. The high-performance graphene composite silver paste according to claim 1, wherein the glass powder is one or more of silicon dioxide, aluminum oxide, sodium oxide and titanium dioxide.
4. The high-performance graphene composite silver paste according to claim 1, wherein the organic solvent is one or more of ethylene glycol, glycerol, terpineol, turpentine and diethylene glycol monobutyl ether.
5. The high-performance graphene composite silver paste according to claim 1, wherein the dendritic organic molecules are one or more of polyamide-amine, polyethylene glycol-polyamide-amine, lysine-polyamide-amine, maleic amide, ammonium chloride with poly (benzyl ether triacetate) and ethylenediamine-polyamide-amine.
6. The preparation method of the high-performance graphene composite silver paste according to any one of claims 1 to 5, wherein the method comprises the following steps:
s1, sequentially weighing graphite powder, nano silver paste, glass powder, dendritic organic molecules and an organic solvent according to the proportion;
s2, mixing the dendritic organic molecules and graphite powder in an organic solvent, uniformly stirring, and then stripping at a high speed to obtain a graphene organic solution;
s3, adding glass powder into the graphene organic solution, stirring, performing pulse ultrasonic treatment, and concentrating to obtain graphene slurry;
and S4, mixing the graphene slurry with the nano silver paste, and continuously stirring for 12 hours to obtain the graphene composite silver paste.
7. The preparation method of the high-performance graphene composite silver paste according to claim 6, wherein the high-speed stripping conditions in S2 are as follows: stripping at 3000r/min for 6h at normal temperature and pressure.
8. The preparation method of the high-performance graphene composite silver paste according to claim 6, wherein stirring conditions in S3 are 1000rpm for 3 hours, and the pulse ultrasonic time is 5 min.
9. The method for preparing the high-performance graphene composite silver paste according to claim 6, wherein the solid content of the graphene composite silver paste in S3 is 180-210 mg/mL, the sheet diameter is 3-10 μm, and the thickness of a sheet layer is 0.5-3 nm.
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| CN111540502A (en) * | 2020-05-06 | 2020-08-14 | 北京石墨烯研究院有限公司 | Graphene-doped front silver paste and preparation method and application thereof |
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