CN115223745A - Electrode slurry, preparation method and filter - Google Patents
Electrode slurry, preparation method and filter Download PDFInfo
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- CN115223745A CN115223745A CN202211008387.6A CN202211008387A CN115223745A CN 115223745 A CN115223745 A CN 115223745A CN 202211008387 A CN202211008387 A CN 202211008387A CN 115223745 A CN115223745 A CN 115223745A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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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
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/20—Frequency-selective devices, e.g. filters
- H01P1/2002—Dielectric waveguide filters
Abstract
The invention discloses electrode paste, a preparation method and a filter, relates to the technical field of electronic materials and component processing, and aims to solve the problems of poor performance adhesive pull force, uneven film thickness and poor strength after drying of the electrode paste. The electrode paste is used for a filter of a ceramic dielectric, and comprises: the silver conductive material comprises a first carrier, a second carrier, a dispersant, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide; the first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1). The slurry is prepared by a slurry preparation method. The invention discloses electrode slurry, a preparation method and the electrode slurry of a filter for preparing a ceramic medium.
Description
Technical Field
The invention relates to the technical field of electronic material and component processing, in particular to electrode slurry, a preparation method and a filter.
Background
The ceramic filter realizes selection and control of signal frequency by printing a circuit on the surface of ceramic and welding the circuit board, and silver has the advantages of strong conductive capability, thermal expansion coefficient close to that of a ceramic blank, good thermal stability, capability of directly welding metal on a silver layer and the like, so that electrode slurry containing silver is one of key materials of the filter, and the conductive performance of the electrode slurry and the compactness of a conductive layer formed by silver paste have important influence on the performance of the filter.
The electrode slurry of the samarium-calcium-aluminum ceramic system filter is prepared by attaching silver slurry to the surface of a samarium-calcium-aluminum ceramic substrate by using a spraying process, and covering a silver film conductive layer on the surface layer of a ceramic body by drying and sintering. However, the performance of the electrode slurry of the samarium-calcium-aluminum ceramic filter at the present stage still has the defects of low Q value, poor adhesive tension, uneven film thickness, poor strength after drying and the like.
Disclosure of Invention
The invention aims to provide electrode paste, a preparation method and a filter, so as to ensure that the prepared electrode paste has the advantages of large adhesion tension, uniform film thickness and high strength after drying.
In order to achieve the above object, the present invention provides an electrode paste for a filter of a ceramic dielectric, comprising:
the silver-based conductive coating comprises a first carrier, a second carrier, a dispersing agent, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide;
the first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1).
Compared with the prior art, in the electrode slurry provided by the invention, the organic solvent contained in the first carrier is alcohol ester twelve, and the used resins are ethyl cellulose and rosin. The ethyl cellulose resin has good film forming property, and a formed film can keep high strength and good toughness at high temperature and low temperature, and in addition, the rosin resin can provide high viscosity after being dissolved by the alcohol ester twelve, so that the first carrier, the second carrier and other raw materials are tightly bonded, and sufficient adhesive strength and excellent long-term stability are provided. The organic solvent contained in the second carrier is terpineol and the thixotropic agent used is hydrogenated castor oil. The hydrogenated castor oil can swell and gel in the terpineol, weak hydrogen bond bonding is generated among swelling particles due to polar groups in the hydrogenated castor oil molecules, a thixotropic network structure is formed, the suspension property of electrode slurry formed in the subsequent steps can be improved, and the sagging of the slurry is controlled without sacrificing the flowing property and the leveling property. Particularly, the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1), under the combined action of the first carrier and the second carrier, the electrode slurry formed in the subsequent steps has fluidity, and meanwhile, the phenomenon of interface sagging is not easy to occur, so that when the electrode slurry is applied to a ceramic filter, the film thickness is uniform, the phenomenon of skinning and bubbling is not generated, and the spraying effect is good. And under the action of the rosin resin, the formed electrode slurry is provided with enough adhesive strength and excellent long-term stability, so that the strength of the electrode slurry after drying is obviously improved in the processes of spraying, drying and the like. And because the metal contained in the glass powder is the same as the metal contained in the metal oxide, the glass powder and the silver powder are sintered, and the weldability and the adhesion tension are improved. In addition, the colloidal organic carrier is obtained after swelling by the organic solvent, and the colloidal organic carrier has better mixing and dispersing performance with subsequent silver conductive materials, metal oxides, glass powder and other materials, and improves the spraying effect and the uniformity and the flatness of the slurry.
In a second aspect, the present invention also provides a method for preparing an electrode paste, comprising providing a first support and a second support;
and mixing a dispersing agent, metal oxide, glass powder, silver powder and a diluent with the first carrier and the second carrier to obtain the electrode slurry.
In a third aspect, the present invention further provides a filter, including: the electrode is made of electrode slurry, and the electrode is made of the electrode slurry by a preparation method.
Compared with the prior art, the preparation method of the electrode slurry and the filter provided by the invention have the same beneficial effects as those of the first aspect, and are not described herein again.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a flow chart for preparing an electrode paste provided in this example;
FIG. 2 (a) is an electron micrograph showing a first appearance of an electrode paste according to a first embodiment of the present invention after sintering;
FIG. 2 (b) is a second appearance electron microscope image of the electrode paste after sintering according to the first embodiment of the invention;
FIG. 3 (a) is an electron micrograph showing a first appearance of an electrode paste according to a second example of the present invention after sintering;
fig. 3 (b) shows a second appearance electron microscope image of the electrode paste of the second embodiment of the present invention after sintering.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise. The meaning of "a number" is one or more unless specifically limited otherwise.
At the present stage, the defects of low Q value, poor adhesive force, uneven film thickness, poor strength after drying and the like still exist in the performance of the electrode slurry of the samarium-calcium-aluminum ceramic system filter.
To overcome this phenomenon, an embodiment of the present invention provides an electrode paste for a filter of a ceramic dielectric, including: the silver conductive material comprises a first carrier, a second carrier, a dispersing agent, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide. Wherein the first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1).
Illustratively, the first carrier comprises an alcohol ester twelve organic solvent and the resins used are ethyl cellulose and rosin. The ethyl cellulose resin has good film forming property, and a formed film can keep high strength and good toughness at high temperature and low temperature, and in addition, the rosin resin can provide high viscosity after being dissolved by the alcohol ester, so that the first carrier, the second carrier and other raw materials are tightly bonded, and sufficient adhesive strength and excellent long-term stability are provided. The organic solvent contained in the second carrier is terpineol and the thixotropic agent used is hydrogenated castor oil. The hydrogenated castor oil can swell and gel in the terpineol, weak hydrogen bond bonding is generated among swelling particles due to polar groups in the hydrogenated castor oil molecules, a thixotropic network structure is formed, the suspension property of electrode slurry formed in the subsequent steps can be improved, and the sagging of the slurry is controlled without sacrificing the flowing property and the leveling property. Particularly, the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1), under the combined action of the first carrier and the second carrier, the electrode slurry formed in the subsequent steps has fluidity, and meanwhile, the phenomenon of interface sagging is not easy to occur, so that when the electrode slurry is applied to a ceramic filter, the film thickness is uniform, the phenomenon of skinning and bubbling is not generated, and the spraying effect is good. And under the action of the rosin resin, the formed electrode slurry is provided with enough adhesive strength and excellent long-term stability, so that the strength of the electrode slurry after drying is obviously improved in the processes of spraying, drying and the like. And because the metal contained in the glass powder is the same as the metal contained in the metal oxide, the glass powder and the silver powder are sintered, and the weldability and the adhesion tension are improved. In addition, the colloidal organic carrier is obtained after swelling by the organic solvent, and the colloidal organic carrier has better mixing and dispersing performance with subsequent silver conductive materials, metal oxides, glass powder and other materials, and improves the spraying effect and the uniformity and the flatness of the slurry.
Illustratively, in the first carrier, the mass parts of alcohol ester twelve are 215 to 220, the mass parts of ethyl cellulose are 45 to 50, and the mass parts of rosin are 30 to 35; in the second carrier, the mass portion of the terpineol is 70-75 parts, and the mass portion of the hydrogenated castor oil is 25-30 parts. The strength of the first carrier and the second carrier prepared in the mass part range is obviously improved after drying, and can reach 4B as measured by experiments, the resin can be fully expanded in an organism system to form layer-by-layer coating, and under the influence of a proper amount of thixotropic agent, the electrode slurry can have fluidity and is not easy to generate an interface sagging phenomenon, the effect is excellent during spraying, and the thickness is uniform and does not peel.
In an optional manner, the mass parts of the dispersant, the metal oxide, the glass powder, the silver conductive material, the first carrier and the second carrier are 0.1 to 1 part, 0.2 to 1 part, 0.5 to 1.5 parts, 75 to 80 parts, 10 to 15 parts and 0.5 to 1 part, respectively.
Illustratively, the metal oxide is at least one of bismuth oxide and cuprous oxide, and the glass frit is a Bi — Cu — Sm system glass frit. Wherein, for the Bi-Cu-Sm system glass powder, the glass powder at least comprises bismuth oxide, cuprous oxide and samarium oxide, and can also comprise one or more of lithium oxide, sodium oxide, potassium oxide, magnesium oxide, calcium oxide, strontium oxide, barium oxide, phosphorus oxide, titanium oxide and nickel oxide. In the sintering process, organic resin and organic solvent are volatilized and decomposed, bi-Cu-Sm system glass powder is fused into a film which can form a firm and conductive coating with a silver conductive material, but when the glass powder is used alone to participate in the reaction, the adhesive force of the prepared electrode slurry can not meet the requirement of tension, so that metal oxide is required to be matched with the glass powder for the reaction. The experiment shows that the adhesive force of the prepared electrode slurry can be remarkably improved especially when bismuth oxide and cuprous oxide are used for being matched with bismuth-copper-samarium system glass for sintering.
Illustratively, the dispersant used in the embodiments of the present invention is a cationic surfactant, which can improve the storage stability of the resulting electrode slurry. The cationic surfactant is at least one of dodecyl trimethyl ammonium bromide and dodecyl dimethyl benzyl ammonium chloride. In the embodiment of the invention, a diluent can be used, wherein the diluent is 10-14 parts by mass and is at least one of acetone, ethanol and glycol monoethyl ether.
Illustratively, the silver conductive material includes at least two different morphologies of silver conductive material; when the form of the silver conductive material is spherical, the average grain diameter of the spherical silver conductive material is 1.5-2 μm; when the silver conductive material is in the form of a flake, the average particle diameter of the flake-shaped silver conductive material is 3.5 μm to 4.5. Mu.m.
As an example, the silver conductive material is a main component of the electrode paste, and its content in the electrode paste is directly related to the conductive property. When the silver conductive material is 75 to 80 parts by mass, it is advantageous to improve its conductivity. In practical application, if the mass part of the silver conductive material exceeds 80 parts, the conductivity of the silver conductive material cannot be improved, the probability of being coated by resin is low, the adhesive force of the silver conductor is reduced after the silver conductive material is solidified into a film, and the silver conductive material is in danger of falling off; when the mass fraction of the silver conductive material is less than 60 parts, the change in resistance is unstable. Furthermore, the average particle diameter of the silver conductive material is also related to the conductive property of the electrode paste. Under the same volume, the average grain diameter of the silver conductive material is small, the contact probability among the silver conductive materials is higher, and the conductivity is improved. And the reserved space is smaller, so that the phenomenon that the reserved larger space is blocked by nonconductive resins such as ethyl cellulose, rosin and the like due to the large average particle diameter of the silver conductive material is avoided, and the reduction of the conductivity is avoided. Therefore, when the spherical silver conductive material with the average grain diameter of 1.5-2 μm is selected, the prepared electrode slurry has high conductive performance. Similarly, when the flake-shaped silver conductive material with the average grain diameter of 3.5-4.5 μm is selected, the prepared electrode paste has higher conductive performance.
Fig. 1 shows a flow chart of the preparation of the electrode paste provided in this example. As shown in fig. 1, the preparation method of the electrode paste provided by the present invention comprises:
step 101: a first carrier and a second carrier are provided.
Illustratively, 215-220 parts by mass of twelve organic solvent alcohol ester are placed in a container, and the container is placed in a water bath kettle at 75-90 ℃ for preheating. Weighing 45-50 parts by mass of ethyl cellulose and 30-35 parts by mass of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at a rotation speed of 900-2000 r/min to prepare the first carrier. Placing 70-75 parts by mass of terpineol in a container, and placing the container in a water bath kettle at 75-90 ℃ for preheating. Weighing 25-30 parts by mass of hydrogenated castor oil, adding the hydrogenated castor oil into preheated terpineol, and dispersing for 2 hours at the rotating speed of 900-2000 r/min to prepare the second carrier. Wherein, if hydrogenated castor oil is added to terpineol above 90 ℃ and the dispersion time is less than or equal to 30 min-40 min, the hydrogenated castor oil can not form thixotropic gel network and can separate out 'grains'.
Step 102: and mixing a dispersing agent, metal oxide, glass powder, a silver conductive material and a diluent with the first carrier and the second carrier to obtain the electrode slurry.
Illustratively, 0.1-1 part by mass of a dispersant, 0.2-1 part by mass of a metal oxide, 0.5-1.5 parts by mass of glass powder, 75-80 parts by mass of a silver conductive material, 10-15 parts by mass of a prepared first carrier and 0.5-1 part by mass of a second carrier are added into a container, the materials in the container are fully dispersed by using a homogenizer, and the material is rolled by a three-roll mill to ensure that the fineness is below 7 after the materials are uniformly dispersed. At this time, 10 to 14 parts by mass of a diluent can be added to meet the spraying requirement of the slurry.
The embodiment of the invention also provides a filter, which comprises a ceramic medium and an electrode formed on the ceramic medium, wherein the electrode is made of the electrode slurry and is prepared by the preparation method of the electrode slurry.
In order to verify the effects of the electrode paste provided in the examples of the present invention, the examples of the present invention were demonstrated by comparing the examples with comparative examples.
Example one
The embodiment of the invention provides electrode slurry for a filter of a ceramic medium, which comprises the following components: the silver conductive material comprises a first carrier, a second carrier, a dispersing agent, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide. The first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1). An appearance electron microscope image after sintering the electrode slurry is shot for 2 times, and fig. 2 (a) shows a first appearance electron microscope image after sintering the electrode slurry of the first embodiment of the invention;
fig. 2 (b) shows a second appearance electron microscope image of the electrode paste according to the first embodiment of the present invention after sintering. As can be seen from fig. 2 (a) and 2 (b), the electrode paste according to the first embodiment of the present invention has a uniform surface and small pores after being sintered.
The preparation method of the electrode slurry provided by the embodiment of the invention comprises the following steps:
a first step of preparing a first carrier and a second carrier: 219.6g of the alcohol ester twelve was placed in a vessel, which was preheated in a 75 ℃ water bath. Weighing 49.4g of ethyl cellulose and 31g of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at the rotating speed of 900r/min to prepare the first carrier. 75g of terpineol was placed in a container, and the container was placed in a water bath at 90 ℃ for preheating. Weighing 25g of hydrogenated castor oil, adding the hydrogenated castor oil into preheated terpineol, and dispersing for 2 hours at the rotating speed of 2000r/min to prepare a second carrier.
Step two, preparing electrode slurry: adding 0.6g of dodecyl trimethyl ammonium bromide, 0.3g of bismuth oxide, 0.2g of cuprous oxide, 0.7g of bismuth-copper-samarium system glass, 75g of spherical silver conductive material with the average particle size of 1.5-2 mu m, 12g of prepared first carrier and 0.5g of prepared second carrier into a container; and fully dispersing the materials in the container by using a homogenizer, and rolling by using a three-roll mill after uniform dispersion to ensure that the fineness is below 7. 10ml acetone (analytical grade) was added to bring the slurry to the spray requirements. The performance of the electrode slurry was tested as shown in table 1.
Example two
The embodiment of the invention provides electrode slurry for a filter of a ceramic medium, which comprises the following components: the silver conductive material comprises a first carrier, a second carrier, a dispersing agent, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide. The first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1). An appearance electron microscope image after sintering the electrode slurry is shot for 2 times, and fig. 3 (a) shows a first appearance electron microscope image after sintering the electrode slurry of the second embodiment of the invention;
fig. 3 (b) shows a second appearance electron microscope image of the electrode paste of the second embodiment of the present invention after sintering. As can be seen from fig. 3 (a) and 3 (b), the electrode paste according to the second embodiment of the present invention has a uniform surface and smaller pores after sintering.
The preparation method of the electrode slurry provided by the embodiment of the invention comprises the following steps:
a first step of preparing a first carrier and a second carrier: 216g of the alcohol ester twelve was placed in a vessel, which was preheated in a water bath at 80 ℃. Weighing 46g of ethyl cellulose and 30g of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at the rotating speed of 900r/min to prepare the first carrier. 70g of terpineol was placed in a container, and the container was placed in a water bath at 90 ℃ for preheating. Weighing 30g of hydrogenated castor oil, adding the hydrogenated castor oil into preheated terpineol, and dispersing for 2 hours at the rotating speed of 2000r/min to prepare a second carrier.
Step two, preparing electrode slurry: adding 0.5g of dodecyl dimethyl benzyl ammonium chloride, 0.5g of bismuth oxide, 0.5g of cuprous oxide, 1.5g of bismuth-copper-samarium system glass, 75g of spherical silver conductive material with the average particle size of 1.5-2 mu m, 11g of prepared first carrier and 1.0g of prepared second carrier into a container; and fully dispersing the material in the container by using a homogenizer, and rolling by using a three-roll mill after uniform dispersion to ensure that the fineness is below 7. 11ml of ethanol (analytical grade) was added to bring the slurry to spray requirements. The results of the performance test of the electrode slurry are shown in table 1.
EXAMPLE III
The embodiment of the invention provides electrode slurry for a filter of a ceramic medium, which comprises the following components: the silver conductive material comprises a first carrier, a second carrier, a dispersing agent, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide. The first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1).
The preparation method of the electrode slurry provided by the embodiment of the invention comprises the following steps:
a first step of preparing a first carrier and a second carrier: 215g of the alcohol ester twelve was placed in a vessel, which was preheated in a water bath at 85 ℃. Weighing 50g of ethyl cellulose and 35g of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at the rotating speed of 1000r/min to prepare the first carrier. 74g of terpineol was placed in a container, which was placed in a water bath at 90 ℃ for preheating. 26g of hydrogenated castor oil is weighed, added into preheated terpineol and dispersed for 2 hours at the rotating speed of 1500r/min to prepare a second carrier.
Step two, preparing electrode slurry: adding 1.0g of dodecyl dimethyl benzyl ammonium chloride, 0.1g of bismuth oxide, 0.1g of cuprous oxide, 0.8g of bismuth-copper-samarium system glass, 75g of flake silver conductive material with the average particle size of 3.5-4.5 mu m, 10.5g of prepared first carrier and 0.5g of prepared second carrier into a container; and fully dispersing the materials in the container by using a homogenizer, and rolling by using a three-roll mill after uniform dispersion to ensure that the fineness is below 7. 12ml of ethylene glycol monoethyl ether (analytically pure) was added to bring the slurry to the spray requirements. The results of the performance test of the electrode slurry are shown in table 1.
Example four
The embodiment of the invention provides electrode slurry for a filter of a ceramic medium, which comprises the following components: the silver conductive material comprises a first carrier, a second carrier, a dispersing agent, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide. The first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1).
The preparation method of the electrode slurry provided by the embodiment of the invention comprises the following steps:
a first step of preparing a first carrier and a second carrier: 215g of the alcohol ester twelve was placed in a vessel, which was preheated in a water bath at 80 ℃. Weighing 50g of ethyl cellulose and 35g of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at the rotating speed of 1000r/min to prepare the first carrier. 74g of terpineol was placed in a container, and the container was placed in a water bath at 90 ℃ for preheating. 26g of hydrogenated castor oil is weighed and added into preheated terpineol, and dispersed for 2 hours at the rotating speed of 1500r/min to prepare a second carrier.
Step two, preparing electrode slurry: adding 0.1g of dodecyl dimethyl benzyl ammonium chloride, 0.1g of bismuth oxide, 0.1g of cuprous oxide, 0.8g of bismuth-copper-samarium system glass, 55g of spherical silver conductive material with the average particle size of 1.5-2 mu m, 20g of flake silver conductive material with the average particle size of 3.5-4.5 mu m, 11.4g of prepared first carrier and 0.5g of prepared second carrier into a container; and fully dispersing the material in the container by using a homogenizer, and rolling by using a three-roll mill after uniform dispersion to ensure that the fineness is below 7. 12ml of ethylene glycol monoethyl ether (analytically pure) was added to bring the slurry to the spray requirements. The results of the performance test of the electrode slurry are shown in table 1.
Comparative example 1
The comparative example of the present invention provides an electrode paste for a filter of a ceramic dielectric, comprising: the silver conductive material comprises a first carrier, a second carrier, a dispersing agent, glass powder and a silver conductive material. The first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1).
The preparation method of the electrode slurry provided by the comparative example comprises the following steps:
a first step of preparing a first carrier and a second carrier: 215g of the alcohol ester twelve was placed in a vessel, which was preheated in a water bath at 80 ℃. Weighing 50g of ethyl cellulose and 35g of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at the rotating speed of 1000r/min to prepare the first carrier. 74g of terpineol was placed in a container, which was placed in a water bath at 90 ℃ for preheating. 26g of hydrogenated castor oil is weighed, added into preheated terpineol and dispersed for 2 hours at the rotating speed of 1500r/min to prepare a second carrier.
Step two, preparing electrode slurry: adding 0.1g of dodecyl dimethyl benzyl ammonium chloride, 1.0g of bismuth-copper-samarium system glass, 55g of spherical silver conductive material with the average particle size of 1.5-2 mu m, 20g of sheet-shaped silver conductive material with the average particle size of 3.5-4.5 mu m, 11.4g of prepared first carrier and 0.5g of prepared second carrier into a container; and fully dispersing the material in the container by using a homogenizer, and rolling by using a three-roll mill after uniform dispersion to ensure that the fineness is below 7. 12ml of ethylene glycol monoethyl ether (analytical grade) was added to bring the slurry to the spray requirements. The results of the performance test of the electrode slurry are shown in table 1.
Comparative example No. two
The invention provides an electrode slurry for a filter of a ceramic dielectric, comprising: the silver conductive material comprises a first carrier, a dispersing agent, glass powder and a silver conductive material. The first carrier comprises alcohol ester twelve, ethyl cellulose and rosin.
The preparation method of the electrode slurry provided by the comparative example comprises the following steps:
first step, preparing a first carrier: 215g of the alcohol ester twelve was placed in a vessel, which was preheated in a water bath at 80 ℃. Weighing 50g of ethyl cellulose and 35g of rosin, adding the raw materials into preheated alcohol ester twelve, and dispersing for 2 hours at the rotating speed of 1000r/min to prepare the first carrier.
Step two, preparing electrode slurry: adding 0.1g of dodecyl dimethyl benzyl ammonium chloride, 1.0g of bismuth-copper-samarium system glass, 55g of spherical silver conductive material with the average particle size of 1.5-2 mu m, 20g of sheet-shaped silver conductive material with the average particle size of 3.5-4.5 mu m, 11.4g of prepared first carrier and 0.5g of prepared second carrier into a container; and fully dispersing the material in the container by using a homogenizer, and rolling by using a three-roll mill after uniform dispersion to ensure that the fineness is below 7. 12ml of ethylene glycol monoethyl ether (analytically pure) was added to bring the slurry to the spray requirements. The results of the performance test of the electrode slurry are shown in table 1.
Table 1 results of performance test of electrode pastes of examples one to four and comparative examples one to two
As can be seen from Table 1, the electrode pastes according to the examples one to four and the comparative examples one to twoThe adhesion of the paste was tested twice, which shows that the electrode pastes prepared in examples one to four had large adhesion and no chance was found in the test results. The electrode pastes prepared in the first and second comparative examples have small adhesive force, and 29.8N/mm in an adhesive force test 2 ～36.2N/mm 2 The welding spot is dropped off and no ceramic body is carried away, which shows that the adhesive force of the prepared electrode slurry is obviously improved by using metal oxides (such as bismuth oxide and cuprous oxide) in combination with the glass powder. Furthermore, as can be seen from table 1, the Q values of the first to fourth examples of the present invention are much larger than those of the first to second comparative examples. In addition, as shown in fig. 2 (a), fig. 2 (b), fig. 3 (a) and fig. 3 (b), in the embodiment of the present invention, when the first carrier including the alcohol ester dodeca, the ethyl cellulose and the rosin and the second carrier including the terpineol and the hydrogenated castor oil are added to the raw materials, under the combined action of the two carriers, the sintered electrode paste has a uniform film thickness, does not generate a peeling and foaming phenomenon, and has a good spraying effect. Next, of examples one to four and comparative examples one to two, examples one to four and comparative example one using the first support and the second support were higher in dry strength, while comparative example two not using the second support was much lower in dry strength than examples one to four and comparative example one.
While the foregoing is directed to embodiments of the present invention, it will be apparent that various modifications and combinations can be made without departing from the spirit and scope of the invention. Accordingly, the specification and figures are merely exemplary of the invention as defined in the appended claims and are intended to cover any and all modifications, variations, combinations, or equivalents within the scope of the invention. It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. Any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present disclosure, and all such changes or substitutions are included in the scope of the present disclosure. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An electrode paste for a filter for a ceramic dielectric, the electrode paste comprising: the silver conductive material comprises a first carrier, a second carrier, a dispersant, a metal oxide, glass powder and a silver conductive material, wherein the metal contained in the glass powder is the same as the metal contained in the metal oxide;
the first carrier comprises alcohol ester dodeca, ethyl cellulose and rosin, the second carrier comprises terpineol and hydrogenated castor oil, and the mass ratio of the first carrier to the second carrier is (10-15): (0.5-1).
2. The electrode slurry according to claim 1, wherein the first carrier contains 215 to 220 parts by mass of the alcohol ester twelve, 45 to 50 parts by mass of the ethyl cellulose, and 30 to 35 parts by mass of the rosin;
in the second carrier, the mass portion of the terpineol is 70-75 parts, and the mass portion of the hydrogenated castor oil is 25-30 parts.
3. The electrode paste according to claim 1, wherein the dispersant is 0.1 to 1 part by mass, the metal oxide is 0.2 to 1 part by mass, the glass frit is 0.5 to 1.5 parts by mass, the silver conductive material is 75 to 80 parts by mass, the first carrier is 10 to 15 parts by mass, and the second carrier is 0.5 to 1 part by mass.
4. The electrode paste as claimed in claim 3, wherein the metal oxide is at least one of bismuth oxide and cuprous oxide, and the glass frit is a Bi-Cu-Sm system glass frit.
5. The electrode slurry of claim 3, wherein the silver conductive material comprises at least two different morphologies of silver conductive material;
when the form of the silver conductive material is spherical, the average grain diameter of the spherical silver conductive material is 1.5-2 μm; when the silver conductive material is in the form of a sheet, the average particle diameter of the sheet-shaped silver conductive material is 3.5 μm to 4.5 μm.
6. The electrode slurry according to claim 3, wherein the dispersant is a cationic surfactant, and the cationic surfactant is at least one of dodecyltrimethylammonium bromide and dodecyldimethylbenzylammonium chloride.
7. A method for preparing electrode paste, comprising:
providing a first carrier and a second carrier;
and mixing a dispersing agent, a metal oxide, glass powder, a silver conductive material and a diluent with the first carrier and the second carrier to obtain the electrode slurry.
8. The method of preparing an electrode slurry according to claim 7, wherein the providing the first support and the second support includes:
heating alcohol ester twelve in water bath, mixing ethyl cellulose, rosin and the heated alcohol ester twelve, and stirring to obtain the first carrier;
and heating terpineol in a water bath, mixing hydrogenated castor oil with the heated terpineol, and stirring to obtain the second carrier.
9. The method for preparing electrode slurry according to claim 8, wherein the heating temperature is 75 ℃ to 90 ℃; the stirring speed is 900r/min to 2000r/min.
10. A filter comprising a ceramic dielectric and an electrode formed on the ceramic dielectric, wherein the electrode is made of the electrode paste according to any one of claims 1 to 6, and the electrode is made of the electrode paste according to any one of claims 7 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116543948A (en) * | 2023-06-30 | 2023-08-04 | 浙江晶科新材料有限公司 | Silver-aluminum paste for N-type TOPCON solar cell and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116543948A (en) * | 2023-06-30 | 2023-08-04 | 浙江晶科新材料有限公司 | Silver-aluminum paste for N-type TOPCON solar cell and preparation method thereof |
| CN116543948B (en) * | 2023-06-30 | 2023-10-31 | 浙江晶科新材料有限公司 | Silver-aluminum paste for N-type TOPCON solar cell and preparation method thereof |
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