CN116665987A - High-printability roll printing slurry and preparation process thereof - Google Patents
High-printability roll printing slurry and preparation process thereof Download PDFInfo
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- CN116665987A CN116665987A CN202310664188.9A CN202310664188A CN116665987A CN 116665987 A CN116665987 A CN 116665987A CN 202310664188 A CN202310664188 A CN 202310664188A CN 116665987 A CN116665987 A CN 116665987A
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- 239000002002 slurry Substances 0.000 title claims abstract description 65
- 238000007639 printing Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 230000000694 effects Effects 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000000853 adhesive Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000010008 shearing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 8
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000001856 Ethyl cellulose Substances 0.000 claims description 6
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 6
- 229910002113 barium titanate Inorganic materials 0.000 claims description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 6
- 229920001249 ethyl cellulose Polymers 0.000 claims description 6
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- VATRWWPJWVCZTA-UHFFFAOYSA-N 3-oxo-n-[2-(trifluoromethyl)phenyl]butanamide Chemical compound CC(=O)CC(=O)NC1=CC=CC=C1C(F)(F)F VATRWWPJWVCZTA-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Chemical group C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Chemical group O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004840 adhesive resin Substances 0.000 claims description 2
- 229920006223 adhesive resin Polymers 0.000 claims description 2
- 229910021523 barium zirconate Inorganic materials 0.000 claims description 2
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 2
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 claims description 2
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011267 electrode slurry Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 claims description 2
- 239000003822 epoxy resin Chemical group 0.000 claims description 2
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 2
- 150000002602 lanthanoids Chemical class 0.000 claims description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
- 239000001095 magnesium carbonate Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- 229920000647 polyepoxide Chemical group 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 2
- 229940116411 terpineol Drugs 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Chemical group OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010020 roller printing Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
- H01G4/008—Selection of materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Conductive Materials (AREA)
- Powder Metallurgy (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a preparation process of high-printability roll printing slurry, which comprises the following steps: step one: stirring and mixing the co-materials by using a planetary grinder at the rotating speed of 250-500rpm for 2-4 hours to obtain a co-material mixture; step two: then, shearing and dispersing the mixture after the step one by using a three-roller mill, wherein the rotating speed is 400-600rpm, and the time is 1-1.5h, so as to achieve the effect of dispersing the co-material particles, and the step three: and (3) adding metal powder and an adhesive into the mixture obtained in the step two, and mixing by using a double-planetary mixer at the rotating speed of 200-300rpm for 30-60min to obtain a slurry mixture. The roll printing paste prepared by the treatment has good dispersibility, smooth and uniform paste distribution, no powder agglomeration and agglomeration phenomenon when observed under an electron microscope, and the printing pattern is smooth, has no edge seepage and high printing property and high product reliability when the roll printing process is performed by using the paste.
Description
Technical Field
The invention relates to the technical field of roller printing slurry preparation, in particular to high-printability roller printing slurry and a preparation process thereof.
Background
With the development of vehicle-mounted electronic and high-end 5G mobile phone communication, the domestic demand for high-end MLCC is increasing, the development trend is gradually from past 100nF capacity to 10 mu F and 100 mu F, and meanwhile, the reliability requirement is also higher and higher, and particularly, the temperature characteristic requirement of the vehicle-mounted electronic is that the temperature is 150 ℃, and the temperature of the corresponding MLCC product with X5R, X R characteristic is higher than the temperature of 85 ℃ and 125 ℃. On the other hand, the capacity of the conventional screen printing cannot meet the market demand due to the increase of the demand, and there is an urgent need for a production mode with high efficiency to improve the capacity and meet the market demand.
The roll printing process printing is applied to the production of MLCC products due to high production efficiency and high reliability. It is known that the efficiency of a roll printing process production line is more than 10 times that of a silk screen printing process line, and manufacturers gradually introduce the roll printing process production line for this purpose, so that the production efficiency is improved, and the productivity scale is enlarged. In order to match the roll printing paste printed by the roll printing process, the import is mainly relied on in China at present, and mature roll printing paste products are temporarily absent.
In this regard, a process technology for preparing a roll printing paste is provided, the paste prepared by using the process technology has high printability, can be matched with the roll printing process printing technology, has smooth patterns after printing, has no problems of edge penetration and tailing, and has high reliability.
Patent CN113823437B "a roll printing paste for MLCC intaglio printing process and a preparation process thereof" discloses a novel method for manufacturing a roll printing paste, which comprises the specific operations of firstly stirring and dispersing metal powder, adhesive and solvent by using a planetary stirrer to obtain a paste semi-finished product, and then performing high-pressure dispersion treatment by using a high-pressure homogenizer. And filtering to obtain the finished slurry. The method can meet the basic dispersion of the roll printing slurry, but the dispersed semi-finished product has more coarse grains due to insufficient shearing force of the dispersion effect of the planetary mixer, so that the high-pressure homogenizer is difficult to process, the prepared slurry has insufficient dispersibility, the printed pattern has burrs and edge seepage, the requirement of high printability cannot be met, and the reliability of the prepared MLCC product cannot meet the requirement of high-end MLCC.
Disclosure of Invention
The invention aims to provide high-printability roller printing slurry and a preparation process thereof, which solve the problems of burrs and edge penetration of printed patterns caused by insufficient slurry dispersion effect and agglomerated coarse grains, meet the printability requirement of the roller printing slurry for high-end MLCC, and meet the electrical property and reliability of products.
In order to achieve the above purpose, the present invention provides the following technical solutions: a process for preparing a high printability roll printing paste comprising the steps of:
step one: stirring and mixing the co-materials by using a planetary grinder at the rotating speed of 250-500rpm for 2-4 hours to obtain a co-material mixture;
step two: then, shearing and dispersing the mixture obtained in the step one by using a three-roller mill, wherein the rotating speed is 400-600rpm, and the time is 1-1.5 hours, so that the effect of dispersing the co-material particles is achieved;
step three: adding metal powder and an adhesive into the mixture obtained in the step two, and mixing by using a double-planetary mixer at the rotating speed of 200-300rpm for 30-60min to obtain a slurry mixture;
step four: shearing and dispersing the mixture obtained in the step three by using a nano sand mill at the rotating speed of 2000-3000rpm for 2-3 hours to achieve the effect of primarily dispersing the slurry powder;
step five: finally, re-refining and dispersing the slurry after the fourth dispersing step by using a circulating dispersing machine; the rotating speed is 2000-2500rpm, the dispersing time is 3-4 hours, and the good dispersing of the roll printing paste is finally realized;
step six: and (3) filtering the slurry obtained in the step five, selecting a filter element with the filter element specification of 0.4-3.0 mu m according to the type of the product, filtering at the pressure of 0.1-0.8mpa, and packaging to obtain the finished slurry.
Preferably, the double-planetary mixer is provided with two closed square stirring heads, is attached to the inner wall by less than or equal to 2mm, and can perform revolution and rotation simultaneously, so that powder is fully mixed without being adhered to the inner wall.
Preferably, the nickel internal electrode slurry comprises the following components in percentage by weight:
40-60% of nickel powder, wherein the nickel powder can be selected from 80-400 nm particle size, sphere-like shape and good crystallinity;
5-10% of ceramic additive, wherein the optional types of the ceramic additive comprise, but are not limited to, barium titanate, calcium titanate, strontium titanate, barium zirconate titanate, calcium strontium zirconate, and the particle size range comprises 10-300 nm;
0.5-3.5% of additive, wherein the optional additive comprises manganese dioxide, zirconium dioxide, barium carbonate, yttrium oxide, magnesium carbonate, titanium dioxide, silicon oxide, aluminum oxide, lithium oxide, most lanthanide rare earth elements and the like, and the particle size of the powder is less than 100nm;
25-45% of a solvent, wherein the solvent can be selected from cyclic ethanol acetate, methyl acetate, ethyl acetate, terpineol, n-propanol, dipropylene glycol dimethyl ether, hydrogenated terpineol and other solvents meeting environmental protection requirements;
3-4% of adhesive resin, and the organic resin can be selected from ethyl cellulose, rosin, epoxy resin, powder ring resin, polyvinyl butyral, acrylic resin, etc.
Compared with the prior art, the invention has the following beneficial effects:
1. the roll printing slurry prepared by the treatment has good dispersibility, and no slurry is evenly distributed and smooth and no powder agglomeration phenomenon is caused when observed under an electron microscope.
2. The invention performs roller printing process printing by using the sizing agent, the printed pattern is smooth, no edge seepage exists, the printing performance is high, and the product reliability is high.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is an SEM image of 20000x slurry in example 1 of the present invention;
FIG. 2 is a view of the pattern after printing by the roll printing process in example 1 of the present invention under a 200X microscope;
FIG. 3 is an SEM image of 20000x slurry according to example 2 of the present invention;
FIG. 4 is a view of the pattern printed by the roll printing process in example 2 of the present invention under a 200X microscope;
FIG. 5 is an SEM image of 20000x slurry according to comparative example 1 of the present invention;
FIG. 6 is a view of the pattern printed by the roll printing process in comparative example 1 of the present invention under a 200X microscope;
FIG. 7 is an SEM image of 20000x slurry according to comparative example 2 of the present invention;
fig. 8 is a view of the pattern printed by the roll printing process in comparative example 2 of the present invention under a 200x microscope.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Embodiment case 1:
in one embodiment of the process for preparing the roll printing slurry, the slurry comprises the following components in parts by weight: 55 parts of nickel powder, 6 parts of barium titanate, 1 part of additive, 34 parts of hydrogenated terpineol and 4 parts of ethyl cellulose. The preparation process comprises the following steps:
step one: stirring and mixing the co-materials by using a planetary grinder, wherein the rotating speed is 250rpm, and the time is 3 hours, so as to obtain a co-material mixture;
step two: then, shearing and dispersing the mixture obtained in the step one by using a three-roller mill, wherein the rotating speed is 400rpm, and the time is 1.5 hours, so that the effect of dispersing the co-material particles is achieved;
step three: adding metal powder and an adhesive into the mixture obtained in the step two, and mixing by using a double-planetary mixer at the rotating speed of 200rpm for 60min to obtain a slurry mixture;
step four: shearing and dispersing the mixture obtained in the step three by using a nano sand mill at the rotating speed of 2000rpm for 3 hours to achieve the effect of primarily dispersing the slurry powder;
step five: carrying out re-refining dispersion treatment on the slurry after the step four dispersion by using a circulating dispersion machine; the rotating speed is 2000rpm, the dispersing time is 3 hours, and the roll printing paste is refined and dispersed;
step six: and (3) filtering the slurry obtained in the step five, wherein the specification of the filter element is 0.5 mu m, the filtering pressure is 0.2mpa, and packaging to obtain the finished slurry.
As shown in figure 1, when observed under SEM at 20000x, the slurry is evenly dispersed and distributed, and the phenomenon of powder agglomeration and caking is avoided. The pattern printed by the roll printing process is observed under a 200x microscope (as shown in fig. 2), and the printed pattern is flat, has no edge penetrating and has high printability. Meanwhile, the reliability of the MLCC product measured after lamination-cutting-adhesive discharging-sintering-end capping-end firing-deposition is high as shown in table 1.
Embodiment case 2:
in one embodiment of the process for preparing the roll printing slurry, the slurry comprises the following components in parts by weight: 45 parts of nickel powder, 6 parts of barium titanate, 1 part of additive, 44 parts of hydrogenated terpineol and 4 parts of ethyl cellulose. The preparation process comprises the following steps:
step one: stirring and mixing the co-materials by using a planetary grinder, wherein the rotating speed is 400rpm, and the time is 2 hours, so as to obtain a co-material mixture;
step two: then, shearing and dispersing the mixture obtained in the step one by using a three-roller mill, wherein the rotating speed is 600rpm, and the time is 1h, so that the effect of dispersing the co-material particles is achieved;
step three: adding metal powder and an adhesive into the mixture obtained in the step two, and mixing by using a double-planetary mixer at the rotating speed of 250rpm for 60min to obtain a slurry mixture;
step four: shearing and dispersing the mixture after the step three by using a nano sand mill, wherein the rotating speed is 3000rpm, and the dispersing time is 2 hours, so that the effect of primarily dispersing slurry powder is achieved;
step five: carrying out re-refining dispersion treatment on the slurry after the step four dispersion by using a circulating dispersion machine; the rotation speed is 2500rpm, the dispersion time is 3 hours, and the roll printing slurry is refined and dispersed;
step six: and (3) filtering the slurry obtained in the step five, wherein the specification of the filter element is 0.5 mu m, the filtering pressure is 0.2mpa, and packaging to obtain the finished slurry.
As shown in FIG. 3, when observed under SEM at 20000x, the slurry is evenly dispersed and distributed, and no agglomeration of powder is caused. The pattern printed by the roll printing process is observed under a 200x microscope (as shown in fig. 4), and the printed pattern is flat, has no edge penetrating and has high printability. Meanwhile, the reliability of the MLCC product measured after lamination-cutting-adhesive discharging-sintering-end capping-end firing-deposition is high as shown in table 1.
Comparative example 1:
in one embodiment of the process for preparing the roll printing slurry, the slurry comprises the following components in parts by weight: 65 parts of nickel powder, 6 parts of barium titanate, 1 part of additive, 24 parts of hydrogenated terpineol and 4 parts of ethyl cellulose. The preparation process carried out is the same as in example 1, comprising the following steps:
step one: stirring and mixing the co-materials by using a planetary grinder, wherein the rotating speed is 250rpm, and the time is 3 hours, so as to obtain a co-material mixture;
step two: then, shearing and dispersing the mixture obtained in the step one by using a three-roller mill, wherein the rotating speed is 400rpm, and the time is 1.5 hours, so that the effect of dispersing the co-material particles is achieved;
step three: adding metal powder and an adhesive into the mixture obtained in the step two, and mixing by using a double-planetary mixer at the rotating speed of 200rpm for 60min to obtain a slurry mixture;
step four: shearing and dispersing the mixture obtained in the step three by using a nano sand mill at the rotating speed of 2000rpm for 3 hours to achieve the effect of primarily dispersing the slurry powder;
step five: carrying out re-refining dispersion treatment on the slurry after the step four dispersion by using a high-pressure dispersing machine; the rotation speed is 2000rpm, the dispersion time is 3 hours, and the roll printing slurry is refined and dispersed;
step six: and (3) filtering the slurry obtained in the step five, wherein the specification of the filter element is 0.5 mu m, the filtering pressure is 0.2mpa, and packaging to obtain the finished slurry.
As shown in fig. 5, the slurry was observed to be dispersed with agglomerates at 20000x under SEM to form voids, indicating that the slurry was slightly agglomerated and dispersed. The pattern printed by the roll printing process is observed under a 200x microscope (as shown in fig. 6), the end of the printed pattern has pinholes, the phenomenon of no printing is generated, and the printability is general. Meanwhile, the reliability of the MLCC product measured after lamination-cutting-adhesive discharging-sintering-end capping-end firing-deposition is shown in table 1 as it is. The analysis is that the content of nickel powder is too high, the dispersion difficulty is increased, and partial agglomeration is formed, so that the reliability of the MLCC product is reduced.
Comparative case 2:
an example of a process for preparing a roll printing slurry according to the invention comprises the following components (as in example 1) in parts by weight: 55 parts of nickel powder, 6 parts of barium titanate, 1 part of additive, 34 parts of hydrogenated terpineol and 4 parts of ethyl cellulose. The preparation process comprises the following steps:
step one: stirring and mixing the co-materials by using a planetary grinder, wherein the rotating speed is 250rpm, and the time is 3 hours, so as to obtain a co-material mixture;
step two: adding metal powder and an adhesive into the mixture obtained in the step one, and mixing by using a double-planetary mixer at the rotating speed of 200rpm for 60min to obtain a slurry mixture;
step three: carrying out refining and dispersing treatment on the slurry mixture in the second step by using a circulating dispersing machine; the rotation speed is 2500rpm, the dispersion time is 3 hours, and the roll printing slurry is dispersed;
step four: and (3) filtering the slurry obtained in the step (III), wherein the specification of the filter element is 0.5 mu m, the filtering pressure is 0.2mpa, and packaging to obtain the finished slurry.
As shown in fig. 7, the slurry was observed to have more clusters and more voids under SEM at 20000x, indicating that the slurry had more clusters and had worse dispersion. The pattern printed by the roll printing process was observed under a 200x microscope (as shown in fig. 8), and a large number of pinholes appeared in the middle of the printed pattern, and the printability was poor. Meanwhile, the reliability of the MLCC product measured after lamination-cutting-adhesive discharging-sintering-end capping-end firing-deposition is poor as shown in table 1. The analytical reasons are poor printability due to the inability of the dispersion process for preparing the roll printing paste to disperse the paste well, and poor reliability of the MLCC product.
TABLE 1
| Name of the name | Slurry dispersion | Reliability of |
| Example 1 | Good (good) | High height |
| Example 2 | Good (good) | High height |
| Comparative example 1 | In general | In general |
| Comparative example2 | Poor quality | Poor quality |
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (3)
1. A preparation process of high-printability roll printing slurry is characterized by comprising the following steps of: the method comprises the following steps:
step one: stirring and mixing the co-materials by using a planetary grinder at the rotating speed of 250-500rpm for 2-4 hours to obtain a co-material mixture;
step two: then, shearing and dispersing the mixture obtained in the step one by using a three-roller mill, wherein the rotating speed is 400-600rpm, and the time is 1-1.5 hours, so that the effect of dispersing the co-material particles is achieved;
step three: adding metal powder and an adhesive into the mixture obtained in the step two, and mixing by using a double-planetary mixer at the rotating speed of 200-300rpm for 30-60min to obtain a slurry mixture;
step four: shearing and dispersing the mixture obtained in the step three by using a nano sand mill at the rotating speed of 2000-3000rpm for 2-3 hours to achieve the effect of primarily dispersing the slurry powder;
step five: finally, re-refining and dispersing the slurry after the fourth dispersing step by using a circulating dispersing machine; the rotating speed is 2000-2500rpm, the dispersing time is 3-4 hours, and the good dispersing of the roll printing paste is finally realized;
step six: and (3) filtering the slurry obtained in the step five, selecting a filter element with the filter element specification of 0.4-3.0 mu m according to the type of the product, filtering at the pressure of 0.1-0.8mpa, and packaging to obtain the finished slurry.
2. The process according to claim 1, wherein: the double-planetary mixer is provided with two closed square mixing heads, is attached to the inner wall by less than or equal to 2mm, and can perform revolution and rotation simultaneously, so that powder is fully mixed without being attached to the inner wall.
3. The preparation process according to any one of claims 1 to 2, characterized in that: the nickel internal electrode slurry comprises the following components in percentage by weight:
40-60% of nickel powder, wherein the nickel powder can be selected from 80-400 nm particle size, sphere-like shape and good crystallinity;
5-10% of ceramic additive, wherein the optional types of the ceramic additive comprise, but are not limited to, barium titanate, calcium titanate, strontium titanate, barium zirconate titanate, calcium strontium zirconate, and the particle size range comprises 10-300 nm;
0.5-3.5% of additive, wherein the optional additive comprises manganese dioxide, zirconium dioxide, barium carbonate, yttrium oxide, magnesium carbonate, titanium dioxide, silicon oxide, aluminum oxide, lithium oxide, most lanthanide rare earth elements and the like, and the particle size of the powder is less than 100nm;
25-45% of a solvent, wherein the solvent can be selected from cyclic ethanol acetate, methyl acetate, ethyl acetate, terpineol, n-propanol, dipropylene glycol dimethyl ether, hydrogenated terpineol and other solvents meeting environmental protection requirements;
3-4% of adhesive resin, and the organic resin can be selected from ethyl cellulose, rosin, epoxy resin, powder ring resin, polyvinyl butyral, acrylic resin, etc.
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