CN112071464A - Co-fired hole-filling conductor slurry and preparation method thereof - Google Patents
Co-fired hole-filling conductor slurry and preparation method thereof Download PDFInfo
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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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Abstract
The invention relates to a co-fired hole-filling conductor slurry and a preparation method thereof, wherein the slurry comprises the following components in parts by mass: 70-90 parts of metal powder, 5.0-15.0 parts of inorganic powder, 5-15 parts of organic carrier and 0.1-5 parts of curing agent. The preparation method comprises the following steps: (1) weighing the components of the organic carrier according to the mass ratio, and heating and fully stirring to obtain the organic carrier; (2) adding metal powder, inorganic powder and a curing agent into an organic carrier according to the mass parts, and rolling and dispersing to obtain the co-fired pore-filling conductor slurry. Compared with the prior art, the invention can not only prevent the filled pore columns from sinking due to the secondary volatilization of the solvent, but also improve the strength of the drying film.
Description
Technical Field
The invention relates to the field of hole filling slurry, in particular to co-fired hole filling conductor slurry and a preparation method thereof.
Background
LTCC (low temperature co-fired ceramic) and HTCC (high temperature co-fired ceramic) technologies have become mainstream technologies for passive integration, are easy to realize more wiring layers, and become a development direction in the field of passive components and an economic growth point of new component industries. The electronic components manufactured by the co-firing process have the characteristics of good performance, high reliability, good consistency, compact structure, small volume, light weight and the like, and have become the first choice mode of integration and modularization of electronic elements by virtue of excellent electronic, mechanical and thermal properties, so that the electronic components are widely applied to the fields of military, aerospace, computers and the like.
In the multilayer co-fired ceramic technology, ceramic green ceramic chips and conductor slurry are required to be co-fired and molded, wherein the sintering temperature of LTCC is 700-1000 ℃, and the sintering temperature of HTCC is more than 1200 ℃. The conventional pore-filling slurry only considers the problem of the sinking of the pore-filling slurry after printing, and for the sinking of the pore-filling slurry after equal temperature and pressure equalization, the sinking mainly occurs in the cavity and is generally solved by increasing the thickness of the pore-filling printing in the cavity, so that the process difficulty is increased, and the efficiency is reduced.
Patent application CN 110544550 a relates to a high temperature co-fired pore-filling slurry, which is composed of micron-sized metal powder, inorganic additive and organic carrier, wherein the organic carrier contains phthalate. The slurry has too high leveling property and low drying film strength in the temperature and equal pressure equalizing process, so that the problem of secondary volatilization cannot be solved, and the filled pore column sinks.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a co-fired pore-filling conductor slurry which prevents pore-filling columns from sinking due to secondary volatilization of a solvent and has high drying film strength and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
according to the conventional multilayer co-firing technology, the hole-filling slurry needs to be subjected to processes of printing, laminating, drying and the like before co-firing, then the hole-filling slurry is leveled and laminated, the laminated hole-filling slurry is slightly higher than the green ceramic chips by 2-5 mu m, and finally, the laminated green ceramic chips are subjected to equal-temperature pressure equalization at the temperature of about 70 ℃.
The inventor gradually discovers in long-term research and time that the drying temperature after printing the slurry is between room temperature and 65 ℃ because the temperature equal-pressure temperature (70 ℃) is higher than the temperature in the drying process (room temperature-65 ℃), the drying temperature after printing the slurry is between room temperature and 65 ℃ generally, and the storage time of the drying process at the temperature is too short because of the requirement of capacity, the organic solvent in the slurry has the phenomenon of incomplete drying, particularly the pore-filling slurry, the thickness of the pore column is about 100 mu m, and the complete drying is more difficult. Therefore, when the temperature and the like are equalized, the viscosity of the incompletely dried pore-filling slurry is reduced and the solvent is volatilized for the second time along with the rise of the temperature, the pore-filling slurry with extremely high fluidity can be sunken to fill the pores formed after the solvent is volatilized for the second time, so that the pore-filling slurry is sunken, the sunken phenomenon can be remained in the sintering process, the conduction between LTCC layers is poor, the pore-filling slurry frequently appears in the pores of the cavity of the multilayer substrate, the problem is a technical bias which is often ignored by technical personnel in the field, the phenomenon that the pore-filling slurry is not completely filled is mistaken, and in order to solve the problems, the inventor provides the following specific scheme:
a co-fired hole-filling conductor slurry comprises the following components in parts by mass: 70-90 parts of metal powder, 5.0-15.0 parts of inorganic powder, 5-15 parts of organic carrier and 0.1-5 parts of curing agent.
Further, the metal powder comprises one or more of gold powder, silver powder, palladium powder, platinum powder, tungsten powder and molybdenum powder; the particle size of the metal powder is 0.5-10 μm. Preferably 2-8 μm.
The inorganic powder comprises ceramic powder and/or glass powder, and the ceramic powder comprises one or more of alumina, zirconia, aluminum nitride or silica; the glass powder comprises zinc borosilicate glass powder; the particle size of the inorganic powder is 0.5-10 μm. Preferably 1-5 μm.
The inorganic powder comprises two substances, one of which mainly plays a filling role in the pore-filling slurry, and the other of which is selected from substances with high melting point and no reaction with the co-fired ceramic, and mainly comprises oxides and nitrides, such as alumina, zirconia, silica, aluminum nitride and the like; another type is inorganic powders that are compatible with or close to the constituents of the cofired ceramics and that can react with the cofired ceramics to improve adhesion, including various types of glass frits, such as zinc borosilicate glass frits.
Further, the organic vehicle comprises a solvent, a thermosetting resin and a binder; the mass ratio of the thermosetting resin to the binder is (40:60) - (15: 85).
Further, the thermosetting resin comprises one or more of epoxy resin, phenolic resin or acrylic resin.
Further, the binder comprises one or more of ethyl cellulose, nitrocellulose or acrylic resin; the solvent comprises one or more of terpineol, butyl carbitol, acetic acid and butyl carbitol.
Further, the curing agent comprises a latent medium-temperature curing agent with the curing temperature of 60-85 ℃. Such as HP-655, Fuji chemical company FXR1081, CZ-1020, azobisisobutyronitrile, propylene carbonate, Edikco EH-5031S, etc.
Further, the curing agent comprises alicyclic polyamine or imidazole curing agent.
Because the curing agent and the thermosetting resin are added into the pore-filling slurry, the curing agent and the thermosetting resin react during the drying process to cure the pore-filling slurry, so that the strength of the dried slurry film is improved and the slurry film is not deformed. When the subsequent temperature and the like are equalized, the problems of hole filling and sinking caused by the reduction of the viscosity of the slurry and the secondary volatilization of the solvent due to the increase of the temperature can be avoided.
A preparation method of the co-fired hole-filling conductor paste comprises the following steps:
(1) weighing the components of the organic carrier according to the mass ratio, and heating and fully stirring to obtain the organic carrier;
(2) adding metal powder, inorganic powder and a curing agent into an organic carrier according to the mass parts, and rolling and dispersing to obtain the co-fired pore-filling conductor slurry. The obtained pore-filling slurry needs to be stored at low temperature after being prepared, and the temperature can not exceed 35 ℃.
Further, the heating temperature is 60-90 ℃.
Compared with the prior art, the invention has the following advantages:
(1) in the face of the problem of sinking of the pore-filling slurry, a person skilled in the art usually only considers the flowing performance of the slurry to fully fill the pore column, but neglects the important secondary volatilization problem to cause the performance of the pore-filling slurry to be unsatisfactory all the time, and the invention just seeks the essential problem and overcomes the bias of the prior art;
(2) the hole-filling conductor slurry can keep good leveling performance when not cured, can be well filled in a hole column, and can be cured along with the rise of temperature, so that the strength of a dried slurry film layer is increased, and in the process of facing the secondary volatilization of a solvent, the slurry is converted into a solid, the shape is fixed, the hardness is high, and the physical structure cannot be damaged due to the volatilization of the solvent, so that the slurry filling effect cannot be damaged;
(3) by adopting the hole-filling conductor paste, the problem of secondary volatilization is solved, so that the drying time can be reduced in the drying process, all solvents are not required to be volatilized completely, the productivity is improved, and the production rhythm is accelerated.
Detailed Description
A preparation method of the co-fired hole-filling conductor paste comprises the following steps:
(1) weighing the components of the organic carrier, namely the solvent, the thermosetting resin and the binder, heating to 60-90 ℃, and fully stirring to obtain the organic carrier; wherein the mass ratio of the thermosetting resin to the binder is (40:60) - (15: 85);
(2) 70-90 parts of metal powder, 5.0-15.0 parts of inorganic powder and 0.1-5 parts of curing agent are added into an organic carrier and are dispersed by rolling, so that the co-fired pore-filling conductor paste is obtained. The obtained pore-filling slurry needs to be stored at low temperature after being prepared, and the temperature can not exceed 35 ℃. Wherein the particle size of the metal powder is 0.5-10 μm. The particle size of the inorganic powder is 0.5-10 μm.
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Dissolving 0.8 part of ethyl cellulose and 2 parts of epoxy resin (E44) in a mixed solvent of 5 parts of butyl carbitol acetate and 2 parts of terpineol to obtain an organic carrier; adding 80 parts of gold powder, 7 parts of zinc borosilicate glass powder, 3 parts of alumina powder and 0.2 part of curing agent (HP-655) into a dissolved organic carrier in advance, and rolling and dispersing to obtain the co-fired hole-filling conductor paste.
Example 2
Dissolving 1 part of ethyl cellulose and 5 parts of epoxy resin (EP-828) in a mixed solvent of 5 parts of butyl carbitol acetate and 1 part of terpineol to obtain an organic carrier; 70 parts of silver powder, 8 parts of zinc borosilicate glass powder, 6.7 parts of alumina powder and 0.3 part of curing agent (Fuji chemical company FXR1081) are added into an organic carrier dissolved in advance and are dispersed by rolling, so that the co-fired hole-filling conductor paste is obtained.
Example 3
Dissolving 1 part of ethyl cellulose and 1 part of epoxy resin (E44) in a mixed solvent of 1 part of butyl carbitol acetate and 2 parts of terpineol to obtain an organic carrier; 89.8 parts of tungsten powder, 5 parts of alumina powder and 0.2 part of curing agent (CZ-1020) are added into an organic carrier dissolved in advance, and rolling dispersion is carried out, so as to obtain the co-fired pore-filling conductor slurry.
Example 4
Dissolving 3 parts of ethyl cellulose and 1 part of acrylic resin in a mixed solvent of 5 parts of butyl carbitol acetate and 1 part of terpineol to obtain an organic carrier; and adding 74.8 parts of silver powder, 15 parts of zinc borosilicate glass powder and 0.2 part of azobisisobutyronitrile into a dissolved organic carrier in advance, and rolling and dispersing to obtain the co-fired hole-filling conductor paste.
Example 5
Dissolving 3 parts of ethyl cellulose and 3 parts of phenolic resin in a mixed solvent of 7 parts of butyl carbitol acetate and 2 parts of terpineol to obtain an organic carrier; adding 85 parts of tungsten powder, 8 parts of aluminum nitride powder and 0.4 part of propylene carbonate into a dissolved organic carrier in advance, and rolling and dispersing to obtain the co-fired hole-filling conductor slurry.
Example 6
Dissolving 1 part of ethyl cellulose and 1 part of epoxy resin (E44) in a mixed solvent of 5 parts of butyl carbitol acetate and 2 parts of terpineol to obtain an organic carrier; adding 80 parts of gold powder, 5 parts of zinc borosilicate glass powder, 3 parts of alumina powder and 0.2 part of curing agent (Adecaco EH-5031S) into a dissolved organic carrier in advance, and rolling and dispersing to obtain the co-fired hole-filling conductor paste.
Comparative example
Adding 4 parts of ethyl cellulose, 1 part of butyl carbitol acetate and 2 parts of terpineol into a mixed solvent to obtain an organic carrier; adding 80 parts of gold powder and 10 parts of zinc borosilicate glass powder into a dissolved organic carrier in advance, and rolling and dispersing to obtain the co-fired hole-filling conductor slurry.
Test of projection height after temperature isostatic pressing of pore-filling slurries prepared in examples 1-6 and comparative example
The prepared pore-filling slurries of examples 1 to 6 and comparative example were subjected to 300 μm pore-filling printing on LTCC green sheets via stainless steel, dried at 60 to 65 ℃ for 10 to 15min, leveled, laminated in a cavity pattern and tested for substrate pore-filling height; and (4) carrying out equal temperature and pressure equalization, wherein the temperature of water is 70 ℃, the pressure is 3000PSI, and the hole filling height of the substrate is tested after the pressure is maintained for 15 min.
And (3) performing a hole filling protrusion height test on 20 holes on each substrate, wherein the protrusion height of-15 to +15 mu m is qualified. The test results are given in table 1 below:
TABLE 1
| Sample number | Height of protrusion | Whether it is qualified or not |
| Example 1 | -10～+1μm | Qualified |
| Example 2 | -10～+5μm | Qualified |
| Example 3 | -8～+10μm | Qualified |
| Example 4 | -5～+1μm | Qualified |
| Example 5 | -5～-3μm | Qualified |
| Example 6 | -10～-6μm | Qualified |
| Comparative example | -55～-185μm | Fail to be qualified |
As shown in Table 1, after all the pore-filling slurry is dried and leveled, the protruding height is in the range of-15 to +15 μm, and the requirement is met. After the pressure is maintained for 15min at 70 ℃ and 3000PSI, the slurry with the curing agent added in the comparative example cannot overcome the problem of secondary volatilization, and the protrusion height is obviously reduced to (-55 to-185 mu m), and exceeds the qualified range. In examples 1 to 6, the strength of the pore-filling slurry was improved by adding the curing agent, and the pore-filling slurry was less affected by the temperature and pressure equalization (70 ℃ C., 3000PSI) and had a small change in the protrusion height.
Test examples 1-6 and comparative example the prepared pore-filling slurries were tested for dry film strength by baking.
The pore-filling pastes of examples 1 to 6 and comparative examples were screen-printed on an alumina fired porcelain substrate, dried at 60 to 65 ℃ for 10 to 15min, and oven-dried to a film thickness of 15 to 20 μm. The pastes were tested for dry film strength by reference to the "scratch test for paint and clear-coat films of GB/T9286-1998, cut at 6X 6 and tested with 3M600 tape. The test results are shown in table 2:
TABLE 2
As shown in table 2, the strength of the pore-filling slurry after the curing agent was added was 4B or more, which is higher than the strength (2B) of the comparative example, and thus it was found that the strength of the dried film of the pore-filling slurry was effectively improved by adding the curing agent, and it was estimated that the strength was certainly improved after the slurry was cured in the pore column.
Claims (10)
1. The co-fired hole-filling conductor slurry is characterized by comprising the following components in parts by mass: 70-90 parts of metal powder, 5.0-15.0 parts of inorganic powder, 5-15 parts of organic carrier and 0.1-5 parts of curing agent.
2. The co-fired hole-filling conductor paste as claimed in claim 1, wherein the metal powder comprises one or more of gold powder, silver powder, palladium powder, platinum powder, tungsten powder and molybdenum powder; the particle size of the metal powder is 0.5-10 μm.
3. The co-fired pore-filling conductor paste as claimed in claim 1, wherein the inorganic powder comprises ceramic powder and/or glass powder, the ceramic powder comprises one or more of alumina, zirconia, aluminum nitride or silica; the glass powder comprises zinc borosilicate glass powder; the particle size of the inorganic powder is 0.5-10 μm.
4. The co-fired via-filling conductor paste as claimed in claim 1, wherein the organic vehicle comprises a solvent, a thermosetting resin and a binder; the mass ratio of the thermosetting resin to the binder is (40:60) - (15: 85).
5. The co-fired hole-filling conductor paste as claimed in claim 4, wherein the thermosetting resin comprises one or more of epoxy resin, phenolic resin or acryl resin.
6. The co-fired via-filling conductor paste as claimed in claim 4, wherein the binder comprises one or more of ethyl cellulose, nitrocellulose or acrylic; the solvent comprises one or more of terpineol, butyl carbitol, acetic acid and butyl carbitol.
7. The co-fired pore-filling conductor paste according to claim 1, wherein the curing agent comprises a latent medium-temperature curing agent with a curing temperature of 60-85 ℃.
8. The co-fired pore-filling conductor paste as claimed in claim 1, wherein the curing agent comprises alicyclic polyamine or imidazole curing agent.
9. A method of preparing a co-fired via-fill conductor paste as claimed in any one of claims 1 to 8, comprising the steps of:
(1) weighing the components of the organic carrier according to the mass ratio, and heating and fully stirring to obtain the organic carrier;
(2) adding metal powder, inorganic powder and a curing agent into an organic carrier according to the mass parts, and rolling and dispersing to obtain the co-fired pore-filling conductor slurry.
10. The method according to claim 9, wherein the heating temperature is 60-90 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113035405A (en) * | 2021-03-10 | 2021-06-25 | 安徽华封电子科技有限公司 | Pore-filling slurry for co-fired ceramic system |
| CN113851251A (en) * | 2021-11-30 | 2021-12-28 | 西安宏星电子浆料科技股份有限公司 | Transitional pore filling slurry for connecting upper and lower gold and silver layers of membrane tape in LTCC substrate |
| CN115557794A (en) * | 2022-11-02 | 2023-01-03 | 无锡海古德新技术有限公司 | High-temperature co-fired ceramic HTCC preparation process based on tungsten paste for screen printing |
| CN118271914A (en) * | 2024-03-29 | 2024-07-02 | 江苏飞特尔通信有限公司 | Electroplating pore-filling agent for LTCC (Low temperature Co-fired ceramic) and preparation method and application thereof |
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| CN118271914A (en) * | 2024-03-29 | 2024-07-02 | 江苏飞特尔通信有限公司 | Electroplating pore-filling agent for LTCC (Low temperature Co-fired ceramic) and preparation method and application thereof |
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