CN112289482B - high-Q-value silver paste for 5G ceramic dielectric filter - Google Patents
high-Q-value silver paste for 5G ceramic dielectric filter Download PDFInfo
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- 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
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention discloses a high-Q-value silver paste for a 5G ceramic dielectric filter, which comprises the following components in percentage by mass: 75-85% of silver powder, 1-3.5% of glass binder, 0.1-1% of inorganic additive and 12-23% of organic carrier, wherein the silver powder is obtained by performing wet high-pressure heat treatment on a mixture of spherical silver powder and flake silver powder in a mass ratio of 1: 1-7: 1, the average particle diameter of the spherical silver powder is 0.7-1.15 mu m, and the tap density is 4.5-5.5 g/cm3The silver flake has an average particle diameter of 0.8 to 5.0 μm and a tap density of 4.0 to 7.0g/cm3. According to the invention, the two silver powders are subjected to high-pressure heat treatment for crystallization to obtain the mixed silver powder with high crystallinity, the silver powder has reliable performance and stable high-temperature sintering molding, and a better sintering compact film layer can be obtained. After the silver paste is matched on a ceramic substrate of a 5G ceramic dielectric filter, the leveling property is good, the compactness of the silver layer is high, the adhesion with the ceramic substrate of the filter is high, the weldability is good, the Q value is high, and the insertion loss is low.
Description
Technical Field
The invention belongs to the technical field of 5G filters, and particularly relates to a high-Q-value silver paste for a 5G ceramic dielectric filter.
Background
With the development of mobile communication networks, wireless frequency bands become very dense, so that the metal cavity filter cannot realize high-inhibition system compatibility, and the problem can be solved by manufacturing the cavity filter by adopting a ceramic dielectric material. Compared with the traditional metal cavity resonator, the ceramic dielectric resonator filter has the characteristics of high suppression, small insertion loss and good temperature drift characteristic, and the power capacity and the passive intermodulation performance are greatly improved. The ceramic dielectric resonant filter represents the development direction of high-end radio frequency devices, and has wider application space in the field of mobile communication by virtue of excellent performance. In order to improve the performance of the ceramic filter, silver paste is printed on the surface of a ceramic body substrate of the filter by utilizing screen printing, and a compact conductive film layer is formed on the surface layer of the ceramic body by drying and sintering.
The existing silver conductor slurry of the ceramic dielectric filter mainly has the following problems in the using process: (1) the silver powder used by the high solid content silver paste has poor crystallinity, low surface activity, non-compact silver layer after sintering and large shrinkage; (2) the ceramic body is poor in combination, and large-area falling phenomenon occurs; (3) after silver paste is used, the Q value is low, and the insertion loss is high. Silver conductor pastes used in ceramic dielectric filters are required to minimize internal losses in the filter itself.
Disclosure of Invention
The invention aims to provide the high-Q-value silver paste for the 5G ceramic dielectric filter, which takes the high-crystallization and high-dispersibility silver powder as the main functional material of the paste, and the silver paste can improve the adhesive force and effectively reduce the insertion loss.
Aiming at the purposes, the high-Q-value silver paste for the 5G ceramic dielectric filter comprises the following components in percentage by mass: 75-85% of silver powder, 1-3.5% of glass binder, 0.1-1% of inorganic additive, 12-23% of organic carrier and less than or equal to 8.0 mu m in fineness, wherein the silver powder is obtained by performing wet high-pressure heat treatment on a mixture of spherical silver powder and flake silver powder in a mass ratio of 1: 1-7: 1, the average particle diameter of the spherical silver powder is 0.7-1.15 mu m, and the tap density is 4.5-5.5 g/cm3The silver flake has an average particle diameter of 0.8 to 5.0 μm and a tap density of 4.0 to 7.0g/cm3。
The silver powder is preferably obtained by subjecting a mixture of spherical silver powder and plate-like silver powder at a mass ratio of 3:1 to wet autoclaving.
The method for carrying out wet high-pressure heat treatment on the silver powder comprises the following steps: weighing spherical silver powder and flake silver powder according to a ratio, fully and uniformly mixing by using a powder mixer, pumping, filtering and washing the mixed silver powder by using absolute ethyl alcohol, adding the obtained product into a high-pressure reaction kettle, adding heavy water into the high-pressure reaction kettle, heating the high-pressure reaction kettle to 250-300 ℃ under the conditions of sealing and stirring, carrying out high-pressure heat treatment on the silver powder for crystallization for 4-8 hours, taking out the silver powder after the heat treatment, carrying out vacuum drying, and sieving by using a 120-250-mesh sieve.
In the wet-type high-pressure heat treatment method for silver powder, the addition amount of the heavy water is preferably 10 to 20 times of the total mass of the spherical silver powder and the flake silver powder.
In the wet high-pressure heat treatment method for silver powder, the temperature of the high-pressure reaction kettle is preferably uniformly increased to 250-300 ℃ at a speed of 2-5 ℃/min.
In the wet-type high-pressure heat treatment method for silver powder, the preferable vacuum drying temperature is 60-100 ℃, and the drying time is 6-12 hours.
The glass binder is preferably Bi-Si-Cu-Mn glass, and the glass system comprises the following components in percentage by mass: bi2O3 50％～60％，SiO23-15 percent of CuO, 20-35 percent of CuO and 1-5 percent of MnO. The preparation method comprises the following steps: weighing the oxides in proportion, fully mixing the oxides uniformly, placing the mixture in an oven at 100-230 ℃ for drying for 1-2 hours, and then smelting the mixture at 1000-1200 ℃ for 100-150 min. Water quenching the uniformly melted glass to obtain coarse glass particles, adding the coarse glass particles into a polyurethane tank for ball milling for 10-15 hours to obtain powder with the average particle size of less than or equal to 2.0 mu m, and drying at 125 ℃ to obtain the glass binder.
The inorganic additive is preferably any one of nickel oxide, zinc oxide and titanium dioxide, and the particle size range of the inorganic additive is 0.7-1.5 mu m.
The organic carrier consists of the following raw materials in percentage by mass: 5-16% of resin, 0.5-3% of organic additive and 82-93% of organic solvent, wherein the resin is one or more of rosin resin, terpene resin, maleic acid resin, polyvinyl butyral and ethyl cellulose, the organic additive is one or a mixture of polyethylene wax and hydrogenated castor oil, and the organic solvent is one or a mixture of more of terpineol, diethylene glycol dibutyl ether and butyl carbitol acetate.
The preparation method of the silver paste comprises the following steps: according to the formula proportion, firstly, the weighed glass binder, the inorganic additive and part of the organic carrier are mixed in advance, then the rest organic carrier, the silver powder and the premixed mixture are mixed by a stirring dispersion machine, and after uniform mixing, the mixture is fully ground and rolled on a three-roller machine to obtain the silver paste with the fineness of less than or equal to 8.0 microns.
The invention has the following beneficial effects:
1. the silver paste adopts the spherical silver powder and the flake silver powder to be matched for use, and has good filling property. Meanwhile, the mixed silver powder with high crystallinity can be obtained after wet high-pressure heat treatment, the silver powder has good dispersibility, reliable performance, small shrinkage during sintering and stable high-temperature sintering molding, and can improve the compactness of a silver layer after sintering, further improve the adhesive force and keep a filter to have good Q value and low insertion loss.
2. The invention adds the inorganic additive as the adhesive force additive, can control the shrinkage of silver in the sintering process, can be slightly combined with the porcelain body, is favorable for improving the adhesive force of the electrode on the premise of not influencing the electrical property,
3. the Bi-Si-Cu-Mn glass is selected, so that the silver paste and the porcelain body can be effectively ensured to have good wettability after being rapidly sintered at low temperature, and the metal silver powder and the porcelain body are ensured to be in contact with each other to form good adhesive force.
4. After the silver paste is matched on a ceramic substrate of a 5G ceramic dielectric filter, the leveling property is good, the sintering surface is smooth, the adhesion with the ceramic substrate of the filter is high, the weldability is good, the Q value is high, and the insertion loss is low.
Drawings
Fig. 1 is an XRD of the untreated mixed silver powder in comparative example 1.
FIG. 2 is an XRD of the mixed silver powder after wet autoclaving in example 3.
Fig. 3 is a scanning electron microscope image of (a) after sintering of a silver paste prepared from the wet autoclaved mixed silver powder in example 3 and (b) after sintering of a silver paste prepared from the untreated mixed silver powder in comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to these examples.
Examples 1 to 6
100g of silver paste is prepared according to the mass percentage composition of the examples 1-6 in the table 1, and the specific preparation method is as follows:
1. wet high pressure heat treatment of silver powder
Weighing spherical silver powder and flake silver powder, fully and uniformly mixing the spherical silver powder and the flake silver powder by using a powder mixer, carrying out suction filtration and washing by using absolute ethyl alcohol, then placing the mixed silver powder into a high-pressure reaction kettle, adding heavy water which is 20 times of the mass of the mixed silver powder, starting a stirring paddle of the reaction kettle, keeping the rotating speed of the stirring paddle at 1000r/min, controlling the reaction kettle to uniformly heat up to 250 ℃ at the speed of 2 ℃/min, carrying out high-pressure heat treatment on the mixed silver powder for crystallization for 6 hours, and finishing the pretreatment of the silver powder.
2. Preparation of glass binder
The weight percentages are as follows: bi2O3 55％、SiO 210% of CuO, 30% of MnO and 5% of Bi2O3、SiO2Mixing CuO and MnO, baking in 120 deg.C oven for 80min, and smelting at 1200 deg.C for 120 min. Water quenching the molten glass to obtain coarse glass particles, adding the coarse glass particles into a polyurethane tank for ball milling for 12 hours to obtain powder with the average particle size of less than or equal to 2.0 microns, and drying at 125 ℃ to obtain the glass binder.
3. Preparation of organic vehicle
Adding 50g of terpineol and 35g of butyl carbitol acetate into a beaker, heating the mixture to 75 ℃ in a water bath under the stirring condition, then adding 9g of ethyl cellulose and 1g of polyethylene wax, continuing stirring for 30min, then adding 5g of terpene resin, continuing stirring until the resin is completely dissolved, keeping the constant temperature at 80 ℃, stirring for 1h, and filtering through a 250-mesh screen to obtain the organic carrier.
4. Preparation of silver paste for 5G filter
The weighed glass binder, inorganic additive (nano zinc oxide) and 1/3 organic carrier are mixed in advance, then the rest 2/3 organic carrier, the silver powder subjected to wet high-pressure heat treatment and the premixed mixture are mixed by a stirring dispersion machine, and after uniform mixing, the mixture is fully ground and rolled on a three-roller machine to obtain the silver paste with the fineness of less than or equal to 8.0 mu m.
TABLE 1 silver paste formulation
Meanwhile, 100g of silver paste is prepared according to the method by using the mass percentage compositions and the preparation conditions of comparative examples 1-9 in the table 1, and is used as a control experiment.
The silver paste is naturally leveled for 10min according to the thickness of 10mm multiplied by 10mm on a ceramic body, after drying for 10min at 150 ℃, the sample is placed in a belt sintering furnace at 850 +/-5 ℃ for sintering, the sintering period is 90min, the peak value is kept for 10min, a test sample is prepared, and the following performance tests are carried out:
leveling property: visual inspection was carried out.
And (3) sintering surface appearance: the surface state of the sintered film of the obtained sample piece was observed under a microscope at 20 times magnification.
Shrinkage (%): (thickness of dried film-thickness of sintered mold)/thickness of dried film, the film thickness was measured in accordance with the method specified by 104 in SJT 11512-2015.
Weldability: the procedure was as defined in 202 of SJT 11512-2015.
Initial tension: and punching 6 phi 2 holes on the label paper, and attaching the label paper to the sintered ceramic body. Lead wire with phi 0.8 is used for welding along the direction vertical to the plane of the porcelain body, and the welding time is less than 3S. An initial tensile test was performed with a tensile machine.
Q value: selecting a standard medium block (20 × 10mm), spraying, dip-coating or printing the outer surface of the medium block, drying, sintering, cooling to normal temperature, and testing by using a network analyzer by using a resonant cavity method.
The results of the above tests are shown in Table 2.
Table 2 comparison of properties of different silver pastes
As can be seen from FIGS. 1 and 2, the diffraction peak of the silver powder after the wet high-pressure heat treatment is higher than that of the silver powder mixed by the untreated spherical silver powder and the flake silver powder in comparative example 1, which indicates that the crystallinity of the silver powder is significantly improved after the wet high-pressure heat treatment, and meanwhile, as can be seen from Table 2, the silver pastes prepared by the silver powders in examples 1 to 6 of the present invention after the wet high-pressure heat treatment have lower sintering shrinkage than that of the untreated comparative example 1. Comparing the SEM images of fig. 3a (silver paste prepared from silver powder after wet autoclaving) and b (silver paste prepared from silver powder without treatment) after sintering, it is evident from the SEM images that the silver paste prepared from silver powder after wet autoclaving has few pores on the surface after sintering, and the silver layer has good compactness, so that it has high adhesion, good solderability, and a larger Q value; example 3 in comparison with comparative examples 2, 3, 4 and 5, when the temperature of the wet autoclaving is lower than 250 ℃ (e.g. 200 ℃) or higher than 300 ℃ (e.g. 400 ℃), or the treatment time is too short or too long, the adhesion and Q-value of the product are reduced to some extent; compared with the comparative example 6, in the wet high-pressure heat treatment, compared with the method that heavy water is adopted to prepare silver powder by using deionized water, the silver paste prepared by the method has the advantages of lower shrinkage rate after sintering, large adhesive force and high Q value; compared with the comparative examples 7-9, when the ratio of the spherical silver powder to the flake silver powder is greater than 1:1, the prepared silver paste has better leveling property, flat sintered surface, good tensile force and large Q value.
Claims (9)
1. The high-Q-value silver paste for the 5G ceramic dielectric filter comprises the following components in percentage by mass: 75-85% of silver powder, 1-3.5% of glass binder, 0.1-1% of inorganic additive and 12-23% of organic carrier, and is characterized in that: the silver powder is obtained by performing wet high-pressure heat treatment on a mixture of spherical silver powder and flake silver powder in a mass ratio of 1: 1-7: 1, wherein the spherical silver powder isThe powder has an average particle diameter of 0.7 to 1.15 μm and a tap density of 4.5 to 5.5g/cm3The silver flake has an average particle diameter of 0.8 to 5.0 μm and a tap density of 4.0 to 7.0g/cm3；
The method for carrying out wet high-pressure heat treatment on the silver powder comprises the following steps: weighing spherical silver powder and flake silver powder according to a ratio, fully and uniformly mixing by using a powder mixer, pumping, filtering and washing the mixed silver powder by using absolute ethyl alcohol, adding the obtained product into a high-pressure reaction kettle, adding heavy water into the high-pressure reaction kettle, heating the high-pressure reaction kettle to 250-300 ℃ under the conditions of sealing and stirring, carrying out high-pressure heat treatment on the silver powder for crystallization for 4-8 hours, taking out the silver powder after the heat treatment, carrying out vacuum drying, and sieving by using a 120-250-mesh sieve.
2. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1, wherein: the silver powder is obtained by performing wet high-pressure heat treatment on a mixture of spherical silver powder and flake silver powder in a mass ratio of 3: 1.
3. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1 or 2, wherein: in the wet-type high-pressure heat treatment method for silver powder, the addition amount of heavy water is 10-20 times of the total mass of the spherical silver powder and the flake silver powder.
4. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1 or 2, wherein: in the wet-type high-pressure heat treatment method for silver powder, the temperature of a high-pressure reaction kettle is uniformly increased to 250-300 ℃ at the speed of 2-5 ℃/min.
5. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1 or 2, wherein: in the wet-type high-pressure heat treatment method for silver powder, the vacuum drying temperature is 60-100 ℃, and the drying time is 6-12 hours.
6. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1, wherein: the glass binder is Bi-Si-Cu-Mn glassThe mass percentage of each component of the system is as follows: bi2O3 50%～60%，SiO23%～15%，CuO 20%～35%，MnO 1%～5%。
7. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1, wherein: the inorganic additive is any one of nickel oxide, zinc oxide and titanium dioxide, and the particle size range of the inorganic additive is 0.7-1.5 mu m.
8. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1, wherein: the organic carrier is composed of the following raw materials in percentage by mass: 5-16% of resin, 0.5-3% of organic additive and 82-93% of organic solvent, wherein the resin is one or more of rosin resin, terpene resin, maleic acid resin, polyvinyl butyral and ethyl cellulose, the organic additive is one or a mixture of polyethylene wax and hydrogenated castor oil, and the organic solvent is one or a mixture of more of terpineol, diethylene glycol dibutyl ether and butyl carbitol acetate.
9. The high-Q silver paste for the 5G ceramic dielectric filter according to claim 1, wherein: the fineness of the silver paste is less than or equal to 8.0 mu m.
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| CN112992426A (en) * | 2021-02-25 | 2021-06-18 | 上海怡上电子科技有限公司 | Surface spraying high-Q value slurry for ceramic dielectric filter and preparation method and application thereof |
| CN112820442B (en) * | 2021-04-19 | 2021-07-06 | 西安宏星电子浆料科技股份有限公司 | Strong-adhesion silver conductor paste for 5G ceramic dielectric filter |
| CN113161036A (en) * | 2021-04-28 | 2021-07-23 | 佛山市顺德区百锐新电子材料有限公司 | Anti-adhesion and anti-vulcanization surface electrode silver paste and preparation method thereof |
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| CN114530276A (en) * | 2022-02-16 | 2022-05-24 | 无锡晶睿光电新材料有限公司 | Graphene-doped ceramic filter spraying silver paste and preparation method thereof |
| CN114530280A (en) * | 2022-04-21 | 2022-05-24 | 西安宏星电子浆料科技股份有限公司 | Low-cost thick-film conductor paste |
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| US7361377B2 (en) * | 2003-07-18 | 2008-04-22 | Brookhaven Science Associates, Llc | Fluorinated precursors of superconducting ceramics, and methods of making the same |
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| JP2013122077A (en) * | 2011-12-12 | 2013-06-20 | Sumitomo Metal Mining Co Ltd | Silver powder and manufacturing method thereof |
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