CN114039188A - Ceramic dielectric filter surface metallization method and ceramic dielectric filter - Google Patents
Ceramic dielectric filter surface metallization method and ceramic dielectric filter Download PDFInfo
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- CN114039188A CN114039188A CN202111375964.0A CN202111375964A CN114039188A CN 114039188 A CN114039188 A CN 114039188A CN 202111375964 A CN202111375964 A CN 202111375964A CN 114039188 A CN114039188 A CN 114039188A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/02—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by distortion, beating, or vibration of the surface to be cleaned
- B08B7/026—Using sound waves
- B08B7/028—Using ultrasounds
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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
- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
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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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P11/00—Apparatus or processes specially adapted for manufacturing waveguides or resonators, lines, or other devices of the waveguide type
- H01P11/007—Manufacturing frequency-selective devices
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Abstract
The invention discloses a surface metallization method of a ceramic dielectric filter, which comprises the following steps: cleaning and drying the ceramic substrate of the filter; coating conductive silver paste on the surface of a ceramic substrate of the filter; sintering to form a conductive silver layer; the step of cleaning and drying the ceramic substrate of the filter is as follows: step 1, alkaline cleaning; step 2, washing with water; step 3, acid cleaning; step 4, washing with water; step 5, ultrasonic cleaning; step 6, hot water ultrasonic cleaning; and 7, drying. The invention also discloses a ceramic dielectric filter. Compared with the prior art, the invention can effectively improve the adhesive force of the conductive silver layer and the surface of the ceramic substrate at lower cost and improve the electrical performance of the filter.
Description
Technical Field
The invention relates to a manufacturing process of a ceramic dielectric filter, in particular to a surface metallization method of the ceramic dielectric filter.
Background
In the 5G era, electromagnetic wave frequency requires millimeter-sized electromagnetic waves, and in order to realize millimeter-sized signal coverage and high-density connection, the size of a base station antenna is reduced to millimeter level, so that a miniature base station is gradually realized. In the background of the development, the size of the filter used in the base station is gradually reduced to millimeter level, and the dielectric filter, especially the ceramic dielectric filter, becomes the mainstream filter in the 5G era due to its advantages of small loss, small volume, high Q value, etc.
The ceramic dielectric filter realizes the conversion of an electric signal, mechanical vibration and an electric signal by utilizing the piezoelectric effect of a ceramic material, replaces an LC filter circuit in an electronic circuit and ensures that the electronic circuit works more stably. The ceramic dielectric filter is a filter which is formed by coating a conductive material on the surface of a ceramic substrate to be used as an electrode and has a piezoelectric effect after direct-current high-voltage polarization. Compared with the 4G filter which adopts an aluminum alloy cavity plated with silver, the 5G filter which adopts the microwave dielectric ceramic resonator as the core component of the 5G filter is made into a filter with strong signal through a plurality of groups of microwave dielectric ceramic resonators, which is equivalent to hundreds or even thousands of 4G aluminum alloy cavity filters. The signal transmission and the electric conduction of the dielectric filter are realized by a metal layer (usually a silver or copper layer) on the surface of a dielectric, and the quality of the metal layer directly influences key performance indexes of the dielectric filter, such as a Q value, reliability, welding performance and the like; the adhesion of the metal layer directly affects the reliability of the dielectric filter against soldering heat, and plays an important role in the reliability of the dielectric filter. Therefore, as with the metal cavity filter, the key technology of the ceramic dielectric filter includes a surface metallization process of the dielectric substrate in addition to the properties of the cavity material itself and the cavity structure.
The traditional ceramic dielectric filter surface metallization usually adopts a process of coating silver paste in batches and then sintering, namely, after the surface of a ceramic matrix is cleaned and dried, the silver paste is coated on the surface of the ceramic matrix in a screen printing or spraying mode, and then sintering is carried out to form a conductive silver layer on the surface of the ceramic matrix. The silver paste used in the process consists of conductive silver powder, an inorganic binder (usually glass powder) and an organic carrier. The method has the problems of high consumption of conductive silver paste and high metallization cost of the ceramic surface; moreover, due to the difference of the silver paste formula, the cleaning of the ceramic substrate and the silver paste sintering process, the metal layer sintered on the surface of the ceramic is not smooth enough, and the phenomena of peeling, bubbles, pinholes and the like are easy to occur, so that the insertion loss of the filter is too high and the Q value is reduced to the extent that the use requirement of an electronic device cannot be met in severe cases.
To overcome the above problems, some other surface metallization processes have been proposed, for example, the method disclosed in CN 108675834 a, which includes: sequentially cleaning the ceramic matrix with a low-polarity to high-polarity solvent, and then baking at high temperature for 1-3h in a normal pressure environment; depositing a metal layer A by utilizing a magnetron sputtering technology; depositing an alloy layer AB by utilizing a magnetron sputtering technology; and depositing the metal layer B by utilizing the magnetron sputtering technology again. For another example, CN 108950496 a discloses a surface treatment method and application of a ceramic resonator body based on 5G communication technology, including: performing pre-plating treatment on the ceramic resonator, then placing the treated ceramic resonator into a vacuum chamber, vacuumizing, and filling protective gas into the vacuum chamber when the vacuum degree is less than 10-2 Pa; then, a single metal layer or an alloy layer is formed as a bottom layer by vacuum plating, and then the metal is thickened by vacuum plating, chemical plating or electroplating. For another example, CN 112899683 a discloses a method for metallizing a surface of a ceramic dielectric filter, the method comprising the steps of: chemically plating nickel on the surface of the ceramic substrate subjected to the roughening treatment to obtain the ceramic substrate with a nickel-plated layer; sequentially carrying out chemical copper plating and electro-coppering on the surface of the ceramic substrate with the nickel plating layer to obtain the ceramic substrate with the copper plating layer; and plating silver on the surface of the ceramic substrate with the copper plating layer to obtain the ceramic dielectric filter with the metalized surface.
Although the improved method can improve the surface metallization quality to a certain extent, improve the Q value of the filter and reduce the insertion loss, the improved method needs complex and expensive process equipment such as magnetron sputtering, vacuum plating and the like, needs compounding of a plurality of different metal layers, has overhigh realization cost and is not suitable for large-scale production.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a surface metallization method of a ceramic dielectric filter, which can effectively improve the adhesive force between a conductive silver layer and the surface of a ceramic substrate at lower cost and improve the electrical performance of the filter.
The invention specifically adopts the following technical scheme to solve the technical problems:
a method of metallizing a surface of a ceramic dielectric filter comprising: cleaning and drying the ceramic substrate of the filter; coating conductive silver paste on the surface of a ceramic substrate of the filter; sintering to form a conductive silver layer; the step of cleaning and drying the ceramic substrate of the filter is as follows:
step 1, alkaline cleaning: adding 2-6 wt% of alkaline cleaning agent and heating to 50-70 ℃ of deionized water for cleaning for 10-30 min;
step 2, washing: cleaning in deionized water for 10-20 min;
step 3, acid cleaning: cleaning for 10-30min in deionized water added with 2-6% of acidic cleaning agent;
step 4, washing: cleaning in deionized water for 10-20 min;
step 5, ultrasonic cleaning: ultrasonic cleaning is carried out in deionized water at normal temperature for 10-30 min;
step 6, hot water ultrasonic cleaning: ultrasonic cleaning is carried out in deionized water at the temperature of 60-80 ℃ for 10-30 min;
and 7, drying: drying the mixture for 20-30min at the temperature of 100-160 ℃.
Further, the step of sintering to form the conductive silver layer specifically uses the following sintering process: heating to 400 +/-30 ℃ at the speed of 55-60 ℃/min; heating to 600 +/-30 ℃ at the speed of 25-30 ℃/min; heating to 750 +/-30 ℃ at the speed of 21-25 ℃/min; heating to the melting point of the inorganic binder in the conductive silver paste at the speed of 15-20 ℃/min; heating at the rate of 0.5-1.0 ℃/min for 5 ℃; cooling to the melting point of the inorganic binder in the conductive silver paste at the speed of 0.5-1.0 ℃/min; cooling to 760 +/-30 ℃ at the speed of 15-20 ℃/min; naturally cooling to room temperature.
Preferably, the surface of the ceramic substrate of the filter is coated with conductive silver paste by using a spraying method.
Further preferably, the spraying thickness of the conductive silver paste is 10-18 μm.
Preferably, the step of sintering to form the conductive silver layer is performed using a continuous sintering furnace.
Based on the same inventive concept, the following technical scheme can be obtained:
a ceramic dielectric filter comprises a filter ceramic base body and a metal layer on the surface of the filter ceramic base body; the metal layer is obtained by using the surface metallization method of any one of the above technical schemes.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
on the basis of the traditional process of coating silver paste and then sintering, the cleaning and drying process of the ceramic substrate is greatly improved, and the cleaning mode of organically combining alkaline cleaning, acid cleaning, water washing and ultrasonic cleaning is adopted, so that dust, oil stains and the like which affect the surface of the ceramic substrate and are attached to the conductive silver layer can be thoroughly removed, and the adhesive force between the conductive silver layer and the surface of the ceramic substrate is effectively improved; the invention further improves the sintering process according to the characteristics of the conductive silver paste, further improves the surface metallization quality, greatly improves the adhesive force of the silver layer, and greatly reduces the insertion loss of the finally obtained ceramic dielectric filter.
Drawings
FIG. 1 is a schematic process flow diagram of an embodiment of the present invention.
Detailed Description
Aiming at the defects in the prior art, the invention aims to improve the ceramic substrate cleaning and drying process and the silver layer sintering process on the basis of the traditional process of coating silver paste and then sintering, thereby greatly improving the surface metallization quality with lower cost.
The inventor conducts intensive research on the traditional process of coating silver paste and then sintering, and finds that the existing cleaning process of deionized water and ultrasonic waves adopted by cleaning and drying the ceramic substrate is difficult to clean the surface of the ceramic substrate, and particularly fine dust and oil stains remained in the previous working procedures of forming, sintering and the like of the ceramic substrate can seriously affect the adhesive force of the silver layer. Therefore, there is a need for an improvement to the existing ceramic substrate cleaning and drying.
To this end, the inventor proposes a method for metallizing a surface of a ceramic dielectric filter according to the present invention, comprising: cleaning and drying the ceramic substrate of the filter; coating conductive silver paste on the surface of a ceramic substrate of the filter; sintering to form a conductive silver layer; the step of cleaning and drying the ceramic substrate of the filter is as follows:
step 1, alkaline cleaning: adding 2-6 wt% of alkaline cleaning agent and heating to 50-70 ℃ of deionized water for cleaning for 10-30 min;
step 2, washing: cleaning in deionized water for 10-20 min;
step 3, acid cleaning: cleaning for 10-30min in deionized water added with 2-6% of acidic cleaning agent;
step 4, washing: cleaning in deionized water for 10-20 min;
step 5, ultrasonic cleaning: ultrasonic cleaning is carried out in deionized water at normal temperature for 10-30 min;
step 6, hot water ultrasonic cleaning: ultrasonic cleaning is carried out in deionized water at the temperature of 60-80 ℃ for 10-30 min;
and 7, drying: drying the mixture for 20-30min at the temperature of 100-160 ℃.
In addition, in order to meet the performance requirements of the sintered silver paste such as conductivity, compactness and the like, the conductive silver paste is usually composed of conductive silver powder, an inorganic binder, an organic binder, an additive, a dispersing agent, a thixotropic agent and the like, wherein the inorganic binder is usually glass powder; the organic binder is usually one or more of ethyl cellulose, rosin and acrylic resin; the solvent is usually an aliphatic hydrocarbon, an aliphatic hydrocarbon derivative, an alcohol derivative, and an acetate derivative; the inorganic additive is one or more of zinc oxide, bismuth oxide, aluminum oxide, silver oxide and magnesium oxide; the dispersant is usually one or two of triamines citrate and polymethacrylic acid amine; the thixotropic agent is typically a polyamide wax or hydrogenated castor oil. The sintering process used in the prior art is generally to heat up to a sintering temperature (a temperature exceeding the melting point of an inorganic binder in conductive silver paste) at a fixed heating rate, then to keep the temperature for a period of time, and finally to naturally cool. The sintering process cannot give full play to the best performance of the silver paste.
Therefore, the inventor further proposes the following further improved technical scheme:
the step of sintering to form the conductive silver layer specifically uses the following sintering process: heating to 400 +/-30 ℃ at the speed of 55-60 ℃/min; heating to 600 +/-30 ℃ at the speed of 25-30 ℃/min; heating to 750 +/-30 ℃ at the speed of 21-25 ℃/min; heating to the melting point of the inorganic binder in the conductive silver paste at the speed of 15-20 ℃/min; heating at the rate of 0.5-1.0 ℃/min for 5 ℃; cooling to the melting point of the inorganic binder in the conductive silver paste at the speed of 0.5-1.0 ℃/min; cooling to 760 +/-30 ℃ at the speed of 15-20 ℃/min; naturally cooling to room temperature.
For the public to understand, the technical scheme of the invention is explained in detail by a specific embodiment and the accompanying drawings:
the inorganic binder in the conductive silver paste used in the embodiment is glass powder, and the melting point of the inorganic binder is 880 ℃; the continuous sintering furnace used in this example is most commonly used in actual production. As shown in fig. 1, the specific steps of the surface metallization of the ceramic dielectric filter in this embodiment are as follows:
s101, alkaline cleaning:
adding 2-6% alkaline cleaning agent into a cleaning tank filled with deionized water and heated, heating to 50-70 deg.C, and cleaning ceramic substrate of the filter for 10-30 min; the alkaline cleaning agent can adopt various common cleaning agents, such as ZJ880, dikang 90, RBS T115 and the like;
s102, washing:
putting the filter ceramic substrate subjected to alkaline cleaning into deionized water for cleaning for 10-20 min;
s103, acid cleaning:
adding 2-6% acidic cleaning agent into a cleaning tank filled with deionized water, and cleaning the ceramic substrate of the filter for 10-30 min; the acidic cleaning agent can adopt various common types of cleaning agents, such as RBS IND 945, FDK-829C, LEX-826 and the like;
s104, water washing:
putting the filter ceramic substrate subjected to acid cleaning into deionized water for cleaning for 10-20 min;
s105, ultrasonic cleaning:
putting the ceramic substrate of the filter into an ultrasonic cleaning tank filled with deionized water for cleaning for 10-30 min;
s106, ultrasonic hot water cleaning:
ultrasonically cleaning a ceramic matrix of the filter in deionized water at 60-80 ℃ for 10-30 min;
s107, drying:
putting the washed ceramic substrate of the filter into an oven at the temperature of 100-160 ℃ for drying for 20-30 min;
s108, conductive silver paste spraying:
spraying conductive silver paste on the surface of the ceramic substrate of the filter, wherein the thickness is controlled to be 10-18 mu m, and the preferred thickness is 15 mu m;
s109, drying:
drying in an oven at the temperature of 150-;
s110, sintering of the conductive silver layer:
the filter ceramic substrate with the conductive silver paste is sintered by setting a plurality of sintering temperature zones in a sintering furnace according to the following sintering process so as to form a conductive silver layer on the surface of the filter ceramic substrate: heating to 400 ℃ at the speed of 55-60 ℃/min; heating to 600 ℃ at the speed of 25-30 ℃/min; heating to 750 ℃ at the speed of 21-25 ℃/min; heating to 880 ℃ at the speed of 15-20 ℃/min; heating to 885 ℃ at the speed of 0.5-1.0 ℃/min; cooling to 880 ℃ at the speed of 0.5-1.0 ℃/min; cooling to 760 ℃ at a speed of 15-20 ℃/min; naturally cooling to room temperature. The sintering process does not adopt the traditional method of continuously preserving heat at the highest sintering temperature, but according to the melting point of the inorganic binder, after the melting point of the inorganic binder is reached, the temperature is raised to the peak temperature which is 5 ℃ higher than the melting point, so that the inorganic binder in the silver layer is fully melted to improve the adhesive force.
In order to verify the effect of the technical scheme of the invention, the ceramic dielectric filter prepared by the process is compared with the ceramic dielectric filter prepared by the traditional process, and the adhesion and insertion loss of the silver layer are analyzed, wherein the specific results are shown in the following table 1:
TABLE 1
| Test item | Conventional process | The invention |
| Insertion loss (max) dB | 0.95 | 0.79 |
| Insertion loss (Avg) dB | 0.69 | 0.56 |
| Silver layer adhesion (Avg) N/mm2 | 16.4 | 25.8 |
Obviously, the insertion loss performance and the silver layer adhesive force of the ceramic dielectric filter obtained by the surface metallization method are improved by more than 15 percent compared with those of the traditional scheme, and the method does not need to use complex and expensive process equipment such as magnetron sputtering, vacuum plating and the like, does not need to use a plurality of different metal layers for compounding, has no obvious increase in cost compared with the traditional process, and is extremely suitable for large-scale production.
Claims (6)
1. A method of metallizing a surface of a ceramic dielectric filter comprising: cleaning and drying the ceramic substrate of the filter; coating conductive silver paste on the surface of a ceramic substrate of the filter; sintering to form a conductive silver layer; the method is characterized in that the step of cleaning and drying the ceramic substrate of the filter is as follows:
step 1, alkaline cleaning: adding 2-6 wt% of alkaline cleaning agent and heating to 50-70 ℃ of deionized water for cleaning for 10-30 min;
step 2, washing: cleaning in deionized water for 10-20 min;
step 3, acid cleaning: cleaning for 10-30min in deionized water added with 2-6% of acidic cleaning agent;
step 4, washing: cleaning in deionized water for 10-20 min;
step 5, ultrasonic cleaning: ultrasonic cleaning is carried out in deionized water at normal temperature for 10-30 min;
step 6, hot water ultrasonic cleaning: ultrasonic cleaning is carried out in deionized water at the temperature of 60-80 ℃ for 10-30 min;
and 7, drying: drying the mixture for 20-30min at the temperature of 100-160 ℃.
2. The method of metallizing a surface of a ceramic dielectric filter as recited in claim 1, wherein said step of sintering to form the conductive silver layer comprises the following sintering process: heating to 400 +/-30 ℃ at the speed of 55-60 ℃/min; heating to 600 +/-30 ℃ at the speed of 25-30 ℃/min; heating to 750 +/-30 ℃ at the speed of 21-25 ℃/min; heating to the melting point of the inorganic binder in the conductive silver paste at the speed of 15-20 ℃/min; heating at the rate of 0.5-1.0 ℃/min for 5 ℃; cooling to the melting point of the inorganic binder in the conductive silver paste at the speed of 0.5-1.0 ℃/min; cooling to 760 +/-30 ℃ at the speed of 15-20 ℃/min; naturally cooling to room temperature.
3. A method for metallizing a surface of a ceramic dielectric filter according to claim 1 or 2, wherein a conductive silver paste is applied to the surface of the ceramic substrate of the filter by a spray coating method.
4. The method for metallizing the surface of a ceramic dielectric filter of claim 3 wherein the conductive silver paste is applied to a thickness of 10-18 μm.
5. A method for metallizing a surface of a ceramic dielectric filter according to claim 1 or 2, wherein said step of sintering to form the conductive silver layer is performed using a continuous sintering furnace.
6. A ceramic dielectric filter comprises a filter ceramic base body and a metal layer on the surface of the filter ceramic base body; the method for metallizing a metal surface of a semiconductor device is characterized in that the metal layer is obtained by the surface metallization method according to any one of claims 1 to 5.
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| CN111908954A (en) * | 2020-08-18 | 2020-11-10 | 广东国华新材料科技股份有限公司 | Resonator, filter and metallization method for resonator and filter |
| CN112615124A (en) * | 2020-12-28 | 2021-04-06 | 京信射频技术(广州)有限公司 | Dielectric waveguide filter and method for processing dielectric ceramic silver layer thereof |
| CN112934832A (en) * | 2021-04-19 | 2021-06-11 | 北京北方华创微电子装备有限公司 | Method for cleaning ceramic parts |
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2021
- 2021-11-19 CN CN202111375964.0A patent/CN114039188A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102664055A (en) * | 2012-04-11 | 2012-09-12 | 深圳市大富科技股份有限公司 | Conductive silver paste, method for preparing same and surface metallization method for microwave dielectric ceramics |
| CN104307781A (en) * | 2014-08-27 | 2015-01-28 | 富乐德科技发展（天津）有限公司 | Cleaning method for removing oxide film attached to surface of ceramic part |
| CN111908954A (en) * | 2020-08-18 | 2020-11-10 | 广东国华新材料科技股份有限公司 | Resonator, filter and metallization method for resonator and filter |
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