CN114976563A - Surface metallization process of ceramic filter - Google Patents

Surface metallization process of ceramic filter Download PDF

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Publication number
CN114976563A
CN114976563A CN202210485530.4A CN202210485530A CN114976563A CN 114976563 A CN114976563 A CN 114976563A CN 202210485530 A CN202210485530 A CN 202210485530A CN 114976563 A CN114976563 A CN 114976563A
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copper
ceramic filter
metallization layer
slurry
ceramic
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姜南求
朴灿映
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Suzhou Aicheng Technology Co ltd
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Suzhou Aicheng Technology Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01PWAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
    • H01P11/00Apparatus or processes specially adapted for manufacturing waveguides or resonators, lines, or other devices of the waveguide type
    • H01P11/007Manufacturing frequency-selective devices
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5111Ag, Au, Pd, Pt or Cu
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/88Metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01PWAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
    • H01P1/00Auxiliary devices
    • H01P1/20Frequency-selective devices, e.g. filters
    • H01P1/2002Dielectric waveguide filters
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to a surface metallization process of a ceramic filter, which comprises the following steps: firstly, preparing slurry by using copper powder and metal oxide powder; then evenly coating the ceramic filter blank on the surface of the ceramic filter blank; finally, sintering the copper alloy at high temperature in a reducing atmosphere after drying to form a copper metallization layer; compared with the traditional method that glass frit is added into silver components, the method adopts a Cu-O eutectic bonding mode to densify the metallization layer, so that the conductivity of the copper metallization layer is reduced to the minimum, meanwhile, the ceramic structure and the copper metallization layer are endowed with enough bonding strength, the price of copper is one tenth of that of silver, and the production cost is greatly reduced.

Description

Surface metallization process of ceramic filter
Technical Field
The invention relates to the technical field of ceramic filters, in particular to a surface metallization process of a ceramic filter.
Background
A Ceramic waveguide filter (Ceramic waveguide filter) is an RF filter that uses a cavity conductive metal structure to transmit RF (radio frequency, beyond the audible audio range of a human) signals. Ceramic waveguide filters filter frequencies, i.e. determining the pass and reject frequencies, according to the structural shape, which makes them a practical solution in the microwave (microwave) and millimeter wave (millimeter wave) bandwidths. In addition, high frequency signals can be transmitted with very low losses, and the short wavelength of the high frequency signals enables a relatively small waveguide filter structure.
One of the typical methods for manufacturing ceramic waveguide filters is to prepare powdery powder particles from oxides of CaCO3, MgO, and TiO2 as main raw materials by mixing, then mold the powdery powder particles by dp (dry press) or other molding equipment, and then sinter (sintering) the powder particles at a temperature of about 1350 to 1400 ℃ in a sintering furnace in an oxidizing atmosphere to obtain a ceramic structure. And forming a silver metallization layer (metalizing layer) from several microns to tens of microns on the surface of the ceramic structure by using silver paste (Ag paste), thereby forming the ceramic waveguide filter.
The existing ceramic waveguide filter adopts a mode of forming a metallization layer by using expensive silver paste, and in this case, the silver accounts for more than 60% of the total raw material cost, which can result in the increase of the whole manufacturing cost. In addition, in order to obtain sufficient bonding force between the silver metallization layer and the ceramic structure, glass frit (glass frit) needs to be added to the silver component, but the glass frit exists inside the metallization layer after sintering, and as shown in fig. 1, the conductivity of the silver metallization layer is also reduced by 20% to 30% or more.
Although the conventional copper paste (Cu paste) method can be used for forming a metallization layer on the surface of a ceramic waveguide filter, copper (5.8 × 107S/m) having a conductivity similar to silver (6.3 × 107S/m) has a problem that the conductivity is decreased by 30% or more when applicable because a dense metallization layer cannot be formed due to a glass frit contained in the paste as shown in fig. 2 if the conventional copper paste method is used.
Disclosure of Invention
The present invention is to overcome the disadvantages of the prior art and to provide a surface metallization process for a ceramic filter, in which a metallization layer is formed by a new bonding method using copper, which is less expensive than silver 1/10, to minimize the reduction in physical properties and to improve the cost.
In order to achieve the purpose, the invention adopts the technical scheme that: a surface metallization process of a ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at a high temperature in a reducing atmosphere to form the copper metallization layer.
Preferably, in step 1, the metal oxide powder is copper oxide powder or surface-oxidized copper powder.
Preferably, in step 1, the proportion of copper is 97-99.94%, and the proportion of oxygen is 0.06-3%.
Preferably, in step 3, the ceramic filter blank coated with the slurry is sintered at 1065-1083 ℃ in a reducing atmosphere.
Preferably, in step 3, the thickness of the copper metallization layer is 10-20 μm.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
compared with the traditional method that glass frit is added into silver components, the method adopts a Cu-O eutectic bonding mode to densify the metallization layer, so that the conductivity of the copper metallization layer is reduced to the minimum, meanwhile, the ceramic structure and the copper metallization layer are endowed with enough bonding strength, the price of copper is one tenth of that of silver, and the production cost is greatly reduced.
Drawings
The technical scheme of the invention is further explained by combining the accompanying drawings as follows:
FIG. 1 is a diagram of a metallization layer formed by adding glass to a silver composition according to the prior art;
FIG. 2 is a diagram of a metallization layer formed by adding glass to a copper composition according to the prior art;
FIG. 3 is a diagram of a metallization layer formed by Cu-O eutectic bonding in accordance with the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the embodiments.
Example 1
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 99.94 percent, and the oxygen accounts for 0.06 percent;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: the ceramic filter blank coated with the slurry was dried and then sintered at 1065-1083 c in a reducing atmosphere, as shown in fig. 3, to form a copper metallization layer.
Example 2
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 99.89 percent, and the oxygen accounts for 0.11 percent;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 3
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper content is 99.83 percent, and the oxygen content is 0.17 percent;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 4
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 99.78 percent, and the oxygen accounts for 0.22 percent;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 5
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper content is 99.66%, and the oxygen content is 0.34%;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and 3, step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 6
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 99.44 percent, and the oxygen accounts for 0.56 percent;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 7
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the proportion of copper is 99.22%, and the proportion of oxygen is 0.78%;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 8
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 99.00 percent, and the oxygen accounts for 1.00 percent;
and 2, step: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and 3, step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 9
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 98.50 percent, and the oxygen accounts for 1.50 percent;
and 2, step: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
Example 10
The surface metallization process of the ceramic filter comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder, wherein the copper accounts for 97 percent, and the oxygen accounts for 3 percent;
step 2: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at 1065-1083 ℃ in a reducing atmosphere to form the copper metallization layer.
The bond strengths of the copper metallization layers obtained in examples 1-10 are shown in the following table:
Figure BDA0003629039870000081
the results show that: in the case of O2 (oxygen), it may be supplied in the form of a metal oxide containing Cu2O, CuO or O2, and after bonding in a reducing atmosphere, the residual amount of O2 (oxygen) remaining after the actual reaction is less than the charged amount due to the reduction reaction in the reaction layer. Generally, an increase in the amount of O2 (oxygen) initially charged results in an increase in the bonding strength between the ceramic and copper layers during bonding, but since an increase in the amount of oxygen in the copper layer formed after bonding may lead to a decrease in electrical properties, it is preferable to use O2 (oxygen) initially charged at a level equivalent to a desired bonding strength.
The above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. The technical solutions formed by using equivalent transformation or equivalent substitution are all within the protection scope of the present invention.

Claims (5)

1. A surface metallization process of a ceramic filter is characterized in that: comprises the following steps:
step 1: preparing slurry by using copper powder and metal oxide powder;
and 2, step: uniformly coating the slurry prepared in the step (1) on the surface of a ceramic filter blank;
and step 3: and drying the ceramic filter blank coated with the slurry, and sintering at a high temperature in a reducing atmosphere to form the copper metallization layer.
2. The surface metallization process of a ceramic filter according to claim 1, characterized in that: in step 1, the metal oxide powder is copper oxide powder or copper powder with an oxidized surface.
3. The surface metallization process of a ceramic filter according to claim 2, characterized in that: in the step 1, the proportion of copper is 97-99.94%, and the proportion of oxygen is 0.06-3%.
4. A surface metallization process of a ceramic filter according to any of the claims 1-3, characterized in that: in step 3, the ceramic filter blank coated with the slurry is sintered at 1065-1083 ℃ in a reducing atmosphere.
5. The surface metallization process of a ceramic filter according to claim 4, characterized in that: in step 3, the thickness of the copper metallization layer is 10-20 μm.
CN202210485530.4A 2022-05-06 2022-05-06 Surface metallization process of ceramic filter Pending CN114976563A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0431725A2 (en) * 1989-09-25 1991-06-12 General Electric Company Direct bonded metal-substrate structures
US5161728A (en) * 1988-11-29 1992-11-10 Li Chou H Ceramic-metal bonding
CN111763450A (en) * 2020-05-21 2020-10-13 深圳市信维微电子有限公司 Slurry for 5G dielectric waveguide filter and preparation method thereof
CN113903495A (en) * 2021-09-17 2022-01-07 江苏国瓷泓源光电科技有限公司 Copper slurry for dielectric ceramic filter and preparation and spraying film forming methods thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5161728A (en) * 1988-11-29 1992-11-10 Li Chou H Ceramic-metal bonding
EP0431725A2 (en) * 1989-09-25 1991-06-12 General Electric Company Direct bonded metal-substrate structures
CN111763450A (en) * 2020-05-21 2020-10-13 深圳市信维微电子有限公司 Slurry for 5G dielectric waveguide filter and preparation method thereof
CN113903495A (en) * 2021-09-17 2022-01-07 江苏国瓷泓源光电科技有限公司 Copper slurry for dielectric ceramic filter and preparation and spraying film forming methods thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
J. F. BURGESS 等: "金属与陶瓷的直接键接以及在电子学中的应用", 半导体情报 *

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