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CN111763450A - Slurry for 5G dielectric waveguide filter and preparation method thereof - Google Patents

Slurry for 5G dielectric waveguide filter and preparation method thereof Download PDF

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Publication number
CN111763450A
CN111763450A CN202010435788.4A CN202010435788A CN111763450A CN 111763450 A CN111763450 A CN 111763450A CN 202010435788 A CN202010435788 A CN 202010435788A CN 111763450 A CN111763450 A CN 111763450A
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CN
China
Prior art keywords
slurry
dielectric waveguide
waveguide filter
filter according
organic solvent
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Pending
Application number
CN202010435788.4A
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Chinese (zh)
Inventor
苏聪
虞成城
宋喆
姚月月
徐帆
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Shenzhen Xinwei Microelectronics Co ltd
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Shenzhen Xinwei Microelectronics Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
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Priority to CN202010435788.4A priority Critical patent/CN111763450A/en
Publication of CN111763450A publication Critical patent/CN111763450A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C09D129/14Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
    • 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
    • C04B41/5127Cu, e.g. Cu-CuO eutectic
    • 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • 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
    • 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
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/085Copper
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2262Oxides; Hydroxides of metals of manganese

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

The invention discloses slurry for a 5G dielectric waveguide filter and a preparation method thereof, wherein the slurry comprises the following raw materials in percentage by weight: 2-3% of additive, 1-2% of glass, 0.5-1% of dispersing agent, 10-15% of resin colloid, and the balance of copper powder and organic solvent. The Cu slurry replaces Ag to carry out surface metallization of the filter, so that the cost of a metallization material can be greatly reduced, and the reliability of a product is improved.

Description

Slurry for 5G dielectric waveguide filter and preparation method thereof
Technical Field
The invention relates to the technical field of communication, in particular to slurry for a 5G dielectric waveguide filter and a preparation method thereof.
Background
Generally, the metallization process of the ceramic dielectric surface includes screen printing, bulk dipping of Ag, surface silver spraying, and the like. However, the metallized Ag paste used in each process is a noble metal and has high cost. And the high-performance Ag pulp mainly takes imported Ag pulp and is high in price. In addition, the use of Ag paste itself has some problems that are difficult to overcome, for example, Ag ions are easy to migrate at the interface of the ceramic material. In the field of microwave devices, a dielectric waveguide filter for a base station has a severe application environment and needs to be used for a long time at the temperature of-40-150 ℃, and the migration of Ag ions increases the product risk.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the slurry for the 5G dielectric waveguide filter and the preparation method thereof are provided, so that the cost can be effectively reduced, and the reliability of the product can be improved.
In order to solve the technical problems, the invention adopts the technical scheme that:
the slurry for the 5G dielectric waveguide filter comprises the following raw materials in percentage by weight: 2-3% of additive, 1-2% of glass, 0.5-1% of dispersing agent, 10-15% of resin colloid, and the balance of copper powder and organic solvent.
The invention adopts another technical scheme that:
the preparation method of the slurry for the 5G dielectric waveguide filter comprises the steps of mixing copper powder, an additive, glass, a dispersing agent and an organic solvent, and then carrying out ball milling to obtain a first mixture; and adding resin colloid into the first mixture, and grinding to obtain the slurry for the 5G dielectric waveguide filter.
The invention has the beneficial effects that: the Cu slurry replaces Ag to carry out surface metallization of the filter, so that the cost of a metallization material can be greatly reduced; through the filter metallized by the Cu paste, the failure risk of the product caused by Ag ion migration is avoided, the reliability of the product in a severe application environment is favorably improved, and the service life of the product is prolonged.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is as follows: the Cu slurry replaces Ag to carry out surface metallization of the filter, so that the cost of a metallization material can be greatly reduced, and the reliability of a product is improved.
The slurry for the 5G dielectric waveguide filter comprises the following raw materials in percentage by weight: 2-3% of additive, 1-2% of glass, 0.5-1% of dispersing agent, 10-15% of resin colloid, and the balance of copper powder and organic solvent.
From the above description, the beneficial effects of the present invention are: the Cu slurry replaces Ag to carry out surface metallization of the filter, so that the cost of a metallization material can be greatly reduced; through the filter metallized by the Cu paste, the failure risk of the product caused by Ag ion migration is avoided, the reliability of the product in a severe application environment is favorably improved, and the service life of the product is prolonged.
Further, the viscosity of the slurry is 100-300 cps.
As can be seen from the above description, the viscosity of the slurry can be adjusted by adjusting the ratio of the copper powder to the organic solvent.
Further, the additive is a mixture of manganese oxide and bismuth oxide, and the mass ratio of the manganese oxide to the bismuth oxide in the additive is 1: 1.
Furthermore, the glass is calcium-boron-silicon glass, and the softening point temperature of the glass is 600-800 ℃.
Further, the particle size D50 of the copper powder is 100-400 nm.
Further, the resin colloid is a mixture of PVB resin and an organic solvent.
Further, the organic solvent is at least one of butyl carbitol, terpineol and petroleum ether.
Further, the dispersing agent is at least one of triethyl phosphate and a silane coupling agent.
From the above description, the kinds of the organic solvent and the dispersant may be selected as required.
The invention relates to another technical scheme which is as follows:
the preparation method of the slurry for the 5G dielectric waveguide filter comprises the steps of mixing copper powder, an additive, glass, a dispersing agent and an organic solvent, and then carrying out ball milling to obtain a first mixture; and adding resin colloid into the first mixture, and grinding to obtain the slurry for the 5G dielectric waveguide filter.
As can be seen from the above description, the preparation process of the slurry is simple and the cost is low.
Further, ball milling was performed by a planetary ball mill, and milling was performed by a three-roll mill.
Example one
The embodiment one of the invention is a slurry for a 5G dielectric waveguide filter, which comprises the following raw materials in percentage by weight: 2-3% of additive, 1-2% of glass, 0.5-1% of dispersing agent, 10-15% of resin colloid, and the balance of copper powder and organic solvent. The proportion of the copper powder and the resin can be adjusted according to the needs, and when the amount of the organic solvent is large, the viscosity of the obtained slurry is small; when the amount of copper powder is large, the viscosity of the resulting slurry becomes large. The particle size D50 of the copper powder is 100-400 nm.
In this embodiment, the additive is a mixture of manganese oxide and bismuth oxide, and the mass ratio of manganese oxide to bismuth oxide in the additive is 1: 1. The glass is calcium-boron-silicon glass, and the softening point temperature of the glass is 600-800 ℃. The resin colloid is a mixture of PVB resin and an organic solvent, the organic solvent used in the resin colloid is the same as the organic solvent, the resin colloid can be obtained by mixing the organic solvent and the PVB resin according to the volume ratio of 2:1, and the resin colloid can be obtained after the PVB resin is completely dissolved in the organic solvent. The organic solvent is at least one of butyl carbitol, terpineol and petroleum ether. The dispersant is at least one of triethyl phosphate and a silane coupling agent (such as KH 550).
The preparation method of the slurry for the 5G dielectric waveguide filter comprises the following steps: mixing copper powder, an additive, glass, a dispersing agent and an organic solvent, and then carrying out ball milling to obtain a first mixture; and adding resin colloid into the first mixture, and grinding to obtain the slurry for the 5G dielectric waveguide filter. In the embodiment, the ball milling is carried out by a planetary ball mill for 4-8 h, and the grinding is carried out by a three-roller grinding machine, so that the viscosity of the finally obtained slurry is 100-300 cps.
Example two
The second embodiment of the invention is a slurry for a 5G dielectric waveguide filter, which is different from the first embodiment in that:
the slurry comprises the following raw materials in percentage by weight: 2.5 percent of additive, 1.5 percent of glass, 0.8 percent of dispersant, 12 percent of resin colloid, and the balance of copper powder and organic solvent. Wherein the organic solvent is butyl carbitol, and the dispersant is triethyl phosphate.
EXAMPLE III
The third embodiment of the invention is a slurry for a 5G dielectric waveguide filter, which is different from the first embodiment in that:
the slurry comprises the following raw materials in percentage by weight: 2% of additive, 2% of glass, 0.5% of dispersant, 10% of resin colloid and the balance of copper powder and organic solvent. Wherein the organic solvent is terpineol, and the dispersant is KH 550.
Example four
The fourth embodiment of the invention is a slurry for a 5G dielectric waveguide filter, which is different from the first embodiment in that:
the slurry comprises the following raw materials in percentage by weight: 3% of additive, 1% of glass, 1% of dispersant, 15% of resin colloid, and the balance of copper powder and organic solvent. Wherein the organic solvent is petroleum ether, and the dispersant is KH 550.
And spraying the slurry prepared in the second to fourth embodiments on blind holes, through grooves, small holes, surfaces and side surfaces of the ceramic substrate by using a spraying device, wherein the spraying thickness is 10-15 μm. The dried ceramic matrix surface copper paste has good appearance, uniform coating and no adverse phenomena such as falling, sagging and the like.
And then sintering the dried ceramic matrix at 850-890 ℃ in a protective atmosphere, wherein the sintered copper crystal grains grow well and have compact structure. The ceramic substrate was subjected to an insertion loss test, and the test results are shown in table 1.
Table 1 results of performance testing
Sample (I) Appearance of the product Loss of insertion
Silver paste sample All have no cracks -0.67dB@3.5GHz
Example two All have no cracks -0.68dB@3.5GHz
EXAMPLE III All have no cracks -0.69dB@3.5GHz
Example four All have no cracks -0.68dB@3.5GHz
The silver paste samples in table 1 are filter silver pastes purchased from hunan reed electronic paste limited.
As can be seen from Table 1, after the slurry prepared by the invention is used for a ceramic dielectric filter, the appearance of the ceramic dielectric filter is not cracked, the insertion loss is equivalent to that of a silver paste sample, and the cost can be greatly reduced.
In summary, according to the slurry for the 5G dielectric waveguide filter and the preparation method thereof provided by the invention, the Cu slurry replaces Ag to carry out surface metallization on the filter, so that the cost of a metallization material can be greatly reduced, and the reliability of a product is improved.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.

Claims (10)

1. The slurry for the 5G dielectric waveguide filter is characterized by comprising the following raw materials in percentage by weight: 2-3% of additive, 1-2% of glass, 0.5-1% of dispersing agent, 10-15% of resin colloid, and the balance of copper powder and organic solvent.
2. The slurry for a 5G dielectric waveguide filter according to claim 1, wherein the viscosity of the slurry is 100 to 300 cps.
3. The slurry for a 5G dielectric waveguide filter according to claim 1, wherein the additive is a mixture of manganese oxide and bismuth oxide, and the mass ratio of manganese oxide to bismuth oxide in the additive is 1: 1.
4. The paste for a 5G dielectric waveguide filter according to claim 1, wherein the glass is a calboro-silicate glass having a softening point temperature of 600 to 800 ℃.
5. The slurry for a 5G dielectric waveguide filter according to claim 1, wherein the particle diameter D50 of the copper powder is 100 to 400 nm.
6. The paste for a 5G dielectric waveguide filter according to claim 1, wherein the resin colloid is a mixture of PVB resin and an organic solvent.
7. The slurry for a 5G dielectric waveguide filter according to claim 6, wherein the organic solvent is at least one of butyl carbitol, terpineol and petroleum ether.
8. The paste for a 5G dielectric waveguide filter according to claim 1, wherein the dispersant is at least one of triethyl phosphate and a silane coupling agent.
9. The method of preparing a slurry for a 5G dielectric waveguide filter according to any one of claims 1 to 8, wherein copper powder, an additive, glass, a dispersant and an organic solvent are mixed and then ball-milled to obtain a first mixture; and adding resin colloid into the first mixture, and grinding to obtain the slurry for the 5G dielectric waveguide filter.
10. The method of preparing a slurry for a 5G dielectric waveguide filter according to claim 9, wherein the ball milling is performed by a planetary ball mill and the milling is performed by a three-roll mill.
CN202010435788.4A 2020-05-21 2020-05-21 Slurry for 5G dielectric waveguide filter and preparation method thereof Pending CN111763450A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114976563A (en) * 2022-05-06 2022-08-30 苏州艾成科技技术有限公司 Surface metallization process of a ceramic filter
CN115274177A (en) * 2021-04-30 2022-11-01 南京以太通信技术有限公司 Copper paste for metallization, glass powder and preparation method, dielectric filter
CN115274176A (en) * 2021-04-30 2022-11-01 南京以太通信技术有限公司 Metallization method, copper paste for metallization, preparation method and dielectric filter

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115274177A (en) * 2021-04-30 2022-11-01 南京以太通信技术有限公司 Copper paste for metallization, glass powder and preparation method, dielectric filter
CN115274176A (en) * 2021-04-30 2022-11-01 南京以太通信技术有限公司 Metallization method, copper paste for metallization, preparation method and dielectric filter
CN114976563A (en) * 2022-05-06 2022-08-30 苏州艾成科技技术有限公司 Surface metallization process of a ceramic filter

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Application publication date: 20201013