CN108878055A - The preparation method of high conductivity metal layer applied to high-temperature co-fired ceramics - Google Patents

The preparation method of high conductivity metal layer applied to high-temperature co-fired ceramics Download PDF

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Publication number
CN108878055A
CN108878055A CN201810458117.2A CN201810458117A CN108878055A CN 108878055 A CN108878055 A CN 108878055A CN 201810458117 A CN201810458117 A CN 201810458117A CN 108878055 A CN108878055 A CN 108878055A
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preparation
temperature
wcu
fired ceramics
metal layer
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CN201810458117.2A
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CN108878055B (en
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张鹏飞
夏庆水
唐利锋
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CETC 55 Research Institute
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CETC 55 Research Institute
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal

Abstract

Proposed by the present invention is a kind of preparation method of high conductivity metal layer applied to high-temperature co-fired ceramics, is included the following steps:(1)Aluminium oxide green band is obtained by casting technique;(2)Prepare the WCu Metal slurry and W Metal slurry for meeting silk-screen printing;(3)WCu Metal slurry is printed on aluminium oxide green belt surface;(4)Using identical printed pattern, in WCu metallization pattern surface printing W Metal slurry;(5)It realizes that multilayer aluminium oxide green band combines using lamination stack technique and obtains metalization layer;(6)Single ripe porcelain porcelain piece is obtained by Sheng Qie and sintering.Advantage:Technical process is simple, and the square resistance for the high temperature co-firing substrate surface metallization prepared has both excellent bending strength, platability and preferable economy down to about 5m Ω.

Description

The preparation method of high conductivity metal layer applied to high-temperature co-fired ceramics
Technical field
The present invention relates to a kind of preparation methods of high conductivity metal layer applied to high-temperature co-fired ceramics, belong to Technical field of electronic encapsulation.
Background technique
The transmission end lead resistance of super high power solid state microwave device encapsulation can bring insertion loss and tube core operating voltage The problem of decline, and then device output power is influenced, especially in super high power solid state microwave device, such problems is especially Obviously.Develop according to the prior art, applying in the following 3-5 will reach in the radio frequency power tube output power of X-band 5000W.It being found by calculating, the transmission port of mainstream IK encapsulation 40m Ω can satisfy dozens to hundreds of earthenware part output and require, But pressure drop power loss introduced in super high power solid state microwave device reaches 0.6dB, seriously affects the output work of device Rate.
High-temperature co-fired ceramics(HTCC)Technology is the cofiring technology that sintering temperature is greater than 1000 DEG C.Because firing temperature is high, HTCC cannot be using low melting point metal materials such as gold, silver, copper, it is necessary to using the insoluble metals materials such as tungsten, molybdenum, manganese, these materials Resistance to oxidation, conductivity be not low, solderability is poor, it is difficult to meet in the encapsulation of high power solid state microwave device and draw since lead resistance is excessive The problems such as loss and tube core pressure drop for entering.At present about by adjusting printed metallization composition of layer to realize high-temperature co-fired ceramics The method of high conductivity metal layer preparation is rarely reported.Therefore, the high conductivity metal layer system of high-temperature co-fired ceramics is realized It is standby to require to be this field technology urgently to be resolved with the transmission lead resistance for meeting the encapsulation of high-power and super high power microwave device Problem.
Summary of the invention
Proposed by the present invention is a kind of preparation method of high conductivity metal layer applied to high-temperature co-fired ceramics, mesh Be solve the loss and tube core pressure drop of the excessive introducing of transmission lead resistance of high-power and super high power microwave device encapsulation The problems such as.
Technical solution of the invention:The preparation method of high conductivity metal layer applied to high-temperature co-fired ceramics, Include the following steps:
(1)Aluminium oxide green band is obtained by casting technique;
(2)Prepare the WCu Metal slurry and W Metal slurry for meeting silk-screen printing;
(3)WCu Metal slurry is printed on aluminium oxide green belt surface;
(4)Using identical printed pattern, in WCu metallization pattern surface printing W Metal slurry;
(5)It realizes that multilayer aluminium oxide green band combines using lamination stack technique and obtains metalization layer;
(6)Single ripe porcelain porcelain piece is obtained by Sheng Qie and sintering.
Advantages of the present invention:
1)Porcelain piece stable physical property, the transmission lead resistance that can satisfy the encapsulation of high-power and super high power microwave device are wanted It asks;
2)The square resistance of surface metalation significantly reduces in Microwave Power Tubes encapsulation down to about 5m Ω since lead resistance is excessive The loss and tube core pressure drop of introducing;
3)Technical process is simple, the cost of material is low, bending strength is excellent, platability is preferable.
Detailed description of the invention
Attached drawing 1 is the flow chart of the preparation method of the high conductivity metal layer applied to high-temperature co-fired ceramics.
Specific embodiment
As shown in Figure 1, being applied to the preparation method of the high conductivity metal layer of high-temperature co-fired ceramics, including walk as follows Suddenly:
(1)Aluminium oxide green band is obtained by casting technique;
(2)Prepare the WCu Metal slurry and W Metal slurry for meeting silk-screen printing;
(3)WCu Metal slurry is printed on aluminium oxide green belt surface;
(4)Using identical printed pattern, in WCu metallization pattern surface printing W Metal slurry;
(5)It realizes that multilayer aluminium oxide green band combines using lamination stack technique and obtains metalization layer;
(6)Single ripe porcelain porcelain piece is obtained by Sheng Qie and sintering.
The step(1)In casting technique be aluminium oxide casting technique using anhydrous PVB system.
The step(2)Select 1 μm of superfine cupper powder below, 0.7~2 μm of metal tungsten powder as conductive phase, with second The organic medias such as base cellulose, terpinol, DBP, CS12 are as carrier, with metal oxide, nonmetal oxide, magnesium silicic acid One of salt, metal oxide precursor or several inorganic material are as Binder Phase, by conductive gold by way of stirring Belong to and Binder Phase is dispersed in organic carrier and prepares WCu Metal slurry and W Metal slurry respectively.
The step(3)WCu Metal slurry is printed on aluminium oxide green band using silk-screen printing technique, is placed in 2min is dried in 45 DEG C of baking oven, forms uniform WCu layer of metallized film in green belt surface;
The step(4)Using silk-screen printing technique in step(3)In obtain WCu metallised image surface and republish one layer of W The metallization paste bed of material is placed in 45 DEG C of baking oven and dries 2min;
The step(5)Including by green band, lamination is laminated under 0.1 ~ 1.0KPSI pressure, and by the aluminum oxide multi-layer of preparation Ceramics are at 35 ~ 75 DEG C earnestly at individual unit;
The step(6)Including by step(5)The individual unit of middle acquisition is placed on Mo plate, is restored at 1000~1600 DEG C Property atmosphere under be sintered, obtain single ripe porcelain porcelain piece.
The aluminium oxide green band is ceramic whiteware green band or black porcelain green band.
The metalization layer with a thickness of 10 ~ 30 μm.
Embodiment
Technical solution of the present invention is further illustrated below according to embodiment.
The preparation of high conductivity metal layer applied to high-temperature co-fired ceramics, includes the following steps:
Step 1:Aluminium oxide green band is prepared using the aluminium oxide casting technique of anhydrous PVB system, uses ceramic whiteware in the present embodiment Al2O3Green band can according to need in specific implementation using black porcelain Al2O3Green band;
Step 2:Select 0.3 ~ 1.0 μm of superfine cupper powder, 0.7~2 μm of metal tungsten powder as conductive phase, with ethyl cellulose, The organic medias such as terpinol, DBP, CS12 are as carrier, using metal oxide, nonmetal oxide as Binder Phase, by stirring Conductive metal and Binder Phase are dispersed in organic carrier by the mode mixed, and are prepared WCu and W respectively according to certain C u, W ratio and are starched Material;
Step 3:WCu Metal slurry is printed on aluminium oxide green band using silk-screen printing by the silk screen for selecting certain figure On, it is placed in 45 DEG C of baking oven and dries 2min, which is 8 ~ 20 μm;
Step 4:W Metal slurry is printed on WCu figure dry film, is placed in 45 DEG C by the chromatography silk screen for selecting same figure Baking oven in dry 2min, the W thickness of dry film be 5 ~ 16 μm;
Step 5:By above-mentioned green band, lamination is laminated under 0.1KPSI pressure, and by the aluminum oxide multi-layer ceramics of preparation 35 ~ Earnestly at individual unit at 75 DEG C;
Step 6:The individual unit obtained in step 5 is placed on Mo plate, is sintered under 1430 DEG C, reducing atmosphere, is obtained Single ripe porcelain;
Step 7:Test the metalization layer resistance on ripe porcelain surface.
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not Therefore limitations on the scope of the patent of the present invention are interpreted as.It should be pointed out that those skilled in the art, not taking off Under the premise of from present inventive concept, several improvement can also be made, these are all within the scope of protection of the present invention.Therefore, this hair The scope of protection shall be subject to the appended claims for bright patent.

Claims (9)

1. being applied to the preparation method of the high conductivity metal layer of high-temperature co-fired ceramics, it is characterized in that including the following steps:
(1)Aluminium oxide green band is obtained by casting technique;
(2)Prepare the WCu Metal slurry and W Metal slurry for meeting silk-screen printing;
(3)WCu Metal slurry is printed on aluminium oxide green belt surface;
(4)Using identical printed pattern, in WCu metallization pattern surface printing W Metal slurry;
(5)It realizes that multilayer aluminium oxide green band combines using lamination stack technique and obtains metalization layer;
(6)Single ripe porcelain porcelain piece is obtained by Sheng Qie and sintering.
2. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the step(1)In casting technique be aluminium oxide casting technique using anhydrous PVB system.
3. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the step(2)Select 1 μm of superfine cupper powder below, 0.7~2 μm of metal tungsten powder as conductive phase, with ethyl fibre Element, terpinol, DBP, CS12 organic media are tieed up as carrier, with metal oxide, nonmetal oxide, magnesium silicate, metal One of oxide precursor or several inorganic material are as Binder Phase, by conductive metal and bonding by way of stirring It is mutually dispersed in organic carrier and prepares WCu Metal slurry and W Metal slurry respectively.
4. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the step(3)WCu Metal slurry is printed on aluminium oxide green band using silk-screen printing technique, is placed in 45 DEG C Baking oven in dry 2min, form uniform WCu layer of metallized film in green belt surface.
5. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the step(4)Using silk-screen printing technique in step(3)In obtain WCu metallised image surface and republish one layer of W The metallization paste bed of material is placed in 45 DEG C of baking oven and dries 2min.
6. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the step(5)Including by green band, lamination is laminated under 0.1 ~ 1.0KPSI pressure, and by the aluminum oxide multi-layer of preparation Ceramics are at 35 ~ 75 DEG C earnestly at individual unit.
7. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the step(6)Including by step(5)The individual unit of middle acquisition is placed on Mo plate, is restored at 1000~1600 DEG C Property atmosphere under be sintered, obtain single ripe porcelain porcelain piece.
8. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is that the aluminium oxide green band is ceramic whiteware green band or black porcelain green band.
9. the preparation method of the high conductivity metal layer according to claim 1 applied to high-temperature co-fired ceramics, special Sign is the metalization layer with a thickness of 10 ~ 30 μm.
CN201810458117.2A 2018-05-14 2018-05-14 Preparation method of high-conductivity metallization layer applied to high-temperature co-fired ceramic Active CN108878055B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113130111A (en) * 2019-12-30 2021-07-16 郑州登电银河科技有限公司 Hole-filling printing slurry for HTCC and preparation method thereof
CN116003166A (en) * 2022-12-05 2023-04-25 中国电子科技集团公司第五十五研究所 Medium-temperature ceramic suitable for microwave power device packaging shell and preparation method

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CN2879427Y (en) * 2006-01-10 2007-03-14 中国电子科技集团公司第十三研究所 Visible light power luminous tube for metal ceramic casing package
CN101118939A (en) * 2006-08-02 2008-02-06 中强光电股份有限公司 Luminous element packaging device
CN102314957A (en) * 2011-07-06 2012-01-11 中国电子科技集团公司第五十五研究所 Multilayer high-temperature co-fired-ceramic thick-film tungsten conductor paste and preparation method thereof
CN105347777A (en) * 2015-11-30 2016-02-24 中国电子科技集团公司第五十五研究所 Method for preparing low-loss high-temperature co-firing aluminum oxide black porcelain applied to high-frequency circuit

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0211063A1 (en) * 1985-01-22 1987-02-25 American National Can Company Redundant control system for automatic forming machine
CN2879427Y (en) * 2006-01-10 2007-03-14 中国电子科技集团公司第十三研究所 Visible light power luminous tube for metal ceramic casing package
CN101118939A (en) * 2006-08-02 2008-02-06 中强光电股份有限公司 Luminous element packaging device
CN102314957A (en) * 2011-07-06 2012-01-11 中国电子科技集团公司第五十五研究所 Multilayer high-temperature co-fired-ceramic thick-film tungsten conductor paste and preparation method thereof
CN105347777A (en) * 2015-11-30 2016-02-24 中国电子科技集团公司第五十五研究所 Method for preparing low-loss high-temperature co-firing aluminum oxide black porcelain applied to high-frequency circuit

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113130111A (en) * 2019-12-30 2021-07-16 郑州登电银河科技有限公司 Hole-filling printing slurry for HTCC and preparation method thereof
CN116003166A (en) * 2022-12-05 2023-04-25 中国电子科技集团公司第五十五研究所 Medium-temperature ceramic suitable for microwave power device packaging shell and preparation method
CN116003166B (en) * 2022-12-05 2024-04-12 中国电子科技集团公司第五十五研究所 Medium-temperature ceramic suitable for microwave power device packaging shell and preparation method

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