CN114230374A - Silicon nitride surface metallization method - Google Patents

Silicon nitride surface metallization method Download PDF

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Publication number
CN114230374A
CN114230374A CN202111546449.4A CN202111546449A CN114230374A CN 114230374 A CN114230374 A CN 114230374A CN 202111546449 A CN202111546449 A CN 202111546449A CN 114230374 A CN114230374 A CN 114230374A
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silicon nitride
laser
ceramic
nitride ceramic
metal
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惠宇
武英斌
姜伟伟
孙文萍
郭佳星
刘旭东
那兆霖
王兴安
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Dalian University
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Dalian University
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    • 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
    • C04B41/5116Ag or Au
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/36Removing material
    • B23K26/362Laser etching
    • 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
    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • 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
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/45Coating 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
    • C04B41/5144Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the metals of the iron group
    • CCHEMISTRY; METALLURGY
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    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/50Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
    • B23K2103/52Ceramics

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Abstract

The invention belongs to the technical field of metallization, and discloses a method for metalizing a silicon nitride surface. The technical scheme of the invention realizes the modification of the surface of the silicon nitride ceramic, can obtain a uniform and compact active metal conducting layer which is well connected with the ceramic matrix on the surface of the silicon nitride ceramic, relieves the stress between the ceramic matrix and the metal coating, and obviously improves the spreadability and wettability of the brazing filler metal on the surface of the ceramic in the brazing process.

Description

Silicon nitride surface metallization method
Technical Field
The invention belongs to the technical field of metallization, and particularly relates to a silicon nitride surface metallization method.
Background
The silicon nitride ceramic is an inorganic nonmetal strong covalent bond compound, has the advantages of high specific strength, high specific modulus, high temperature resistance, oxidation resistance, wear resistance, high thermal shock resistance and the like, and has special use value in the working environment with high temperature, high speed and strong corrosive medium. However, due to the disadvantages of large brittleness, low ductility, difficult processing and the like, the application of the ceramic material in engineering is limited to a great extent, parts with large size and complex shape are difficult to manufacture for use, and the metal material has excellent room temperature strength and ductility, and a ceramic-metal composite member is obtained by connecting the ceramic and the metal, so that the advantages of the ceramic and the metal can be combined, the excellent performance of the ceramic material can be fully exerted, and the application range of the ceramic is further expanded. Therefore, the silicon nitride ceramic surface metallization is realized by adopting a proper method, and the active metal coating is prepared, so that the wear resistance of the ceramic can be improved, the wetting and spreading performance of the brazing filler metal on the ceramic surface in the brazing process can be improved, and the method has a particularly important significance for improving the internal stress distribution state of a structural member, reducing the manufacturing cost and widening the application range of the ceramic material.
Common ceramic surface metallization methods include a chemical Ni plating method, an electroplating Ni method, a sintering Ag method, a Mo-Mn method and a vacuum evaporation coating method, but the traditional metallization method is long in time consumption and high in cost. The properties of the silicon nitride ceramic such as hardness and toughness are different from those of common dense ceramics, so that the traditional metallization method cannot be well applied to realizing the surface metallization of the silicon nitride ceramic.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the surface metallization method of the silicon nitride ceramic, which can be implemented at room temperature, does not need post-treatment, has low cost, and can realize the surface modification of the silicon nitride ceramic and the high-strength effective connection between the silicon nitride ceramic and a metal material.
The above purpose of the invention is realized by the following technical scheme:
a silicon nitride surface metallization method specifically comprises the following steps: and completely covering the laser-etched uniform metal conducting layer on the surface of the silicon nitride ceramic through laser scanning.
Further, the method comprises the following specific implementation steps:
the method comprises the following steps: drawing a pattern of a metalized area on laser parameter control software carried by the fiber laser according to the size of the silicon nitride ceramic igniter and setting laser parameters;
step two: placing the silicon nitride ceramic igniter on a laser workbench, and coating a metal foil on the surface of the silicon nitride ceramic igniter to enable the metal foil to be tightly attached to the silicon nitride ceramic;
step three: and starting a power supply of the optical fiber laser, and then starting laser etching until laser completes one scanning according to the path of the pattern of the metalized area, which indicates that the laser scanning etching is finished, and forming a metal layer on the surface of the silicon nitride ceramic, namely completing the metallization of the surface of the silicon nitride ceramic.
Furthermore, after the third step is completed, the second step and the third step can be repeated on the obtained product, and any one of copper, silver and nickel metal foils can be selected in the process of repeating the second step, and the repeated etching times are 1-10 times.
Furthermore, the method further comprises the following step four: the metallized silicon substrate waits for soldering or surface circuit etching.
As a further alternative, the pattern of the metalized area is designed according to the size of the ceramic, and includes a rectangular shape, a circular shape or other figures.
As a further alternative, the metal foil comprises any one of copper, silver and nickel sheets, and the thickness is 10 μm to 20 μm.
Furthermore, the optical fiber laser adopted by the method is produced by Changchun optical precision machinery and physical research institute of Chinese academy of sciences, New Changchun industry optoelectronics technology Co., Ltd, and is JK-MAX-50 with the number of HPW-YE0560D, and the laser parameter control software is EZCad2.5.3.
Furthermore, the power of the optical fiber laser is 0-1000W, the scanning speed is 1-1000mm/s, and the scanning distance is 0.01-1 mm.
Compared with the prior art, the invention has the beneficial effects that:
the technical scheme of the invention realizes the modification of the surface of the silicon nitride ceramic, can obtain a uniform and compact active metal conducting layer which is well connected with the ceramic matrix on the surface of the silicon nitride ceramic, relieves the stress between the ceramic matrix and the metal coating, and obviously improves the spreadability and wettability of the brazing filler metal on the surface of the ceramic in the brazing process.
1. The invention focuses on a method for forming a metal conducting layer on the surface of ceramic through copper-clad sheet laser etching, the laser etching method can be effectively applied to the surface modification of ceramic, silicon nitride ceramic is selected as a substrate, and the existence of a ceramic porous structure can buffer and absorb the energy of laser in the etching process, so that a metallization layer is melted on the surface of the ceramic, permeates into pores and reacts in a ceramic aggregate to form the tightly connected metal conducting layer. The formation of the metallized conducting layer improves the wear resistance of the surface of the silicon nitride ceramic and obviously improves the spreadability and wettability of the brazing filler metal on the surface of the ceramic in the brazing process.
2. Compared with the prior high-temperature sintering technology, the method does not need post-heat treatment, saves a large amount of energy, the power of the high-temperature sintering furnace is about 10KW, and the power of equipment used by the method does not exceed 300W, so the method saves a large amount of energy and has low cost.
3. The metal layer is a single metal uniform conducting layer, and is simpler, and has better electrical conductivity and thermal conductivity compared with the prior metal mixture.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources.
Example 1
S1, drawing related metallized area patterns in a computer by using EZCad2.5.3 software, and setting laser parameters, wherein the laser power is 600W, the scanning speed is 200mm/s, and the scanning distance is 0.02 mm;
s2, horizontally placing the silicon nitride ceramic substrate on a laser processing workbench, and covering a layer of copper foil with the thickness of 10 mu m on the surface of the ceramic to enable the copper foil to be tightly attached to the ceramic;
s3, starting a power supply of the optical fiber laser, aligning the laser focal length to the ceramic metalized area, and starting to perform laser scanning to etch the copper foil;
s4, the metallized silicon nitride ceramics waits for welding or surface circuit etching is carried out. After brazing at 400 ℃ under the temperature of 300-.
Example 2
S1, drawing related metallized area patterns in a computer by using EZCad2.5.3 software, and setting laser parameters, wherein the laser power is 600W, the scanning speed is 200mm/s, and the scanning distance is 0.02 mm;
s2, horizontally placing the silicon nitride ceramic substrate on a laser processing workbench, and covering a silver foil with the thickness of 10 mu m on the surface of the ceramic to enable the silver foil to be tightly attached to the ceramic;
s3, starting a power supply of the optical fiber laser, aligning the laser focal length to the ceramic metalized area, and starting to perform laser scanning etching on the silver foil;
s4, the metallized silicon nitride ceramics waits for welding or surface circuit etching is carried out. After brazing at 400 ℃ under the temperature of 300-.
Example 3
S1, drawing related metallized area patterns in a computer by using EZCad2.5.3 software, and setting laser parameters, wherein the laser power is 600W, the scanning speed is 200mm/s, and the scanning distance is 0.02 mm;
s2, placing the silicon nitride ceramic substrate on a laser processing workbench, and covering a layer of nickel foil with the thickness of 10 mu m on the surface of the ceramic to enable the nickel foil to be tightly attached to the ceramic;
s3, starting a power supply of the optical fiber laser, aligning the laser focal length to the ceramic metalized area, and starting to perform laser scanning etching on the silver foil;
s4, the metallized silicon nitride ceramics waits for welding or surface circuit etching is carried out. After brazing at 400 ℃ under the temperature of 300-.
The above embodiments of the present invention are described in detail, and specific embodiments are applied to illustrate the principle and the implementation manner of the present invention, and the above description of the embodiments is only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and the content of the present specification should not be construed as a limitation to the present invention.

Claims (8)

1. A silicon nitride surface metallization method is characterized by specifically comprising the following steps: and completely covering the laser-etched uniform metal conducting layer on the surface of the silicon nitride ceramic through laser scanning.
2. The silicon nitride surface metallization method of claim 1, characterized by the specific implementation steps of:
the method comprises the following steps: drawing a pattern of a metalized area on laser parameter control software carried by the fiber laser according to the size of the silicon nitride ceramic igniter and setting laser parameters;
step two: placing the silicon nitride ceramic igniter on a laser workbench, and coating a metal foil on the surface of the silicon nitride ceramic igniter to enable the metal foil to be tightly attached to the silicon nitride ceramic;
step three: and starting a power supply of the optical fiber laser, and then starting laser etching until laser completes one scanning according to the path of the pattern of the metalized area, which indicates that the laser scanning etching is finished, and forming a metal layer on the surface of the silicon nitride ceramic, namely completing the metallization of the surface of the silicon nitride ceramic.
3. The method for metalizing silicon nitride surface according to claim 2, wherein the obtained product can be repeated in the second step and the third step after the third step is completed, and any one of copper, silver and nickel metal foils can be selected during the repeated step two, and the repeated etching times are 1-10 times.
4. A method for metallizing a silicon nitride surface as defined in claim 2 further comprising the steps of four: the metallized silicon substrate waits for soldering or surface circuit etching.
5. The method of claim 2, wherein the pattern of the first metalized area is designed according to ceramic dimensions, and comprises a rectangle, a circle or other figures.
6. The method of claim 2, wherein the metal foil of step two comprises any one of a copper foil, a silver foil and a nickel foil, and has a thickness of 10 μm to 20 μm.
7. The method of claim 2, wherein the model of the fiber laser used in the third step is JK-MAX-50, and the laser parameter control software is ezcad2.5.3.
8. The silicon nitride surface metallization method of claim 2, wherein the power of the fiber laser in step three is 0-1000W, the scanning speed is 1-1000mm/s, and the scanning distance is 0.01-1 mm.
CN202111546449.4A 2021-12-16 2021-12-16 Silicon nitride surface metallization method Pending CN114230374A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6437484A (en) * 1987-08-04 1989-02-08 Nippon Steel Corp Metallizing of ceramic by active metal
JPS6437483A (en) * 1987-08-04 1989-02-08 Nippon Steel Corp Metallizing of ceramic by alloy comprising noble metal as main component
CN103880478A (en) * 2012-12-21 2014-06-25 比亚迪股份有限公司 Ceramic surface selective metallization method and ceramic
CN106413270A (en) * 2016-11-04 2017-02-15 大连大学 Aluminum nitride ceramic circuit board and preparation method thereof
CN110240494A (en) * 2019-06-28 2019-09-17 大连大学 A kind of fiber reinforcement Cf/SiC composite plate weld connector
CN111269028A (en) * 2020-03-05 2020-06-12 哈尔滨工业大学(威海) Silicon nitride ceramic surface metallization method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6437484A (en) * 1987-08-04 1989-02-08 Nippon Steel Corp Metallizing of ceramic by active metal
JPS6437483A (en) * 1987-08-04 1989-02-08 Nippon Steel Corp Metallizing of ceramic by alloy comprising noble metal as main component
CN103880478A (en) * 2012-12-21 2014-06-25 比亚迪股份有限公司 Ceramic surface selective metallization method and ceramic
CN106413270A (en) * 2016-11-04 2017-02-15 大连大学 Aluminum nitride ceramic circuit board and preparation method thereof
CN110240494A (en) * 2019-06-28 2019-09-17 大连大学 A kind of fiber reinforcement Cf/SiC composite plate weld connector
CN111269028A (en) * 2020-03-05 2020-06-12 哈尔滨工业大学(威海) Silicon nitride ceramic surface metallization method

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Application publication date: 20220325