CN106892685B - Ceramic metallized film and preparation method thereof - Google Patents

Ceramic metallized film and preparation method thereof Download PDF

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CN106892685B
CN106892685B CN201510958543.9A CN201510958543A CN106892685B CN 106892685 B CN106892685 B CN 106892685B CN 201510958543 A CN201510958543 A CN 201510958543A CN 106892685 B CN106892685 B CN 106892685B
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ceramic
metal
film
transition layer
composite transition
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CN106892685A (en
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李帅
吕琴丽
何迪
张超
张华�
刘晓鹏
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GRIMN Engineering Technology Research Institute Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Abstract

The invention discloses a ceramic metalized film and a preparation method thereof. The ceramic metallized film is composed of a ceramic metal composite transition layer, a first metal film and a second metal film which are sequentially applied on a ceramic substrate, wherein the ceramic metal composite transition layer is formed by compounding a first metal and a component which is the same as that of the ceramic substrate, and the proportion of the first metal in the ceramic metal composite transition layer is 20-80 at%; the ceramic matrix is made of Al2O3、ZrO2、AlN、BN、SiC、Si3N4One of the above; the first metal is one of Nb, Ti, Cr, Zr, V and Ta; the second metal is one or a mixture of more of Ni, Mo, Au, Cu, Pt and W. The preparation method comprises the following steps: (1) depositing a ceramic metal composite transition layer on the ceramic substrate by a sputtering coating method; (2) and sequentially depositing a first metal film and a second metal film on the ceramic-metal composite transition layer by a sputtering coating method. The ceramic metalized film has the advantages of accurate control of ceramic size and high tensile strength.

Description

Ceramic metallized film and preparation method thereof
Technical Field
The invention relates to a ceramic metalized film and a preparation method thereof, belonging to the technical field of ceramic metalized application.
Background
The ceramic has excellent high temperature resistance, corrosion resistance, abrasion resistance, radiation resistance, high-frequency and high-voltage insulation resistance and other properties, and is widely applied to modern industries such as electronics, nuclear energy, information and the like. The connection of ceramics and the connection of ceramics and metal can more effectively and fully play the respective special properties of the materials, and the ceramic connection technology occupies an important position in the application of ceramics.
The ceramic brazing connection process requires metallization of the ceramic surface to improve the wetting of the ceramic surface to the solder. The traditional ceramic metallization mostly adopts a sintered metal powder method, and refractory metal powder (such as W, Mo) is mixed with a small amount of low-melting-point metal powder (such as Fe, Mn and Ti) and coated on the surface of the ceramic to be sintered at high temperature. The method has high sintering temperature, high cost and large thickness (20-60 mu m) of the metallization layer, and is not beneficial to the precise control of the size of the ceramic piece.
Disclosure of Invention
The invention aims to provide a ceramic metalized film, wherein a metalized layer of the ceramic metalized film has high tensile strength and accurate size control.
The invention also aims to provide a preparation method of the ceramic-containing metallized film.
In order to achieve the purpose, the invention adopts the following technical scheme:
a ceramic metallized film is composed of a ceramic metal composite transition layer, a first metal film and a second metal film which are sequentially applied on a ceramic substrate, wherein the ceramic metal composite transition layer is formed by compounding a first metal and a component which is the same as that of the ceramic substrate; the ceramic matrix is made of Al2O3、ZrO2、AlN、BN、SiC、Si3N4One of the above; the first metal is one of Nb, Ti, Cr, Zr, V and Ta; the second metal is one or a mixture of more of Ni, Mo, Au, Cu, Pt and W.
Wherein the thickness of the ceramic-metal composite transition layer is 20-200nm, and the proportion of the first metal in the ceramic-metal composite transition layer is 20-80 at%. The thickness of the first metal film is 20-200 nm; the thickness of the second metal film is 1-10 μm.
A preparation method of the ceramic metalized film comprises the following steps:
(1) depositing a ceramic metal composite transition layer on the ceramic substrate by a sputtering coating method;
(2) and sequentially depositing a first metal film and a second metal film on the ceramic-metal composite transition layer by a sputtering coating method.
The preparation of the ceramic-metal composite transition layer adopts a codeposition sputtering coating method, adopts a metal target and a ceramic target, and realizes the content adjustment of metal components and ceramic components in the transition layer by adjusting sputtering power.
The invention has the advantages that:
the invention adopts the film metallization method to prepare the ceramic metallized film through the gas phase process, and the ceramic dimension control is accurate. The adopted ceramic-metal composite transition layer can effectively reduce the mismatch of the thermal expansion coefficients of the metal film and the ceramic substrate, and the tensile strength of the film metallization layer is obviously improved compared with that of a sintered metal powder method.
Drawings
FIG. 1 is a schematic structural view of a ceramic metallized film according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the embodiments of the invention are not limited thereto.
As shown in fig. 1, the ceramic metallized film of the present invention is composed of a ceramic metal composite transition layer 2, a first metal thin film 3, and a second metal thin film 4, which are sequentially applied on a ceramic base 1.
Example 1
1)Al2O3Cleaning a substrate with acetone and alcohol, and preparing Ti/Al by adopting a magnetron co-sputtering method2O3And a transition layer. Using a metallic Ti target and ceramic Al2O3The vacuum of the back bottom of the target and the vacuum cavity is better than 2.0 multiplied by 10-3pa, Ti target power 60W, Al2O3The target power was 100W, the working gas pressure was 1.5Pa, and the deposition time was 90 minutes. The thickness of the transition layer was 150nm and the Ti content was 45 at%.
2) In the presence of Ti/Al2O3Preparing Ti layer on the transition layer by magnetron sputtering method, using metal Ti target and vacuum cavityVacuum of back of body is better than 2.0X 10-3Pa, Ti target power of 100W, working gas pressure of 1.5Pa, deposition time of 30 minutes. The thickness of the Ti film is 100 nm.
3) Preparing a Ni layer on the Ti layer by a magnetron sputtering method, adopting a metal Ni target, and ensuring that the vacuum of the back bottom of a vacuum cavity is better than 2.0 multiplied by 10-3Pa, Ni target power 150W, deposition time 350 minutes, working pressure 2.0 Pa. The Ni film thickness was 3.5. mu.m.
The alumina standard ceramic part using the metallized film was subjected to a tensile strength test (SJT3326-2001), and the average tensile strength was 134 MPa.
The tensile strength obtained by the common metal powder method is about 80MPa, and the highest tensile strength is about 100 MPa.
Example 2
1)Al2O3Cleaning a substrate with acetone and alcohol, and preparing Ti/Al by adopting a magnetron co-sputtering method2O3And a transition layer. Using a metallic Ti target and ceramic Al2O3The vacuum of the back bottom of the target and the vacuum cavity is better than 2.0 multiplied by 10-3Pa, Ti target power of 80W, Al2O3The target power was 100W, the working gas pressure was 1.5Pa, and the deposition time was 80 minutes. The thickness of the transition layer was 130nm and the Ti content was 75 at%.
2) In the presence of Ti/Al2O3The Ti layer is prepared on the transition layer by a magnetron sputtering method, a metal Ti target is adopted, and the vacuum of the back bottom of the vacuum cavity is superior to 2.0 multiplied by 10-3Pa, Ti target power of 100W, working gas pressure of 1.5Pa, deposition time of 30 minutes. The thickness of the Ti film is 100 nm.
3) The Ni/Mo layer is prepared on the Ti layer by a magnetron sputtering method, a Ni/Mo alloy target is adopted, and the vacuum of the back bottom of the vacuum cavity is superior to 2.0 multiplied by 10-3Pa, Ni/Mo alloy target power 150W, deposition time 350 minutes, working gas pressure 2.0 Pa. The thickness of the Ni/Mo film was 3.5. mu.m.
The alumina standard ceramic part using the metallized film was subjected to a tensile strength test (SJT3326-2001), and the average tensile strength was 130 MPa.
The tensile strength obtained by the common metal powder method is about 80MPa, and the highest tensile strength is about 100 MPa.
Example 3
1) And cleaning the SiC matrix by acetone and alcohol, and preparing the Nb/SiC transition layer by adopting a magnetron co-sputtering method. The metal Nb target and the ceramic SiC target are adopted, and the vacuum of the back bottom of the vacuum cavity is better than 2.0 multiplied by 10-3Pa, Nb target power of 50W, SiC target power of 100W, working gas pressure of 1.5Pa, deposition time of 70 minutes. The thickness of the transition layer was 120nm and the Nb content was 25 at%.
2) The Nb layer is prepared on the Nb/SiC transition layer by a magnetron sputtering method, a metal Nb target is adopted, and the vacuum of the back bottom of a vacuum cavity is superior to 2.0 multiplied by 10-3Pa, Nb target power of 100W, working gas pressure of 1.5Pa, deposition time of 24 minutes. The thickness of the Nb film is 80 nm.
3) The Ni/Mo layer is prepared on the Nb layer by a magnetron sputtering method, a Ni/Mo alloy target is adopted, and the vacuum of the back bottom of a vacuum cavity is superior to 2.0 multiplied by 10-3Pa, Ni/Mo alloy target power 150W, working gas pressure 2.0Pa, deposition time 300 minutes. The thickness of the Ni/Mo film was 3 μm.
The silicon carbide standard ceramic part using the metallized film was subjected to a tensile strength test (SJT3326-2001), and the average tensile strength was 145 MPa.
The tensile strength obtained by the common metal powder method is about 80MPa, and the highest tensile strength is about 100 MPa.

Claims (7)

1. A ceramic metallized film is characterized by comprising a ceramic metal composite transition layer, a first metal film and a second metal film which are sequentially applied on a ceramic substrate, wherein the ceramic metal composite transition layer is formed by compounding a first metal and a component which is the same as that of the ceramic substrate by a codeposition sputtering coating method; the ceramic matrix is made of Al2O3、ZrO2、BN、SiC、Si3N4One of the above; the first metal is one of Nb, Cr, Zr, V and Ta; the second metal is one or a mixture of more of Ni, Mo, Au, Cu, Pt and W.
2. The ceramic metallized film of claim 1, wherein the ceramic metal composite transition layer has a thickness of 20-200 nm.
3. The ceramic-metallized film of claim 1, wherein the first metal is present in the ceramic-metal composite transition layer at a concentration of 20 to 80 at%.
4. The ceramic metallized film of claim 1, wherein the first metal film has a thickness of 20-200 nm.
5. The ceramic metallized film of claim 1, wherein the thickness of said second metal film is 1-10 μm.
6. A method of making a ceramic metallized film according to any one of claims 1 to 5, comprising the steps of:
(1) depositing a ceramic metal composite transition layer on the ceramic substrate by a sputtering coating method;
(2) and sequentially depositing a first metal film and a second metal film on the ceramic-metal composite transition layer by a sputtering coating method.
7. The method for preparing a ceramic metallized film according to claim 6, wherein the ceramic metal composite transition layer is prepared by a co-deposition sputtering coating method, and the content adjustment of the metal component and the ceramic component in the transition layer is realized by adjusting the sputtering power by using a metal target and a ceramic target.
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CN109136848B (en) * 2018-07-17 2020-04-28 西安交通大学 Method for connecting aluminum nitride ceramic plate and metal based on PVD (physical vapor deposition) deposition method
CN110370754B (en) * 2019-06-28 2022-01-04 厦门理工学院 High-damage-tolerance ceramic-metal composite material and preparation method thereof
CN112479733B (en) * 2020-11-25 2022-02-11 西安交通大学 Surface modification method of ceramic bonding area suitable for ceramic/metal connection
CN112975032B (en) * 2021-02-23 2022-09-27 浙江浙能兰溪发电有限责任公司 Brazing method of silicon carbide ceramic
CN113716978A (en) * 2021-07-29 2021-11-30 富士新材(深圳)有限公司 Metallized ceramic plate and preparation method thereof
CN113560110B (en) * 2021-08-04 2023-04-14 湖南省美程陶瓷科技有限公司 Ceramic-metal composite atomizing sheet and preparation method thereof
CN114000112B (en) * 2021-10-21 2024-03-22 苏州玖凌光宇科技有限公司 Aluminum nitride copper-clad AMB method
CN114702335B (en) * 2022-04-22 2022-12-13 湖南省新化县鑫星电子陶瓷有限责任公司 Metallization process of alumina ceramic
CN115124374A (en) * 2022-06-15 2022-09-30 深圳元点真空装备有限公司 Technology for coating thick metal layer on SBC ceramic surface and ceramic packaging substrate thereof

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