CN115805236A - Process for preparing kovar alloy/AgCu alloy composite foil strip - Google Patents
Process for preparing kovar alloy/AgCu alloy composite foil strip Download PDFInfo
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- CN115805236A CN115805236A CN202310090424.0A CN202310090424A CN115805236A CN 115805236 A CN115805236 A CN 115805236A CN 202310090424 A CN202310090424 A CN 202310090424A CN 115805236 A CN115805236 A CN 115805236A
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Images
Abstract
The invention discloses a process for preparing a kovar alloy/AgCu alloy composite foil strip, which comprises the following steps: step one, preparing an AgCu alloy coating on the surface of a kovar alloy to obtain a primary composite foil strip plated with the AgCu alloy; and step two, performing rolling treatment on the primary composite foil strip plated with the AgCu alloy to obtain a kovar alloy/AgCu alloy foil strip. According to the method, the AgCu alloy metal layer is prepared on the surface of the kovar alloy by adopting a material increase process, then the compound rolling treatment is adopted to obtain the kovar alloy/AgCu alloy compound foil strip, the complex processes of a special expensive rolling mill required by the compound rolling process, annealing and the like are required for each pass, the AgCu alloy metal layer is directly deposited on the surface of the base strip close to the final thickness or the final thickness, and then the rolling is assisted to reach the roughness and the thickness required finally.
Description
Technical Field
The invention belongs to the technical field of electronic materials and composite materials, and particularly relates to a process for preparing a kovar alloy/AgCu alloy composite foil strip.
Background
With the rapid development of science and technology and the continuous pursuit of electronic product performance, electronic devices have increasingly prominent functions in the fields of electric power, communication and the like, sealing materials are required to be adopted during the production of the electronic devices, and people have more and more requirements on the sealing materials.
The sealing material used in electronic industry and electric vacuum industry mainly adopts sealing alloy, which is also called expansion alloy or kovar alloy, has constant low expansion coefficient, higher Curie point and good low-temperature structure stability in the temperature range of-70 ℃ to 500 ℃, is easy to weld and weld, has good plasticity, and is widely used for manufacturing electric vacuum elements, transmitting tubes, kinescopes, switch tubes, transistors, sealing plugs, relay shells and the like. The expansion coefficient of kovar alloy is close to that of the sealed materials such as glass or ceramic, so that the effect of matched sealing is achieved. The main types are Fe-Ni, fe-Ni-Co, fe-Ni-Cr and Fe-Ni-Cu alloys. And oxygen-free copper, tungsten, molybdenum, and alloys and composites thereof, commonly 4J29 and 4J50.
The kovar alloy has a disadvantage that its crystalline structure is easily transformed (osthole to martensite) during deformation processing to cause changes in properties such as increase in resistivity. Therefore, after such processing, kovar alloys must be annealed. Before sealing, the kovar alloy needs to be annealed in wet hydrogen at about 1000 ℃ to eliminate stress and decarbonize the surface, so that the kovar alloy can not generate air bubbles at the sealing position due to the oxidation of surface carbon to reduce the strength of the sealing position and cause chronic air leakage when sealing and heating are performed in the future. In addition, because of the high resistivity of kovar alloys, it is common to plate a layer of high conductivity material, such as gold, silver, copper, or make large area contacts to the surface of kovar alloys to form a composite material, if the cracking problem caused by overheating is considered. However, the conventional composite rolling preparation process adopted by the structure is complex, the annealing times are multiple, the difficulty is high, the process control is more complicated, the yield is low, and the cost and profit margin are gradually compressed.
Therefore, a new technical route and a composite process of the kovar alloy and the AgCu alloy are searched, and the method has important technical and economic significance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a process for preparing a kovar alloy/AgCu alloy composite foil strip aiming at the defects of the prior art. The AgCu alloy coating is prepared on the surface of the kovar alloy, the AgCu alloy coating and the kovar alloy form strong mechanical occlusion at an interface and even metallurgical bonding, then the AgCu alloy coating and the kovar alloy are fully combined into a whole through rolling treatment to form a kovar alloy/AgCu alloy foil strip, only a common rolling machine is needed to complete the final rolling action, a multi-pass heat treatment tempering treatment procedure is not needed, excessive energy consumption is reduced, and the process has the advantage of low cost.
In order to solve the technical problems, the invention adopts the technical scheme that: a process for preparing a kovar/AgCu alloy composite foil strip, characterized in that the process comprises the steps of:
step one, preparing an AgCu alloy coating on the surface of a kovar alloy to obtain a primary composite foil strip plated with the AgCu alloy; the kovar alloy is a foil or a strip;
and step two, performing rolling treatment on the AgCu alloy plated primary composite foil strip obtained in the step one to obtain a kovar alloy/AgCu alloy foil strip.
According to the method, the AgCu alloy coating is prepared on the surface of the kovar alloy, the AgCu alloy coating and the kovar alloy form strong mechanical occlusion at an interface and even metallurgical bonding, and then the AgCu alloy coating and the kovar alloy are fully bonded into a whole through rolling treatment to form the kovar alloy/AgCu alloy foil strip.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that the process for preparing the AgCu alloy coating in the step one is as follows: adopting one or more groups of spray heads to continuously spray the surface of the kovar alloy; the spraying is wire explosion, powder explosion, supersonic flame spraying, plasma spraying or spray welding. According to the method, one or more groups of spray heads are adopted to uniformly spray the AgCu alloy on the surface of the kovar alloy according to the width, the required composite thickness and the different spraying processes of the kovar alloy, the application range of the prepared AgCu alloy coating is wider by adopting the different spraying processes, the wire explosion and the powder explosion are two technical forms of electric explosion, and the wire and the powder are excited by high-voltage discharge to generate explosion particles which are deposited on the surface of a matrix.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that the process for preparing the AgCu alloy coating in the step one is as follows: continuously spray-welding island AgCu alloy coatings on the surfaces of the Kovar alloy foil strips by adopting one or more groups of spray nozzles, wherein the island AgCu alloy coatings have the diameter of between 20mm and 100mm and the height of between 0.05mm and 0.2mm, the edges of the adjacent island AgCu alloy coatings are overlapped and covered with each other, and the overlapping and covering area is 5-50% of the area of the island AgCu alloy coatings. The island-shaped AgCu alloy coating is continuously sprayed and welded on the surface of the kovar alloy in an array form by adopting one or more groups of spray heads, the edges of the adjacent island-shaped AgCu alloy coatings are overlapped and covered mutually, a uniform AgCu alloy coating is formed on the kovar alloy by matching with subsequent rolling treatment, the uneven problem caused by spraying is solved by island-shaped spraying and welding, the island-shaped AgCu alloy coating is leveled and homogenized by rolling treatment and reduced in roughness, and the island-shaped AgCu alloy coating can not generate obvious physical boundary in the subsequent rolling process and can be internally connected by mutual regionalized overlapping and covering.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that the process for preparing the AgCu alloy coating in the step one is as follows: and continuously spraying an AgCu alloy coating on the surface of the kovar alloy foil by adopting one or more groups of spray nozzles, wherein the thickness of the AgCu alloy coating is 0.05mm to 0.1mm, and the width of the AgCu alloy coating is 20mm to 300mm. The invention adopts one or more groups of spray heads to continuously spray and weld the laminar AgCu alloy coating on the surface of the kovar alloy, and forms a uniform AgCu alloy coating on the kovar alloy by matching with subsequent rolling treatment, so that the uneven problem caused by spraying is solved, and the alloy coating does not generate obvious physical boundary in the subsequent rolling process and can be internally connected by rolling treatment, leveling and homogenizing and reducing the roughness.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that in the first step, the kovar alloy is a 4J29 alloy or a 4J50 alloy. The invention is suitable for various kovar alloys, 4J29 alloy or 4J50 alloy, has constant low expansion coefficient, higher Curie point and good low-temperature structure stability in the temperature range of-70 to 500 ℃, is easy to weld and weld, has good plasticity, and is widely used for manufacturing electric vacuum elements, transmitting tubes, kinescopes, switch tubes, transistors, sealing plugs, relay shells and the like.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that in the first step, the AgCu alloy coating comprises AgCu8515 alloy, agCu28 alloy and AgCu50 alloy. According to the application, by controlling the components of the AgCu alloy coating, the adopted silver and copper belong to materials with high conductivity, the AgCu alloy has excellent conductivity, is compounded on Kovar alloy, is a product which is recognized in large scale in the electronic industry, also comprises alloy or ceramic materials which can be sprayed, and the AgCu alloy is widely used in the field of electronic materials as a conductive material due to good conductivity, thermal conductivity, arc burning resistance, fusion welding resistance, small electric wear and low and stable contact resistance.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that in the second step, the rolling treatment is one or more times of rolling treatment, and the pressing amount of each pass in the rolling treatment is 5% -50%. The Kovar alloy and the AgCu alloy are fully compounded by rolling treatment once or for multiple times and controlling the pressing amount, and the defects and the destressing of the two materials are considered in each pressing process, so that the primary composite foil strip plated with the AgCu alloy achieves the required thickness and roughness.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that in the second step, the AgCu alloy plated primary composite foil strip is subjected to primary annealing after being subjected to rolling treatment, wherein the annealing temperature is 200-600 ℃, and the annealing time is 60min-300min. The kovar alloy has the defects that the crystal structure of the kovar alloy is easy to change during deformation processing, and the osthol is converted into the martin to change the performance, such as the resistivity is increased, so the kovar alloy needs to be annealed after the processing, the traditional composite rolling method is completely compounded by two materials through rolling action, the extension coefficients are inconsistent, the interfaces of the materials cannot be really occluded, the defects at the interfaces are accumulated, and the stress accumulation exists in the two materials.
The process for preparing the kovar alloy/AgCu alloy composite foil strip is characterized in that in the second step, the thickness of the kovar alloy/AgCu alloy foil strip is 20-300 mu m, the roughness Ra is not more than 0.1 mu m, the lateral bending is not more than 3mm/m, the thickness range of the AgCu alloy layer is less than 0.003mm, the hardness of the kovar alloy surface is 250HV to 280HV, and the hardness of the AgCu alloy surface is not less than 140HV. The kovar alloy/AgCu alloy foil strip prepared by the invention has excellent mechanical properties.
Compared with the prior art, the invention has the following advantages:
1. according to the method, the AgCu alloy coating is prepared on the surface of the kovar alloy, the AgCu alloy coating and the kovar alloy form strong mechanical occlusion at an interface, even metallurgical bonding, and then the AgCu alloy coating and the kovar alloy are fully combined into a whole through rolling treatment to form the kovar alloy/AgCu alloy foil strip.
2. The island-shaped AgCu alloy coating is continuously sprayed and welded on the surface of the kovar alloy in an array form by adopting one or more groups of spray heads, the edges of the adjacent island-shaped AgCu alloy coatings are overlapped and covered with each other, a uniform AgCu alloy coating is formed on the kovar alloy by matching with subsequent rolling treatment, the uneven problem caused by spraying is solved by island-shaped spraying and welding, the island-shaped alloy coating is leveled and homogenized by rolling treatment and reduced in roughness, and the island-shaped alloy coating does not generate obvious physical boundary in the subsequent rolling process and can be internally connected by mutual regionalized overlapping and covering.
3. The method can obtain the thickness and the roughness required by the final product only by adopting the kovar alloy foil strip with the thickness close to the thickness of the final product, avoids the defects that the traditional composite rolling means needs special equipment of a composite rolling mill, the equipment is expensive to purchase, does not need to introduce a harsh heat treatment system required by different passes, needs few steps and generates few defective products, and has the advantage of simple operation.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic view showing the structure of a spray welding and rolling process performed in example 1 of the present invention.
FIG. 2 is a cross-sectional view of a kovar/AgCu alloy strip made in example 1 of the present invention.
Description of reference numerals:
| 1-a spray head; | 2-4J 29 kovar alloy strip; | 3-island AgCu50 alloy coating; |
| 4-primary composite tape; | 5-AgCu 50 alloy wire; | and 6, rolling. |
Detailed Description
Example 1
The embodiment comprises the following steps:
firstly, three groups of spray heads 1 are adopted to continuously spray-weld the island-shaped AgCu50 alloy coating 3 on the surface of a 4J29 kovar alloy strip 2 with the thickness of 300 mu m and the width of 200mm to obtain a primary composite strip 4 plated with AgCu alloy; the island-shaped AgCu alloy coating 3 is 60mm in diameter and 0.05mm in height, the edges of the adjacent island-shaped AgCu alloy coatings 3 are overlapped and covered with each other, and the overlapping and covering area is 30% of that of the island-shaped AgCu alloy coating; the AgCu50 alloy coating 3 adopts an AgCu50 alloy wire 5 with the wire diameter of 0.5mm, as shown in figure 1;
step two, carrying out three times of rolling treatment on the AgCu alloy plated primary composite belt 4 obtained in the step one, and then carrying out primary annealing to obtain a kovar alloy/AgCu alloy belt material; the rolling amount of each pass in the rolling treatment is 33%, the roughness Ra of the roller 6 adopted in the rolling treatment is less than or equal to 0.1mm, and the graph is shown in figure 1.
Through detection, the thickness of the kovar alloy/AgCu alloy strip prepared in the embodiment is 150 μm, wherein the thickness of the kovar alloy layer is 120 μm, the thickness of the AgCu50 alloy coating is 30 μm, the roughness is Ra0.1 μm, the lateral bending is 3mm/m, the thickness range of the AgCu alloy layer is 0.003mm, the hardness of the kovar alloy surface is 260HV, and the hardness of the AgCu alloy surface is 140HV.
Fig. 2 is a cross-sectional view of the kovar alloy/AgCu alloy strip prepared in this embodiment, and it can be seen from fig. 2 that the kovar alloy/AgCu alloy strip prepared in this embodiment has good flatness and a smooth surface, the thickness of the kovar alloy substrate at the bottom and the thickness of the AgCu alloy at the surface layer meet the product requirements, and an effective bonding area is generated at the interface.
Example 2
The present embodiment is different from embodiment 1 in that: in the step one, the overlapped area is 5% of the island-shaped area, the diameter of the island-shaped AgCu alloy coating is 20mm, the height of the island-shaped AgCu alloy coating is 0.1mm, and the pressing amount of each pass in the step two is 5%.
Example 3
The present embodiment is different from embodiment 1 in that: the overlapping area in the first step is 50% of the island-shaped area, the diameter of the island-shaped AgCu alloy coating is 100mm, the height of the island-shaped AgCu alloy coating is 0.08mm, and the pressing amount of each pass in the second step is 50%.
Example 4
The embodiment comprises the following steps:
step one, adopting three groups of spray heads to continuously spray AgCu8515 alloy coatings on the surfaces of 4J50 kovar alloy strips with the thickness of 200 mu m and the width of 300mm through supersonic flame to obtain AgCu alloy plated primary composite foil strips; the thickness of the AgCu alloy coating is 0.1mm, and the width of the AgCu alloy coating is 100mm; the AgCu50 alloy coating adopts AgCu8515 alloy wire with the wire diameter of 1 mm;
step two, carrying out three times of rolling treatment on the primary composite foil strip plated with the AgCu alloy obtained in the step one, and then carrying out primary annealing to obtain a kovar alloy/AgCu alloy foil strip; the rolling amount of each pass in the rolling treatment is 40%, and the roughness Ra of the roller adopted in the rolling treatment is less than or equal to 0.1mm.
According to detection, the thickness of the kovar alloy/AgCu alloy foil strip prepared in the embodiment is 100 μm, wherein the thickness of the kovar alloy layer is 80 μm, the thickness of the AgCu50 alloy coating is 20 μm, the roughness is Ra0.08 μm, the lateral bending is 2.5mm/m, the thickness of the AgCu alloy layer is extremely different by 0.002mm, the hardness of the kovar alloy surface is 280HV, and the hardness of the AgCu alloy surface is 150HV.
Example 5
The embodiment comprises the following steps:
step one, adopting a group of spray heads to perform continuous plasma spraying of an AgCu28 alloy coating on the surface of a 4J29 kovar alloy strip with the thickness of 180 mu m and the width of 100mm to obtain a primary composite foil strip plated with the AgCu alloy; the thickness of the AgCu alloy coating is 0.08mm, and the width of the AgCu alloy coating is 50mm; the AgCu28 alloy coating adopts AgCu28 alloy wires with the wire diameter of 1 mm;
step two, carrying out three times of rolling treatment on the primary composite foil strip plated with the AgCu alloy obtained in the step one, and then carrying out primary annealing to obtain a kovar alloy/AgCu alloy foil strip; the rolling reduction of the first pass in the rolling treatment is 16.7%, the rolling reduction of the second pass is 12.1%, the rolling reduction of the third pass is 12.1%, and the roughness Ra of the roller adopted in the rolling treatment is less than or equal to 0.1mm.
According to detection, the thickness of the kovar alloy/AgCu alloy foil strip prepared in the embodiment is 150 μm, wherein the thickness of the kovar alloy layer is 120 μm, the thickness of the AgCu50 alloy coating is 30 μm, the roughness is Ra0.09 μm, the lateral bending is 2.0mm/m, the thickness range of the AgCu alloy layer is 0.001mm, the hardness of the kovar alloy surface is 250, and the hardness of the AgCu alloy surface is 155HV.
Example 6
The present embodiment is different from embodiment 5 in that: and in the first step, continuous wire explosion spraying of the AgCu50 alloy coating is carried out on the surface of the 4J29 kovar alloy strip, the thickness of the AgCu alloy coating is 0.05mm, and the width of the AgCu alloy coating is 300mm.
Example 7
This embodiment is different from embodiment 5 in that: in the first step, the AgCu50 alloy coating is continuously sprayed on the surface of the 4J29 kovar alloy strip through powder explosion, the thickness of the AgCu alloy coating is 0.08mm, and the width of the AgCu alloy coating is 20mm.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (9)
1. A process for preparing a kovar/AgCu alloy composite foil strip, characterized in that the process comprises the steps of:
step one, preparing an AgCu alloy coating on the surface of a kovar alloy to obtain a primary composite foil strip plated with the AgCu alloy; the kovar alloy is a foil or a strip;
and step two, performing rolling treatment on the AgCu alloy plated primary composite foil strip obtained in the step one to obtain a kovar alloy/AgCu alloy foil strip.
2. The process for preparing a kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein the process for preparing the AgCu alloy coating in the step one is as follows: adopting one or more groups of spray heads to continuously spray the surface of the kovar alloy; the spraying is wire explosion, powder explosion, supersonic flame spraying, plasma spraying or spray welding.
3. The process for preparing a kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein the process for preparing the AgCu alloy coating in the step one is as follows: the method comprises the steps of continuously spray-welding island-shaped AgCu alloy coatings on the surfaces of Kovar alloy foil strips by adopting one or more groups of spray nozzles, wherein the island-shaped AgCu alloy coatings are from 20mm to 100mm in diameter and from 0.05mm to 0.2mm in height, the edges of the adjacent island-shaped AgCu alloy coatings are overlapped and covered with each other, and the overlapping and covering area is 5% -50% of the area of the island-shaped AgCu alloy coatings.
4. The process for preparing a kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein the process for preparing the AgCu alloy coating in the step one is as follows: and continuously spraying an AgCu alloy coating on the surface of the kovar alloy foil by adopting one or more groups of spray nozzles, wherein the thickness of the AgCu alloy coating is 0.05mm to 0.1mm, and the width of the AgCu alloy coating is 20mm to 300mm.
5. The process for preparing the kovar alloy/AgCu alloy composite foil strip according to claim 1, wherein in the first step, the kovar alloy is 4J29 alloy or 4J50 alloy.
6. The process for preparing the kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein the AgCu alloy coating in the step one comprises AgCu8515 alloy, agCu28 alloy and AgCu50 alloy.
7. The process for preparing the kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein the rolling treatment in the second step is one or more rolling treatments, and the pressing amount in each pass of the rolling treatment is 5% -50%.
8. The process for preparing the kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein in step two, the AgCu alloy coated primary composite foil strip is subjected to primary annealing after being subjected to calendaring treatment, and the annealing temperature is 200-600 ℃ and the annealing time is 60min-300min.
9. The process for preparing the kovar alloy/AgCu alloy composite foil strip as claimed in claim 1, wherein the thickness of the kovar alloy/AgCu alloy foil strip in the second step is 20 μm to 300 μm, the roughness Ra is not more than 0.1 μm, the lateral bending is not more than 3mm/m, the thickness range of the AgCu alloy layer is less than 0.003mm, the hardness of the kovar alloy surface is 250HV to 280HV, and the hardness of the AgCu alloy surface is not less than 140HV.
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| GB1224213A (en) * | 1967-04-28 | 1971-03-03 | Cockerill | Process for the continuous production of coated metal strips |
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