CN113927970A - Silver/molybdenum/silver metal-based layered composite material and preparation process thereof - Google Patents
Silver/molybdenum/silver metal-based layered composite material and preparation process thereof Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 119
- 239000004332 silver Substances 0.000 title claims abstract description 119
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 88
- 239000011733 molybdenum Substances 0.000 title claims abstract description 88
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005096 rolling process Methods 0.000 claims abstract description 38
- 238000009792 diffusion process Methods 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000005498 polishing Methods 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000003723 Smelting Methods 0.000 claims description 15
- 238000004381 surface treatment Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 14
- 238000010008 shearing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000005554 pickling Methods 0.000 claims description 10
- 238000005098 hot rolling Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000003490 calendering Methods 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 description 15
- 238000013329 compounding Methods 0.000 description 11
- 238000007602 hot air drying Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000007547 defect Effects 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 229940100890 silver compound Drugs 0.000 description 3
- 150000003379 silver compounds Chemical class 0.000 description 3
- 238000009966 trimming Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
- B21B2001/386—Plates
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/202—Conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B2307/00—Properties of the layers or laminate
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Abstract
The invention discloses a silver/molybdenum/silver metal-based layered composite material and a preparation process, wherein the composite material is of a three-layer layered structure, the total width is 25mm-95mm, the total thickness is 27 mu m-57 mu m, the first layer and the third layer are both silver layers, the thickness is 6 mu m, the oxygen content is lower than 50ppm, the second layer is a molybdenum layer, and the thickness is 15 mu m-45 mu m; the preparation process adopts a different-temperature rolling composite mode and adopts high-temperature diffusion at 900-950 ℃. The composite material prepared by the invention belongs to a metallurgically bonded layered composite material, has the advantages of excellent heat resistance, high-temperature mechanical property and stable expansion coefficient of molybdenum, fully exerts the conductive property and atmospheric corrosion resistance of silver, and can greatly improve the reliability of high-low temperature impact application occasions in the field of electronic and electric appliances, thereby greatly improving the service life of electronic components.
Description
Technical Field
The invention relates to a metal-based layered composite material and a preparation process thereof, in particular to a silver/molybdenum/silver metal-based layered composite material and a preparation process thereof in high-low temperature impact application occasions in the field of electronic and electric appliances.
Background
Pure silver foil is widely used in electronic and electric products because of its good conductivity and resistance to atmospheric pollution. However, in some special electronic and electrical fields, thermal shock is caused by severe temperature change, and the pure silver material is soft and low in strength, so that fracture and failure are easy to occur. Molybdenum has excellent heat resistance, high-temperature mechanical properties and stable expansion coefficient, so that molybdenum is introduced into related industries and applied, but molybdenum has the characteristics of poor conductivity and poor atmospheric pollution resistance. In order to solve the problems of molybdenum, silver-plated molybdenum foils are generally adopted in the industry to solve the problems, but due to the adoption of an electroplating chemical deposition mode, the adhesion strength is not high, the thickness of an electroplated layer is relatively thin (the thickness of the electroplated layer is usually between 1 mu and 2 mu), and under the action of thermal stress, the silver layer on the surface of an electroplated material is easy to corrode and fall off to lose efficacy.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silver/molybdenum/silver metal-based layered composite material and a preparation process thereof, the composite material is produced by heating, rolling and compounding and is subjected to high-temperature diffusion, in the high-temperature diffusion, because the oxygen content is controlled within 50ppm, no bubbling can occur on an interface, and the silver and the molybdenum are completely metallurgically bonded, so that the silver and the molybdenum cannot fall off in high and low temperature environments, and the reliability and the service life of electronic components are greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the silver/molybdenum/silver metal-based layered composite material is a three-layer layered structure, the total width is 25mm-95mm, the total thickness is 27 mu m-57 mu m, the first layer and the third layer are both silver layers, the thickness is 6 mu m, the oxygen content is lower than 50ppm, the second layer is a molybdenum layer, and the thickness is 15 mu m-45 mu m.
A preparation process of a silver/molybdenum/silver metal-based layered composite material comprises the following steps:
firstly, smelting a pure silver plate with the purity of more than 99.99 percent into a silver plate with the oxygen content of less than 50ppm in a multiple vacuum smelting mode, and then processing the silver plate into a silver strip with the thickness of 0.6mm and the width of 30mm-100mm for later use through calendaring, annealing, surface treatment and shearing;
step two, dividing the silver belt for standby in the step one into two halves, respectively carrying out acid pickling and polishing, simultaneously carrying out acid pickling and polishing on the molybdenum belt with the thickness of 1.5-4.5 mm and the width of 30-100 mm, and then carrying out continuous different temperature rolling by adopting a different temperature rolling composite process, wherein the molybdenum belt is arranged on the second layer, the silver belt is arranged on the first layer and the third layer, the temperature of the silver belt is controlled between 100 ℃ and 200 ℃, the temperature of the molybdenum belt is controlled between 1000 ℃ and 1200 ℃, the deformation of the different temperature rolling is not less than 50%, and a silver/molybdenum/silver composite blank with the thickness of 1.0-2.35 mm and the width of 30-100 mm is formed after the composite;
step three, carrying out continuous diffusion heat treatment on the silver/molybdenum/silver composite blank obtained in the step two, wherein the temperature of the diffusion heat treatment is controlled to be 900-950 ℃, and the time of the diffusion heat treatment is not less than 3 minutes;
cutting the silver/molybdenum/silver composite blank subjected to diffusion heat treatment in the third step into a blank with the width of 27mm-97mm, and performing repeated hot rolling, surface treatment and continuous heat treatment after acid cleaning and polishing to obtain a finished coil stock with the total thickness of 27 mu m-57 mu m, wherein the thickness of the silver layers of the first layer and the third layer is 6 mu m, and the thickness of the molybdenum layer of the second layer is 15 mu m-45 mu m;
and step five, cutting the silver/molybdenum/silver composite finished coil stock with the total thickness of 27-57 microns and the total width of 27-97 mm obtained in the step four into a coil stock with the total width of 25-95 mm, and obtaining the composite material.
Further, the smelting vacuum degree in the step one is not less than 10-2Pa, smelting times is not less than two times.
Furthermore, the different-temperature rolling composite process in the step two adopts four-roller rolling, more than three continuous unreeling is adopted, and each coiled strip material adopts independent resistance heating equipment and an independent temperature control device to control the temperature.
Further, the heat treatment in the third step adopts nitrogen and ammonia decomposition gas for protection, so as to prevent silver from absorbing oxygen.
Further, acid cleaning in the second step and the fourth step adopts 10-20% dilute sulfuric acid for cleaning, and felt grinding is adopted for polishing.
Further, the surface treatment in the fourth step is grinding treatment, and the grinding medium is felt grinding.
Further, the hot rolling in the fourth step is performed by using a multi-roll mill having four or more rolls.
Has the advantages that:
1. according to the silver/molybdenum/silver metal-based layered composite material prepared by the invention, because the composite material is subjected to hot rolling compounding and high-temperature diffusion, and the composite material belongs to a layered composite material which is completely metallurgically combined, the composite material has extremely good heat resistance, high-temperature mechanical property and stable expansion coefficient of molybdenum, and simultaneously fully exerts the conductive performance and atmospheric corrosion resistance of silver; in the invention, because the silver is repeatedly vacuum-smelted, the oxygen content of the silver is controlled below 50ppm, and the silver is treated at a high temperature of 900-950 ℃, the interface of the silver and the molybdenum can not bubble in the high-temperature process, and the reliability of the composite material under high-low temperature thermal shock is also ensured.
2. The silver/molybdenum/silver metal-based layered composite material prepared by the invention adopts a different-temperature rolling composite process, because the silver and molybdenum have large recrystallization temperature difference and large deformation resistance difference, the silver and molybdenum are controlled by different temperatures, and meanwhile, the deformation is controlled to be more than 50 percent, the silver and molybdenum interface can form interatomic combination, and the interface can form a diffusion layer between the silver and the molybdenum through high-temperature diffusion subsequently, thereby ensuring the reliability of the composite material; the speed ratio between the silver and the molybdenum can be accurately controlled by adopting the different-temperature rolling composite process, so that the thickness ratio between the silver/the molybdenum/the silver is stable.
3. The invention uses traditional metallurgical equipment, can realize continuous batch production, and has the characteristics of low cost, convenient production and the like.
Drawings
FIG. 1 is a schematic structural view of a silver/molybdenum/silver metal-based layered composite material of the present invention;
in the figure: 1-silver layer and 2-molybdenum layer.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1
The invention provides a silver/molybdenum/silver metal-based layered composite material, as shown in figure 1, the composite material is of a three-layer layered structure, the total width is 25mm, the total thickness is 27 mu m, wherein the first layer and the third layer are both silver layers 1, the thickness is 6 mu m, the oxygen content is lower than 50ppm, the second layer is a molybdenum layer 2, and the thickness is 15 mu m.
The invention also provides a preparation process of the silver/molybdenum/silver metal-based layered composite material, which comprises the following steps:
step one, melting a pure silver plate with the purity of more than 99.99 percent into a silver plate with the oxygen content of less than 50ppm by two vacuum melting modes, and performing vacuum meltingThe vacuum degree of the smelting equipment in the smelting process is not less than 10-2Pa. The silver plate is processed into a silver belt with the thickness of 0.6mm and the width of 30mm for standby through surface treatment, calendaring processing, annealing and shearing. The rolling processing adopts a common two-roller mill or four-roller mill for rolling, the annealing is mainly softening annealing, the annealing temperature is 300 ℃, the surface treatment is mainly to eliminate the defects of smelting of the silver surface and processing in the process, the processing is usually carried out by adopting a planing or milling mode, and the shearing is carried out by adopting longitudinal shearing equipment for shearing and removing burrs;
and step two, dividing the silver belt reserved in the step one into two parts, respectively carrying out acid cleaning and polishing, and simultaneously carrying out acid cleaning and polishing on the molybdenum belt with the thickness of 1.5mm and the width of 30mm in a continuous roll-to-roll mode, wherein 10% -20% of dilute sulfuric acid is adopted for acid cleaning, felt grinding is adopted for polishing, and hot air drying is adopted for water washing. The material is continuously rolled and compounded by adopting different-temperature rolling compound equipment, the different-temperature rolling compound equipment is roll-to-roll continuous compound equipment and is provided with more than three continuous unreels, a molybdenum strip is coiled in the middle, a silver strip is respectively unreeled upwards and unreeled downwards, each strip is controlled in temperature by adopting independent resistance heating and an independent temperature control device, and four-roller rolling compound is adopted for rolling and compounding. During compounding, the temperature of the silver strip is controlled between 100 ℃ and 120 ℃, the temperature of the molybdenum strip is controlled between 1000 ℃ and 1100 ℃, the rolling compound deformation is not less than 50 percent, and the silver/molybdenum/silver compound blank with the thickness of 1.0mm and the width of 30mm is formed after compounding;
step three, carrying out continuous diffusion heat treatment on the silver/molybdenum/silver composite blank obtained in the step two, wherein the diffusion heat treatment temperature is 900-950 ℃, the diffusion heat treatment time is 3.5 minutes, and in order to prevent silver from absorbing oxygen, the continuous heat treatment needs to be protected by nitrogen and ammonia decomposition gas;
step four, trimming the silver/molybdenum/silver composite blank subjected to diffusion heat treatment in the step three into a blank with the width of 27mm, pickling and polishing, wherein the pickling and polishing are carried out in a continuous roll-to-roll mode, 10% -20% of dilute sulfuric acid is used for cleaning, felt grinding is used for polishing, and hot air drying is used for water washing. Then, obtaining a finished coil stock with the total thickness of 27 mu m by hot rolling, surface treatment and continuous heat treatment of four-roller or more rolling mills, wherein the thickness of the silver layers on the two sides is 6 mu m, and the thickness of the molybdenum layer in the middle is 15 mu m;
and step five, cutting the silver/molybdenum/silver composite finished coil stock with the total thickness of 27 microns and the width of 27mmm in the step four into a coil stock with the width of 25mm by using a continuous slitting machine to obtain the composite material.
Example 2
The invention provides a silver/molybdenum/silver metal-based layered composite material, as shown in figure 1, the composite material is of a three-layer layered structure, the total width is 75mm, the total thickness is 42 mu m, wherein the first layer and the third layer are both silver layers 1, the thickness is 6 mu m, the oxygen content is lower than 50ppm, the second layer is a molybdenum layer 2, and the thickness is 30 mu m.
The invention also provides a preparation process of the silver/molybdenum/silver metal-based layered composite material, which comprises the following steps:
step one, melting a pure silver plate with the purity of more than 99.99% into a silver plate with the oxygen content of less than 50ppm by a three-time vacuum melting mode, wherein the vacuum degree of melting equipment in the vacuum melting process is not less than 10-2Pa. The silver plate is processed into a silver belt with the thickness of 0.6mm and the width of 80mm for standby through surface treatment, calendaring processing, annealing and shearing. The rolling processing adopts a common two-roller mill or four-roller mill for rolling, the annealing is mainly softening annealing, the annealing temperature is 350 ℃, the surface treatment is mainly to eliminate the defects of smelting of the silver surface and processing in the process, the processing is usually carried out by adopting a planing or milling mode, and the shearing is carried out by adopting longitudinal shearing equipment for shearing and removing burrs;
and step two, dividing the silver belt reserved in the step one into two parts, respectively carrying out acid cleaning and polishing, and simultaneously carrying out acid cleaning and polishing on the molybdenum belt with the thickness of 3.0mm and the width of 80mm in a continuous roll-to-roll mode, wherein 10% -20% of dilute sulfuric acid is adopted for acid cleaning, felt grinding is adopted for polishing, and hot air drying is adopted for water washing. The material is continuously rolled and compounded by adopting different-temperature rolling compound equipment, the different-temperature rolling compound equipment is roll-to-roll continuous compound equipment and is provided with more than three continuous unreels, a molybdenum strip is coiled in the middle, a silver strip is respectively unreeled upwards and unreeled downwards, each strip is controlled in temperature by adopting independent resistance heating and an independent temperature control device, and four-roller rolling compound is adopted for rolling and compounding. During compounding, the temperature of the silver strip is controlled between 150 ℃ and 170 ℃, the temperature of the 4J29 alloy strip is controlled between 1000 ℃ and 1150 ℃, the rolling compound deformation is not less than 50 percent, and the silver/molybdenum/silver compound blank with the thickness of 2.0mm and the width of 77mm is formed after compounding;
step three, carrying out continuous diffusion heat treatment on the silver/molybdenum/silver composite blank obtained in the step two, wherein the diffusion heat treatment temperature is 900-950 ℃, the diffusion heat treatment time is 5 minutes, and in order to prevent silver from absorbing oxygen, the continuous heat treatment needs to be protected by nitrogen and ammonia decomposition gas;
step four, trimming the silver/molybdenum/silver composite blank subjected to diffusion heat treatment in the step three into a blank with the width of 77mm, pickling and polishing, wherein the pickling and polishing are carried out in a continuous roll-to-roll mode, 10% -20% of dilute sulfuric acid is used for cleaning, felt grinding is used for polishing, and hot air drying is used for water washing. Then, hot rolling, surface treatment and continuous heat treatment are carried out by a multi-roll mill with four or more rolls to obtain a finished coil stock with the total thickness of 42 mu m, wherein the thickness of silver layers on two sides is 6 mu m, and the thickness of a molybdenum layer in the middle is 30 mu m;
and step five, cutting the silver/molybdenum/silver composite finished coil stock with the total thickness of 42 microns and the width of 27mmm in the step four into a coil stock with the width of 75mm by using a continuous slitting machine to obtain the composite material.
Example 3
The invention provides a silver/molybdenum/silver metal-based layered composite material, as shown in figure 1, the composite material is of a three-layer layered structure, the total width is 95mm, the total thickness is 57 mu m, wherein the first layer and the third layer are both silver layers 1, the thickness is 6 mu m, the oxygen content is lower than 50ppm, the second layer is a molybdenum layer 2, and the thickness is 45 mu m.
The invention also provides a preparation process of the silver/molybdenum/silver metal-based layered composite material, which comprises the following steps:
step oneSmelting a pure silver plate with the purity of more than 99.99 percent into a silver plate with the oxygen content of less than 50ppm by a three-time vacuum smelting mode, wherein the vacuum degree of smelting equipment in the vacuum smelting process is not less than 10-2Pa. The silver plate is processed into a silver belt with the thickness of 0.6mm and the width of 100mm for standby through surface treatment, rolling processing, annealing and shearing. The rolling processing adopts a common two-roller mill or four-roller mill for rolling, the annealing is mainly softening annealing, the annealing temperature is 450 ℃, the surface treatment is mainly to eliminate the defects of smelting of the silver surface and processing in the process, the processing is usually carried out by adopting a planing or milling mode, and the slitting adopts longitudinal shearing equipment for shearing and removing burrs;
and step two, dividing the silver belt reserved in the step one into two parts, respectively carrying out acid cleaning and polishing, and simultaneously carrying out acid cleaning and polishing on the molybdenum belt with the thickness of 4.5mm and the width of 100mm in a continuous roll-to-roll mode, wherein 10% -20% of dilute sulfuric acid is adopted for acid cleaning, felt grinding is adopted for polishing, and hot air drying is adopted for water washing. The material is continuously rolled and compounded by adopting different-temperature rolling compound equipment, the different-temperature rolling compound equipment is roll-to-roll continuous compound equipment and is provided with more than three continuous unreels, a molybdenum strip is coiled in the middle, a silver strip is respectively unreeled upwards and unreeled downwards, each strip is controlled in temperature by adopting independent resistance heating and an independent temperature control device, and four-roller rolling compound is adopted for rolling and compounding. During compounding, the temperature of the silver strip is controlled between 180 ℃ and 200 ℃, the temperature of the molybdenum strip is controlled between 1150 ℃ and 1200 ℃, the rolling compound deformation is not less than 50 percent, and the silver/molybdenum/silver compound blank with the thickness of 2.35mm and the width of 100mm is formed after compounding;
step three, carrying out continuous diffusion heat treatment on the silver/molybdenum/silver composite blank obtained in the step two, wherein the diffusion heat treatment temperature is 900-950 ℃, the diffusion heat treatment time is 8 minutes, and in order to prevent silver from absorbing oxygen, the continuous heat treatment needs to be protected by nitrogen and ammonia decomposition gas;
step four, trimming the silver/molybdenum/silver composite blank subjected to diffusion heat treatment in the step three into a blank with the width of 97mm, pickling and polishing, wherein the pickling and polishing are carried out in a continuous roll-to-roll mode, 10% -20% of dilute sulfuric acid is used for cleaning, felt grinding is used for polishing, and hot air drying is used for water washing. Then, obtaining a finished coil stock with the total thickness of 57 mu m by hot rolling, surface treatment and continuous heat treatment of four-roller or more multi-roller rolling mills, wherein the thickness of the silver layers on two sides is 6 mu m, and the thickness of the molybdenum layer in the middle is 45 mu m;
and step five, cutting the silver/molybdenum/silver composite finished coil stock with the total thickness of 57 mu m and the width of 97mmm in the step four into a coil stock with the width of 95mm by a continuous slitting machine to obtain the composite material.
In conclusion, the silver/molybdenum/silver metal-based layered composite material prepared by the preparation process disclosed by the invention belongs to a metallurgically bonded layered composite material, has the excellent heat resistance, high-temperature mechanical property and stable expansion coefficient of molybdenum, fully exerts the conductive property and atmospheric corrosion resistance of silver, and can greatly improve the reliability of the electronic and electric appliance field under high and low temperature thermal shock.
The limitation of the protection scope of the present invention is understood by those skilled in the art, and various modifications or changes which can be made by those skilled in the art without inventive efforts based on the technical solution of the present invention are still within the protection scope of the present invention.
Claims (8)
1. The silver/molybdenum/silver metal-based layered composite material is characterized by being of a three-layer layered structure, the total width of the composite material is 25mm-95mm, the total thickness of the composite material is 27 mu m-57 mu m, the first layer and the third layer are both silver layers (1), the thickness of the first layer and the third layer is 6 mu m, the oxygen content of the first layer is lower than 50ppm, and the second layer is a molybdenum layer (2), and the thickness of the second layer is 15 mu m-45 mu m.
2. A preparation process of a silver/molybdenum/silver metal-based layered composite material is characterized by comprising the following steps:
firstly, smelting a pure silver plate with the purity of more than 99.99 percent into a silver plate with the oxygen content of less than 50ppm in a multiple vacuum smelting mode, and then processing the silver plate into a silver strip with the thickness of 0.6mm and the width of 30mm-100mm for later use through calendaring, annealing, surface treatment and shearing;
step two, dividing the silver belt for standby in the step one into two halves, respectively carrying out acid pickling and polishing, simultaneously carrying out acid pickling and polishing on the molybdenum belt with the thickness of 1.5-4.5 mm and the width of 30-100 mm, and then carrying out continuous different temperature rolling by adopting a different temperature rolling composite process, wherein the molybdenum belt is arranged on the second layer, the silver belt is arranged on the first layer and the third layer, the temperature of the silver belt is controlled between 100 ℃ and 200 ℃, the temperature of the molybdenum belt is controlled between 1000 ℃ and 1200 ℃, the deformation of the different temperature rolling is not less than 50%, and a silver/molybdenum/silver composite blank with the thickness of 1.0-2.35 mm and the width of 30-100 mm is formed after the composite;
step three, carrying out continuous diffusion heat treatment on the silver/molybdenum/silver composite blank obtained in the step two, wherein the temperature of the diffusion heat treatment is controlled to be 900-950 ℃, and the time of the diffusion heat treatment is not less than 3 minutes;
cutting the silver/molybdenum/silver composite blank subjected to diffusion heat treatment in the third step into a blank with the width of 27mm-97mm, and performing repeated hot rolling, surface treatment and continuous heat treatment after acid cleaning and polishing to obtain a finished coil stock with the total thickness of 27 mu m-57 mu m, wherein the thickness of the silver layers of the first layer and the third layer is 6 mu m, and the thickness of the molybdenum layer of the second layer is 15 mu m-45 mu m;
and step five, cutting the silver/molybdenum/silver composite finished coil stock with the total thickness of 27-57 microns and the total width of 27-97 mm obtained in the step four into a coil stock with the total width of 25-95 mm, and obtaining the composite material.
3. The process for preparing silver/molybdenum/silver metal-based layered composite material according to claim 2, wherein the degree of vacuum of melting in the first step is not less than 10-2Pa, smelting times is not less than two times.
4. The process for preparing the silver/molybdenum/silver metal-based layered composite material according to claim 2, wherein the differential temperature rolling composite process in the second step adopts four-roll rolling and more than three continuous unreeling, and each coil of strip is subjected to temperature control by adopting separate resistance heating equipment and a separate temperature control device.
5. The process for preparing a silver/molybdenum/silver metal-based layered composite material according to claim 2, wherein the heat treatment in the third step is protected with nitrogen and ammonia decomposition gas.
6. The process for preparing the silver/molybdenum/silver metal-based layered composite material according to claim 2, wherein the acid washing in the second step and the fourth step is performed by washing with 10-20% dilute sulfuric acid, and the polishing is performed by grinding with felt.
7. The process for preparing a silver/molybdenum/silver metal-based layered composite material according to claim 2, wherein the surface treatment in the fourth step is a grinding treatment, and the grinding medium is felt grinding.
8. The process for preparing a silver/molybdenum/silver metal-based layered composite material according to claim 2, wherein the hot rolling in the fourth step is performed by using a four-roll or more multi-roll mill.
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