CN102126112A - Preparation method of electromagnetic shielding multi-layer composite material in electric vacuum device - Google Patents
Preparation method of electromagnetic shielding multi-layer composite material in electric vacuum device Download PDFInfo
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- CN102126112A CN102126112A CN 201110063177 CN201110063177A CN102126112A CN 102126112 A CN102126112 A CN 102126112A CN 201110063177 CN201110063177 CN 201110063177 CN 201110063177 A CN201110063177 A CN 201110063177A CN 102126112 A CN102126112 A CN 102126112A
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Abstract
The invention relates to a preparation method of an electromagnetic shielding multi-layer composite material in an electric vacuum device, which belongs to the field of preparation of layered composite materials. The preparation process comprises the following steps: firstly performing large-deformation rolling bonding on oxygen-free copper after surface treatment and an electrical pure iron thin plate, and getting a Cu/Fe/Cu composite foil with higher parallelism and mechanical properties; and then combining and stacking the Cu/Fe/Cu foil with a molybdenum sheet and other low thermal expansion refractory metals, placing in a diffusion welding furnace to perform diffusion welding at a certain temperature and pressure, and further preparing the multi-layer composite material with good magnetic shielding effect, high dimensional precision, strong mechanical properties and good thermal matching. By adopting the new preparation process, not only the problem that the low thermal expansion metals are difficult to compound is solved, but also the advantages of rolling bonding and the diffusion welding process can be fully played, thereby realizing good parallelism among laminated layers, high dimensional precision and excellent mechanical properties of the material, simultaneously having relatively low cost and high production efficiency, and being easy to realize large-scale and industrialized production.
Description
Technical field
The invention belongs to the laminar composite preparation field, be specifically related to electromagnetic shielding its preparing process in a kind of electron tube.
Background technology
Now along with electronic electric equipment use more and more frequent with extensively, information exchange also staged numerical expression increases, these are all inevitably to the environmental radiation electromagnetic energy, this not only produces harmful effect to miscellaneous equipment, but also causing electromagnetic leakage easily, the research and development of various electromagnetic shielding materials more and more are subject to people's attention thus.Magnetic cup material in electron tube, also have complex environment characteristics such as working band is wide, volume is little, stream time is long, environment temperature height, for reducing the wherein influence of transverse field, in the electron tube material, generally adopt the swage structure, and this often reaches the alignment effect by the lamination composite.This class laminate mainly contains: copper/stainless steel, Cu/Fe/Cu sheet, Cu/Mo/Cu sheet and Mo/Cu/Fe lamination etc.But all there is certain shortcoming in these materials: copper/stainless steel exists that Magnetic Shielding Effectiveness is poor, poor radiation, the unmatched problem of thermal coefficient of expansion; The Cu/Fe/Cu sheet exists that intensity is low, the unmatched shortcoming of thermal coefficient of expansion; There is the problem of Magnetic Shielding Effectiveness difference in the Cu/Mo/Cu sheet; Though Mo/Cu/Fe multi-layer stacks composite has excellent comprehensive performances in each side such as thermal conductivity, thermal coefficient of expansion, magnetic shield performance, but adopt that traditional diffusion welding method prepares and exist that the Cu/Fe interlaminar strength is low, the problems such as depth of parallelism difference between the Fe paper tinsel, cause machining finished product rate very low, reduced the performance of Mo/Cu/Fe material, thereby limited its application prospect, sought a kind of new preparation process thus and seem particularly important and urgent at multicomponent, many laminations magnetic cup material.
Summary of the invention
The object of the present invention is to provide that a kind of technology is simple, easy to operate, production efficiency is higher, cost is low, be easy to realize electromagnetic shielding its preparing process in the electron tube that scale, industrialization produce.
Electromagnetic shielding its preparing process in a kind of electron tube of the present invention comprises the steps:
The first step: the surface treatment of electrical pure iron sheet and anaerobic copper sheet
Get electrical pure iron sheet and the anaerobic copper sheet that thickness is 1~3mm and carry out surface treatment respectively, then, carry out hacking again and handle;
Second step: rolling compound
First step gained pure iron, anaerobic copper sheet are pressed stacked, the riveted of Cu/Fe/Cu order, then, be rolled compoundly, obtain the Cu/Fe/Cu composite plate;
The 3rd step: multi-pass is cold roller and deformed
It is cold roller and deformed to design thickness that the second step gained Cu/Fe/Cu composite plate is carried out multi-pass, obtains the Cu/Fe/Cu composite insulating foil, and every time carries out protective atmosphere annealing after cold rolling;
The 4th step: Diffusion Welding
The 3rd step gained Cu/Fe/Cu composite insulating foil and low-thermal-expansion refractory metallic sheet are stacked, place heating in the protective atmosphere Diffusion Welding stove, carry out cooling off with stove after the Diffusion Welding, prepare Mo/Cu/Fe multi-layer stacks composite.
In the electromagnetic shielding its preparing process, described oxygen-free copper purity>99.97%, pure iron are DT4~DT9 electrical pure iron in a kind of electron tube of the present invention.
In a kind of electron tube of the present invention in the electromagnetic shielding its preparing process, pickling, alkali cleaning, ultrasonic washing or at least a in handling of coating are selected in described surface treatment.
In the electromagnetic shielding its preparing process, described hacking is handled and is adopted steel brush hacking to described pure iron, anaerobic copper sheet surface to expose fresh metal, improves both combined strength binations in a kind of electron tube of the present invention.
In a kind of electron tube of the present invention in the electromagnetic shielding its preparing process, described low-thermal-expansion refractory metal is a kind of in molybdenum sheet, tungsten sheet, MoCu sheet, the WCu sheet, and its surface roughness is less than Ra1.6.
In a kind of electron tube of the present invention in the electromagnetic shielding its preparing process, described rolling compound be cold rolling or hot rolling; Described cold rolling reduction ratio 〉=70%; Described hot rolling reduction ratio 〉=50%, hot-rolled temperature are 820 ℃~850 ℃.
In the electromagnetic shielding its preparing process, the cold roller and deformed pass deformation of described multi-pass is 5%-40% in a kind of electron tube of the present invention; Described protective atmosphere annealing temperature is 450~600 ℃, and temperature retention time is 20~60min, and protective atmosphere is inert gas or hydrogen.
In the electromagnetic shielding its preparing process, described Diffusion Welding temperature is 800~900 ℃ in a kind of electron tube of the present invention, and be 10~30 minutes weld interval, pressure 10~50MPa; Described protective atmosphere is a kind of in argon gas, nitrogen, hydrogen or the vacuum, and described vacuum is less than 1.0 * 10
-2Pa.
The present invention is owing to adopt above-mentioned process to prepare electromagnetic shielding multilayer materials in the electron tube; made full use of the advantage of rolling compound and two kinds of technologies of Diffusion Welding; the laminate of preparing; not only the depth of parallelism is good between strength of materials height, each lamination layer, product thickness control is even and accurate; realized the unification of laminate function and mechanical property, and production efficiency is higher, relative cost is low, be easy to realize scale, industrialization production.Problem such as overcome that the Cu/Fe interlaminar strength is low, the depth of parallelism between the Fe paper tinsel is poor, and the low-thermal-expansion refractory metal is difficult compound, and the processed finished products rate is low.The electromagnetic shielding multilayer materials of the present invention's preparation, magnetic cup is effective, dimensional accuracy is high, mechanical property is strong, good, the low magnetic resistance of heat coupling, has good broadband electromagnetical shielding properties, it both can be widely used in the shielding of high accuracy, high sensitivity product in Aero-Space and military equipment equipment, also can be used as the shielding material of ordinary electronic product, thereby have broad application prospects.
Description of drawings:
The comparison of Cu/Fe/Cu composite that accompanying drawing 1 makes for the embodiment of the invention 1 and pure iron, oxygen-free copper tensile mechanical properties;
Accompanying drawing 2 is the embodiment of the invention 3 is represented the MoCu/Cu/Fe lamination composite of low-thermal-expansion refractory metal preparation with MoCu SEM figure.
Wherein: in the accompanying drawing 1, curve 1 is the tensile stress strain curve of oxygen-free copper, and curve 2 is tensile stress strain curves of the Cu/Fe/Cu that makes of the embodiment of the invention 1, and curve 3 is tensile stress strain curves of pure iron;
In the accompanying drawing 2,4-electrical pure iron, 5-oxygen-free copper, 6-MoCu;
From accompanying drawing 1 as can be seen the Cu/Fe/Cu sheet of embodiment 1 preparation compare oxygen-free copper and have higher tensile strength, its percentage elongation is than pure iron also some improvement.The Cu/Fe/Cu sheet of embodiment 1 preparation shows good comprehensive mechanical properties;
From accompanying drawing 2 as can be seen the ESEM picture after amplifying 500 times, no matter through the low-thermal-expansion refractory metallic sheet of Diffusion Welding still through rolling compound oxygen-free copper and electrical pure iron, all compare " totally " at the interface and be intimate-association state; In addition, each lamination constituent element depth of parallelism is good, and gauge is even, and its thickness error is in ± 10 μ m.
The specific embodiment:
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1:
DT9 electrical pure iron and TU1 oxygen-free copper thin plate that selection makes through vacuum induction and electric slag refusion and smelting technology, both are 2mm by thickness, get the raw materials ready according to the size cutting of 100 * 30mm; Carry out silicon carbide paper polishing, ultrasonic wave cleaning, 10%NaOH+10%Na respectively to getting the raw materials ready
2CO
3Aqueous slkali and concentration are 15%HCl+10%HNO
3Acid solution carries out the surface preparation of steps such as soda acid is washed, last alcohol wash; Again the steel brush hacking is adopted in two kinds of metal surfaces, expose fresh metal; The back according to Cu/Fe/Cu assembled in sequence riveted lamination, and carry out immediately reduction ratio be 70% cold rolling compound; Carry out repeatedly inert gas shielding annealing with cold rolling to rolling component again, annealing temperature is: 450~500 ℃, pass deformation is: 5%-15%, be thinned to 0.3mm, and obtain the Cu/Fe/Cu paper tinsel; Choose the molybdenum sheet that surface roughness is Ra0.8 at last, molybdenum sheet is closed the superimposed assembling of Cu/Fe/Cu paper tinsel with having rolled, and put into vacuum diffusion welding and connect stove and carry out Diffusion Welding, 800 ℃ of Diffusion Welding temperature, be incubated 30 minutes, the 15MPa that keep-ups pressure during diffusion welding (DW) is carried out, product machined after Performance Detection is qualified promptly obtains required product after the seam.Record that the Cu/Fe/Cu sheet interface shearing-resistance shearing stress after cold rolling the closing reaches 84MPa in this technology, the tensile strength of Cu/Fe/Cu sheet integral body reaches the 276MPa percentage elongation and reaches 34%.And the tensile strength of pure iron is 240MPa, percentage elongation 31%, and the tensile strength of oxygen-free copper is 208MPa, percentage elongation 57%.
Embodiment 2:
DT8 electrical pure iron and TU1 oxygen-free copper thin plate that selection makes through vacuum induction and electric slag refusion and smelting technology, both are 1mm by thickness, get the raw materials ready according to the size cutting of 100 * 30mm; Carry out silicon carbide paper polishing, ultrasonic wave cleaning, 10%NaOH+10%Na respectively to getting the raw materials ready
2CO
3Aqueous slkali and concentration are 15%HCl+10%HNO
3Acid solution carries out the surface preparation of steps such as soda acid is washed, last alcohol wash; Again the steel brush hacking is adopted in two kinds of metal surfaces, expose fresh metal; The back is according to Cu/Fe/Cu assembled in sequence riveted lamination, and to carry out temperature immediately be that 850 ℃ of reduction ratios are that 50% hot rolling is compound; Carry out repeatedly inert gas shielding annealing with cold rolling to rolling component again, annealing temperature is: 500~550 ℃, pass deformation is: 20%-30%, be thinned to 0.1mm, and obtain the Cu/Fe/Cu paper tinsel; Choosing surface roughness at last is the WCu sheet of Ra1.6, the WCu sheet is closed the superimposed assembling of Cu/Fe/Cu paper tinsel with having rolled, and put into vacuum diffusion welding and connect stove and carry out Diffusion Welding, 900 ℃ of Diffusion Welding temperature, be incubated 10 minutes, the 10MPa that keep-ups pressure during diffusion welding (DW) is carried out, product machined after Performance Detection is qualified promptly obtains required product after the seam.Record in this technology that Cu/Fe/Cu sheet interface shearing-resistance shearing stress reaches 153MPa after hot rolling is closed, the tensile strength of Cu/Fe/Cu sheet integral body reaches the 271MPa percentage elongation and reaches 33%.And the tensile strength of pure iron is 240MPa, percentage elongation 31%, and the tensile strength of oxygen-free copper is 208MPa, percentage elongation 57%.
Embodiment 3
DT8 electrical pure iron and TU1 oxygen-free copper thin plate that selection makes through vacuum induction and electric slag refusion and smelting technology, both are 3mm by thickness, get the raw materials ready according to the size cutting of 100 * 30mm; Carry out silicon carbide paper polishing, ultrasonic wave cleaning, 10%NaOH+10%Na respectively to getting the raw materials ready
2CO
3Aqueous slkali and concentration are 15%HCl+10%HNO
3Acid solution carries out the surface preparation of steps such as soda acid is washed, last alcohol wash; Again the steel brush hacking is adopted in two kinds of metal surfaces, expose fresh metal; The back is according to Cu/Fe/Cu assembled in sequence riveted lamination, and to carry out temperature immediately be that 820 ℃ of reduction ratios are that 50% hot rolling is compound; Carry out repeatedly hydrogen shield annealing with cold rolling to rolling component again, annealing temperature is: 550~600 ℃, pass deformation is: 30%-40%, be thinned to 0.2mm, and obtain the Cu/Fe/Cu paper tinsel; Choosing surface roughness at last is the MoCu sheet of Ra1.0, the MoCu sheet is closed the superimposed assembling of Cu/Fe/Cu paper tinsel with having rolled, and put into vacuum diffusion welding and connect stove and carry out Diffusion Welding, 850 ℃ of Diffusion Welding temperature, be incubated 20 minutes, the 50MPa that keep-ups pressure during diffusion welding (DW) is carried out, product machined after Performance Detection is qualified promptly obtains required product after the seam.Record in this technology that Cu/Fe/Cu sheet interface shearing-resistance shearing stress reaches 178MPa after hot rolling is closed, the tensile strength of Cu/Fe/Cu sheet integral body reaches the 282MPa percentage elongation and reaches 35%.And the tensile strength of pure iron is 240MPa, percentage elongation 31%, and the tensile strength of oxygen-free copper is 208MPa, percentage elongation 57%.
Claims (8)
1. the interior electromagnetic shielding its preparing process of electron tube comprises the steps:
The first step: the surface treatment of electrical pure iron sheet and anaerobic copper sheet
Get electrical pure iron sheet and the anaerobic copper sheet that thickness is 1~3mm and carry out surface treatment respectively, then, carry out hacking again and handle;
Second step: rolling compound
First step gained pure iron, anaerobic copper sheet are pressed stacked, the riveted of Cu/Fe/Cu order, then, be rolled compoundly, obtain the Cu/Fe/Cu composite plate;
The 3rd step: multi-pass is cold roller and deformed
It is cold roller and deformed to design thickness that the second step gained Cu/Fe/Cu composite plate is carried out multi-pass, obtains the Cu/Fe/Cu composite insulating foil, carries out protective atmosphere annealing after every time is cold rolling;
The 4th step: Diffusion Welding
The 3rd step gained Cu/Fe/Cu composite insulating foil and low-thermal-expansion refractory metallic sheet are stacked, place heating in the protective atmosphere Diffusion Welding stove, carry out cooling off with stove after the Diffusion Welding, prepare Mo/Cu/Fe multi-layer stacks composite.
2. electromagnetic shielding its preparing process in a kind of electron tube according to claim 1, it is characterized in that: described oxygen-free copper purity>99.97%, pure iron are DT4~DT9 electrical pure iron.
3. electromagnetic shielding its preparing process in a kind of electron tube according to claim 2 is characterized in that: pickling, alkali cleaning, ultrasonic washing or at least a in handling of coating are selected in described surface treatment.
4. electromagnetic shielding its preparing process in a kind of electron tube according to claim 3, it is characterized in that: described hacking is handled and is adopted steel brush hacking to described pure iron, anaerobic copper sheet surface to expose fresh metal, improves both combined strength binations.
5. electromagnetic shielding its preparing process in a kind of electron tube according to claim 4, it is characterized in that: described low-thermal-expansion refractory metal is a kind of in molybdenum sheet, tungsten sheet, MoCu sheet, the WCu sheet, and its surface roughness is less than Ra1.6.
6. electromagnetic shielding its preparing process in a kind of electron tube according to claim 5 is characterized in that: the described rolling compound cold rolling or hot rolling that is; Described cold rolling reduction ratio 〉=70%; Described hot rolling reduction ratio 〉=50%, hot-rolled temperature are 820 ℃~850 ℃.
7. electromagnetic shielding its preparing process in a kind of electron tube according to claim 6, it is characterized in that: during described multi-pass was cold roller and deformed, each pass deformation was 5%-40%; Described protective atmosphere annealing temperature is 450~600 ℃, and temperature retention time is 20~60min, and protective atmosphere is inert gas or hydrogen.
8. according to electromagnetic shielding its preparing process in any described a kind of electron tube of claim 1-7, it is characterized in that: described Diffusion Welding temperature is 800~900 ℃, and be 10~30 minutes weld interval, pressure 10~50MPa; Described protective atmosphere is a kind of in argon gas, nitrogen, hydrogen or the vacuum, and described vacuum is less than 1.0 * 10-2Pa.
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CN103264261A (en) * | 2013-05-22 | 2013-08-28 | 周旭红 | Method for preparing multi-laminated-layer molybdenum-copper composite material |
CN103273270A (en) * | 2013-05-22 | 2013-09-04 | 周旭红 | Copper-based composite material for shaped charge liner and preparation method |
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CN103264261B (en) * | 2013-05-22 | 2016-03-23 | 周旭红 | A kind of preparation method of many laminations molybdenum-carbon/carbon-copper composite material |
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CN111451275A (en) * | 2019-10-17 | 2020-07-28 | 湖南稀土金属材料研究院 | Preparation method of Nd/Sm rare earth metal foil |
CN111451273A (en) * | 2019-10-17 | 2020-07-28 | 湖南稀土金属材料研究院 | Preparation method of metal ytterbium foil |
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CN111451274A (en) * | 2019-10-17 | 2020-07-28 | 湖南稀土金属材料研究院 | Rare earth metal L a/Ce/Pr foil and preparation method thereof |
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