CN102965634B - Method for preparing beryllium-copper alloy sheet by adopting continuous magnetron sputtering physical-vapor deposition method - Google Patents
Method for preparing beryllium-copper alloy sheet by adopting continuous magnetron sputtering physical-vapor deposition method Download PDFInfo
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Abstract
The invention relates to a method for preparing a beryllium-copper alloy sheet, and particularly relates to a method for preparing the beryllium-copper alloy sheet by adopting a continuous magnetron sputtering physical-vapor deposition method. The method for preparing the beryllium-copper alloy sheet by adopting the continuous magnetron sputtering physical-vapor deposition method comprises the following steps: depositing a pure Be or Be-rich membrane with good combination on the single surface or both surfaces of a pure copper strip by taking a pure Be metal target or a beryllium-copper alloy target with high beryllium content as a cathode and the pure copper strip as an anode and adopting the magnetron sputtering physical-vapor deposition method; and then carrying out diffusion treatment at high temperature to enable Be atoms to be diffused inwards and permeated into a pure copper base body till the content of Be contained in the pure copper strip reaches 1-3 percent by weight so as to obtain a Cu-Be alloy strip, which is excellent in mechanical property and conductive property, with the Be content of 1-3 percent by weight. The method disclosed by the invention has the advantages of simplicity, easiness for operation, high work efficiency, energy-saving and environment-friendly preparation process, controllable quality and great suitability for industrialized application.
Description
Technical field
The present invention relates to a kind of method of preparing beryllium copper thin plate, more particularly, refer to that an employing continuous magnetron sputtering physical vaporous deposition prepares the method for high performance Cu-1～3wt.%Be latten.
Background technology
Beryllium copper is a kind of typical precipitation strength type alloy, have snappiness, high strength, high conductivity, solidity to corrosion, antifatigue, elastic lag little, nonmagnetic, do not produce the series of advantages such as spark while impacting, be widely used in, in space flight, aviation, electronics, communication, machinery, oil, chemical industry, automobile and household electrical appliances industry, having broad application prospects.
At present, beryllium copper Strip is all to adopt rolling preparation substantially, mainly comprises direct chill casting ingot+milling epidermis+heating+roughing+quenching+reroll+quenching+pickling+scrub+operations such as finish rolling.Because beryllium copper ingot casting trends towards secondary segregation when the crystallization, beryllium element, to the enrichment of ingot casting top layer, causes ingot casting different aspects plasticity to have very big-difference, is easy to form crackle during hot rolling.So general ingot casting size and weight are all less, must milling before ingot rolling go its surface at least 2.5mm deeply feel layer.Large, the lumber recovery of rolling beryllium copper technical difficulty, production efficiency are low as can be seen here.And in atmospheric environment melting beryllium copper, there is the drawbacks such as beryllium metallic pollution environment.
Physical gas phase deposition technology has that film coating composition purity is high, process controllability is strong, cleanliness without any pollution and be easy to realize the industrialization advantage such as production continuously; particularly, aspect environment protection, physical vacuum gas phase deposition technology has the unrivaled superiority of other general technologies.The present invention adopts continuous magnetron sputtering physical vapor deposition to prepare Cu-1～3wt.%Be latten method and avoids the technical bottleneck that melting ingot casting in rolling is easy to occur component segregation, selecting the fine copper strip that is highly susceptible to roll forming is base material, adopt the magnetron sputtering technology of high-efficient energy-saving environment friendly in fine copper base band, to deposit rich beryllium rete, and then carry out DIFFUSION TREATMENT, obtain the beryllium copper band of suitable beryllium content.
Summary of the invention
The object of the invention is to avoid the deficiencies in the prior art a kind of method that adopts continuous magnetron sputtering physical vaporous deposition to prepare beryllium copper thin plate is provided.Method sedimentation rate of the present invention is fast, quality controllable, working efficiency is high, and preparation process, under vacuum condition, without beryllium element oxidation and contaminate environment, harmful to human security problems, is therefore extremely applicable to industrial applications.
For achieving the above object, the technical scheme that the present invention takes is: a kind of method that adopts continuous magnetron sputtering physical vaporous deposition to prepare beryllium copper thin plate, and its principal feature is that step is:
(1). the pure copper strips of choosing thickness and be 0.1～0.25mm is made substrate, and does pre-treatment: at concentration 3～5%, 60～80 ℃ of alkali lye of temperature, clean 3～5 minutes, remove oil stain; Then at concentration 3～5% dilute sulphuric acids, clean 3～5 minutes scale removal; Use clear water rinsing; In dehydrated alcohol ultrasonic cleaning, dry up stand-by;
(2). choose pure Be target or high beryllium content beryllium copper 50～80wt.%Be alloy target material:
Preparation
circle or the square pure Be of 1000～1500mm * 180～300mm * 6～20mm or high beryllium content beryllium copper 50～80wt.%Be alloy target material are as magnetic control spattering target, stand-by;
(3). the pure copper strips after step (1) is processed is arranged on the chip bench of magnetron sputtering equipment as anode; The pure Be target of step (2) or high beryllium content beryllium copper 50～80wt.%Be alloy target material are packed among magnetron sputtering coater target stand, as negative electrode again;
Suction to 2 * 10
-3～8 * 10
-4after Pa, pass into argon gas and make pressure-stabilisation in magnetron sputtering coater in 0.2～0.8Pa scope;
Regulate magnetron sputtering deposition condition:
Preheating pure copper strips to 200 ℃～500 ℃;
Sparking voltage 280V～700V, electric current 2A～40A, sedimentation rate are 0.8～1.5 μ m/min;
Under this condition, carry out pure copper strips rich surface Be thin film deposition, depositing time 10～30 minutes, makes plated film copper strips;
(4). the plated film copper strips after step (3) is processed is carried out to 650～750 ℃ of DIFFUSION TREATMENT, and diffusion time, 10～30min, obtained Cu-1～3wt.%Be latten material of section distributed components.
Described employing continuous magnetron sputtering physical vapor deposition is prepared Cu-1～3wt.%Be latten method, in step (3), by the pure Be of a plurality of identical components or high beryllium content beryllium copper target are placed on respectively on a plurality of target position that in magnetron sputtering coater, opposition is installed, pure copper strips passes from centre, realizes the quick continuous coating of wide cut substrate Double-side Synchronous and processes.
Described employing continuous magnetron sputtering physical vapor deposition is prepared Cu-1～3wt.%Be latten method, and in step (3), the rich Be film thickness of pure copper strips surface deposition is 10～35 μ m.
Described employing continuous magnetron sputtering physical vapor deposition is prepared Cu-1～3wt.%Be latten method, and in step (2), target is selected described high beryllium content beryllium copper target, and beryllium content is at 50～80wt.%.
Beneficial effect of the present invention: the present invention adopts continuous magnetron sputtering physical vapor deposition to prepare Cu-1～3wt.%Be latten method can continuously, controllably ooze beryllium and process in technique.By to the choosing of a plurality of target position in magnetron sputtering coater, can carry out arbitrarily the deposition of one side and/or two-sided Be, also can regulate sedimentation rate simultaneously, its depositing operation is simple to operate.
In the present invention, select rolling pure copper strips for oozing Be base material.Choose different B e content target plated film and ooze Be experiment.Result shows, after method of the present invention is processed, can obtain Cu-1～3wt.%Be latten.
The inventive method is compared with traditional rolling, simple for process, and beryllium content height is controlled flexibly, can meet the Special use demand of various occasion beryllium coppers, preparation technology can be applicable to industrialization and produce continuously, and finished product rate is high, steady quality, and cheap for manufacturing cost.
Embodiment
Below principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1: a kind of employing continuous magnetron sputtering physical vapor deposition is prepared Cu-1～3wt.%Be latten method, the steps include:
It is that the pure copper strips of 0.1～0.25mm is made substrate that step 1. is chosen thickness, and does following pre-treatment:
(1) concentration 3～5%, 60～80 ℃ of sodium carbonate alkali lye of temperature clean 3～5 minutes, remove oil stain;
(2) concentration 3～5% dilute sulphuric acids clean 3～5 minutes, scale removal;
(3) clear water rinsing;
(4) dehydrated alcohol ultrasonic cleaning, dries up stand-by;
Step 2. is chosen pure Be target or high beryllium content beryllium copper (50～80wt.%Be) alloy target material:
Preparation
circle or the square pure Be of 1000～1500mm * 180～300mm * 6～20mm or high beryllium content beryllium copper 50～80wt.%Be alloy target material are as magnetic control spattering target, stand-by;
(3). the pure copper strips after step (1) is processed is arranged on the chip bench of magnetron sputtering equipment as anode; The pure Be target of step 2 or high beryllium content beryllium copper 50～80wt.%Be alloy target material are packed among magnetron sputtering target stand, as negative electrode again;
Suction to 2 * 10
-3～8 * 10
-4after Pa, pass into argon gas and make pressure-stabilisation in magnetron sputtering coater in 0.2～0.8Pa scope;
Regulate magnetron sputtering deposition condition:
Preheating pure copper strips to 200 ℃～500 ℃;
Sparking voltage 280V～700V, electric current 2A～40A, sedimentation rate are 0.8～1.5 μ m/min;
Under this condition, carry out pure copper strips rich surface Be thin film deposition, depositing time 10～30 minutes, makes plated film copper strips;
Step 4. is carried out 650～750 ℃ of DIFFUSION TREATMENT by the plated film copper strips after step 3 is processed, and diffusion time, 10～30min, obtained Cu-1～3wt.%Be latten material of section distributed components.
In step 3, by the pure Be of a plurality of identical components or high beryllium content beryllium copper target are placed on respectively on a plurality of target position that in magnetron sputtering coater, opposition is installed, pure copper strips passes from centre, realizes the quick continuous coating of wide cut substrate Double-side Synchronous and processes.
In step 3, the rich Be film thickness of pure copper strips surface deposition is 10～35 μ m.
In step 2, when choosing high Be content beryllium copper and be target, beryllium content is at 50～80wt.%.
Described employing continuous magnetron sputtering physical vapor deposition is prepared Cu-1～3wt.%Be latten method, and the microhardness of the Cu-1～3wt.%Be latten preparing is at 320～380HV0.1, and tensile strength reaches 480～520Mpa.
Adopt continuous magnetron sputtering physical vapor deposition to prepare the method for Cu-1～3wt.%Be latten, magnetron sputtering physical gas-phase deposite method makes Ar pneumoelectric from producing glow plasma under vacuum, electric field action, bombardment beryllium (or beryllium copper) target as sputter goes out high-energy Be(or Be, Cu) atom, deposit to pure Cu substrate surface, form in conjunction with good rich Be rete; And then carry out DIFFUSION TREATMENT, and realize the beryllium that oozes of pure copper strips is processed, obtain a kind of preparation method of novel Cu-1～3wt.%Be latten.
Adopt continuous magnetron sputtering physical vapor deposition to prepare Cu-1～3wt.%Be latten method and rolling comparison, do not have strip-rolling problems of crack, processing method is simple, and vacuum plating mode target purity is high, composition is controlled; Its post-depositional surface quality is good and even; Fine copper base band magnetron sputtering oozes the features such as beryllium process controllability is strong, the feature of environmental protection is good.
Cu-1～3wt.%Be the latten that adopts continuous magnetron sputtering physical vapor deposition to prepare has (1) entirely to be composed direct-reading spectrometer through Auger electron spectrometer and ICP to measure its chemical composition Be content is 1～3wt.%, and presents and be uniformly distributed along cross section; (2) mechanical property of latten reaches 480～520Mpa as tensile strength, and microhardness is at 320～380HV0.1.
Embodiment 2 magnetron sputtering vapour deposition one sides ooze Be
Step 1: choose pure Cu substrate
Choose 200mm * 200mm, the pure copper strips of thick 0.20mm is made substrate, first with concentration 5%, temperature 60 C sodium carbonate alkali lye, cleans 5 minutes, removes oil stain; The dilute hydrochloric acid that is 4% by concentration again cleans 3 minutes, scale removal; Then use clear water rinsing; Use again dehydrated alcohol ultrasonic cleaning, dry up stand-by.
Step 2: choose pure Be target
Preparation
circular pure Be target is as magnetic control spattering target, stand-by;
(3). the pure copper strips after step (1) is processed is arranged on the chip bench of magnetron sputtering equipment as anode; The pure Be target of step 2 is packed among magnetron sputtering target stand, as negative electrode again;
Suction to 1.2 * 10
-3after Pa, pass into argon gas and make pressure-stabilisation in magnetron sputtering coater at 0.6Pa;
Regulate magnetron sputtering deposition condition:
Preheating pure copper strips to 350 ℃;
Sparking voltage 480V, electric current 3.5A, sedimentation rate are 1.2 μ m/min;
Under this condition, carry out pure copper strips surface Be film deposition 20 minutes, prepare the plated film copper strips of thicknesses of layers 20～22m;
Step 4: the plated film copper strips after step 3 is processed is carried out to 720 ℃ of DIFFUSION TREATMENT, and be 25min diffusion time, obtains the uniform Cu-1～3wt.%Be of section composition latten material.
It is 1.9wt.% that the above-mentioned Cu-1～3wt.%Be latten preparing is composed to the average Be content that direct-reading spectrometer detects sample entirely through Auger electron spectrometer and ICP, and composition presents and is uniformly distributed along cross section.Its microhardness reaches 338～355HV0.1 after testing, and tensile strength reaches 488～506Mpa.
Embodiment 3 magnetron sputtering vapour deposition one sides ooze Be
Step 1: choose pure Cu substrate
Choose 1000mm * 200mm, the pure copper strips of thick 0.15mm is made substrate, first with concentration 5%, temperature 60 C sodium carbonate solution, cleans 5 minutes, removes oil stain; The dilute hydrochloric acid that is 4% by concentration again cleans 3 minutes, scale removal; Then use clear water rinsing; Use again dehydrated alcohol ultrasonic cleaning, dry up stand-by.
Step 2: choose high Be content beryllium copper target
The high Be content of founding 1200mm * 200mm * 15mm beryllium copper (Cu-80wt.%Be) alloy target material, stand-by;
Step 3: the pure copper strips after step 1 is processed is arranged on the substrate of magnetron sputtering film machine as anode; Again the beryllium copper target after step 2 is processed is put into magnetron sputtering coater, as negative electrode;
Suction to 1 * 10
-3after Pa, pass into argon gas and make pressure-stabilisation in magnetron sputtering coater at 0.6Pa;
Regulate magnetron sputtering deposition condition:
Preheating pure copper strips to 320 ℃;
Sparking voltage 660V, electric current 35A, sedimentation rate are 1.5～2 μ m/min;
Under this condition, carry out pure copper strips rich surface Be film deposition, preparing thicknesses of layers is the plated film copper strips of 20～22m;
Step 4: the plated film copper strips after step 3 is processed is carried out to 750 ℃ of DIFFUSION TREATMENT, and be 60min diffusion time, obtains the uniform Cu-1～3wt.%Be of section composition latten material.
It is 1.92wt% that the above-mentioned Cu-1～3wt.%Be latten preparing is composed to the average Be content that direct-reading spectrometer detects sample entirely through Auger electron spectrometer and ICP, and composition presents and is uniformly distributed along cross section.Its microhardness reaches 325～348HV0.1 after testing, and tensile strength reaches 486～510Mpa.
The two-sided Be that oozes of embodiment 4 magnetron sputtering vapour deposition
Step 1: choose pure Cu substrate
Choose 200mm * 200mm, the pure copper strips of thick 0.25mm is made substrate, first with concentration 5%, temperature 60 C sodium carbonate alkali lye, cleans 5 minutes, removes oil stain; The dilute hydrochloric acid that is 4% by concentration again cleans 3 minutes, scale removal; Then use clear water rinsing; Use again dehydrated alcohol ultrasonic cleaning, dry up stand-by.
Step 2: choose pure Be target
Choose
2 of pure Be targets, stand-by;
Step 3: 2 pure Be targets after step 2 is processed are put among two target position of magnetron sputtering coater vis-a-vis, as negative electrode, then the pure copper strips after step 1 is processed is hung at magnetron sputtering coater two in the middle of target surface, as anode;
Suction to 8 * 10
-4after Pa, pass into argon gas and make pressure-stabilisation in magnetron sputtering coater at 0.4Pa;
Regulate magnetron sputtering codeposition condition:
Preheating pure copper strips to 300 ℃;
Sparking voltage 480V, electric current 20A, sedimentation rate are 1.2～1.5m/min;
Under this condition, to pure copper strips is two-sided, carry out synchronous Be deposition 10 minutes, prepare the plated film copper strips that upper and lower surface thicknesses of layers is 13～14m;
Step 4: the plated film copper strips after step 3 is processed is carried out to 720 ℃ of DIFFUSION TREATMENT, and be 15min diffusion time, obtains the uniform Cu-1～3wt.%Be of section composition latten material.
It is 2.1wt.% that the above-mentioned Cu-1～3wt.%Be latten preparing is composed to the average Be content that direct-reading spectrometer detects sample entirely through Auger electron spectrometer and ICP, and composition presents and is uniformly distributed along cross section.Its microhardness reaches 350～372HV0.1 after testing, and tensile strength reaches 498～512Mpa.
What the present invention adopted carries out Double-side Synchronous continuous magnetron sputtering plated film and method of diffusion is prepared Cu-1～3wt.%Be latten that 0.1～0.25mm is thick to fine copper thin plate, can be controlled at and in 10～30min, complete the deposition procedures of oozing Be.And its Large-Area-Uniform deposition characteristics also can meet the industrialization continuous production requirement of Cu-1～3wt.%Be thin plate completely, for finally realizing magnetron sputtering method, prepare Cu-1～3wt.%Be thin plate and build and established good basis at industrially scalable tinuous production.
Beryllium copper is a kind of typical precipitation strength type alloy, and Cu-1～3wt.%Be thin plate prepared by aforesaid method, after processing through further solid solution aging, has splendid use properties.Beryllium copper is the indispensable strategic materials of national defense construction and scientific progress, is again day by day to improve with living standards of the people the important materials that has close ties.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. adopt continuous magnetron sputtering physical vaporous deposition to prepare a method for beryllium copper thin plate, it is characterized in that step is:
(1) choosing thickness is that the pure copper strips of 0.1～0.25 mm is made substrate, and does pre-treatment: at concentration 3～5 %, 60～80 ℃ of alkali lye of temperature, clean 3～5 minutes, remove oil stain; Then at concentration 3～5% dilute sulphuric acids, clean 3～5 minutes scale removal; Use clear water rinsing; Use dehydrated alcohol ultrasonic cleaning, dry up stand-by;
(2) choose pure Be target or high beryllium content beryllium copper 50～80wt.%Be alloy target material:
The pure Be that preparation 80～100 mm * 6～20 mm are circular or mm * 6～20,1000～1500mm * 180～300 mm is square or high beryllium content beryllium copper 50～80wt.%Be alloy are as magnetic control spattering target, stand-by;
(3) pure copper strips after step (1) is processed is arranged on the chip bench of magnetron sputtering equipment as anode; The pure Be target of step 2 or high beryllium content beryllium copper 50～80wt.%Be alloy target material are packed among magnetron sputtering coater target stand, as negative electrode again;
Suction to 2 * 10
-3～8 * 10
-4after Pa, pass into argon gas and make pressure-stabilisation in magnetron sputtering coater in 0.2～0.8 Pa scope;
Regulate magnetron sputtering deposition condition:
Preheating pure copper strips to 200 ℃～500 ℃;
Sparking voltage 280V～700V, electric current 2 A～40 A, sedimentation rate are 0.8～1.5 μ m/min;
Under this condition, carry out pure copper strips rich surface Be thin film deposition, depositing time 10～30 minutes, makes plated film copper strips;
(4) the plated film copper strips after step (3) is processed is carried out to 650～750 ℃ of DIFFUSION TREATMENT, diffusion times 10～30, min, obtained the Cu-1～3 wt.% Be latten material of section distributed components.
2. employing continuous magnetron sputtering physical vaporous deposition as claimed in claim 1 is prepared the method for beryllium copper thin plate, it is characterized in that: in step (3), by the pure Be of a plurality of identical components or high beryllium content beryllium copper target are placed on respectively on a plurality of target position that in magnetron sputtering coater, opposition is installed, pure copper strips passes from centre, realizes the quick continuous coating of wide cut substrate Double-side Synchronous and processes.
3. employing continuous magnetron sputtering physical vaporous deposition as claimed in claim 1 is prepared the method for beryllium copper thin plate, it is characterized in that: in step (3), the rich Be film thickness of pure copper strips surface deposition is 10～35 μ m.
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| CN111168182B (en) * | 2020-01-06 | 2022-03-01 | 中航力源液压股份有限公司 | Preparation method of intermediate transition layer applied to vacuum diffusion welding |
| CN113088753B (en) * | 2021-03-31 | 2022-02-15 | 五矿铍业股份有限公司 | Method for preparing beryllium-copper master alloy by adopting vacuum consumable arc melting |
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| CN1616691A (en) * | 2004-11-26 | 2005-05-18 | 宋协福 | Beryllium copper alloy |
| CN101550504A (en) * | 2009-05-25 | 2009-10-07 | 扬中市利达合金制品有限公司 | Manufacturing method of high-conductivity low-beryllium bronze band |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1616691A (en) * | 2004-11-26 | 2005-05-18 | 宋协福 | Beryllium copper alloy |
| CN101550504A (en) * | 2009-05-25 | 2009-10-07 | 扬中市利达合金制品有限公司 | Manufacturing method of high-conductivity low-beryllium bronze band |
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