CN104005062B - Preparation method of aluminum-copper alloy material - Google Patents

Preparation method of aluminum-copper alloy material Download PDF

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Publication number
CN104005062B
CN104005062B CN201410209761.8A CN201410209761A CN104005062B CN 104005062 B CN104005062 B CN 104005062B CN 201410209761 A CN201410209761 A CN 201410209761A CN 104005062 B CN104005062 B CN 104005062B
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electrode material
negative electrode
mesh
plating
positive electrode
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CN104005062A (en
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朱承飞
瞿澄
马超
姚力军
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The invention discloses a preparation method of an aluminum-copper alloy material which is short in production cycle and low in cost. The preparation method comprises the following steps: (1) successively using 320 mesh, 500 mesh and 1000 mesh waterproof abrasive paper to polishing a negative electrode material and a positive electrode material until the electrode materials are specular bright; (2) first washing the polished negative electrode material with ethanol, then using distilled water to wash away surface residual ethanol, then soaking the negative electrode material and the positive electrode material in a hot alkaline solution for alkaline washing to remove surface oil contamination, taking the negative electrode material and the positive electrode material out, then using the distilled water to wash away surface residual surface residual alkaline solution; putting the negative electrode material into a pickling solution to remove a surface oxide film to activate a negative pole; (3) connecting a circuit, turning on a DC power supply, soaking the connected negative electrode material and positive electrode material in to an electrolyte for deposition and electroplating; and (4) putting an electroplated sample in a tubular atmosphere furnace for heat treatment to obtain the aluminum-copper alloy material. The positive electrode material is a pure aluminum sheet, and the negative electrode material is a pure copper sheet.

Description

A kind of preparation method of aluminum copper alloy material
Technical field
The present invention relates to a kind of preparation method of alloy material, more specifically to a kind of preparation of aluminum copper alloy material Method, belongs to field of material surface treatment.
Background technology
Aluminium copper is also referred to as duralumin, hard alumin ium alloy, is one of industry-wide structural metallic materials.Due to its have good The good high-temperature behavior of good comprehensive mechanical property, such as high intensity, good ductility and plasticity and machinability are wide Apply the civil area such as some parts in Aerospace Products, lightweight armor and automobile generally.Such as Aero-Space knot Component, welding rod solder, machining product, engine piston wheel etc..Duan Wenyan etc. have studied HIGH PRESSURE TREATMENT to albronze Microstructure mechanical property and the impact of friction factor.Result shows:After 2GPa HIGH PRESSURE TREATMENT, the organizing of albronze To refinement, it is distributed more uniform;Its nano-indentation hardness, elastic modelling quantity, hard bullet ratio and elastic recovery coefficient all increase, but Friction factor is in a slight decrease.Zhang Lei etc. is prepared for semisolid Al-4.5Cu alloy blank using pulsed magnetic field technology, investigates The impact to semi-solid blank Primary α-Al Phase pattern and size of cooling velocity and pulse frequency.Result shows, Primary α-Al Phase Average grain size and average shape factor respectively the increase of the reduction with cooling velocity and pulse frequency and reduce accordingly And increase.
Al-Cu class alloy is the cast aluminium alloy of industrial earliest employing.Its advantage of casting technique is to can be made into shape again Blank miscellaneous, that particularly there is complicated inner cavity.The preparation research of aluminium copper is concentrated mainly on degasification, deoxidation, slagging-off, rotten place The aspects such as reason.Because the crystallization range of aluminium copper is less, good fluidity, but body shrinkage ratio is larger, is easily formed The defects such as shrinkage cavity.Further, since easily producing one layer of Al2O3 diaphragm during the melting of aluminium copper surface, copper liquid can be stoped Oxidation.But this layer of Al2O3 diaphragm is easy to be destroyed in fusion process, using wood therefore generally in fusion process The refining flux such as the covering fluxes such as charcoal, glass or Na2CO3, CaF2 comes anti-oxidation and air-breathing.The addition of refining flux certainly will Cause material purity, electric conductivity and mechanical properties decrease.The aluminium copper quality of vacuum melting is preferable, but because vacuum sets Standby high cost, production efficiency is low, Gu little adopt.Often aluminum oxide slag inclusion in aluminum bronze ingot surface after melting and inside, This thick oxide inclusions will substantially reduce the mechanical property of aluminium copper.In order to avoid in producing, the problems referred to above occur, Need to research and develop a kind of new method to prepare aluminium copper.
Content of the invention
It is an object of the invention to solving that aluminium copper produces draw in actual production process, to fill the type casting such as bad scarce Sunken problem, provides a kind of preparation method of aluminum copper alloy material.The method shortens technological process, improves operating efficiency, Greatly reduce energy consumption, cycle is short, low cost.
The present invention is achieved by the following technical solutions:
The preparation method of the aluminum copper alloy material of the present invention, it comprises the following steps:
(1) successively with 320 mesh, 500 mesh, 1000 mesh silicon carbide papers by yin, yang electrode material sanding and polishing to bright in mirror surface;
(2) cathode material after polishing is first used ethanol purge, then fall the ethanol of remained on surface with distilled water flushing, then Yin, yang electrode material is immersed in thermokalite washing lotion and carries out alkali cleaning removing surface and oil contaminant, with steaming after yin, yang electrode material is taken out Distilled water cleaning electrode remained on surface alkali lye;Again removing surface film oxide, activated cathode in pickle are put in cathode material pole;
(3) connect circuit, open dc source, carry out depositing in immersion electrolyte after yin, yang electrode material is connected, Plating;
(4) sample after plating is put in tube-type atmosphere furnace and be heat-treated, heat treatment obtains final product aluminium copper after terminating Material;
Wherein said anode material is fine aluminium piece, and cathode material is pure copper sheet.
The preparation method of the aluminum copper alloy material of the present invention, its further technical scheme is described alkali cleaning formula of liquid For:NaOH5~15g/L, Na2CO325~45g/L, NaPO330~50g/L, 50~70 DEG C of alkali cleaning liquid temp, alkali cleaning time 10~ 20min;Pickling formula of liquid is:HCl20~40g/L, acid-wash activation time 1~2min;The electricity taking out from alkali wash water, pickle Extremely all dried up with after flowing distilled water flushing.
The preparation method of the aluminum copper alloy material of the present invention, its further technical scheme can also be described electrolyte In anhydrous AlCl3, NaCl, KCl mass ratio be 3:1:1~8:1:1, described depositing current density is 0.5~5A/dm2, deposition Temperature is 140~180 DEG C;Electrolyte stirring is kept, to guarantee the uniformity of molten salt composition and temperature in whole electroplating process;Electricity After plating terminates, sample is put into rapidly and dries up after being cleaned by ultrasonic in water.
The preparation method of the aluminum copper alloy material of the present invention, its further technical scheme can also be described electroplating Sample afterwards is put into and is carried out heat treatment step in tube-type atmosphere furnace and be:Sample after plating is put into tube-type atmosphere furnace, leads to 1 in advance Heated up with the programming rate of 5 DEG C/min after the air that hour argon gas displaces in system;Heat treatment temperature is 650~850 DEG C, protects Temperature was cooled to room temperature after 4~6 hours, maintained argon flow amount 80mL/min in whole process.
The invention has the beneficial effects as follows:
The present invention prepares aluminium copper using heat-treating methods after plating, effectively prevent in actual production because body is received Contracting and form the defects such as shrinkage cavity, and the decline of the mechanical property of aluminium copper that thick oxide inclusions cause.Additionally The production cycle can be shortened, avoid using some heavy mechanical equipments, thus reducing energy consumption, the purpose of saving production cost. The aluminium copper that the preparation technology being proposed obtains has face-centered cubic crystal structure, and lattice paprmeter is Microhardness is 117.66~132.57HV, and corrosion electric current density is 1.375 × 10-6~1.323 × 10-5A/dm2.
Brief description
Fig. 1 is electrolysis unit schematic diagram, 1:Dc source, 2:Ammeter, 3:Oil bath, 4:Argon gas;
Fig. 2 is current density 0.5~2A/dm in embodiment 12, deposit under the conditions of 170~180 DEG C of depositing temperature, through 650 The X ray diffracting spectrum (XRD) of material after~850 DEG C of heat treatment 4~6h;
Fig. 3-1 is current density 2~3A/dm in embodiment 22, deposit under the conditions of 160~170 DEG C of depositing temperature, through 650 The cross-sectional scans electron microscopic picture (SEM) of material after~850 DEG C of heat treatment 4~6h;
Fig. 3-2 is current density 2~3A/dm in embodiment 22, deposit under the conditions of 160~170 DEG C of depositing temperature, through 650 The distribution diagram of element of material after~850 DEG C of heat treatment 4~6h;
Fig. 4 is current density 3~4A/dm in embodiment 32, deposit under the conditions of 150~160 DEG C of depositing temperature, through 650~ Material after 850 DEG C of heat treatment 4~6h and fine copper microhardness figure;
Fig. 5 is current density 4~5A/dm in embodiment 42, deposit under the conditions of 140~150 DEG C of depositing temperature, through 650~ Material after 850 DEG C of heat treatment 4~6h and fine copper polarization curve.
Specific embodiment
Processed using following methods in the preparation method of the present invention:
(1) successively with 320 mesh, 500 mesh, 1000 mesh silicon carbide papers by yin, yang electrode material sanding and polishing to bright in mirror surface;
(2) cathode material after polishing is first used ethanol purge, then fall the ethanol of remained on surface with distilled water flushing, then Yin, yang electrode material is immersed in thermokalite washing lotion and carries out alkali cleaning removing surface and oil contaminant, with steaming after yin, yang electrode material is taken out Distilled water cleaning electrode remained on surface alkali lye;Again removing surface film oxide, activated cathode in pickle are put in cathode material pole;
(3) connect circuit, open dc source, carry out depositing in immersion electrolyte after yin, yang electrode material is connected, Plating;
(4) sample after plating is put in tube-type atmosphere furnace and be heat-treated, heat treatment obtains final product aluminium copper after terminating Material;
Wherein said anode material is fine aluminium piece, and cathode material is pure copper sheet.
Embodiment 1
Anodic-cathodic sequentially passes through sanding and polishing, alkali cleaning oil removing, and after acid-wash activation, immersion electrolyte is electrolysed.Anhydrous AlCl3, NaCl, KCl mass ratio be 4:1:1~5:1:1, current density 0.5~2A/dm2, 170~180 DEG C of depositing temperature.Deposition Sample afterwards is through 650~850 DEG C of heat treatment 4~6h.After heat treatment, the crystal structure of material is as shown in Fig. 2 illustrate this technique bar Face-centered cubic solid solution has been obtained under part.Do not find other miscellaneous peaks simultaneously in XRD spectrum, illustrate that the aluminium copper being obtained has relatively High-purity.The lattice paprmeter of this processing alloy isMicrohardness 123.47~127.04HV, corrosion current Density 1.198 × 10-5~1.207 × 10-5A/dm2.
Embodiment 2
Anodic-cathodic sequentially passes through sanding and polishing, alkali cleaning oil removing, and after acid-wash activation, immersion electrolyte is electrolysed.Anhydrous AlCl3, NaCl, KCl mass ratio be 3:1:1~4:1:1, current density 2~3A/dm2, 160~170 DEG C of depositing temperature.After deposition Sample through 650~850 DEG C heat treatment 4~6h.The cross-sectional scans electron microscopic picture (SEM) of material and Elemental redistribution after heat treatment As shown in figure 3, Elemental redistribution in figure other elements in addition to Al, Cu, illustrate that the alloy being obtained has higher pure Degree.In addition any crack does not occur between alloy-layer and parent metal, show that matrix and alloy have stronger bonding strength. Fig. 3 shows that the thickness of alloy-layer is about 36 μm.The lattice paprmeter of this processing alloy isMicrohardness 128.92~132.57HV, corrosion electric current density 6.731 × 10-6~6.739 × 10-6A/dm2.
Embodiment 3
Anodic-cathodic sequentially passes through sanding and polishing, alkali cleaning oil removing, and after acid-wash activation, immersion electrolyte is electrolysed.Anhydrous AlCl3, NaCl, KCl mass ratio be 3:1:1~5:1:1, current density 3~4A/dm2, 150~160 DEG C of depositing temperature.After deposition Sample through 650~850 DEG C heat treatment 4~6h.After heat treatment material microhardness as shown in figure 4, with fine copper (>=80HV) Compare microhardness and improve 47.8~50.9%.The lattice paprmeter of this processing alloy isMicrohardness 117.66~120.72HV, corrosion electric current density 1.375 × 10-6~1.384 × 10-6A/dm2.
Embodiment 4
Anodic-cathodic sequentially passes through sanding and polishing, alkali cleaning oil removing, and after acid-wash activation, immersion electrolyte is electrolysed.Anhydrous AlCl3, NaCl, KCl mass ratio be 6:1:1~8:1:1, current density 4~5A/dm2, 140~150 DEG C of depositing temperature.After deposition Sample through 650~850 DEG C heat treatment 4~6h.Material polarization curve after heat treatment as shown in figure 5, with fine copper (1.577 × 10- 5A/dm2) compare corrosion electric current density and have dropped 19.2~20%.The lattice paprmeter of this processing alloy is Microhardness 128.95~131.94HV, corrosion electric current density 1.314 × 10-5~1.323 × 10-5A/dm2.

Claims (1)

1. a kind of preparation method of aluminum copper alloy material is it is characterised in that comprise the following steps:
(1) successively with 320 mesh, 500 mesh, 1000 mesh silicon carbide papers by yin, yang electrode material sanding and polishing to bright in mirror surface;
(2) cathode material after polishing is first used ethanol purge, then fall the ethanol of remained on surface with distilled water flushing, then will Yin, yang electrode material is immersed in thermokalite washing lotion and carries out alkali cleaning removing surface and oil contaminant, with distillation after yin, yang electrode material is taken out Water cleaning electrode remained on surface alkali lye;Again cathode material is put into removing surface film oxide, activated cathode in pickle;
(3) connect circuit, open dc source, carry out depositing in immersion electrolyte after yin, yang electrode material is connected, electricity Plating;
(4) sample after plating is put in tube-type atmosphere furnace and be heat-treated, heat treatment obtains final product aluminum copper alloy material after terminating;
Wherein said anode material is fine aluminium piece, and cathode material is pure copper sheet;Described alkali cleaning formula of liquid is:NaOH5~ 15g/L、Na2CO325~45g/L, NaPO330~50g/L, 50~70 DEG C of alkali cleaning liquid temp, alkali cleaning time 10~20min;Acid Lotion prescription is:HCl 20~40g/L, acid-wash activation time 1~2min;The electrode taking out from alkali wash water, pickle is all used Dry up after flowing distilled water flushing;Anhydrous AlCl in described electrolyte3, NaCl, KCl mass ratio be 3:1:1~8:1:1, institute When the carrying out stated deposits, its current density is 0.5~5A/dm2, depositing temperature be 140~180 DEG C;Keep in whole electroplating process Electrolyte stirs, to guarantee the uniformity of molten salt composition and temperature;After plating terminates, sample is put into rapidly in water and be cleaned by ultrasonic After dry up;Described put into the sample after plating carries out heat treatment step and is in tube-type atmosphere furnace:Sample after plating is put Enter tube-type atmosphere furnace, heated up with the programming rate of 5 DEG C/min after leading to the air that 1 hour argon gas displaces in system in advance;At heat Reason temperature is 650~850 DEG C, and insulation was cooled to room temperature after 4~6 hours, maintains argon flow amount 80mL/min in whole process..
CN201410209761.8A 2014-05-19 2014-05-19 Preparation method of aluminum-copper alloy material Expired - Fee Related CN104005062B (en)

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CN105568324B (en) * 2016-02-25 2017-12-15 南京工业大学 A kind of preparation method of high performance surface alloying copper product
CN107144483B (en) * 2017-05-11 2023-10-03 兰州大学 Nanometer indentation multi-field test system based on liquid nitrogen refrigeration
CN111769300B (en) * 2020-02-28 2023-06-30 上海市机电设计研究院有限公司 Preparation method of aluminum-based copper-plated current collector for all-vanadium redox flow battery

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