CN101092707A - Method for preparing aluminium and lead composite electrode material - Google Patents
Method for preparing aluminium and lead composite electrode material Download PDFInfo
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- CN101092707A CN101092707A CN 200710065788 CN200710065788A CN101092707A CN 101092707 A CN101092707 A CN 101092707A CN 200710065788 CN200710065788 CN 200710065788 CN 200710065788 A CN200710065788 A CN 200710065788A CN 101092707 A CN101092707 A CN 101092707A
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Abstract
This invention provides a method for preparing aluminum-tin composite electrode material. The method comprises: (1) removing the oxide film on the surface of an aluminum material; (2) coating the treated aluminum material with 400-550 deg.C liquid transition element; (3) performing liquid-solid compounding on the coated aluminum material and molten tin ot tin alloy at 350-500 deg.C, and cooling to obtain the aluminum-tin composite electrode material. The obtained aluminum-tin composite electrode material has aluminum core, tin outer layer, and transition element middle layer. The aluminum-tin composite electrode material has such advantages as low internal resistance, high strength, light weight, low tank voltage, high corrosion resistance and low tin consumption.
Description
Technical field
The present invention relates to a kind of preparation method of combination electrode material, especially a kind of preparation method of aluminium and lead composite electrode material belongs to the processing and manufacturing technical field of combination electrode material.
Technical background
The used electrode materials of hydrometallurgy and lead storage battery all is based on the combination of the multicomponent alloy of lead, the founding by prior art, rolling or processing method such as draw in the net and alloy material is prepared into the battery lead plate (or grid) of desired shape.Because these alloy electrodes all are to be that the material of major ingredient (Pb＞more than 90%) is made in order to lead, thus have that physical strength is low, internal resistance greatly, defectives such as Heavy Weight.For after reducing weight, reducing internal resistance and have the aluminium powder of employing, lead powder to mix according to a certain ratio, aluminium-lead electrode material of making by mechanical alloying or powder metallurgy process; Or will adopt spray-deposition method to make " alloy " electrode materials of aluminium-plumbous homogeneous mixture after aluminium, the plumbous fusing respectively.The material of these method preparations, only just different big or small aluminum particulate and plumbous particulate mechanically mixing body or block polymers, aluminium, plumbous bonding interface still are physical bond.Because there are the interface binding deficient in aluminium, lead, certainly will form a new galvanic cell between them, under the effect of electrolytic solution, will speed up the etch of this electrode interior aluminium.Therefore, adopt the aluminium one lead electrode material of method for preparing, do not overcome thermodynamics energy barrier in theory, on performance,, all do not have practical value as electrode internal resistance, solidity to corrosion etc.
Summary of the invention
Be low, the deficiencies such as internal resistance big, Heavy Weight of physical strength that overcome existing lead alloy electrode materials existence, and the boundary defect that adopts aluminium-lead electrode material existence of method for preparing.The invention provides a kind of preparation method of aluminium and lead composite electrode material, make that aluminium, plumbous junction are compound to be one, realize aluminium and plumbous metallurgical binding, improve aluminium, plumbous interfacial state, improve the over-all properties of electrode materials.
The present invention realizes by following technical proposal: a kind of preparation method of aluminium and lead composite electrode material is characterized in that through following process steps:
The oxide film of A, removal aluminium material surface;
B, be that 400～550 ℃ liquid phase transition element is plated on aluminium material surface, form the i.e. alloying layer of the 3rd constituent element of aluminium-transition element layer temperature;
C, will have the aluminium of transition element layer and fusion of lead or lead alloy to carry out liquid-solid composite (under 350～500 ℃ of temperature) through B step plating, and promptly get the middle part after the cooling and be the aluminium core, the outside be a lead layer, and the centre is the aluminium-lead composite material of transition element layer.
In the described B step, the transition element that is plated on aluminium material surface is one or more in tin, bismuth, zinc, calcium, magnesium, antimony, tellurium, titanium, selenium, the silicon, and the thickness of coating of its transition element is controlled between 5～1000 μ m.
In the described C step, being compounded in plating, lead alloy on the aluminium of transition element layer is arranged is a kind of among existing P b-Ca-Sn, Pb-Ca-Sn-Al, Pb-Ca-Ag, Pb-Ag, Pb-Ca-Ag-rare earth, the Pb-Sb-As-Se, perhaps be other existing any lead alloy material, the gauge control of its lead-coat or lead alloy coating is at 1～5mm.
The technical barrier that the present invention solves is: utilize the 3rd constituent element and aluminium, the characteristic of plumbous enthalpy of mixing Δ H＜0, generate the continuous transition layer of microalloying by regulation and control between aluminium and plumbous interface, promptly at aluminium, introduce one or more transition element layers (also claiming the 3rd constituent element) between the plumbous interface, make aluminium-plumbous bonding interface obtain the interfacial energy compensation, promptly compensated because of aluminium and plumbous enthalpy of mixing Δ H＞0, thereby cause aluminium, the maximum system energy of junction, plumbous interface---Gibbs free energy reduces, it is the thermodynamics barrier of Δ G=Δ H-T Δ S＜0, fundamentally solved in the aluminium-lead composite material, the compatibility problem of aluminium and plumbous bonding interface, make aluminium, lead is molten at the interface at it to be one, thoroughly improved aluminium, plumbous bonded interfacial state, again by the i.e. diffusion of the 3rd constituent element of transition element, wetting action, realize aluminium and plumbous metallurgical binding at the interface, this electrode materials is compared with traditional lead alloy electrode materials, internal resistance reduces 28%, intensity improves 37%, weight saving 36%, bath voltage reduces by 8.4%, and corrosion rate reduces 40%.This is to reducing the consumption of lead metal, and saving electric energy has obvious effect.
The present invention is owing to introduced the 3rd constituent element between aluminium and lead, aluminium, plumbous compatibility problem have been solved, make aluminium, plumbous interface form metallurgical binding truly, the tissue signature that has possessed aluminium and lead composite electrode material, promptly the microtexture of aluminium-plumbous bonding interface has formed the i.e. connective tissue's structure of the microalloying of the 3rd constituent element/lead of aluminium/transition element.Therefore, with the aluminium and lead composite electrode material of the present invention's preparation, its shearing force and sticking power obviously improve.Can be used for preparing hydrometallurgy with positive plate and lead storage battery grid with the combination electrode material of the inventive method preparation, and products obtained therefrom intensity height, internal resistance are low, in light weight, corrosion-resistant.
Description of drawings
Fig. 1 is the shearing test synoptic diagram of the aluminium and lead composite electrode material of the present invention's method preparation;
Fig. 2 is the sem photograph with the aluminium and lead composite electrode material of the present invention's method preparation;
Fig. 3 is the energy-spectrum scanning figure with the aluminium and lead composite electrode material of the present invention's method preparation.
Wherein, 1 among Fig. 1 is aluminum layer, and 2 is the 3rd constituent element alloying layer, and 3 is plumbous outer.Y among Fig. 3 is mischmetals such as tin, bismuth, zinc, calcium, magnesium, antimony, tellurium, titanium, selenium, silicon.
Embodiment
Below in conjunction with embodiment the present invention is described further.
1, selecting thickness is the technical grade aluminium sheet of 1mm, shears the rectangle band of growth * wide=80 * 20mm, after cleaning oil removing, removes the oxide film on aluminum strip surface with mechanical means;
2, above-mentioned aluminium strip being put into temperature is that 400 ℃ transition element tin liquor is carried out immersion plating, when coating reaches 100 μ m, takes out to such an extent that surperficially be the aluminum strip of tin layer;
3, above-mentioned aluminum strip is packed in the punching block of location, and make it be in medium position, under 350 ℃ of temperature, fusion of lead is injected punching block, make lead layer thickness reach 2mm, promptly get the middle part rapidly after the cooling and be the aluminium core, the outside is a lead layer, and the centre is the aluminium-lead composite material of transition element layer.
4, above-mentioned gained material is made test sample, and carry out the test analysis of mechanical property and heterogeneous microstructure, its result is as follows:
The shearing resistance of the 3rd constituent element alloy layer of A, aluminium-plumbous compound interface has surpassed lead layer tensile strength, aluminium in tension test-plumbous compound interface place does not destroy, and the section of lead alloy has been broken, illustrates that aluminium and lead are combined into one, realized metallurgical binding, as shown in Figure 1.
The bonding interface feature of B, employing scanning electron microscope (model is XL30ESEM-TMP) observation analysis sample is carried out energy spectrum analysis to its interface simultaneously, and with the changing conditions of micro interface alloying constituent, the result shows:
(a) shape characteristic of sample bonding interface shows, the 3rd constituent element to aluminium, the diffusion of lead metal layer, has formed irregular dentation form, and aluminium and lead have not had tangible line of delimitation, as shown in Figure 2.
(b) the one-tenth component curve of sample is earlier by the plumbous peak value of fine aluminium peak value → progressively be changed to aluminium-Xi → progressively be changed to again tin-lead alloy → change at last, illustrate that the interface has formed the microalloy continuous distribution state of aluminium/tin/lead, possessed the due interface feature of matrix material, as shown in Figure 3.
1, selecting thickness is the aluminium net of 1mm, after cleaning oil removing, removes the oxide film of aluminium net surface with mechanical means;
2, above-mentioned aluminium net being put into temperature is that 500 ℃ transition element zinc liquid carries out immersion plating, when coating reaches 50 μ m, takes out to such an extent that surperficially be the aluminium net of tin layer;
3, be that to put into temperature be 460 ℃ fusion Pb-Ca-Sn alloy (composition Ca=0.06% for the aluminium net of tin layer with the surface of above-mentioned 2 step gained, Sn=0.4%, the Pb surplus) in, be the lead alloy of 1mm at aluminium net surface hot dip process one layer thickness fast, promptly get the middle part after the cooling and be the aluminium core, the outside is a lead layer, and the centre is the aluminium-lead composite material of transition element layer.
Claims (3)
1, a kind of preparation method of aluminium and lead composite electrode material is characterized in that through following process steps:
The oxide film of A, removal aluminium material surface;
B, be that 400～550 ℃ liquid phase transition element is plated on aluminium material surface, form the i.e. alloying layer of the 3rd constituent element of aluminium-transition element layer temperature;
C, the aluminium of transition element layer will be arranged through B step plating, and carry out liquid-solid composite with fusion of lead or lead alloy under 350～500 ℃ of temperature, and promptly get the middle part after the cooling and be the aluminium core, the outside is a lead layer, and the centre is the aluminium-lead composite material of transition element layer.
2, the preparation method of aluminium and lead composite electrode material according to claim 1, it is characterized in that in the described B step, the transition element that is plated on aluminium material surface is one or more in tin, bismuth, zinc, calcium, magnesium, antimony, tellurium, titanium, selenium, the silicon, and the thickness of coating of its transition element is controlled between 5～1000 μ m.
3, the preparation method of aluminium and lead composite electrode material according to claim 1, it is characterized in that in the described C step, being compounded in plating, the lead alloy on the aluminium of transition element layer is arranged is any lead alloy material of the prior art, and the gauge control of its lead-coat or lead alloy coating is at 1～5mm.
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| CN 200710065788 CN101092707A (en) | 2007-04-06 | 2007-04-06 | Method for preparing aluminium and lead composite electrode material |
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| CN 200710065788 CN101092707A (en) | 2007-04-06 | 2007-04-06 | Method for preparing aluminium and lead composite electrode material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315455A (en) * | 2010-10-18 | 2012-01-11 | 长沙灿能能源科技有限公司 | Aluminium-based light-type grid for plumbic acid cells and preparation method thereof |
| WO2013143245A1 (en) * | 2012-03-27 | 2013-10-03 | 昆明理工恒达科技有限公司 | Aluminum-based lead or lead alloy composite material and manufacturing method therefor |
| CN106601974A (en) * | 2016-11-29 | 2017-04-26 | 江苏海宝电池科技有限公司 | Carbon fiber grid for power battery and application of carbon fiber grid |
| CN110546791A (en) * | 2017-12-11 | 2019-12-06 | 株式会社高崎电化工业所 | Electrode body for lead-acid battery and lead-acid battery using the same |
| CN110838571A (en) * | 2019-11-25 | 2020-02-25 | 北京居安瑞韩电子有限公司 | Lead-coated aluminum electrode manufacturing method and storage battery |
-
2007
- 2007-04-06 CN CN 200710065788 patent/CN101092707A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315455A (en) * | 2010-10-18 | 2012-01-11 | 长沙灿能能源科技有限公司 | Aluminium-based light-type grid for plumbic acid cells and preparation method thereof |
| WO2012051797A1 (en) * | 2010-10-18 | 2012-04-26 | 中南大学 | Composite porous electrode for sulfuric acid system and preparation method thereof |
| CN102315455B (en) * | 2010-10-18 | 2013-08-14 | 长沙灿能能源科技有限公司 | Aluminium-based light-type grid for plumbic acid cells and preparation method thereof |
| WO2013143245A1 (en) * | 2012-03-27 | 2013-10-03 | 昆明理工恒达科技有限公司 | Aluminum-based lead or lead alloy composite material and manufacturing method therefor |
| CN106601974A (en) * | 2016-11-29 | 2017-04-26 | 江苏海宝电池科技有限公司 | Carbon fiber grid for power battery and application of carbon fiber grid |
| CN110546791A (en) * | 2017-12-11 | 2019-12-06 | 株式会社高崎电化工业所 | Electrode body for lead-acid battery and lead-acid battery using the same |
| US11342550B2 (en) | 2017-12-11 | 2022-05-24 | Hideaki Kato | Electrode body for lead-acid battery, lead-acid battery using the same, and method of manufacturing electrode body for lead-acid battery |
| CN110838571A (en) * | 2019-11-25 | 2020-02-25 | 北京居安瑞韩电子有限公司 | Lead-coated aluminum electrode manufacturing method and storage battery |
| CN110838571B (en) * | 2019-11-25 | 2021-04-02 | 北京居安瑞韩电子有限公司 | Lead-coated aluminum electrode manufacturing method and storage battery |
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Open date: 20071226 |