CN101481807A - Method for manufacturing Al/Pb layered composite electrode - Google Patents
Method for manufacturing Al/Pb layered composite electrode Download PDFInfo
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- CN101481807A CN101481807A CNA2009100940054A CN200910094005A CN101481807A CN 101481807 A CN101481807 A CN 101481807A CN A2009100940054 A CNA2009100940054 A CN A2009100940054A CN 200910094005 A CN200910094005 A CN 200910094005A CN 101481807 A CN101481807 A CN 101481807A
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title description 2
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 229910000978 Pb alloy Inorganic materials 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 229910052745 lead Inorganic materials 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 238000009792 diffusion process Methods 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims description 7
- 238000007747 plating Methods 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- 238000009854 hydrometallurgy Methods 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract 3
- 230000008018 melting Effects 0.000 abstract 3
- 239000011162 core material Substances 0.000 abstract 2
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- DBRHOLYIDDOQSD-UHFFFAOYSA-N alumane;lead Chemical compound [AlH3].[Pb] DBRHOLYIDDOQSD-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 230000008520 organization Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
本发明提供了一种Al/Pb层状复合电极的制备方法，属于湿法冶金领域用电极的制备技术。本法先将350～500℃的Pb合金液浇铸成型为该层状复合电极的工作表面(外壳)，将熔化状态的中间介质在低于300℃时的温度下注入Pb壳体，把表面镀覆好该中间介质的Al芯材预热到150～250℃，迅速插入Pb壳体的中间介质液中，保持150～300℃之间中间介质的熔点以上的温度液固扩散烧结10－60分钟，自然冷却到室温，得到中部为Al芯、外部为Pb层、中间为连接介质的Al/Pb层状复合电极。本发明解决了熔点较低的中间介质与Al、Pb的相容性问题及制备工艺的难题，适用于中间介质的熔点低于金属Al和Pb的熔点的情况。
The invention provides a method for preparing an Al/Pb layered composite electrode, which belongs to the preparation technology of electrodes in the field of hydrometallurgy. In this method, the Pb alloy liquid at 350-500°C is firstly cast into the working surface (shell) of the layered composite electrode, and the molten intermediate medium is injected into the Pb shell at a temperature lower than 300°C, and the surface is plated. The Al core material covered with the intermediate medium is preheated to 150-250°C, quickly inserted into the intermediate medium liquid of the Pb shell, and kept at a temperature above the melting point of the intermediate medium between 150-300°C for liquid-solid diffusion sintering for 10-60 minutes , and naturally cooled to room temperature, the Al/Pb layered composite electrode with Al core in the middle, Pb layer in the outside and connecting medium in the middle was obtained. The invention solves the problem of the compatibility between the intermediate medium with low melting point and Al and Pb and the difficult problem of the preparation process, and is suitable for the situation that the melting point of the intermediate medium is lower than that of the metals Al and Pb.
Description
Technical field
The present invention relates to the preparation method of used Al/Pb layered composite electrode in a kind of hydrometallurgy, be particularly related to the preparation method of Al/Pb layered composite electrode that selected intermediate medium fusing point is lower than the fusing point of Al core and working-surface Pb, belong to the processing and manufacturing technical field of combined electrode.
Technical background
200710065789.9) and " preparation method of aluminium lead composite electrode material " (number of patent application: further improvement 200710065788.4) the present invention is the Chinese patent application " aluminium lead layer shape matrix material " submitted to of the applicant to a application (application number:.
In the hydrometallurgy, not only require the good conductivity of electrode, stable performance, and owing to common electrode need be soaked in the middle of the stronger solution of corrodibility, thereby the material of counter electrode has stronger corrosion-resistant requirement.In traditional hydrometallurgy, usually adopting with Pb is that the Pb alloy that main raw material is made is an electrode, its erosion resistance is stronger, but its physical strength is low, internal resistance is big, weight is big, though by the mode that adds alloy some performances are made moderate progress, can cause new disadvantageous effect again to other performances.For this reason, the applicant has invented " aluminium lead layer shape matrix material " and " preparation method of aluminium lead composite electrode material ", electrode materials used in the hydrometallurgy is improved, by stratiform compoundly go into to conduct electricity very well, in light weight, middle core (as Al, Mg etc.) that cost is low and connect medium, greatly improve disadvantages such as conventional P b alloy electrode inherent physical strength is low, internal resistance is big, weight is big, and realized the metallurgy combination at Al/Pb interface.The applicant has also applied for another patent " a kind of method for preparing aluminum/lead system laminar composite material metallic phase example and display organization " (number of patent application: 200810058704.9), provide a kind of at the metallographic sample preparation method of this matrix material and the method for display organization.Yet, in above-mentioned " preparation method of aluminium lead composite electrode material ", also the weak point of Cun Zaiing is: be lower than at the fusing point of selected intermediate medium under the situation of fusing point on Al core and Pb work top layer, when adopting liquid-solid cast molding, because the too high interface binding medium that causes of Pb liquid temp may partly be washed away, the metallurgical binding intensity at Al/Pb interface is affected, thereby causes electroconductibility, bath voltage, the corrosion rate of this electrode to be affected.
Summary of the invention
Purpose of the present invention is to be lower than at selected intermediate medium fusing point the situation of the fusing point on Al core and Pb work top layer, and a kind of preparation method of new Al/Pb layered composite electrode is provided, and to improve the bonding state at interface, improves the over-all properties of electrode materials.
Purpose of the present invention is achieved through the following technical solutions: the preparation method of described a kind of new A l/Pb layered composite electrode comprises following process steps:
A, oxide film is removed on the Al core surface that cuts, the good intermediate medium of plating naturally cools to room temperature state in 300～350 ℃ of temperature ranges.
B, be to have the cavity structure body Pb work top layer that outer working-surface and an end have the end with 350～500 ℃ Pb liquid cast moldings.
Inject the cavity on the Pb work top layer that the B step prepares under C, the temperature of intermediate medium when being lower than 300 ℃ with fusing, its injection rate is: insert the volume that can just fill up cavity behind the Al core in intermediate medium.
D, when B, C step are carried out, the Al core of the good intermediate medium of plating that A is set by step obtained is preheating to 150～250 ℃.
E, the ready Al core of D step inserted rapidly as inner core in the intermediate medium liquid of Pb work top layer cavity of C step, above 10～60 minutes time of temperature diffusion-sintering of the fusing point of intermediate medium between keeping 150～300 ℃, naturally cool to room temperature, obtain the middle part and be the Pb layer for Al core, outside, middle for connecting the Al/Pb layered composite electrode of medium.
Pb liquid in the described B step, its material is any Pb alloy material in the existing hydrometallurgical technology.
Intermediate medium in the described C step is a kind of among Bi, the Sn or by several made, alloys that its fusing point is lower than Al and Pb fusing point among Bi, Ca, Mg, Sb, Sn, the Zn, it is controlled between 50～1500 μ m between the thickness of diffusion layer between Al and the Pb.
The invention has the beneficial effects as follows: because the present invention has reduced the temperature of Pb liquid and intermediate medium in technology, and the Al core that makes the good intermediate medium of plating remains on above 10～60 minutes the time of temperature diffusion-sintering of fusing point of intermediate medium between 150～300 ℃, solved lower intermediate medium and the compatibility problem of Al, Pb and preparation technology's the difficult problem of fusing point, make the Al/Pb interface realize metallurgical binding, more possessed the complete tissue signature of the microalloying continuous transition of Al/ intermediate medium/Pb.Prepared Al/Pb layered composite electrode is all being obtained gratifying effect aspect interface bond strength, electroconductibility, bath voltage, the corrosion rate.
Description of drawings
Fig. 1 is the Pb alloy structure body with the Al/Pb layered composite electrode of the present invention's method preparation.
Fig. 2 is the energy-spectrum scanning figure at the Al/Sn/Pb layered composite electrode interface of the present invention's method preparation.
The Al/Pb layered composite electrode profile synoptic diagram that Fig. 3 makes for the inventive method.
The energy-spectrum scanning figure at the Al/Bi/Pb layered composite electrode interface that Fig. 4 makes for the inventive method.
Among the figure, the 1:Pb top layer of working; 2: intermediate medium; The 3:Al core.
Embodiment
Below in conjunction with implementing the present invention is described further, but embodiment is not a limitation of the invention.
Embodiment 1
Selecting thickness is the Al plate of the technical grade of 1.2mm, is cut into suitable band, through cleaning oil removing, remove surface film oxide with mechanical means, immerse temperature and be immersion plating in 375 ℃ the Sn liquid, when coating is about 150 μ m, taking out the surface is the Al bar of Sn layer, naturally cools to room temperature.375 ℃ Pb alloy liquid (Pb-1Ag-0.1Ca) poured into be cast into structure in the punching block with skin (working-surface) and inner chamber, the cool to room temperature demoulding, the chamber is thick to be 1.5mm (as shown in Figure 1).The Sn liquid of 280 ℃ of fusings is injected the Pb alloy structure body cavity of 1 step, and liquid level is provided with temperature controller and makes system's insulation at 280 ℃ at its 2/3 volume place.Above-mentioned Al bar is preheating to 250 ℃, insert rapidly in the intermediate medium Sn liquid of fusing in the Pb alloy structure body cavity body, temperature remains on 250～280 ℃ of liquid-solid diffusion-sinterings 1 hour, naturally cool to room temperature, obtain the middle part and be Al core, the outside Al/Pb layered composite electrode that connects medium for Pb layer, centre for Sn.
With this Al/Pb layered composite electrode according to patent of invention " a kind of method for preparing aluminum/lead system laminar composite material metallic phase example and display organization " (publication number: CN 101319974A) its interface is handled, obtain interface power spectrum scintigram (as shown in Figure 2), can be clear that the elemental distribution of direction at the interface along Al to Pb is the Gradient distribution that Al and Pb element all present similar " Z " font, the distribution of Sn then show at the interface relatively uniformly the diffusion, Al in conjunction with figure, the waviness scattering and permeating situation of Pb side, the interface that whole matrix material is described has been realized metallurgical integrated, has possessed the due binding characteristic in stratified composite interface.
Sample preparation steps is substantially the same manner as Example 1, difference is that selected intermediate medium is the Bi of 290 ℃ of fusings, Al inserts in the intermediate medium Bi liquid of fusing in the Pb alloy structure body cavity body, temperature remains on 280～300 ℃ of liquid-solid diffusion-sinterings 30 minutes, naturally cool to room temperature, obtain the middle part and be the Al core, the outside is the Pb layer, the middle Al/Pb layered composite electrode (as Fig. 3) that connects medium for Bi, with this Al/Pb layered composite electrode according to patent of invention " a kind of method for preparing aluminum/lead system laminar composite material metallic phase example and display organization " (publication number: CN 101319974A) its interface is handled, obtain interface power spectrum scintigram (as shown in Figure 4), can be clear that the distribution of Sn in Bi similar embodiment 1 sample of interface, Al, the distribution of Pb is several same with embodiment 1, the interface that whole matrix material is described has been realized metallurgical integrated, has possessed the due binding characteristic in stratified composite interface.
Sample preparation steps is substantially the same manner as Example 1, difference is that selected intermediate medium is the Sn-5Zn-3Bi alloy of 245 ℃ of fusings, Al inserts in the intermediate medium liquid of fusing in the Pb alloy structure body cavity body, temperature remains on 260～280 ℃ of liquid-solid diffusion-sinterings 40 minutes, naturally cool to room temperature, obtain the middle part and be Al core, the outside Al/Pb layered composite electrode that connects medium for Pb layer, centre for Sn-5Zn-3Bi, after handling, metallographic sample preparation shows that this electrode has possessed the due binding characteristic in stratified composite interface, has realized metallurgical integrated.
Claims (3)
1, a kind of preparation method of Al/Pb layered composite electrode is characterized in that: the present invention comprises following process steps successively:
A, oxide film is removed on Al core (3) surface that cuts, the good intermediate medium of plating (2) naturally cools to room temperature state in 300～350 ℃ of temperature ranges;
B, be to have the cavity structure body Pb work top layer (1) that outer working-surface and an end have the end with 350～500 ℃ Pb liquid cast moldings;
Inject the cavity on the Pb work top layer (1) that the B step prepares under C, the temperature of intermediate medium (2) when being lower than 300 ℃ with fusing, its injection rate is: the volume that can just fill up cavity in intermediate medium (2) behind the insertion Al core (3);
D, when B, C step are carried out, the Al core (3) of the good intermediate medium of plating that A is set by step obtained is preheating to 150～250 ℃;
E, the ready Al core of D step (3) inserted rapidly as inner core in intermediate medium (2) liquid of Pb work top layer (1) cavity of C step, above 10～60 minutes time of temperature diffusion-sintering of the fusing point of intermediate medium (2) between keeping 150～300 ℃, naturally cool to room temperature, obtain the middle part and be the Pb layer for Al core, outside, middle for connecting the Al/Pb layered composite electrode of medium.
2, the preparation method of a kind of Al/Pb layered composite electrode according to claim 1 is characterized in that: the Pb liquid in the described B step, its material is any Pb alloy material in the existing hydrometallurgical technology.
3, the preparation method of a kind of Al/Pb layered composite electrode according to claim 1, it is characterized in that: the intermediate medium (2) in the described C step is for a kind of among Bi, the Sn or by several made, alloys that its fusing point is lower than Al and Pb fusing point among Bi, Ca, Mg, Sb, Sn, the Zn, it is controlled between 50～1500 μ m between the thickness of diffusion layer between Al and the Pb.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009100940054A CN101481807A (en) | 2009-01-04 | 2009-01-04 | Method for manufacturing Al/Pb layered composite electrode |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009100940054A CN101481807A (en) | 2009-01-04 | 2009-01-04 | Method for manufacturing Al/Pb layered composite electrode |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102243274A (en) * | 2011-05-05 | 2011-11-16 | 昆明理工大学 | Method for measuring and calculating interface resistivity of Pb-Sn-Al laminated composite material |
| CN102747408A (en) * | 2012-07-12 | 2012-10-24 | 内蒙古第一机械集团有限公司 | Lead-based multivariant alloy electroplating anode |
| CN102864469A (en) * | 2011-07-08 | 2013-01-09 | 浙江盈联科技有限公司 | Method for preparing novel composite anode plate |
| CN103710731A (en) * | 2013-12-10 | 2014-04-09 | 中南大学 | Composite anode used for wet metallurgy |
| CN113571622A (en) * | 2021-07-22 | 2021-10-29 | 厦门三安光电有限公司 | Light-emitting diode and method of making the same |
-
2009
- 2009-01-04 CN CNA2009100940054A patent/CN101481807A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102243274A (en) * | 2011-05-05 | 2011-11-16 | 昆明理工大学 | Method for measuring and calculating interface resistivity of Pb-Sn-Al laminated composite material |
| CN102243274B (en) * | 2011-05-05 | 2013-05-15 | 昆明理工大学 | A Method for Measuring and Calculating the Interface Resistivity of Pb-Sn-Al Layered Composite Material |
| CN102864469A (en) * | 2011-07-08 | 2013-01-09 | 浙江盈联科技有限公司 | Method for preparing novel composite anode plate |
| CN102864469B (en) * | 2011-07-08 | 2015-11-25 | 浙江盈联科技有限公司 | A kind of making method of novel composite anode plate |
| CN102747408A (en) * | 2012-07-12 | 2012-10-24 | 内蒙古第一机械集团有限公司 | Lead-based multivariant alloy electroplating anode |
| CN103710731A (en) * | 2013-12-10 | 2014-04-09 | 中南大学 | Composite anode used for wet metallurgy |
| CN113571622A (en) * | 2021-07-22 | 2021-10-29 | 厦门三安光电有限公司 | Light-emitting diode and method of making the same |
| CN113571622B (en) * | 2021-07-22 | 2022-08-23 | 厦门三安光电有限公司 | Light emitting diode and method for manufacturing the same |
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Open date: 20090715 |