CN104043824B - A kind of raising AB3The method of modifying of type hydrogen storage alloy chemical property - Google Patents
A kind of raising AB3The method of modifying of type hydrogen storage alloy chemical property Download PDFInfo
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- CN104043824B CN104043824B CN201410299117.4A CN201410299117A CN104043824B CN 104043824 B CN104043824 B CN 104043824B CN 201410299117 A CN201410299117 A CN 201410299117A CN 104043824 B CN104043824 B CN 104043824B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 43
- 239000000956 alloy Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000001257 hydrogen Substances 0.000 title claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 14
- 239000000126 substance Substances 0.000 title claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 229910001122 Mischmetal Inorganic materials 0.000 claims abstract description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 230000006698 induction Effects 0.000 claims abstract description 6
- 238000004137 mechanical activation Methods 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005275 alloying Methods 0.000 claims description 10
- 239000008188 pellet Substances 0.000 claims description 10
- 229910017052 cobalt Inorganic materials 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 22
- 229910018095 Ni-MH Inorganic materials 0.000 abstract description 7
- 229910018477 Ni—MH Inorganic materials 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 229910000714 At alloy Inorganic materials 0.000 abstract 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 239000012279 sodium borohydride Substances 0.000 abstract 1
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 238000011160 research Methods 0.000 description 3
- 239000001996 bearing alloy Substances 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910002335 LaNi5 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
The invention discloses a kind of raising AB3The method of modifying of type hydrogen storage alloy chemical property.AB is prepared by vacuum induction melting method3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47(Mm is mischmetal, and the percentage by weight of composition is: 82.3% La and 17.7%Nd) precursor alloy, alloy pig is by after mechanical activation comminution, and ball milling 60 ~ 90 minutes, the particle powder screening out 200 ~ 300 orders is used for the preparation of modified alloy；Prepared alloy is put into plating solution (CoCl2, HCl) in, stir 5 minutes, add NaBH4Solution, continues stirring 20 minutes, filters, washing, and namely vacuum drying prepares the AB of plating nickel on surface3Type modified alloy.The present invention, by being coated with metal simple-substance at alloy surface, improves cyclical stability and the dynamic performance of alloy, the development of Ni-MH battery is of great practical significance.
Description
Technical field
The invention belongs to materials chemistry, metallurgical chemistry and electrochemical research field, improve AB particularly to one3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47The method of modifying of hydrogen storage alloy electrochemical performance.
Background technology
Since first Ni-MH battery is after Japan is commercially used, Ni-MH battery has been obtained for being widely applied.AB3Type hydrogen storage alloy becomes the focus of countries in the world Ni-MH battery area research owing to having higher specific discharge capacity, but it is easily corroded in alkaline solution so that its application in Ni-MH battery is restricted.Owing to the performance of battery is limited mainly by the impact of alloy surface structure, the electro catalytic activity of such as alloy surface and corrosion resistance and the maximum discharge capacity of NiH electrode, charge-discharge power, cyclical stability are closely related, and therefore the research of alloy surface texture just has the meaning of particular importance.In recent decades, researcher adopts the method alloys such as alkali process, ball-milling process, fluorination treatment, electroplating technology, electroless plating technology to carry out surface modification, to expect the overall chemical property improving hydrogen bearing alloy.Wherein, electroless cobalt plating is a kind of highly effective method.
Summary of the invention
It is an object of the invention to provide a kind of raising AB3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47The method of modifying of hydrogen storage alloy electrochemical performance.
The thinking of the present invention: use the method for electroless cobalt plating to AB3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47(Mm is mischmetal, and the percentage by weight of composition is: 82.3%La and 17.7%Nd) hydrogen bearing alloy carries out surface modification, to improve its chemical property so that it is can better be applied in Ni-MH battery.
Concretely comprise the following steps:
(1) weigh purity raw metal more than 99% according to target product mol ratio, under argon shield, prepare AB by vacuum induction melting method3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Precursor alloy, alloy pig by after mechanical activation comminution, with the rotating speed ball milling 60 ~ 90 minutes of 250 ~ 300 revs/min on planetary ball mill, screens out the Mm of 200 ~ 300 orders0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is standby；Described Mm is mischmetal, and the percentage by weight of composition is: 82.3%La and 17.7%Nd.
(2) Mm that 2 grams of steps (1) prepare is taken0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is put in 200 milliliters of plating solutions, stirs 5 minutes, adds the NaBH of 50 milliliters of 0.01 ~ 0.04mol/L4Solution, continues stirring 20 minutes, filters, and with deionized water and absolute ethanol washing, then vacuum drying 6 ~ 10 hours at 60 DEG C, prepares the AB of surface cobalt plating3Type modified alloy, namely completes AB3The raising of type hydrogen storage alloy chemical property modifiies；Containing 0.6 × 10 in described plating solution-2~2.4×10-2The CoCl of mol/L2With 0.5 × 10-3~2.0×10-3The HCl of mol/L.
The inventive method does not change the structure of precursor alloy by electroless cobalt plating, and modified alloy is still by LaNi5Phase and La2Ni7Phase composition, improves cyclical stability and the dynamic performance of alloy, the development of Ni-MH battery is of great practical significance.
Detailed description of the invention
Embodiment 1:
(1) weigh purity raw metal more than 99% according to target product mol ratio, under argon shield, prepare AB by vacuum induction melting method3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Precursor alloy, alloy pig by after mechanical activation comminution, with the rotating speed ball milling 75 minutes of 270 revs/min on planetary ball mill, screens out the Mm of 250 orders0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is standby；Described Mm is mischmetal, and the percentage by weight of composition is: 82.3%La and 17.7%Nd.
(2) Mm that 2 grams of steps (1) prepare is taken0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is put in 200 milliliters of plating solutions, stirs 5 minutes, adds the NaBH of 50 milliliters of 0.01mol/L4Solution, continues stirring 20 minutes, filters, and with deionized water and absolute ethanol washing, then vacuum drying 8 hours at 60 DEG C, prepares the AB of surface cobalt plating3Type modified alloy Co-1, namely completes AB3The raising of type hydrogen storage alloy chemical property modifiies；Containing 0.6 × 10 in described plating solution-2The CoCl of mol/L2With 0.5 × 10-3The HCl of mol/L.
Embodiment 2:
(1) weigh purity raw metal more than 99% according to target product mol ratio, under argon shield, prepare AB by vacuum induction melting method3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Precursor alloy, alloy pig by after mechanical activation comminution, with the rotating speed ball milling 75 minutes of 270 revs/min on planetary ball mill, screens out the Mm of 250 orders0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is standby；Described Mm is mischmetal, and the percentage by weight of composition is: 82.3%La and 17.7%Nd.
(2) Mm that 2 grams of steps (1) prepare is taken0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is put in 200 milliliters of plating solutions, stirs 5 minutes, adds the NaBH of 50 milliliters of 0.02mol/L4Solution, continues stirring 20 minutes, filters, and with deionized water and absolute ethanol washing, then vacuum drying 8 hours at 60 DEG C, prepares the AB of surface cobalt plating3Type modified alloy Co-2, namely completes AB3The raising of type hydrogen storage alloy chemical property modifiies；Containing 1.2 × 10 in described plating solution-2The CoCl of mol/L2With 1.0 × 10-3The HCl of mol/L.
Embodiment 3:
(1) weigh purity raw metal more than 99% according to target product mol ratio, under argon shield, prepare AB by vacuum induction melting method3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Precursor alloy, alloy pig by after mechanical activation comminution, with the rotating speed ball milling 75 minutes of 270 revs/min on planetary ball mill, screens out the Mm of 250 orders0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is standby；Described Mm is mischmetal, and the percentage by weight of composition is: 82.3%La and 17.7%Nd.
(2) Mm that 2 grams of steps (1) prepare is taken0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is put in 200 milliliters of plating solutions, stirs 5 minutes, adds the NaBH of 50 milliliters of 0.04mol/L4Solution, continues stirring 20 minutes, filters, and with deionized water and absolute ethanol washing, then vacuum drying 8 hours at 60 DEG C, prepares the AB of surface cobalt plating3Type modified alloy Co-3, namely completes AB3The raising of type hydrogen storage alloy chemical property modifiies；Containing 2.4 × 10 in described plating solution-2The CoCl of mol/L2With 2.0 × 10-3The HCl of mol/L.
The AB that above-mentioned 3 embodiments are prepared3Type modified alloy Co-1, Co-2 or Co-3 preparation is Electrode Negative sheet: take 0.1 gram of Co-1, Co-2 or Co-3, carbonyl nickel powder mix homogeneously is added by weight 1:2, mixed-powder is pressed into, with the pressure of 10MPa, the small pieces that diameter is for 11.5 millimeters by desk-top tablet machine, then by two panels nickel foam, electrode slice is coated with, the pressure compaction adopting 10MPa prepares into negative plate, calculates the real content of alloyed powder sample.
Measuring the phase structure of alloy, cyclical stability and dynamic performance respectively with LAND5.3B battery test system, XRD diffractometer and CHI660E electrochemical workstation, result is as follows:
A. the maximum discharge capacity of alloy electrode is from 292.3mAh/g (AB3) increase to 312.6mAh/g(Co-3).
B. after cobalt plating processes, the cyclical stability of alloy electrode is improved significantly, and after 50 circulations, the circulation volume conservation rate of electrode is from 83.3% (AB3) increase to 97.2% (Co-1), then it is reduced to 93.6%(Co-3).
C. the exchange current density of electrode, limiting current density, corrosion potential and electro-chemical activity are obtained for raising.
Claims (1)
1. one kind is improved AB3The method of modifying of type hydrogen storage alloy chemical property, it is characterised in that concretely comprise the following steps:
(1) weigh purity raw metal more than 99% according to target product mol ratio, under argon shield, prepare AB by vacuum induction melting method3Type Mm0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Precursor alloy, alloy pig by after mechanical activation comminution, with the rotating speed ball milling 60 ~ 90 minutes of 250 ~ 300 revs/min on planetary ball mill, screens out the Mm of 200 ~ 300 orders0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is standby；Described Mm is mischmetal, and the percentage by weight of composition is: 82.3%La and 17.7%Nd；
(2) Mm that 2 grams of steps (1) prepare is taken0.78Mg0.22Ni2.48Mn0.09Al0.23Co0.47Alloying pellet powder is put in 200 milliliters of plating solutions, stirs 5 minutes, adds the NaBH of 50 milliliters of 0.01 ~ 0.04mol/L4Solution, continues stirring 20 minutes, filters, and with deionized water and absolute ethanol washing, then vacuum drying 6 ~ 10 hours at 60 DEG C, prepares the AB of surface cobalt plating3Type modified alloy, namely completes AB3The raising of type hydrogen storage alloy chemical property modifiies；Containing 0.6 × 10 in described plating solution-2~2.4×10-2The CoCl of mol/L2With 0.5 × 10-3~2.0×10-3The HCl of mol/L.
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| CN104942279A (en) * | 2015-05-17 | 2015-09-30 | 桂林理工大学 | Method for using polyaniline surface modification AB3 type hydrogen storage alloy |
| CN106001546A (en) * | 2016-07-21 | 2016-10-12 | 桂林理工大学 | Method for modifying La-Mg-Ni based hydrogen storage alloy through n-heptanal p-phenylenediamine bis-schiff base |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6270547B1 (en) * | 1997-09-30 | 2001-08-07 | Sanyo Electric Co., Ltd. | Hydrogen absorbing alloy electrode and process for fabricating same |
| CN101338417A (en) * | 2008-08-14 | 2009-01-07 | 南京工业大学 | Surface treating method for hydrogen occluding alloy |
| CN101476127A (en) * | 2009-01-24 | 2009-07-08 | 燕山大学 | Surface recombination processing method for rare earth-magnesium-nickel based AB3 type hydrogen storage alloy |
| CN103111616A (en) * | 2013-03-07 | 2013-05-22 | 桂林理工大学 | Fluorination modification method for AB3-type hydrogen storage alloy |
| CN103611930A (en) * | 2013-12-19 | 2014-03-05 | 桂林理工大学 | Method for surface modification of AB3 type hydrogen storage alloy |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07118704A (en) * | 1993-10-25 | 1995-05-09 | Matsushita Electric Ind Co Ltd | Hydrogen storage alloy powder, nickel-hydrogen battery having the powder in negative electrode active material and production of the powder |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6270547B1 (en) * | 1997-09-30 | 2001-08-07 | Sanyo Electric Co., Ltd. | Hydrogen absorbing alloy electrode and process for fabricating same |
| CN101338417A (en) * | 2008-08-14 | 2009-01-07 | 南京工业大学 | Surface treating method for hydrogen occluding alloy |
| CN101476127A (en) * | 2009-01-24 | 2009-07-08 | 燕山大学 | Surface recombination processing method for rare earth-magnesium-nickel based AB3 type hydrogen storage alloy |
| CN103111616A (en) * | 2013-03-07 | 2013-05-22 | 桂林理工大学 | Fluorination modification method for AB3-type hydrogen storage alloy |
| CN103611930A (en) * | 2013-12-19 | 2014-03-05 | 桂林理工大学 | Method for surface modification of AB3 type hydrogen storage alloy |
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Application publication date: 20140917 Assignee: Guilin Qingjiang Construction Engineering Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044223 Denomination of invention: A Modification Method for Improving the Electrochemical Performance of AB3Hydrogen Storage Alloys Granted publication date: 20160629 License type: Common License Record date: 20231024 |
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Application publication date: 20140917 Assignee: GUANGXI CHAOXING SOLAR ENERGY TECHNOLOGY Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044955 Denomination of invention: A Modification Method for Improving the Electrochemical Performance of AB3Hydrogen Storage Alloys Granted publication date: 20160629 License type: Common License Record date: 20231031 |
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Application publication date: 20140917 Assignee: Guangxi Guiren Energy Saving Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980045072 Denomination of invention: A Modification Method for Improving the Electrochemical Performance of AB3Hydrogen Storage Alloys Granted publication date: 20160629 License type: Common License Record date: 20231101 |