CN109930042A - A kind of magnesium-alloy anode material and the preparation method and application thereof - Google Patents
A kind of magnesium-alloy anode material and the preparation method and application thereof Download PDFInfo
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- CN109930042A CN109930042A CN201910296640.4A CN201910296640A CN109930042A CN 109930042 A CN109930042 A CN 109930042A CN 201910296640 A CN201910296640 A CN 201910296640A CN 109930042 A CN109930042 A CN 109930042A
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Abstract
The present invention relates to magnesium air battery magnesium-alloy anode material field, specifically a kind of magnesium-alloy anode materials and the preparation method and application thereof.The alloy anode material is by following weight percentage at being grouped as: 1 ~ 9% Al, 1 ~ 6% Ge, surplus be magnesium.For magnesium-alloy anode material of the invention by alloy element Al, the synergistic effect of Ge and solution treatment have obtained the excellent air cell anode material of comprehensive discharge performance.This magnesium-alloy anode material is 60 mAcm in current density‑2Under, the discharge potential measured by chronoptentiometry is average are as follows: -1.726 ~ -1.752V, discharging efficiency reach 70.9% ~ 74.1%.
Description
Technical field
The present invention relates to magnesium air battery magnesium-alloy anode material field, specifically a kind of magnesium-alloy anode material and its
Preparation method and application.
Background technique
Standard electrode EMF of the magnesium in acid and alkaline medium is not for -2.37V and -2.69V, the theoretical electrochemistry of magnesium
Equivalent is 2.20Ahg-1, therefore magnesium is a kind of ideal anode material in air cell.Magnesium air battery is a kind of novel
Semi-fuel cell, it using magnesium anode to react and discharging by the oxygen that cathode is spread in active material, with air,
Have many advantages, such as that at low cost, nontoxic, pollution-free, specific power is high, specific energy is high.Magnesium air battery as portable electrical power applications in
Various small-sized electronic products, such as mobile phone, electronic game machine, digital camera, laptop computer；It is used for as middle-size and small-size mobile power source
Buggy, such as electric car, fork truck, golf cart, battery-operated motor cycle, grass mower；As emergency stock power supply,
Such as emergency light.
But there is also some problems for magnesium anode material, magnesium alloy electric discharge activity is low, its standard is far not achieved in discharge potential
Electrode potential (- 2.37V vs SHE)；In electric discharge, there are self-corrosion evolving hydrogen reactions, cause utilization rate low；It is deposited when initial discharge
In " voltage delay " effect, cause start battery slow；Corrosion product is not easy to peel off when electric discharge, and guiding discharge activity is low, electric discharge
It is inefficient.
Therefore it is negative to design a kind of discharge potential, the high magnesium anode material of discharging efficiency is particularly important.
Summary of the invention
The present invention in order to solve problems existing for existing magnesium anode material, provide a kind of magnesium-alloy anode material and
Preparation method and application.
The present invention is achieved by the following technical solutions: a kind of magnesium-alloy anode material, the alloy anode material be by
Following weight percentage at being grouped as: 1~9% Al, 1~6% Ge, surplus are magnesium.
Invention further provides a kind of preparation methods of magnesium-alloy anode material, comprising the following steps:
(1) magnesium ingot, aluminium ingot are pre-processed respectively: removes the oxide and greasy dirt of magnesium ingot, aluminium ingot surface respectively, then passes through
After washes of absolute alcohol is clean, drying to constant weight under the conditions of at a temperature of 90 °C, that is, respectively obtains pretreated magnesium ingot, aluminium
Ingot；
(2) germanium grain is pre-processed: the oxide and greasy dirt on removal germanium grain surface, then it is clean through washes of absolute alcohol
Afterwards, drying to constant weight under the conditions of at a temperature of 90 °C to get pretreated germanium grain is arrived；
(3) pretreated magnesium ingot, aluminium ingot are placed in CO2And SF6700-760 is warming up in mixed gas protected smelting furnace
DEG C make its fusing；
(4) in 700-760 DEG C of heat preservation 25-35min after melting, then it is warming up to 770-800 DEG C, germanium grain is added, in CO2And SF6
Protection under and stir evenly, obtain fusant, keep the temperature 35-60min；
(5) fusant is cooled to 650-700 DEG C, cast after standing 10-20min, casting steel die is preparatory
It is heated to 200-300 DEG C, the ingot casting cooled to room temperature；
(6) ingot casting is put into high-temperature cabinet, is heated to 420 DEG C of heat preservations for 24 hours, taken out water hardening to room temperature, obtain magnesium
Alloy anode material.
Certainly, in the preparation process of magnesium-alloy anode material of the present invention, some impurity, Er Qiesuo will necessarily be brought into
Also can have impurity in magnesium ingot, aluminium ingot and the germanium grain used, thus magnesium-alloy anode material of the invention in addition to it is above-mentioned at
Point, it further include inevitable impurity, this is general knowledge known in this field.
As the further improvement of preparation method technical solution of the present invention, removal magnesium ingot, aluminium ingot surface oxide and
Before greasy dirt, magnesium ingot and aluminium ingot are cut into 100mm × 30mm × 20mm fritter.In this way convenient for removal magnesium ingot, the oxygen on aluminium ingot surface
Compound and greasy dirt, and facilitate fusing magnesium ingot and aluminium ingot.
As the further improvement of preparation method technical solution of the present invention, the germanium grain is technical grade purity or more.
Invention further provides a kind of application of the magnesium-alloy anode material in magnesium air battery.And it mentions
The magnesium-alloy anode material for having supplied a kind of preparation method of magnesium-alloy anode material to be prepared is in magnesium air battery
Application.
The beneficial effects of the present invention are:
1) add alloy element Al, can effectively improve the casting character and mechanical property of magnesium alloy, and Al element with
Magnesium will form uniform and dispersed distribution precipitated phase Mg17Al12, increase the active site of alloy, improve alloy electric discharge activity.
2) alloying element Ge is added, crystal grain can be refined and improve the overpotential of hydrogen evolution of magnesium alloy, its self-corrosion is inhibited to analyse
Hydrogen reaction.Ge element solubility in magnesium is lower simultaneously, can form a large amount of, equally distributed precipitated phase Mg with magnesium2Ge, Mg2Ge
Micro cell is formed with magnesium alloy substrate, galvanic corrosion occurs, improves alloy electric discharge activity.And Ge can be provided in the magnesium alloy
Volume energy density be 7.382Whcm-3, effectively promote alloy volume energy density.
3) by the alloy after solution treatment, Al element is completely dissolved in matrix, improves the activity of matrix.And with
The dissolution of Al element, the Ge element in matrix are all precipitated, and form more Mg2Ge phase increases more active sites, because
This electric discharge activity improves.
4) by alloy element Al, the synergistic effect of Ge and solution treatment are obtained magnesium-alloy anode material of the invention
Comprehensive discharge performance excellent air cell anode material.This magnesium-alloy anode material is 60mAcm in current density-2Under,
The discharge potential measured by chronoptentiometry are as follows: -1.726~-1.752V, discharging efficiency reach 70.9%~74.1%.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is magnesium-alloy anode material obtained in embodiment 1 in 30mAcm-2And 60mAcm-2Under current density
Constant current discharge curve graph.From figure 1 it appears that the magnesium-alloy anode material is in 30mAcm-2Under current density, electric discharge electricity
Position reaches -1.762V, in 60mAcm-2Discharge potential reaches -1.743V under current density, and discharge curve is steady, discharge potential
Negative, activity of discharging is strong.
Fig. 2 is the displaing micro tissue topography SEM figure of magnesium-alloy anode material obtained in embodiment 1.It can from Fig. 2
Out, the second phase in the magnesium-alloy anode material is evenly distributed, and electric discharge active site is more.
Fig. 3 is magnesium-alloy anode material obtained in embodiment 1 in 30mAcm-2And 60mAcm-2Current density
Lower constant current discharge 1200s, corrosion removal product post-etching shape appearance figure.From figure 3, it can be seen that the magnesium-alloy anode material discharges
Etch pit is evenly distributed, and corrosion product is easy to peel off.
Fig. 4 is magnesium-alloy anode material obtained in comparative example 1 in 30mAcm-2And 60mAcm-2Under current density
Constant current discharge curve graph.Figure 4, it is seen that the magnesium-alloy anode material of comparative example 1 is in 30mAcm-2And 60mA
cm-2Discharge potential calibration under current density, discharge curve fluctuation is larger, poor activity of discharging.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
Technical solution of the present invention is described in detail with reference to the accompanying drawing.
Embodiment 1
A kind of magnesium-alloy anode material, which is (mass percent): 6%Al, 1%Ge, remaining
Amount is magnesium.
The preparation method preparation method of the magnesium-alloy anode material, comprising the following steps:
(1) respectively to magnesium ingot, aluminium ingot, pre-process: magnesium ingot, aluminium ingot are cut into 100mm × 30mm × 20mm respectively
Fritter, and the oxide and greasy dirt on surface are removed according to a conventional method, then after washes of absolute alcohol is clean, at a temperature of 90 °C
Under the conditions of drying to constant weight, that is, respectively obtain pretreated magnesium ingot, aluminium ingot；
(2) germanium grain is pre-processed: germanium grain is removed to the oxide and greasy dirt on surface according to a conventional method, then through anhydrous second
After alcohol cleans up, drying to constant weight under the conditions of at a temperature of 90 °C to get pretreated germanium grain is arrived；
(3) pretreated magnesium ingot, aluminium ingot are placed in CO2And SF6750 DEG C are warming up in mixed gas protected smelting furnace makes
It is melted；
(4) in 750 DEG C of heat preservation 30min after melting, then 800 DEG C are warming up to, germanium grain are added, in CO2And SF6Protection under simultaneously
It stirs evenly, obtains fusant, keep the temperature 50min；
(5) fusant is cooled to 700 DEG C, cast after standing 10min, casting is previously heated to steel die
250 DEG C, the ingot casting cooled to room temperature；
(6) ingot casting is put into high-temperature cabinet, is heated to 420 DEG C of heat preservations for 24 hours, taken out water hardening to room temperature, obtain magnesium
Alloy anode material.
Embodiment 2
A kind of magnesium-alloy anode material, the alloy product is by following weight percentage (g/g) at being grouped as: 6%Al,
3%Ge, surplus are magnesium.
Preparation step such as embodiment 1.
Embodiment 3
A kind of magnesium-alloy anode material, the alloy product is by following weight percentage (g/g) at being grouped as: 6%Al,
5%Ge, surplus are magnesium.
Preparation step such as embodiment 1.
Comparative example 1
A kind of as-cast magnesium alloy anode material, the alloy product is by following weight percentage (g/g) at being grouped as: 6%
Al, 3%Ge, surplus are magnesium.
The step of preparation step such as embodiment 1 (1)-(5), does not carry out step (6).
Comparative example 2
A kind of as-cast magnesium alloy anode material, the alloy product is by following weight percentage (g/g) at being grouped as: 6%
Al, surplus are magnesium.
Preparation step such as comparative example 1.
Comparative example 3
A kind of as-cast magnesium alloy anode material, the alloy product is by following weight percentage (g/g) at being grouped as: 3%
Ge, surplus are magnesium.
Preparation step such as comparative example 1.
In above-described embodiment 1~3 and comparative example 1~3, magnesium ingot, aluminium ingot, germanium grain are technical grade purity or more.
Performance detection:
Finished product magnesium-alloy anode material made from Example 1~3 and comparative example 1~3 is tested for the property respectively, is surveyed
Strip part are as follows: room temperature (25 DEG C), 3.5wt% sodium chloride solution.
30mAcm is tested with chronoptentiometry-2And 60mAcm-2Constant current discharge averaged discharge electricity under current density
Position calculates discharging efficiency by electric discharge front and back mass loss.The results are shown in Table 1.
The discharge performance of the different magnesium-alloy anode materials of table 1
Embodiment 4
A kind of magnesium-alloy anode material, which is (mass percent): 1%Al, 6%Ge, remaining
Amount is magnesium.
The preparation method preparation method of the magnesium-alloy anode material, comprising the following steps:
(1) respectively to magnesium ingot, aluminium ingot, pre-process: magnesium ingot, aluminium ingot are cut into 100mm × 30mm × 20mm respectively
Fritter, and the oxide and greasy dirt on surface are removed according to a conventional method, then after washes of absolute alcohol is clean, at a temperature of 90 °C
Under the conditions of drying to constant weight, that is, respectively obtain pretreated magnesium ingot, aluminium ingot；
(2) germanium grain is pre-processed: germanium grain is removed to the oxide and greasy dirt on surface according to a conventional method, then through anhydrous second
After alcohol cleans up, drying to constant weight under the conditions of at a temperature of 90 °C to get pretreated germanium grain is arrived；
(3) pretreated magnesium ingot, aluminium ingot are placed in CO2And SF6700 DEG C are warming up in mixed gas protected smelting furnace makes
It is melted；
(4) in 760 DEG C of heat preservation 25min after melting, then 770 DEG C are warming up to, germanium grain are added, in CO2And SF6Protection under simultaneously
It stirs evenly, obtains fusant, keep the temperature 60min；
(5) fusant is cooled to 650 DEG C, cast after standing 20min, casting is previously heated to steel die
200 DEG C, the ingot casting cooled to room temperature；
(6) ingot casting is put into high-temperature cabinet, is heated to 420 DEG C of heat preservations for 24 hours, taken out water hardening to room temperature, obtain magnesium
Alloy anode material.
Embodiment 5
A kind of magnesium-alloy anode material, which is (mass percent): 9%Al, 6%Ge, remaining
Amount is magnesium.
The preparation method preparation method of the magnesium-alloy anode material, comprising the following steps:
(1) respectively to magnesium ingot, aluminium ingot, pre-process: magnesium ingot, aluminium ingot are cut into 100mm × 30mm × 20mm respectively
Fritter, and the oxide and greasy dirt on surface are removed according to a conventional method, then after washes of absolute alcohol is clean, at a temperature of 90 °C
Under the conditions of drying to constant weight, that is, respectively obtain pretreated magnesium ingot, aluminium ingot；
(2) germanium grain is pre-processed: germanium grain is removed to the oxide and greasy dirt on surface according to a conventional method, then through anhydrous second
After alcohol cleans up, drying to constant weight under the conditions of at a temperature of 90 °C to get pretreated germanium grain is arrived；
(3) pretreated magnesium ingot, aluminium ingot are placed in CO2And SF6760 DEG C are warming up in mixed gas protected smelting furnace makes
It is melted；
(4) in 700 DEG C of heat preservation 35min after melting, then 780 DEG C are warming up to, germanium grain are added, in CO2And SF6Protection under simultaneously
It stirs evenly, obtains fusant, keep the temperature 35min；
(5) fusant is cooled to 650 DEG C, cast after standing 20min, casting is previously heated to steel die
300 DEG C, the ingot casting cooled to room temperature；
(6) ingot casting is put into high-temperature cabinet, is heated to 420 DEG C of heat preservations for 24 hours, taken out water hardening to room temperature, obtain magnesium
Alloy anode material.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (7)
1. a kind of magnesium-alloy anode material, which is characterized in that the alloy anode material is by following weight percentage into grouping
At: 1 ~ 9% Al, 1 ~ 6% Ge, surplus are magnesium.
2. a kind of preparation method of magnesium-alloy anode material described in claim 1, which comprises the following steps:
(1) magnesium ingot, aluminium ingot are pre-processed respectively: removes the oxide and greasy dirt of magnesium ingot, aluminium ingot surface respectively, then through anhydrous
After ethyl alcohol cleans up, drying to constant weight under the conditions of at a temperature of 90 °C, that is, respectively obtains pretreated magnesium ingot, aluminium ingot；
(2) germanium grain is pre-processed: the oxide and greasy dirt on removal germanium grain surface, then after washes of absolute alcohol is clean,
Drying to constant weight under the conditions of at a temperature of 90 °C to get pretreated germanium grain is arrived；
(3) pretreated magnesium ingot, aluminium ingot are placed in CO2And SF6700-760 is warming up in mixed gas protected smelting furnace
DEG C make its fusing；
(4) in 700-760 DEG C of heat preservation 25-35 min after melting, then it is warming up to 770-800 DEG C, germanium grain is added, in CO2With
SF6Protection under and stir evenly, obtain fusant, keep the temperature 35-60 min；
(5) fusant is cooled to 650-700 DEG C, cast after standing 10-20 min, casting steel die adds in advance
Heat is to 200-300 DEG C, the ingot casting cooled to room temperature；
(6) ingot casting is put into high-temperature cabinet, is heated to 420 DEG C of heat preservations for 24 hours, taken out water hardening to room temperature, obtain magnesium alloy
Anode material.
3. a kind of preparation method of magnesium-alloy anode material according to claim 2, which is characterized in that removal magnesium ingot,
Before the oxide and greasy dirt on aluminium ingot surface, magnesium ingot and aluminium ingot are cut into 100mm × 30mm × 20mm fritter.
4. a kind of preparation method of magnesium-alloy anode material according to claim 2 or 3, which is characterized in that the germanium grain
For technical grade purity or more.
5. a kind of application of the magnesium-alloy anode material described in claim 1 in magnesium air battery.
6. the magnesium-alloy anode material that a kind of preparation method of magnesium-alloy anode material described in claim 2 or 3 is prepared
Application in magnesium air battery.
7. the magnesium-alloy anode material that a kind of preparation method of magnesium-alloy anode material as claimed in claim 4 is prepared is in magnesium
Application in air cell.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110048129A (en) * | 2019-03-18 | 2019-07-23 | 深圳清华大学研究院 | Metal-air battery metal electrode material and its preparation method and application |
| CN110380045A (en) * | 2019-07-24 | 2019-10-25 | 易航时代(北京)科技有限公司 | A kind of magnesium-alloy anode material and its preparation method and application, magnesium air battery |
| CN111394631A (en) * | 2020-05-25 | 2020-07-10 | 太原理工大学 | Magnesium alloy and preparation method thereof |
| CN111575563A (en) * | 2020-05-25 | 2020-08-25 | 太原理工大学 | Magnesium alloy and preparation method and application thereof |
| CN111668502A (en) * | 2020-05-29 | 2020-09-15 | 烟台南山学院 | Magnesium alloy anode material, preparation method and application thereof, and magnesium air battery |
| CN114107771A (en) * | 2021-11-30 | 2022-03-01 | 东北大学 | Anode material suitable for high-power magnesium air battery at low temperature and preparation method thereof |
-
2019
- 2019-04-14 CN CN201910296640.4A patent/CN109930042A/en active Pending
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| LIU XIAODA, ET AL.: "Corrosion Behavior of the As-Cast and As-Solid Solution Mg-Al-Ge Alloy", 《MATERIALS (BASEL, SWITZERLAND)》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110048129A (en) * | 2019-03-18 | 2019-07-23 | 深圳清华大学研究院 | Metal-air battery metal electrode material and its preparation method and application |
| CN110380045A (en) * | 2019-07-24 | 2019-10-25 | 易航时代(北京)科技有限公司 | A kind of magnesium-alloy anode material and its preparation method and application, magnesium air battery |
| CN110380045B (en) * | 2019-07-24 | 2021-02-05 | 易航时代(北京)科技有限公司 | Magnesium alloy anode material, preparation method and application thereof, and magnesium air battery |
| CN111394631A (en) * | 2020-05-25 | 2020-07-10 | 太原理工大学 | Magnesium alloy and preparation method thereof |
| CN111575563A (en) * | 2020-05-25 | 2020-08-25 | 太原理工大学 | Magnesium alloy and preparation method and application thereof |
| CN111668502A (en) * | 2020-05-29 | 2020-09-15 | 烟台南山学院 | Magnesium alloy anode material, preparation method and application thereof, and magnesium air battery |
| CN114107771A (en) * | 2021-11-30 | 2022-03-01 | 东北大学 | Anode material suitable for high-power magnesium air battery at low temperature and preparation method thereof |
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Application publication date: 20190625 |