CN108193110A - A kind of preparation method of magnesium-alloy anode material - Google Patents
A kind of preparation method of magnesium-alloy anode material Download PDFInfo
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- CN108193110A CN108193110A CN201810067334.9A CN201810067334A CN108193110A CN 108193110 A CN108193110 A CN 108193110A CN 201810067334 A CN201810067334 A CN 201810067334A CN 108193110 A CN108193110 A CN 108193110A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F13/00—Inhibiting corrosion of metals by anodic or cathodic protection
- C23F13/02—Inhibiting corrosion of metals by anodic or cathodic protection cathodic; Selection of conditions, parameters or procedures for cathodic protection, e.g. of electrical conditions
- C23F13/06—Constructional parts, or assemblies of cathodic-protection apparatus
- C23F13/08—Electrodes specially adapted for inhibiting corrosion by cathodic protection; Manufacture thereof; Conducting electric current thereto
- C23F13/12—Electrodes characterised by the material
- C23F13/14—Material for sacrificial anodes
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Abstract
The invention discloses a kind of preparation method of magnesium-alloy anode material, including annealing process, which is characterized in that described to be annealed into homogenizing annealing.The present invention, using homogenizing annealing, promotes Mg when preparing magnesium-alloy anode material17Al12The peeling of phase, and make magnesium matrix and Al8Mn5The composition of particle is relatively uniform, and then promotes discharge process, improves the electro-chemical activity of magnesium-alloy anode material.
Description
Technical field
The present invention relates to anode material technical fields, and in particular to a kind of preparation method of magnesium-alloy anode material.
Background technology
Magnesium alloy is due to active high, and cell voltage is high, and voltage range is wide, and power density is high, and density is relatively low, electrode potential
It is low, the features such as long lifespan, have been developed that as the anode material used in seawater, such as sonar buoy, beacon, emergency set, gas
Bag battery and life vest.AP65 is one of magnesium anode Mg-6%Al-5%Pb (mass fraction) main component.It is reported that aluminium can be with
Surface-active of the magnesium alloy in sodium chloride solution is improved, and influences the corrosion resistance of magnesium alloy.Although lead is not environmentally, magnesium alloy
Activity can also increase with the addition of lead.
Udhayan etc. [R.Udhayan, D.P.Bhatt, J.Power.Sources.63 (1996) 105-110.] has studied
The electrochemical behavior of AP65 anodes in the magnesium perchlorate solution of various concentration finds its electrode/electrolyte interface process by activating
Control reaction determines.For the magnesium anode used in seawater battery system, chemical property is considerable.Magnesium alloy shows
Go out strong electro-chemical activity and thermodynamics bears average potential.However, since corrosion product is covered in anode surface, cause to postpone
Reach stable state and reduce discharge rate, so the significant reduction of their negative potential.
The electric discharge of AP65 anodes is active to be determined by forming for magnesium matrix with the property of the second phase, and second in as cast condition anode
Phase Mg17Al12It meets and hinders discharge process, reduce electric discharge activity.
Invention content
Technical problems based on background technology, the present invention propose a kind of preparation method of magnesium-alloy anode material,
To realize the purpose for improving magnesium-alloy anode material electro-chemical activity.
A kind of preparation method of magnesium-alloy anode material proposed by the present invention, it is described to be annealed into uniformly including annealing process
Annealing.
Preferably, the preparation method includes the following steps：
S1, after pure magnesium is melted in resistance furnace in the atmosphere of argon gas, alloying element is added in, kept the temperature, stirring is melted
Melt state alloy；
S2, by molten state alloy pour into rectangle steel mold preheat founding into casting postcooling to room temperature, in resistance furnace
After homogenizing annealing, water quenching is polished, and is polished, and is cleaned, dry, obtains magnesium-alloy anode material.
Preferably, in S1, the purity of pure magnesium for 99.99% and more than.
Preferably, in S1, alloying element includes fine aluminium, pure lead and Al-30%Mn alloys.
Preferably, the purity of fine aluminium for 99.99% and more than.
Preferably, the purity of pure lead for 99.99% and more than.
Preferably, in S1, alloying element is added at a temperature of 500-1000 DEG C.
Preferably, in S1, the temperature of heat preservation is 500-1000 DEG C, time 10-20min.
Preferably, in S1, the time of stirring is 1-10min.
Preferably, in S2, the temperature of preheating is 100-300 DEG C.
Preferably, in S2, homogenizing annealing carries out in the atmosphere of rare gas.
Preferably, homogenizing annealing carries out in the atmosphere of argon gas.
Preferably, in S2, the temperature of homogenizing annealing is 300-1000 DEG C, time 1-72h.
Preferably, it in S2, is polished using SiC sand paper.
Preferably, it in S2, is polished using 0.2-1 μm of diamond slurry.
Preferably, in S2, cleaning is cleaned using EtOH Sonicate.
Preferably, it is dry to be dried using cold air in S2.
Used equipment has no special limitation when the present invention melts magnesium pure in step 1, using people in the art
Equipment known to member；The present invention is preferably resistance furnace.
The present invention has no special limitation to the equipment that founding into casting are preheated in step 2, using those skilled in the art
Well known equipment；The preferably rectangular steel mold of the present invention, and carry out in molten state alloy toppling process sulphur dusting with
It avoids burning and reduces oxidation.
The present invention has no the equipment of homogenizing annealing in step 2 special limitation, using known to those skilled in the art
Equipment；The present invention is preferably resistance furnace.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is when preparing magnesium-alloy anode material using equal
Annealing is homogenized, promotes Mg17Al12The peeling of phase, and make magnesium matrix and Al8Mn5The composition of particle is relatively uniform, and then promotes electric discharge
Process improves the electro-chemical activity of magnesium-alloy anode material.
Description of the drawings
Fig. 1 is XRD testing result comparison diagrams in test example 1 of the present invention.
Fig. 2 is electrochemical impedance spectroscopy testing result comparison diagram in test example 2 of the present invention.
Fig. 3 is electron-microscope scanning result schematic diagram in test example 2 of the present invention.
Specific embodiment
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of magnesium-alloy anode material, it is described to be annealed into homogenizing annealing including annealing process.
Embodiment 2
A kind of preparation method of magnesium-alloy anode material, it is described to be annealed into homogenizing annealing including annealing process；
Wherein, the preparation method includes the following steps：
S1, after pure magnesium is melted in resistance furnace in the atmosphere of argon gas, alloying element is added in, kept the temperature, stirring is melted
Melt state alloy；
S2, by molten state alloy pour into rectangle steel mold preheat founding into casting postcooling to room temperature, in rare gas
Atmosphere in, in resistance furnace after homogenizing annealing, water quenching, the polishing of SiC sand paper, the polishing of 0.2-1 μm of diamond slurry, ethyl alcohol surpasses
Sound cleans, and cold air drying obtains magnesium-alloy anode material；
In S1, the purity of pure magnesium for 99.99% and more than；
In S1, alloying element includes fine aluminium, pure lead and Al-30%Mn alloys；
The purity of fine aluminium for 99.99% and more than；
The purity of pure lead for 99.99% and more than；
In S1, alloying element is added at a temperature of 500 DEG C；
In S1, the temperature of heat preservation is 500 DEG C, time 10min；
In S1, the time of stirring is 1min；
In S2, the temperature of preheating is 300 DEG C；
In S2, the temperature of homogenizing annealing is 300 DEG C, time 72h.
Embodiment 3
A kind of preparation method of magnesium-alloy anode material, it is described to be annealed into homogenizing annealing including annealing process；
Wherein, the preparation method includes the following steps：
S1, after pure magnesium is melted in resistance furnace in the atmosphere of argon gas, alloying element is added in, kept the temperature, stirring is melted
Melt state alloy；
S2, by molten state alloy pour into rectangle steel mold preheat founding into casting postcooling to room temperature, in rare gas
Atmosphere in, in resistance furnace after homogenizing annealing, water quenching, the polishing of SiC sand paper, the polishing of 0.2-1 μm of diamond slurry, ethyl alcohol surpasses
Sound cleans, and cold air drying obtains magnesium-alloy anode material；
In S1, the purity of pure magnesium for 99.99% and more than；
In S1, alloying element includes fine aluminium, pure lead and Al-30%Mn alloys；
The purity of fine aluminium for 99.99% and more than；
The purity of pure lead for 99.99% and more than；
In S1, alloying element is added at a temperature of 1000 DEG C；
In S1, the temperature of heat preservation is 1000 DEG C, time 20min；
In S1, the time of stirring is 10min；
In S2, the temperature of preheating is 100 DEG C；
In S2, the temperature of homogenizing annealing is 1000 DEG C, time 1h.
Embodiment 4
A kind of preparation method of magnesium-alloy anode material, it is described to be annealed into homogenizing annealing including annealing process；
Wherein, the preparation method includes the following steps：
S1, after pure magnesium is melted in resistance furnace in the atmosphere of argon gas, alloying element is added in, kept the temperature, stirring is melted
Melt state alloy；
S2, by molten state alloy pour into rectangle steel mold preheat founding into casting postcooling to room temperature, in rare gas
Atmosphere in, in resistance furnace after homogenizing annealing, water quenching, the polishing of SiC sand paper, the polishing of 0.2-1 μm of diamond slurry, ethyl alcohol surpasses
Sound cleans, and cold air drying obtains magnesium-alloy anode material；
In S1, the purity of pure magnesium for 99.99% and more than；
In S1, alloying element includes fine aluminium, pure lead and Al-30%Mn alloys；
The purity of fine aluminium for 99.99% and more than；
The purity of pure lead for 99.99% and more than；
In S1, alloying element is added at a temperature of 600 DEG C；
In S1, the temperature of heat preservation is 600 DEG C, time 15min；
In S1, the time of stirring is 5min；
In S2, the temperature of preheating is 200 DEG C；
In S2, the temperature of homogenizing annealing is 400 DEG C, and the time is for 24 hours.
Embodiment 5
A kind of preparation method of magnesium-alloy anode material, it is described to be annealed into homogenizing annealing including annealing process；
Wherein, the preparation method includes the following steps：
S1, after pure magnesium is melted in resistance furnace in the atmosphere of argon gas, alloying element is added in, kept the temperature, stirring is melted
Melt state alloy；
S2, by molten state alloy pour into rectangle steel mold preheat founding into casting postcooling to room temperature, in rare gas
Atmosphere in, in resistance furnace after homogenizing annealing, water quenching, the polishing of SiC sand paper, the polishing of 0.2-1 μm of diamond slurry, ethyl alcohol surpasses
Sound cleans, and cold air drying obtains magnesium-alloy anode material；
In S1, the purity of pure magnesium for 99.99% and more than；
In S1, alloying element includes fine aluminium, pure lead and Al-30%Mn alloys；
The purity of fine aluminium for 99.99% and more than；
The purity of pure lead for 99.99% and more than；
In S1, alloying element is added at a temperature of 600 DEG C；
In S1, the temperature of heat preservation is 600 DEG C, time 15min；
In S1, the time of stirring is 5min；
In S2, the temperature of preheating is 200 DEG C；
In S2, the temperature of homogenizing annealing is 400 DEG C, time 72h.
Test example 1
Casting and the obtained magnesium-alloy anode material of embodiment 4 and 5 before being made annealing treatment to embodiment 4 or 5 respectively into
Row XRD is detected, and is denoted as 1 group, 2 groups and 3 groups successively, testing result comparison diagram is as shown in Figure 1.
Test example 2
The magnesium-alloy anode material that casting and embodiment 4 and 5 before embodiment 4 or 5 is made annealing treatment obtain is as sun
Pole is detected respectively by the three-electrode system of standard, is denoted as a groups, b groups and c groups successively.
Detection method is as follows：
After 1. with 1200 mesh sand paper, anode surface is continuously polished, it is encapsulated in the epoxy resin of 10mm × 10mm, 25
DEG C glassware in be exposed to 100mL mass fractions be 3.5wt% sodium chloride solution in；
2. using platinum filament as to electrode, saturated calomel electrode (SCE) is as reference electrode.Sun is carried out with the speed of sweeping of 1mV/s
Pole polarization test, and test its electrochemical impedance spectroscopy (EIS)；Wherein potential-time curve is tested by constant current in 180mA/
cm2Anodic current density under continue 600s obtain.
3. after constant current experiment, anode from electrolytic cell is taken out, the corruption of corrosion product is checked by scanning electron microscope (SEM)
Surface is lost, to determine the second phase on the pattern and corrosion surface of corrosion surface.
The electrochemical impedance spectroscopy testing result comparison diagram of three groups of a groups, b groups and c groups is as shown in Fig. 2, the electron-microscope scanning knot of a groups
Fruit is as shown in Figure 3.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of magnesium-alloy anode material, including annealing process, which is characterized in that the homogenization that is annealed into is moved back
Fire.
2. the preparation method of magnesium-alloy anode material according to claim 1, which is characterized in that the preparation method is included such as
Lower step：
S1, after pure magnesium is melted in the atmosphere of argon gas, alloying element is added in, kept the temperature, stirring obtains molten state alloy；
S2, molten state alloy being preheated into founding into casting postcooling to room temperature, carries out homogenizing annealing, water quenching is polished, polishing,
Cleaning, it is dry, obtain magnesium-alloy anode material.
3. the preparation method of magnesium-alloy anode material according to claim 2, which is characterized in that in S1, the purity of pure magnesium is
99.99% and more than；Preferably, in S1, alloying element includes fine aluminium, pure lead and Al-30%Mn alloys；Preferably, fine aluminium
Purity for 99.99% and more than；Preferably, the purity of pure lead for 99.99% and more than.
4. the preparation method of magnesium-alloy anode material according to Claims 2 or 3, which is characterized in that in S1, in 500-1000
Alloying element is added at a temperature of DEG C.
5. according to the preparation method of any one of the claim 2-4 magnesium-alloy anode materials, which is characterized in that in S1, heat preservation
Temperature for 500-1000 DEG C, time 10-20min；Preferably, in S1, the time of stirring is 1-10min.
6. according to the preparation method of any one of the claim 2-5 magnesium-alloy anode materials, which is characterized in that in S2, preheating
Temperature be 100-300 DEG C.
7. according to the preparation method of any one of claims 1 or 2-6 magnesium-alloy anode material, which is characterized in that in S2,
Annealing is homogenized to carry out in the atmosphere of rare gas；Preferably, homogenizing annealing carries out in the atmosphere of argon gas；Preferably, S2
In, the temperature of homogenizing annealing is 300-1000 DEG C, time 1-72h.
8. according to the preparation method of any one of the claim 2-7 magnesium-alloy anode materials, which is characterized in that in S2, use
SiC sand paper is polished.
9. according to the preparation method of any one of the claim 2-8 magnesium-alloy anode materials, which is characterized in that in S2, use
0.2-1 μm of diamond slurry is polished.
10. according to the preparation method of any one of the claim 2-9 magnesium-alloy anode materials, which is characterized in that in S2, cleaning
It is cleaned using EtOH Sonicate；Preferably, it is dry to be dried using cold air in S2.
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| CN201810067334.9A CN108193110A (en) | 2018-01-24 | 2018-01-24 | A kind of preparation method of magnesium-alloy anode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114908278A (en) * | 2021-02-08 | 2022-08-16 | 通用汽车环球科技运作有限责任公司 | Magnesium alloy and forged component |
| CN115637434A (en) * | 2022-10-20 | 2023-01-24 | 常州大学 | Aluminum sacrificial anode alloy and preparation method thereof |
-
2018
- 2018-01-24 CN CN201810067334.9A patent/CN108193110A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 张俊昌，冯艳，王乃光，杨明: "挤压比对海水激活电池用AP65镁合金阳极材料放电性能的影响", 《有色金属科学与工程》 * |
| 王日初,王乃光,彭超群,曾苏民: "Mn对海水激活电池用AP65镁合金阳极材料电化学性能的影响", 《有色金属科学与工程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114908278A (en) * | 2021-02-08 | 2022-08-16 | 通用汽车环球科技运作有限责任公司 | Magnesium alloy and forged component |
| US11987864B2 (en) | 2021-02-08 | 2024-05-21 | GM Global Technology Operations LLC | Magnesium alloy and forged component |
| CN115637434A (en) * | 2022-10-20 | 2023-01-24 | 常州大学 | Aluminum sacrificial anode alloy and preparation method thereof |
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