CN112647001A - AZ31M alloy and preparation method and application thereof - Google Patents
AZ31M alloy and preparation method and application thereof Download PDFInfo
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- CN112647001A CN112647001A CN202011512655.9A CN202011512655A CN112647001A CN 112647001 A CN112647001 A CN 112647001A CN 202011512655 A CN202011512655 A CN 202011512655A CN 112647001 A CN112647001 A CN 112647001A
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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
- 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
Abstract
The invention relates to an AZ31M alloy, which is characterized in that the alloy components are represented by the mass percentage of Mg-3Al-1Zn-xM, wherein x is 0,0.3,0.5,0.7,0.9,1.1 and 1.3 wt%, Mg is 94.7% -95.7%, Al is 3%, Zn is 1% and M is 0.3% -1.3%, and the preparation method of the AZ31M alloy adopts an RLL-1100 light alloy smelting furnace, is convenient to operate and simple in process, and the weight loss ratio of a magnesium alloy anode of the AZ31M alloy to the cathode protection of carbon steel after 60 days of operation is only 0.57%, the protection effect is obvious, and the AZ31M has better protection effect and better current efficiency in all magnesium anodes.
Description
Technical Field
The invention relates to the field of alloy materials, in particular to an AZ31M alloy and a preparation method and application thereof.
Background
In an electric power system, in order to ensure the safe operation of a transformer substation, a grounding device needs to be buried in soil, but the grounding device is subjected to serious natural corrosion, the forced corrosion of an alternating current/direct current grounding device is more serious with the increase of the electric power capacity of China in recent years, and serious electric power safety accidents caused by the corrosion of a grounding grid frequently occur in China. There are many methods for preventing corrosion of metals, mainly for improving corrosion resistance of metals themselves, coating methods, treatment methods of corrosive media, and cathodic protection methods. The cathodic protection achieves the metal anticorrosion effect by externally adding current or a sacrificial anode, wherein the sacrificial anode method has the advantages of small interference on adjacent structures, no need of an external power supply, uniform protection current distribution, simple and convenient construction and the like, is applied to the protection of metal structures in soil, fresh water and marine environments, and plays an increasingly important role. Therefore, the demand for sacrificial anode materials in the market is also steadily increasing.
The commonly used magnesium-based sacrificial anode alloy systems are AZ (Mg-Al-Zn) series and AK (Mg-Zn-Zr) series, and compared with the AK series, the AZ series magnesium alloy has the advantages of large effective capacitance, negative electrode potential and the like, and is suitable for cathodic protection in fresh water and high-resistivity soil. However, in the case of AZ series magnesium anodes, certain elements (such as elements with low oxygen evolution overpotential) in the alloy promote the autolysis of magnesium in a corrosion medium, and impurity elements such as Fe, Ni, Cu, etc. existing in the smelting process can serve as cathode phases to accelerate the formation of micro-galvanic corrosion, thereby reducing the current efficiency. For the reasons, the existing magnesium-based sacrificial anode cannot well play a role in corrosion resistance on metal materials.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention adds a certain amount of alloy elements into magnesium to weaken the adverse effect of impurity elements, discusses the influence of an organization structure, a corrosion potential, current efficiency, grain refinement and the like on the performance of the Mg-Al-based sacrificial anode from the aspect of thermodynamics, thereby achieving the bridging among component design, a microstructure, performance and a preparation process, further achieving the prediction and design from a material microstructure to a macroscopic performance, developing the AZ31M alloy with high efficiency and low energy consumption, providing a preparation method of the AZ31M alloy, and providing the specific application of the AZ31M alloy.
One of the specific technical schemes adopted for realizing the invention is as follows: the AZ31M alloy is characterized in that the expression of each element of the alloy composition by mass percent is Mg-3Al-1Zn-xM, wherein x is 0,0.3,0.5,0.7,0.9,1.1 and 1.3 wt%, Mg is 94.7-95.7%, Al is 3%, Zn is 1% and M is 0.3-1.3%.
Preferably, the alloy comprises the following elements in percentage by mass: 94.9%, Al: 3%, Zn: 1%, M: 1.1 percent.
The second concrete technical scheme adopted by the invention is as follows: the preparation method of the AZ31M alloy adopts an RLL-1100 light alloy smelting furnace for preparation, and specifically comprises the following steps:
1) adopting a CALPHAD method, calculating a vertical cross section diagram of a Mg-Al binary, AZ ternary and AZ31+ xM quaternary alloy by using Thermo-calc software according to a TCS Mg-based alloy Datebase 3.0 database, preliminarily drafting components, calculating the relative content and distribution of each phase, determining the transformation and the components of each phase of the alloy with the drafted components in the solidification process, finally determining the distribution condition of each phase in the alloy at room temperature, wherein the atomic percentage expression of the alloy components is AZ31M, converting the atomic percentages of the determined raw materials into mass ratios, and respectively weighing the raw materials, including pure magnesium: 99.99%, pure aluminum: 99.99%, pure zinc: 99.99% and Mg-25M master alloy;
2) polishing the surface of the cut magnesium block to remove an oxide film on the surface of the magnesium block, cleaning a crucible for smelting, and then putting magnesium alloy and a covering agent into the crucible, wherein the covering agent is MgCl2: KCl 1: 1, putting the crucible into an oven, and drying at the temperature of 80 ℃ for 30 min; opening a ventilation valve and injecting carbon dioxide protective gas 5min before smelting; 1min before smelting, opening a circulating cooling water valve;
3) opening a light alloy smelting furnace, ascending a furnace cover, moving the furnace body leftwards, stably placing the dried crucible into the furnace, placing a magnesium ingot into the middle position of the crucible, uniformly covering a covering agent around the magnesium ingot, moving the furnace body rightwards, and descending the furnace cover;
4) rapidly heating to 720 ℃ at a heating speed of 10 ℃/min, opening the furnace body after the magnesium alloy is melted, adding the dried alloying elements by using a dosing spoon, and reducing the furnace body;
5) starting a stirring device to uniformly disperse the elements Al and Zn in the alloy liquid, stirring for 3min, continuously heating to 750 ℃, and preserving heat for 30 min;
6) and (5) turning off the power supply, and naturally cooling the furnace body to finish smelting.
The third concrete technical scheme adopted by the invention is as follows: an AZ31M alloy, characterized in that the magnesium anode of the AZ31M alloy is used for cathodic protection of carbon steel.
The AZ31M alloy and the preparation method and the application thereof have the beneficial effects that:
1. the AZ31M alloy has different component contents, directly influences the microstructure of the alloy and further influences the electrochemical performance of the alloy, Al mainly exists in the magnesium alloy in the form of intermetallic compounds, can form a micro couple with a close-packed hexagonal (hcp) matrix to promote the occurrence of corrosion, precipitates during solid solution to strengthen the magnesium alloy, and the intermetallic compounds at the grain boundary block the corrosion of the hcp matrix; zn has higher activity and more negative potential, and can improve the comprehensive performance of the magnesium anode; m exists mainly in the form of orthorhombic solid solution, a small amount of orthorhombic solid solution can be used as a cathode phase to accelerate corrosion, and can also cooperate with intermetallic compounds to inhibit corrosion;
2. a preparation method of AZ31M alloy adopts an RLL-1100 light alloy smelting furnace, and has convenient operation and simple process;
3. after the application of the magnesium alloy anode of the AZ31M alloy to the cathodic protection of carbon steel, the weight loss ratio of the magnesium alloy anode of the AZ31M alloy after 60 days of operation is only 0.57 percent, and the weight loss rate of a steel sheet in cathodic protection of the anode to a Q235 stainless steel test piece is only 0.0033 g/(m)2H), the protective effect is obvious, and the protective effect of AZ31M is more effective in all magnesium anodesGood and has better current efficiency.
Drawings
Figure 1 is an AZ31+ xM (a-g x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%, respectively) XRD pattern;
fig. 2 is a tissue morphology of AZ31+ xM (a-g, x is 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%);
fig. 3 is a graph of the self-etching discharge rate of AZ31+ xM (x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%) in a 0.62mol/l nacl solution;
fig. 4 is a plot of the self-etching discharge rate of AZ31+ xM (x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%) in a 0.62mol/LNa2SO4 solution;
fig. 5 is a polarization curve of AZ31+ xM (x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%) in a 0.62mol/l nacl solution;
fig. 6 is a polarization curve of AZ31+ xM (x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%) in a 0.62mol/LNa2SO4 solution;
FIG. 7 is a schematic view of a partitioned soil box;
FIG. 8 is a schematic view of a bagged sacrificial anode installation.
Detailed Description
The present invention will be described in further detail with reference to the accompanying fig. 1-8 and the specific embodiments described herein, which are provided for illustration only and are not intended to limit the present invention.
Example 1:
in this example, the AZ31M alloy includes the following elements by mass percent, Mg: 94.9%, Al: 3%, Zn: 1%, M: 1.1 percent.
Respectively weighing raw materials comprising pure magnesium: 99.99%, pure aluminum: 99.99%, pure zinc: 99.99% and Mg-25M master alloy;
polishing the surface of the cut magnesium block, removing an oxide film on the surface of the magnesium block, cleaning a crucible for smelting, and then putting a magnesium alloy and a covering agent into the crucible: MgCl2: KCl 1: 1, putting the crucible into an oven, and drying at the temperature of 80 ℃ for 30 min; opening a ventilation valve and injecting carbon dioxide protective gas 5min before smelting; 1min before smelting, opening a circulating cooling water valve;
opening a light alloy smelting furnace, ascending a furnace cover, moving the furnace body leftwards, stably placing the dried crucible into the furnace, placing a magnesium ingot into the middle position of the crucible, uniformly covering a covering agent around the magnesium ingot, moving the furnace body rightwards, and descending the furnace cover;
rapidly heating to 720 ℃ at a heating speed of 10 ℃/min, opening the furnace body after the magnesium alloy is melted, adding the dried alloying elements by using a dosing spoon, and reducing the furnace body;
starting a stirring device to uniformly disperse the elements Al and Zn in the alloy liquid, stirring for 3min, continuously heating to 750 ℃, and preserving heat for 30 min;
and (5) turning off the power supply, and naturally cooling the furnace body to finish smelting.
Example 2:
in this example, the AZ31M alloy includes the following elements by mass percent, Mg: 95.7%, Al: 3%, Zn: 1%, M: 0.3 percent.
Respectively weighing raw materials comprising pure magnesium: 99.99%, pure aluminum: 99.99%, pure zinc: 99.99% and Mg-25M master alloy;
polishing the surface of the cut magnesium block, removing an oxide film on the surface of the magnesium block, cleaning a crucible for smelting, and then putting a magnesium alloy and a covering agent into the crucible: MgCl2: KCl 1: 1, putting the crucible into an oven, and drying at the temperature of 80 ℃ for 30 min; opening a ventilation valve and injecting carbon dioxide protective gas 5min before smelting; 1min before smelting, opening a circulating cooling water valve;
opening a light alloy smelting furnace, ascending a furnace cover, moving the furnace body leftwards, stably placing the dried crucible into the furnace, placing a magnesium ingot into the middle position of the crucible, uniformly covering a covering agent around the magnesium ingot, moving the furnace body rightwards, and descending the furnace cover;
rapidly heating to 720 ℃ at a heating speed of 10 ℃/min, opening the furnace body after the magnesium alloy is melted, adding the dried alloying elements by using a dosing spoon, and reducing the furnace body;
starting a stirring device to uniformly disperse the elements Al and Zn in the alloy liquid, stirring for 3min, continuously heating to 750 ℃, and preserving heat for 30 min;
and (5) turning off the power supply, and naturally cooling the furnace body to finish smelting.
Example 3:
in this example, the AZ31M alloy includes the following elements by mass percent, Mg: 94.7%, Al: 3%, Zn: 1%, M: 1.3 percent.
Respectively weighing raw materials comprising pure magnesium: 99.99%, pure aluminum: 99.99%, pure zinc: 99.99% and Mg-25M master alloy;
polishing the surface of the cut magnesium block, removing an oxide film on the surface of the magnesium block, cleaning a crucible for smelting, and then putting a magnesium alloy and a covering agent into the crucible: MgCl2: KCl 1: 1, putting the crucible into an oven, and drying at the temperature of 80 ℃ for 30 min; opening a ventilation valve and injecting carbon dioxide protective gas 5min before smelting; 1min before smelting, opening a circulating cooling water valve;
opening a light alloy smelting furnace, ascending a furnace cover, moving the furnace body leftwards, stably placing the dried crucible into the furnace, placing a magnesium ingot into the middle position of the crucible, uniformly covering a covering agent around the magnesium ingot, moving the furnace body rightwards, and descending the furnace cover;
rapidly heating to 720 ℃ at a heating speed of 10 ℃/min, opening the furnace body after the magnesium alloy is melted, adding the dried alloying elements by using a dosing spoon, and reducing the furnace body;
starting a stirring device to uniformly disperse the elements Al and Zn in the alloy liquid, stirring for 3min, continuously heating to 750 ℃, and preserving heat for 30 min;
and (5) turning off the power supply, and naturally cooling the furnace body to finish smelting.
Firstly, the structural characteristics of the alloy are as follows:
as can be seen from fig. 1, from the XRD pattern of AZ31+ xM (a-g is x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%, respectively), it can be seen that the as-cast structure of the AZ31 magnesium alloy without the addition of rare earth M is hcp matrix phase and intermetallic compound at room temperature; the as-cast structure at room temperature after addition of the M element was mainly hcp matrix phase, intermetallic compound and orthorhombic solid solution, which is consistent with the results of thermodynamic calculations, wherein no MgAlZn phase was detected, probably as a result of solid dissolution of this phase in the hcp matrix phase when the Zn content was too low.
As shown in fig. 2, it can be seen that the AZ31M alloy prepared by the present invention has the clearest equiaxed crystal characteristics, the smallest alloy grain size, and the more uniform new phase distribution from the texture map of AZ31+ xM (a-g is x ═ 0,0.3,0.5,0.7,0.9,1.1,1.3 wt.%); wherein the dark color dendritic crystal is an intermetallic compound, the bright part is an hcp matrix, new phases appearing in the crystal grains are orthogonal solid solution and MgAlZn phase, and the composition and distribution of the alloy phase are basically consistent with the thermodynamic calculation result at room temperature.
II, alloy corrosion test condition:
as can be seen from FIG. 3, the self-etching discharge rate curves of the examples in 0.62mol/L NaCl solution show that AZ31+0.7M and AZ31+1.1M have lower self-etching rates and higher current efficiency as anode materials.
As can be seen from FIG. 4, the molar ratio is 0.62mol/LNa2SO4As can be seen from the self-corrosion discharge rate curve in the solution, the AZ31+ xM corrosion rate is obviously reduced in the first 24h, the corrosion rate tends to be stable in a certain range after 24h, and AZ31+0.7M, AZ31+0.9M and AZ31M have lower self-discharge rates, so that the self-corrosion discharge rate curve in Na2SO4The self-loss of the solution is low.
Polarization curve of alloy:
as can be seen from FIGS. 5 and 6, the concentration of Na in the solution was 0.62mol/L NaCl/Na, respectively2SO4The polarization curve in the solution shows that the corrosion current starts to increase when the M content is 0.3 wt.% and 0.5 wt.%, and the self-corrosion current of the alloy starts to decrease when the M element reaches 7 wt.%, and that the self-corrosion rate of the anode is the lowest when the M is added at 1.1 wt.%, indicating that the current efficiency of the alloy is the highest and the degree of wear is the lowest when the alloy is used as a sacrificial anode. Therefore, when the content of M is 0.7 to 1.3 wt.%, the electrochemical performance of the AZ31 magnesium alloy sacrificial anode can be improved to a certain extent.
Thirdly, testing the practical application of the alloy in soil:
fig. 7 is a partition type soil box, fig. 8 is a schematic view of installation of the bagged sacrificial anode, and the installation includes the following notes:
(1) and (3) taking out weeds and sundries on the surface coating by using a shovel, taking out soil 20cm below the ground surface, and taking out the soil with the resistivity meeting the requirement and putting the soil into a partition type soil box.
(2) And filing a groove on the periphery of the polished test piece by using a file, wherein the depth of the groove is 2mm, and the position of the groove is the upper half part of the test piece. And extruding a copper wire into the groove, heating the electric soldering iron, connecting the copper wire with the polished small test piece by taking tin as an adhesion medium, and requiring no gap between the copper wire and the metal in the groove.
(3) When the magnesium anode is installed in soil, the bare anode cannot be directly put into the soil, and a filling material with the capacities of activating the anode, retaining water and the like is arranged around the bare anode.
(4) The welded magnesium anode is filled in a filler bag, and in order to ensure that the anode and the filler thereof are fully contacted with soil, the filler bag needs to be a cotton bag or a jute bag with good permeability. The magnesium anode is positioned in the center of the cotton bag, and the filler with the components of the formula shown in the table 1 is added around the magnesium anode, wherein the adding thickness is 30 mm.
TABLE 1
(5) Digging an anode arrangement pit in a sectional type soil box, packaging the bagged magnesium anode as a whole, installing the packaged magnesium anode in the anode arrangement pit, and backfilling and compacting soil after the anode is in place.
(6) Pouring 200mL of water at the arrangement positions of the three groups of anodes, leading out the leads, inserting the leads into the protected Q235 stainless steel fixing holes for winding and fixing, burying the stainless steel sheets in soil for 20cm, and adding a layer of preservative film on the upper part of the soil box in order to keep the soil in the soil box to keep a relatively stable environment, thereby ensuring that the soil has a relatively stable water content.
Magnesium alloy anode-to-carbon of AZ31M alloy prepared by the inventionThe weight loss ratio of the steel sheet in the cathodic protection of the steel after 60 days of operation is only 0.57 percent, and the weight loss rate of the steel sheet in the cathodic protection of the anode to Q235 stainless steel test piece is only 0.0033 g/(m)2H), the protective effect is obvious. Of all magnesium anodes, AZ31M was more effective in protection and had better current efficiency.
The foregoing is considered as illustrative and not restrictive of the preferred forms of the invention, and it is understood that various changes and modifications may be made therein by those skilled in the art without departing from the spirit of the invention, and equivalents thereof are to be considered within the scope of the invention.
Claims (4)
1. The AZ31M alloy is characterized in that the expression of each element of the alloy composition by mass percent is Mg-3Al-1Zn-xM, wherein x is 0,0.3,0.5,0.7,0.9,1.1 and 1.3 wt%, Mg is 94.7-95.7%, Al is 3%, Zn is 1% and M is 0.3-1.3%.
2. The AZ31M alloy of claim 1, wherein the alloy comprises the following elements in mass percent, Mg: 94.9%, Al: 3%, Zn: 1%, M: 1.1 percent.
3. The AZ31M alloy of claim 1 or 2, wherein the preparation method is performed by using an RLL-1100 light alloy melting furnace, and comprises the following steps:
1) adopting a CALPHAD method, calculating a vertical cross section diagram of a Mg-Al binary, AZ ternary and AZ31+ xM quaternary alloy by using Thermo-calc software according to a TCS Mg-based alloy Datebase 3.0 database, preliminarily drafting components, calculating the relative content and distribution of each phase, determining the transformation and the components of each phase of the alloy with the drafted components in the solidification process, finally determining the distribution condition of each phase in the alloy at room temperature, wherein the atomic percentage expression of the alloy components is AZ31M, converting the atomic percentages of the determined raw materials into mass ratios, and respectively weighing the raw materials, including pure magnesium: 99.99%, pure aluminum: 99.99%, pure zinc: 99.99% and Mg-25M master alloy;
2) polishing the surface of the cut magnesium block to remove an oxide film on the surface of the magnesium block, cleaning a crucible for smelting, and then putting magnesium alloy and a covering agent into the crucible, wherein the covering agent is MgCl2: KCl 1: 1, putting the crucible into an oven, and drying at the temperature of 80 ℃ for 30 min; opening a ventilation valve and injecting carbon dioxide protective gas 5min before smelting; 1min before smelting, opening a circulating cooling water valve;
3) opening a light alloy smelting furnace, ascending a furnace cover, moving the furnace body leftwards, stably placing the dried crucible into the furnace, placing a magnesium ingot into the middle position of the crucible, uniformly covering a covering agent around the magnesium ingot, moving the furnace body rightwards, and descending the furnace cover;
4) rapidly heating to 720 ℃ at a heating speed of 10 ℃/min, opening the furnace body after the magnesium alloy is melted, adding the dried alloying elements by using a dosing spoon, and reducing the furnace body;
5) starting a stirring device to uniformly disperse the elements Al and Zn in the alloy liquid, stirring for 3min, continuously heating to 750 ℃, and preserving heat for 30 min;
6) and (5) turning off the power supply, and naturally cooling the furnace body to finish smelting.
4. An AZ31M alloy according to claim 1 or 2, wherein the magnesium anode of said AZ31M alloy is used for cathodic protection of carbon steel.
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| CN114134379A (en) * | 2021-11-30 | 2022-03-04 | 东北电力大学 | AZ31M alloy and application thereof |
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