CN109930043B - Preparation method of as-cast high-strength rapid corrosion magnesium alloy - Google Patents
Preparation method of as-cast high-strength rapid corrosion magnesium alloy Download PDFInfo
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Abstract
The invention relates to the technical field of metal alloy materials, in particular to a preparation method of an as-cast high-strength rapid corrosion magnesium alloy. The method comprises the following steps: (1) respectively pretreating a magnesium ingot and an aluminum ingot; (2) pretreating germanium particles; (3) melting the pretreated magnesium ingot and aluminum ingot; (4) adding germanium particles after melting to obtain a melt; (5) and cooling the melt, then casting, and naturally cooling the cast ingot to room temperature to obtain the as-cast high-strength rapid corrosion magnesium alloy, wherein the as-cast high-strength rapid corrosion magnesium alloy comprises the following components in percentage by weight: 2-8% of Al, 0.5-7% of Ge and the balance of magnesium. The invention fully utilizes the action of Al and Ge elements to improve the strength and corrosion rate of the magnesium alloy, and obviously improves the mechanical property and corrosion rate of the magnesium alloy by less alloy element addition types and less addition amount.
Description
Technical Field
The invention relates to the technical field of metal alloy materials, in particular to a preparation method of an as-cast high-strength rapid corrosion magnesium alloy.
Background
Magnesium alloys are the lightest material of structural metals (density 1.74 g/cm)3) It has the characteristics of low density, high specific strength and the like, so it is widely used in the automobile and aerospace industry, but its application is limited due to high corrosion rate. However, in some applications, materials with high corrosion rates are more desirable. For example, a degradable fracturing sphere for use in shale gas development. In actual engineering, a fracturing ball or a fracturing ball seat, which is one of the key tools of the multistage fracturing technology, must have sufficient strength to withstand high pressure, and the materials used for the fracturing ball are usually Polyetheretherketone (PEEK), TORLON, low carbon steel, and aluminum alloy. Fracturing made of these materialsThe conventional method of ball removal from oil and gas wells is by milling or drilling, which is a very complicated and time consuming and laborious process that adds to the cost. By utilizing the characteristic of high corrosion rate of the magnesium alloy, the prepared degradable fracturing ball can be completely corroded in 3 percent potassium chloride solution at 90 ℃ within a few days, so that the drilling process is more economical and time-saving.
Disclosure of Invention
The invention provides a preparation method of an as-cast high-strength rapid corrosion magnesium alloy, aiming at solving the problems of complex process, time consumption, labor consumption and cost increase of the existing method for eliminating a fracturing ball.
The invention is realized by the following technical scheme: a preparation method of as-cast high-strength rapid corrosion magnesium alloy comprises the following steps:
(1) respectively pretreating a magnesium ingot and an aluminum ingot: respectively removing oxides and oil stains on the surfaces of the magnesium ingot and the aluminum ingot, cleaning the magnesium ingot and the aluminum ingot by absolute ethyl alcohol, and drying the magnesium ingot and the aluminum ingot at the temperature of 90 ℃ to constant weight to respectively obtain the pretreated magnesium ingot and the pretreated aluminum ingot;
(2) pretreating germanium particles: removing oxides and oil stains on the surface of the germanium particles, cleaning the germanium particles by absolute alcohol, and drying the germanium particles to constant weight at the temperature of 90 ℃ to obtain pretreated germanium particles;
(3) putting the pretreated magnesium ingot and aluminum ingot in CO2And SF6Heating the smelter under the protection of the mixed gas to 700 ℃ and 760 ℃ to melt the smelter;
(4) keeping the temperature at 760 ℃ of 700-2And SF6Stirring uniformly under the protection of (1) to obtain a melt, and keeping the temperature for 35-60 min;
(5) cooling the melt to 650-700 ℃, standing for 10-20min, then casting, preheating a steel mould for casting to 200-300 ℃, and naturally cooling the cast ingot to room temperature to obtain the as-cast high-strength rapid corrosion magnesium alloy, wherein the as-cast high-strength rapid corrosion magnesium alloy comprises the following components in percentage by weight: 2-8% of Al, 0.5-7% of Ge and the balance of magnesium.
Of course, impurities are inevitably introduced in the preparation process of the as-cast high-strength rapid-corrosion magnesium alloy of the present invention, and impurities are also present in the magnesium ingot, the aluminum ingot and the germanium grains, so that the as-cast high-strength rapid-corrosion magnesium alloy of the present invention includes unavoidable impurities in addition to the aforementioned components, which is common knowledge in the art.
As a further improvement of the technical scheme of the invention, before removing the oxides and oil stains on the surfaces of the magnesium ingot and the aluminum ingot, the magnesium ingot and the aluminum ingot are cut into small blocks of 100mm, × 30mm, × 20mm and 3520 mm, so that the oxides and the oil stains on the surfaces of the magnesium ingot and the aluminum ingot are conveniently removed, and the magnesium ingot and the aluminum ingot are also conveniently melted.
As a further improvement of the technical scheme of the invention, the germanium particles have industrial-grade purity and above.
Compared with the prior art, the invention has the following advantages:
1) the addition of the alloy element Al can effectively improve the casting performance and the mechanical property of the magnesium alloy, and the Al element and the magnesium can form a uniformly and dispersedly distributed precipitated phase Mg17Al12The corrosion sites of the alloy are increased, and the corrosion rate of the alloy is improved.
2) The addition of the alloy element Ge can refine grains and strengthen grain boundaries, so that the tensile strength and the yield strength of the magnesium alloy are effectively improved, and meanwhile, the Ge element has low solubility in magnesium and can form a large amount of uniformly distributed precipitated phase Mg with magnesium2Ge，Mg2The Ge and magnesium alloy matrix form a micro battery to generate galvanic corrosion, so that the dissolution of the matrix is accelerated, and the alloy corrosion rate is improved.
3) The invention fully utilizes the action of Al and Ge elements to improve the strength and corrosion rate of the magnesium alloy, and obviously improves the mechanical property and corrosion rate of the magnesium alloy by less alloy element addition types and less addition amount. The compressive strength of the fracturing ball can reach 380-400 MPa, the corrosion rate in a 3% KCl solution at 90 ℃ can reach 350-480 mm/a, the fracturing ball can meet the performance requirement, and the fracturing ball can be used as a structural member and can be quickly dissolved under a specific condition.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a stress-strain curve obtained by a compression test of the as-cast high-strength rapid-corrosion magnesium alloy prepared in example 3. It can be seen from the figure that the compressive strength of example 3 can reach 391 MPa.
FIG. 2 is a microstructure diagram of an as-cast high-strength rapid-corrosion magnesium alloy prepared in example 3. It can be seen from the figure that the second phase in example 3 is uniformly distributed, has more corrosion active sites, and can effectively improve the corrosion rate of the alloy.
FIG. 3 is a polarization curve measured by potentiodynamic scanning at 25 ℃ in the cast high-strength rapid-corrosion magnesium alloy prepared in example 3 and comparative examples 1-2. It can be seen from the graph that the corrosion current density of example 3 is significantly higher than that of comparative examples 1-2, and the corrosion rate of example 3 is faster at room temperature.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The technical solution of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
An as-cast high-strength fast-corrosion magnesium alloy comprises the following chemical components in percentage by mass: 6% of Al, 1% of Ge and the balance of magnesium.
The preparation method of the as-cast high-strength rapid corrosion magnesium alloy comprises the following steps:
(1) respectively pretreating a magnesium ingot and an aluminum ingot, namely respectively cutting the magnesium ingot and the aluminum ingot into small blocks of 100mm × 30mm, 3530 mm and × 20mm, removing oxides and oil stains on the surfaces by a conventional method, cleaning the small blocks by absolute ethyl alcohol, and drying the cleaned small blocks to constant weight at the temperature of 90 ℃ to obtain the pretreated magnesium ingot and the pretreated aluminum ingot;
(2) pretreating germanium particles: removing oxides and oil stains on the surface of the germanium particles by a conventional method, cleaning the germanium particles by absolute alcohol, and drying the germanium particles to constant weight at the temperature of 90 ℃ to obtain pretreated germanium particles;
(3) putting the pretreated magnesium ingot and aluminum ingot in CO2And SF6Heating the smelter under the protection of mixed gas to 750 ℃ to melt the smelter;
(4) melting, maintaining at 750 deg.C for 30min, heating to 800 deg.C, adding germanium particles, and adding CO2And SF6Stirring uniformly under the protection of (1) to obtain a melt, and keeping the temperature for 50 min;
(5) and cooling the melt to 700 ℃, standing for 10min, then casting, preheating a steel mould for casting to 250 ℃, and naturally cooling the cast ingot to room temperature to obtain the as-cast high-strength rapid corrosion magnesium alloy.
The compressive strength of the prepared magnesium alloy is 384Mpa, and the corrosion rate is 355 mm/a.
Example 2
An as-cast high strength fast corrosion magnesium alloy product is composed of the following components in percentage by weight (g/g): 6% of Al, 3% of Ge and the balance of magnesium.
The procedure was as in example 1.
The compressive strength of the prepared magnesium alloy is 399MPa, and the corrosion rate is 442 mm/a.
Example 3
An as-cast high strength fast corrosion magnesium alloy product is composed of the following components in percentage by weight (g/g): 6% of Al, 5% of Ge and the balance of magnesium.
The procedure was as in example 1.
The compressive strength of the prepared magnesium alloy is 391MPa, and the corrosion rate is 483 mm/a.
Comparative example 1
An as-cast high strength fast corrosion magnesium alloy product is composed of the following components in percentage by weight (g/g): 6% of Al, and the balance of magnesium.
The procedure was as in example 1.
Comparative example 2
An as-cast high strength fast corrosion magnesium alloy product is composed of the following components in percentage by weight (g/g): 3% Ge, balance magnesium.
The procedure was as in example 1.
In examples 1 to 3 and comparative examples 1 to 2, the magnesium ingot, the aluminum ingot, and the germanium grains were all of industrial grade purity or higher.
And (3) performance detection:
and respectively taking the finished magnesium alloy prepared in the examples 1-3 and the comparative examples 1-2 for corrosion performance test, wherein the test conditions are as follows: temperature (90 ℃ C.), 3.0 wt.% potassium chloride solution.
The corrosion rate of the magnesium alloy was measured by the weight loss method, and the results are shown in table 1.
TABLE 1 examples and comparative corrosion rates
| Test specimen | Corrosion rate/(mm. a)-1) |
| Example 1 | 355 |
| Example 2 | 442 |
| Example 3 | 483 |
| Comparative example 1 | 1.42 |
| Comparative example 2 | 4.56 |
Taking the finished magnesium alloy prepared in the embodiment 3 and the comparative examples 1-2 to carry out potentiodynamic scanning test at room temperature, wherein the test conditions are as follows: at room temperature (25 ℃ C.), 3.0% by weight of potassium chloride solution.
The fitting parameters were tested using potentiodynamic scanning and the results are shown in table 2.
TABLE 2 examples and comparative potentiodynamic scan parameters
Example 4
An as-cast high-strength fast-corrosion magnesium alloy comprises the following chemical components in percentage by mass: 2% of Al, 7% of Ge and the balance of magnesium.
The preparation method of the as-cast high-strength rapid corrosion magnesium alloy comprises the following steps:
(1) respectively pretreating a magnesium ingot and an aluminum ingot, namely respectively cutting the magnesium ingot and the aluminum ingot into small blocks of 100mm × 30mm, 3530 mm and × 20mm, removing oxides and oil stains on the surfaces by a conventional method, cleaning the small blocks by absolute ethyl alcohol, and drying the cleaned small blocks to constant weight at the temperature of 90 ℃ to obtain the pretreated magnesium ingot and the pretreated aluminum ingot;
(2) pretreating germanium particles: removing oxides and oil stains on the surface of the germanium particles by a conventional method, cleaning the germanium particles by absolute alcohol, and drying the germanium particles to constant weight at the temperature of 90 ℃ to obtain pretreated germanium particles;
(3) putting the pretreated magnesium ingot and aluminum ingot in CO2And SF6Heating the furnace to 700 ℃ under the protection of mixed gas to melt the mixture;
(4) melting, maintaining the temperature at 760 deg.C for 25min, and heatingHeating to 770 deg.C, adding germanium particles in CO2And SF6Stirring uniformly under the protection of (1) to obtain a melt, and keeping the temperature for 60 min;
(5) and cooling the melt to 650 ℃, standing for 20min, then casting, preheating a steel mould for casting to 200 ℃, and naturally cooling the cast ingot to room temperature to obtain the as-cast high-strength rapid corrosion magnesium alloy.
Example 5
An as-cast high-strength fast-corrosion magnesium alloy comprises the following chemical components in percentage by mass: 8% of Al, 0.5% of Ge and the balance of magnesium.
The preparation method of the as-cast high-strength rapid corrosion magnesium alloy comprises the following steps:
(1) respectively pretreating a magnesium ingot and an aluminum ingot, namely respectively cutting the magnesium ingot and the aluminum ingot into small blocks of 100mm × 30mm, 3530 mm and × 20mm, removing oxides and oil stains on the surfaces by a conventional method, cleaning the small blocks by absolute ethyl alcohol, and drying the cleaned small blocks to constant weight at the temperature of 90 ℃ to obtain the pretreated magnesium ingot and the pretreated aluminum ingot;
(2) pretreating germanium particles: removing oxides and oil stains on the surface of the germanium particles by a conventional method, cleaning the germanium particles by absolute alcohol, and drying the germanium particles to constant weight at the temperature of 90 ℃ to obtain pretreated germanium particles;
(3) putting the pretreated magnesium ingot and aluminum ingot in CO2And SF6Heating the smelter under the protection of mixed gas to 760 ℃ to melt the smelter;
(4) maintaining the temperature at 700 deg.C for 35min after melting, heating to 780 deg.C, adding germanium particles in CO2And SF6Stirring uniformly under the protection of (1) to obtain a melt, and keeping the temperature for 35 min;
(5) and cooling the melt to 650 ℃, standing for 20min, then casting, preheating a steel mould for casting to 300 ℃, and naturally cooling the cast ingot to room temperature to obtain the as-cast high-strength rapid corrosion magnesium alloy.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (3)
1. The preparation method of the as-cast high-strength rapid corrosion magnesium alloy is characterized by comprising the following steps of:
(1) respectively pretreating a magnesium ingot and an aluminum ingot: respectively removing oxides and oil stains on the surfaces of the magnesium ingot and the aluminum ingot, cleaning the magnesium ingot and the aluminum ingot by absolute ethyl alcohol, and drying the magnesium ingot and the aluminum ingot at the temperature of 90 ℃ to constant weight to respectively obtain the pretreated magnesium ingot and the pretreated aluminum ingot;
(2) pretreating germanium particles: removing oxides and oil stains on the surface of the germanium particles, cleaning the germanium particles by absolute alcohol, and drying the germanium particles to constant weight at the temperature of 90 ℃ to obtain pretreated germanium particles;
(3) putting the pretreated magnesium ingot and aluminum ingot in CO2And SF6Heating the smelter under the protection of the mixed gas to 700 ℃ and 760 ℃ to melt the smelter;
(4) keeping the temperature at 760 ℃ of 700-2And SF6Stirring uniformly under the protection of (1) to obtain a melt, and keeping the temperature for 35-60 min;
(5) cooling the melt to 650-plus-700 ℃, standing for 10-20min, then casting to obtain a cast ingot, preheating a steel mould to 200-plus-300 ℃, and naturally cooling the cast ingot to room temperature to obtain the as-cast high-strength rapid corrosion magnesium alloy, wherein the as-cast high-strength rapid corrosion magnesium alloy comprises the following components in percentage by weight: 6% of Al, 0.5-7% of Ge and the balance of magnesium.
2. The method for preparing as-cast high-strength rapid corrosion magnesium alloy according to claim 1, wherein the magnesium ingot and the aluminum ingot are cut into small pieces of 100mm × 30mm, × 20mm before removing oxides and oil stains on the surfaces of the magnesium ingot and the aluminum ingot.
3. The method for preparing as-cast high-strength rapid corrosion magnesium alloy according to claim 1 or 2, wherein the germanium particles have an industrial grade purity of at least.
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