CN114657407B - Protective solvent for DKM7 alloy smelting and preparation method thereof - Google Patents
Protective solvent for DKM7 alloy smelting and preparation method thereof Download PDFInfo
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- CN114657407B CN114657407B CN202210320209.0A CN202210320209A CN114657407B CN 114657407 B CN114657407 B CN 114657407B CN 202210320209 A CN202210320209 A CN 202210320209A CN 114657407 B CN114657407 B CN 114657407B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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Abstract
The invention relates to the technical field of magnesium alloy smelting, in particular to a protective solvent for DKM7 alloy smelting and a preparation method thereof. The protective solvent for smelting the DKM7 alloy comprises the following components in percentage by mass: 1 to 2 percent of magnesium chloride, 54 to 56 percent of potassium chloride, 18 to 20 percent of barium chloride, 1.5 to 2.5 percent of calcium fluoride and 20 to 25.5 percent of calcium chloride. The protective solvent for smelting the DKM7 alloy can be spread on the surface of a solution when the DKM7 alloy is melted through the coordination effect of all components, plays an excellent protective role, and plays an excellent role in removing slag inclusion through standing and settling. The metallurgical quality of the cast reaches HB7780-2005 type I requirements, and no solvent is mixed.
Description
Technical Field
The invention relates to the technical field of magnesium alloy smelting, in particular to a protective solvent for DKM7 alloy smelting and a preparation method thereof.
Background
Magnesium is active in chemical property, and magnesium alloy usually contains a large amount of oxides and impurity elements such as Ni, fe and CuThese impurities reduce the mechanical properties and corrosion resistance of the magnesium alloy. The DKM7 alloy is a newly developed alloy having a specific gravity of about 1.843g/mm 3 And about 1.7g/mm of prior art magnesium alloy 3 There is a difference that it requires a special solvent.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a protective solvent for smelting DKM7 alloy, which can be spread on the surface of a solution when the DKM7 alloy is melted through the coordination effect of all components to achieve an excellent protective effect, and can be settled after standing to achieve an excellent slag inclusion removing effect.
The invention also aims to provide a preparation method of the protective solvent for smelting the DKM7 alloy, which is simple and feasible.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass:
1 to 2 percent of magnesium chloride, 54 to 56 percent of potassium chloride, 18 to 20 percent of barium chloride, 1.5 to 2.5 percent of calcium fluoride and 20 to 25.5 percent of calcium chloride.
Preferably, the protective solvent for smelting the DKM7 alloy comprises the following components in percentage by mass:
1.2 to 1.8 percent of magnesium chloride, 54.5 to 55.6 percent of potassium chloride, 18.5 to 20 percent of barium chloride, 1.7 to 2.3 percent of calcium fluoride and 20.3 to 24.1 percent of calcium chloride.
Preferably, the protective solvent for smelting the DKM7 alloy comprises the following components in percentage by mass:
1.4 to 1.6 percent of magnesium chloride, 54.9 to 55.3 percent of potassium chloride, 19 to 20 percent of barium chloride, 1.9 to 2.2 percent of calcium fluoride and 20.9 to 22.8 percent of calcium chloride.
Preferably, the melting point of the protective solvent is 385 to 410 ℃.
Preferably, the liquid density of the protective solvent is 1770-1800 kg/m.
Preferably, the particle size of the protective solvent is 200 to 250 mesh.
The preparation method of the protective solvent for smelting the DKM7 alloy comprises the following steps:
heating the mixture of the components to melt to obtain a melt, pouring the melt into an ingot mold, pouring the melt into blocks, and crushing the blocks.
Preferably, the mixture of the components is heated to melt to obtain a melt, and the method specifically comprises the following steps: the mixture of the components is heated to 700-720 ℃ and then heated to 730-735 ℃.
Preferably, the temperature is raised to 730-735 ℃ and then stirring treatment is carried out;
the stirring treatment time is 15-25 min.
Preferably, the heating of the mixture is performed in a crucible.
Compared with the prior art, the invention has the beneficial effects that:
(1) The protective solvent for smelting the DKM7 alloy can be spread on the surface of a solution when the DKM7 alloy is melted through the coordination effect of all components, plays an excellent protective role, and plays an excellent role in removing slag inclusion through standing and settling.
(2) The invention also aims to provide a preparation method of the protective solvent for smelting the DKM7 alloy, which is simple and feasible. The metallurgical quality of the cast reaches the HB7780-2005 type I requirement, and no solvent is mixed.
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, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is an as-cast metallographic microstructure of a DKM7 alloy of the invention;
fig. 2 is a T4 metallographic microstructure of a DKM7 alloy of the invention;
fig. 3 is a T6 metallographic microstructure of a DKM7 alloy of the invention;
FIG. 4 is a block diagram of a cast article obtained using the protective solvent of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
According to one aspect of the invention, the invention relates to a protective solvent for smelting DKM7 alloy, which comprises the following components in percentage by mass:
1 to 2 percent of magnesium chloride, 54 to 56 percent of potassium chloride, 18 to 20 percent of barium chloride, 1.5 to 2.5 percent of calcium fluoride and 20 to 25.5 percent of calcium chloride.
In one embodiment, the DKM7 alloy consists essentially of, in mass percent: 2.1 to 2.5 percent of Gd, 0.5 to 1.0 percent of Zr, 0.3 to 0.6 percent of Zn, 2.7 to 3.1 percent of Nd, and the balance of Mg and inevitable impurities. The preparation method of DKM7 specifically comprises the following steps: the magnesium, zinc, magnesium-gadolinium intermediate alloy, magnesium-zirconium intermediate alloy and magnesium-neodymium intermediate alloy are used as raw materials, and are smelted and cast after being proportioned in proportion. The composition of the DKM7 alloy can be found in particular in patent application No. 202110693616.1.
In one embodiment, the DKM7 consists essentially of, in mass percent: 2.2% of Gd, 0.55% of Zr, 0.4% of Zn, 2.9% of Nd, and the balance of Mg and inevitable impurities.
The DKM7 alloy is a newly developed alloy that differs in specific gravity from prior art magnesium alloys in that it requires a special solvent. The DKM7 had a solid density of 1843 kg/m and a liquid density of about 1720 kg/m.
In one embodiment, the protective solvent has a liquid density of 1770 to 1800 kg/m. In one embodiment, the liquid density of the protective solvent includes, but is not limited to, 1770 kg/m, 1780 kg/m, 1790 kg/m, 1800 kg/m,
Through the coordination and coordination of the components, the obtained protective solvent can be spread on the surface of a solution when the DKM7 alloy is melted, so that the excellent protective effect is achieved, and then the excellent slag inclusion removing effect can be achieved through standing and settling.
The melting point of a low-melting-point mixture formed by proper amounts of magnesium chloride, calcium chloride and potassium chloride is about 400 ℃ and is lower than the melting point (550-600 ℃) and the oxidation temperature of the magnesium alloy, so that the magnesium alloy can be conveniently covered on the surface of the magnesium alloy.
In one embodiment, the magnesium chloride includes, but is not limited to, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2% by mass.
In one embodiment, potassium chloride includes, but is not limited to, 54.2%, 54.5%, 54.6%, 54.7%, 54.8%, 54.9%, 55%, 55.1%, 55.3%, 55.5%, 55.7%, or 55.9% by mass.
In one embodiment, the calcium chloride is present in an amount of 20%, 21%, 21.5%, 22%, 22.5%, 23%, 23.5%, 24%, 25% by mass.
The addition of a proper amount of barium chloride mainly plays a role in adjusting the specific gravity of the solvent, so that the specific gravity of the solvent is higher than that of the DKM7 magnesium alloy in a liquid state, impurities in a filtering solution can sink, but the density cannot be too high, otherwise, the sedimentation degree is too high, and the filtering and protecting effects are poor.
In one embodiment, barium chloride includes, but is not limited to, 18.2%, 18.5%, 18.7%, 18.9%, 19%, 19.2%, 19.5%, 19.7%, or 19.9% by mass.
Proper amount of calcium fluoride promotes the mutual dissolution of all the components to form a complex, and a layer of magnesium liquid surface protective film can be formed.
In one embodiment, calcium fluoride includes, but is not limited to, 1.6%, 1.7%, 1.8%, 1.9%, 2%, 2.1%, 2.2%, 2.3%, or 2.4% by mass.
In one embodiment, the protective solvent for DKM7 alloy smelting comprises the following components in percentage by mass:
1.2 to 1.8 percent of magnesium chloride, 54.5 to 55.6 percent of potassium chloride, 18.5 to 20 percent of barium chloride, 1.7 to 2.3 percent of calcium fluoride and 20.3 to 24.1 percent of calcium chloride.
In one embodiment, the protective solvent for DKM7 alloy smelting comprises the following components in percentage by mass:
1.4 to 1.6 percent of magnesium chloride, 54.9 to 55.3 percent of potassium chloride, 19 to 20 percent of barium chloride, 1.9 to 2.2 percent of calcium fluoride and 20.9 to 22.8 percent of calcium chloride.
By further optimizing the dosage proportion of each component, the protection effect of the protective solvent on the DKM7 alloy smelting can be obviously improved, and the metallurgical quality of the DKM7 alloy is improved.
In one embodiment, the protective solvent for DKM7 alloy smelting comprises the following components in percentage by mass: 1.5% of magnesium chloride, 55% of potassium chloride, 19% of barium chloride, 2% of calcium fluoride and 22.5% of calcium chloride.
In one embodiment, the protective solvent for DKM7 alloy smelting comprises the following components in percentage by mass: 1.5% of magnesium chloride, 55% of potassium chloride, 20% of barium chloride, 2% of calcium fluoride and 21.5% of calcium chloride.
In one embodiment, the protective solvent has a melting point of 385 to 410 ℃. In one embodiment, the melting point of the protective solvent includes, but is not limited to, 385 ℃, 387 ℃, 390 ℃, 393 ℃, 395 ℃, 397 ℃, 400 ℃, 405 ℃, or 409 ℃.
In one embodiment, the protective solvent further comprises sodium chloride and calcium oxide; the sodium chloride and the calcium oxide are not more than 2% by mass. In one embodiment, the total content of sodium chloride and calcium oxide is 0.1%, 0.2%, 0.3%, 0.5%, 0.7%, 0.9%, 1%, 1.2%, 1.5%, 1.6%, 1.8%, or 1.9% by mass. Calcium oxide and sodium chloride are impurities.
In one embodiment, the protective solvent further comprises insolubles; the insoluble matter is not more than 1.5% by mass. The insoluble substances include high-melting point oxides such as alumina, and are also impurities.
In one embodiment, the insolubles include, but are not limited to, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1%, 1.2%, or 1.4% by mass.
In one embodiment, the protective solvent further comprises magnesium oxide; the magnesium oxide is not more than 0.2% by mass. Magnesium oxide is also an impurity. In one embodiment, the magnesium oxide includes, but is not limited to, 0.01%, 0.03%, 0.05%, 0.07%, 0.09%, 0.1%, 0.13%, 0.15%, 0.17% by mass.
According to another aspect, the invention also relates to a preparation method of the protective solvent for DKM7 alloy smelting, comprising the following steps:
heating the mixture of the components to melt to obtain a melt, pouring the melt into an ingot mold, pouring the melt into blocks, and crushing the blocks.
Preferably, the mixture of the components is heated to melt to obtain a melt, and the method specifically comprises the following steps: the mixture of the components is heated to 700-720 ℃ and then heated to 730-735 ℃.
In one embodiment, the mixture of components is heated to a temperature of 700 to 720 ℃, and may also be 702 ℃, 705 ℃, 707 ℃, 709 ℃, 710 ℃, 711 ℃, 712 ℃, 715 ℃, 718 ℃ or 720 ℃. Then the temperature is raised to 730-735 ℃, and 731 ℃, 732 ℃, 733 ℃ and 734 ℃ can be selected.
Preferably, the temperature is raised to 730-735 ℃ and then stirring treatment is carried out; the stirring treatment time is 15-25 min. It can also be selected from 16min, 18min, 20min, 22min or 24min.
Preferably, the heating of the mixture is performed in a crucible.
In one embodiment, a method of smelting a DKM7 alloy comprises the steps of:
(1) Preheating a crucible to dark red, scattering a proper amount of fusing agent on the wall and the bottom of the crucible, preheating furnace materials to be more than 200 ℃, and drying the fusing agent for 1-2 hours at 180-220 ℃; the magnesium-zirconium intermediate alloy is preheated to 300-400 ℃ before being added into the crucible.
(2) Adding preheated pure magnesium ingot, spreading proper flux on the furnace charge, heating and melting.
(3) When the temperature is increased to 720-740 ℃, the magnesium-gadolinium intermediate alloy is directly added into the melted pure magnesium ingot, and after the magnesium-gadolinium intermediate alloy is completely melted, the mixture is stirred for 1-2 min;
(4) Adjusting the temperature to 750-760 ℃, and adding zinc particles;
(5) Continuously heating to 780-800 ℃, and slowly adding 3/4 of the total amount of the magnesium-neodymium intermediate alloy and the magnesium-zirconium intermediate alloy in batches.
(6) After all the alloy is melted, fishing out the bottom and stirring for 10-15 min to homogenize the alloy.
(1) Melting and stirring the magnesium and zirconium added are enough to ensure that the components of the magnesium liquid are uniform;
(7) Refining at 770-790 ℃ after homogenizing the alloy;
(1) sinking a refining spoon or a mechanical stirrer into the 2/3 depth of the molten metal; (2) violently and vertically stirring the alloy liquid for 10-15 min from top to bottom until the alloy liquid presents silvery white mirror luster; in the stirring process, the flux is uniformly and continuously sprinkled on the metal liquid surface; (3) stopping stirring, and standing for 20-25 min;
(8) Adding the rest 1/4 of magnesium-zirconium intermediate alloy 30min before casting, stirring until the magnesium-zirconium intermediate alloy is completely melted, and then stirring for 2-4 min;
(9) Pouring after the alloy liquid is cooled to the pouring temperature; SF6 and sulfur are used for protection in the casting process.
The present invention will be further explained with reference to specific examples and comparative examples.
Fig. 1 is an as-cast metallographic microstructure of a DKM7 alloy of the invention. Fig. 2 is a T4 metallographic microstructure of a DKM7 alloy of the invention. Fig. 3 is a T6 metallographic microstructure of a DKM7 alloy of the invention. FIG. 4 is a block diagram of a cast article obtained using the protective solvent of the present invention.
Example 1
A protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass: 1.5% of magnesium chloride, 55% of potassium chloride, 19% of barium chloride, 2% of calcium fluoride and 22.5% of calcium chloride;
the preparation method of the protective solvent comprises the following steps:
the mixture of the components is heated to melt (700 deg.C), warmed to about 730 deg.C, and stirred for about 20 minutes to obtain a melt, which is poured into an ingot mold, cast into blocks, and the blocks are pulverized into powder (200-250 mesh).
Example 2
A protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass: 1.5% of magnesium chloride, 55% of potassium chloride, 20% of barium chloride, 2% of calcium fluoride and 21.5% of calcium chloride;
the preparation method of the protective solvent comprises the following steps:
example 3
A protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass: 1.2% of magnesium chloride, 54.5% of potassium chloride, 18.5% of barium chloride, 1.7% of calcium fluoride and 24.1% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Example 4
A protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass:
1.8% of magnesium chloride, 55.6% of potassium chloride, 20% of barium chloride, 2.3% of calcium fluoride and 20.3% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Example 5
A protective solvent for smelting a DKM7 alloy comprises the following components in percentage by mass:
1% of magnesium chloride, 54% of potassium chloride, 18% of barium chloride, 1.5% of calcium fluoride and 25.5% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Example 6
A protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass:
2% of magnesium chloride, 56% of potassium chloride, 20% of barium chloride, 2.5% of calcium fluoride and 20% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Example 7
The DKM7 alloy smelting method comprises the following steps:
(1) Preheating a crucible to dark red, scattering a proper amount of protective solvent on the wall and the bottom of the crucible, preheating furnace materials to 210 ℃, and drying the protective solvent for 1.5 hours at 195 ℃; the magnesium-zirconium master alloy is preheated to 350 ℃ before being added into the crucible.
(2) Adding preheated pure magnesium ingot, spreading proper flux on the furnace charge, heating and melting.
(3) When the temperature is raised to 730 ℃, directly adding the magnesium-gadolinium intermediate alloy into the molten pure magnesium ingot, and stirring for 2min after the magnesium-gadolinium intermediate alloy is completely molten;
(4) Adjusting the temperature to 755 ℃, and adding zinc particles;
(5) The temperature is continuously increased to 760 ℃, and 3/4 of the total amount of the magnesium-neodymium intermediate alloy and the magnesium-zirconium intermediate alloy is added in batches and slowly.
(6) After all the alloy is melted, fishing the bottom and stirring for 12min to homogenize the alloy.
(1) Melting and stirring the magnesium and zirconium added are enough to ensure that the components of the magnesium liquid are uniform;
(7) Refining at 780 ℃ after homogenizing the alloy;
(1) sinking a refining spoon or a mechanical stirrer into the 2/3 depth of the molten metal; (2) violently stirring the alloy liquid from top to bottom for 12min until the alloy liquid has silvery white mirror luster; in the stirring process, the flux is uniformly and continuously sprinkled on the metal liquid surface; (3) stopping stirring, and standing for 20min;
(8) Adding the rest 1/4 of magnesium-zirconium intermediate alloy 30min before casting, stirring until the magnesium-zirconium intermediate alloy is completely melted, and stirring for 3min;
(9) Pouring after the alloy liquid is cooled to the pouring temperature; SF6 and sulfur are used for protection in the casting process.
Comparative example 1
A protective solvent for smelting a DKM7 alloy comprises the following components in percentage by mass: 1.5% of magnesium chloride, 55% of potassium chloride, 15% of barium chloride, 2% of calcium fluoride and 26.5% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Comparative example 2
A protective solvent for smelting a DKM7 alloy comprises the following components in percentage by mass: 1.5% of magnesium chloride, 55% of potassium chloride, 25% of barium chloride, 2% of calcium fluoride and 16.5% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Comparative example 3
A protective solvent for smelting a DKM7 alloy comprises the following components in percentage by mass: 0.5% of magnesium chloride, 56% of potassium chloride, 20% of barium chloride, 1% of calcium fluoride and 22.5% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Comparative example 4
A protective solvent for smelting DKM7 alloy comprises the following components in percentage by mass: 0.5% of magnesium chloride, 50% of potassium chloride, 20% of barium chloride, 1.5% of calcium fluoride and 28% of calcium chloride.
The preparation method of the protective solvent is the same as that of example 1.
Examples of the experiments
Referring to the method of example 7, the protective solvents of examples and comparative examples were added during the DKM7 alloy melting process, and the post-pouring metallurgical quality and the solvent inclusion of the resulting castings were measured, with the specific results shown in table 1.
TABLE 1 post-pouring metallurgical quality and solvent inclusions of the castings
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. A protective solvent for smelting DKM7 alloy is characterized by comprising the following components in percentage by mass:
1.2 to 1.8 percent of magnesium chloride, 54.5 to 55.6 percent of potassium chloride, 18.5 to 20 percent of barium chloride, 1.7 to 2.3 percent of calcium fluoride and 20.3 to 24.1 percent of calcium chloride;
the melting point of the protective solvent is 385-410 ℃;
the liquid density of the protective solvent is 1770-1800 kg/m;
the particle size of the protective solvent is 200-250 meshes.
2. The protective solvent for smelting DKM7 alloy as claimed in claim 1, wherein the protective solvent for smelting DKM7 alloy consists of the following components in percentage by mass:
1.4 to 1.6 percent of magnesium chloride, 54.9 to 55.3 percent of potassium chloride, 19 to 20 percent of barium chloride, 1.9 to 2.2 percent of calcium fluoride and 20.9 to 22.8 percent of calcium chloride.
3. The process for the preparation of a protective solvent for DKM7 alloy smelting according to any one of claims 1 to 2, characterized by comprising the steps of:
heating the mixture of the components to melt to obtain a melt, pouring the melt into an ingot mold, pouring the melt into blocks, and crushing the blocks.
4. The method of claim 3, wherein the mixture of components is heated to melt to obtain a melt, and the method comprises: the mixture of the components is heated to 700-720 ℃ and then heated to 730-735 ℃.
5. The method for preparing a protective solvent for DKM7 alloy melting according to claim 4, wherein the stirring treatment is performed after the temperature is raised to 730-735 ℃;
the stirring treatment time is 15-25 min.
6. The method of claim 3, wherein the heating of the mixture is performed in a crucible.
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| KR100760581B1 (en) * | 2006-06-30 | 2007-09-20 | 주식회사 포스코 | Magnesium Alloy Refining Molten Salt |
| CN100529129C (en) * | 2008-04-24 | 2009-08-19 | 上海交通大学 | Mg-Gd-Y-Zr magnesium alloy refining flux and producing method thereof |
| CN102851523A (en) * | 2012-08-22 | 2013-01-02 | 淄博宏泰防腐有限公司 | Refining flux for smelting of WE43 magnesium alloy, and preparation and usage method thereof |
| CN103468976B (en) * | 2013-10-12 | 2014-10-08 | 青海三工镁业有限公司 | No-pollution green environment-friendly fluxing agent for magnesium and magnesium alloy and preparation method thereof |
| CN104438422A (en) * | 2014-09-28 | 2015-03-25 | 洛阳镁鑫合金制品有限公司 | Process for rolling ZK61M magnesium alloy sheets |
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