CN113976841A - Protective agent for magnesium alloy melt pouring, magnesium alloy casting and preparation method thereof - Google Patents
Protective agent for magnesium alloy melt pouring, magnesium alloy casting and preparation method thereof Download PDFInfo
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- CN113976841A CN113976841A CN202111594012.8A CN202111594012A CN113976841A CN 113976841 A CN113976841 A CN 113976841A CN 202111594012 A CN202111594012 A CN 202111594012A CN 113976841 A CN113976841 A CN 113976841A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
- B22D21/04—Casting aluminium or magnesium
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Abstract
The invention belongs to the technical field of magnesium alloy, and particularly relates to a protective agent for magnesium alloy melt pouring, a magnesium alloy casting and a preparation method thereof, wherein the protective agent for magnesium alloy melt pouring comprises boric anhydride and sulfur, the mass content of the boric anhydride is 30-60% of the total amount of the protective agent, and the mass content of the sulfur is 40-70% of the total amount of the protective agent. The protective agent not only improves the thickness of a multi-layer protective layer formed during pouring, but also improves the compactness of a single protective layer, thereby well protecting a magnesium alloy melt, further ensuring the purity of a magnesium alloy casting prepared from the protective agent, improving the performance of the magnesium alloy casting and ensuring excellent metallurgical quality; and can avoid the oxidation and combustion of the magnesium alloy.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a protective agent for magnesium alloy melt pouring, a magnesium alloy casting and a preparation method thereof.
Background
The smelting preparation process of magnesium alloy generally comprises the following stages: melting of charge, modification treatment, refining, fracture inspection and pouring, and solidification molding. The magnesium alloy is very active, so that the magnesium alloy is easy to generate oxidation reaction with oxygen in a molten state to release heat to form oxidation slag inclusion, and the reaction product magnesium oxide is a non-compact film to ensure that the reaction of magnesium and oxygen continuously occurs; therefore, it is required to protect the magnesium alloy during the melting, refining and casting stages of the magnesium alloy, respectively. In the melting stage, RJ series (e.g., RJ-2) flux is typically added; in the refining stage, a refining flux containing low-melting-point compounds such as sodium chloride and calcium chloride is usually added; which can block oxygen on the surface of a relatively static magnesium alloy melt.
In the casting stage, because the magnesium alloy melt is in a multi-dynamic flowing state, the protective film is easily damaged, the requirement on the protection strength of the protective agent (or called flame retardant) is high, and the quality, especially the purity, of the magnesium alloy also needs to be ensured. The conventional protective agent in the melting or refining stage cannot be used for casting, because, on one hand, solvent inclusion is easy to generate, and the purity of the magnesium alloy is seriously influenced; on the other hand, the protective film formed in the multi-dynamic situation is easily damaged, so that the protective film cannot be effectively protected at all in the casting stage.
During the process of casting magnesium alloy melt, two methods are generally adopted to protect the magnesium alloy melt:
1. the solvent (mainly salts) is added for isolation protection, and the corrosion resistance of the magnesium is greatly reduced because the solvent can form a solvent slag inclusion product which is easy to pollute;
2. with gas (SO)2) Protecting to form a compact layer, wherein the effect is general, and a mixture of sulfur and boric acid needs to be added during pouring, but hydrogen is generated due to the reaction of boric acid and magnesium, so that deflagration is easy to occur, magnesium liquid splashes, safety accidents are caused, and the magnesium liquid can escape and is dangerous; and air holes are easy to appear in the casting, so that the quality of the casting is influenced.
Therefore, in the magnesium alloy melt casting stage, a protective agent which can effectively protect and ensure the quality of the magnesium alloy is needed.
Disclosure of Invention
The invention aims to overcome the defect that the performance of a formed magnesium alloy casting is reduced because a protective agent for pouring cannot effectively protect the magnesium alloy in the prior art, and provides the protective agent for pouring a magnesium alloy melt, the magnesium alloy casting and a preparation method thereof, wherein the protective agent is used for preparing the magnesium alloy casting and can form compact multilayer protection so as to effectively protect the magnesium alloy casting; and can avoid the oxidation and combustion of the magnesium alloy; but also can ensure the purity of the magnesium alloy casting, and improve the performance of the magnesium alloy casting, especially the purity of magnesium.
In order to achieve the above purpose, in a first aspect, the present invention provides a protective agent for magnesium alloy melt casting, including boron anhydride and sulfur, wherein the mass content of the boron anhydride is 30-60% of the total amount of the protective agent, and the mass content of the sulfur is 40-70% of the total amount of the protective agent.
In some preferred embodiments, the mass content of the boric anhydride is 35-55% of the total amount of the protective agent, and the mass content of the sulfur is 45-65% of the total amount of the protective agent.
In some preferred embodiments, the mass content of the boric anhydride is 35-50% of the total amount of the protective agent, and the mass content of the sulfur is 50-65% of the total amount of the protective agent.
In some preferred embodiments, the mass ratio of the boron anhydride to the sulfur is 1: 1-1.3.
In some preferred embodiments, boric acid is not present in the protectant.
In a second aspect, the invention provides a method for preparing a magnesium alloy casting, comprising pouring a magnesium alloy melt, and introducing the protective agent of the first aspect before and/or during the pouring.
In some preferred embodiments, in the casting, the protective agent forms a multi-layer protective layer on the surface of the magnesium alloy melt, the multi-layer protective layer comprising a dense film, a glass melt layer, and a gas layer.
More preferably, the thickness of the glass melt layer is 0.1 to 0.5 mm.
More preferably, the dense film contains magnesium oxide, magnesium sulfide, and elemental boron.
In a third aspect, the invention provides a magnesium alloy casting prepared by the method of the second aspect.
The invention adopts the boric anhydride and the sulfur which are added with proper amount as the protective agent for the magnesium alloy melt casting, and has at least the following advantages:
on the first hand, a proper amount of boric anhydride can form a glassy state melt with proper thickness at high temperature (more than 420 ℃) and spread on the surface of the magnesium alloy melt, the glassy state melt has proper thickness, the reaction of magnesium liquid and oxygen is prevented, and the boric anhydride and magnesium react to generate magnesium oxide and elemental boron; meanwhile, the appropriate amount of sulfur can generate magnesium sulfide on one hand, and a film formed by the magnesium sulfide, magnesium oxide and elemental boron is a compact oxide film compared with a magnesium oxide film, so that the magnesium oxide film can prevent further reaction of magnesium and oxygen, and on the other hand, the sulfur can also react with oxygen to generate sulfur dioxide to form a gas layer; thereby forming multilayer cooperative protection and having better protectiveness;
in the second aspect, the density of the glassy melt is less than that of the magnesium alloy melt, and the glassy melt can always cover the surface of the magnesium alloy melt even under the multi-dynamic condition and can always form a continuous and compact multi-layer protective layer together with a gas layer;
in the third aspect, boric acid does not need to be added into the protective agent, so that the magnesium alloy can be prevented from being oxidized and combusted.
In a word, the thickness of a multi-layer protective layer formed in the process of pouring is increased, and the compactness of a single protective layer is also increased, so that the magnesium alloy melt is well protected, the purity of a magnesium alloy casting prepared by the method is ensured, the performance of the magnesium alloy casting is improved, and the metallurgical quality is excellent; and can avoid the oxidation combustion of the magnesium alloy without generating hydrogen.
Drawings
FIG. 1 is a schematic protection diagram of the protective agent of the present invention in a working state.
FIG. 2 is a drawing of a magnesium alloy casting of the present invention.
Description of the reference numerals
1-crucible, 2-magnesium alloy melt, 3-glass melt layer, 4-dense film, and 5-gas layer.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In order to prevent the adverse effects caused by solvent slag inclusion products and/or oxidative combustion and the like caused by the existing casting protective agent, the invention provides, in a first aspect, the casting protective agent for the magnesium alloy melt, which comprises boric anhydride and sulfur, wherein the mass content of the boric anhydride is 30-60% of the total amount of the protective agent, and the mass content of the sulfur is 40-70% of the total amount of the protective agent.
In the scheme of the invention, the boric anhydride can form continuous glass-state melt with proper thickness during casting and spread on the surface of the magnesium alloy melt to form a glass melt layer; meanwhile, boric anhydride reacts with magnesium to generate a compact film of magnesium oxide and elemental boron; the compact film is positioned below the glass melt layer, and can synergistically and effectively prevent the oxidation reaction of magnesium in the magnesium alloy melt and prevent the combustion of the magnesium alloy melt, so that the quality, particularly the corrosion resistance and the purity of a magnesium alloy casting are ensured. The inventor also finds that under the same conditions, if the amount of the boric anhydride is not suitable, particularly, the amount is too small, the boric anhydride mainly plays a role of glass bonding, namely, the boric anhydride becomes a bonding agent after becoming a glass state, a layered glass state melt with enough thickness cannot be formed, and the boric anhydride is easily damaged under a multi-dynamic scene of casting, has a protection dead point and cannot form effective protection.
In addition, sulfur and oxygen react to generate sulfur dioxide, and the sulfur dioxide and magnesium react to generate magnesium sulfide and magnesium oxide to form a more compact film, so that the compactness of the film is further improved, and the protection capability is enhanced; meanwhile, sulfur dioxide forms a gas layer for synergistic multilayer protection. The inventor also found that under the same conditions, when sulfur is not contained, only boric anhydride is used as a protective agent, a small amount of slag inclusion and partial oxidation combustion phenomena still occur.
As shown in figure 1, a dense film 4, a glass melt layer 3 and a gas layer 5 are sequentially formed from bottom to top above a magnesium alloy melt 2 in a crucible 1; it has excellent protection performance.
In some preferred embodiments, the mass content of the boric anhydride is 35-55% of the total amount of the protective agent, and the mass content of the sulfur is 45-65% of the total amount of the protective agent.
In some preferred embodiments, the mass content of the boric anhydride is 35-50% of the total amount of the protective agent, and the mass content of the sulfur is 50-65% of the total amount of the protective agent. Under the preferred scheme, the method is more beneficial to forming a multilayer protective layer with proper thickness and proper proportion, the protective capability is better, and the quality of the magnesium alloy casting molded by casting is better.
In some preferred embodiments, the mass ratio of the boron anhydride to the sulfur is 1: 1-1.3. In this preferred embodiment, the thicknesses of the respective layers in the formed multi-layer protective layer have a suitable ratio, which can maximize the protective synergy.
In some preferred embodiments, boric acid is not present in the protectant. In the preferred scheme, boric acid is not required to be added, so that effective multilayer protection can be obtained, and oxidation and combustion of the magnesium alloy can be prevented.
The protective agent for pouring the magnesium alloy melt is particularly suitable for the pouring process of multiple dynamic scenes, can adapt to multiple scenes without being damaged, can still form continuous, continuous and strong protective action, and effectively ensures the quality of formed magnesium alloy castings.
The protective agent can be suitable for pouring castings in any field and can meet the requirements of aviation standards HB7780-2005 on the castings.
In a second aspect, the invention provides a method for preparing a magnesium alloy casting, comprising pouring a magnesium alloy melt, and introducing the protective agent of the first aspect before and/or during the pouring.
The protective agent can be introduced before and/or during the pouring according to actual requirements, so long as the protective agent can be beneficial to protecting the magnesium alloy melt, and the quality of the magnesium alloy casting can be ensured. Preferably, the majority of the protectant is introduced prior to the casting, and an appropriate amount of protectant is introduced during the casting process.
It will be appreciated that, because of the relatively high temperature of the magnesium alloy melt (typically around 700 ℃), the protective agent will melt very quickly after introduction and form a protective layer.
The invention does not impose any restrictions on the time of addition before the pouring, as long as protection and rapid melting are facilitated. Illustratively, the protective agent is introduced at least 5min before the casting.
In the casting of the present invention, the protective agent forms a multi-layer protective layer on the surface of the magnesium alloy melt, and as shown in fig. 1, the multi-layer protective layer comprises a dense film 4, a glass melt layer 3 and a gas layer 5.
In some embodiments, the dense film 4 comprises magnesium oxide, magnesium sulfide, and elemental boron.
In some embodiments, the glass melt layer 3 has a thickness of 0.1 to 0.5 mm.
In a third aspect, the invention provides a magnesium alloy casting prepared by the method of the second aspect.
As shown in figure 2, the magnesium alloy casting provided by the invention has smooth surface, no black oxidation, good quality and excellent corrosion resistance, and the metallurgical quality can meet the requirements of aviation standard HB7780-2005 class I castings.
The present invention is illustrated in more detail below with reference to examples.
Example 1
The ZM5 alloy aviation support is cast by using the protective agent.
The material composition is ZM5 alloy, which is specifically shown in Table 1.
TABLE 1
The materials are adopted for smelting as follows:
1. melting of charge
Preheating the crucible to dark red, preheating the furnace charge (namely the materials) to more than 200 ℃, and drying the fusing agent (RJ-2) and the alterant (hexachloroethane) for 1.5 hours at the temperature of 140 ℃.
RJ-2 fusing agent is sprinkled on the bottom of the crucible, and master alloy ingot, magnesium ingot, foundry returns and the like in the preheated furnace charge are added, and the temperature is raised for melting.
After the furnace burden is completely melted, the temperature is adjusted to 720 ℃, the intermediate alloy and the zinc ingot in the furnace burden are added, and after the furnace burden is completely melted, the mixture is stirred for 5 min.
2. Modification treatment
Adjusting the temperature to 750 ℃, and adding 0.7wt% of hexachloroethane for modification treatment; specifically, the alterant is wrapped by aluminum foil and placed in a preheated bell-shaped cover, and the alterant is slowly pressed into the alloy liquid from 1/2 to 2/3 depths by the bell-shaped cover and smoothly moves horizontally until the alterant is completely decomposed. The deterioration duration is not less than 5 min.
The burning place on the surface of the alloy liquid can be covered by flux to extinguish.
Removing slag on the liquid surface, and spraying a layer of flux.
3. Refining
The temperature is adjusted to 740 ℃, a stirring spoon or a mechanical stirrer is used for sinking into the molten metal 2/3, and the alloy liquid is stirred for 10min from top to bottom until the surface of the alloy liquid is mirror.
During the stirring process, refining solvent (RJ-2) is uniformly and continuously sprinkled on the liquid surface, and the consumption amount of the solvent is about 1.5 percent of the total weight of the charging materials.
4. Fracture inspection
And (3) removing slag on a pouring nozzle, a baffle (the baffle arranged on the crucible), the crucible wall and the surface of the alloy liquid, spraying RJ-2 fusing agent, adjusting the temperature to 760 ℃, and standing for 13 min.
And pouring a fracture sample, and checking the fracture. After the molten metal is scooped up, the protective agent (namely the mass ratio of the sulfur to the boric anhydride is 55: 45) is dispersed for protection, and the dosage is added until the magnesium liquid is not oxidized and combusted violently.
In the meantime, when the fracture fails, the deterioration and refining are allowed to be repeated, but the total number is not more than 3 times.
5. Pouring
And adjusting the temperature to the pouring temperature of 750 ℃ after the fracture is qualified, and discharging and pouring. Adding the protective agent (namely the mass ratio of the sulfur to the boric anhydride is 55: 45) before casting for 5min for flame-retardant protection. The thickness of the glass melt layer is 0.1-0.5 mm.
And after the alloy is subjected to modification treatment, pouring within 1h, otherwise, re-checking the fracture, and continuing pouring by using the method after the fracture is qualified, wherein if the fracture is unqualified, modification and refining treatment are allowed to be performed again.
And (5) after the pouring is finished, carrying out solidification molding to obtain the magnesium alloy casting.
As shown in figure 2, the obtained magnesium alloy casting has smooth surface and no oxidation and combustion phenomenon in the smelting process. Tests show that the metallurgical quality meets the requirements of aviation standard HB7780-2005 class I castings, and X-ray fluoroscopy does not contain any inclusion (slag).
Comparative example 1
The method is carried out according to the embodiment 1, except that the proportion of the used protective agents is different, and specifically, the mass ratio of the sulfur to the boric anhydride is 90: 10, the rest is the same as example 1.
The magnesium alloy casting has smooth surface and oxidation and combustion phenomenon in the smelting and casting process. Tests show that the metallurgical quality is lower than the requirement of aviation standard HB7780-2005 class I castings, and large-area inclusions (slag) are generated in X-ray perspective.
Comparative example 2
The procedure is as in example 1 except that a different protectant formulation is used, the protectant being boric anhydride (i.e., no sulfur).
The surface of the obtained magnesium alloy casting has black oxide, and the oxidation and combustion phenomena exist in the smelting and casting process. Tests show that the metallurgical quality is lower than the requirement of aviation standard HB7780-2005 class I castings, and large-area inclusions (slag) are generated in X-ray perspective.
Example 2
The method is carried out according to the embodiment 1, except that the proportion of the used protective agents is different, and specifically, the mass ratio of the sulfur to the boric anhydride is 50: 50, the rest is the same as example 1.
The obtained magnesium alloy casting has smooth surface and no oxidation combustion phenomenon in the smelting process. Tests show that the metallurgical quality meets the requirements of aviation standard HB7780-2005 class I castings, and X-ray fluoroscopy does not contain any inclusion (slag).
Example 3
The method is carried out according to the embodiment 1, except that the proportion of the used protective agents is different, and specifically, the mass ratio of the sulfur to the boric anhydride is 40: 60, the rest is the same as example 1.
The obtained magnesium alloy casting has smooth surface and no oxidation combustion phenomenon in the smelting process. Through tests, the metallurgical quality has tiny inclusions (slag) through X-ray fluoroscopy, but reaches the requirements of aviation standard HB7780-2005 class I castings.
As can be seen from the above examples and comparative examples, the protective effect is significantly better and the metallurgical quality is better by using the protective agent with proper composition; and the protective agent has improper composition, so that the phenomena of casting slag inclusion and oxidation combustion cannot be avoided. Further, as can be seen from examples 1 and 3, the protective agent having a preferable appropriate composition according to the present invention can exert a better protective effect and can provide a higher metallurgical quality.
Claims (10)
1. The protective agent for magnesium alloy melt pouring is characterized by comprising 30-60% of boric anhydride and 40-70% of sulfur by mass.
2. The protective agent according to claim 1, wherein the mass content of the boric anhydride is 35-55% of the total amount of the protective agent, and the mass content of the sulfur is 45-65% of the total amount of the protective agent.
3. The protective agent according to claim 2, wherein the mass content of the boric anhydride is 35-50% of the total amount of the protective agent, and the mass content of the sulfur is 50-65% of the total amount of the protective agent.
4. The protective agent according to claim 1, wherein the mass ratio of the boric anhydride to the sulfur is 1: 1-1.3.
5. The protective agent according to claim 1, characterized in that boric acid is not contained in the protective agent.
6. A method for producing a magnesium alloy casting, comprising pouring a magnesium alloy melt, characterized in that the protective agent according to any one of claims 1 to 5 is introduced before and/or during said pouring.
7. The production method according to claim 6, wherein in the pouring, the protective agent forms a multilayer protective layer on the surface of the magnesium alloy melt, the multilayer protective layer including a dense film, a glass melt layer, and a gas layer.
8. A production method according to claim 7, wherein the thickness of the glass melt layer is 0.1 to 0.5 mm.
9. The production method according to claim 7, wherein the dense film contains magnesium oxide, magnesium sulfide, and elemental boron.
10. A magnesium alloy casting, characterized by being produced by the method of any one of claims 6 to 9.
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Cited By (1)
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| WO2023109101A1 (en) * | 2021-12-13 | 2023-06-22 | 河北钢研德凯科技有限公司 | Highly-inert mold shell for casting, preparation method therefor, and method for improving precision of magnesium alloy casting |
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Inventor after: Shao Chong Inventor after: Wang Kai Inventor after: Wu Hailong Inventor after: Yang Wuqiang Inventor after: Zhu Xiaoping Inventor after: Xing Changyong Inventor after: Zhang Guochi Inventor after: Wang Ziyang Inventor after: Mo Xueyan Inventor after: Jia Linyue Inventor before: Shao Chong Inventor before: Wang Kai Inventor before: Wu Hailong Inventor before: Yang Wuqiang Inventor before: Zhu Xiaoping Inventor before: Xing Changyong Inventor before: Zhang Guochi Inventor before: Wang Ziyang Inventor before: Mo Xueyan Inventor before: Jia Linyue |