CN112921225A - Aluminum-coated nano Al for Mg-Al alloy4C3Granular grain refiner and preparation method thereof - Google Patents
Aluminum-coated nano Al for Mg-Al alloy4C3Granular grain refiner and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminum-coated nano Al for Mg-Al series alloy4C3A process for preparing granular grain refiner includes such steps as mixing Al powder, C powder and Mg powder, loading in ball grinder, adding big, middle and small zirconium oxide balls, low-speed ball grinding, high-speed intermittent ball grinding for a certain time, and mechanical alloying between Al powder and C powder to obtain nano-class Al powder4C3Particles. Standing the ball milling tank for a period of time, opening the ball milling tank, then filling a certain amount of Al powder, vacuumizing and sealing the ball milling tank, and then performing coating ball milling to finally form the aluminum-coated nano Al4C3A large-particle-shaped refiner of particles. The invention has simple operation process and production costThe prepared refiner has good refining effect on the grains of the Mg-Al alloy, so that the strength and the toughness of the Mg-Al alloy can be obviously improved, and the refining efficiency has no dependence on the components of the Mg-Al alloy.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy casting, and relates to aluminum-coated nano Al for Mg-Al alloy4C3A granular grain refiner and a preparation method thereof.
Background
The Mg-Al series magnesium alloy is one of the most common magnesium alloys and has the advantages of high specific strength, specific rigidity, excellent casting performance, excellent mechanical processing performance and the like. However, the interval between the liquid and solid temperature ranges of Mg-Al alloy is generally large, and casting defects such as shrinkage porosity, air holes, cracks and the like are easily generated in the solidification process. In addition, the coarse grains directly cause the low tensile strength and deformability of the alloy, and limit the wider application of the alloy.
The grain refining technology can effectively improve the casting defects and simultaneously improve the strength and the toughness of the alloy. At present, the grain refining method of Mg-Al series as-cast alloy is mainly to add carbon (C) containing substance (C refiner) into the melt, and C reacts with the Mg-Al melt to generate Al with nucleation capability4C3. But due to the fact that for Al4C3The heterogeneous nucleation mechanism of (A) is not deeply known, so that a plurality of problems exist in the preparation and the use of the C-type refiner. Firstly, the preparation problem of the refiner is as follows: directly using C powder or Al4C3The introduction of C into Mg-Al in the form of ceramic particles has the problems of poor wettability with magnesium alloy melt, difficult reaction and the like; and introducing C into the Mg-Al melt2Cl6Harmful gas is generated, and the environment is seriously polluted; the preparation of a C-containing intermediate alloy is a better solution, and the Al-C intermediate alloy prepared by adopting a powder metallurgy method can solve the wettability of Al/C to a certain extent and promote the reaction to occur, but the product Al of the Al-C intermediate alloy4C3The size of the magnesium alloy is large, and when the content of C is high, the C-type refiner is not easy to melt in the magnesium alloy melt, and the preparation process is relatively complex. The second problem is that the Al-C intermediate alloy refiner obtained by the powder metallurgy process has larger variation of refining effect and has the effect of improving the Mg-containing material with low aluminum contentThe refining effects of the 3Al and the Mg-9Al alloy with high aluminum content are different, namely the refining efficiency has obvious dependence on the components of the Mg-Al alloy.
Therefore, how to prepare a catalyst containing fine Al by in situ reaction4C3The C-class refiner of the particles is the key to research and development of the C-class refiner. A literature search of the prior art shows that N.Q. Wu et Al, Journal of Alloys and Compounds, written "alloying in the Al-C system by mechanical alloying" indicates that high energy ball milling under certain conditions can cause mechanical alloying of Al and C to produce nanosized Al4C3Therefore, it is necessary to further study the principle and process of preparing the novel C-containing refiner by a high-energy ball milling method, especially study the rule of influence of key process parameters such as Al/C powder ratio, ball milling speed, ball milling time and the like on Al-C reaction process, product size and distribution.
Disclosure of Invention
The invention provides a simple and effective aluminum-coated nano Al for Mg-Al alloy4C3A granular grain refiner and a preparation method thereof. Solves the problems of complex preparation process, long refining response time and low refining efficiency of the common C-based refiner, and Al4C3The grain refiner has the advantages of large size, difficult dispersion in a melt and the like, and simultaneously has remarkable refining effect, and improves the dependence of the refining efficiency of the C-type grain refiner on Mg-Al alloy components.
The technical scheme of the invention is as follows:
aluminum-coated nano Al for Mg-Al alloy4C3The preparation method of the granular grain refiner comprises the steps of mixing Al powder, C powder and Mg powder according to the mass ratio of 6:2:1, firstly carrying out low-speed ball milling, and then carrying out vacuum intermittent high-energy ball milling; after ball milling, standing for a period of time, adding Al powder into a ball milling tank, and then performing high-speed coating molding ball milling; the prepared granular refiner is added into Mg-Al alloy melt to be refined, the addition amount of the granular refiner is controlled to be 0.2-1%, and after the granular refiner is kept for 5 minutes, the subsequent operation steps of argon refining, cooling pouring and the like can be carried out, so that a good grain refining effect can be obtained.
Compared with other preparation methods of C-type refiners, the preparation method has the advantages of simple preparation process, low production cost and Al product4C3Small size, uniform distribution under the action of Al coating and bonding, easy dispersion after being added into Mg-Al alloy melt, and improved Al content4C3The utilization ratio of (2). At the same time, due to Al4C3The size of the nanometer grade, the number of effective nucleation cores is increased, and the addition amount of the refiner can be reduced; the refining effect of the refiner does not depend on the components of Mg-Al alloy, and the C-type refiner prepared by the invention has good refining effect on Mg-3Al alloy with low Al content or Mg-9Al alloy with high Al content, and obviously improves the strength and the toughness.
Drawings
FIG. 1 is a macroscopic view of a granular, mass C, refiner made according to the present invention.
FIG. 2 is a microstructure view of a Mg-3Al alloy to which no refiner is added.
FIG. 3 is a microstructure of the Mg-3Al alloy after 0.2wt.% refiner.
FIG. 4 is a microstructure view of a Mg-9Al alloy to which no refiner is added.
FIG. 5 is a microstructure of the Mg-9Al alloy after the addition of 0.2wt.% refiner.
Detailed Description
The present invention is further illustrated in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
Aluminum-coated nano Al for Mg-Al alloy4C3A particulate grain refiner comprising the steps of:
(1) determination of mixture ratio of mixed powder and ball-material ratio
Weighing 15g of Al powder, 5g of C powder and 2.5g of Mg powder, and weighing ZrO powders with diameters of 10mm, 8mm and 6mm respectively2Grinding balls of 80g are put into a ball milling tank and then the ball milling tank is put at a low speedMixing powder, wherein the ball milling rotating speed is 200r/min, and the ball milling time is 60 min.
(2) High speed intermittent ball mill
And (3) carrying out vacuum pumping treatment on the ball milling tank subjected to low-speed ball milling in the step (1) by adopting a common mechanical pump for 5 min. And then carrying out high-speed intermittent ball milling, wherein the ball milling speed is 500r/min, the ball milling time is 80h, and the stopping time is 20min every 5 h.
(3) Molding cladding ball mill
After the high-speed intermittent ball milling is finished, standing the ball mill for 24 hours, opening a ball milling tank, and adding 77.5g of Al powder and 320g of grinding balls with three specifications; sealing the ball milling tank, vacuumizing for 5min, and continuously performing high-speed intermittent ball milling at a ball milling speed of 800r/min for 60min, and stopping for 5min every 10 min. After the ball milling is finished, the aluminum-coated nano Al can be obtained4C3A granular grain refiner.
(4) Refinement effect verification
Preheating a crucible and Mg and Al cast ingots, adding pure Mg when the crucible is heated to 500 ℃, adding 3 percent of pure Al and 9 percent of pure Al after Mg is melted, and scattering RJ-2 covering agent on the surface. The temperature of the melt is raised to 690 ℃, a refiner (the mass fraction is 0.5%) is scattered on the surface of the melt, and the melt is simply stirred to ensure that Al in large particles4C3Effectively dispersing and keeping the temperature for 2-5 minutes. Refining with high-purity argon for 1 minute, cooling to 670 deg.C, and pouring at 640 deg.C into a metal mold to obtain a bar material with diameter of 55 × 140 mm.
The metallographic phase and mechanical properties of the Mg-3Al and Mg-9Al alloys before and after the thinning are respectively shown in Table 1 and FIGS. 2 to 5. The refining effect of the refiner obtained in examples 2-4 is equivalent to that of example 1, and is not listed.
Example 2
Aluminum-coated nano Al for Mg-Al alloy4C3A particulate grain refiner comprising the steps of:
(1) determination of mixture ratio of mixed powder and ball-material ratio
Weighing 20g of Al powder, 5g of C powder and 2.5g of Mg powder, and weighing ZrO powder with diameters of 10mm, 8mm and 6mm respectively2And (3) grinding balls of 90g are filled into a ball milling tank and then mixed at a low speed, the ball milling speed is 200r/min, and the ball milling time is 60 min.
(2) High speed intermittent ball mill
And (3) carrying out vacuum pumping treatment on the ball milling tank subjected to low-speed ball milling in the step (1) by adopting a common mechanical pump for 5 min. And sealing, and performing high-speed intermittent ball milling at the ball milling speed of 500r/min for 100h and 20min for every 5 h.
(3) Molding cladding ball mill
After the high-speed intermittent ball milling is finished, standing the ball mill for 24 hours, opening a ball milling tank, and adding 72.5g of Al powder and 320g of grinding balls with three specifications; sealing the ball milling tank, vacuumizing for 5min, and continuously performing high-speed intermittent ball milling at a ball milling speed of 800r/min for 60min, and stopping for 5min every 10 min. After the ball milling is finished, the aluminum-coated nano Al can be obtained4C3A granular grain refiner.
(4) Refinement effect verification
Preheating a crucible and Mg and Al cast ingots, adding pure Mg when the crucible is heated to 500 ℃, adding 3 percent of pure Al and 9 percent of pure Al after Mg is melted, and scattering RJ-2 covering agent on the surface. Heating the melt to 690 deg.C, adding a refiner (0.5 wt.%) to the surface of the melt, and simply stirring the melt to obtain Al powder4C3Effectively dispersing and keeping the temperature for 2-5 minutes. Refining with high-purity argon for 1 minute, cooling to 670 deg.C, and pouring into mold at 640 deg.C to obtain bar stock of 55 mm in diameter and 140mm in diameter.
Example 3
Aluminum-coated nano Al for Mg-Al alloy4C3A particulate grain refiner comprising the steps of:
(1) determination of mixture ratio of mixed powder and ball-material ratio
Weighing 20g of Al powder, 5g of C powder and 2.5g of Mg powder, and weighing ZrO powder with diameters of 10mm, 8mm and 6mm respectively2And (3) grinding balls of 90g are filled into a ball milling tank and then mixed at a low speed, the ball milling speed is 200r/min, and the ball milling time is 60 min.
(2) High speed intermittent ball mill
And (3) carrying out vacuum pumping treatment on the ball milling tank subjected to low-speed ball milling in the step (1) by adopting a common mechanical pump for 5 min. And sealing, and performing high-speed intermittent ball milling at the ball milling speed of 600r/min for 80h and stopping for 20min every 5 h.
(3) Molding cladding ball mill
After the high-speed intermittent ball milling is finished, standing the ball mill for 24 hours, opening a ball milling tank, and adding 72.5g of Al powder and 320g of grinding balls with three specifications; sealing the ball milling tank, vacuumizing for 5min, and continuously performing high-speed intermittent ball milling at a ball milling speed of 800r/min for 60min, and stopping for 5min every 10 min. After the ball milling is finished, the aluminum-coated nano Al can be obtained4C3A granular grain refiner.
(4) Refinement effect verification
Preheating a crucible and Mg and Al cast ingots, adding pure Mg when the crucible is heated to 500 ℃, adding 3 percent of pure Al and 9 percent of pure Al after Mg is melted, and scattering RJ-2 covering agent on the surface. Heating the melt to 690 deg.C, adding a refiner (0.5 wt.%) to the surface of the melt, and simply stirring the melt to obtain Al powder4C3Effectively dispersing and keeping the temperature for 2-5 minutes. Refining with high-purity argon for 1 minute, cooling to 670 deg.C, and pouring into mold at 640 deg.C to obtain bar stock of 55 mm in diameter and 140mm in diameter.
Example 4
Aluminum-coated nano Al for Mg-Al alloy4C3A particulate grain refiner comprising the steps of:
(1) determination of mixture ratio of mixed powder and ball-material ratio
Weighing 15g of Al powder, 5g of C powder and 2.5g of Mg powder, and weighing ZrO powders with diameters of 10mm, 8mm and 6mm respectively2And (4) grinding balls of 80g are filled into a ball milling tank and then mixed at a low speed, the ball milling speed is 200r/min, and the ball milling time is 60 min.
(2) High speed intermittent ball mill
And (3) carrying out vacuum pumping treatment on the ball milling tank subjected to low-speed ball milling in the step (1) by adopting a common mechanical pump for 5 min. And sealing, and performing high-speed intermittent ball milling at the ball milling speed of 400r/min for 100h and 20min for every 5 h.
(3) Molding cladding ball mill
After the high-speed intermittent ball milling is finished, standing the ball mill for 24 hours, opening a ball milling tank, and adding 77.5g of Al powder and 320g of grinding balls with three specifications; sealing the ball milling tank, vacuumizing for 5min, and continuing to perform high-speed processAnd (4) intermittent ball milling, wherein the ball milling speed is 800r/min, the ball milling time is 60min, and the ball milling is stopped for 5min every 10 min. After the ball milling is finished, the aluminum-coated nano Al can be obtained4C3A granular grain refiner.
(4) Refinement effect verification
Preheating a crucible and Mg and Al cast ingots, adding pure Mg when the crucible is heated to 500 ℃, adding 3 percent of pure Al and 9 percent of pure Al after Mg is melted, and scattering RJ-2 covering agent on the surface. Heating the melt to 690 deg.C, adding a refiner (0.5 wt.%) to the surface of the melt, and simply stirring the melt to obtain Al powder4C3Effectively dispersing and keeping the temperature for 2-5 minutes. Refining with high-purity argon for 1 minute, cooling to 670 deg.C, and pouring into mold at 640 deg.C to obtain bar stock of 55 mm in diameter and 140mm in diameter.
TABLE 1 grain size and tensile Properties of Mg-3/9Al alloy before and after addition of refiner
| Grain size (μm) | Tensile strength (MPa) | Elongation (%) | |
| Mg-3Al without refiner | 298 | 165.8 | 8.3 |
| Mg-3Al addition refiner | 140 | 189.1 | 10.9 |
| Mg-9Al without refiner | 185 | 183.2 | 5.9 |
| Mg-9Al addition refiner | 87 | 210.6 | 8.7 |
As can be seen from the comparison of FIG. 2 with FIG. 3 and FIG. 4 and Table 1, the refining method of the present invention can obviously refine the grain sizes of Mg-3Al and Mg-9Al alloys and effectively improve the mechanical properties of the alloys.
Although preferred embodiments have been depicted and described in detail herein, it will be understood by those skilled in the relevant art that the present invention is not limited to the embodiments described above, and that various changes and modifications can be made without departing from the spirit of the invention, which are intended to be within the scope of the invention as defined by the appended claims.
Claims (9)
1. Aluminum-coated nano Al for Mg-Al alloy4C3The granular grain refiner is characterized in that the refiner is Al-C-Mg composite metal particles, and the mass percentage of the elements is 80-97% of Al, C: 2-10%, Mg: 1 to 10 percent.
2. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 14C3A granular grain refiner, characterized in that the process is carried out according to the following steps:
1) low-speed ball milling and powder mixing in advance: mixing a certain amount of Al powder, C powder and Mg powder with ZrO according to a certain proportion2Putting the grinding balls into a ball milling tank together, carrying out low-speed ball milling and powder mixing, and stopping ball milling for about 30-60 min;
2) carrying out vacuum pumping treatment on the ball milling tank, and carrying out high-speed intermittent ball milling for a certain time;
3) standing for a period of time after the ball milling is finished, opening a ball milling tank, and adding a certain amount of ZrO2Balls and Al powder;
4) sealing the ball milling tank, and continuing to perform high-speed intermittent ball milling for a certain time after vacuumizing.
3. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 24C3The preparation method of the granular grain refiner is characterized in that the mass parts of Al powder, C powder and Mg powder which are added in the step 1 are 10-30 parts, 2-10 parts and 1-10 parts respectively based on 100 parts by mass of the prepared target C-type refiner. The mass ratio of the ball materials in the step 1 is not less than 3:1, and the ball milling speed is 100-200 r/min.
4. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 24C3The preparation method of the granular grain refiner is characterized in that the high-speed ball milling speed in the step 2 is 300 r/min-800 r/min, the ball milling time is 20 h-100 h, and the gap time of every 5h is 10-30 min.
5. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 24C3The preparation method of the granular grain refiner is characterized in that the Al powder added in the step 3 accounts for 80-90 percent of the total mass, and ZrO is added2The quality of the balls ensures that the total ball-to-material ratio is not lower than 3: 1.
6. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 24C3The preparation method of the granular grain refiner is characterized in that the ball milling speed in the step 4 is 400 r/min-800 r/min, the ball milling time is 30-120min, and the gap time of every 10min is 5-20 min.
7. A process for the preparation of Mg-Al system as claimed in claim 1Aluminum-coated nano Al of alloy4C3The application of the granular grain refiner is characterized in that the addition amount of the granular grain refiner in the Mg-Al alloy is 0.2-1% of the mass of the Mg-Al alloy.
8. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 64C3The application of the granular grain refiner is characterized by comprising the following steps:
1) heating the Mg-Al alloy under the protection of a covering agent until the alloy is completely melted;
2) heating the melt to 680-720 ℃;
3) adding a granular C-type refiner into the Mg-Al alloy melt, and keeping the temperature for 5-10 min;
4) and refining the melt by inert gas, slagging off and casting into a preheated metal mold.
9. The aluminum-coated nano Al for Mg-Al system alloy as claimed in claim 74C3Use of a particulate grain refiner, characterized in that in step 4) the inert gas is high purity argon.
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| CN1410566A (en) * | 2002-11-25 | 2003-04-16 | 山东大学 | Fining agent used for magnesium alloy and its preparation method |
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