| Certification: | ISO |
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| Shape: | Block |
| Purification Method: | Electromigration |
| Preparation Method: | Metallothermic Reductio |
| Application: | Catalyst Masses, Photoelectric Material, Photorecording Material, Computer |
| Product Type: | Rare Earth Metal |
| Samples: |
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| Customization: |
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Aluminum-zirconium alloy with high strength, high plasticity, good toughness and corrosion resistance and other excellent properties, and is widely used in aerospace, electric power and ship and other fields. The commonly used preparation methods of aluminum-zirconium alloy include mechanical alloying, admixture, combustion synthesis and molten salt electrolysis.
3. Mechanical alloying method is based on zirconium powder and aluminum powder as raw materials, in the high-energy ball mill for a long time, through the interatomic diffusion and solid chemical reaction and other physical and chemical processes to form aluminum-zirconium alloy powder. This method uses expensive metal zirconium as raw material, resulting in high cost, and the product is powder, need to be processed again before practical application.
4. Admixture method is also called fusion method, which is to melt sponge zirconium and aluminum in an electric furnace, and then prepare intermediate alloy with a certain proportion, and then prepare the intermediate alloy and aluminum into the required components of aluminum-zirconium alloy. Because zirconium has a higher melting point, remelting adds energy and costs.
5. Combustion synthesis method: zr powder and al powder are pressed, heated and ignited to generate Al zirconium alloy by self-spreading reaction. This method has high production efficiency, but the cost of using zr powder as raw material is high, and zr powder is easy to absorb oxygen in the reaction process.
6. Molten salt electrolysis method: zirconium dioxide, aluminum powder, potassium zirconium fluoride, cryolite furnace heating to the melting state of the reaction to produce aluminum-zirconium alloy, this method has a low cost, but the reaction produced by the salt by-product is difficult to completely remove, and the yield is relatively low.
7. The patent document cn1514044a discloses a method of electrolytic production of aluminum-zirconium alloy. The method takes aluminum and zirconium oxide as raw materials and forms aluminum-zirconium alloy directly after electrolytic precipitation in cryolite system. Zirconium content in the alloy is 0.8-3wt %, al+zr≥98.5wt %. The patent document cn105274372a discloses a preparation method of aluminum-zirconium alloy. The method uses aluminum-calcium alloy as a compound reducing agent, zirconium dioxide as raw material, cratite, potassium hexafluorozirconate and sodium chloride as covering agent. After reduction, the content of zirconium in the alloy is 4-7wt %, al+zr≥99wt %.
8. The above aluminum-zirconium alloy preparation process is carried out in the furnace, which has high energy consumption and low zirconium content in the obtained alloy.
Technical implementation elements:
9. The purpose of the invention is to provide a preparation method of aluminum-zirconium intermediate alloy. The method is an external thermite reduction method with low energy consumption and can obtain aluminum-zirconium intermediate alloy with zirconium content up to 45 ~ 55wt %.
10. To realize the above purpose, the invention adopts the following technical scheme:
11. A preparation method for an aluminum-zirconium intermediate alloy consists of the following steps:
12.(1) Using zirconia as raw material, aluminum powder, aluminum-calcium-alloy powder or aluminum-magnesium alloy powder as reducing agent, potassium chlorate as oxidant, calcium oxide and calcium fluoride as slagging agent, zirconia, reducing agent, potassium chlorate, calcium oxide and calcium fluoride are mixed evenly in a certain proportion, loaded into the crucible and compacted;
13.(2) Use magnesium dust or magnesium powder to in the upper part of the charge, and the reaction will be spontaneous until the end of the reaction. Then the aluminum zirconium intermediate alloy can be obtained by crushing and separating.
14. In the present invention, the oxidizing agent potassium chlorate can react with reducing agent aluminum powder, aluminum-calcium alloy powder or aluminum-magnesium alloy powder to exothermic heat, providing sufficient heat for the melting of reaction products. Preferably, the calorific value of the unit charge in step (2) is 2800
~ 3800kj/kg.
15. In the present invention, on the one hand, the reducing agent should completely reduce zirconia, and on the other hand, it should react with the oxidizer to exothermic heat to provide enough heat for the system. The amount of calcium oxide and calcium fluoride added is al2o
3-cao phase diagram and al2o
3-caf2 phase diagram basis. Preferably, the mass ratio of each raw material component in step (1) is as follows: zirconia: aluminum powder: oxidizer: calcium oxide: calcium fluoride = 80 ~ 110∶100 ~ 150∶60 ~ 80∶30 ~ 60∶10 ~ 25.
16. In the present invention, the zirconia is powder with purity ≥95wt % and particle size ≤1mm. The reducing agent is preferably aluminum powder with purity ≥95wt % and particle size ≤1mm.
17. The oxidizer of the invention is industrial grade potassium chlorate with a purity greater than 95wt %; Slagging agents calcium oxide and calcium fluoride are industrial grade with purity greater than 95wt %.
18. In the present invention, the crucible may be made of alumina, corundum or magnesium oxide.
19. The advantages of the invention lie in:
20. The invention can prepare aluminum-zirconium intermediate alloy with low impurity content and high zirconium content through the control of raw material composition, ratio and reaction thermal effect, zirconia reduction, aluminum-zirconium alloying and slag gold separation in one step. The main component of the aluminum-zirconium intermediate alloy prepared by the invention is al3zr, zirconium content up to 45 ~ 55wt %, al+zr≥99wt %. The preparation process of the invention has no pollution, low cost, high production efficiency, simple and feasible technology without equipment limitation, and the product composition is stable.
Attached drawing description
21. Figure 1 is a schematic diagram of the equipment structure used in the method of the invention.
Specific mode of implementation
22. The invention is further explained in combination with the attached drawings and embodiments. It should be emphasized that the following instructions are illustrative only and are not intended to limit the scope and application of the invention.
23. As shown in Figure 1, the equipment used in the method of the present invention includes an iron barrel 1, a crucible 3 arranged in an iron barrel 1, a magnesia 2 filled between an iron barrel 1 and a crucible 3, a charge 4 placed in a crucible 3, and a magnesium chip or powder 5 used for igniting the charge placed on the upper part of the charge 4.
24. Example 1
25. Firstly, 50g zirconia, 70g aluminum, 45g potassium chlorate, 20g calcium oxide and 8g calcium fluoride are mixed evenly. The unit caloric value of the charge is 3800kj/kg; Then put the charge in the ceramic crucible and compact the crucible with sand around it. Add magnesium powder to the upper part of the charge and the reaction. After the reaction is over, cool to room temperature and the broken products get alloy ingots. The yield of the alloy is 68.7%, the phase is al3zr and al, the content of zr reaches 50.8wt %, zr+al = 99.5wt %.
26. Embodiment 2
27. Firstly, 100g zirconia, 140g aluminum, 80g potassium chlorate, 40 calcium oxide and 15g calcium fluoride are mixed evenly. The unit caloric value of the charge is 3600kj/kg; Then put the charge in the ceramic crucible and compact the crucible with sand around it. Add magnesium powder to the upper part of the charge and the reaction. After the reaction is over, cool to room temperature and the broken products get alloy ingots. The alloy yield is 73.9%, the phase is al3zr and al, the content of zr reaches 52.5wt %, zr+al = 99.4wt %.
28. Example 3
29. Firstly, 500g zirconia, 700g aluminum-magnesium alloy powder, 356g potassium chlorate, 200g calcium oxide and 80g calcium fluoride are evenly mixed. The unit caloric value of the charge is 3300kj/kg; Then put the charge in the ceramic crucible and compact the crucible with sand around it. Add magnesium powder to the upper part of the charge andthe reaction. After the reaction is over, cool to room temperature and the broken products get alloy ingots.
The yield of the alloy is 77.7%, the phase is al3zr and al, the content of zr reaches 53.3wt %, zr+al = 99.7wt %.
30. Example 4
31. Firstly, 2kg zirconia, 2.988kg aluminum-calcium alloy powder, 1.214kg potassium chlorate, 0.8kg calcium oxide and 0.32kg calcium fluoride are evenly mixed. The unit calorific value of the charge is 3000kj/kg. Then put the charge in the ceramic crucible and compact the crucible with sand around it. Add magnesium powder to the upper part of the charge andthe reaction. After the reaction is over, cool to room temperature and the broken products get alloy ingots. The alloy yield is 83.7%, the phase is al3zr and al, the content of zr reaches 54.1wt %, zr+al = 99.8wt %.
32. Example 5
33. Firstly, 10kg zirconia, 14.65kg aluminum, 6.51kg potassium chlorate, 4kg calcium oxide and 1.6kg calcium fluoride are mixed evenly. The unit calorific value of the charge is 2800kj/kg; Then put the charge in the ceramic crucible and compact the crucible with sand around it. Add magnesium powder to the upper part of the charge andhe reaction. After the reaction is over, cool to room temperature and the broken products get alloy ingots. The alloy yield is 90.7%, the phase is al3zr and al, the content of zr reaches 54.6wt %, zr+al = 99.8wt %.
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