CN117265271B - Aluminum-molybdenum-silicon alloy and production method thereof - Google Patents
Aluminum-molybdenum-silicon alloy and production method thereofInfo
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- CN117265271B CN117265271B CN202311408165.8A CN202311408165A CN117265271B CN 117265271 B CN117265271 B CN 117265271B CN 202311408165 A CN202311408165 A CN 202311408165A CN 117265271 B CN117265271 B CN 117265271B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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Abstract
The invention relates to the field of alloy materials, and discloses an aluminum-molybdenum-silicon alloy and a production method thereof. The alloy contains 35-45 wt% of molybdenum, 4-10 wt% of silicon, the balance of aluminum, less than or equal to 0.05 and wt% of iron, less than or equal to 0.02 and wt% of carbon, less than or equal to 0.01 and wt% of oxygen and less than or equal to 0.005 and wt% of nitrogen. The method comprises the steps of mixing molybdenum trioxide and byproduct sodium silicate solution in proportion, stirring uniformly, then slowly adding ammonium sulfate solution, adjusting pH, reacting at high temperature, carrying out reduced pressure suction filtration on the reaction solution, washing, drying and sintering to obtain MoO 3/SiO2 compound, mixing MoO 3/SiO2 compound and aluminum powder in proportion uniformly, and carrying out vacuum aluminothermic reaction to obtain the aluminum-molybdenum-silicon alloy. The invention prepares MoO 3/SiO2 compound by taking low modulus water glass solution containing sodium molybdate as a byproduct in molybdenum industry as a raw material, prepares the aluminum-molybdenum-silicon ternary alloy with high uniformity and low impurity content by a vacuum aluminothermic method, solves the problems of serious segregation and overhigh content of oxygen and nitrogen elements in the traditional aluminothermic reaction production of the aluminum-molybdenum-silicon ternary intermediate alloy while realizing comprehensive utilization of resources, and provides a new thought for the production of the aluminum-molybdenum-silicon ternary intermediate alloy.
Description
Technical Field
The invention relates to the technical field of alloy materials, in particular to an aluminum-molybdenum-silicon alloy and a production method thereof.
Background
The sodium silicate content in the conventional water glass solution is 56-60 wt% and the modulus is 1.5-3.5, so that the water glass solution is a common adhesive in industry. In the industrial molybdenum production process, byproduct sodium silicate solution (containing 20 wt% of sodium molybdate) is prepared, the sodium silicate content is 35: 35 wt%, and the sodium silicate modulus is 0.4-1.5. The sodium molybdate content in the byproduct sodium silicate solution is too high, the modulus is too low, the sodium molybdate can not be used as a conventional binder, the subsequent treatment is difficult, the resource waste is caused, and the environment is polluted.
CN1629331a discloses an aluminium molybdenum silicon intermediate alloy and its preparation method, using aluminium, metallic silicon, molybdenum oxide, potassium chlorate and calcium fluoride as raw materials, producing aluminium molybdenum silicon alloy by aluminium thermal reduction method, the alloy contains many impurities, the gas impurity content is high, the quality is lower, CN101037741 discloses a vacuum level aluminium molybdenum silicon alloy production method, preparing aluminium thermal method first grade alloy by aluminium thermal reduction method, further refining the first grade alloy in medium frequency vacuum induction furnace to obtain aluminium molybdenum silicon alloy ingot, but the segregation of molybdenum element in upper and lower parts of the produced aluminium molybdenum silicon alloy ingot is larger, between 1-2.5 wt%, and the alloy quality is affected by aluminium thermal method molten pool material, medium frequency vacuum induction furnace crucible material, there is quality hidden trouble in the use process of high quality titanium alloy.
Therefore, how to provide an aluminum-molybdenum-silicon alloy with high quality and simple and easy production method is a problem to be solved by workers in the field.
Disclosure of Invention
In view of the above, the invention provides an aluminum-molybdenum-silicon alloy and a production method thereof, and the invention can produce a high-quality aluminum-molybdenum-silicon alloy, thereby solving the problems of more impurities, high gas impurity content and serious segregation of the aluminum-molybdenum-silicon alloy produced by the aluminothermic method.
Specifically, the invention takes molybdenum industry byproduct sodium silicate solution as raw material, prepares MoO 3/SiO2 compound with uniform dispersion through treatment, and greatly improves the mixing uniformity and stability of the MoO 3/SiO2 compound state in a mixer compared with the conventional state, thereby ensuring the high uniformity of the produced alloy ingot. And aluminum-molybdenum-silicon intermediate alloy with high purity and low gas impurity content is prepared through vacuum aluminothermic reaction, so that key material guarantee is provided for high-end titanium alloy materials in China.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a production method of an aluminum-molybdenum-silicon alloy, which comprises the following steps:
1. Adding molybdenum trioxide into a byproduct sodium silicate solution according to a proportion, and fully and uniformly stirring to obtain a suspension;
2. Slowly adding an ammonium sulfate solution into the suspension, stirring uniformly after the material feeding is completed, transferring into a high-pressure reaction kettle after the pH is regulated, carrying out vacuum filtration on the mixed solution after the reaction at a high temperature, and washing, drying and sintering to obtain a MoO 3/SiO2 compound;
3. Mixing the MoO 3/SiO2 compound and aluminum powder in proportion, fully and uniformly mixing, loading into a crucible of a vacuum aluminothermic furnace, closing the furnace body, starting a Roots pump, vacuumizing, heating by a resistance wire to ignite furnace burden in the crucible, performing vacuum aluminothermic reaction, and opening the furnace and removing slag to obtain an aluminum-molybdenum-silicon alloy ingot after the reaction is completed.
Preferably, the sodium silicate content in the byproduct water glass solution is 35wt%, the water glass modulus is 0.4-1.5, and the sodium molybdate content is 20 wt%.
Preferably, the weight ratio of the molybdenum trioxide to the water glass solution is (3.8-5.4): 10, and the MoO 3/SiO2 compound with corresponding proportion can be prepared by supplementing the molybdenum trioxide according to the content requirement of the aluminum-molybdenum-silicon alloy.
Preferably, the suspension is stirred at 20-80 rpm/min to 30-60 min to ensure that the molybdenum trioxide is uniformly dispersed in the water glass solution.
Preferably, the content of ammonium sulfate in the ammonium sulfate solution is 50-65wt%, the weight ratio of the ammonium sulfate solution to the byproduct sodium silicate solution is (3.9-5.2): 10, and the ammonium sulfate feeding amount is determined based on the reaction formula of sodium molybdate and ammonium sulfate.
Na2MoO4 + (NH4)2SO4 → (NH4)2MoO4 + Na2SO4
Preferably, the pH of the suspension is adjusted to be 1.2-1.8 by using 35% hydrochloric acid solution, so that hydrochloric acid reacts with sodium silicate to neutralize the alkalinity of the suspension and generate a large amount of silicon oxide seed crystals.
Na2O·nSiO2 + 2HCl → 2NaCl + H2O + nSiO2
Preferably, transferring the suspension into a high-pressure reaction kettle to react for 20-36 hours at 200-230 ℃ so that ammonium molybdate grows on silicon oxide in situ.
Preferably, after the reaction is finished, a filter cake is obtained through decompression and suction filtration, high-purity water is used for washing until the pH value of a washing solution is more than 6.8, excessive hydrochloric acid and sodium chloride are washed, the filter cake is dried at 70-80 ℃ for 10-24 h, moisture in the filter cake is removed, the filter cake is transferred to a muffle furnace at 400-550 ℃ to decompose ammonium molybdate to generate molybdenum trioxide, the molybdenum trioxide grows on the surface of silicon oxide in situ, and the MoO 3/SiO2 compound which is uniformly dispersed is obtained after heat preservation is carried out on 8-12 h.
(NH4)2MoO4 → 2NH3（g）+ H2O（g） + MoO3(s)
Preferably, the iron content in the aluminum powder is less than 0.02 wt%, so that the iron content in the aluminum powder is prevented from exceeding the standard due to the fact that the iron content in the aluminum powder is too high.
Preferably, the mass ratio of the MoO 3/SiO2 compound to the aluminum powder is (0.72-1.07): 1, so that the vacuum thermit reaction is ensured to be smoothly carried out, and the alloy content is in a control range.
Preferably, the crucible in the vacuum aluminothermic furnace is made of red copper, so that impurities are prevented from being introduced into the alloy due to the problem of the crucible, a mechanical pump is turned off, a furnace body is turned on, vacuum pumping is performed until the vacuum degree is less than 300 Pa, so that gas impurities such as oxygen and nitrogen are prevented from being introduced into the alloy, meanwhile, high vacuum provides negative pressure conditions for alloy melt, aluminum oxide is favorably mixed and separated from an alloy ingot, the resistance wire is made of metal chromium, high-resistivity metal wires are favorably used for rapid ignition reaction, and vacuum heat preservation is performed for 3-5 hours after the vacuum aluminothermic reaction is completed.
The content of the aluminum-molybdenum-silicon alloy produced by the method is 35-45 wt percent of molybdenum, 4-10 wt percent of silicon, the balance of aluminum is less than or equal to 0.05 and wt percent of iron, less than or equal to 0.02 and wt percent of carbon, less than or equal to 0.01 and wt percent of oxygen and less than or equal to 0.005 and wt percent of nitrogen.
Compared with the prior art, the aluminum-molybdenum-silicon alloy and the production method thereof provided by the invention have the following excellent effects:
The invention prepares MoO 3/SiO2 compound by taking low modulus water glass solution containing sodium molybdate as a byproduct in molybdenum industry as a raw material, prepares the aluminum-molybdenum-silicon ternary alloy with high uniformity and low impurity content by a vacuum aluminothermic method, solves the problems of serious segregation and overhigh content of oxygen and nitrogen elements in the traditional aluminothermic reaction production of the aluminum-molybdenum-silicon ternary intermediate alloy while realizing comprehensive utilization of resources, and provides a new thought for the production of the aluminum-molybdenum-silicon ternary intermediate alloy.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is SEM image (a) and TEM image (b) of MoO 3/SiO2 complex prepared in example 1.
FIG. 2 is a graph of multipoint sampling of an Al-Mo-Si alloy.
FIG. 3 is an SEM image (a) and a gold phase diagram (b) of an Al-Mo-Si alloy produced in example 1.
FIG. 4 is SEM image (a) and TEM image (b) of MoO 3/SiO2 complex prepared in example 2.
FIG. 5 is an SEM image (a) and a gold phase diagram (b) of an Al-Mo-Si alloy produced in example 2.
Fig. 6 is a metallographic diagram of an aluminum-molybdenum-silicon alloy prepared by the aluminothermic method of comparative example 1.
Fig. 7 is a metallographic diagram of an aluminum-molybdenum-silicon alloy prepared by the medium frequency vacuum induction melting method of comparative example 2.
FIG. 8 is SEM image (a) and TEM image (b) of MoO 3/SiO2 complex prepared in example 3.
FIG. 9 is an SEM image (a) and a gold phase diagram (b) of an Al-Mo-Si alloy produced in example 3.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The word "embodiment" as used herein does not necessarily mean that any embodiment described as "exemplary" is preferred or advantageous over other embodiments. Performance index testing in the examples of the present application, unless otherwise specified, was performed using conventional testing methods in the art. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure.
Unless otherwise defined, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs, and other test methods and techniques not specifically mentioned herein are meant to be common to those of ordinary skill in the art.
Numerous specific details are set forth in the following examples in order to provide a better understanding of the present application. It will be understood by those skilled in the art that the present application may be practiced without some of these specific details. In the examples, some methods, means, instruments, devices, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present application.
On the premise of no conflict, the technical features disclosed by the embodiment of the application can be combined at will, and the obtained technical scheme belongs to the disclosure of the embodiment of the application.
The present invention will be further specifically illustrated by the following examples, which are not to be construed as limiting the invention, but rather as falling within the scope of the present invention, for some non-essential modifications and adaptations of the invention that are apparent to those skilled in the art based on the foregoing disclosure.
Example 1
A production method of high-quality aluminum-molybdenum-silicon alloy comprises the following steps:
Molybdenum trioxide 50 kg is added into a 100 kg byproduct sodium silicate solution (sodium silicate content 35 wt%, sodium silicate modulus 0.7, sodium molybdate content 20 wt%), stirring is started, 40 min is stirred at 40 rpm/min, 55 wt% ammonium sulfate solution 46.7 kg is added into the suspension, after uniform mixing, the pH of the mixed solution is regulated to 1.5 by hydrochloric acid, the mixed solution is transferred to a high-pressure reaction kettle, and the high-pressure reaction degree is reacted at 210 ℃ for 24 h. After the reaction was completed, the mixed solution was subjected to suction filtration under reduced pressure, washed with high purity water until the effluent pH became 6.85, and the filter cake was transferred to a forced air drying oven and dried at 75 ℃ for 12 h. Further, the filter cake was kept at 500 ℃ in a muffle furnace for 10 h hours, 77.9 kg of MoO 3/SiO2 complex was obtained, and SEM and TEM patterns of the MoO 3/SiO2 complex were shown in FIG. 1.
The SEM (a) of figure 1 shows that the silicon oxide in the MoO 3/SiO2 compound coats the molybdenum trioxide micro-rods, and a certain agglomeration phenomenon exists in a microscopic state. According to the TEM spectrum (b) in the figure 1, the surface of the molybdenum trioxide is fully coated by the silicon oxide, and compared with the conventional state, the mixing uniformity and stability of the molybdenum trioxide and the silicon oxide in a mixer are greatly improved in the MoO 3/SiO2 composite state, so that the uniformity of an alloy ingot is ensured.
And (3) fully and uniformly mixing 77.9 kg of MoO 3/SiO2 compound and 83.3 kg aluminum powder (iron: 0.011 wt%), then placing the mixture into a crucible of a vacuum aluminothermic furnace, closing a furnace body, starting a Roots pump, vacuumizing until the air pressure in the furnace is 250 Pa, taking chromium wires as heating sources to ignite materials to perform vacuum aluminothermic reaction, cooling by 4h after the reaction is completed, opening the furnace, and deslagging to obtain an aluminum-molybdenum-silicon alloy ingot 99.2 kg.
Example 2
A production method of high-quality aluminum-molybdenum-silicon alloy comprises the following steps:
The byproduct sodium silicate solution in the example 1 is only added with molybdenum trioxide 50 kg to obtain MoO 3/SiO2 compound 79.5 kg, and the vacuum aluminothermic reaction ingredients are changed into MoO 3/SiO2 compound 77.5 kg and 83.4 kg aluminum powder to complete the reaction to obtain aluminum molybdenum silicon alloy ingot 99.3 kg.
The SEM and TEM patterns of the MoO 3/SiO2 compound are shown in figure 4, and the observation shows that the silicon oxide uniformly coats the molybdenum trioxide micro rods.
Example 3
A production method of high-quality aluminum-molybdenum-silicon alloy comprises the following steps:
The preparation method comprises the steps of adding molybdenum trioxide 42 kg into a byproduct water glass solution with the modulus of 1 in the embodiment 1 to obtain MoO 3/SiO2 compound 72.9 kg, and changing the vacuum aluminothermic reaction ingredients into MoO 3/SiO2 compound 72.9 kg and 86 kg aluminum powder to obtain an aluminum-molybdenum-silicon alloy ingot 98.6 kg.
The SEM and TEM patterns of the MoO 3/SiO2 compound are shown in figure 8, and the observation shows that the silicon oxide uniformly coats the molybdenum trioxide micro rods.
In order to further demonstrate the beneficial effects of the present invention for a better understanding of the present invention, the technical features disclosed herein are further illustrated by the following comparative examples, which are not to be construed as limiting the present invention. Other modifications of the invention which do not involve the inventive work, as would occur to those skilled in the art in light of the foregoing teachings, are also considered to be within the scope of the invention.
Comparative example 1
Uniformly mixing aluminum powder 83.25 kg, molybdenum trioxide 63.9 kg, aluminum powder 69 kg and potassium chlorate 14.1 kg according to a proportion, placing the mixture into a molten pool formed by corundum transfer, igniting the mixture by using a magnesium strip, and cooling the mixture to obtain an aluminum-molybdenum-silicon alloy ingot 96.4 kg.
Comparative example 2
The thermite alloy of example 1 was melted in an intermediate frequency vacuum induction furnace under the conditions of a pre-melting vacuum of 0.58 Pa, an argon shield vacuum of 80 Pa during melting, a melting temperature of 1480 ℃, a refining temperature of 1550 ℃ and a refining time of 10 min.
The aluminum-molybdenum-silicon alloy ingots prepared in the above examples and comparative examples were sampled at multiple points according to fig. 2, and the experimental results are shown below:
TABLE 1 analysis of the results of sampling of the Al-Mo-Si alloy produced in example 1
| Test number | Mowt% | Siwt% | Al | Fewt% | Cwt% | Owt% | Nwt% |
| 1 | 42.66 | 6.60 | Allowance of | 0.021 | 0.018 | 0.006 | 0.005 |
| 2 | 42.15 | 6.35 | Allowance of | 0.023 | 0.016 | 0.009 | 0.004 |
| 3 | 42.27 | 6.65 | Allowance of | 0.021 | 0.014 | 0.009 | 0.004 |
| 4 | 42.75 | 6.45 | Allowance of | 0.019 | 0.013 | 0.01 | 0.005 |
| 5 | 42.70 | 6.66 | Allowance of | 0.022 | 0.014 | 0.006 | 0.003 |
| 6 | 42.53 | 6.31 | Allowance of | 0.024 | 0.015 | 0.008 | 0.004 |
| 7 | 42.18 | 6.51 | Allowance of | 0.021 | 0.016 | 0.008 | 0.005 |
| 8 | 42.30 | 6.40 | Allowance of | 0.023 | 0.017 | 0.01 | 0.004 |
| 9 | 42.19 | 6.75 | Allowance of | 0.017 | 0.016 | 0.008 | 0.004 |
| Maximum value | 42.75 | 6.75 | / | 0.024 | 0.018 | 0.01 | 0.005 |
| Minimum value | 42.15 | 6.31 | / | 0.017 | 0.013 | 0.006 | 0.003 |
| Standard deviation of | 0.230 | 0.145 | / | 0.002 | 0.001 | 0.001 | 0.001 |
The observation of the table shows that the segregation of Mo and Si elements in the aluminum-molybdenum-silicon alloy is less than 0.5 wt percent, the oxygen and nitrogen content of impurity elements are far lower than that of the conventional aluminum-molybdenum-silicon alloy (such as comparative example 1 and comparative example 2), the purity of the alloy is high, and the uniformity is good. The SEM of the aluminum-molybdenum-silicon alloy is shown in fig. 3 (a), and the metallographic diagram is shown in fig. 3 (b). The observation shows that the alloy has no obvious alumina inclusion inside and high purity.
TABLE 2 analysis of sample results of AlMoSi alloy produced in example 2
| Test number | Mowt% | Siwt% | Al | Fewt% | Cwt% | Owt% | Nwt% |
| 1 | 42.14 | 7.38 | Allowance of | 0.023 | 0.017 | 0.006 | 0.004 |
| 2 | 42.13 | 7.32 | Allowance of | 0.020 | 0.017 | 0.008 | 0.003 |
| 3 | 42.49 | 7.20 | Allowance of | 0.028 | 0.015 | 0.007 | 0.004 |
| 4 | 42.64 | 7.48 | Allowance of | 0.028 | 0.016 | 0.009 | 0.003 |
| 5 | 42.54 | 7.33 | Allowance of | 0.022 | 0.016 | 0.006 | 0.003 |
| 6 | 42.71 | 7.38 | Allowance of | 0.026 | 0.017 | 0.008 | 0.003 |
| 7 | 42.37 | 7.23 | Allowance of | 0.028 | 0.016 | 0.004 | 0.005 |
| 8 | 42.76 | 7.62 | Allowance of | 0.022 | 0.017 | 0.01 | 0.005 |
| 9 | 42.32 | 7.24 | Allowance of | 0.021 | 0.016 | 0.007 | 0.004 |
| Maximum value | 42.76 | 7.62 | / | 0.028 | 0.017 | 0.01 | 0.005 |
| Minimum value | 42.13 | 7.2 | / | 0.02 | 0.015 | 0.004 | 0.003 |
| Standard deviation of | 0.219 | 0.126 | / | 0.003 | 0.001 | 0.002 | 0.001 |
The observation of the table shows that the uniformity of Mo and Si elements in the aluminum-molybdenum-silicon alloy is high, the oxygen and nitrogen of impurity elements are far lower than those of the conventional aluminum-molybdenum-silicon alloy (such as comparative example 1 and comparative example 2), the SEM and metallographic patterns of the aluminum-molybdenum-silicon alloy are shown in figure 5, and the observation shows that the interior of the alloy has no obvious alumina inclusion, the purity of the alloy is high, and the quality of the alloy is higher than that of similar products.
TABLE 3 analysis of sample results for AlMoSi alloys produced in example 3
| Test number | Mowt% | Siwt% | Al | Fewt% | Cwt% | Owt% | Nwt% |
| 1 | 37.30 | 8.00 | Allowance of | 0.026 | 0.015 | 0.006 | 0.003 |
| 2 | 37.00 | 7.72 | Allowance of | 0.020 | 0.017 | 0.008 | 0.004 |
| 3 | 37.67 | 8.35 | Allowance of | 0.025 | 0.016 | 0.007 | 0.004 |
| 4 | 36.95 | 8.17 | Allowance of | 0.024 | 0.014 | 0.007 | 0.004 |
| 5 | 37.32 | 7.92 | Allowance of | 0.025 | 0.013 | 0.010 | 0.005 |
| 6 | 37.30 | 8.37 | Allowance of | 0.028 | 0.016 | 0.008 | 0.005 |
| 7 | 37.55 | 7.89 | Allowance of | 0.028 | 0.016 | 0.010 | 0.004 |
| 8 | 37.44 | 8.27 | Allowance of | 0.021 | 0.014 | 0.007 | 0.004 |
| 9 | 37.22 | 7.99 | Allowance of | 0.023 | 0.014 | 0.009 | 0.003 |
| Maximum value | 37.67 | 8.37 | / | 0.028 | 0.017 | 0.01 | 0.005 |
| Minimum value | 36.95 | 7.72 | / | 0.02 | 0.013 | 0.006 | 0.003 |
| Standard deviation of | 0.221 | 0.213 | / | 0.003 | 0.001 | 0.001 | 0.001 |
The observation of the table shows that the uniformity of Mo and Si elements in the aluminum-molybdenum-silicon alloy is high, the SEM and metallographic patterns of the aluminum-molybdenum-silicon alloy are shown as figure 9, the observation shows that the interior of the alloy has no obvious alumina inclusion, and the quality of the alloy is higher than that of similar products.
TABLE 4 analysis of sampling results of aluminum-molybdenum-silicon alloy produced in comparative example 1
| Test number | Mowt% | Siwt% | Al | Fewt% | Cwt% | Owt% | Nwt% |
| 1 | 41.63 | 6.47 | Allowance of | 0.092 | 0.065 | 0.056 | 0.017 |
| 2 | 42.55 | 6.78 | Allowance of | 0.085 | 0.045 | 0.082 | 0.018 |
| 3 | 42.08 | 6.81 | Allowance of | 0.090 | 0.046 | 0.058 | 0.010 |
| 4 | 42.45 | 6.16 | Allowance of | 0.108 | 0.050 | 0.083 | 0.013 |
| 5 | 41.50 | 6.10 | Allowance of | 0.080 | 0.070 | 0.077 | 0.017 |
| 6 | 41.63 | 6.22 | Allowance of | 0.069 | 0.042 | 0.054 | 0.012 |
| 7 | 41.12 | 6.15 | Allowance of | 0.110 | 0.060 | 0.040 | 0.025 |
| 8 | 43.14 | 7.10 | Allowance of | 0.081 | 0.063 | 0.080 | 0.017 |
| 9 | 41.86 | 6.12 | Allowance of | 0.063 | 0.044 | 0.072 | 0.016 |
| Maximum value | 43.14 | 7.1 | / | 0.11 | 0.07 | 0.083 | 0.025 |
| Minimum value | 41.12 | 6.1 | / | 0.063 | 0.042 | 0.04 | 0.01 |
| Standard deviation of | 0.590 | 0.352 | / | 0.015 | 0.010 | 0.014 | 0.004 |
The observation of the table shows that the segregation degree of main elements in the aluminum-molybdenum-silicon alloy produced by aluminothermic reaction is obviously increased, and the iron, carbon, oxygen and nitrogen elements are obviously increased under the influence of a crucible and a reaction environment. The metallographic diagram of the aluminum-molybdenum-silicon alloy prepared by the aluminothermic method is shown in figure 6, a large amount of alumina inclusions and agglomeration occur in the metallographic diagram, and the alloy quality is poor.
TABLE 5 analysis of sample results for the Al-Mo-Si alloy produced in comparative example 2
| Test number | Mowt% | Siwt% | Al | Fewt% | Cwt% | Owt% | Nwt% |
| 1 | 42.03 | 6.59 | Allowance of | 0.100 | 0.033 | 0.020 | 0.023 |
| 2 | 42.41 | 7.11 | Allowance of | 0.116 | 0.031 | 0.021 | 0.024 |
| 3 | 42.53 | 6.57 | Allowance of | 0.072 | 0.026 | 0.022 | 0.024 |
| 4 | 43.90 | 5.97 | Allowance of | 0.065 | 0.027 | 0.022 | 0.021 |
| 5 | 43.83 | 6.09 | Allowance of | 0.078 | 0.026 | 0.016 | 0.020 |
| 6 | 43.47 | 6.75 | Allowance of | 0.078 | 0.031 | 0.015 | 0.024 |
| 7 | 43.10 | 7.05 | Allowance of | 0.068 | 0.045 | 0.020 | 0.023 |
| 8 | 43.51 | 6.51 | Allowance of | 0.063 | 0.046 | 0.015 | 0.023 |
| 9 | 42.54 | 6.62 | Allowance of | 0.065 | 0.032 | 0.016 | 0.024 |
| Maximum value | 43.9 | 7.11 | / | 0.116 | 0.046 | 0.022 | 0.024 |
| Minimum value | 42.03 | 5.97 | / | 0.063 | 0.026 | 0.015 | 0.02 |
| Standard deviation of | 0.641 | 0.357 | / | 0.017 | 0.007 | 0.003 | 0.001 |
The observation of the table shows that the segregation degree of molybdenum element in the aluminum-molybdenum-silicon alloy is increased, the content of carbon and oxygen element is reduced, and the uniformity of the alloy is poor. The metallographic pattern of the aluminum-molybdenum-silicon alloy prepared by the medium-frequency vacuum induction melting method is shown as figure 7, and the observation shows that the metallographic pattern has no agglomeration phenomenon of alumina inclusions, but a small amount of alumina inclusions exist, and the purity of the alloy is lower than that of the alloy of the invention although the purity of the alloy is relatively higher.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A method for producing an aluminum-molybdenum-silicon alloy, characterized in that the method comprises the following steps:
(1) Mixing molybdenum trioxide and byproduct water glass solution in proportion, uniformly stirring, then slowly adding ammonium sulfate solution, adjusting pH and reacting at high temperature, adjusting pH to 1.2-1.8, and reacting at 200-230 ℃ for 20-36 h;
(2) Carrying out reduced pressure suction filtration on the reaction solution, washing, drying and sintering to obtain MoO 3/SiO2 compound;
(3) Uniformly mixing the MoO 3/SiO2 compound and aluminum powder in proportion, and carrying out vacuum aluminothermic reaction to obtain an aluminum-molybdenum-silicon alloy;
the specific operation of the step (2) is as follows:
after the reaction is finished, a filter cake is obtained through decompression and suction filtration, the filter cake is washed by high-purity water until the pH value of a washing liquid is more than 6.8, and after the filter cake is dried at 70-80 ℃ for 10-24 h, the filter cake is transferred to a muffle furnace for heat preservation at 400-550 ℃ for 8-12: 12 h, so as to obtain the MoO 3/SiO2 compound.
2. The method for producing an aluminum-molybdenum-silicon alloy according to claim 1, wherein the sodium silicate content in the byproduct water glass solution is 32-42 wt%, the water glass modulus is 0.4-1.5, and the sodium molybdate content in the water glass solution is 20 wt%.
3. The method for producing an aluminum-molybdenum-silicon alloy according to claim 1 or 2, wherein the mass ratio of molybdenum trioxide to water glass solution is (3.8-5.4): 10, the content of ammonium sulfate in the ammonium sulfate solution is 50-65 wt%, and the mass ratio of the ammonium sulfate solution to byproduct water glass solution is (3.9-5.2): 10.
4. The method for producing aluminum-molybdenum-silicon alloy according to claim 1, wherein the iron content in the aluminum powder is less than 0.02 wt%, and the mass ratio of MoO 3/SiO2 compound to aluminum powder is (0.72-1.07): 1.
5. The method for producing aluminum-molybdenum-silicon alloy according to claim 1 or 4, wherein the crucible in the vacuum aluminothermic furnace is made of red copper, a mechanical pump is turned off, the furnace body is turned on, vacuum is pumped to a vacuum degree of less than 300 Pa, and after the vacuum aluminothermic reaction is completed, the vacuum is maintained for 3-5 hours.
6. An aluminum-molybdenum-silicon alloy produced by the method of claim 1, wherein the aluminum-molybdenum-silicon alloy contains 35-45 wt% of molybdenum, 4-10 wt% of silicon, the balance of aluminum, less than or equal to 0.05 wt% of iron, less than or equal to 0.02 wt% of carbon, less than or equal to 0.01 wt% of oxygen, and less than or equal to 0.005 wt% of nitrogen.
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| CN108048809A (en) * | 2017-09-22 | 2018-05-18 | 南京航空航天大学 | The argentiferous MoO of anti-corrosion antibacterial3-SiO2The preparation method of nanocrystalline composite coating |
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| CN116005043B (en) * | 2023-01-30 | 2024-06-18 | 承德天大钒业有限责任公司 | Aluminum-molybdenum-vanadium intermediate alloy and preparation method thereof |
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| CN108048809A (en) * | 2017-09-22 | 2018-05-18 | 南京航空航天大学 | The argentiferous MoO of anti-corrosion antibacterial3-SiO2The preparation method of nanocrystalline composite coating |
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