CN113186414A - Preparation process of aerospace grade TA15 special alloy - Google Patents
Preparation process of aerospace grade TA15 special alloy Download PDFInfo
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- CN113186414A CN113186414A CN202110293198.7A CN202110293198A CN113186414A CN 113186414 A CN113186414 A CN 113186414A CN 202110293198 A CN202110293198 A CN 202110293198A CN 113186414 A CN113186414 A CN 113186414A
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- C—CHEMISTRY; METALLURGY
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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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
- 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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention provides a preparation process of an aerospace grade TA15 special alloy, which comprises the following steps: the method comprises the following steps of primary batching, material mixing and thermit reaction, secondary batching, secondary material mixing, secondary smelting, crushing, material picking, finished product inspection and warehousing. The invention mixes vanadium-aluminum alloy and molybdenum-aluminum alloy prepared by primary smelting with other three alloys, adjusts the proportion, carries out secondary smelting in a medium-frequency induction furnace, and prepares the finished special alloy by the working procedures of crushing and the like after the reaction is finished. Compared with the traditional process of smelting TA15 ingot by simply adding a plurality of alloy elements, the TA15 ingot smelted by the special alloy for TA15 prepared by the invention is more stable and close to the detection value and the proportioning value of each element component in the obtained TA15 ingot, meanwhile, the uniformity and the consistency of each component of the ingot are greatly improved, impurities are easier to control, the quality and the stability of the TA15 ingot are obviously improved, and the requirement of aerospace-grade quality standard can be better met.
Description
Technical Field
The invention belongs to the technical field of metal materials, relates to a master alloy material for titanium alloy, and particularly relates to a preparation process of an aerospace grade TA15 special alloy.
Background
The titanium alloy material is mainly applied to the industries of aerospace industry, national defense military industry and the like. Among them, the application in the aerospace industry is in the largest demand, about 50%, and is mainly used for manufacturing airplanes and engines. In the development process of titanium alloy materials, a titanium alloy ingot is the most important and most critical ring, and the quality of the titanium alloy ingot directly influences whether the performance index of a finished product subjected to subsequent processing meets the product requirement. In the process of preparing the titanium alloy, different grades of titanium alloy are generated due to different performance requirements, the different grades of the titanium alloy depend on different addition elements and contents in the components of the titanium alloy, and the alloy serving as the addition element is called as intermediate alloy. The titanium alloy ingot is prepared by smelting sponge titanium and intermediate alloy together. Therefore, the quality and stability of the added master alloy directly affect the quality of the titanium alloy ingot. At present, a titanium alloy ingot with one grade is prepared, and a plurality of different types of intermediate alloys or elements are usually required to be added to meet the requirements of element components. This brings the following disadvantages:
1. the deviation fluctuation of the detection value and the proportioning value of each element component in the titanium alloy ingot is large, and the irregularity is difficult to control in an accurate range; the proportion of components among elements is unstable, the influence of various raw material components and smelting is large, the uniformity and consistency of the components of all parts of the cast ingot are poor, the components need to be improved in a mode of smelting for many times, and the economic cost is increased.
2. Because the addition of intermediate alloy or elements is various, impurity components such as iron, carbon, nitrogen, oxygen and the like in the titanium alloy ingot are difficult to control, and the titanium alloy ingot is prepared by depending on empirical values in most cases, so that the quality and the stability of the titanium alloy ingot are difficult to ensure.
Disclosure of Invention
The invention provides a preparation process of a special alloy for aerospace-grade TA15, wherein detection values and proportioning values of various element components in a TA15 cast ingot smelted by using the special alloy are more stable and approximate, meanwhile, the uniformity and consistency of various components of the cast ingot are greatly improved, impurity components such as silicon, carbon, nitrogen, oxygen and the like are more easily controlled, the quality and stability of the TA15 cast ingot are greatly improved, and the requirement of the aerospace-grade quality standard can be better met. The specific technical scheme is as follows:
a preparation process of an aerospace grade TA15 special alloy is characterized by comprising the following steps:
step 1), primary batching: according to the set mass percentage ratio of the materials:
selecting pure V with proper granularity2O5、Al、CaF2Powder is formed to form a material before vanadium-aluminum alloy mixing, and the material is baked to be dry;
selecting pure Mo with proper granularity2O3Al and CaF powder to form a material before molybdenum and aluminum alloy mixing, and baking to dry;
step 2), carrying out a primary mixing and aluminothermic reaction: mixing the baked vanadium-aluminum alloy material V2O5、Al、CaF2Weighing the powder in proportion to form a material S1;
the material Mo before mixing the molybdenum and the aluminum alloy2O3、Al、CaF2Weighing the powder in proportion to form a material S2;
respectively placing the materials S1 and S2 into different blenders, mixing the materials at 120-130 ℃ for 30-50 Min to form uniformly mixed materials, then placing the materials into different crucibles to form furnace burden, igniting magnesium chips, then placing the materials into different crucibles to ignite the furnace burden to perform aluminothermic reaction, namely 3V2O5+10Al=6V+5Al2O3To produce vanadium-aluminum alloy, Mo2O3+2Al=2Mo+Al2O3Generating molybdenum-aluminum alloy;
step 3), secondary batching: baking the vanadium-aluminum alloy and the molybdenum-aluminum alloy with proper particle sizes, Al beans, sponge Zr and Fe nails, and weighing the materials in proportion to form a material S3 before mixing of the special alloy for TA 15;
step 4), secondary mixing: putting the material S3 into a mixer, mixing the materials for 30-50 minutes at the temperature of 120-130 ℃ to form a uniformly mixed material, and then putting the uniformly mixed material into a crucible of a medium-frequency induction furnace;
step 5), secondary smelting: performing secondary smelting by using a medium-frequency induction furnace, adjusting the power to 10kW1 hours, 30kW1 hours, vacuumizing to 5Pa1 hours, gradually increasing the power to 70kW after the vacuum is completely pumped, completely melting the material S3, reducing the power to 30kW, and then performing cooling casting to form a TA15 special alloy block Al-V-Mo-Zr-Fe, namely an alloy block S4;
step 6), crushing and sieving: crushing the alloy block S4 into large blocks, adding the large blocks into a crusher for further crushing and refining, sieving the crushed blocks by using a sieve with the specification of 6mm, and crushing the alloy blocks which are larger than 6mm again; the alloy blocks S4 sieved by the same batch are immediately barreled, weighed and marked with batch numbers;
step 7), selecting materials: manually picking out impurities, foreign matters or oxides from the alloy blocks S4 under the crushing screen; the surface of the alloy is not required to be provided with a loose layer, an oxide layer and foreign matters;
step 8), warehousing qualified products: and (4) performing sampling inspection on the picked alloy blocks S4 by inspectors according to 5 percent of the alloy blocks specially used for the batch TA15, and judging that the alloy blocks are qualified for warehousing if no impurities, foreign matters or oxides are found.
Further, the special alloy for TA15 comprises the following components in percentage by mass: 53.9% of Al, 16.6% of V, 11.6% of Mo, 16.7% of Zr and 1.2% of Fe.
Further, the material S1 is 100kg V2O592kg of Al powder, 15kg of CaF2Pulverizing; the material S2 is 90kg of Mo2O375kg of Al powder and 15kg of CaF2And (3) pulverizing.
Further, the material S3 is 48kg of vanadium-aluminum alloy, 31kg of molybdenum-aluminum alloy, 61kg of aluminum beans, 29kg of sponge zirconium and 2kg of iron nails.
The invention has the technical effects that:
1. as the steps of mixing and smelting are carried out for multiple times, the special alloy (Al-V-Mo-Zr-Fe) for TA15 is taken as an intermediate alloy, and the proportion of each element component in the alloy is solidified and controllable. The TA15 cast ingot directly smelted by the alloy and the sponge titanium has more stable and approximate detection value and proportioning value of each element component, and simultaneously, the uniformity and consistency of each component of the cast ingot are greatly improved.
2. Compared with the traditional process of smelting TA15 cast ingot by simply adding a plurality of alloy elements, the variable influencing impurity components is greatly reduced after the TA15 special alloy is added and the TA15 cast ingot is smelted, impurities such as silicon, carbon, nitrogen, oxygen and the like are easier to control, the quality and stability of the TA15 cast ingot are greatly improved, and the quality standard requirement of aerospace grade can be better met.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Take the preparation of a special alloy for TA15, i.e. Al-V-Mo-Zr-Fe as an example. The specific implementation steps are as follows:
step 1), primary batching: calculating and batching according to the set mass percentages of 53.9% of Al, 16.6% of V, 11.6% of Mo, 16.7% of Zr and 1.2% of Fe of the special alloy for TA15, and selecting pure vanadium pentoxide, pure aluminum powder and pure fluorite powder with the granularity smaller than 100 meshes to form a material before mixing the vanadium-aluminum alloy; pure molybdenum trioxide with the granularity smaller than 100 meshes, pure aluminum powder and pure fluorite powder are formed into a material before molybdenum and aluminum alloy mixing and are baked to be dry;
step 2), carrying out a primary mixing and aluminothermic reaction: mixing the roasted vanadium-aluminum alloy with a material V before mixing2O5、CaF2Al powder is weighed according to the proportion, namely 100kg of vanadium pentoxide, 92kg of aluminum powder, 15kg of fluorite powder and Mo-Al alloy material before mixing2O3、CaF2The Al powder is weighed according to a proportion, namely 90kg of molybdenum trioxide, 75kg of aluminum powder and 15kg of fluorite powder are respectively put into different blenders to be mixed for 30-50 minutes at the temperature of 120-130 ℃ to form uniformly mixed materials, then the uniformly mixed materials are put into different crucibles to form furnace materials, 20g of magnesium chips are ignited and then put into different crucibles to ignite the furnace materials, and the aluminothermic reaction is carried out for 3V2O5+10Al=6V+5Al2O3,Mo2O3+2Al=2Mo+Al2O3;
Step 3), secondary batching: baking finished products of vanadium-aluminum alloy, molybdenum-aluminum alloy, aluminum beans, sponge zirconium and iron nails with proper granularity, and weighing the finished products according to the proportion, namely 48kg of vanadium-aluminum alloy, 31kg of molybdenum-aluminum alloy, 61kg of aluminum beans, 29kg of sponge zirconium and 2kg of iron nails to form a material before TA15 special alloy mixing;
step 4), secondary mixing: placing the materials before mixing of the special alloy for TA15 into a mixer, mixing for 30-50 minutes at 120-130 ℃ to form uniformly mixed materials, and then placing the uniformly mixed materials into a crucible of a medium-frequency induction furnace;
step 5), secondary smelting in a medium-frequency induction furnace: adjusting the power to 10kW1 hours, 30kW1 hours, vacuumizing to 5Pa1 hours, gradually increasing the power to 70kW after the vacuum is exhausted until the materials are completely melted, reducing the power to 30kW, and then cooling and casting.
Step 6), crushing: crushing the special alloy blocks for TA15 into large blocks, adding the large blocks into a crusher for further crushing and refining, and sieving the large blocks by using a sieve with the specification of 6mm, wherein the special alloy blocks for TA15 with the size of more than 6mm need to be crushed again; the alloy blocks specially used for TA15 sieved in the same batch are immediately barreled, weighed and marked with batch numbers;
step 7), selecting materials: manually picking out impurities, foreign matters or oxides from the TA15 special alloy blocks under the crushing screen; the surface of the alloy is not required to be provided with a loose layer, an oxide layer and foreign matters;
step 8), finished product inspection and warehousing: and (4) performing sampling inspection on the picked TA15 special alloy blocks according to 5 percent of the TA15 special alloy blocks in the batch by inspectors, judging that the alloy blocks are qualified and warehousing the alloy blocks.
The comparison of the components of TA15 titanium alloy ingots melted by the conventional process and the alloy process of this example is shown in table 1 "comparison table of the contents of main components of TA15 ingots melted by different alloy processes" and table 2 "comparison table of the contents of impurity components of TA15 ingots melted by different alloy processes". As can be seen from Table 1, compared with the conventional process, the detection values and the proportioning values of the components of the elements in the TA15 cast ingot obtained by the method are more stable and approximate, and the uniformity and the consistency of the components of each part of the cast ingot are greatly improved. From table 2, it can be seen that, compared with the conventional process, after the TA15 special alloy is added and smelted into the ingot, the variables influencing the impurity components are greatly reduced, the impurities such as silicon, carbon, nitrogen, oxygen and the like are easier to control, the components of each batch tend to be stable, the quality and stability of the TA15 ingot are greatly improved, and the quality standard requirements of aerospace grade can be better met.
TABLE 1 comparison of main component contents of TA15 ingots smelted by different alloy processes
TABLE 2 comparison table of impurity contents of TA15 ingot produced by different alloy processes
Claims (4)
1. The preparation process of the aerospace grade TA15 special alloy is characterized by comprising the following steps of:
step 1), primary batching: according to the set mass percentage ratio of the materials:
selecting pure V with proper granularity2O5、Al、CaF2Powder is formed to form a material before vanadium-aluminum alloy mixing, and the material is baked to be dry;
selecting pure Mo with proper granularity2O3Al and CaF powder to form a material before molybdenum and aluminum alloy mixing, and baking to dry;
step 2), carrying out a primary mixing and aluminothermic reaction:
mixing the baked vanadium-aluminum alloy material V2O5、Al、CaF2Weighing the powder in proportion to form a material S1;
mixing the molybdenum-aluminum alloy to obtain a material Mo2O3、Al、CaF2Weighing the powder in proportion to form a material S2;
respectively placing the materials S1 and S2 into different mixers, mixing the materials at 120-130 ℃ for 30-50 Min to form uniformly mixed materials, then placing the materials into different crucibles to form furnace burden, igniting magnesium chips, then placing the materials into different crucibles to ignite the furnace burden, and carrying out aluminothermic reaction to generate vanadium-aluminum alloy and molybdenum-aluminum alloy;
step 3), secondary batching: baking the vanadium-aluminum alloy and the molybdenum-aluminum alloy with proper particle sizes and Al beans, sponge Zr and Fe nails to be dry and weighing in proportion to form a material S3 before mixing of the special alloy for TA 15;
step 4), secondary mixing: putting the material S3 into a mixer, mixing the materials for 30-50 minutes at the temperature of 120-130 ℃ to form a uniformly mixed material, and then putting the uniformly mixed material into a crucible of a medium-frequency induction furnace;
step 5), secondary smelting: performing secondary smelting by using a medium-frequency induction furnace, adjusting the power to 10kW1 hours and 30kW1 hours, gradually increasing the power to 70kW after vacuumizing to 5Pa1 hours, and reducing the power to 30kW after the material S3 is completely melted, and then performing cooling casting to form an alloy block Al-V-Mo-Zr-Fe special for TA15, namely an alloy block S4;
step 6), crushing and sieving: crushing and refining the alloy blocks S4, sieving the alloy blocks by using a sieve with the specification of 6mm, crushing the alloy blocks S4 which are sieved in the same batch immediately, barreling, weighing and marking batch numbers, wherein the alloy blocks S4 are required to be crushed and refined again when the alloy blocks are larger than 6 mm;
step 7), selecting materials: manually removing impurities, foreign matters or oxides from the alloy blocks S4 which are crushed and sieved, wherein the alloy surface has no loose layer, no oxidation layer and no foreign matters;
step 8), warehousing qualified products: and (4) performing sampling inspection on the picked alloy blocks S4 by inspectors according to 5% of the alloy blocks specially used for the batch TA15, and judging the alloy blocks to be qualified for warehousing when no impurities, foreign matters or oxides are found.
2. The preparation process of claim 1, wherein the TA15 special alloy comprises the following components in percentage by mass: 53.9% of Al, 16.6% of V, 11.6% of Mo, 16.7% of Zr and 1.2% of Fe.
3. The process according to claim 1 or 2,
the material S1 is 100kg V2O592kgAl powder,15kg CaF2Pulverizing;
the material S2 is 90kg of Mo2O375kg of Al powder and 15kg of CaF2And (3) pulverizing.
4. The process according to claim 1, 2 or 3, wherein the material S3 is 48kg of vanadium-aluminum alloy, 31kg of molybdenum-aluminum alloy, 61kg of Al beans, 29kg of sponge Zr and 2kg of Fe nails.
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CN113718131A (en) * | 2021-09-03 | 2021-11-30 | 立中四通轻合金集团股份有限公司 | Short-flow low-cost preparation method of titanium-molybdenum intermediate alloy |
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CN113718131A (en) * | 2021-09-03 | 2021-11-30 | 立中四通轻合金集团股份有限公司 | Short-flow low-cost preparation method of titanium-molybdenum intermediate alloy |
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