CN102534315B - Al-Mo intermediate alloy and preparing method thereof - Google Patents
Al-Mo intermediate alloy and preparing method thereof Download PDFInfo
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- CN102534315B CN102534315B CN201210016952.3A CN201210016952A CN102534315B CN 102534315 B CN102534315 B CN 102534315B CN 201210016952 A CN201210016952 A CN 201210016952A CN 102534315 B CN102534315 B CN 102534315B
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Abstract
The invention discloses an Al-Mo intermediate alloy comprising the following components by weight percent: 45 to 70 percent of Mo; 0 to 0.2 percent of Fe; 0 to 0.1 percent of O; 0 to 0.1 percent of C; 0 to 0.2 percent of Si; 0 to 0.005 percent of B; 0 to 0.03 percent of N; 0 to 0.05 percent of H; and Al in balancing amount. The invention further provides a preparing method for the Al-Mo intermediate alloy. The smelting process of the preparing method comprises two steps, so that compared with the conventional outside-furnace smelting method, the preparing method has the advantage that ingredients obtained according to the preparing method are more uniform; particularly, Al is added twice in each of the two steps, so that the uniformity of the ingredients is better than that of ingredients obtained according to a method in which Al is added once. Moreover, the invention further adopts a unique smelting method in which a carbon crucible coated with a yttrium oxide layer serves as a smelting container in a vacuum furnace, so that compared with the conventional method in which a water-cooling copper crucible is required to be adopted, the invention has the advantages that the manufacturing cost is greatly reduced, and the introduction of impurities can be controlled better.
Description
Technical field
The present invention relates to a kind of master alloy and preparation method thereof, relate in particular to a kind of aluminium molybdenum master alloy of smelting use and preparation method thereof.
Background technology
Along with the development of titanium alloy, adopt master alloy to add in the smelting of titanium alloy more and more general.Master alloy for adding, requires segregation-free, and without metal inclusion, foreign matter content is low as much as possible.
Current master alloy adopts single stage method to smelt more, and the alloy of smelting not only foreign matter content is higher, and homogeneity is not fine.
Summary of the invention
The object of the present invention is to provide a kind of aluminium molybdenum master alloy and preparation method thereof, the foreign matter content of vanadium aluminium intermediate alloy can reach titanium alloy and smelt the requirement of adding, and the preparation method of master alloy can more easily control.
A kind of aluminium molybdenum master alloy provided by the invention, comprises following component: Mo45~70%, Fe≤0.2%, O≤0.1%, C≤0.1%, Si≤0.2%, B≤0.005%, N≤0.03%, H≤0.005%, and surplus is Al; Wherein, described per-cent is weight percentage; Described aluminium molybdenum master alloy makes as follows:
1) according to MoO
3100 parts, Al63~125 part, CaF
220~41 parts, KClO
30~20 part of 0~15 part, slag take each starting material;
2), by the shove charge at normal temperatures of each starting material, adopt the outer aluminothermy smelting method of stove to carry out the first step smelting;
3) 0~5 part of Al starting material taking are in addition placed in to vacuum melting furnace with smelt the primary products that obtain in the first step together with and carry out vacuum melting, the smelting temperature of vacuum melting is 1450~1600 ℃, vacuum tightness is less than 0.67Pa, the refining 6~15 minutes of seething with excitement in short-term under the high temperature of 1500 ℃ after furnace charge fusing, and under vacuum condition, carry out alloy casting.
Preferably, comprise following component: Mo45~70%, Fe≤0.1%, O≤0.05%, C≤0.05%, Si≤0.1%, B≤0.003%, N≤0.02%, H≤0.003%, surplus is Al; Wherein, described per-cent is weight percentage.
Preferably, comprise following component: Mo45~70%, Fe≤0.05%, O≤0.03%, C≤0.03%, Si≤0.05%, B≤0.002%, N≤0.01%, H≤0.002%, surplus is Al; Wherein, described per-cent is weight percentage.
The present invention also provides a kind of preparation method of aluminium molybdenum master alloy, comprises the steps:
1) according to MoO
3100 parts, Al63~125 part, CaF
220~41 parts, KClO
30~20 part of 0~15 part, slag take each starting material;
2), by the shove charge at normal temperatures of each starting material, adopt the outer aluminothermy smelting method of stove to carry out the first step smelting;
3) 0~5 part of Al starting material taking are in addition placed in to vacuum melting furnace with smelt the primary products that obtain in the first step together with and carry out vacuum melting, the smelting temperature of vacuum melting is 1450~1600 ℃, vacuum tightness is less than 0.67Pa, the refining 6~15 minutes of seething with excitement in short-term under the high temperature of 1500 ℃ after furnace charge fusing, and under vacuum condition, carry out alloy casting.
Preferably, when described vacuum melting furnace carries out melting, adopt carbon crucible filling furnace charge, and apply one deck yttrium oxide in described carbon crucible.
The present invention is by adopting two-step approach to smelt, the outer smelting method of the existing stove of comparing, the composition obtaining is more even, especially adopts and in two steps, adds at twice respectively Al, make that the homogeneity of composition more once adds better; In addition, the present invention has also adopted in vacuum oven and has used and be coated with the carbon crucible of one deck yttrium oxide as unique smelting process of smelting vessel, like this, compare with the water-cooled copper crucible that will adopt in the past, not only manufacturing cost reduces greatly, and the stability of system is better, and can be better the introducing of controlling impurity.
Embodiment
The present invention adopts two-step approach to smelt aluminium molybdenum master alloy, mainly comprises the steps:
1) according to MoO
3100 parts, Al63~125 part, CaF
220~41 parts, KClO
30~20 part of 0~15 part, slag take each starting material;
2), by the shove charge at normal temperatures of each starting material, adopt the outer aluminothermy smelting method of stove to carry out the first step smelting;
3) 0~5 part of Al starting material taking are in addition placed in to vacuum melting furnace with smelt the primary products that obtain in the first step together with and carry out vacuum melting, the smelting temperature of vacuum melting is 1450~1600 ℃, vacuum tightness is less than 0.67Pa, after furnace charge is melted to 1/4 to 2/5, can be filled with argon gas, furnace pressure is remained in 50~80Pa, to prevent that in stove, solution too seethes with excitement.After furnace charge in stove melts completely, make to carry out short time high temperature boiling refining in stove, refining time is 6~15 minutes, temperature >=1500 ℃.Until alloy liquid level is tranquil, without bubble, overflow, then when being 1480~1550 ℃, alloy solution temperature casts.
In step 3), what the present invention adopted in vacuum oven is carbon crucible, and is coated with one deck yttrium oxide at the internal surface of crucible.Owing to adopting such container to load the alloy of smelting, compared with adopt water-cooled copper crucible in the past on the one hand, production cost reduces greatly, and, due to yttrium oxide, under the condition of 1450~1600 ℃, also can keep good stability, therefore can prevent from introducing other impurity in the process of smelting, the control of the homogeneity of the tissue of alloy and the content of impurity plays a good role.
In addition, the present invention adds in two steps starting material Al in step 3), can make more disposable the wanting better of adding in the first step of homogeneity of composition.In addition, in the present invention, the yttrium oxide of coating preferably adopts analytically pure yttrium oxide.
In addition, in step 2) in, employing be that the outer thermite reaction of stove is smelted method, in order to make N content low as much as possible, for example, lower than 0.001%, adopt vacuum aluminum thermal response smelting process in stove, specific practice is:
The starting material that step 1) is weighed are put in crucible, then crucible is placed in to vacuum oven, and connect the portfire of igniting, vacuumize, and then are filled with helium, light a fire, thereby carry out thermite reaction by portfire.
Below, by specific embodiment, come that the present invention is further described, the concrete method adopting is same as the above-mentioned method.
Embodiment 1
The weight YiKgWei unit of batching, MoO
3100Kg, Al117Kg, CaF
226Kg, KClO
36.7Kg takes each starting material; In step 3), add the 0.1KgAl measuring in addition, through two steps, smelt the alloy component obtaining as follows:
Mo is 45.75%, Fe is 0.08%, O is 0.05%, C is 0.04%, Si is 0.06%, B is 0.003%, N is 0.02%, H is 0.004%; Surplus is Al; Wherein, the per-cent is here weight percentage.
It is that stove is smelted outward that two steps of the present embodiment are smelted the employing of the method the first step.
Embodiment 2
The weight YiKgWei unit of batching, MoO
3100Kg, Al104Kg, CaF
234Kg, slag 11.1Kg take each starting material; In step 3), add the 0.4KgAl measuring in addition, through two steps, smelt the alloy component obtaining as follows:
Mo is 52.93%, Fe is 0.07%, O is 0.04%, C is 0.04%, Si is 0.05%, B is 0.004%, N is 0.002%, H is 0.005%; Surplus is Al; Wherein, the per-cent is here weight percentage.
It is vacuum metling in stove that two steps of the present embodiment are smelted the employing of the method the first step.
Embodiment 3
The weight YiKgWei unit of batching, MoO
3100Kg, Al84Kg, CaF
236.8Kg, slag 14.4Kg take each starting material; In step 3), add the 3.6Kg measuring in addition, through two steps, smelt the alloy component obtaining as follows:
Mo is 57.32%, Fe is 0.05%, O is 0.03%, C is 0.06%, Si is 0.02%, B is 0.002%, N is 0.002%, H is 0.005%; Surplus is Al; Wherein, the per-cent is here weight percentage.
It is vacuum metling in stove that two steps of the present embodiment are smelted the employing of the method the first step.
Embodiment 4
The weight YiKgWei unit of batching, MoO
3100Kg, Al70.2Kg, CaF
238.6Kg, slag 14.8Kg take each starting material; In step 3), add the 4.2Kg measuring in addition, through two steps, smelt the alloy component obtaining as follows:
Mo is 66.19%, Fe is 0.06%, O is 0.06%, C is 0.05%, Si is 0.03%, B is 0.003%, N is 0.001%, H is 0.005%; Surplus is Al; Wherein, the per-cent is here weight percentage.
It is vacuum metling in stove that two steps of the present embodiment are smelted the employing of the method the first step.
Claims (5)
1. an aluminium molybdenum master alloy, is characterized in that, comprises following component: Mo45~70%, Fe≤0.2%, O≤0.1%, C≤0.1%, Si≤0.2%, B≤0.005%, N≤0.03%, H≤0.005%, and surplus is Al; Wherein, described per-cent is weight percentage; Described aluminium molybdenum master alloy makes as follows:
1) according to MoO
3100 parts, Al63~125 part, CaF
220~41 parts, KClO
30~20 part of 0~15 part, slag take each starting material;
2), by the shove charge at normal temperatures of each starting material, adopt the outer aluminothermy smelting method of stove to carry out the first step smelting;
3) 0~5 part of Al starting material taking are in addition placed in to vacuum melting furnace with smelt the primary products that obtain in the first step together with and carry out vacuum melting, the smelting temperature of vacuum melting is 1450~1600 ℃, vacuum tightness is less than 0.67Pa, the refining 6~15 minutes of seething with excitement in short-term under the high temperature of 1500 ℃ after furnace charge fusing, and under vacuum condition, carry out alloy casting.
2. aluminium molybdenum master alloy as claimed in claim 1, is characterized in that, comprises following component: Mo45~70%, Fe≤0.1%, O≤0.05%, C≤0.05%, Si≤0.1%, B≤0.003%, N≤0.02%, H≤0.003%, and surplus is Al; Wherein, described per-cent is weight percentage.
3. aluminium molybdenum master alloy as claimed in claim 2, is characterized in that, comprises following component: Mo45~70%, Fe≤0.05%, O≤0.03%, C≤0.03%, Si≤0.05%, B≤0.002%, N≤0.01%, H≤0.002%, and surplus is Al; Wherein, described per-cent is weight percentage.
4. a preparation method for aluminium molybdenum master alloy, is characterized in that, comprises the steps:
1) according to MoO
3100 parts, Al63~125 part, CaF
220~41 parts, KClO
30~20 part of 0~15 part, slag take each starting material;
2), by the shove charge at normal temperatures of each starting material, adopt the outer aluminothermy smelting method of stove to carry out the first step smelting;
3) 0~5 part of Al starting material taking are in addition placed in to vacuum melting furnace with smelt the primary products that obtain in the first step together with and carry out vacuum melting, the smelting temperature of vacuum melting is 1450~1600 ℃, vacuum tightness is less than 0.67Pa, the refining 6~15 minutes of seething with excitement in short-term under the high temperature of 1500 ℃ after furnace charge fusing, and under vacuum condition, carry out alloy casting.
5. method as claimed in claim 4, is characterized in that, when described vacuum melting furnace carries out melting, adopts carbon crucible filling furnace charge, and apply one deck yttrium oxide in described carbon crucible.
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CN103849805A (en) * | 2012-12-07 | 2014-06-11 | 东港市东方高新金属材料有限公司 | Aluminum molybdenum vanadium titanium alloy for preparing titanium alloy and preparation method thereof |
CN103397237A (en) * | 2013-08-01 | 2013-11-20 | 大连融德特种材料有限公司 | Molybdenum-aluminum intermediate alloy and production method thereof |
CN103924103A (en) * | 2014-03-11 | 2014-07-16 | 宁夏东方钽业股份有限公司 | Production technology of metal molybdenum |
CN103898386B (en) * | 2014-03-31 | 2016-02-03 | 承德天大钒业有限责任公司 | A kind of aluminium molybdenum niobium copper zirconium master alloy and preparation method thereof |
CN108149082B (en) * | 2018-01-08 | 2019-08-27 | 东北大学 | A kind of Al-Mo intermediate alloy and preparation method thereof |
CN109811225A (en) * | 2019-03-18 | 2019-05-28 | 河北四通新型金属材料股份有限公司 | A kind of molybdenum aluminium silicon intermediate alloy and preparation method thereof |
CN109913709A (en) * | 2019-04-22 | 2019-06-21 | 山西瑞格金属新材料有限公司 | A kind of preparation method of AlMo intermediate alloy |
CN110408816B (en) * | 2019-08-22 | 2021-07-30 | 承德天大钒业有限责任公司 | Nickel-boron-carbon intermediate alloy and preparation method thereof |
CN111945049B (en) * | 2020-08-29 | 2021-07-30 | 承德天大钒业有限责任公司 | Aluminum-molybdenum intermediate alloy and preparation method thereof |
CN113737034B (en) * | 2021-08-06 | 2022-03-15 | 上海康臣特种金属材料有限公司 | Method and device for preparing aluminum-vanadium intermediate alloy by two-step method |
CN117248140B (en) * | 2023-11-14 | 2024-05-10 | 西安稀有金属材料研究院有限公司 | Aluminum-molybdenum intermediate alloy for aerospace-grade titanium alloy and preparation method thereof |
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