CN113528872B - Preparation method of residual titanium plate blank combined package melting assembly welding remelting titanium ingot - Google Patents
Preparation method of residual titanium plate blank combined package melting assembly welding remelting titanium ingot Download PDFInfo
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- CN113528872B CN113528872B CN202110844086.6A CN202110844086A CN113528872B CN 113528872 B CN113528872 B CN 113528872B CN 202110844086 A CN202110844086 A CN 202110844086A CN 113528872 B CN113528872 B CN 113528872B
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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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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/20—Arc remelting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention provides a preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot, which comprises the following steps: and sequentially polishing and cleaning the residual titanium plate blank to obtain an oxide skin, pickling, baking, stacking in a consumable furnace, packaging a primary smelting auxiliary electrode and performing secondary vacuum consumable smelting to obtain a titanium ingot. The method adopts a mode of adjusting the polishing, cleaning and optimizing the assembly welding of the residual titanium plate blank, utilizes the smelting auxiliary electrode to package the residual titanium plate blank, adopts the consumable smelting process of the second smelting, and obtains the cast ingot with phi being more than or equal to 600mm through twice vacuum consumable smelting. The method provided by the invention can ensure the internal quality and the single-branch weight of the residual titanium slab smelting ingot, and provides a new process for residual titanium utilization.
Description
Technical Field
The invention belongs to the technical field of titanium ingots, and particularly relates to a preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot.
Background
With the enterprise's increasing emphasis on the utilization of sawing blanks, the reuse of blank heads becomes a profit growth point for the factory. How to produce qualified pure titanium cast ingots by utilizing residual titanium slabs becomes a difficult point of current technical control: the residual titanium plate blank has more contents of impurities such as oxidation, oil stain, dust and the like, and how to clean and assemble and weld a large unit weight consumable electrode is a difficult point for preparing the residual titanium plate blank ingot.
Disclosure of Invention
In view of this, the present invention provides a method for preparing a titanium ingot by fusion welding and remelting of a residual titanium slab assembly package.
The invention provides a preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot, which comprises the following steps:
and sequentially polishing and cleaning the residual titanium plate blank to obtain an oxide skin, pickling, baking, stacking in a consumable furnace, packaging a primary smelting auxiliary electrode and performing secondary vacuum consumable smelting to obtain a titanium ingot.
Preferably, the residual titanium slab comprises the following components:
Fe≤0.15wt％；
O≤0.1wt％；
C≤0.01wt％；
N≤0.01wt％；
H≤0.005wt％；
the balance being Ti.
Preferably, the method for polishing and cleaning the oxide skin is grinding by using a grinding wheel.
Preferably, the acid-washing agent comprises HF and HNO 3 The mixed solution of (1).
Preferably, the mass concentration of HF in the mixed solution is 5-10%;
HNO in the mixed solution 3 The mass concentration of (A) is 20-30%.
Preferably, the baking temperature is 140-160 ℃;
the baking time is more than or equal to 3 hours.
Preferably, 3 layers are stacked in the consumable furnace, 1-2 slabs are stacked at the bottom layer, and 3 slabs are stacked at the first layer and the second layer.
Preferably, the current in the primary smelting auxiliary electrode packaging process is 8-15 kA.
Preferably, the current of the secondary vacuum consumable melting is 15-20 kA.
Preferably, the diameter of the titanium ingot is more than or equal to 600 mm; the weight is more than 1.5 t.
The invention provides a preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot, which is suitable for production of preparing the titanium ingot from the residual titanium plate blank. The method comprises the steps of grinding, cleaning and baking the residual titanium plate blank, stacking and combining the residual titanium plate blank in a consumable melting crucible, electrifying and melting the stacked residual titanium plate blank by using a large-size auxiliary electrode, enabling molten liquid to flow below the crucible and fill a gap, and packaging the stacked residual titanium plate blank in a liquid solidification body (with the specification diameter phi 560 mm); cooling for 4 hours after stopping power supply, discharging, and then loading into a crucible with the diameter of 660mm for secondary melting, and finally preparing the pure titanium ingot meeting the requirements.
The new process provided by the invention can produce pure titanium ingots with the section diameter of phi 660mm, the unit weight of the ingots is more than 1.5t (ton), and a new process for utilizing residual titanium is provided. The novel process provided by the invention is simple to operate, and the residual titanium plate blank is subjected to polishing cleaning, acid cleaning, clean water soaking cleaning and baking; and then, the auxiliary electrode which is smelted by self-consumption is used for packaging, and the packaged electrode is firmly combined.
The method adopts a mode of adjusting the polishing, cleaning and optimizing the assembly welding of the residual titanium plate blank, utilizes the smelting auxiliary electrode to package the residual titanium plate blank, adopts the consumable smelting process of the second smelting, and obtains the cast ingot with phi being more than or equal to 600mm through twice vacuum consumable smelting. The new method provided by the invention can ensure the internal quality and the single-branch weight of the residual titanium slab smelting ingot, and provides a new process for residual titanium utilization.
Drawings
FIG. 1 is a photograph of a stack in a consumable furnace in an embodiment of the present invention;
FIG. 2 is a diagram of an embodiment of the present invention after an auxiliary electrode is encapsulated in a primary smelting process;
FIG. 3 is a picture of a titanium ingot prepared in an example of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used are conventional methods unless otherwise specified.
The invention provides a preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot, which comprises the following steps:
and sequentially polishing and cleaning the residual titanium plate blank to obtain an oxide skin, pickling, baking, stacking in a consumable furnace, packaging a primary smelting auxiliary electrode and performing secondary vacuum consumable smelting to obtain a titanium ingot.
In the invention, the residual titanium plate blank is a plate head which is sawed after being heated, forged and formed at a high temperature, and the surface of the plate head is provided with a thicker high-temperature oxidation layer; the residual titanium plate blank preferably comprises the following components:
Fe≤0.15wt％；
O≤0.1wt％；
C≤0.01wt％；
N≤0.01wt％；
H≤0.005wt％；
the balance being Ti.
In the invention, the mass content of Fe is preferably 0.05-0.13%, more preferably 0.08-0.1%, and most preferably 0.09%; the mass content of O is preferably 0.05-0.09%, more preferably 0.06-0.08%, and most preferably 0.07%; the mass content of C is preferably 0.005-0.01%, more preferably 0.006-0.008%, and most preferably 0.007%; the mass content of N is preferably 0.005-0.01%, more preferably 0.006-0.008%, and most preferably 0.007%; the content of H is preferably 0.001 to 0.005% by mass, more preferably 0.002 to 0.004% by mass, and most preferably 0.003% by mass.
In the invention, the polishing and cleaning oxide skin is preferably polished and cleaned by using a grinding wheel.
In the present invention, the agent for acid washing preferably comprises HF and HNO 3 The mixed solution of (1).
In the present invention, the solvent in the mixed solution is preferably water.
In the invention, the mass concentration of HF in the mixed solution is preferably 5-10%, more preferably 6-9%, and most preferably 7-8%; HNO in the mixed solution 3 The mass concentration of (b) is preferably 20 to 30%, more preferably 22 to 28%, more preferably 24 to 26%, and most preferably 25%.
In the invention, the acid cleaning can remove dust on the surface of the polished residual titanium plate blank and an oxide layer which is not polished and cleaned.
In the present invention, it is preferable that the acid cleaning further comprises:
and soaking the pickled product in clear water to remove residual acid solution, draining water and baking.
In the present invention, the baking is preferably carried out in a baking oven; the baking temperature is preferably 140-160 ℃, more preferably 145-155 ℃, and most preferably 150 ℃; the baking time is preferably not less than 3 hours, more preferably 3-5 hours, and most preferably 4 hours.
In an embodiment of the invention, a picture of a stack in a consumable furnace is shown in fig. 1. In the invention, 3 layers (a bottom layer, a first layer and a second layer) are preferably stacked in the consumable furnace, residual titanium plate blanks with proper sizes are selected for stacking, 2-3 residual titanium plate blanks are preferably stacked in the bottom layer, and 1-3 residual titanium plate blank combinations are preferably stacked in the first layer and the second layer; more preferably, 3 residual titanium slabs are stacked on the bottom layer, 2 residual titanium slabs are stacked on the first layer, and 1 slab is stacked on the third layer. In the invention, the size of the residual titanium plate blank is preferably 150-200 × 200-300 × 1000-1500 mm, more preferably 160-190 × 220-280 × 1100-1400 mm, and most preferably 170-180 × 240-260 × 1200-1300 mm.
The invention carries out twice smelting in a consumable smelting furnace, and the first smelting is marked as a primary smelting auxiliary electrode package. In the invention, the stacked residual titanium plate blanks are preferably loaded into a consumable smelting furnace to carry out primary smelting auxiliary electrode packaging, wherein the primary smelting auxiliary electrode packaging refers to the adoption of the auxiliary electrode packaging stacked residual titanium plate blanks in the primary smelting process. In the invention, the diameter of the crucible in the primary smelting auxiliary electrode packaging process is preferably 550-570 mm, more preferably 555-565 mm, and most preferably 560 mm. In the invention, a large-diameter large-single-weight auxiliary electrode is preferably adopted in the primary smelting auxiliary electrode packaging process, the auxiliary electrode is melted by small current, liquid smelted by the auxiliary electrode flows to the bottom of the crucible along with the gap, and packaged and stacked residual titanium plate blanks are filled. In the invention, the current in the primary smelting auxiliary electrode packing process (current in the packing process) is preferably 8-15 kA, more preferably 10-13 kA, and most preferably 12 kA. In the invention, the mass of the auxiliary electrode packaged by the primary smelting auxiliary electrode is preferably not less than 500KG, more preferably 600-800 KG, and most preferably 700 KG; the composition of the auxiliary electrode is preferably:
Fe≤0.13wt％；
O≤0.08wt％；
C≤0.01wt％；
N≤0.01wt％；
H≤0.005wt％；
the balance being Ti.
In the invention, the mass content of Fe is preferably 0.05-0.13%, more preferably 0.08-0.1%, and most preferably 0.09%; the mass content of O is preferably 0.05-0.08%, more preferably 0.06-0.08%, and most preferably 0.07%; the mass content of C is preferably 0.005-0.01%, more preferably 0.006-0.008%, and most preferably 0.007%; the mass content of N is preferably 0.005-0.01%, more preferably 0.006-0.008%, and most preferably 0.007%; the content of H is preferably 0.001 to 0.005% by mass, more preferably 0.002 to 0.004% by mass, and most preferably 0.002% by mass.
In the invention, the vacuum degree is preferably controlled to be less than or equal to 1Pa, more preferably 0.5-0.08 Pa, more preferably 0.1-0.4 Pa, and most preferably 0.2-0.3 Pa in the primary smelting auxiliary electrode packaging process; the smelting voltage is preferably 30-40V, more preferably 32-38V, and most preferably 34-36V; the smelting current is preferably 8-15 kA, more preferably 8-13 kA, more preferably 9-12 kA, and most preferably 10-11 kA.
In the invention, in the primary smelting auxiliary electrode packaging process, after the melting of the auxiliary electrode is finished, the vacuum cooling is preferably carried out for more than or equal to 4 hours, and after the cooling, the auxiliary electrode is taken out of the furnace and is demoulded.
In the present invention, the vacuum cooling time is preferably 4 to 6 hours, and more preferably 5 hours.
In the embodiment of the present invention, the picture after the primary smelting auxiliary electrode is encapsulated is shown in fig. 2.
In the present invention, the method for packaging the primary smelting auxiliary electrode preferably includes:
stacking the residual titanium slab in a crucible, vacuumizing, feeding power to assist an electrode to melt, flowing from a high position to a low position, solidifying upwards from the bottom surface of the crucible, and gradually coating the residual titanium slab to obtain the electrode.
In the invention, the second melting in the consumable melting furnace is marked as the second vacuum consumable melting. In the invention, after the primary smelting auxiliary electrode is packaged, the packaged product is preferably put into a consumable melting furnace for secondary vacuum consumable melting, and the diameter of the consumable melting furnace for secondary vacuum consumable melting is preferably 650-670 mm, more preferably 655-665 mm, and most preferably 660 mm.
In the invention, a product obtained after the primary smelting auxiliary electrode is encapsulated in the secondary vacuum consumable melting process is used as the consumable electrode of the secondary vacuum consumable melting, no special requirement is required for the auxiliary electrode in the secondary vacuum consumable melting process, and the components of the auxiliary electrode are consistent with those in the technical scheme, and are not described again here.
In the invention, the secondary vacuum consumable melting is preferably high-current rapid melting, and the melting current is preferably 15-20 kA, more preferably 16-19 kA, and most preferably 17-18 kA.
In the invention, the vacuum degree is preferably controlled to be less than or equal to 1Pa, more preferably 0.3-0.7 Pa, more preferably 0.4-0.6 Pa, and most preferably 0.5Pa in the secondary vacuum consumable melting process; the melting voltage is preferably 25 to 35V, more preferably 28 to 32V, and most preferably 30V.
In the present invention, after the secondary vacuum consumable melting is completed, the method preferably further includes:
and (4) cooling the smelted product in vacuum for more than or equal to 6 hours, discharging from the furnace after cooling, and demoulding to obtain the pure titanium ingot.
In the present invention, the vacuum cooling time is preferably 6 to 8 hours, and more preferably 7 hours.
In the invention, the diameter of the titanium ingot is preferably more than or equal to 600mm, more preferably 650-670 mm, and most preferably 660 mm; the weight is preferably > 1.5t (ton), more preferably 1.5 to 2.0t, most preferably 1.6 to 1.8 t; the titanium ingot is the titanium ingot prepared by the method of the technical scheme in the invention.
The picture of the titanium ingot prepared by the embodiment of the invention is shown in figure 3.
The method adopts a mode of adjusting the polishing, cleaning and optimizing the assembly welding of the residual titanium plate blank, utilizes the smelting auxiliary electrode to package the residual titanium plate blank, adopts the consumable smelting process of the second smelting, and obtains the cast ingot with phi being more than or equal to 600mm through twice vacuum consumable smelting. The novel process provided by the invention can ensure the internal quality and the single-branch weight of the residual titanium slab smelting ingot, and provides a novel process for residual titanium utilization. The novel process provided by the invention can produce the pure titanium cast ingot with the section diameter of phi 660mm, and the unit weight of the cast ingot is more than 1.5 t. The novel process provided by the invention is simple to operate, and the residual titanium plate blank is subjected to polishing cleaning, acid cleaning, clean water soaking cleaning and baking; and then, the auxiliary electrode which is smelted by self-consumption is used for packaging, and the packaged electrode is firmly combined.
The components of the residual titanium plate blank adopted in the following embodiment of the invention are as follows: fe: 0.09 wt%; o: 0.08 wt%; c: 0.009 wt%; n: 0.007 wt%; h: 0.001 wt%; the balance being Ti.
Example 1
Polishing the residual titanium plate blank by using a grinding wheel to clean oxide skin and pickling, wherein reagents for pickling are HF and HNO 3 The mixed solution of (1); the mass concentration of HF in the mixed solution is 7%; HNO in mixed solution 3 The mass concentration of (2) is 25%; the acid cleaning can remove dust on the surface of the polished residual titanium plate blank and an oxide layer which is not polished and cleaned; soaking the pickled product in clear water to remove residual acid solution, draining water and baking; the baking temperature is 150 ℃; the baking time was 4 hours.
Stacking the residual titanium plate blanks in a consumable furnace according to the diagram shown in figure 1, stacking 3 residual titanium plate blanks at the bottom layer, stacking 2 residual titanium plate blanks at the first layer, and stacking 1 residual titanium plate blank at the second layer; the size of the residual titanium slab is 180 x 250 x 1250 mm.
Smelting in a consumable smelting furnace for two times, wherein the first smelting is marked as a primary smelting auxiliary electrode package, and the auxiliary electrode package is adopted in the primary smelting process to package the stacked residual titanium plate blanks; the diameter of the crucible in the primary smelting auxiliary electrode packaging process is 560 mm; in the primary smelting auxiliary electrode packaging process, a large-diameter large-single-weight auxiliary electrode is adopted, the auxiliary electrode is melted through small current, liquid smelted by the auxiliary electrode flows to the bottom of the crucible along with the gap, and packaged and stacked residual titanium plate blanks are filled; the current in the primary smelting auxiliary electrode packaging process is 12 kA; the mass of the auxiliary electrode is 600KG, and the auxiliary electrode comprises the following components: fe: 0.11 wt%; o: 0.0:7 wt%; c: 0.008 wt%; n: 0.008 wt%; h: 0.002 wt%; the balance being Ti; controlling the vacuum degree in the primary smelting auxiliary electrode packaging process: 0.9Pa, melting voltage: 35V, melting current: 11 kA; and in the primary smelting auxiliary electrode packaging process, after the auxiliary electrode is melted, the auxiliary electrode is cooled for 5 hours in vacuum, and after cooling, the auxiliary electrode is taken out of the furnace for demolding.
The second smelting in the consumable smelting furnace is marked as secondary vacuum consumable smelting, a packaged product obtained after the primary smelting auxiliary electrode is packaged is loaded into the consumable smelting furnace for secondary vacuum consumable smelting, and the diameter of the consumable smelting furnace for secondary vacuum consumable smelting is 660 mm; and (3) packaging the primary smelting auxiliary electrode in the secondary vacuum consumable smelting process to obtain a product serving as a consumable electrode for secondary vacuum consumable smelting, and controlling the vacuum degree in the secondary vacuum consumable smelting process: 0.8Pa, melting voltage: 32V, the smelting current is 18 kA; and (3) cooling the smelted product for 7 hours in vacuum, discharging from the furnace after cooling, and demolding to obtain a pure titanium ingot with the weight of 1.95 tons.
The components of the pure titanium ingot prepared in the embodiment 1 of the invention are detected according to the standard requirements of GB/T4698, and the detection results are as follows:
| element(s) | Fe | O | C | N | H |
| Standard GB/T3620 | ≤0.2％ | ≤0.18％ | ≤0.08％ | ≤0.03％ | ≤0.015％ |
| Ingot casting head | 0.10％ | 0.11％ | 0.018％ | 0.011％ | 0.005％ |
| Cast ingot tail | 0.11％ | 0.10％ | 0.015％ | 0.012％ | 0.004％ |
Note: the head of the ingot is 300mm away from the top end of the ingot, the tail of the ingot is 300mm away from the tail end of the ingot, and the rest component elements are Ti.
According to the detection result, the chemical components of the cast ingot produced by the method meet the GB/T3620 specification.
The invention provides a preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot, which is suitable for production of preparing the titanium ingot from the residual titanium plate blank. The method comprises the steps of grinding, cleaning and baking the residual titanium plate blank, stacking and combining the residual titanium plate blank in a consumable melting crucible, electrifying and melting the stacked residual titanium plate blank by using a large-size auxiliary electrode, enabling molten liquid to flow below the crucible and fill a gap, and packaging the stacked residual titanium plate blank in a liquid solidification body (with the specification diameter phi 560 mm); cooling for 4 hours after stopping power supply, discharging, and then loading into a crucible with the diameter of 660mm for secondary melting, and finally preparing the pure titanium ingot meeting the requirements.
The new process provided by the invention can produce pure titanium ingots with the section diameter of phi 660mm, the unit weight of the ingots is more than 1.5t, and the new process for utilizing residual titanium is provided. The novel process provided by the invention is simple to operate, and the residual titanium plate blank is subjected to polishing cleaning, acid cleaning, clean water soaking cleaning and baking; and then, the auxiliary electrode which is smelted by self-consumption is used for packaging, and the packaged electrode is firmly combined.
The method adopts a mode of adjusting the polishing, cleaning and optimizing the assembly welding of the residual titanium plate blank, utilizes the smelting auxiliary electrode to package the residual titanium plate blank, adopts the consumable smelting process of the second smelting, and obtains the cast ingot with phi being more than or equal to 600mm through twice vacuum consumable smelting. The novel process provided by the invention can ensure the internal quality and the single-branch weight of the residual titanium slab smelting ingot, and provides a novel process for residual titanium utilization.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (6)
1. A preparation method of a residual titanium plate blank combined package fusion assembly welding remelting titanium ingot comprises the following steps:
sequentially polishing and cleaning an oxide skin, pickling, baking, stacking in a consumable furnace, packaging a primary smelting auxiliary electrode and performing secondary vacuum consumable smelting on the residual titanium plate blank to obtain a titanium ingot;
stacking in the consumable furnace comprises 3 layers, stacking 2-3 plate blanks at the bottom layer, and stacking 1-3 plate blanks at the first layer and the second layer;
the current in the primary smelting auxiliary electrode packaging process is 8-15 kA;
the current of the secondary vacuum consumable smelting is 15-20 kA;
the diameter of the titanium ingot is more than or equal to 600 mm; the weight is more than 1.5 t.
2. The method according to claim 1, characterized in that the composition of the residual titanium slab is:
Fe≤0.15wt％；
O≤0.1wt％；
C≤0.01wt％；
N≤0.01wt％；
H≤0.005wt％；
the balance being Ti.
3. The method of claim 1, wherein the method of grinding to clean scale is wheel grinding.
4. The method of claim 1, wherein the acid-washing agent comprises HF and HNO 3 The mixed solution of (1).
5. The method according to claim 4, wherein the mass concentration of HF in the mixed solution is 5-10%;
HNO in the mixed solution 3 The mass concentration of (A) is 20-30%.
6. The method according to claim 1, wherein the baking temperature is 140-160 ℃;
the baking time is more than or equal to 3 hours.
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| CN103866130A (en) * | 2014-03-19 | 2014-06-18 | 洛阳双瑞精铸钛业有限公司 | Method for melting titanium scraps and pure titanium wastes of thin titanium plates by electron beam cold hearth melting furnace |
| CN106119576A (en) * | 2016-06-30 | 2016-11-16 | 洛阳双瑞精铸钛业有限公司 | A kind of melting recovery method of lath-shaped titanium defective material |
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| 用等离子电子束炉生产的钛扁锭;小谷良男等;《稀有金属材料与工程》;19820825(第04期);全文 * |
| 钛合金熔炼技术的进展;王琛等;《热加工工艺》;20090910(第17期);全文 * |
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