CN108384966B - Method for smelting TA10 titanium alloy by using electron beam cold hearth furnace - Google Patents

Method for smelting TA10 titanium alloy by using electron beam cold hearth furnace Download PDF

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CN108384966B
CN108384966B CN201810331403.2A CN201810331403A CN108384966B CN 108384966 B CN108384966 B CN 108384966B CN 201810331403 A CN201810331403 A CN 201810331403A CN 108384966 B CN108384966 B CN 108384966B
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CN108384966A (en
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周武
赵统福
杜彬
陈生
李明
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Qinghai Supower Titanium Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • C22B9/22Remelting metals with heating by wave energy or particle radiation
    • C22B9/228Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium

Abstract

The application discloses a method for smelting TA10 titanium alloy by using an electron beam cold bed furnace, belonging to the field of titanium alloy. The method comprises the following steps: 1) mixing and pressing materials containing titanium, nickel and molybdenum into a material block, and then drying; 2) smelting the dried material block by using an electron beam cooling bed furnace to obtain TA10 titanium alloy; the electron beam cold hearth furnace smelting comprises a gun starting stage, an ingot casting bottom making stage and a stable smelting stage; the electron beam cold hearth furnace comprises a melting zone, a refining zone and a crystallization zone which are adjacent in sequence, wherein the power of the melting zone in the stable melting stage is 800-1100 Kw, the power of the refining zone is 150-180 Kw, and the power of the crystallization zone is 180-210 Kw. The TA10 titanium alloy prepared by the method has good element distribution uniformity and good surface quality.

Description

Method for smelting TA10 titanium alloy by using electron beam cold hearth furnace
Technical Field
The application relates to a method for smelting TA10 titanium alloy by using an electron beam cold bed furnace, belonging to the field of titanium alloy.
Background
With the rapidly increasing use of titanium alloys in the aerospace industry, the metallurgical quality of the alloys is of increasing importance. According to the statistics of various countries, many flight accidents are caused by early failure due to the metallurgical defects of titanium alloy components. In order to produce the titanium alloy for the high-quality and high-cleanness aeroengine rotating part, a cold bed smelting technology is internationally introduced in the end of the 80 th 20 th century, and the titanium alloy ingot for the aeronautical key part has unique advantages in production due to excellent removal effects of low-density inclusions (called LDI for short) and high-density inclusions (called HDI for short). The electron beam cold hearth melting (EB for short) technology can better eliminate high-density and low-density impurities, also can recover a large amount of residual materials, reduce the production cost, can produce flat ingots and hollow ingots, reduce the subsequent processing during the production of plates and pipes, and can melt into ingots once for certain purposes.
The TA10 titanium alloy is a low-alloying Ti-Mo-Ni near alpha alloy developed for improving the crevice corrosion performance of pure titanium, and the alloy contains 0.3 percent of Mo and 0.8 percent of Ni (mass fraction), thereby not only strengthening the alloy, but also having good crevice corrosion resistance to high-temperature and low-pH chloride or weak reducing acid. The TA10 titanium alloy has good process plasticity and welding performance, and has been widely applied in the fields of chemical industry, medical treatment, aviation and the like.
The EB melting technology in China is still in the initial stage, and large-scale application in the aspect of titanium and titanium alloy forming is not formed. The Baoji titanium industry Co., Ltd and the Yunnan titanium industry Co., Ltd respectively carry out research on an electron beam cold hearth melting one-time forming process of TA10 titanium alloy, and the research shows that: the problems of excessive volatilization of Ni element and poor distribution uniformity of the prepared TA10 alloy exist in the process of smelting the TA10 titanium alloy by using an electron beam cold bed furnace.
Disclosure of Invention
According to one aspect of the application, the method for smelting the TA10 titanium alloy by using the electron beam cold hearth furnace is provided, and the TA10 titanium alloy prepared by the method has good element distribution uniformity and good surface quality.
The method for smelting the TA10 titanium alloy by using the electron beam cold hearth furnace is characterized by comprising the following steps of:
1) mixing and pressing materials containing titanium, nickel and molybdenum into a material block, and then drying;
2) smelting the dried material block by using an electron beam cooling bed furnace to obtain TA10 titanium alloy;
the electron beam cold hearth smelting process comprises a gun starting stage, an ingot casting bottom making stage and a stable smelting stage;
the nickel content in the material block used in the gun starting stage and the ingot bottom making stage is 0.85-1.05 wt%, and the nickel content in the material block used in the stable smelting stage is 0.80-0.90 wt%;
the electron beam cold hearth furnace comprises a melting zone, a refining zone and a crystallization zone which are adjacent in sequence, wherein the power of the melting zone in the stable melting stage is 800-1100 Kw, the power of the refining zone is 150-180 Kw, and the power of the crystallization zone is 180-210 Kw.
Preferably, the lower limit of the nickel content in the charge for the start-up phase and the bottom-making phase of the ingot is selected from 0.87 wt%, 0.89 wt%, 0.90 wt%, 0.92 wt%, or 0.94 wt%, and the upper limit is selected from 0.95 wt%, 0.97 wt%, 0.99 wt%, 1.00 wt%, 1.02 wt%, or 1.04 wt%;
the lower limit of the nickel content in the mass for the stationary smelting stage is selected from 0.80 wt%, 0.82 wt%, 0.83 wt% or 0.84 wt% and the upper limit is selected from 0.85 wt%, 0.86 wt%, 0.87 wt%, 0.88 wt% or 0.89 wt%.
Further preferably, the content of nickel in the material blocks used in the gun starting stage and the ingot bottom making stage is 0.95 wt%, and the content of nickel in the material blocks used in the stable smelting stage is 0.85 wt%.
Preferably, the content of molybdenum element in the material containing titanium, nickel and molybdenum is 0.25-0.35 wt%. Further preferably, the content of molybdenum element in the material of the electron beam cold hearth smelting process is 0.3 wt%.
Preferably, the thickness of the block is 100-. Further preferably, the thickness of the panel has a lower limit selected from 110mm, 120mm, 130mm, 140mm, 150mm or 160mm and an upper limit selected from 150mm, 160mm, 170mm, 180mm or 190 mm. Even more preferably, the thickness of the panel is 170 mm.
Preferably, the lumps are fed into the melting zone in a single layer, and the feeding speed is 8-20 mm/min. Further preferably, the lower limit of the feed rate is selected from 9mm/min, 10mm/min, 11mm/min, 12mm/min, 13mm/min, 14mm/min, 15mm/min, 16mm/min or 17mm/min and the upper limit is selected from 12mm/min, 13mm/min, 14mm/min, 15mm/min, 16mm/min, 17mm/min, 18mm/min or 19 mm/min. Even more preferably, the feed rate is 14 mm/min.
Alternatively, the feed to the electron beam cold hearth melting zone may be single-sided feed and/or double-sided feed. According to one embodiment, the feed rate per side is 4-10 mm/min when the feed system is double-sided feeding.
Optionally, the dimensions of the panel are length x width x thickness: 200mm x 170mm, the mass of the mass being 20Kg according to one embodiment.
According to the size of the feeding bin of the electron beam cold hearth furnace and the quantity of materials to be smelted, the materials can be pressed into a plurality of material blocks with the same or different thicknesses. Preferably, the thickness of the plurality of blocks is the same. Alternatively, briquetting may be performed using an oil press.
Preferably, the ingot pulling speed of the electron beam cold hearth smelting process is 1-6 mm/min.
More preferably, the ingot pulling speed of the electron beam cold hearth melting process is 3 mm/min.
Preferably, four first electron guns are arranged in the melting zone, one second electron gun is arranged in the refining zone, and two third electron guns are arranged in the crystallization zone;
the current range of the first electron gun in the stable smelting stage is 7.0-9.0A, the current range of the second electron gun is 5.0-6.2A, the current range of the third electron gun is 6.0-7.0A, and the value of the vacuum degree in the electron beam cold hearth furnace is less than 7.8 multiplied by 10-3torr. The current range of the third electron gun is 6.0-7.0A, which is more beneficial to the fluidity of the Ni element and increases the uniformity of the distribution of the Ni element.
More preferably, the current range of the first electron gun in the stable smelting stage is 7.8-8.5A, the current range of the second electron gun is 5.8-6.2A, the current range of the third electron gun is 6.3-6.7A, and the value of the vacuum degree in the electron beam cold hearth in the stable smelting stage is less than 6.8 multiplied by 10-3torr。
Further preferably, the vacuum degree in the electron beam cold hearth furnace in the stable smelting stage is 0.25-0.80 Pa. Still more preferably, the vacuum degree in the electron beam cold hearth furnace in the stable smelting stage is 6.0X 10-3Pa。
Optionally, the current range of the first electron gun in the gun starting stage is 2.0-5.0A, the current range of the second electron gun is not more than 5.0A, the current range of the third electron gun is 0-2.0A, and the value of the vacuum degree in the electron beam cooling bed furnace in the gun starting stage is less than 1.2 × 10-2torr。
Preferably, the vacuum degree in the electron beam cold bed furnace in the gun starting stage is 1.0 multiplied by 10-2torr。
Preferably, the start-up phase holding time is not more than 2 h.
Optionally, the current range of the first electron gun in the ingot bottom making stage is 5.0-7.0A, and the second electron gun in the ingot bottom making stageThe current range of the electron gun is 5.0-6.0A, the current range of the third electron gun is not more than 6.5A, and the value of the vacuum degree in the electron beam cold hearth furnace in the ingot bottom making stage is less than 9.1 multiplied by 10-3torr。
Preferably, the vacuum degree in the electron beam cold hearth furnace in the ingot bottom making stage is 7.5 multiplied by 10-3torr。
Preferably, the holding time of the ingot bottom making stage is not more than 50 min.
Preferably, the electron beam cold hearth melting further comprises a feeding process.
Preferably, the feeding process comprises fine-tuning the shrink pattern at intervals between the X-axis and the Y-axis of the third electron gun until the end.
Further preferably, the feeding process comprises lowering the third electron gun at a speed of 1.3A/8min from 6.5A, and finely adjusting the shrinkage pattern every 8min by the X-axis and the Y-axis of the third electron gun until the end.
According to one embodiment of the application, the feeding process comprises the step of uniformly reducing the third electron gun at intervals of 1.3A/8min from 6.5A after the stable smelting is finished, wherein the X-axis and the Y-axis of the third electron gun graph are finely adjusted to shrink graphs until the third electron gun graph is finished every 1.3A, the feeding process time is 30-50min, and further the feeding process time is 40 min.
Preferably, the ingot prepared after the feeding process of electron beam cold bed melting is naturally cooled.
Preferably, the drying conditions in step 1) are: the temperature is 100-200 ℃, and the time is 1-4 h.
More preferably, the drying conditions in step 1) are: the temperature is 120 ℃ and the time is 2 h.
Optionally, the material comprises a mixture of titanium sponge and molybdenum-nickel alloy, and/or titanium-molybdenum-nickel alloy. The Ti-Mo-Ni alloy is adopted as a raw material, a consumable furnace is adopted to prepare a Ti-Mo-Ni alloy ingot, then an alloy scrap sample is prepared, and finally the TA10 titanium alloy is cast according to the alloy proportion, wherein the Ti-Mo-Ni alloy is closer to the melting point of a matrix titanium element, the uniform distribution of the Mo and Ni elements is facilitated, and the uniformity of the cast TA10 titanium alloy is better.
Preferably, the model of the electron beam cold hearth furnace is BMO-01.
According to another aspect of the present application, a TA10 titanium alloy is provided, the TA10 titanium alloy being prepared by the above method.
In this application, the electron beam cold bed furnace is abbreviated as EB.
Low density inclusions are abbreviated as LDI.
High density inclusions are abbreviated as HDI.
The starting period from the start of the electron gun until the first flow of the titanium liquid into the crystallizer is defined as the starting period.
The first time the titanium liquid flows into the crystallizer to the first time the ingot is pulled down is defined as the ingot bottom making stage.
And pulling down from the first time of the ingot casting to the end of melting of the materials to form a stable melting stage.
The beneficial effects that this application can produce include:
1) the method for smelting the TA10 titanium alloy by using the electron beam cold hearth furnace solves the problems of excessive volatilization of nickel element and poor distribution uniformity of elements in the TA10 titanium alloy in the smelting process of the TA10 titanium alloy ingot, and the prepared TA10 titanium alloy has qualified quality, uniform components and good surface quality.
2) The method for smelting the TA10 titanium alloy has the advantages of high smelting speed and high TA10 titanium alloy ingot casting yield.
3) The TA10 titanium alloy provided by the application has the beneficial effects of qualified quality, uniform components and good surface quality.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic view of an electron cold beam hearth furnace used in an embodiment of the present application.
FIG. 2a is a schematic view of a portion of an electron gun of an electron cold beam hearth furnace according to an embodiment of the present invention; FIG. 2b is a schematic view of the irradiation position of the electron gun.
Detailed Description
Unless otherwise indicated, the raw materials in the examples of the present application were all purchased commercially, wherein the sponge titanium was purchased from Kogyo Kindao corporation under model No. JD1704-233-4, and the Ni-Mo alloy was purchased from Chengdian vanadium industry, Inc. under model No. JNM 20170601.
The electron beam cold hearth furnace used in the examples of the present application was a BMO-01 model electron beam cold hearth furnace from Qinghai energy titanium industries, Inc.
The analysis method in the examples of the present application is as follows:
and (4) analyzing the contents of oxygen, nitrogen and hydrogen by utilizing an ONH2000 oxygen-nitrogen-hydrogen analyzer.
And (4) analyzing the content of the carbon element by using an HCS140 infrared carbon sulfur instrument.
The content of nickel and molybdenum elements is analyzed by using an ICP-7300V inductively coupled plasma emission spectrometer of PE company in America.
The present application will be described in detail below with reference to embodiments and drawings, but the present application is not limited to these embodiments and drawings.
The electron beam cold bed furnace that this application embodiment adopted is shown in fig. 1, block 4 is placed in feeder 3, the ejector pin on feeder 3 transports block 4 and gets into melting zone, electron gun 6 shines block 4 and melts, watch-dog 7 monitors melting process, titanium liquid flows into cold bed 2 from melting zone, set up baffle 5 between melting zone and cold bed in order to control the liquid level height of the titanium liquid that flows into cold bed 2, titanium liquid carries out the crystallization under the irradiation of electron gun 6 in flowing into crystallizer 1 from cold bed 2, later flow into ingot casting 9, titanium liquid carries out the ingot casting under the irradiation of electron gun 6, monitor the crystallizer liquid level through crystallizer liquid level monitor 8.
Fig. 2a is a schematic view of an electron gun portion of an electron beam cold hearth furnace according to an embodiment of the present invention, and fig. 2b is a schematic view of an irradiation position of the electron gun. The electron beam cold hearth furnace adopted in the embodiment of the application comprises a melting zone, a refining zone and a crystallization zone which are adjacent in sequence, wherein the melting zone is provided with four positions 10 irradiated by first electron guns, and the four first electron guns are respectively marked as 1-4 # electron guns; the refining area 14 is provided with a position 11 irradiated by a second electron gun, and the second electron gun is marked as a No. 5 electron gun; the crystallization zone is provided with two positions 12 for irradiation by a third electron gun, which are designated as the 6# and 7# electron guns, respectively, and three bins are placed on each side of the positions where the material blocks are placed.
In the following embodiments, the voltage of the electron gun is 30V, and the electron gun division is as follows:
1) heating the raw material to melt the raw material into liquid metal and flowing the liquid metal into a cooling bed (1-4 # electron gun);
2) heating liquid metal at the front end of the cooling bed, removing a furnace accretion in the pouring gate, and making the melt flow into a crystallizer (a deep No. 5 electron gun);
3) liquid metal in the crystallizer is heated, liquid level temperature is guaranteed to be balanced, and cold grids (6-7 # electron guns) are avoided.
Example 1 compression of briquettes No. 1-5 #, comparative briquettes D1# -D2#
Mixing raw materials containing titanium, nickel and molybdenum to prepare raw material blocks with the same accurate mass, pressing the raw material blocks into material blocks with specific dimensions and specifications, and drying. The compositions of the materials of the blocks No. 1 to No. 5 and the preparation conditions are shown in Table 1.
TABLE 1
Figure GDA0002884532920000061
Figure GDA0002884532920000071
The preparation method of the block is represented by a block No. 1 and comprises the following steps:
a. mixing materials of 640Kg (total weight of 0 grade) titanium sponge and Ni-Mo intermediate alloy, and pressing the materials into raw material blocks of 20 Kg/block (wherein 19.77Kg titanium sponge and 0.23Kg intermediate alloy) of 32 blocks;
b. the specification and the size of the pressed alloy material block are as follows: 200mm × 200mm × 170 mm;
c. before each electronic scale is used, calibration is needed, the measuring precision is detected by using a test weight block, and after alloy packaging weighing and bagging are finished, re-weighing is needed; after the material block is pressed, using a 100Kg electronic scale to randomly check the weight of the material block according to the proportion of 100 percent and recording, and using an electronic hanging scale to weigh the total weight of the material block and recording;
d. and (3) putting the pressed titanium mounds into an oven for baking, setting the temperature at 120 ℃, and operating for 2 hours.
Feeding method of embodiment 2 block blocks 1# to 5# and comparative sample block blocks D1# to D2#
Prepared material blocks 1# to 5# and comparative material blocks D1# to 2# are respectively stacked on a feeder 3 of an electron beam cold bed smelting furnace shown in Table 2to carry out smelting of TA10 titanium alloy, and the stacking rule of the material blocks is explained by taking the material block 1# as a typical representative, and the stacking requirement is as follows:
a. total requirement for stacking
Left side stacking rule: 4 pieces are put in each row in a single layer, 16 alloy material pieces are piled up in total, and 4 rows are counted;
right side stacking rule: 4 pieces are arranged in each row in a single layer, and 16 alloy material blocks are stacked in total, and 4 rows are total.
b. The specific stacking positions are schematically shown in table 2: (A represents a feed material block at the starting and ingot bottom-making stages, and B represents a feed material block at the stable melting stage)
TABLE 2
Figure GDA0002884532920000081
Example 3 preparation of ingots Nos. 1# to 5# and comparative ingots Nos. D1# to D2#
The blocks 1# to 5# prepared in the example 1 and the comparative blocks D1# to 2# are placed in a feeder according to the stacking rule of the example 2, and then are smelted in an electron beam cold bed furnace to prepare ingots, which are respectively marked as ingots 1# to 5# and comparative ingots D1# to D2#, wherein the smelting process of the electron beam cold bed furnace comprises the following stages:
(1) stage of starting electron gun
And (3) starting the gun: the condensing shell was heated without melting, and the change of vacuum in the furnace was observed. The current range of No. 1-5 gun should be strictly controlled not to be large during the furnace drying periodAt 5.0A; and simultaneously, the current range of the gun to be started 6-7 # is not more than 2.0A to preheat the bottom support. After confirming that all the electron guns have no abnormal state and the vacuum in the furnace is stable, further increasing the current to melt the condensed shell, wherein the vacuum degree in the furnace is 1.0 multiplied by 10-2torr。
(2) Ingot bottom making stage
A bottom support manufacturing stage: feeding after the surface layer of the condensation shell is completely melted, keeping the 1-4 # electron guns as synchronous as possible and keeping the current not too high, setting the current of the 1-4 # electron guns to be 6.0A, and setting the current of the 5# electron gun to be 5.5A; the left and right feeding speeds are kept consistent as much as possible; stably increasing the 6# and 7# gun currents in the bottom making process, and setting the currents to be 6.3A; cooling is not carried out after the bottom making is finished, the ingot is pulled down and directly enters a smelting stage, the vacuum degree in the furnace is 7.5 multiplied by 10-3torr。
(3) Stable smelting stage
In the stable smelting stage, the current of a No. 1-4 electron gun is set to be 8.0A, and the feeding speeds of the left side and the right side are kept consistent as much as possible; the current of a No. 5 electron gun in the refining area is set to be 5.5A, so that impurity elements are smoothly removed; after the stable smelting working condition is entered, the currents of the 6# and 7# electron guns are finely adjusted (reduced), are set to be 6.5A, and the scanning tracks of the 6# and 7# electron guns are controlled to be not overlapped at the central part of the crystallizer. Reasonably distributing electron gun scanning patterns during stable smelting period, ensuring no cold zone in cold bed and crystallizer, and vacuum degree in furnace being 6.0X 10-3torr。
(4) Feeding stage
After smelting is finished, the current of the 6# and 7# electron guns is controlled to be about 6.5A, the current of the 6# and 7# electron guns is uniformly reduced in the same time with the scanning range interval, and the 6# and 7# guns are finely adjusted to be steadily and slowly reduced from the edge to the center at the same time interval until a molten pool disappears.
(5) Discharging ingot
And (5) introducing argon into the cast ingot, cooling for 3 hours, and then discharging the cast ingot safely.
The process of smelting the ingot is described by taking the ingot 1# as a typical representative, and the preparation process of the ingot 1# comprises the following steps:
(1) the power supply cabinet is started at 20: 15 days in 8 months in 2017, and then the current of the 1-5 # electron gun is gradually increased.
(2) And starting the 6# and 7# electron guns at 15: 20.
(3) The alloy liquid flows into the crystallizer for the first time at the ratio of 16: 35.
(4) Pulling ingot for the first time at 17: 05.
(5) And (4) stopping pushing by the left pushing rod at 18: 40.
(6) And the right side of the 18:45 material pushing rod stops pushing material.
(7) And (4) stopping the No. 1-5 electron gun immediately after the materials are melted at 18:50, and beginning feeding.
(8) Ending the feeding at a ratio of 19:30, reducing the current of the No. 6-7 electron gun to 5A in the feeding process by 1A every 8 minutes, and finely adjusting the shrinkage pattern in the X axis and the Y axis of the No. 6 and 7 patterns after the current is reduced until the completion.
(9) Machining
The weight of the spindle is 618.5kg, and the size is 420 multiplied by 1320 multiplied by 250 mm; wherein the initial weight of the shell building is 195kg, the updated weight of the shell building is 205kg, the weight of the alloy lost by volatilization and sputtering is 11.5kg in the whole smelting stage, and the loss rate of the volatilization and sputtering is 1.8%.
And secondly, finishing ingot milling and sawing according to requirements, wherein the sawing amount of the head part is 30mm, and the sawing amount of the tail part is 80 mm. The experimental finished ingot weighed 450kg (sampled, planed and weighed) and had dimensions 310X 1310X 245 mm.
Example 4 stability of ingot Nos. 1-5 and comparative ingot Nos. D1-D2 in the melting Process
The process stability of the smelting process of the ingot casting No. 1-5 # and the comparative ingot casting D1-D2 # is tested, the stability of the feeding speed and the ingot pulling speed during the smelting period is analyzed, and the stability of the smelting process is explained by the smelting process of the ingot casting No. 1 #. The parameters of feed and ingot pulling speed variation during the ingot bottoming stage and the steady state melting in the preparation of ingot 1# of example 3 are shown in table 3.
TABLE 3 Process parameters during smelting
Figure GDA0002884532920000101
From the above parameters, it can be seen that:
(1) during the whole normal smelting period, the adjustment of the feeding speeds at the left side and the right side is basically kept synchronous, the feeding speed is basically controlled to be 4-10 mm/min, and the average feeding speed is 7 mm/min.
(2) The ingot pulling speed has larger fluctuation and shows the tendency of increasing and then decreasing in stages, and the average ingot pulling speed is 3 mm/min.
Chemical composition analysis of ingots Nos. 1# -5# of example 5 and comparative ingots Nos. D1# to D2#
The sampling method for analyzing the chemical components of the cast ingot comprises the following steps: sampling points are arranged on six surfaces and a section of the cast ingot after machining in the cast ingot machining workshop, and the arrangement of the sampling points can accurately reflect the distribution condition of chemical components of the cast ingot.
O, N content was measured by ONH2000 oxy-nitrogen hydrogen analyzer, and the hydrogen content was sampled at 20% of the sample. The carbon content was sampled at 20% of the sample using HCS140 infrared carbon sulfur instrument. And making marks for sampling chips on two large surfaces and the top surface of the cast ingot. An end mill is used to drill a sample of mill cuttings at the sampling point. The chemical compositions of nickel and molybdenum were analyzed using an ICP-7300V inductively coupled plasma emission spectrometer (PE corporation, USA).
The chemical composition of ingots No. 1-5 # and comparative ingots D1-D2 # were analyzed, and samples were taken from a position 70mm away from the head of the ingot, a position 140mm away from the head of the ingot, a position 210mm away from the head of the ingot, and a position 280mm away from the head of the ingot on either surface of the ingot. The results of specific chemical component measurements of ingot No. 1, which is a representative of the ingots prepared in the present application, are shown in table 4, the results of specific chemical component measurements of comparative ingot No. D1, and the results of specific chemical component measurements of comparative ingot No. D2, are shown in table 6.
TABLE 4 ingot 1# chemical composition
Figure GDA0002884532920000111
As can be seen from Table 4, in ingot 1#, the average value of the Mo element content was 0.30%, and the standard deviation was 0.019; the average value of the content of the Ni element is 0.76 percent, and the standard deviation is 0.034; all elements meet the national standard and have good uniformity. The elements are distributed uniformly, the chemical components of the cast ingot are stable, and the cast ingot meets the national standard requirements. The sampling points 6, 7 and 8 are positioned in the ingot casting stage, the average content of the Ni element is 0.75%, the material blending value is 0.95%, and the volatilization loss is 21%. The sampling points 1-5 are positioned in a normal smelting stage, the average content of Ni element is 0.77%, the material proportioning value is 0.85%, and the volatilization loss is 9%. Therefore, in the bottom making stage of the ingot, the volatilization loss rate of the Ni element is about 21 percent, and in the normal smelting stage, the volatilization loss rate of the Ni element is about 9 percent.
TABLE 5 chemical composition of comparative ingot D1#
Figure GDA0002884532920000121
TABLE 6 composition of comparative ingot D2#
Figure GDA0002884532920000122
As can be seen from tables 5 and 6, the comparative ingot D1# and comparative ingot D2# had poorer uniformity of surface element distribution, particularly poor uniformity of nickel element, than the ingots prepared in accordance with the present application.
Example 6 Ni element loss test of ingots Nos. 1# -5# and comparative sample ingot D3#
The loss rate of the Ni element in the preparation process of the cast ingot 1# to 5# is tested, and in the bottom making stage of the cast ingot, the volatilization loss rate of the Ni element is about 21 percent, and in the normal smelting stage, the volatilization loss rate of the Ni element is about 9 percent.
Comparative ingot D3# was prepared differently from ingot 1# by the following method: the current of the No. 1-4 electron gun in the bottom making stage of the ingot is 4.5A, the current of the No. 5 electron gun is set to be 6.5A, and the current of the No. 6 and No. 7 electron guns is set to be 5.5A; the current of the 1-4 # electron gun in the stable smelting stage is 6.5A, the current of the 5# electron gun is 6.7A, and the current range of the 6# and 7# guns is 5.5A.
The chemical composition of ingot D3# was tested. As shown in table 7:
TABLE 7 composition of comparative ingot D3#
Figure GDA0002884532920000131
The loss rate of the Ni element in the preparation process of the ingot D3# is tested, the volatilization loss rate of the Ni element in the ingot D3# in the ingot bottom making stage in the preparation process is about 35%, and the volatilization loss rate of the Ni element in the normal smelting stage is about 22%.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.

Claims (15)

1. A method for smelting TA10 titanium alloy by using an electron beam cold hearth furnace is characterized by comprising the following steps:
1) mixing and pressing materials containing titanium, nickel and molybdenum into a material block, and then drying;
2) smelting the dried material block by using an electron beam cooling bed furnace to obtain TA10 titanium alloy;
the electron beam cold hearth smelting process comprises a gun starting stage, an ingot casting bottom making stage and a stable smelting stage;
the gun starting stage is from the start of an electron gun until titanium liquid flows into the crystallizer for the first time, the ingot casting bottom making stage is from the first flow of the titanium liquid into the crystallizer to the first pull-down of an ingot casting, and the stable smelting stage is from the first pull-down of the ingot casting to the completion of material melting;
the nickel content in the material block used in the gun starting stage and the ingot bottom making stage is 0.85-1.05 wt%, and the nickel content in the material block used in the stable smelting stage is 0.80-0.90 wt%;
the electron beam cold hearth furnace comprises a melting zone, a refining zone and a crystallization zone which are adjacent in sequence, wherein the power of the melting zone in the stable melting stage is 800-1100 Kw, the power of the refining zone is 150-180 Kw, and the power of the crystallization zone is 180-210 Kw;
the melting zone is provided with four first electron guns, the refining zone is provided with one second electron gun, and the crystallization zone is provided with two third electron guns;
the current range of the first electron gun in the ingot bottom making stage is 5.0-7.0A, the current range of the second electron gun is 5.0-6.0A, the current range of the third electron gun is not more than 6.5A, and the value of the vacuum degree in the electron beam cooling bed furnace in the ingot bottom making stage is less than 9.1 multiplied by 10 < -3 > torr;
the current range of the first electron gun in the stable smelting stage is 7.0-9.0A, the current range of the second electron gun is 5.0-6.2A, the current range of the third electron gun is 6.0-7.0A, and the value of the vacuum degree in the electron beam cold hearth furnace is less than 7.8 multiplied by 10-3torr。
2. The method of claim 1, wherein the mass used in the lance start-up stage and the ingot bottoming stage has a nickel content of 0.95 wt%,
the nickel content in the mass used in the stationary smelting stage was 0.85 wt%.
3. The method according to claim 1, wherein the content of molybdenum in the material containing titanium, nickel and molybdenum is 0.25 to 0.35 wt%.
4. The method according to claim 3, wherein the content of molybdenum element in the material containing titanium, nickel and molybdenum is 0.30 wt%.
5. The method as claimed in claim 1, wherein the thickness of the lump is 100 to 200mm, a single layer of feed material is fed to the melting zone, and the feed material velocity is 8 to 20 mm/min.
6. A method as claimed in claim 5, wherein the lumps are 170mm thick and a single layer is fed to the melting zone, the feed rate being 14 mm/min.
7. The method according to claim 1, wherein the ingot pulling speed of the electron beam cold hearth melting process is 1-6 mm/min.
8. The method of claim 7, wherein the ingot pull speed of the electron beam cold hearth melting process is 3 mm/min.
9. The method of claim 1,
the current range of the first electron gun in the stable smelting stage is 7.8-8.5A, the current range of the second electron gun is 5.8-6.2A, the current range of the third electron gun is 6.3-6.7A, and the value of the vacuum degree in the electron beam cold hearth in the stable smelting stage is less than 6.8 multiplied by 10-3torr。
10. The method according to claim 1, wherein the current range of the first electron gun in the gun start-up phase is 2.0-5.0A, the current range of the second electron gun is not more than 5.0A, the current range of the third electron gun is 0-2.0A,
the value of the vacuum degree in the electron beam cold hearth in the gun starting stage is less than 1.2 multiplied by 10 < -2 > torr.
11. The method of claim 1, wherein the electron beam cold hearth melting further comprises a feeding process.
12. The method of claim 11, wherein the feeding process comprises fine tuning the shrink pattern to the end at intervals of the X-axis and the Y-axis of the third electron gun.
13. The method of claim 12, wherein the feeding process comprises lowering the third gun from 6.5A at a rate of 1.3A/8min, and wherein the X-axis and Y-axis of the third gun fine-tune the shrink pattern every 8min to the end.
14. The method of any one of claims 1 to 13, wherein the electron beam cold hearth furnace is of the BMO-01 type.
15. A TA10 titanium alloy, characterized in that it has been prepared by a method according to any one of claims 1 to 14.
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