CN114277255B - Method for improving component uniformity of niobium-tungsten alloy cast ingot - Google Patents
Method for improving component uniformity of niobium-tungsten alloy cast ingot Download PDFInfo
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- CN114277255B CN114277255B CN202111531123.4A CN202111531123A CN114277255B CN 114277255 B CN114277255 B CN 114277255B CN 202111531123 A CN202111531123 A CN 202111531123A CN 114277255 B CN114277255 B CN 114277255B
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 129
- GAYPVYLCOOFYAP-UHFFFAOYSA-N [Nb].[W] Chemical compound [Nb].[W] GAYPVYLCOOFYAP-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000003723 Smelting Methods 0.000 claims abstract description 115
- 238000005520 cutting process Methods 0.000 claims abstract description 28
- 238000007493 shaping process Methods 0.000 claims abstract description 13
- 230000006872 improvement Effects 0.000 claims abstract description 11
- 238000003466 welding Methods 0.000 claims description 43
- 238000010894 electron beam technology Methods 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000004140 cleaning Methods 0.000 claims description 18
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 6
- VDGISCYUNHSYCS-UHFFFAOYSA-N [C].[Nb].[W] Chemical compound [C].[Nb].[W] VDGISCYUNHSYCS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 42
- 229910045601 alloy Inorganic materials 0.000 abstract description 29
- 239000000956 alloy Substances 0.000 abstract description 29
- 238000005238 degreasing Methods 0.000 abstract description 7
- 229910052721 tungsten Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000010955 niobium Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000000265 homogenisation Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- GNKXRMZGUNTBMD-UHFFFAOYSA-N [4-[(2-methylsulfanylpyrimidin-4-yl)amino]phenyl]arsonic acid Chemical compound CSC1=NC=CC(NC=2C=CC(=CC=2)[As](O)(O)=O)=N1 GNKXRMZGUNTBMD-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 238000009826 distribution Methods 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
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- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
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- 238000005204 segregation Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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Abstract
The invention discloses a method for improving component uniformity of niobium-tungsten alloy ingots, which comprises the following steps: step one, preparing a laminated electrode; step two, smelting for the first time; step three, shaping to obtain a bar; fourthly, cutting, namely marking the original outer surface and the cutting surface; fifthly, degreasing and deoxidizing; step six, combining the cleaned equal-divided bars, enabling the cutting surface of one cleaned equal-divided bar to contact the original outer surface of the other cleaned equal-divided bar to obtain a combined bar, and fixing the combined bar to obtain a combined fixed bar; step seven, secondary smelting is carried out to obtain a secondary smelting cast ingot; and step eight, repeating the steps three to seven to finish the uniformity improvement of the components of the niobium-tungsten alloy cast ingot. The method can improve the component uniformity of the niobium-tungsten alloy cast ingot, the component content in the cast ingot meets the alloy element requirement of the qualified high-carbon niobium-tungsten alloy cast ingot, and the deviation of each element at different parts of the cast ingot is within 10%.
Description
Technical Field
The invention belongs to the technical field of material processing, and particularly relates to a method for improving component uniformity of a niobium-tungsten alloy cast ingot.
Background
The refractory metal niobium has the characteristics of high melting point, low density, highest specific strength in the range of 1093-1427 ℃, good plasticity and processability at the low temperature of-200 ℃, and the most easily added components to form an alloy, so that the refractory metal niobium is the most preferred structural material and thermal protection material in the prior aerospace. The main alloy elements of the niobium-tungsten alloy are W, mo and Zr, wherein W, mo elements and Nb have the atomic radius close to each other, so that the niobium-tungsten alloy not only has the function of solid solution strengthening, but also can improve the high-temperature strength and creep property; the Zr element not only can play a role in precipitation strengthening, but also can reduce nonmetallic inclusion and interstitial impurity aggregation on the grain boundary, thereby being beneficial to improving the plasticity and the workability of the alloy. The working temperature of the niobium-tungsten alloy under the protection of the molybdenum silicide coating can reach 1600 ℃, compared with the C103 alloy, the niobium-tungsten alloy can greatly reduce the propellant for cooling and improve the specific impulse of an engine, and has gradually become the niobium alloy with the largest dosage in recent years.
Today, niobium tungsten alloys are available in both low carbon niobium tungsten alloys and high carbon niobium tungsten alloys. It was found that carbon can form various carbides with Nb, zr, etc. as matrix in the alloy, and that the higher the carbon content, the higher the content of these carbides. Carbide dispersedly distributes crystal inside or at crystal boundary, plays a role of refining crystal grains, and simultaneously plays a role of blocking the movement of the crystal boundary in the high-temperature deformation process of the material, so that the high-temperature performance of the material is improved, and therefore, the existing high-carbon niobium tungsten alloy has a tendency of becoming the mainstream niobium tungsten alloy.
The oxygen content of the high-carbon niobium-tungsten alloy is required to be not more than 0.01wt percent, and the carbon content is 0.05 to 0.12wt percent; the low carbon niobium tungsten alloy has an oxygen content of no greater than 0.023wt.% and a carbon content of no greater than 0.02wt.%. The alloy elements of the qualified high-carbon niobium tungsten alloy cast ingot are as follows: c: (0.05 to 0.12) wt.%, W: (4.5 to 5.5) wt.%, mo: (1.7 to 2.3) wt.%, zr: (0.7 to 1.2) wt.%. In industry, the low-carbon niobium-tungsten alloy is purified by vacuum electron beam melting firstly and then subjected to alloy homogenization by vacuum consumable arc melting, and the cast ingot prepared by the method not only can homogenize main alloy elements W, mo and Zr, but also can ensure that the oxygen content meets the requirement. However, for the high-carbon niobium tungsten alloy with more strict oxygen content requirement, the vacuum degree of the arc melting furnace is far less than that of the electron beam melting furnace, and oxygen enrichment exists in the arc melting in the melting process, so that the condition that the oxygen content of an ingot after the arc melting is always more than 0.01wt.% occurs, and the chemical components of the ingot are unqualified, therefore, the ingot can only be prepared by using the electron beam melting in the industry.
In the prior art, due to the shallow depth of a molten pool of electron beam melting, lack of stirring of an electric arc in arc melting and large density difference of each alloy element, the alloy elements are extremely unevenly distributed in the molten pool, so that the uniformity of components of an ingot is poor. The common problems about chemical components in the existing high-carbon niobium tungsten alloy cast ingot are as follows: on the cross section of the ingot, 1) the content of the high-density element W in the center is higher than that in the side, the maximum deviation exceeds 20%, wherein the deviation value= (large value-small value)/small value; 2) The distribution of the low-density elements C, mo and Zr is extremely uneven, the characteristic that the content of the edge part is slightly higher than that of the core part is shown, and the maximum deviation is up to 30%; 3) The non-uniformity of the alloy elements causes local overscaling so that the components of the cast ingot are disqualified. In addition, the alloy elements are unevenly distributed in the ingot along with the increase of the specification of the ingot, so that the performance of the processed material has great fluctuation, and the use stability in a high-temperature environment is affected.
Disclosure of Invention
Alloying is realized by utilizing thermodynamic movement of metal elements in a crucible molten pool for preparing the niobium tungsten alloy ingot by using an electron beam smelting technology, and the niobium tungsten alloy ingot with uniform section elements is difficult to obtain due to segregation caused by density differences of different alloy elements. The technical problem to be solved by the invention is to provide a method for improving the component uniformity of the niobium-tungsten alloy cast ingot aiming at the defects in the prior art. According to the method, the uniformity of components of the niobium-tungsten alloy cast ingot is improved by preparing laminated electrodes, primary smelting, shaping, dividing and cutting equally, cleaning bars, combining and welding the bars, secondary smelting and repeated smelting, the C, W, mo, zr component content in the niobium-tungsten alloy cast ingot meets the alloy element requirement of the qualified high-carbon niobium-tungsten alloy cast ingot, and the deviation of each element at different parts of the cast ingot is within 10%.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for improving the uniformity of components of a niobium tungsten alloy ingot, comprising the steps of:
step one, preparing a laminated electrode, wherein the laminated electrode comprises a plurality of layers of electrode parts which are sequentially arranged along the height direction of the laminated electrode, and each layer of electrode part is made of niobium-tungsten alloy;
step two, smelting the laminated electrode for the first time to obtain a primary smelting ingot, wherein the section of the primary smelting ingot is circular;
step three, shaping the primary smelting ingot to obtain a bar with a square section;
cutting the bars in the third step to obtain two equal-divided bars, and marking the original outer surface and the cutting surface on each equal-divided bar;
Step five, carrying out oil removal and deoxidation on the equal-divided bars in the step four to obtain equal-divided bars after cleaning;
Step six, combining the cleaned equal-divided bars in the step five, so that the cutting surface of one cleaned equal-divided bar contacts the original outer surface of the other cleaned equal-divided bar to obtain a combined bar, and fixing the combined bar to obtain a combined fixed bar;
Step seven, carrying out secondary smelting on the bar after the bar is combined and fixed in the step six to obtain a secondary smelting cast ingot, wherein the section shape of the secondary smelting cast ingot is circular;
And step eight, repeating the steps three to seven to finish the uniformity improvement of the components of the niobium-tungsten alloy cast ingot.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the first step, the niobium-tungsten alloy in the same electrode part has the same batch.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the first step, the preparation method of the laminated electrode comprises the following steps: and determining the number of the niobium-tungsten alloy layers according to the number of the preset laminated electrode layers, stacking the layers along the height direction of the preset laminated electrode, binding to form a whole, and welding to obtain the laminated electrode.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the first step, the niobium-tungsten alloy is high-carbon niobium-tungsten alloy; the height and width of the laminated electrode are 200-300 mm.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the second step, the size of the circular section is phi 220-phi 380mm.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized by comprising the following specific steps of: smelting the laminated electrode in a vacuum electron beam furnace to obtain a primary smelting ingot; in the primary smelting process, the ingot pulling rate is 1-2 mm/min, the smelting power is 240 kW-580 kW, and the smelting vacuum is less than 1.0X10-2 Pa.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the third step, the ratio of the cross-sectional area of the primary smelting cast ingot to the cross-sectional area of the bar is 1.57:1; in the fourth step, the cross section of the equally-divided bar is rectangular.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the step six, the fixing is performed through argon arc welding, and the welding current of the argon arc welding is 400-550A.
The method for improving the component uniformity of the niobium-tungsten alloy cast ingot is characterized in that in the seventh step, the secondary smelting is carried out in a double-gun vacuum electron beam furnace, the ingot pulling rate of the secondary smelting is 3-4 mm/min, the smelting power is 260 kW-600 kW, and the smelting vacuum is less than 1.0x10 -2 Pa.
The method for improving the uniformity of the components of the niobium-tungsten alloy cast ingot is characterized in that in the seventh step, the size of the circular section is phi 220-phi 380mm.
Compared with the prior art, the invention has the following advantages:
1. According to the method for improving the component uniformity of the niobium-tungsten alloy cast ingot, particularly the high-carbon niobium-tungsten alloy cast ingot, is improved by preparing a laminated electrode, carrying out primary smelting, dividing and cutting equally, cleaning bars, combining and welding the bars, carrying out secondary smelting and repeated smelting, wherein the niobium-tungsten alloy bars are subjected to low-speed smelting deep purification and then recombination welding, different interface alloy elements can be combined and mixed, and the mixed smelting of the alloy elements at different positions in space dimension and time dimension is realized through repeated smelting, so that the homogenization of the alloy elements is realized.
2. The method comprises the steps of repeatedly shaping, dividing and cutting equally, cleaning bars, combining and welding the bars, and secondary smelting, so that the mixed smelting of elements after the exchange of different spatial positions is further realized.
3. The method comprises the first smelting with the ingot pulling rate of 1-2 mm/min, the second smelting with the ingot pulling rate of 3-4 mm/min and repeated second smelting, wherein the low-speed primary smelting ensures that the components are basically qualified, and the intermediate-speed secondary smelting and the intermediate-speed tertiary smelting can effectively promote the timely mixing and solidification of alloy elements in the recombined bar material, so that the uneven defects caused by element density differences are avoided.
4. Preferably, the second smelting is carried out in a double-gun vacuum smelting furnace, so that metals at different parts are simultaneously irradiated by double-gun electron beams to melt into a molten pool, and the parts with different cross-section alloy element distribution contents are ensured to be simultaneously mixed and solidified in the molten pool.
The technical scheme of the invention is further described in detail below with reference to the accompanying drawings and the examples.
Drawings
FIG. 1 is a schematic diagram of the process of the optimization method of the present invention.
FIG. 2 is a schematic diagram of a step seven feed smelting;
FIG. 3 is a schematic diagram of the analysis site of the sample for component analysis.
Detailed Description
The invention provides a method for improving component uniformity of niobium-tungsten alloy ingots, which comprises the following steps:
step one, preparing a laminated electrode, wherein the laminated electrode comprises a plurality of layers of electrode parts which are sequentially arranged along the height direction of the laminated electrode, each layer of electrode part is made of niobium-tungsten alloy, and the batches of niobium-tungsten alloy in the same layer of electrode part are the same;
The preparation method of the laminated electrode comprises the following steps: determining the number of niobium-tungsten alloy layers according to the number of preset laminated electrode layers, wherein the niobium-tungsten alloy in the same electrode layer has the same batch, and the layers are stacked along the height direction of the preset laminated electrode, bound to form a whole and welded to obtain the laminated electrode; the niobium-tungsten alloy is high-carbon niobium-tungsten alloy; the height of the laminated electrode is 200-300 mm, and the width is 200-300 mm;
Smelting the laminated electrode for the first time to obtain a primary smelting ingot, wherein the section of the primary smelting ingot is circular, and the size of the circular section is phi 220-phi 380mm;
the method specifically comprises the following steps: smelting the laminated electrode in a vacuum electron beam furnace to obtain a primary smelting ingot; in the primary smelting process, the ingot pulling rate is 1-2 mm/min, the smelting power is 240 kW-580 kW, and the smelting vacuum is less than 1.0X10 -2 Pa;
Step three, shaping the primary smelting ingot to obtain a bar with a square section; the ratio of the cross-sectional area of the primary smelting ingot to the cross-sectional area of the bar is 1.57:1;
Cutting the bars in the third step to obtain two equal-divided bars, and marking the original outer surface and the cutting surface on each equal-divided bar; the cross section of the equally-divided bar is rectangular;
Step five, carrying out oil removal and deoxidation on the equal-divided bars in the step four to obtain equal-divided bars after cleaning;
Step six, combining the cleaned equal-divided bars in the step five, so that the cutting surface of one cleaned equal-divided bar contacts the original outer surface of the other cleaned equal-divided bar to obtain a combined bar, and fixing the combined bar to obtain a combined fixed bar;
The fixing is through welding, the welding is through welding of a contact surface along the length direction by argon arc welding, the vacuum degree before the argon arc welding is less than 10Pa, the welding argon filling is 0.1Pa, and the welding current is 400-550A; the contact surface in the length direction is a combined welding surface;
Step seven, carrying out secondary smelting on the bar after the bar is combined and fixed in the step six to obtain a secondary smelting cast ingot, wherein the section shape of the secondary smelting cast ingot is circular; the size of the circular section is phi 220-phi 380mm;
The method specifically comprises the following steps: feeding the combined and fixed bars in the vertical direction in a double-gun vacuum electron beam furnace, and smelting to obtain a secondary smelting cast ingot; the ingot pulling speed is 3-4 mm/min, the smelting power is 260 kW-600 kW, and the smelting vacuum is less than 1.0X10 -2 Pa; each electron gun of the double-gun vacuum electron beam furnace emits two electron beams, one electron beam irradiates and bombards a molten pool, and the other electron beam irradiates and bombards the side surface of the bar after combined and fixed, so that the side surfaces of the bar corresponding to the cutting surface and the original outer surface after combined and fixed are simultaneously dripped and melted;
And step eight, repeating the steps three to seven to finish the uniformity improvement of the components of the niobium-tungsten alloy cast ingot.
The method of the invention realizes the uniformity improvement of the components of the niobium tungsten alloy cast ingot, especially the high-carbon niobium tungsten alloy cast ingot, through preparing a laminated electrode, primary smelting, shaping, dividing and dividing equally, combining and welding bars, secondary smelting and repeated smelting, realizes the combination, mixing and solidification of different interface alloy elements through low-speed smelting deep purification and recombination welding, realizes the mixing and smelting of the alloy elements in different parts in space dimension and time dimension through repeated smelting, and realizes the homogenization of the alloy elements.
The present invention will be specifically described with reference to examples, which are not intended to limit the present invention. The experimental procedures, which are not specified in the following examples, were carried out according to conventional methods and conditions.
The method provided by the invention is used for preparing a series of high-carbon niobium tungsten alloy ingots with improved component uniformity, and the method is specifically as follows.
Example 1
As shown in fig. 1 and 2, the present embodiment provides a method for improving the uniformity of components of a niobium tungsten alloy ingot, which includes the following steps:
Step one, preparing a laminated electrode, wherein the laminated electrode comprises electrode parts which are sequentially arranged along the height direction of the laminated electrode, each layer of electrode part is made of niobium-tungsten alloy, and the niobium-tungsten alloy in the same layer of electrode part has the same batch; in this embodiment, the laminated electrode is a cuboid with a width and a height of 200mm and a length of about 1.5m, and the number of layers is 8; the batches of the niobium tungsten alloy corresponding to the adjacent two layers of electrode parts can be the same or different, in the embodiment, the niobium tungsten alloy in different layers is the same batch, the average oxygen content of the niobium tungsten alloy in the batch is less than or equal to 0.01 wt%, the average C content is 0.05 wt%, the average W content is 4.5%, the average Mo content is 2.0%, the average Zr content is 1.2%, and the components in different batches are slightly different;
the preparation method of the laminated electrode of the embodiment comprises the following steps: according to the preset size of the laminated electrode, paving a niobium tungsten alloy strip into a first layer part with the width of 200mm and the height of 25mm, superposing the niobium tungsten alloy strip on the first layer part to form a second layer part with the same shape, and so on to obtain an 8-layer structure shown in fig. 1, binding all the niobium tungsten alloy strips into a whole, and welding to prepare the laminated electrode; the number of the niobium-tungsten alloy strips corresponding to each layer part can be multiple or one; the length of the niobium-tungsten alloy strip can be equal to or different from that of the laminated electrode, so long as the plurality of niobium-tungsten alloy strips butted in the same layer part are the same in batch; the niobium-tungsten alloy strip is a high-carbon niobium-tungsten alloy strip, and optionally, the high-carbon niobium-tungsten alloy strip is a sintered high-carbon niobium-tungsten alloy strip;
Secondly, smelting the laminated electrode in a vacuum electron beam furnace for one time to obtain a primary smelting cast ingot with a circular cross section and a circular cross section dimension phi 220; in the primary smelting process, the ingot pulling rate is 1mm/min, the smelting power is 240 kW-270 kW, and the smelting vacuum is less than 1.0X10 -2 Pa;
step three, shaping the primary smelting ingot to obtain a bar with square cross section and 156X 156mm square cross section size; the shaping is carried out by utilizing an oil press;
Step four, cutting the bar in the step three along the center line of the square section by using a band sawing machine to obtain two equal-divided bars, and marking the original outer surface and the cutting surface on each equal-divided bar; the sectional shape of the equally-divided bar is rectangular, the rectangular sectional length of the equally-divided bar is equal to the sectional side length of the bar in the step three, the sectional width of the equally-divided bar is half of the sectional side length of the bar in the step three, and the equally-divided bar is equal to the bar in the step three; the cross section of the equally divided bars is rectangular, and the cross section rectangular is 78 multiplied by 156mm;
Step five, carrying out oil removal and deoxidation on the equal-divided bars in the step four to obtain equal-divided bars after cleaning; the degreasing and deoxidization comprises degreasing with a commercial alkaline metal cleaner and deoxidizing with a nitric acid solution until the surface presents a metallic color;
Step six, combining the bars after the cleaning in the step five, enabling the cutting surface of one bar after the cleaning to contact the original outer surface of the other bar after the cleaning to obtain a combined bar, and welding and fixing the combined bar along the combined welding surface by argon arc welding to obtain a combined and fixed bar; the vacuum degree before argon arc welding is less than 10Pa, the welding argon filling is 0.1Pa, and the welding current is 400-450A;
Step seven, in a double-gun vacuum electron beam furnace, feeding the bar materials subjected to combination fixation in the step six in the vertical direction for secondary smelting to obtain a secondary smelting cast ingot with a circular cross section shape and a circular cross section specification phi 220mm, wherein in the secondary smelting, the ingot pulling speed is 3mm/min, the smelting power is 260-290 kW, and the smelting vacuum is less than 1.0x10 -2 Pa; the vertical direction is along the length direction of the bar after combined and fixed; each electron gun of the double-gun vacuum electron beam furnace emits two electron beams, one electron beam irradiates and bombards a molten pool, and the other electron beam irradiates and bombards the side surface of the bar after combined and fixed, so that the side surfaces of the bar corresponding to the cutting surface and the original outer surface after combined and fixed are simultaneously dripped and melted;
and step eight, repeating the steps three to seven to finish the improvement of the component uniformity of the niobium-tungsten alloy cast ingot with the circular cross section and the circular cross section specification phi 220 mm.
The high-carbon niobium tungsten alloy ingot obtained in this example was subjected to chemical component inspection, and 3 parts were taken in the diameter direction of the upper surface, the intermediate layer and the lower surface of the ingot, respectively, and analyzed, the schematic diagram of the parts is shown in fig. 3, and the components of element C, W, mo, zr are summarized in table 1 below.
Table 1 example 1 phi 220mm ingot sample composition summary (wt.%)
| C | W | Mo | Zr | |
| Upper 1 | 0.058 | 4.72 | 1.86 | 0.88 |
| Upper 2 | 0.059 | 4.68 | 1.90 | 0.82 |
| Upper 3 | 0.057 | 4.70 | 1.83 | 0.87 |
| In 1 | 0.061 | 4.65 | 1.85 | 0.81 |
| Middle 2 | 0.062 | 4.73 | 1.96 | 0.85 |
| In 3 | 0.057 | 4.71 | 1.85 | 0.86 |
| Lower 1 | 0.060 | 4.69 | 1.93 | 0.83 |
| Lower 2 | 0.057 | 4.75 | 1.88 | 0.81 |
| Lower 3 | 0.059 | 4.72 | 1.94 | 0.84 |
| Maximum deviation | 8.8％ | 2.2％ | 7.1％ | 8.6％ |
As can be seen from table 1, the component content of the ingot C, W, mo, zr in the embodiment meets the alloy element requirement of the qualified high-carbon niobium tungsten alloy ingot, the deviation of each element in different parts of the ingot is between 2.2% and 8.8%, the requirement of the deviation within 10% is met, the uniformity of the chemical components of the ingot is remarkably improved by the improvement method in the embodiment, and the manufacturing and use of the high-temperature alloy structural member with higher conditions are met.
Example 2
The embodiment provides a method for improving component uniformity of niobium-tungsten alloy ingots, which comprises the following steps:
Step one, preparing a laminated electrode, wherein the laminated electrode comprises electrode parts which are sequentially arranged along the height direction of the laminated electrode, each layer of electrode part is made of niobium-tungsten alloy, and the niobium-tungsten alloy in the same layer of electrode part has the same batch; in this embodiment, the laminated electrode has a width and a height of 250mm, a length of 1.8m, 3 niobium-tungsten alloy batches, and 5 layers;
The preparation method of the laminated electrode of the embodiment comprises the following steps: according to the preset size of the laminated electrode, setting a first batch of niobium tungsten alloy strips as a first layer part with the width of 250mm and the height of 50mm, setting a second batch of niobium tungsten alloy strips as a second layer part with the same shape, setting a third batch of tungsten alloy strips as a third layer part with the same shape, setting the first batch of niobium tungsten alloy strips as a fourth layer part, setting the second batch of niobium tungsten alloy strips as a fifth layer part, stacking the second layer part on the first layer part, stacking like the above, binding all niobium tungsten alloy strips into a whole, and preparing the laminated electrode by welding; the number of the niobium-tungsten alloy strips in the batch corresponding to each layer part can be multiple or one; the length of the niobium-tungsten alloy strip can be equal to or different from that of the laminated electrode, so long as the plurality of niobium-tungsten alloy strips butted in the same layer part are the same in batch; the niobium tungsten alloy strips are high-carbon niobium tungsten alloy strips, the oxygen content is not more than 0.01wt.%, the carbon content is 0.05-0.12 wt.%, and the high-carbon niobium tungsten alloy strips are sintered high-carbon niobium tungsten alloy strips;
Secondly, smelting the laminated electrode in a vacuum electron beam furnace for one time to obtain a primary smelting cast ingot with a circular section and a circular section size phi 300 mm; in the primary smelting process, the ingot pulling rate is 1.5mm/min, the smelting power is 350 kW-380 kW, and the smelting vacuum is less than 1.0X10 -2 Pa;
Step three, shaping the primary smelting ingot to obtain a bar with a square section and a square section size of 212 multiplied by 212 mm; the shaping is carried out by utilizing an oil press;
step four, cutting the bar in the step three along the center line of the square section by using a band sawing machine to obtain two equal-divided bars, and marking the original outer surface and the cutting surface on each equal-divided bar; the sectional shape of the equally-divided bar is rectangular, the rectangular sectional length of the equally-divided bar is equal to the sectional side length of the bar in the step three, the sectional width of the equally-divided bar is half of the sectional side length of the bar in the step three, and the equally-divided bar is equal to the bar in the step three; the cross section of the equally divided bars is rectangular, and the cross section rectangular is 106 multiplied by 212mm;
Step five, carrying out oil removal and deoxidation on the equal-divided bars in the step four to obtain equal-divided bars after cleaning; the degreasing and deoxidization comprises degreasing with a commercial alkaline metal cleaner and deoxidizing with a nitric acid solution until the surface presents a metallic color;
Step six, combining the bars after the cleaning in the step five, enabling the cutting surface of one bar after the cleaning to contact the original outer surface of the other bar after the cleaning to obtain a combined bar, and welding and fixing the combined bar along the combined welding surface by argon arc welding to obtain a combined and fixed bar; the vacuum degree before argon arc welding is less than 10Pa, the welding argon filling is 0.1Pa, and the welding current is 450-500A;
Step seven, in a double-gun vacuum electron beam furnace, feeding the bar materials subjected to combination fixation in the step six in a vertical direction for secondary smelting to obtain a secondary smelting cast ingot with a round cross section shape and a round cross section specification phi 300mm, wherein in the secondary smelting, the ingot pulling speed is 3.5mm/min, the smelting power is 370-400 kW, and the smelting vacuum is less than 1.0x10 -2 Pa; the vertical direction is along the length direction of the bar after combined and fixed; each electron gun of the double-gun vacuum electron beam furnace emits two electron beams, one electron beam irradiates and bombards a molten pool, and the other electron beam irradiates and bombards the side surface of the bar after combined and fixed, so that the side surfaces of the bar corresponding to the cutting surface and the original outer surface after combined and fixed are simultaneously dripped and melted;
And step eight, repeating the steps three to seven to finish the improvement of the component uniformity of the niobium tungsten alloy cast ingot with the circular cross section and the circular cross section specification phi 300 mm.
The high-carbon niobium tungsten alloy ingot obtained in this example was subjected to chemical component inspection, and 3 parts were taken in the diameter direction of the upper surface, the intermediate layer and the lower surface of the ingot, respectively, and analyzed, the schematic diagram of the parts is shown in fig. 3, and the components of element C, W, mo, zr are summarized in table 1 below.
Table 2 example 2 phi 300mm ingot sample composition summary (wt.%)
As can be seen from table 2, the component content of the ingot C, W, mo, zr in the embodiment meets the alloy element requirement of the qualified high-carbon niobium tungsten alloy ingot, the deviation of each element in different parts of the ingot is between 2.6% and 7.6%, the requirement of the deviation within 10% is met, the uniformity of the chemical components of the ingot is remarkably improved by the improvement method in the embodiment, and the manufacturing and use of the high-temperature alloy structural member with higher conditions are met.
Example 3
The embodiment provides a method for improving component uniformity of niobium-tungsten alloy ingots, which comprises the following steps:
Step one, preparing a laminated electrode, wherein the laminated electrode comprises electrode parts which are sequentially arranged along the height direction of the laminated electrode, each layer of electrode part is made of niobium-tungsten alloy, and the niobium-tungsten alloy in the same layer of electrode part has the same batch; in this embodiment, the laminated electrode is a cuboid with a width and a height of 300mm and a length of 2m, the batch of niobium-tungsten alloy is 3 batches, and the number of layers is 3;
The preparation method of the laminated electrode of the embodiment comprises the following steps: according to the preset size of the laminated electrode, paving a first batch of niobium tungsten alloy strips into a first layer part with the width of 300mm and the height of 100mm, setting a second batch of niobium tungsten alloy strips into a second layer part with the same shape, setting a third batch of tungsten alloy strips into a third layer part with the same shape, stacking the second layer part on the first layer part, stacking the first layer part, binding all niobium tungsten alloy strips into a whole, and welding to prepare the laminated electrode; the number of the niobium-tungsten alloy strips in the batch corresponding to each layer part can be multiple or one; the length of the niobium-tungsten alloy strip can be equal to or different from that of the laminated electrode, so long as the plurality of niobium-tungsten alloy strips butted in the same layer part are the same in batch; the niobium tungsten alloy strip is a high-carbon niobium tungsten alloy strip, the oxygen content is not more than 0.01wt.%, the carbon content is 0.05-0.12 wt.%, and the high-carbon niobium tungsten alloy strip is a sintered high-carbon niobium tungsten alloy strip;
Secondly, smelting the laminated electrode in a vacuum electron beam furnace for one time to obtain a primary smelting cast ingot with a circular section and a circular section size phi 380 mm; in the primary smelting process, the ingot pulling rate is 2mm/min, the smelting power is 550 kW-580 kW, and the smelting vacuum is less than 1.0X10 -2 Pa;
step three, shaping the primary smelting ingot to obtain a bar with square cross section and 269 multiplied by 269mm square cross section size; the shaping is carried out by utilizing an oil press;
Step four, cutting the bar in the step three along the center line of the square section by using a band sawing machine to obtain two equal-divided bars, and marking the original outer surface and the cutting surface on each equal-divided bar; the sectional shape of the equally-divided bar is rectangular, the rectangular sectional length of the equally-divided bar is equal to the sectional side length of the bar in the step three, the sectional width of the equally-divided bar is half of the sectional side length of the bar in the step three, and the equally-divided bar is equal to the bar in the step three; the cross section of the equally divided bars is rectangular, and the cross section rectangular is 134 multiplied by 269mm;
Step five, carrying out oil removal and deoxidation on the equal-divided bars in the step four to obtain equal-divided bars after cleaning; the degreasing and deoxidization comprises degreasing with a commercial alkaline metal cleaner and deoxidizing with a nitric acid solution until the surface presents a metallic color;
Step six, combining the bars after the cleaning in the step five, enabling the cutting surface of one bar after the cleaning to contact the original outer surface of the other bar after the cleaning to obtain a combined bar, and welding and fixing the combined bar along the combined welding surface by argon arc welding to obtain a combined and fixed bar; the vacuum degree before argon arc welding is less than 10Pa, the welding argon filling is 0.1Pa, and the welding current is 500-550A;
Step seven, in a double-gun vacuum electron beam furnace, feeding the bar materials subjected to combination fixation in the step six in the vertical direction for secondary smelting to obtain a secondary smelting cast ingot with a circular cross section shape and a circular cross section specification phi 380mm, wherein in the secondary smelting, the ingot pulling speed is 4mm/min, the smelting power is 570-600 kW, and the smelting vacuum is less than 1.0x10 -2 Pa; the vertical direction is along the length direction of the bar after combined and fixed; each electron gun of the double-gun vacuum electron beam furnace emits two electron beams, one electron beam irradiates and bombards a molten pool, and the other electron beam irradiates and bombards the side surface of the bar after combined and fixed, so that the side surfaces of the bar corresponding to the cutting surface and the original outer surface after combined and fixed are simultaneously dripped and melted;
And step eight, repeating the steps three to seven to finish the improvement of the component uniformity of the niobium-tungsten alloy cast ingot with the circular cross section and the circular cross section specification phi 380 mm.
The high-carbon niobium tungsten alloy ingot obtained in this example was subjected to chemical component inspection, and 3 parts were taken in the diameter direction of the upper surface, the intermediate layer and the lower surface of the ingot, respectively, and analyzed, the schematic diagram of the parts is shown in fig. 3, and the components of element C, W, mo, zr are summarized in table 1 below.
Table 3 example 3 sum of sample components of the Φ380mm ingot (wt.%)
| C | W | Mo | Zr | |
| Upper 1 | 0.107 | 5.29 | 2.09 | 1.05 |
| Upper 2 | 0.105 | 5.34 | 2.07 | 1.04 |
| Upper 3 | 0.101 | 5.31 | 2.10 | 1.10 |
| In 1 | 0.109 | 5.36 | 2.07 | 1.08 |
| Middle 2 | 0.106 | 5.27 | 2.12 | 1.03 |
| In 3 | 0.100 | 5.40 | 2.06 | 1.02 |
| Lower 1 | 0.108 | 5.42 | 2.05 | 1.08 |
| Lower 2 | 0.106 | 5.32 | 2.10 | 1.10 |
| Lower 3 | 0.102 | 5.39 | 2.08 | 1.09 |
| Maximum deviation | 9.0％ | 2.8％ | 3.4％ | 7.8％ |
As can be seen from table 3, the component content of the ingot C, W, mo, zr in the embodiment meets the alloy element requirement of the qualified high-carbon niobium tungsten alloy ingot, the deviation of each element in different parts of the ingot is between 2.8% and 9.0%, the requirement within 10% of the deviation is met, the uniformity of the chemical components of the ingot is remarkably improved by the improvement method in the embodiment, and the manufacturing and use of the high-temperature alloy structural member with higher conditions are met.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent structural changes of the above embodiment according to the technical matter of the present invention still fall within the scope of the technical solution of the present invention.
Claims (8)
1. A method for improving the uniformity of components of a niobium tungsten alloy ingot, comprising the steps of:
Step one, preparing a laminated electrode, wherein the laminated electrode comprises a plurality of layers of electrode parts which are sequentially arranged along the height direction of the laminated electrode, and each layer of electrode part is made of niobium-tungsten alloy; the batches of niobium-tungsten alloy in the same electrode part are the same; the preparation method of the laminated electrode comprises the following steps: determining the number of niobium-tungsten alloy layers according to the number of preset laminated electrode layers, stacking the layers along the height direction of the preset laminated electrode, binding to form a whole, and welding to obtain the laminated electrode;
Step two, smelting the laminated electrode for the first time to obtain a primary smelting ingot, wherein the section of the primary smelting ingot is circular; in the primary smelting process, the ingot pulling speed is 1-2 mm/min;
step three, shaping the primary smelting ingot to obtain a bar with a square section;
cutting the bars in the third step to obtain two equal-divided bars, and marking the original outer surface and the cutting surface on each equal-divided bar;
Step five, carrying out oil removal and deoxidation on the equal-divided bars in the step four to obtain equal-divided bars after cleaning;
Step six, combining the cleaned equal-divided bars in the step five, so that the cutting surface of one cleaned equal-divided bar contacts the original outer surface of the other cleaned equal-divided bar to obtain a combined bar, and fixing the combined bar to obtain a combined fixed bar;
Step seven, carrying out secondary smelting on the bar after the bar is combined and fixed in the step six to obtain a secondary smelting cast ingot, wherein the section shape of the secondary smelting cast ingot is circular; the secondary smelting is carried out in a double-gun vacuum electron beam furnace, and the ingot pulling rate of the secondary smelting is 3-4 mm/min;
And step eight, repeating the steps three to seven to finish the uniformity improvement of the components of the niobium-tungsten alloy cast ingot.
2. The method for improving the composition uniformity of a niobium tungsten alloy ingot according to claim 1, wherein in the first step, the niobium tungsten alloy is a high carbon niobium tungsten alloy; the height and the width of the laminated electrode are 200-300 mm.
3. The method for improving the uniformity of components of a niobium tungsten alloy ingot according to claim 1, wherein in the second step, the size of the circular cross section is Φ220- Φ380mm.
4. The method for improving the uniformity of components of a niobium tungsten alloy ingot according to claim 1, wherein in the second step, the primary melting specifically comprises: smelting the laminated electrode in a vacuum electron beam furnace to obtain a primary smelting ingot; in the primary smelting process, the smelting power is 240 kW-580 kW, and the smelting vacuum is less than 1.0X10 -2 Pa.
5. The method for improving the uniformity of components of a niobium tungsten alloy ingot according to claim 1, wherein in the third step, the ratio of the cross-sectional area of the primary smelting ingot to the cross-sectional area of the bar is 1.57:1; in the fourth step, the cross section of the equally-divided bar is rectangular.
6. The method for improving the uniformity of components of a niobium tungsten alloy ingot according to claim 1, wherein in the sixth step, the fixing is performed by argon arc welding, and the welding current of the argon arc welding is 400-550A.
7. The method for improving the uniformity of components of a niobium tungsten alloy ingot according to claim 1, wherein in the seventh step, smelting power is 260-600 kW, and smelting vacuum is less than 1.0X10 -2 Pa.
8. The method for improving the uniformity of components of a niobium tungsten alloy ingot according to claim 1, wherein in the seventh step, the size of the circular cross section is Φ220- Φ380mm.
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