CN113718132A - Ni alloy for refining grains by solute interaction and preparation method thereof - Google Patents
Ni alloy for refining grains by solute interaction and preparation method thereof Download PDFInfo
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- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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Abstract
The invention discloses a Ni alloy for refining grains by solute interaction and a preparation method thereof, wherein the Ni alloy is represented by the following formula: ni100‑2x‑Qx‑Zx(at.%), wherein x is 0.4-1.0, and Q and Z are metal refining elements and non-metal refining elements in equal atomic ratio. Wherein the enthalpy of mixing Q and Z is-100 to-120 kJ/mol; the solute distribution coefficient of Q is less than 1 and the solute distribution coefficient of Z is less than 1. According to the invention, two refining elements are added into the Ni alloy together, and the segregation and the interaction of the two elements at the front edge of a solid-liquid interface are utilized to inhibit the growth of crystal grains, so that the aims of promoting the transformation of columnar crystal-equiaxial crystal and refining the crystal grains by utilizing microalloying are achieved, the refined crystal grains of the Ni alloy are equiaxial crystal grains, the average crystal grain size is below 150 mu m, and the Ni alloy has the characteristics of uniform structure, isotropy and less element addition. Thereby solving the problems of the prior Ni and Ni-based alloyThe solute effect of the refined crystal grains is not obvious enough, and the finer isometric crystals can not be effectively induced to form.
Description
Technical Field
The invention belongs to the field of metal solidification structure regulation and control, and particularly relates to a Ni alloy for refining grains by utilizing solute interaction and a preparation method thereof.
Background
Ni and Ni-based alloy have excellent comprehensive properties such as high temperature resistance, plasticity, oxidation resistance, corrosion resistance and the like, and are widely applied to the industries such as aerospace, ship traffic, chemical engineering, electronic products and the like. However, as the as-cast alloy structure is generally coarse and has anisotropic structure characteristics, the mechanical properties of the alloy are low, and the application of the alloy in structural materials is limited. According to the research, grain refinement is an effective method for simultaneously improving strength and plasticity.
But the effect of refining the crystal grains of Ni and Ni-based alloy is not obvious at present, and finer isometric crystals cannot be effectively induced to form.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a Ni alloy for refining grains by utilizing solute interaction and a preparation method thereof, aiming at utilizing the common addition of two elements with the mixing enthalpy of-100 to-120 kJ/mol into Ni and utilizing the segregation and the interaction of the two elements at the front edge of a solid-liquid interface in the solidification process to inhibit the grain growth, thereby achieving the purpose of promoting the transformation of columnar crystals and equiaxial crystals and refining the grains by utilizing micro-alloying. Therefore, the technical problems that the solute effect of refined crystal grains of the existing Ni and Ni-based alloy is not obvious enough and finer isometric crystals cannot be effectively induced to form are solved.
To achieve the above object, the present invention provides a Ni alloy for refining grains using solute interaction, the Ni alloy being represented by the following formula: ni100-2x-Qx-Zx(at.%), wherein x is 0.4-1.0, and Q and Z are metal refining elements and non-metal refining elements in equal atomic ratioChemical elements, wherein the mixed enthalpy of Q and Z is-100 to-120 kJ/mol; the solute distribution coefficient of Q is less than 1 and the solute distribution coefficient of Z is less than 1.
Preferably, Q is titanium and Z is carbon.
Preferably, the Ni alloy has equiaxed grains, an average grain size of 150 μm or less, a uniform structure, fine grains, isotropy, and a small amount of added element.
Preferably, the preparation method of the Ni alloy includes the steps of:
s1, sequentially putting Ni, Q and Z meeting the stoichiometric ratio into a water-cooled copper crucible from low melting point to high melting point, wherein Z is carbon, the Z is added in the form of carbon powder and is embedded into a nickel metal block, Q is titanium, the Q is added in the form of a titanium metal block, and the Q is placed above the nickel metal block.
S2, carrying out arc melting in an argon atmosphere, keeping stirring in the melting process to uniformly diffuse elements, and cooling and solidifying to obtain a button ingot; and applying a transverse eddy magnetic field during arc melting, and further promoting elements to be rapidly and uniformly diffused through electromagnetic stirring, wherein the current intensity of the transverse eddy magnetic field is not more than 20A. In the electric arc melting, the maximum melting current is not more than 500A, the single melting time is not less than 3 minutes, and the melting frequency is not less than 5 times.
S3, performing gravity casting on the button ingot to obtain the Ni alloy.
Preferably, during the cooling solidification of the alloy, elements Q and Z are repelled to the front of the solid-liquid interface.
In general, at least the following advantages can be obtained by the above technical solution contemplated by the present invention compared to the prior art.
(1) The invention realizes the promotion of the transformation of columnar crystal-equiaxial crystal and the grain refinement by simultaneously adding two refining elements (metal refining elements and non-metal refining elements) with solute interaction, so that the crystal grains of the Ni alloy are equiaxial crystal grains, the average crystal grain size is below 150 mu m, and the Ni alloy has the characteristics of uniform structure, fine crystal grains, isotropy and small element addition amount. This is because, on the one hand, the distribution coefficients of the two refining elements added simultaneously are both less than 1, indicating that they are repelled to the front of the solid-liquid interface during solidification and aggregate, inhibiting grain growth. On the other hand, the enthalpy of mixing of two refining elements added simultaneously is-100 to-120 kJ/mol, the two refining elements have proper affinity, and the diffusion of the two elements before the interface is slowed down by the synergistic effect (solute interaction) between the two refining elements, so that the two refining elements are aggregated before the solid-liquid interface, thereby forming stronger component supercooling and refining grains more effectively.
The above-mentioned synergy effect is, for example, that in the present invention, the enthalpy of mixing of Ti and C is-109 kJ/mol, which have moderate affinity and have synergy effect, while the enthalpy of mixing of the remaining refining elements such as N and Ti is-190 kJ/mol, so that they are combined before or at the initial stage of solidification to form precipitates, which do not act as synergy effect of solute interaction; while the enthalpy of mixing of Ti and Nb is 2kJ/mol, the two are mutually exclusive and there is no synergistic effect of the two.
(2) The two elements added in the invention are segregated between crystal boundaries or dendrites, so that the crystal grains are obviously refined, and simultaneously, the good comprehensive performance of the initial state is ensured for a series of subsequent processing processes.
(3) In the preparation method provided by the invention, the distribution of the matrix metal elements can be more uniform by adopting an electric arc melting and stirring mode, so that the obtained structure grains are fine and uniform.
Drawings
FIG. 1 shows Ni in example 199.2-Ti0.4-C0.4(at.%) a solidification structure map of the alloy;
FIG. 2 shows Ni in example 299-Ti0.5-C0.5(at.%) a solidification structure map of the alloy;
FIG. 3 shows Ni in example 398.8-Ti0.6-C0.6(at.%) a solidification structure map of the alloy;
FIG. 4 is a diagram showing a coagulated structure of Ni in comparative example 1;
FIG. 5 shows Ni in comparative example 299.5-Ti0.5(at.%) coagulation of the alloyA solid tissue map;
FIG. 6 shows Ni in comparative example 399.5-C0.5(at.%) solidification structure of the alloy.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The present invention provides a Ni alloy for grain refinement using solute interaction, the Ni alloy being represented by the following formula: ni100-2x-Qx-Zx(at.%), wherein x is 0.4-1.0, Q and Z are equal atomic ratio of metal refining elements and non-metal refining elements, wherein the enthalpy of mixing Q and Z is-100 to-120 kJ/mol, the solute distribution coefficient of Q is less than 1, and the solute distribution coefficient of Z is less than 1. The solute partition coefficient refers to the ratio of the solid phase solute concentration to the liquid phase solute concentration.
Q is titanium, and Z is carbon.
The crystal grains of the Ni alloy are equiaxed crystal grains, the average crystal grain size is less than 150 mu m, and the Ni alloy has the characteristics of uniform structure, fine crystal grains, isotropy and small element addition amount.
The preparation method of the Ni alloy comprises the following steps:
s1, sequentially putting Ni, Q and Z meeting the stoichiometric ratio into a water-cooled copper crucible from low melting point to high melting point, wherein Z is carbon, the Z is added in the form of carbon powder and is embedded into a nickel metal block, Q is titanium, the Q is added in the form of a titanium metal block, and the Q is placed above the nickel metal block.
S2, carrying out arc melting in an argon atmosphere, keeping stirring in the melting process to uniformly diffuse elements, and cooling and solidifying to obtain a button ingot; and applying a transverse eddy magnetic field during arc melting, and further promoting elements to be rapidly and uniformly diffused through electromagnetic stirring, wherein the current intensity of the transverse eddy magnetic field is not more than 20A. In the electric arc melting, the maximum melting current is not more than 500A, the single melting time is not less than 3 minutes, and the melting frequency is not less than 5 times.
S3, performing gravity casting on the button ingot to obtain the Ni alloy.
During the cooling solidification of the alloy, elements Q and Z are repelled to the front of the solid-liquid interface.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
This example provides a method for refining Ni alloy grains using solute interaction, the Ni alloy having a composition of Ni99.2-Ti0.4-C0.4(at.％)。
1) The raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, wherein carbon powder is embedded in the middle of a nickel block, a titanium block is placed on the top, and the raw materials are weighed by a thousandth electronic balance to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, beginning to smelt the titanium ingot to absorb residual air to provide a high-purity atmosphere for the subsequent casting operation, and then striking an arc for smelting. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Results and analysis:
metallographic microstructure observation was performed using a scanning electron microscope, small blocks having a size of 8.5mm × 5mm × 5mm were cut out from the sample by wire cutting, polished and brightened with SiC abrasive paper of 80#, 120#, 240#, 500#, 800#, 1000#, 1200# and 2000# in this order, and then electropolished with an electropolishing apparatus to obtain a sample for metallographic observation, and the alloy obtained in example 1 was tested to have an average grain size of 148 μm.
Example 2
This example provides a method for refining Ni alloy grains using solute interaction, the Ni alloy having a composition of Ni99-Ti0.5-C0.5(at.％)。
1) The raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, wherein carbon powder is embedded in the middle of a nickel block, a titanium block is placed on the top, and the raw materials are weighed by a thousandth electronic balance to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, beginning to smelt the titanium ingot to absorb residual air to provide a high-purity atmosphere for the subsequent casting operation, and then striking an arc for smelting. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Results and analysis:
metallographic microstructure observation was performed using a scanning electron microscope, small blocks having a size of 8.5mm × 5mm × 5mm were cut out from the sample by wire cutting, polished and brightened with SiC abrasive paper of 80#, 120#, 240#, 500#, 800#, 1000#, 1200# and 2000# in this order, and then electropolished with an electropolishing apparatus to obtain a sample for metallographic observation, and the alloy obtained in example 2 was tested to have an average grain size of 118 μm.
Example 3
This example provides a method for refining Ni alloy grains using solute interaction, the Ni alloy having a composition of Ni98.8-Ti0.6-C0.6(at.％)。
1) The raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, wherein carbon powder is embedded in the middle of a nickel block, a titanium block is placed on the top, and the raw materials are weighed by a thousandth electronic balance to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, beginning to smelt the titanium ingot to absorb residual air to provide a high-purity atmosphere for the subsequent casting operation, and then striking an arc for smelting. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Results and analysis:
metallographic microstructure observation was performed using a scanning electron microscope, small blocks having a size of 8.5mm × 5mm × 5mm were cut out from the sample by wire cutting, polished and brightened with SiC abrasive paper of 80#, 120#, 240#, 500#, 800#, 1000#, 1200# and 2000# in this order, and then electropolished with an electropolishing apparatus to obtain a sample for metallographic observation, and the alloy obtained in example 3 was tested to have an average grain size of 145 μm.
Example 4
This example provides a method for refining Ni alloy grains using solute interaction, the Ni alloy having a composition of Ni98-Ti1-C1(at.％)。
1) The raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, wherein carbon powder is embedded in the middle of a nickel block, a titanium block is placed on the top, and the raw materials are weighed by a thousandth electronic balance to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, and beginning to smelt the titanium ingot to absorb residual air to provide high-purity gas for the subsequent casting operationPerforming arc striking smelting in an atmosphere. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Comparative example 1
The present comparative example provides a method of preparing Ni and Ni prepared by the method. The method comprises the following steps:
1) the raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, and the raw materials are weighed by a thousandth of an electronic balance so as to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, beginning to smelt the titanium ingot to absorb residual air to provide a high-purity atmosphere for the subsequent casting operation, and then striking an arc for smelting. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Results and analysis:
metallographic microstructure observation was performed using a scanning electron microscope, small blocks of 8.5mm × 5mm × 5mm in size were cut out from the sample by wire cutting, polished to brightness with SiC abrasive paper of 80#, 120#, 240#, 500#, 800#, 1000#, 1200# and 2000# in this order, and then electropolished with an electropolishing apparatus to obtain a sample for metallographic observation, and the average width and length of columnar crystal grains of the alloy obtained in comparative example 1 were determined to be about 269 μm and 990 μm, respectively, by tests.
Comparative example 2
The present comparative example provides a Ni alloy having a composition of Ni and a method for producing the same99.5-Ti0.5(at.％)。
1) The raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, wherein a titanium block is placed on the top, and the raw materials are weighed by a thousandth of an electronic balance so as to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, beginning to smelt the titanium ingot to absorb residual air to provide a high-purity atmosphere for the subsequent casting operation, and then striking an arc for smelting. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Results and analysis:
the metallographic microstructure observation is carried out by adopting a scanning electron microscope, small blocks with the size of 8.5mm multiplied by 5mm are cut from a sample by linear cutting, SiC sand paper of 80#, 120#, 240#, 500#, 800#, 1000#, 1200# and 2000# is used for polishing and brightening in sequence, then an electrolytic polisher is used for electrolytic polishing, the metallographic observation is carried out on the sample, and the average grain size of the alloy obtained in the comparative example 2 is 244 mu m through the test.
Comparative example 3
The present comparative example provides a Ni alloy having a composition of Ni and a method for producing the same99.5-C0.5(at.％)。
1) The raw materials are sequentially placed into a water-cooled copper crucible of a non-consumable vacuum arc melting furnace, wherein carbon powder is embedded in the middle of a nickel block, and the raw materials are weighed by a thousandth electronic balance to reduce experimental errors.
2) After the vacuum chamber is closed, vacuumizing to less than 2X 10-2Pa, then backfilling with high purity argon to about 5X 104Pa, repeating the operation for 2 times, beginning to smelt the titanium ingot to absorb residual air to provide a high-purity atmosphere for the subsequent casting operation, and then striking an arc for smelting. And (3) applying an electromagnetic field for stirring during smelting until the metal is completely solidified, and repeatedly smelting for 5 times to ensure that the component components are uniformly mixed to obtain the alloy button ingot.
3) And moving the button ingot to a casting station, striking an arc and slowly increasing current to melt the button ingot, and when the bottom alloy is completely melted and quickly drops into a copper mold casting mold right below the station, cooling to obtain the ingot with the required size.
Results and analysis:
the metallographic microstructure observation is carried out by adopting a scanning electron microscope, small blocks with the size of 8.5mm multiplied by 5mm are cut from a sample by linear cutting, SiC sand paper of 80#, 120#, 240#, 500#, 800#, 1000#, 1200# and 2000# is used for polishing and brightening in sequence, then an electrolytic polisher is used for electrolytic polishing, the metallographic observation is carried out on the sample, and the average grain size of the alloy obtained in the comparative example 2 is 401 mu m through the test.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A Ni alloy for refining grains by solute interaction, wherein the Ni alloy is represented by the following formula: ni100-2x-Qx-ZxWherein x is 0.4-1.0, Q and Z are metal refining elements and nonmetal refining elements with equal atomic ratio, and the enthalpy of mixing Q and Z is-100 to-120 kJ/mol; the solute distribution coefficient of Q is less than 1 and the solute distribution coefficient of Z is less than 1.
2. The Ni alloy of claim 1, wherein Q is titanium and Z is carbon.
3. The Ni alloy of claim 1, wherein the grains of the Ni alloy are equiaxed grains, have an average grain size of 150 μm or less, and are isotropic.
4. A method of producing the Ni alloy of any one of claims 1 to 3, comprising the steps of:
s1, sequentially putting Ni, Q and Z which meet the stoichiometric ratio into a reactor according to the sequence of melting points from low to high, thereby ensuring that the element with the lowest melting point is arranged at the lowest part;
s2, carrying out arc melting in an argon atmosphere, keeping stirring in the melting process to uniformly diffuse elements, and cooling and solidifying to obtain a button ingot;
s3, performing gravity casting on the button ingot to obtain the Ni alloy.
5. The method of claim 4, wherein Z is carbon and is added in the form of carbon powder and embedded in a nickel metal block, and Q is titanium and is added in the form of a titanium metal block and placed over the nickel metal block.
6. The preparation method of claim 4, wherein in step S2, a transverse eddy current magnetic field is applied during the arc melting, and the element diffusion is promoted to be uniform by electromagnetic stirring, and the current intensity of the transverse eddy current magnetic field is not more than 20A.
7. The production method according to claim 4, wherein in step S2, during the cooling solidification, elements Q and Z are repelled to a front edge of a solid-liquid interface.
8. The preparation method of claim 4, wherein in the step S2, in the arc melting, the maximum melting current is not more than 500A, the single melting time is not less than 3 minutes, and the melting times are not less than 5 times.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114480983A (en) * | 2022-01-26 | 2022-05-13 | 华中科技大学 | Fe alloy for refining grains by utilizing solute interaction at front edge of solidification interface and preparation method thereof |
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