CN113976909B - Method for promoting columnar crystal orientation equiaxial crystal transformation and structure refinement in additive manufacturing of titanium alloy - Google Patents

Method for promoting columnar crystal orientation equiaxial crystal transformation and structure refinement in additive manufacturing of titanium alloy Download PDF

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CN113976909B
CN113976909B CN202110595308.5A CN202110595308A CN113976909B CN 113976909 B CN113976909 B CN 113976909B CN 202110595308 A CN202110595308 A CN 202110595308A CN 113976909 B CN113976909 B CN 113976909B
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titanium alloy
phase
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promoting
crystal orientation
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CN113976909A (en
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张林杰
王祥
宁杰
罗锡柱
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Xian Jiaotong University
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Xian Jiaotong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10Pre-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00Products made by additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses a method for promoting the transformation of columnar crystal orientation equiaxed crystals and the tissue refinement in the additive manufacturing of titanium alloy, which comprises the following steps: before depositing each metal, uniformly coating a layer of micron-sized Fe element alcohol-based suspension on the surface of a position to be deposited, after an alcohol solvent is volatilized, performing metal deposition of the step in an inert gas protective atmosphere until the metal deposition of each step is completed, promoting titanium alloy additive manufacturing columnar crystal orientation equiaxial crystal transformation and forming an ultrafine microstructure through Fe elements, and promoting the titanium alloy additive manufacturing columnar crystal orientation equiaxial crystal transformation and tissue refinement.

Description

Method for promoting columnar crystal orientation equiaxed crystal transformation and structure refinement in additive manufacturing of titanium alloy
Technical Field
The invention belongs to the field of additive manufacturing, and relates to a method for promoting columnar crystal orientation equiaxial crystal transformation and structure refinement in additive manufacturing of titanium alloy.
Background
The additive manufacturing technology has the advantages that the additive manufacturing technology can manufacture components with complex structures and high material utilization rate, and challenges are created for the traditional material reduction manufacturing technology, especially in the field of manufacturing of Ti-6Al-4V titanium alloy components. With the development of titanium alloy additive manufacturing research, a common problem exists in the titanium alloy additive manufacturing process, namely that in the manufacturing process, beta crystals form coarse columnar crystals with the height exceeding the thickness of a few deposition layers in an epitaxial growth mode, the coarse columnar crystals cause anisotropy of the performance of the deposition layers, and a phase transformation process forms a large-size lath-shaped alpha phase, so that the popularization and the application of the titanium alloy component are not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for promoting the transformation and the structure refinement of columnar crystal orientation equiaxed crystal in the additive manufacturing of titanium alloy.
In order to achieve the purpose, the method for promoting the transformation of columnar crystal orientation equiaxed crystal and the structure refinement in the additive manufacturing of the titanium alloy comprises the following steps:
before depositing each metal pass, uniformly coating a layer of micron-sized Fe element alcohol-based suspension on the surface of a position to be deposited, after an alcohol solvent is volatilized, performing metal deposition in the pass under the protective atmosphere of inert gas until the metal deposition in each pass is finished, and promoting the titanium alloy additive to manufacture columnar crystal-orientation equiaxial crystal transformation and form a superfine microstructure through Fe element.
The method specifically comprises the following steps:
1) Preparing ethanol suspension of micron-sized Fe element;
2) Uniformly coating the ethanol suspension of the micron-sized Fe element on the surface of a position to be deposited, and standing to volatilize ethanol;
3) Performing the metal deposition of the pass in the argon atmosphere, and then cooling to room temperature;
4) And repeating the step 2) and the step 3) until all metal deposition passes are finished.
The average size of Fe element in the micron-sized Fe element alcohol-based suspension is 5 mu m.
The mass percent Fe (wt)% =20 x wire feeding speed (m/s) ÷ scanning speed (m/s) × 100% of Fe element in the micron-sized Fe element alcohol-based suspension.
The Fe element enables large components generated at the solidification front of the titanium alloy to be supercooled, promotes the nucleation of the titanium alloy melt at the solidification front, causes nucleation particles generated at the solidification front of a molten pool to grow in a competitive growth mode, and forms isometric crystals in a sediment body.
The addition of Fe element results in the formation of ω -phase and TiFe-phase in the deposit.
The TiFe phase is generated by the eutectoid decomposition of beta phase and is dispersed in the sediment body.
When the beta phase is eutectoid decomposed, the TiFe phase grows before the alpha phase, the TiFe is used as nucleation mass point of the alpha phase to promote the generation of the nano-scale alpha phase, and the size of the alpha phase in the sediment body is nano-scale.
The shape of the primary beta crystal grains of the titanium alloy deposition layer added with the appropriate amount of the Fe element deposition body element is isometric crystal, and the average size is 50 mu m.
The invention has the following beneficial effects:
according to the method for promoting the transformation of columnar crystal to isometric crystal and the structure refinement of the titanium alloy additive manufacturing, during specific operation, the generation of isometric beta crystal is promoted by adding the micron-sized Fe element, and meanwhile, the deposition layer is promoted to form a superfine microstructure, and in addition, the effects of fine crystal strengthening, dispersion strengthening and solid solution strengthening in the deposition body after the Fe element is added are enhanced, so that the deposition body obtains excellent mechanical properties. Compared with the additive manufacturing Ti-6Al-4V alloy without adding Fe element, the size of beta crystal grains in the titanium alloy sediment body is about 50 mu m after adding proper amount of Fe, and the average hardness, yield strength, compressive strength and plastic deformation of the sediment body are respectively improved by 3.5%, 43%, 70% and 79%.
Drawings
FIG. 1 is a scanning photograph of the original Fe powder morphology;
FIG. 2a is a macroscopic metallographic photograph of a cross section of a Ti-6Al-4V deposition layer without Fe addition;
FIG. 2b is a macroscopic metallographic photograph of a Ti-6Al-4V deposition layer cross section with an appropriate amount of Fe added;
FIG. 3a is a schematic diagram showing the growth of nucleation on the solidification front of a Ti-6Al-4V deposition layer without Fe;
FIG. 3b is the nucleation and growth diagram of Ti-6Al-4V deposition layer with proper amount of Fe added in the solidification front
FIG. 4 is a XRD test result picture of Ti-6Al-4V sediment without Fe and with proper amount of Fe;
FIG. 5a is a photograph of a TiFe phase promoting the nucleation of an alpha phase in a Ti-6Al-4V condensate with an appropriate amount of Fe added;
FIG. 5b is an enlarged photograph of area A of FIG. 5 a;
FIG. 6 is a graph comparing the compression curves of Ti-6Al-4V sediment without Fe and with Fe in proper amount;
FIG. 7a is a microhardness curve of Ti-6Al-4V condensate without Fe addition;
FIG. 7b is a micro-hardness curve of Ti-6Al-4V deposit with the addition of appropriate amount of Fe.
Detailed Description
In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments, and do not limit the scope of the disclosure of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present disclosure. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
There is shown in the drawings a schematic block diagram of a disclosed embodiment in accordance with the invention. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of the various regions, layers and their relative sizes, positional relationships are shown in the drawings as examples only, and in practice deviations due to manufacturing tolerances or technical limitations are possible, and a person skilled in the art may additionally design regions/layers with different shapes, sizes, relative positions, according to the actual needs.
The method for promoting the transformation of the columnar crystal orientation equiaxed crystal and the structure refinement of the titanium alloy additive manufacturing comprises the following steps:
before depositing each metal, uniformly coating a layer of micron-sized Fe element alcohol-based suspension on the surface of a position to be deposited, after an alcohol solvent is volatilized, performing metal deposition in the step under the protective atmosphere of inert gas until the metal deposition in each step is finished, promoting the titanium alloy additive manufacturing columnar crystal orientation equiaxial crystal transformation and forming a superfine microstructure through Fe elements.
The method specifically comprises the following steps:
1) Preparing ethanol suspension of micron-sized Fe element;
2) Uniformly coating the ethanol suspension of the micron-sized Fe element on the surface of a position to be deposited, and standing to volatilize ethanol;
3) Performing the metal deposition of the pass in the argon atmosphere, and then cooling to room temperature;
4) And repeating the step 2) and the step 3) until all the metal deposition passes are finished.
The average size of Fe element in the micron-sized Fe element alcohol-based suspension is 5 mu m.
The mass percent of Fe element in the micron-sized Fe element alcohol-based suspension is Fe (wt)% =20 x wire feeding speed (m/s) ÷ scanning speed (m/s) × 100%, the deposition process parameters are that the laser power is 3300KW, the wire feeding speed is 0.064m/s, the scanning speed is 0.02m/s, and the defocusing amount is 20mm.
The Fe element is used for enabling large components generated at the solidification front of the titanium alloy to be supercooled, and promoting the nucleation of a titanium alloy melt at the solidification front, so that nucleation particles generated at the solidification front of a molten pool grow up in a competitive growth mode, and isometric crystals are formed in a sediment body; the addition of Fe element results in the formation of omega phase and TiFe phase in the deposit; the TiFe phase is generated by beta-phase eutectoid decomposition and is dispersed in the sediment body, when the beta-phase eutectoid decomposition is carried out, the TiFe phase grows before the alpha-phase, the TiFe is used as a nucleation particle of the alpha-phase to promote the generation of a nanoscale alpha-phase, the size of the alpha-phase in the sediment body is nanoscale, the shape of a crystal grain of an initial beta crystal of a titanium alloy sediment layer added with a proper amount of Fe element sediment element is isometric crystal, and the average size of the initial beta crystal is 50 mu m.
The microstructure photograph of the Ti-6Al-4V alloy deposition layer without Fe element is shown in figure 2a, the grain size of primary beta crystal exceeds 100 μm; the microstructure photograph of the Ti-6Al-4V alloy deposition layer added with Fe element is shown in FIG. 2b, and the grain size of the primary beta crystal is about 50 μm. As shown in FIG. 3, fe can generate large component supercooling at the solidification front of the titanium alloy, promote the nucleation of the titanium alloy melt at the solidification front, cause the nucleation mass point generated at the solidification front of the molten pool to grow in a competitive growth mode, and form isometric crystals in the sediment body. XRD detection results show that after the Fe element is added, omega phase and TiFe phase can be generated in the sediment, as shown in figure 4. The TiFe phase is generated by β -phase eutectoid decomposition and is dispersed in the deposit body, when β -phase eutectoid decomposition occurs, the growth rate of TiFe phase is faster and grows earlier than α -phase, tiFe phase is generated in β → TiFe + α process, and TiFe phase grows earlier as the first phase in the reaction process, as shown in fig. 5, tiFe after growing up is used as nucleation mass point of α -phase, promoting the generation of nanoscale α -phase.
FIG. 6 is a compressive strength curve of Ti-6Al-4V deposit layer without and with proper addition of Fe element, the yield strength of the deposit layer without addition of Fe element is 1000MPa, the compressive strength is 1670MPa, and the plastic deformation is 24%; after proper Fe element is added, the yield strength of a deposition layer is 1430MPa, the compressive strength is 2830MPa, and the plastic deformation is 43 percent.
FIG. 7 is a graph showing the hardness distribution of Ti-6Al-4V deposition layers to which no Fe element is added and to which an appropriate Fe element is added, the average hardness of the deposition layers to which no Fe element is added being 430HV; the average hardness of the deposit layer after adding proper Fe element is 445HV. After a proper amount of Fe is added, the average hardness, the yield strength, the compressive strength and the plastic deformation of the titanium alloy sediment body are respectively improved by 3.5 percent, 43 percent, 70 percent and 79 percent.
The above examples are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention is described in detail with reference to the above examples, those of ordinary skill in the art should understand that: similar technical approaches can be derived from the solutions given in the figures and examples, as described above. The method can be used in the process of performing additive forming by using titanium alloy wires with different diameters and different alloy element contents as filling metals by utilizing heat sources such as electric arcs, electron beams and the like. Fe element is utilized to promote equiaxial beta crystal to be formed in the sediment body, and meanwhile, the superfine microstructure is generated through the second phase induced sediment body, so that the effects of fine grain strengthening, dispersion strengthening and solid solution strengthening are simultaneously performed on the sediment body. Any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention are within the scope of the technical solution of the present invention.

Claims (4)

1. A method for promoting columnar crystal orientation equiaxed crystal transformation and structure refinement in titanium alloy additive manufacturing is characterized by comprising the following steps:
before depositing each metal, uniformly coating a layer of micron-sized Fe element alcohol-based suspension on the surface of a position to be deposited, after an alcohol-based solvent is volatilized, performing metal deposition in the step under the protective atmosphere of inert gas until the metal deposition in each step is finished, and promoting the titanium alloy additive manufacturing columnar crystal orientation equiaxial crystal transformation and forming a superfine microstructure through Fe elements; the addition of Fe element leads to the formation of omega phase and TiFe phase in the sediment body; the TiFe phase is generated by beta-phase eutectoid decomposition and is dispersed and distributed in the sediment body; when the beta phase is eutectoid decomposed, the TiFe phase grows before the alpha phase, the TiFe is used as nucleation mass point of the alpha phase to promote the generation of the nanoscale alpha phase, and the size of the alpha phase in the sediment body is nanoscale; the shape of the crystal grain of the primary beta crystal of the titanium alloy sedimentary layer added with the sedimentary body element of a proper amount of Fe element is isometric crystal, and the average size is 50 mu m;
the average size of Fe element in the micron-sized Fe element alcohol-based suspension is 5 mu m.
2. The method for promoting columnar crystal orientation equiaxed crystal transformation and structure refinement in additive manufacturing of the titanium alloy as claimed in claim 1, is characterized by comprising the following steps:
1) Preparing ethanol suspension of micron-sized Fe element;
2) Uniformly coating the ethanol suspension of the micron-sized Fe element on the surface of a position to be deposited, and standing to volatilize ethanol;
3) Performing the metal deposition of the pass in the argon atmosphere, and then cooling to room temperature;
4) And repeating the step 2) and the step 3) until all the metal deposition passes are finished.
3. The method for promoting columnar crystal orientation equiaxial crystal transformation and structure refinement of titanium alloy additive manufacturing according to claim 1, wherein the mass percentage of Fe element in the micron-sized Fe element alcohol-based suspension is Fe (wt.)% =20 × wire feeding speed (m/s) ÷ scanning speed (m/s) × 100%.
4. The method for promoting columnar crystal orientation equiaxed crystal transformation and structure refinement of titanium alloy additive manufacturing according to claim 1, characterized in that the titanium alloy is promoted to nucleate at the solidification front by overcooling large components generated at the solidification front of the titanium alloy through Fe element, so that nucleation particles generated at the solidification front of a molten pool are grown up in a competitive growth mode, and equiaxed crystals are formed in a deposited body.
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