CN113984812A - Method for representing original beta grains in selective laser melting TC4 alloy through special-angle grain boundaries - Google Patents
Method for representing original beta grains in selective laser melting TC4 alloy through special-angle grain boundaries Download PDFInfo
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Abstract
The invention discloses a method for representing an original beta grain boundary in a selective laser melting TC4 alloy through a special angle grain boundary, and belongs to the technical field of metal material tissue characterization. The method comprises three steps: mechanically grinding and polishing the selected laser melting TC4 alloy in a stacking state or a heat treatment state, and carrying out corrosion or electrolytic polishing treatment by using a proper mixed reagent; performing back scattered electron diffraction (EBSD) observation in a scanning electron microscope to obtain corresponding grain boundary angle distribution; special Angle Grain Boundaries (SAGB) in the range of 15-55 ° and 70-85 ° were selected for mapping to obtain the profile of the original β grains in the selected zone laser melted TC4 alloy. The original beta grains in the selective laser melting TC4 alloy determine the appearance of the microscopic structure, but the original beta grains are difficult to visually and accurately represent. The method can conveniently obtain the clear outline of the original beta grains in the selective laser melting TC4 alloy, provides a simple and accurate method for researching the evolution of the microscopic structure in the post-treatment and the influence of the microscopic structure form on the mechanical property, and has important significance for the process optimization and exploration of the selective laser melting TC4 alloy.
Description
The technical field is as follows:
the invention belongs to the technical field of metal material characterization, and particularly relates to a method for representing original beta grains in selective laser melting TC4 alloy through special angle grain boundaries.
Background art:
due to high specific strength, good biocompatibility, corrosion resistance and excellent comprehensive mechanical properties, the TC4 alloy is widely applied to the fields of aerospace, biomedicine and the like. However, the conventional Titanium alloy preparation method has the problems of high preparation cost, long delivery cycle, insufficient utilization of raw materials and the like, and prevents further popularization and application [ D.Banerjee, J.C.Williams, Perspectives on Titanium Science and Technology, Acta mater.61(2013) 844-. The Selective Laser Melting (SLM) technology is a typical additive manufacturing method, can realize the reduction of production steps, high design freedom, high material utilization efficiency and near net shape production, and improves the production efficiency of TC4 alloy [ K.G.Prashath, J.Eckert, Formation of metallic cellular microstructure in selective laser melted alloys, J.alloy.Comp.707 (2017)27-34 ]. The TC4 alloy produced by the SLM technique consists of an α' martensite phase contained in the original β grains, the mechanical properties of which are closely related to the structural characteristics. The characteristics of the mesoscopic structure are determined by original beta grains, the mesoscopic structure is expressed as a checkerboard shape related to a printing path on a printing plane, columnar grains growing along the printing direction are arranged on the side surface, and the characteristics of the mesoscopic structure have important influence on the crack propagation behavior of the material. With changes in SLM process parameters and post-processing approaches, the original beta-grain related microstructure changes [ P.Kumar, O.Prakash, U.Ramamurty, Micro-and meso-structures and the inner fluorescence on mechanical properties of selected laser filtered Ti-6Al-4V, Acta mater.154(2018) 246-. However, in the previous research, the original β crystal grains are generally roughly resolved by the clusters of α/α', which is not precise and intuitive enough, so that the research on the evolution of the microstructure and the influence of the microstructure on the performance is hindered, and the research on the microstructure-performance optimization process of preparing the TC4 alloy by SLM is not facilitated.
The invention content is as follows:
aiming at the problem that the original beta grains in the TC4 alloy are subjected to laser melting at a selected area are fuzzy in characterization at present, the invention aims to provide a method for representing the original beta grains in the TC4 alloy by special angle grain boundaries. The method combines the orientation relation between alpha/alpha' phase and parent phase beta in the TC4 alloy and the angle distribution of crystal boundary, uses the crystal boundary with special angle to represent original beta crystal grains, provides convenience for researching the evolution of the microstructure in post treatment and the influence of the microstructure morphology on the mechanical property, and has important significance for optimizing and exploring the process of melting the TC4 alloy by selective laser.
The technical scheme of the invention is as follows:
a method for representing original beta grains in selective laser melting TC4 alloy through special angle grain boundaries specifically comprises the following steps:
(1) mechanically polishing the surface of the TC4 alloy fused by the laser in the selected area in the accumulation state or the heat treatment state until the surface presents a mirror surface without scratches;
(2) using hydrofluoric acid: nitric acid: distilled water 2: 1: 17, or using perchloric acid: methanol: n-butanol 3: 30: 17, carrying out electrolytic polishing on the mixed reagent to remove the surface residual stress;
(3) carrying out back scattering electron diffraction observation in a scanning electron microscope, and carrying out statistics on the angle distribution of the grain boundary;
(4) according to the obtained grain boundary angle distribution result of (3), special angle grain boundaries in the range of 15-55 ° and 70-85 ° were selected for mapping. As the alpha/alpha' phase and the parent phase beta in the two-phase titanium alloy have Burgers orientation relation: {110} β | {0001} α;
the possible alpha/alpha' variants and the orientation differences among the variants can be calculated, and the orientation differences among the 12 variants are found to be distributed around 10 degrees, 60-65 degrees and 90 degrees in a concentrated manner, while the orientation of the original beta grains (parent phase) is randomly distributed, so that the special angle grain boundary selected in (4) can outline the original beta grains.
The material selected in the step (1) is TC4 dual-phase titanium alloy prepared by a selective laser melting method, and deformation is avoided in the post-treatment process.
In the step (2), the etching time is preferably 8 to 15 seconds, and the electrolytic polishing should be carried out at a temperature of-20 ℃ or lower.
In the step (3), the grain boundary angle distribution obtained by the back scattering electron diffraction should be counted before the noise point is removed.
In the step (4), 15-55 degrees and 70-85 degrees are not selected in a fixed range, and the orientation relation among variants and the angle distribution result of the grain boundary are combined, so that the grain boundary which does not contain alpha/alpha' in the selected special angle range is emphasized.
The design idea of the invention is as follows:
the invention discloses a method for representing original beta grains in a selective laser melting TC4 alloy through special angle grain boundaries, which combines the structure characteristics of the selective laser melting TC4 alloy and the orientation relation between alpha/alpha' phase and parent phase beta to concisely obtain the outline of the original beta grains. Because the selective laser melting technology has extremely high cooling speed (10) in the application process4K/s) that undergoes martensitic transformation during cooling, the bulk structure consisting entirely of the martensitic alpha' phase in the original beta grains [ T.Vilaro, C.Colin, J.D.Bartout, As-passivated and heat-treated microstructures of the Ti-6Al-4V alloy processed by selective laser melting, metallic. mater. trans. A42(2011) 3190-.]. The new and old two phases of the martensite phase transformation have strict Burgers orientation relation {110} beta | {0001} alpha;
by combining with the crystallographic symmetry, all 12 variants corresponding to the same parent phase beta and the orientation relationship among the variants can be calculated, the orientation differences among alpha/alpha' are intensively distributed around 10 degrees, 60-65 degrees and 90 degrees and account for more than 90% of the total grain boundary quantity [ H.Beladi, Q.Chao, G.S.Rohr, variable selection and interactive crystalline mapping distribution in texture in Ti-6Al-4V alloy, Acta mater.80(2014)478-489 ].]Although α' in the bulk state is decomposed into α in the subsequent heat treatment, the orientation does not change. Meanwhile, the orientation distribution of the high-temperature stable beta-phase is random, and thus it can be considered that 15 to 55 ℃ and 70-The grain boundaries in the approximate range of 85 ° are all pristine β grain boundaries and may thus represent the pristine β phase in the selected region laser melted TC4 alloy.
The invention has the following beneficial effects:
1. the invention combines the previous researches on the tissue characteristics of TC4 titanium alloy prepared by selective laser melting and the crystallographic relation of phase transformation in the dual-phase titanium alloy, only needs to use the back scattering electron diffraction technology, obtains the crystal orientation distribution and the grain boundary orientation difference distribution of the material at the same time, and expresses the profile of the original beta grains by using the grain boundaries with special angles (15-55 degrees and 70-85 degrees). The method provides convenience for researching the evolution of the microscopic structure and the influence of the microscopic structure on the mechanical performance, and has important significance for optimizing and exploring the process of melting the TC4 alloy by the laser in the selected area.
2. The method can obtain the original beta crystal grains of the selected area laser melting TC4 alloy after different heat treatment processes, because the orientation relation between the alpha/alpha' phase and the parent phase beta is not changed by the heat treatment.
3. The invention can accurately draw the outline of the original beta crystal grain, and provides that the microscopic structure corresponding to the original beta is related to a laser scanning path and is also related to a beta recrystallization phenomenon caused by thermal circulation in the selective laser melting process.
Description of the drawings:
figure 1 schematically shows the heat treatment process in example 1.
FIG. 2 shows the structure characteristics of the stacked selected area laser melted TC4 alloy at different scales, (a)200 Xmetallography; (b-d) EBSD-IPF map at 200X, 1000X, 10000X.
FIG. 3 shows (a) the grain boundary angle distribution in the bulk selective laser melted TC4 alloy; (b) original beta grain profile plotted at 15-55 deg. and 70-85 deg. grain boundaries.
FIG. 4 depicts the structure orientation IPF map and specific angle grain boundaries in the range of 15-55 (black) and 70-85 (red) for various selected regions of solid solution laser melted TC4 alloys.
The specific implementation mode is as follows:
the present invention will be described in more detail with reference to examples. These examples are merely illustrative of the best mode of carrying out the invention and do not limit the scope of the invention in any way.
The invention relates to a method for representing original beta grains in selective laser melting TC4 alloy through special angle grain boundaries, which comprises the following steps: the method comprises the following steps:
(1) mechanically polishing the surface of the TC4 alloy fused by the laser in the selected area in the accumulation state or the heat treatment state until the surface presents a mirror surface without scratches;
(2) using hydrofluoric acid: nitric acid: distilled water 2: 1: 17, or using perchloric acid: methanol: n-butanol 3: 30: 17, carrying out electrolytic polishing on the mixed reagent to remove the surface residual stress;
(3) carrying out back scattering electron diffraction observation in a scanning electron microscope, and carrying out statistics on the angle distribution of the grain boundary;
(4) according to the obtained grain boundary angle distribution result of (3), special angle grain boundaries in the range of 15-55 ° and 70-85 ° were selected for mapping. As the alpha/alpha' phase and the parent phase beta in the two-phase titanium alloy have Burgers orientation relation: {110} β | {0001} α;
the possible alpha/alpha' variants and the orientation differences among the variants can be calculated, and the orientation differences among the 12 variants are found to be distributed around 10 degrees, 60-65 degrees and 90 degrees in a concentrated manner, while the orientation of the original beta grains (parent phase) is randomly distributed, so that the special angle grain boundary selected in (4) can outline the original beta grains.
The material selected in the step (1) is TC4 dual-phase titanium alloy prepared by a selective laser melting method, and deformation is avoided in the post-treatment process.
In the step (2), the etching time is preferably 8 to 15 seconds, and the electrolytic polishing should be carried out at a temperature of-20 ℃ or lower.
In the step (3), the grain boundary angle distribution obtained by the back scattering electron diffraction should be counted before the noise point is removed.
In the step (4), 15-55 degrees and 70-85 degrees are not selected in a fixed range, and the orientation relation among variants and the angle distribution result of the grain boundary are combined, so that the grain boundary which does not contain alpha/alpha' in the selected special angle range is emphasized.
Example 1:
in the embodiment, the method takes the selection of the laser melting TC4 alloy in the stacking state and the solid solution state as an example, and uses a special angle grain boundary to express the original beta grains, and comprises the following specific steps:
step 1: mechanically polishing the stacked and solid solution samples, wherein the heat treatment process is shown in figure 1;
step 2: hydrofluoric acid was used for the above 7 sets of samples: nitric acid: distilled water 2: 1: 17, corroding the mixed solution for 10 s;
and step 3: performing back scattered electron diffraction (EBSD) observation under 20kV by using a ZEISS MERLIN Compact SEM field emission scanning electron microscope, processing according to Channel5 software to obtain a corresponding tissue orientation graph (IPF), and calculating the distribution of grain boundary angles; as shown in fig. 2-3.
And 4, step 4: grain boundaries in the 15-55 ° and 70-85 ° ranges are plotted in Channel5 software. By combining the corresponding IPF results, the special angle grain boundary drawn by the method is found to be well matched with the original beta crystal grains, and the alpha/alpha' sets corresponding to different original parent phases beta can be accurately divided (table 1). At the same time, the recrystallization phenomenon of the original β is clearly indicated.
Table 1 shows the possible variants of martensitic transformation and their relationship to each other according to the Burgers orientation relationship between α and β.
Claims (5)
1. A method for representing original beta grains in selective laser melting TC4 alloy through special angle grain boundaries is characterized in that the Burgers orientation relation between alpha/alpha' phase and parent phase beta in two-phase titanium alloy is utilized: {110} β | {0001} α;
the method for characterizing the original beta grains specifically comprises the following steps:
(1) and carrying out mechanical grinding and polishing treatment on the surface of the TC4 alloy in the selected area in the stacking state or the heat treatment state. Selecting 400-mesh, 800-mesh, 1200-mesh, 2000-mesh and 3000-mesh sand paper from low to high to carry out water grinding, and then mechanically polishing on damping cloth by using a 50-nanometer silicon dioxide aqueous solution until the surface presents a mirror surface without scratches;
(2) using hydrofluoric acid: nitric acid: distilled water 2: 1: 17, or using perchloric acid: methanol: n-butanol 3: 30: 17, carrying out electrolytic polishing on the mixed reagent to remove the surface residual stress;
(3) carrying out back scattering electron diffraction observation in a scanning electron microscope, and carrying out statistics on the angle distribution of the grain boundary;
(4) according to the obtained grain boundary angle distribution result of (3), special angle grain boundaries in the range of 15-55 ° and 70-85 ° were selected for mapping. As the alpha/alpha' phase and the parent phase beta in the two-phase titanium alloy have Burgers orientation relation: {110} β | {0001} α;
the possible alpha/alpha' variants and the orientation difference among the variants can be calculated through the orientation relation and symmetry, and the orientation difference among the 12 variants is intensively distributed around 10 degrees, 60-65 degrees and 90 degrees, while the orientation of the original beta grains (parent phase) is randomly distributed, so that the special angle grain boundary selected in (4) can outline the original beta grains.
2. The method of claim 1 for representing the original beta grains in the selective laser melting TC4 alloy by special angle grain boundaries, wherein the method comprises the following steps: the material selected in the step (1) is TC4 dual-phase titanium alloy prepared by a selective laser melting method, and deformation is avoided in the post-treatment process.
3. The method of claim 1 for representing the original beta grains in the selective laser melting TC4 alloy by special angle grain boundaries, wherein the method comprises the following steps: in the step (2), the etching time is preferably 8 to 15 seconds, and the electrolytic polishing should be performed at a temperature of below-20 ℃.
4. The method of claim 1 for representing the original beta grains in the selective laser melting TC4 alloy by special angle grain boundaries, wherein the method comprises the following steps: in step (3), the grain boundary angle distribution obtained by the back-scattered electron diffraction should be counted before noise points are removed.
5. The method of claim 1 for representing the original beta grains in the selective laser melting TC4 alloy by special angle grain boundaries, wherein the method comprises the following steps: in the step (4)), 15-55 degrees and 70-85 degrees are not selected in fixed ranges, and the orientation relation among variants and the angle distribution result of the grain boundary are combined, so that the grain boundary containing no alpha/alpha' in the selected special angle range is emphasized.
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Citations (5)
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| US20190106777A1 (en) * | 2017-10-06 | 2019-04-11 | University Of Utah Research Foundation | Thermo-hydrogen refinement of microstructure of titanium materials |
| US20190127834A1 (en) * | 2016-05-04 | 2019-05-02 | Université Libre de Bruxelles | Method for manufacturing ti alloys with enhanced strength-ductility balance |
| CN109900727A (en) * | 2019-03-18 | 2019-06-18 | 中国科学院金属研究所 | A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods |
| CN113020624A (en) * | 2021-03-10 | 2021-06-25 | 西北工业大学 | Heat treatment method of laser stereo-forming TC4 titanium alloy |
| CN113215508A (en) * | 2021-03-16 | 2021-08-06 | 中国科学院金属研究所 | Electric pulse treatment method for improving defect or tissue state of titanium alloy manufactured by selective laser melting and material increase |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190127834A1 (en) * | 2016-05-04 | 2019-05-02 | Université Libre de Bruxelles | Method for manufacturing ti alloys with enhanced strength-ductility balance |
| US20190106777A1 (en) * | 2017-10-06 | 2019-04-11 | University Of Utah Research Foundation | Thermo-hydrogen refinement of microstructure of titanium materials |
| CN109900727A (en) * | 2019-03-18 | 2019-06-18 | 中国科学院金属研究所 | A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods |
| CN113020624A (en) * | 2021-03-10 | 2021-06-25 | 西北工业大学 | Heat treatment method of laser stereo-forming TC4 titanium alloy |
| CN113215508A (en) * | 2021-03-16 | 2021-08-06 | 中国科学院金属研究所 | Electric pulse treatment method for improving defect or tissue state of titanium alloy manufactured by selective laser melting and material increase |
Non-Patent Citations (1)
| Title |
|---|
| Y.YANG等: "Crystallographic features of variants and phase for Ti-6Al-4V alloy fabricated by selective laser melting", 《MATERIALS SCIENCE & ENGINEERING A》 * |
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