3.1. Microstructure
Figure 4 and
Figure 5 show the XRD patterns of the XY and YZ planes of the SLM-formed Fe-Mn-Al-C lightweight steel samples under different solution treatment temperatures and holding times. The analysis results indicate that when the solution treatment temperature is 1050 °C, the XY plane of the samples held for 0.5 h to 1.5 h is composed of FCC face-centered cubic γ-austenite, and the diffraction peak intensities of the (111) and (220) crystal planes increase continuously with the increase in holding time. Moreover, the diffraction peak positions shift at 0.5 h and 1 h holding times, but do not shift at 1.5 h. The YZ plane is composed of FCC face-centered cubic γ-austenite and BCC body-centered cubic α-ferrite. Similarly, the diffraction peak positions shift at 0.5 h and 1 h holding times, but do not shift at 1.5 h. The reason for the diffraction peak positions shifting at 0.5 h and 1 h and returning to their original positions at 1.5 h is that there are local textures in the samples held for 0.5 h and 1 h, and the cooperative stress accumulation of the preferentially oriented grain clusters induces the directional shift in the lattice parameters. However, at 1.5 h, the grains have no preferred orientation, and the inter-grain stresses cancel each other out, causing the lattice constants to return to the equilibrium state and the diffraction peaks to reset.
When the solution temperature is 1100 °C, the XY plane of the samples held for 0.5 h to 1.5 h is still composed of FCC face-centered cubic γ-austenite. The diffraction peak intensities of the (111) and (220) crystal planes do not change significantly and do not shift, indicating that the grains on the XY plane of the samples do not have preferred orientation under this holding temperature. The YZ plane is the same as that of the sample held at 1050 °C, composed of FCC γ-austenite and BCC body-centered cubic α-ferrite. However, the diffraction peak intensity of α-ferrite is significantly higher than that of the sample held at 1050 °C, and the diffraction peak intensity of the (110) crystal plane of α-ferrite continuously increases with the increase in holding time, indicating that the content of α-ferrite is continuously increasing. The diffraction peaks on the YZ plane do not shift either, indicating that the grains do not have preferred orientation. When the solution temperature is 1150 °C, the XY plane of the sample held for 0.5 h is composed of only FCC γ-austenite, and the diffraction peaks of the (111) and (220) crystal planes do not shift. However, when the holding time is extended to 1 h and 1.5 h, the XY plane is composed of FCC γ-austenite and BCC α-ferrite. The diffraction peaks do not shift when held for 1 h, but shift when held for 1.5 h. The YZ plane is still composed of FCC γ-austenite and BCC α-ferrite, but it is obvious that the diffraction peak intensity of the (110) crystal plane of α-ferrite is further increased compared to 1100 °C. Similarly to the XY plane, the diffraction peaks of the (111) and (220) crystal planes do not shift when held for 0.5 h and 1 h, but shift when held for 1.5 h. The above diffraction peak phenomena indicate that when there is no preferred orientation on both sides for 0.5 h and 1 h, the lattice strain is uniform, resulting in no peak shift. At 1.5 h, the XY plane shows a weak preferred orientation of austenite due to the island-like formation of a small amount of ferrite. While on the YZ plane, the strong texture and the preferred arrangement of ferrite jointly trigger the lattice cooperative strain, causing the diffraction peaks to shift.
Figure 6 shows the IPF maps and phase composition maps of the XY and YZ planes of the samples after solution treatment at 1050 °C for different holding times. It can be seen from the figure that the microstructure of the SLM-formed lightweight steel after solution treatment at 1050 °C shows anisotropy and time dependence.
Figure 6(a
1–a
3,c
1–c
3) shows that the XY plane presents equiaxed γ austenite grains after holding for 0.5 h, 1 h and 1.5 h, and the phase content is FCC and does not change.
Figure 6(b
1–b
3,d
1–d
3) shows that the microstructure and phase composition of the YZ plane change with holding time: after holding for 0.5 h, the microstructure is composed of long columnar grains, with 99.2% FCC and 0.8% BCC; after holding for 1 h, the columnar grain morphology is maintained but the BCC content increases to 2% and the FCC content decreases to 98%; when the holding time is extended to 1.5 h, the columnar grains transform into equiaxed grains, with 96.2% FCC and 3.8% BCC. This phenomenon shows that the evolution of grain morphology and phase composition is strictly limited to the YZ plane, while the XY plane maintains an equiaxed γ single-phase state throughout.
The essence of maintaining 100% FCC in the XY plane of SLM-formed lightweight steel lies in its ultra-high cooling rate and uniform thermal flow history. The B2 phase is completely dissolved within 0.5 h, unable to provide the nucleation barrier for α-ferrite, ultimately achieving the stabilization of the γ-austenite single phase. The increasing BCC content in the YZ plane is driven by the coupling of solidification genetic segregation and diffusion shear: the cooling rate in the YZ plane is slower compared to the XY plane, leading to the formation of Mn/Ni enrichment bands at the columnar grain boundaries. These segregation bands not only hinder the dissolution of the B2 phase but also reduce the local stacking fault energy, triggering the γ→α transformation in the later stage of holding (>1 h). The newly formed α-ferrite and the remaining B2 phase together constitute the total BCC content, and their evolution is strictly controlled by the unique composition-defect gradient field in the YZ plane. When the solution treatment is held for 1.5 h, the transformation of columnar grains to equiaxed grains in the YZ plane is essentially the release of grain boundary migration degrees of freedom driven by thermal activation. The high dislocation density and small-angle grain boundary network inherited from solidification within the columnar grains are reorganized and reduced through the climb mechanism during continuous holding, and the small-angle grain boundaries gradually transform into large-angle grain boundaries. Meanwhile, the undissolved second-phase particles dissolve over time, reducing their pinning effect on the grain boundaries. Eventually, the grain boundaries migrate under the driving force of interfacial energy, achieving the reorganization of the columnar grain structure to equiaxed grains. This morphological transformation has a fundamental impact on anisotropy: the strong orientation texture characteristic of columnar grains is replaced by random crystal orientations, and the continuous second-phase films at the original columnar grain boundaries are broken, significantly weakening the direction-dependent mechanical response of the material [
15]. The formation of equiaxed grains marks the essential transition of anisotropy from geometric scale to near-uniformity, laying the foundation for the engineering application of additively manufactured components.
The experimental results above reveal that when the lightweight steel formed by SLM is solution-treated at 1100 °C (
Figure 7), it enters the sensitive temperature range for the α-BCC ferrite transformation. However, the XY plane, which has a uniform composition fine-grained structure due to ultra-high cooling rate solidification, remains in the γ-FCC metastable state, maintains 99.5% FCC phase and resists ferrite formation within 0.5 to 1.5 h. In contrast, the YZ plane, affected by slow cooling, experiences continuous reverse transformation in the Al-rich regions between intragranular dendrites due to a significant decrease in the actual phase transformation temperature. At 0.5 h, 3.9% BCC ferrite nucleates in the Al-rich microdomains; at 1 h, Al diffusion drives the phase boundary migration, increasing the BCC content to 15.5%; by 1.5 h, the Al-rich regions are depleted, completing the ferrite transformation (31.3%). This indicates that the thermal history differentiation at 1100 °C, through the preset concentration gradient (uniform state in XY vs. steep segregation in YZ), decisively regulates the ferrite phase transformation kinetics path.
Figure 8 shows the IPF and phase composition maps of the 1150 °C solution-treated samples XY and YZ at different holding times. As seen from
Figure 8(a
1–a
3,c
1–c
3), the FCC-austenite content of the XY surface of the sample was 99.5%, 98.1%, and 98.1% after holding for 0.5 h, 1 h, and 1.5 h, respectively, and the corresponding BCC-ferrite content was 0.5%, 1.9%, and 1.9%. However, the FCC-austenite content of the YZ surface changed significantly and non-monotonically with time, being 86.0%, 62.6%, and 83.0% after holding for 0.5 h, 1 h, and 1.5 h, respectively, and the corresponding BCC-ferrite content was 14.0%, 37.4%, and 17.0%.
According to the analysis, the reason for the slight increase in BCC-ferrite content on the XY surface is as follows: when the temperature exceeds the critical inflection point of about 1100 °C determined by the phase diagram, the driving force for the equilibrium precipitation of ferrite at the austenite grain boundaries increases significantly, causing the ferrite content to rise from less than 0.5% at the solution temperature of 1100 °C to 1.9%. This process is independent of element segregation and is a unique thermodynamic equilibrium response at high temperatures. The fundamental reason for the significant difference in phase composition between the XY and YZ surfaces is that the XY surface achieves complete element homogenization due to the interlayer laser remelting, which suppresses the driving force for the reverse transformation of ferrite. In contrast, the YZ surface is controlled by the dendritic segregation during unidirectional solidification, forming a localized [Al]/[Mn] ratio gradient [
16]. This triggers nucleation through short-range Al diffusion, expands the phase transformation through Mn diffusion delay (37.4% at 1 h), and drives the reversion through reverse C diffusion (16.9% at 1.5 h), resulting in an unbalanced oscillation. In summary, it can be seen that when the temperature of SLM-formed lightweight steel exceeds the inflection point of the BCC-ferrite phase diagram, the holding time needs to be simultaneously controlled to suppress the reoccurrence of anisotropy.
3.3. The Evolution of Grain Boundary Second-Phase Precipitation Behavior
In the research on SLM-formed lightweight steel, it is of significant scientific value to focus on the influence of the size/distribution of the second phase at the grain boundary and the morphology of the intragranular precipitates on mechanical properties and anisotropy. In studies on traditional manufacturing methods of lightweight steel, the large and continuous precipitates at the grain boundary (such as κ-carbides or B2 phase) directly lead to low plasticity along a specific direction (such as the Z-direction of SLM-formed steel) and intergranular brittle fracture by inducing local stress concentration and hindering the coordinated movement of dislocations across the grain boundary; while the size gradient distribution and spatial density difference in intragranular nanoscale precipitates (L12 ordered structure) dominate the competition between dislocation cutting through and around, regulate the work hardening behavior and amplify the interlayer mechanical response difference. The combined effect of the two constitutes the essential root cause of the inverted strength–ductility and anisotropy of SLM lightweight steel. The following text explores the different influences of the microstructure at the grain boundary and in the matrix on mechanical properties and anisotropy through the TEM characterization of three solution treatment samples of lightweight steel (1050 °C/1100 °C/1150 °C for 1 h), providing a core theoretical basis for breaking through the toughening and isotropic design of SLM-formed lightweight steel through grain boundary engineering (controlling the size and type of the second phase at the grain boundary) and intragranular microstructure optimization (regulating the spatial distribution of the second phase).
Figure 10 shows the TEM characterization of the grain boundaries in the XY and YZ planes of the lightweight steel formed by SLM after solution treatment at 1050 °C for 1 h. From the dark field images and HAADF in
Figure 10a,b, it can be seen that there are two types of second phases at the grain boundaries in the XY plane of the solution-treated sample at this temperature. EDS mapping shows that one type of second phase has Mn/Al enrichment and can be inferred to be κ-carbides, with an average length of about 300 nm. The other type of second phase has Ni/Al enrichment and can be inferred to be the B2 phase, with an average length of about 70 nm. From the dark field images and HADDF in
Figure 10c,d, it can be seen that there are also two types of second phases in the YZ plane of the sample, and the second phases are larger in size compared to those in the XY plane. Moreover, large-sized (about 400 nm in length) B2 phases precipitate towards the grain interior near the grain boundaries.
To verify the speculation of the existence of two types of second phases, the selected area electron diffraction (SAED) patterns and high-resolution TEM (HRTEM) images of the regions in the XY and YZ planes of the sample that were speculated to be κ-carbides are presented in
Figure 11a–h. On the XY plane of the sample, the SAED pattern clearly detected 1/2{002} superlattice diffraction spots along the [110] zone axis, indicating the presence of an L12-ordered structure. Quantitative analysis of the high-resolution atomic images revealed three sets of measured interplanar spacings: d(0, 0, −1) = 0.344 nm, which is 10.4% smaller than the theoretical value of 0.384 nm for κ-carbides; d(−1, 1, 0) = 0.253 nm, which is 6.8% smaller than the theoretical value of 0.271 nm; and d(1, 0, −2) = 0.169 nm, which is 1.6% smaller than the theoretical value of 0.172 nm. This non-uniform lattice distortion is evident in multiple regions of the inverse FFT image in
Figure 12. This is because in the layered crystal structure of κ-carbides, the {100} family of crystal planes is parallel to the alternating stacking direction of Mn/Al atoms, and their low elastic modulus makes them highly sensitive to vertical thermal stress, resulting in significant compressive strain in this crystal direction. On the YZ plane of the sample, under the [100] zone axis, d(0, 1, −1) = 0.271 nm perfectly matches the theoretical value of the {110} plane of κ-carbides, while d(0, −1, 1) = 0.256 nm is contracted by 5.5% and d(0, 1, 0) = 0.323 nm is contracted by 15.9%. This is because d(0, 1, −1) belongs to the {110} family of crystal planes, and its normal direction has a small angle with the thermal stress direction, with a low shear component, so the lattice parameter remains normal. However, d(0, −1, 1) and d(0, 1, 0) have a larger angle with the thermal stress direction, resulting in a greater shear stress and thus significant lattice contraction. In summary, the unique anisotropic distortion mechanism of κ-carbides is as follows: the {100} planes contract due to sensitivity to vertical thermal stress, and the {110} planes contract due to differences in shear components. This gradient distortion pattern, coupled with the layered elastic modulus of κ-carbides, serves as a basis for distinguishing it from other second phases [
17,
18].
Figure 13a–h presents the selected area electron diffraction (SAED) patterns and high-resolution TEM (HRTEM) images of the regions in the XY and YZ planes of the sample that are predicted to be B2 phase. It can be seen on the XY plane of the sample that under the [111] zone axis, the 1/2{110} superlattice spots confirm the CsCl-type ordered structure. However, d(−1, 0, −1) = 0.221 nm and d(0, 1, −1) = 0.214 nm, both belonging to the {101} crystal plane family, split into two different values. This abnormal splitting of the {101} interplanar spacing is attributed to the lattice shear distortion induced by the atomic size mismatch of Ni/Al in the B2 phase (
Figure 14). This phenomenon never occurs in κ-carbides and serves as a unique thermodynamic basis for distinguishing the B2 phase from the L12 structure. Similarly, on the YZ plane of the sample, under the [111] zone axis, d(0, 1, −1) = 0.204 nm ({101} plane) contracts by 1.0% compared to the theoretical value of 0.206 nm, while d(1, 1, 0) = 0.214 nm ({110} plane) expands by 3.9% compared to the theoretical value of 0.206 nm. This reverse deviation in the interplanar spacing of the same crystal plane (coexistence of contraction of the {101} plane and expansion of the {110} plane) is due to the shear-type lattice distortion induced by the strict ordered occupation of Ni/Al atoms in the B2 structure, resulting in the breaking of cubic symmetry and the generation of opposite strains on the {101} and {110} planes. This behavior once again proves that it is different from the uniform contraction behavior of κ-carbides in the corresponding crystal direction [
19,
20].
Figure 15 shows the TEM characterization of the microstructure at the grain boundaries of the XY and YZ planes of the lightweight steel formed by SLM after solution treatment at 1100 °C for 1 h. From the dark field images and HAADF in
Figure 15a,b, it can be seen that there are still two second phases at the grain boundaries of the XY plane of the sample at this temperature. EDS mapping shows that κ-carbides and B2 phase still exist at the grain boundaries after solution treatment at this temperature, but unlike at 1050 °C, the quantity and size of κ-carbides are significantly reduced, while the size of the B2 phase increases. Similarly, from the dark field images and HADDF in
Figure 15c,d, it can be seen that the quantity and size of κ-carbides at the YZ plane of the sample are reduced compared to those at 1050 °C, and the size of the B2 phase increases. Moreover, no large plate-like B2 phase is found in the grains near the grain boundaries.
Figure 16a–h presents the SAED and HRTEM images of the κ-carbides regions on the XY and YZ planes of the samples. On the XY plane of the sample, three sets of interplanar spacing data were measured along the [−1–10] zone axis: d(0, 0, 1) = 0.365 nm, which is 5% smaller than the theoretical value; d(−1, 1, 1) = 0.221 nm, which is 0.5% smaller than the theoretical value; and d(1, −1, 0) = 0.271 nm, which is 0.4% smaller than the theoretical value. On the YZ plane of the sample, three sets of interplanar spacing data were measured along the [211] zone axis: d(1, 0, −2) = 0.184 nm, which is 7% larger than the theoretical value; d(1, −2, 0) = 0.172 nm, which is in line with the theoretical value; and d(0, −1, 1) = 0.272 nm, which is also in line with the theoretical value. The above distortion data show a smaller distortion compared to that at 1050 °C and a more random distribution. This indicates that the solution treatment at 1100 °C, by altering the directional coupling ability of the κ-carbides layer modulus, transforms the systematic distortion that leads to performance splitting into local fluctuations that do not harm performance, which plays a key role in eliminating anisotropy [
21,
22,
23].
Figure 17a–h presents the SAED and HRTEM images of the B2 phase regions on the XY and YZ planes of the sample. On the XY plane of the sample, the three sets of interplanar spacing data measured along the [111] zone axis are as follows: d(0, −1, 1) = 0.206 nm, which is 1.5% larger than the theoretical value; d(1, 1, 0) = 0.207 nm, which is 2% larger than the theoretical value; and d(1, 0, 1) = 0.205 nm, which is 1% larger than the theoretical value. On the YZ plane of the sample, the three sets of interplanar spacing data measured along the [001] zone axis are as follows: d(1, 1, 0) = 0.213 nm, which is 0.5% larger than the theoretical value; d(0, 2, 0) = 0.152 nm, which is 1.3% larger than the theoretical value; and d(−1, 1, 0) = 0.213 nm, which is 0.5% larger than the theoretical value. It can be seen that the crystallographic parameters of the B2 phase on the XY and YZ planes are highly convergent after solution treatment at 1100 °C. The reason for this might be that the formation of large B2 phase strips eliminates the modulus anisotropy. This phenomenon is consistent with the isotropic transformation of B2 phase and κ-carbides confirmed in the previous text at 1100 °C.
In summary, after solution treatment at 1100 °C, the cooperative evolution of κ-carbides and B2 phase in the grain boundary region plays a decisive role in eliminating anisotropy in SLM-formed lightweight steel. The increase in solution temperature promotes the complete dissolution of undissolved κ-carbides and its reprecipitation as uniform and small nanoparticles, simultaneously driving the B2 phase to form large particles through Ostwald ripening and completely inhibiting intragranular lamellar precipitation. This process eliminates the hereditary effect of thermal stress through a two-stage mechanism [
24]: (1) the homogenization of κ-carbides size blocks the anisotropy of dislocation slip related to the deposition direction; (2) the coarsening of B2 phase eliminates the stress concentration source at the grain boundary, transforming the residual thermal strain energy from long-range ordered accumulation (1050 °C) to short-range random distribution. The cross-scale homogenization of microstructure ultimately leads to strict isotropy in macroscopic mechanical properties, as evidenced by the minimal strength and plasticity deviations on the XY and YZ planes, demonstrating the elimination of deposition direction anisotropy in SLM components.
Figure 18 shows the TEM characterization of the microstructure at the grain boundaries of the lightweight steel formed by SLM after solution treatment at 1150 °C for 1 h on the XY and YZ planes of the sample. From the dark field image and HAADF, it can be seen that there is no second-phase aggregation at the grain boundaries of the XY and YZ planes of the solution-treated sample at this temperature. This is because the solution temperature of 1150 °C exceeds the κ-carbide dissolution temperature and the B2 phase solid solubility line. The rapid migration of the grain boundaries removes the residual solutes, and the sudden drop in the grain boundary energy inhibits the driving force for segregation, completely eliminating the second-phase aggregation at the grain boundaries.
3.4. Evolution of Matrix Microstructure Morphology
Figure 19(a
1–a
4) and
Figure 19(b
1–b
4), respectively, show the TEM microstructure of the intragranular matrix of the XY and YZ planes of the sample after solution treatment at 1050 °C for 1 h. It can be seen from
Figure 19(a
1–a
4) that the XY plane matrix of the sample is composed of γ-austenite matrix and κ-carbides. The dark field image shows that the κ-carbides in the γ-austenite matrix is distributed in a few strips along the <001> direction, and the SAED confirms the coherent relationship of [001]γ//[001]κ. The measured interplanar spacing of the austenite in the high-resolution image is d(−2, 0, 0) = 0.184 nm (theoretical value 0.182 nm, with 1.1% expansion), d(0, 2, 0) = 0.194 nm (theoretical value 0.182 nm, with 6.6% expansion), and d(−2, 2, 0) = 0.131 nm (theoretical value 0.182 nm, with 1.1% expansion). The abnormal expansion of the {020} crystal plane within this plane dominates the strain, confirming that the strip-shaped κ-carbides applies a transverse tensile stress on the XY plane, inducing preferential deformation of the matrix lattice along the [010] crystal direction. It can be seen from the microstructure of the YZ plane matrix shown in
Figure 19(b
1–b
4) that the κ-carbides in the dark field image is still distributed in a strip-like morphology, but the κ-carbide phase spots in the SAED are significantly enhanced. In the high-resolution image, the austenite d(2, 2, 0) = 0.180 nm (theoretical value 0.182 nm, with 1.1% contraction), and the measured κ-carbides d(0, 2, 0) = 0.183 nm (theoretical value 0.271 nm, with 32.5% contraction), while d(1, 0, 0) = 0.367 nm (theoretical value 0.384 nm, with 4.4% contraction). The severe contraction of the {020} κ-carbides and the microshrinkage of the {220}γ phase in this plane reveal that the thermal stress is concentratedly loaded on the κ-carbides along the deposition axis and the compressive strain is transferred to the adjacent austenite {220} plane through the coherent interface. In summary, the differences between the XY and YZ plane matrices confirm that the spatially oriented distribution of the strip-shaped κ-carbides locks the direction of thermal stress transfer, elongating the matrix along the long axis direction and compressing itself along the short axis direction, forming the core mechanism of mechanical anisotropy.
Figure 19(c
1–c
4) and
Figure 19(d
1–d
4), respectively, show the TEM microstructure of the intragranular matrix of samples after solution treatment at 1100 °C for 1 h on the XY and YZ planes. As seen from
Figure 19(c
1–c
4), in the dark field image on the XY plane, the typical microstructure of γ-austenite matrix and κ-carbides is observed, where the κ-carbides present a fine strip-like morphology and is uniformly distributed within the γ grains. SAED under the Z = [001]γ//[001]κ zone axis confirms the coherent relationship of the cubic lattice of the γ/κ two phases. High-resolution measurements show that the d(0, 2, 0) of the γ matrix {020} crystal plane is 0.196 nm (7.7% expansion from the theoretical value), while the d(2, 0, 0) of the κ-carbides {200} plane is 0.184 nm (4.2% contraction from the theoretical value) and the d(0, 1, 0) of the superlattice {010} plane is 0.375 nm (2.3% contraction from the theoretical value), indicating that the γ matrix is under tensile stress while the κ-carbides are under compressive distortion. As seen from
Figure 19(d
1–d
4), in the dark field image on the YZ plane, the κ-carbides present a coarse strip-like morphology, larger than that on the XY plane. SAED under the same Z = [001]γ//[001]κ zone axis verifies the consistency of crystallographic orientation. High-resolution data reveal that the d(0, 2, 0) of the γ matrix {020} plane is 0.184 nm (1.1% contraction from the theoretical value), the d(0, 2, 0) of the κ-carbides {020} plane is 0.189 nm (1.6% contraction from the theoretical value), and the d(1, 0, 0) of the {100} plane is 0.367 nm (4.4% contraction from the theoretical value). Notably, the number of regularly arranged strip-like κ-carbides on the XY and YZ planes after solution treatment at 1100 °C is increased compared to that at 1050 °C.
The bidirectional proliferation of regularly arranged strip-like κ-carbides phases is attributed to the non-equilibrium phase transformation kinetics triggered by the temperature approaching the complete dissolution temperature of κ-carbides at 1100 °C [
25]: the incomplete dissolution of undissolved κ-carbides at high temperature leaves cores as heterogeneous nucleation sites, while the rapid cooling process inhibits the equilibrium precipitation of equiaxed phases, forcing the κ-carbides to selectively epitaxially grow along the γ matrix {100} plane as strips. The interfacial size difference (YZ plane > XY plane) is driven by the residual anisotropy of the thermal stress field during deposition, with the Z-direction tensile stress promoting the preferential growth of κ-carbides along the direction perpendicular to the stress axis. However, despite the direction-dependent morphology of κ-carbides, no significant difference in macroscopic mechanical properties is observed between the XY and YZ planes, and the anisotropy is eliminated. This is because the difference in κ-carbides is at the nanoscale, and their lattice distortions are almost homogenized. Additionally, although the κ-carbides have size differentiation, the face density is approaching, combined with its nanoscale discrete distribution, which enables the thermal strain energy to be randomly dissipated at the nanocluster scale, blocking the formation of long-range ordered strain fields (phase distribution entropy increase effect). Finally, although the size of the κ-carbides is different on the XY and YZ planes, its size is smaller than the critical size for dislocation bowing, and the resistance for dislocation bypassing only depends on particle spacing. The decay length of the distortion field around the κ-carbides is extremely short, preventing the superposition of directional deformation into long-range strain and blocking the transmission of microscopic morphology differences to macroscopic properties.
Figure 19(e
1–e
4) and
Figure 19(f
1–f
4), respectively, show the TEM microstructure of the intragranular matrix of samples after solution treatment at 1150 °C for 1 h in the XY and YZ planes. As seen from
Figure 19(e
1–e
4), κ-carbides can still be observed in the dark field image of the XY plane, but unlike at 1100 °C, they are distributed diffusely. SAED under the Z = [001]γ//[001]κ zone axis confirmed the coherent relationship of the cubic lattice of the γ/κ two phases. High-resolution measurements revealed that the d(0, 2, 0) of the γ matrix {020} plane was 0.189 nm (5.5% expansion from the theoretical value), while the d(0, 1, 0) of the κ-carbides {010} plane was 0.371 nm (1.6% expansion from the theoretical value), and the d(0, 2, 0) of the {020} plane was 0.187 nm (2.4% expansion from the theoretical value). As seen from
Figure 19(f
1–f
4), in the dark field image of the YZ plane, κ-carbides are also distributed diffusely, but their quantity is significantly greater than that in the XY plane. SAED analysis under the Z = [001]γ//[001]κ zone axis shows that the diffraction spots of κ-carbides in the YZ plane are brighter. High-resolution data reveal that the d(1, 0, 0) of the κ-carbides {100} plane is 0.371 nm (1.6% expansion from the theoretical value), and the d(0, 2, 0) of the {020} plane is 0.187 nm (2.2% expansion from the theoretical value). It can be seen that the expansion degree of κ-carbides in the XY and YZ planes after solution treatment at 1150 °C is greater than that at 1100 °C. This is due to the increase in temperature, which leads to more Al atoms being squeezed into the lattice during high-temperature solution treatment, but the lag in bulk diffusion results in an uneven distribution of Al within the grains in a short time, causing more severe local distortion.
From the perspective of macroscopic mechanical properties, although the number of κ-carbides in the XY and YZ planes after solution treatment at 1150 °C is different, anisotropy has not been re-generated. This is because the uniformity of coherent distortion and the purification at the grain boundaries have weakened the anisotropy. After solution treatment at 1150 °C, the tensile strength does not change much compared to 1100 °C, but the plasticity has decreased significantly. This is because the B2 phase at the grain boundaries is completely dissolved at 1150 °C, irreversibly losing the pinning inhibition ability of the B2 phase on grain boundary migration and the micro-region stress buffering function. At the same time, the intragranular κ-carbides have changed from the regular strip-like arrangement at 1100 °C to a diffuse distribution, forcing the dislocation cutting mechanism to dominate the plasticity process, inducing the early nucleation of microvoids and accelerated crack propagation, ultimately resulting in a decrease in tensile elongation compared to the peak state at 1100 °C. The essence of this plasticity degradation is the combined effect of the failure of the grain boundary constraint mechanism and the hardening of the intragranular deformation mode [
26,
27,
28].