3.2. Microstructure evolution
Figure 9 illustrates the phase analysis outcomes. The structure after centrifugal casting is characterised by good homogeneity (
Figure 10). The copper-enriched α-phase grains have an elongated shape (50–60 µm), which is characteristic of dendritic structures obtained by casting. The iron does not dissolve in copper and forms the intermetallic compound Fe
3Al with aluminium (
Figure 9). The Fe
3Al is deposited into the copper solid solution in the form of dispersed and larger coagulated precipitates. The γ’- and β-phases are located between the α-phase grains and are observed as eutectoid zones
and acicular crystals obtained by a diffusionless (martensite-like) transformation
. The martensitic transformation in centrifugal casting is due to the rapid cooling, a characteristic of casting nonferrous alloys into metal moulds. The quantity of
-phase (Cu
3Al) and γ-phase (Cu
9Al
4) is significantly less than the underlying α-solid solution (
Figure 9).
After quenching at 920°C in water and subsequent ageing at 20°C, a coarse-grained structure is formed (
Figure 11). Dispersed martensitic-type needles are observed at the grain boundaries because of the diffusionless transformation
. Dispersed zones of eutectoid breakdown
are observed between the needles. The iron partially dissolves in the β-phase and separates as the intermetallic compound Fe
3Al in a dispersed form.
After ageing at 200°C, an increase in acicular
-grains is observed in terms of size and quantity (
Figure 12) due to the inverse transformation
(
Figure 9) due to temperature-accelerated diffusion. The β-phase is the hardest phase of all registered phases in
Figure 9: thus, the hardness as an integral mechanical characteristic of the studied bronze is significantly increased (see
Figure 6c). A mechanical mixture of copper-enriched α-grains and the intermetallic compound Fe
3Al is formed between the acicular β-grains. No formed α-grain boundaries are observed.
As the ageing temperature increases to 300°C, the diffusion increases, causing the partial disintegration of acicular
-grains:
(
Figure 13). As a consequence of the coagulation of a dispersed phase of Fe
3Al, relatively large grains of this intermetallic compound are observed.
After ageing at 400°C, grains are observed whose boundaries represent stripe-shaped α-subgrains, marked with a dashed green line in
Figure 14. A partial tearing of the borders is noticeable in places. Temperature-induced diffusion accelerates the nucleation of the α-solid solution network and the transformation
. In the rest of the
-grains, the dissolved iron is separated in the form of dispersed particles of Fe
3Al.
Figure 15 presents the structure after ageing at 500°C. The process of phase separation
is finished. No metastable phases were found (
Figure 9). Precipitated dispersed particles of Fe
3Al are observed in the grains of the α-solid solution. The refinement of the stripe-like α-grains is observed because of diffusion processes, The established maximum tensile strength (see
Table 5) is a consequence of the homogeneous and refined structure and dispersed particles of Fe
3Al.
Figure 16 displays the structure of bronze subjected to ageing at 600°C (i.e., the heating is above the eutectoid line of 565°C; see the static diagram in
Figure 3). In this region, the α-phase,
-phase and
are in equilibrium. All three phases are stable below the eutectoid line. Unlike the static diagram, the heating region also contains a β-phase due to an initially quenched structure (see position 2 in
Figure 9). The metastable
-phase is formed during air cooling, a consequence of the partial martensitic transformation
, and part of the grains undergo diffusion decay
. At this ageing temperature, zones form with lamellar α-subgrains (outlined with a white line).
When the ageing temperature is 700°C, conditions are created for grouping and subsequent coagulation of the coopper-enriched α-phase (
Figure 17). The mechanism of clustering and growth of equiaxed α-grains is likely similar to the process occurring at lower temperature (see
Figure 16). Higher temperatures accelerate the diffusion processes and cause larger grains to enlarge at the expense of smaller grains. Thus, the resulting structure is inhomogeneous with the formed zones of the coarse-grained α-phase and enclosed zones containing a mechanical mixture of partial martensitic and diffusion transformations
. The partial martensitic transformation is due to the higher cooling rate in the air. The β-phase increases its degree of homogeneity (respectively expanding its solubility region) when the heating temperature increases. A study [
9] found that the β-phase partially dissolves iron atoms. This reason may be why no Fe
3Al peak is observed in the X-ray pattern in
Figure 9.
3.3. Effect of heat treatment on mechanical characteristics: planned experiment and optimization
According to the one-factor-at-a-time experimental results, the governing factors were chosen to change as follows:
and
.
Table 2 lists the governing factor levels. The correlation between natural
and coded
coordinates is
where
,
and
are the upper, middle, and lower levels of the
ith factor in natural coordinates, respectively.
The objective functions are the following mechanical characteristics: yield limit (
), tensile strength (
), elongation (
), hardness (
) and impact toughness (
).
Figure 18 provides the experimental points in the plane of governing factors.
Table 3 lists the experimental outcomes for the chosen mechanical characteristics.
An analysis of variance (ANOVA) was conducted via QStatLab [
10] to investigate the significance of the governing factors.
Figure 19 provides the main ANOVA effects. For all objective functions, the more significant factor is
(temperature). Time has the most substantial influence on the tensile strength. The yield limit (
Figure 19a) is maximum when the temperature is at the middle level and the time is at the second level (
). The combination of maximum temperature and time at the middle level minimises the yield limit. The influence of the governing factors on the tensile strength is similar (
Figure 19b). When the temperature and time simultaneously occupy the fourth level
, the elongation is maximal (
Figure 19c). The combination of the minimum time and temperature at the second level (
) minimises the elongation. When the temperature is at the second level
and the time is at the fourth level
, the hardness is maximum (
Figure 19d). The minimum hardness is obtained when the temperature is maximum and the time is at the middle level
. The influence of the governing factors on the impact toughness is analogous to their influence on the elongation (
Figure 19e). The ANOVA predicts the influence of the governing factors only in a qualitative aspect. More accurate results are obtained after mathematically modelling the studied mechanical characteristics.
The experimental results for the mechanical characteristics were subjected to regression analyses. The significance of the regression coefficients was determined at the
. Given the chosen experimental design (five levels for each factor), the approximating polynomials may be of degree 4 or lower:
where
denotes the vector of the governing factors,
represents the number of governing factors, and
indicates the number of objective functions.
The regression analyses were performed using QStatLab [
10], and
Table 4 presents the regression coefficients. The magnitude (absolute value) of the coefficients in front of the dimensionless variables indicates the significance of the corresponding governing factor (variable), and the absolute value of the coefficients in front of the products of the variables indicates the significance of the interaction between the governing factors. The regression coefficients in
Table 4 indicates that: 1) the ageing temperature is a much more significant factor than the ageing time, confirming the ANOVA results, and 2) the interaction between the governing factors is relatively weak, with the exception of the tensile strength.
Table 3 presents the values of the objective functions calculated using Eq. (2) for the experimental points from the plan. The comparison between the experimental results for the objective functions and those predicted by the models (at the experimental points) displays excellent agreement.
Figure 20 presents a graphical visualisation of the models. The type of surfaces confirms that the ageing temperature is the more significant of the two factors. The ageing time influences the tensile strength most strongly (confirming the ANOVA results), whereas the influence is weakly expressed for the other characteristics. The factor least sensitive to the ageing time is the impact toughness.
The two primary characteristics of static strength (yield limit and tensile strength) similarly depend on the temperature. As the temperature increases, the static strength increases and reaches its maximum value between 400°C and 500°C, after which it begins to decrease at a faster rate. The behaviour of hardness is similar, but it reaches its maximum values earlier (in the interval between 250°C and 300°C) and then decreases to a minimum. The elongation and the dynamic strength (impact toughness) display similar behaviour under temperature and time changes because both characteristics have a common physical basis. The behaviour of the dynamic strength when changing the temperature is opposite that of the static strength. The maximum values of all objective functions,
, and their corresponding magnitudes of the governing factors,
, were found with QStatLab using the random search method with 1,000 iterations.
Table 5 lists the results.
Table 5.
Maximum values of the objective functions and the corresponding governing factors.
Table 5.
Maximum values of the objective functions and the corresponding governing factors.
Objective fun ctions |
Governing factors |
|
Codded |
Natural |
|
-0.19582 0.98008 |
|
431.8 |
|
0.33077 -0.99671 |
|
812.9 |
|
0.75517 0.41485 |
|
14.6 |
|
-0.68099 0.39878 |
|
261.8 |
|
0.78857 0.00032 |
|
73.65 |
The correlations between the five objective functions were found by eliminating the governing factors for the pair of considered objective functions. These correlations are essential for setting and solving optimisation problems and for correctly defining the functional constraints. The correlations of the hardness with each of the other four mechanical characteristics were determined.
Figure 21 graphically visualises the data. The dependencies of the mechanical characteristics on the hardness are nonlinear. As the hardness increases, the static strength increases up to a specific hardness value (approximately 230 HB for the yield limit and 210 HB for the tensile strength), and subsequently decreases. The elongation and dynamic strength trendlines indicates a continuous decrease when the hardness increases.
Four optimization tasks, which have the most significant importance for practice, were formulated and solved:
- 1)
Maximum plasticity: ;
- 2)
Maximum impact toughness (dynamic strength): ;
- 3)
-
Simultaneous high hardness and static strength: The objective function vector is
,
where
, and
is the plane of the governing factors
. The objective functions must tend to their maximum values:
,
, and
. Based on
Figure 21, the following are the functional limitations:
,
, and
.
- 4)
-
Simultaneously high hardness, static and dynamic strength: The objective function vector is
.
The objective functions must tend to their maximum values:
,
,
, and
. The following are functional limitations, according to
Figure 21:
,
,
, and
.
The first two single-objective optimisation tasks require determining the largest value of the corresponding function without functional limitations and satisfying the governing factor limitations (
Table 2).
Table 5 lists their solution. The last two are multiobjective optimisation problems. The vector
must be determined so that the objective function magnitudes
to satisfy the conditions of the corresponding multi-objective optimisation task, and
,
, and
are the compromised optimal values of the governing factors. The defined multiobjective optimisation tasks were solved by searching for the Pareto-optimal solution approach. The decision was made through the nondominated sorting genetic algorithm (NSGA-II) [
11] using QstatLab. A Pareto front offering 50 compromised optimal solutions was obtained for each of the two tasks.
Figure 22 and
Figure 23 illustrate the Pareto front for the third and fourth optimisation problems. A compromised optimal solution is selected from each Pareto front.
Table 6 contains detailed information regarding the solution results for the four optimisation tasks.
The results of the optimizations were experimentally verified. For this purpose, additional samples were manufactured for tensile and impact toughness tests, which were hardened at 920°C in water and subjected to subsequent ageing with the optimal values (
Table 6) of the governing factors for the respective optimisation task. The hardness was measured on the impact toughness samples. Each experimental result was obtained as the arithmetic mean of three samples.
Table 7 presents the results. The comparison with the theoretical optimisation results displays good agreement.