100–160 µm | 63–100 µm | <63 µm |
28 | 29 | 43 |
Cite this article as: | Hamid Sazegaran, and Seyyed Mohsen Moosavi Nezhad, Cell morphology, porosity, microstructure and mechanical properties of porous Fe–C–P alloys, Int. J. Miner. Metall. Mater., 28(2021), No. 2, pp.257-265. https://dx.doi.org/10.1007/s12613-020-1995-2 |
Open cell steel foams were successfully fabricated through the powder metallurgy route using urea granules as the water leachable space holder in the present study. The influence of different amounts of phosphorus (0, 0.5wt%, 1wt%, 2wt%, and 4wt%) was investigated on the cell morphology, porosity, microstructure of cell walls, and mechanical properties of steel foams. The cell morphology and microstructure of the cell walls were evaluated using an optical microscope equipped with image processing software and a scanning electron microscope equipped with an energy dispersive X-ray spectrometer. In addition, the compression tests were conducted on the steel foams using a universal testing machine. Based on microscopic images, the porous structure consists of spherical cells and irregularly shaped pores that are distributed in the cell walls. The results indicated that by increasing the phosphorus content, the porosity increases from 71.9% to 83.2%. The partially distributed ferrite and fine pearlite was observed in the microstructure of the cell walls, and α-Fe and Fe3P eutectic extended between the boundaries of agglomerated iron particles. Furthermore, elastic and long saw-toothed plateau regions were observed before fracture in the compressional stress–strain curves. According to the results, by increasing the phosphorus content from 0 to 4wt%, the plateau region of the stress–strain curves shifts to the right and upward. Therefore, increasing phosphorus content causes improvement in the mechanical properties of steel foams.
Metallic foams or cellular metals (also known as highly porous metals), as a neoteric advanced class of engineering materials, have irreplaceable properties, such as low density, high strength-to-weight ratio, good specific stiffness and compressional strength combined with excellent energy absorbing properties, unique thermal and acoustical specifications, large surface area, high permeability, and other good physical and mechanical properties [1–3]. Consequently, these porous materials have been successfully used in fabrication of many parts in various industries [3–6]. Metallic foams are used in parts requiring load-bearing features [2–3], weight-saving components [3,7], impact-energy absorbers and crush protectors [8–11], sandwich panels [12–13], sound and microwave absorbers [14], heat exchangers [15–16], full cells [17], catalysts [18], filtration [19], and medical applications [20–21].
It is known that the cell morphology (open or close cell, cell shape, size, and distribution) has an effect on the behavior and performance of metallic foams. Cell morphology is strongly dependent on the manufacturing process, [3,22–23]. In recent years, numerous manufacturing processes have been successfully developed for the fabrication of the metallic foams. Two primary methods include fusion and powder metallurgy [3,5,22]. The fusion metallurgy is rarely used in the fabrication of steel foams because of the high liquidus temperature and other challenges in melting, solidification, and casting of ferrous alloys. Alternatively, powder metallurgy is cost effective and leads to the formation of a desirable cell morphology [24–25]. Among the various powder metallurgy methods, the newly developed space holder technique can fabricate steel foams with the uniform size, shape, and distribution of cells [26–28].
In this technique, salt particles [26,29–31], carbamide and urea granules [32–36], sucrose [37], tapioca starch [38], magnesium [39–40], expanded polystyrene beads [41–42] are used as appropriate space holder materials. Steel foams are a category of metallic foam that can be used in many structural and non-structural applications because of the irreplaceable properties of steels and cellular structures. The effects of cell morphology [33], process temperature [43–44], boron content and aging condition [45–46], and Ce/Cr coating on the mechanical properties [47], and the influence of Al content on oxidation resistance [25] were recently investigated in steel foams. Despite the many studies on the manufacturing techniques of the steel foams, few studies have focused on the effects of alloying elements on the properties, behavior, and performance of steel foams [24–25,48]. In this work, steel foams were fabricated through the powder metallurgy route using urea granules as a leachable space holder. The effects of phosphorus (as liquid phase sintering agent) content on the cell morphology, porosity, microstructure of cell walls, and mechanical properties of open cell Fe–C–P foams were investigated.
Commercial water atomized iron powder (purity > 99.9%, Khorasan Powder Metallurgy Co.), ferrophosphorus powder (13.5wt% P, Khorasan Powder Metallurgy Co.), and ultrafine graphite powder (particle size < 20 µm, purity > 99.99%, ash content < 0.01wt%, Merck) were applied as initial powder materials. Different amounts of ferrophosphorus powder were added into the powder mixture to investigate their effects on the bond formation between the iron particles in the liquid phase sintering (LPS) process. The size distribution of the iron particles is presented in Table 1. Typical morphologies of iron and ferrophosphorus particles are shown in Fig. 1. The majority of the iron particles have a rounded irregular shape (Fig. 1(a)) and have a size between 45 and 160 µm. In addition, the ferrophosphorus particles consist of two types: (1) rounded irregular particles of size less than 10 µm; (2) angular particles of size greater than 10 µm.
100–160 µm | 63–100 µm | <63 µm |
28 | 29 | 43 |
To prepare the powder mixture, the masses of raw powder materials were measured using a digital balance (accuracy 1 mg) and mixed according to predetermined mass fractions. The iron powder with 0.6wt% of carbon powder, and 0 (as a reference specimen), 3.70wt%, 7.40wt%, 14.81wt%, and 29.63wt% of ferrophosphorus powders were mixed into a blending machine (15.7 rad·s−1 and 30 min) until achieving the complete uniformity. Spherical urea granules (size: 1.2–1.5 mm, sphericity: 0.95, purity > 99.5%) were selected as the water leachable space holder materials because of their very high solubility in distilled water (Fig. 2(a)).
Fabrication of the open cell steel foams with uniform morphology of the cells was performed using the following procedure. Firstly, the spherical urea granules (49wt%) were fully coated by the prepared powder mixtures (49wt%) using a mixing machine (15.7 rad·s−1 for 1 min). To wet the surfaces of urea granules, 2wt% of distilled water was entered into the chamber of mixer before adding the powder mixture. This process results in the coating of powder particles onto the sticky surfaces of urea granules. The uncoated and coated urea granules were illustrated in Fig. 2. After the drying process (75°C for 5 h), the coated urea granules were uniaxially compacted at 150 MPa [25,49] in a cylindrical stainless steel die (d = 12 mm and h = 100 mm). Therefore, green specimens were fabricated in the compaction process in which neighboring iron particles hold together through cold weld process. The compacted specimens are shown in Fig. 3(a).
The green specimens were submerged in the distilled water at 25°C for 1 min to leach out the urea granules. The drying process was followed by 5 h heating at 75°C. These processes are continuously repeated 8 times to complete removal of urea granules. To investigate the removal rate of the urea granules, the weights of the specimens were measured after each leaching stage. The removal rate of the urea granules R was calculated as follows:
R=(W0−WiWu)×100% |
(1) |
where
Next, the leached specimens were sintered in a continuous furnace at 1120°C for 52 min under cracked ammonia atmosphere. At the beginning of the sintering cycle, thermal pyrolysis causes the residual urea to evaporate from the cells of the steel foams. After finishing the sintering process, the specimens were cooled to room temperature in the furnace (Fig. 3(b)).
The weight and the volume of the foam specimens were accurately measured using a digital balance and dimensional calculations, respectively. The density of foams was obtained by dividing the weight of the foams into its volume. The porosity of the steel foams can be determined using the following equation:
P=[1−(ρFρS)]×100% |
(2) |
where
Each of the microscopic specimens were cut from the sintered foams using a wire-cut machine (Dk7732ZAC) and mounted, grinded, and polished. An optical microscope (OM) equipped with microstructural image processing software (MIPTM) and a scanning electron microscope (SEM, LEO 1450VP) equipped with an energy dispersive X-ray spectrometer (EDS) were applied to study the cell morphology and microstructure of the cell walls.
The effect of the phosphorus content on the mechanical properties of steel foams were investigated via the compression test using a displacement-controlled universal testing machine (Zwick Z250) at a cross-head speed of 0.1 mm/min. Compression tests were performed on foam specimens cut from sintered steel foams (d = 12 mm and h = 18 mm) using a wire-cut machine (Dk7732ZAC). At least three specimens of each type of steel foam were mechanically tested.
The removal rate of the urea granules calculated using Eq. (1) is shown in Fig. 4. It is found that variation in the phosphorus content does not have a significant effect on the removal rate. The removal rate of the urea granules is very high up to stage 3 (approximately 65wt% in this stage). In these stages, because of the very high amount of the urea granules in the green specimens, the distilled water significantly contacted with the surfaces of the urea granules and the leaching process was rapidly performed. In the next stages, the decreasing amount of remaining urea granules and the slow flow of water through the formed narrow channel between the cell wall cause the removal rate to decrease [49]. After stage 8, the remaining urea granules of approximately 10% is removed via thermal pyrolysis in the following sintering cycle. Similar results were previously reported on the removal of carbamide as a leachable space holder [45–46,49–50].
It is known that the cell and pore morphologies significantly affect the physical and mechanical properties of metallic foams [1–3]. The size, shape, and distribution of the space holder, the ratio of the space holder to the cell wall ingredient, the removal method of the space holder, and the applied pressure in the compaction operation are affective parameters on the cell and pore morphologies [48–49]. The OM and SEM images of the cells and the cell walls of steel foam containing 2wt% P are shown in Fig. 5. The cells are found to have spherical shape and are uniformly distributed between the cell walls. It is concluded that urea granules were replaced by the cells. Because of the low applied pressure, the urea granules do not deform during the compaction operation, and therefore, the shape and size of the cells are exactly proportional to the shape and size of the urea granules [25]. The internal holes of the cells are known as interconnections because of their function in binding cells. Examples of interconnections are illustrated in Fig. 5(b). These interconnections create internal channels between the cell walls and increase the removal rate of the urea granules. The thickness of the cell walls and the surface fraction of the cells measured using image processing software are approximately 187.3 µm and 0.743, respectively. Note that the addition of phosphorus does not considerably change the thickness of the cell walls and the surface fraction of the cells.
An SEM image of the cell walls of steel foam containing 1wt% P is shown in Fig. 6. Very small pores with irregular shapes are observed in the cell walls. The formation of these isolated pores is probably related to the low applied pressure in the compaction operation to prevent the fracture of urea granules [49–51]. Fig. 7 illustrates the effect of phosphorous content on the surface fraction of the pores. It is found that the surface fraction of the pores decreases with increasing phosphorus content. Eutectic phase transformation in the sintering temperature (1120°C) causes formation of α-Fe and Fe3P phases in the microstructure of cell walls [52–53]. The α-Fe and Fe3P eutectic melts locally at 1048°C and penetrates into the pores between the iron particles, causing LPS. In the sintering cycle, the creation of molten α-Fe and Fe3P eutectic leads to initiation and growth of the narrow necks at contact regions between the iron particles. These narrow necks act as a binder and improve agglomeration of the iron particles. In the steel foams with higher phosphorus content, more α-Fe and Fe3P eutectic is formed that consequently fills the pores between the cell walls and reduces the surface fraction of the pores.
The porosity is one of the important factors affecting the mechanical properties of metallic foams [1–3]. The influence of the phosphorus content on the porosity of the steel foams is shown in Fig. 8. The porosity of steel foams is increased with increasing phosphorus content. Increasing the phosphorus content enhances the diffusion of phosphorus and iron and the activation of LPS. In the steel foams containing phosphorus, higher diffusion rate, and rapid LPS processes cause the cell walls to swell and the cell wall density to increase. The total porosity of steel foams have previously been shown to consist of the amounts of cells formed by the removal of the urea granules and the amounts of pores remaining between the cell walls [49,51]. Although the addition of phosphorus has an insignificant effect on the surface fraction of the cells and reduces the surface fraction of the pores because of the activation of the LPS, very low phosphorus density (1.82 g/cm3) compared to the iron density (7.87 g/cm3) decreases the density of steel foam and, as a result, increases the porosity. The porosity of the steel foams containing copper and chromium reported in the literature is in the range of 72.5%–77% and 74%–75.5%, respectively [51,54]. The low porosity of steel foams containing copper and chromium compared to steel foams containing phosphorous refers to the difference in the copper and chromium density compared to the phosphorus density.
The microstructure of the cell walls of the steel foams fabricated through the leachable space holder-powder metallurgy technique is powerfully dependent upon the chemical composition of the pre-mixed and pre-alloyed powders [24,44] and heat treatment procedure [43]. The SEM image of the cell wall of the steel foam with zero phosphorus content is shown in Fig. 9. The agglomerated iron particles and created boundaries between the iron particles are clearly observed. Fig. 10 shows the microstructures of the cell walls of specimens containing different amounts of phosphorus. Partially distributed ferrite, fine pearlite, and α-Fe and Fe3P eutectic are the main phases in the microstructure of the cell walls of these specimens. The phase fraction of the cell walls is dependent on the phosphorus content. During the heat treating process (1120°C, and 52 min), carbon (0.6wt%) diffuses into the iron particles and forms iron carbide, resulting in alternating pearlite layers [55–56].
Ferrophosphorus powder distributed among the iron particles forms the molten α-Fe and Fe3P eutectic [52–53]. The molten α-Fe and Fe3P eutectic seeps into the pores between the agglomerated iron particles via capillary action. SEM image and EDS results of α-Fe and Fe3P regions are shown in Fig. 11. It is observed that the eutectic microstructure consists of two distinct regions. The lighter region having less phosphorus content is α-Fe (Fig. 11(b)), and the darker region having more phosphorus content is Fe3P (Fig. 11(c)). In the steel foams containing lower amounts of phosphorus (containing 0.5wt% and 1wt% P), the α-Fe and Fe3P eutectic often forms at the intersection of the boundaries, and when the phosphorus content increases (in the steel foams containing 2wt% and 4wt% P), the α-Fe and Fe3P eutectic is observed in all regions of the boundaries. Penetration of the eutectic liquid between the agglomerated iron particles increases with increasing phosphorus content. Therefore, the narrow necks become thicker. As shown in Fig. 10, the surface fraction of α-Fe and Fe3P eutectic increases with increasing phosphorus content (Fig. 12). Based on quantitative metallography results, the surface fractions of the eutectic phase in the specimens containing 0.5wt%, 1wt%, 2wt%, and 4wt% of phosphorous were found to be 3.8%, 7.1%, 13.3%, and 21.7%, respectively.
The engineering stress vs. strain curves of the studied steel foams are plotted in Fig. 13. The stress vs. strain curves consist of the elastic region, the saw-toothed plateau region, and the fracture point. Compressive loading causes reversible deformation of the cell walls in the elastic region and yielding of the steel foams. With increasing phosphorus content, the modulus of elasticity (slope of the linear portion of the stress vs. strain curve) and the yield strength increase. Therefore, it can be concluded that the capacity of recoverable absorbed energy increases with increasing phosphorous content. In the steel foam containing 4wt% P, an individual step is revealed in the elastic region that is probably related to the partial collapse of a row of cells when the cell walls deformed elastically.
In the saw-toothed plateau regions, valleys and peaks of the stress are observed with increasing strain. In a valley, serious collapse occurs in a distinct row of cells, followed by resistance of the applied load by the cell walls resist, resulting in a sharp peak of the stress [43–44]. It is found that the number of stress vs. strain fluctuations and the height of the peaks decrease with increasing phosphorus content. As previously mentioned, a higher phosphorus content leads to formation of a higher liquid phase during the sintering cycle and, consequently, improves the bonding of the iron particles. Thus, serious collapse in a row of cells occurs less frequently and the stress vs. strain fluctuations and the height of the peaks are reduced. By increasing the phosphorus content, the plateau region of the curves shifts upwards and right, resulting in improved compressive properties. As reported in other research studies, with increasing copper content acting as a LPS agent, the compressive properties of the steel foams improve [51].
The effect of phosphorus on the cell morphology, porosity, microstructure, and mechanical properties of open cell Fe–C–P steel foams fabricated through the leachable space holder-powder metallurgy technique was investigated in this work. From the experimental results, the following observations were obtained.
(1) During eight leaching stages, approximately 90% of urea granules are resolved.
(2) The thickness of the cell walls and the surface fraction of the cells are independent of the phosphorous amounts of steel foams. The thickness and the fraction were measured to be 187.3 µm and 0.743, respectively.
(3) When the phosphorus content increases, the surface fraction of the pores remaining between the cell walls decreases from 0.313 to 0.283. The porosity of the steel foam is the sum of the cells created by the leaching of urea granules and the pores remained between the cell walls; this parameter increases by 15.7% with phosphorus content increasing from 0 to 4wt%.
(4) The main phases observed in the microstructure of the cell walls consist of partially distributed ferrite, fine perlite, and α-Fe and Fe3P eutectic. The surface fraction of the α-Fe and Fe3P eutectic increases with increasing phosphorus content.
(5) The compressive strain vs. stress curves includes the elastic region, the saw-toothed plateau region, and the fracture point. Increasing the phosphorus content improves the elastic behavior of the steel foams and moves the plateau region upwards and right.
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