A New Atomized Low Apparent Density “Sponge Like” Iron Powder Francis Hanejko & Howard Rutz Hoeganaes Corporation Cinnaminson, NJ 08077 USA Abstract: The development of an atomized “sponge like” iron powder has been undertaken. The goal of this program was to provide a cost effective atomized powder with high green strength and similar apparent density to existing sponge iron grades. Additional design criteria for the new powder were to match the dimensional change and strength found in sponge powders. New atomizing techniques were utilized to provide a highly irregular powder surface that allows the various design requirements to be met. The successful results of this program will be documented. Introduction: The sponge iron powder process or more precisely the solid-state reduction was the earliest technique to produce metallic iron. Dating back to 6000 BC, this methodology was used primarily to produce weapons. [1] Sponge iron powder was the first commercially mass produced iron powder for PM parts and was successfully used in applications such as self-lubricating bearings, shock absorber pistons and guide rods, friction materials, etc. Alternative uses of iron powder relied on its high specific surface area; these applications included catalysts and hand warmers for prolonged low temperature heating. The process can be summarized as the mining of iron ore, grinding and beneficiating the ore to the proper purity and particle size, reduction via a carbon source at temperatures below the melting point of iron, grinding the agglomerated sticks, followed by annealing and shipment to the customer. Figure 1 presents a schematic illustration of the current sponge process. Typical time spent in the kiln was on the order of 60 / 70 hours with a maximum temperature of ~1200 °C. Despite the advantages of sponge iron (predominantly green strength at low part densities), disadvantages of the process are as follows: Need for high purity iron ore with minimal impurities. Magnetite ore (Fe3O4) is the most common raw material. Impurities such as silicon or titanium oxides negatively affect the overall quality of the finished sponge iron for PM applications. Relatively long processing time to produce the material. The average time in the kiln approaches three days coupled with necessary preparatory and post reduction processing. Internal studies conducted at Hoeganaes Corporation showed an ~30% energy savings in the manufacture of atomized powders compared with the traditional sponge powders. [2] An inability to achieve high density because of the porous nature of the powder produced coupled with low apparent density that results in a greater die fill height. Figure 1: Schematic of Sponge Iron Process To offset these disadvantages, Hoeganaes Corporation initiated a laboratory / production research program targeting the production of a “sponge-like” powder via the melting and atomization process. Selected ferrous scrap is melted in an electric arc furnace, in less than 90 minutes a liquid bath is created that is subsequently water atomized into powder. Electric arc melting of iron enables refining of the liquid metal, producing powder with reduced amounts of residual oxides. [3] Following atomization, dewatering and drying, the powder is annealed, packaged and shipped; often in less than 3 total days from the start of the process. Key considerations in producing a “sponge-like” powder via atomization are the atomization parameters and subsequent particle size of the as-atomized powder. Exact processing details are proprietary; however, a finer as-atomized particle size combined with agglomeration during annealing is a requirement to produce an atomized material with reduced apparent density and improved green strength. Shown in Figure 2 are representative SEM photomicrographs of traditional sponge iron powders, atomized powders, and lastly atomized “sponge like” iron powders. Note the similar appearance of the traditional sponge iron powder and the atomized sponge powder. Both possess internal powder porosity and surface irregularity greater than conventionally water atomized powder. A: Traditional sponge powder from iron ore Figure 2: B: Atomized iron powder C: Atomized sponge iron powder SEM photomicrographs of traditional sponge iron, atomized material, and atomized sponge powder Key powder characteristics of traditional sponge iron powders and atomized low apparent density powder are presented in Table 1. Note the lower hydrogen loss and silicon content of the atomized powder. Apparent density and Hall flow rates of the two materials are similar. The manganese content in the traditional sponge iron powders is predominantly in the form of manganese oxide. Whereas, the manganese in the atomized material acts as a beneficial alloying element. Table 1 Powder Characteristics of Traditional Sponge vs. Atomized Low AD Property Apparent Density, g/cm³ Flow, s/50 g H2 Loss Silicon Content, % Sulfur, % Manganese, % Traditional Sponge Iron 2.50 Rolled Sponge Iron 2.60 Atomized “SpongeLike” Powder 2.60 30 0.26 0.20 0.01 0.10 30 0.26 0.20 0.01 0.10 28 0.15 0.02 0.015 0.15 Review of Selected Premixes Using Traditional Sponge vs. Atomized Low Apparent Density Iron Powder Six laboratory premixes were prepared using the newly developed atomized “sponge like” iron powder and two traditional sponge iron powders. The premix compositions are listed in Table 2. From these six premixes compressibility information, green strength, sintered strength (via transverse rupture strength), and sintered hardness data were developed. Compaction was performed without die heating and sintering was done at 1120 °C in a belt furnace for 20 minutes at temperature using a 90% nitrogen / 10% hydrogen atmosphere with a cooling rate of ~0.6 °C per minute. Table 2 Premix Compositions of Mixes Evaluated All with 0.75% Acrawax Mix ID 1 2 3 4 5 6 Iron Powder Atomized low AD powder Traditional Sponge Rolled Sponge Atomized low AD powder Traditional Sponge Rolled Sponge % Copper 1.5 % Graphite 0.7 1.5 1.5 1.5 0.7 0.7 0.3 1.5 1.5 0.3 0.3 Compressibility data for the 0.7% graphite containing premixes are shown in Figure 3 (compressibility data developed for the 0.3% graphite containing premixes demonstrated a trend similar to the data shown in Figure 3). The atomized “sponge like” iron material has higher compressibility relative to the two traditional sponge iron materials. This higher compressibility results from the liquid metal refining minimizing impurities thus producing a more compressible material. Significance of this data is that parts can be compacted at lower compacting pressures on potentially smaller compaction presses (at potentially faster press rates). Figure 3: Compressibility Data of 0.7% Graphite Containing Premixes Shown in Figure 4 is the green strength comparison of the three premixes with 0.7% added graphite. The traditional sponge material does exhibit higher green strength relative to the atomized grade. Alternatives to increasing the green strength of the atomized material include the use of alternative lubricants. Laboratory testing of an irongraphite-lubricant premix at 6.1 g/cm³ density using both the atomized low AD material and traditional sponge showed green strengths of 12.0 MPa and 12.8 MPa, respectively. The atomized sponge used a proprietary high green strength lubricant and the traditional sponge utilized Kenolube as the powder lubricant. Apparent density and powder flow rates were unaffected and the advantage of a lower compaction pressure was maintained. Thus through innovative lubricants, potential issues relating to lower green strength can be overcome. Figure 4: Green Strength of 0.7% Graphite Containing Premixes A: DC vs. Green Density for 0.7% added graphite containing premixes Figure 5: B: DC vs. Green Density for 0.3% graphite containing premixes Plots of DC. Vs. Green Density for Two Graphite Levels Shown in Figure 5 are the sintered dimensional change data developed for the six premixes. For higher carbon materials (0.7% added graphite), the atomized material has identical dimensional change to the two traditional sponge grades evaluated. At lower added graphite contents, the atomized grade exhibits more positive sintered dimensional change. Additions of a prealloyed carbon steel powder to the atomized sponge lowers the dimensional change to levels comparable with traditional sponge with minimal loss in compressibility and no increase in apparent density. [4] Figure 6 presents the sintered TRS of the six premixes evaluated. Figure 6A shows the TRS for premixes containing 0.7% added graphite and Figure 6B shows the TRS for premixes containing 0.3% added graphite. For both graphite conditions evaluated, the atomized material has equivalent sintered strength at equivalent densities compared with the traditional sponge products. Although not shown, sintered hardness values for the atomized sponge iron are equivalent to the traditional sponge materials. A: Sintered TRS for 0.7% added graphite containing premixes Figure 6: B: Sintered TRS for 0.3% graphite containing premixes Sintered TRS of the six materials evaluated Conclusions: An atomized “sponge like” powder has been developed possessing low apparent density and higher compressibility compared with traditional sponge materials. Sintered TR strength of the atomized low apparent density material is equivalent to the sintered TRS of traditional sponge materials. Sintered dimensional change at higher graphite additions (>0.5% graphite) for the atomized “sponge like” powder is equivalent to the direct reduced iron ore. At lower graphite additions (~0.3% graphite), the atomized “sponge like” exhibits more positive sintered dimensional change. A potential disadvantage of these grades is the reduced green strength; however, utilizing nontraditional powder lubricants overcome this shortcoming and produce green strengths equivalent to traditional sponge materials. These materials have successfully replaced direct reduced iron in many applications. References: 1. Iron Powder Metallurgy Handbook, published by Hoganas-Billesholms AB, Hoganas, Sweden, Vol. 1, 1957. 2. J. Wilson, Internal Hoeganaes Corporation report 3. ASM Handbook, Volume 7, published by ASM International, Metals Park Ohio, 1998, p.36. 4. Hoeganaes Corporation Technical Literature at www.hoeganaes.com, product, unalloyed steel.