Effect of Hydrogen Pressure on Moisture-Based Fabrication of Lotus-Type Porous Nickel

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1 Materials Transactions, Vol. 47, No. 9 (26) pp. 212 to 2124 Special Issue on Porous and Foamed Metals Fabrication, Characterization, Properties and Applications #26 The Japan Institute of Metals Effect of Hydrogen Pressure on Moisture-Based Fabrication of Lotus-Type Porous Nickel Hirofumi Onishi, Soong-Keun Hyun* and Hideo Nakajima The institute of Scientific and Industrial Research, Osaka University, Ibaraki , Japan Lotus-type porous nickel, which has long straight pores aligned in one direction, was fabricated by utilizing moisture during unidirectional solidification in argon atmosphere. We studied the effect of the quantity of hydrogen in the atmosphere on the fabrication of lotus-type porous nickel. Adding hydrogen in the atmosphere, it was expected that the porosity of the lotus-type porous nickel with a smaller pore diameter became larger because not only the moisture but also hydrogen gas in the atmosphere were the supply source of hydrogen bubble. However, in fact, the pore diameter and the porosity of lotus-type porous nickel gradually decreased as the hydrogen partial pressure increased up to a point. When hydrogen was further added to the atmosphere, the pore diameter and porosity increased while the number of pores decreased dramatically. As a result of the fabrication under various pressures, the partial pressure of hydrogen at the border was.5 MPa. No moisture can be dissociated when a large amount of hydrogen is dissolved in the molten nickel. [doi:1.232/matertrans ] (Received February 28, 26; Accepted August 21, 26; Published September 15, 26) Keywords: nickel, unidirectional solidification, moisture, hydrogen pressure 1. Introduction Porous metals such as foamed and cellular metals have been attracting attention because of their specific properties. Therefore, basic and applied researches on porous metals have been carried out for industrial applications of structural materials due to their low density, catalyst and electrode materials due to their huge surface-to-volume ratio, and so on. 1 3) Recently, lotus-type and gasar-type porous metals with many elongated pores and superior mechanical properties than conventional porous materials have been developed. 4 14) The fabrication principle of such porous metals is as follows; the solubility difference of hydrogen, nitrogen or oxygen between the solid and liquid phases can cause gas bubbles during solidification. Elongated pores can be produced by unidirectional solidification using a watercooled hearth as the bottom face of the casting mold. In the case of nickel, unidirectional pores were confirmed in a specimen fabricated in argon atmosphere in spite of the fact that argon was inert gas. 15) Based on the results of the detailed study of gases in these cylindrical pores, the gas was confirmed to be hydrogen. The origin of hydrogen was moisture in the liniment coating inside the mold as a moldrelease agent. 16,17) The lotus-type porous nickel fabricated utilizing the moisture in the mold possessed the similar porosity and a smaller pore diameter than previously reported lotus-type porous nickel fabricated in hydrogen atmosphere possess. 17) A smaller pore diameter results in a large surface area of the specimen with the same porosity value. Surface area will be an important parameter when these metals are applied as functional materials. In this study, lotus-type porous nickel was fabricated in argon-hydrogen atmosphere for controlling the porosity and maintaining a small pore diameter. This paper examines the effect of hydrogen partial pressure, P H2, on the fabrication of lotus-type porous nickel by utilizing the moisture in the mold. *Corresponding author, hyun23@sanken.osaka-u.ac.jp Table 1 Chemical composition of impurity element in nickel (mass%). Co Fe Cu Pb Mn C S Si < :1 < :1 < : Experimental Procedure Lotus-type porous nickel was fabricated from 99.9% pure electrolytic nickel. Chemical analysis of impurity in nickel is compiled in Table 1. For pretreatment, contaminants on the surface of electrolytic nickel were eliminated by grinding, followed by ultrasonic cleaning in acetone. About 12 grams of nickel is weighed out and used as the ingredient for lotustype porous nickel. A schematic drawing of the mold to fabricate lotus type porous metals is shown in Fig. 1. This apparatus consists of a part for melting the materials and another part for solidifying the molten materials. The chamber of this apparatus is connected to gas lines (H 2 and Ar). The total pressure, P total, in the chamber can be controlled from vacuity to approximately 2.8 MPa. By the high pressure probe connected to the chamber, it is possible to measure and control the pressure in the chamber to an accuracy of.1 MPa. Metals are heated in a crucible set up inside the high-frequency copper coil in the melting part. Graphite crucibles have been commonly used in making lotus-type porous metals, but alumina crucibles are used in this study because of the high reactivity of nickel with graphite. A pyrometer is used for the measurement of the molten metal temperature by observing through the observation window. Molten metal in the alumina crucible was cast into a mold located in the solidification part by rotating the apparatus by 9 degrees. A copper hearth is assembled at the bottom of the mold in order to obtain unidirectional solidification from the bottom to the top of the mold. For cooling, water at approximately 29 K flowed through the copper hearth. A molybdenum sheet with a thickness of.1 mm was

2 Effect of Hydrogen Pressure on Moisture-Based Fabrication of Lotus-Type Porous Nickel 2121 Mold Ar atmosphere Water cooling Mo Ni(melt) Mixture of alumina, water glass and water Pore Fig. 1 A schematic showing the melting and unidirectional solidification process of lotus-type porous nickel without dissolving with the gas in the atmosphere. formed on a cylinder with an inner diameter of approximately 3 mm and a height of approximately 8 mm as the side wall of the mold. A mixture of alumina powder (1 mm), water glass (54.5% H 2 O, 31.2% SiO 2 and 14.3% Na 2 O) and water in the volume ratio of 8:2:5was applied to the inside of the molybdenum mold. This mixture served not only as a water retention material but also as a heat insulation material for preventing the reaction of nickel and the mold. Subsequently, after the mold was dried at 423 K for 7.2 ks in the oven to completely dry off the moisture in the mixture, the mold was kept in a closed vessel with constant humidity (75 or 9%) for a given time in order to measure the mass of moisture reabsorbed inside the mold. The alumina crucible and the mold were set in the chamber. After the chamber was evacuated to several Pa by using a rotary pump, Ar was introduced in the chamber, and the vacuum level in the chamber was again further increased using the rotary pump. Ar and H 2 were introduced in the chamber to a certain partial pressure. Then, the heating of nickel was started by increasing the voltage of the highfrequency copper coil until nickel dissolved completely. The molten nickel was cast and solidified in one direction. During solidification, the moisture absorbed by Al 2 O 3 Na 2 SiO 3 at atmospheric temperature was expected to be dissolved into the melt thereby forming gas pores at the solid-liquid interface. 15,16) The resulting ingots had a diameter of 28 mm and a maximum height of 9 mm, and they were characterized by porosity depending on the P H2. The P total during fabrication was.4 or.8 MPa, and the P H2 ranged from to.15 MPa. An ingot of lotus-type porous nickel was cut parallel to the direction of pore growth by a spark-erosion wire cutting machine (Model A32D, Sodic Co.) for observing the longitudinal section. The specimen for cross-sectional observation was cut perpendicular to the direction of pore growth at a distance of 5 mm from the cooling surface because pores were not generated uniformly near the surface. The porosity of the specimen was calculated using the volume of the specimen, the mass of the specimen, and the density of nickel as follow: " ¼ 1 m ds 1 where ", m, d and s denote the porosity, the mass, the thickness and the cross-sectional area of the specimen, respectively, and is the density of nonporous nickel. The pores were circular in the cross-sectional image because the pores had a cylindrical configuration and the longitudinal direction of the pores was in the direction of solidification. The average pore diameter was measured by analyzing the cross-sectional image (Win ROOF, Mitani Co.). The oxygen content in lotus-type porous nickel fabricated under P total ¼ :8 MPa was determined by an oxygen analyzer (Model TC-3, LECO Co.). Quantitative analysis of oxygen was performed by the He carrier melting-infrared absorption method. The analyzability value of this apparatus ranges from 2 to 2 mass ppm, and the smallest analyzability value is.2 mass ppm. 3. Results and Discussion 3.1 Moisture in the mold The mass of absorbed moisture in the mold is important to understand the fabricating process utilizing the moisture. We determined the mass of moisture by measuring the difference in weight of the mold before and after the absorption of moisture. The mass of the mold drastically increased within a short time by absorbing the moisture in the atmosphere even if the mass depends on the weather or the season. For this reason, the mold was kept in a closed vessel with constant humidity (75 or 9%). Figure 2 shows the time dependence of the mass of absorbed moisture in the closed vessel kept at constant humidity. The mass of the mixture of alumina, water glass and water in the volume ratio of 8:2:5was constant to 1.2 g. The mass of absorbed moisture tended to increase Mass of moisture, m / g Time, t / ks : Humidity 75 % : Humidity 9 % Fig. 2 Dependence of the mass of absorbed moisture on time in a closed vessel with constant humidity (75 or 9%). ð1þ

3 2122 H. Onishi, S.-K. Hyun and H. Nakajima linearly with either 75 or 9% humidity when the time ranged from to 7.2 ks. However, the mass of absorbed moisture tended to be constant after this period. As a result, the potential mass of absorbed moisture was attributed to the humidity of the atmosphere in which the mold was kept, and the saturated values of the mass of absorbed moisture depended on the humidity. Additionally, the absorbed moisture in the mold was subjected to the molten Ni in this study after evacuation of the chamber by the rotary pump. The variation of the mass of absorbed moisture in the mold (which was kept in the closed vessel with 9% humidity for 7.2 ks) under vacuum is shown in Fig. 3. After starting the rotary pump, the mass of moisture decreased for 7.2 ks. However, after 7.2 ks, the mass of moisture hardly decreased. In addition, it was revealed that Mass of moisture, m / g Fig Time, t / ks Dependence of the mass of moisture in the mold on time in vacuum. the mass of moisture become a constant value as time advances. Based on this result, the mass of moisture in the mold for fabricating lotus-type porous nickel could be easily estimated. The condition used for absorbing moisture in this study was 9% humidity for 7.2 ks. 3.2 Pore morphology Figure 4 shows the longitudinal and cross-sectional images of lotus-type porous nickel fabricated under P total ¼ :8 MPa. Figure 5 shows the relationship between the average pore diameter and porosity and the partial pressure of hydrogen. In either of the fabricating conditions, the value of the pore diameter slightly increased with increasing the P H2 to.5 MPa. Following this, the value of pore diameter decreased down to a certain partial pressure and increased again. On the other hand, the value of porosity decreased up to the same partial pressure followed by an increase in Fig. 5(a). The pore diameter and porosity tended to become minimum at approximately P H2 ¼ :5 MPa when the P total was both.4 MPa and.8 MPa. The change of pore diameter and porosity with an increase in the P H2 is examined as follows. Figure 6 shows a schematic of the casting process under P total ¼ :8 MPa; the P H2 is (a) MPa, (b).5 MPa and (c) above.5 MPa. When the P H2 is MPa as shown in Fig. 6(a), the molten nickel in the crucible does not contain any hydrogen. However, the moisture in the mold is dissociated during solidification and then hydrogen can be absorbed by molten nickel. Furthermore, oxygen intrudes into molten nickel and oxides such as SiO 2 are formed. Consequently, the pore diameter is smaller than that of porous nickel fabricated under pressure above P H2 ¼ :5 MPa as shown in Fig. 5 (a) (b) (c) Fig. 4 Optical micrographs of parallel section to the direction of pore growth fabricated under total pressure of.8 MPa; hydrogen partial pressure is (a) MPa, (b).5 MPa and (c).1 MPa.

4 Effect of Hydrogen Pressure on Moisture-Based Fabrication of Lotus-Type Porous Nickel 2123 (a) 15 1 Average pore diameter, d / µ m Porosity (%) Hydrogen pressure / MPa (b) 15 1 Average pore diameter, d / µ m Porosity (%) Fig. 5 Dependence of porosity and average pore diameter on the partial pressure of hydrogen; total pressure is (a).4 MPa and (b).8 MPa. 2 Fig. 6 Schematic showing the casting process under total pressure of.8 MPa; partial pressure of hydrogen is (a) MPa, (b).5 MPa and (c).5.1 MPa. because these oxides act as pore nucleation site. Furthermore, the pore number density is higher than that of porous nickel fabricated under pressure above P H2 ¼ :5 MPa as shown in Fig. 7. When the P H2 is.5 MPa as shown in Fig. 6(b), the molten nickel in the crucible contains a small amount of hydrogen from the atmosphere. It is believed that less moisture is dissociated when molten nickel contains hydrogen. Consequently, the porosity and pore diameter decrease as the P H2 increases. However, the pore number density is almost constant because of the oxides such as SiO 2 generated by the dissociation of moisture. These oxides created from impurity element exist a very small amount in melt, which may not receive an effect in decrease of oxygen supply. When the P H2 is above.5 MPa as shown in Fig. 6(c), the molten nickel in the crucible contains a large amount of hydrogen from the atmosphere because of high P H2. In this Pore number density, n / mm Fig. 7 Dependence of pore number density on the partial pressure of hydrogen (total pressure:.8 MPa). case, it is expected that no moisture is dissociated because of a large amount of hydrogen in the molten nickel. In other words, only in this case, lotus-type porous nickel is fabricated by utilizing hydrogen in the atmosphere. As a result, the porosity and pore diameter increased while the number of pores decreased; this was observed even in case of lotus-type porous metals fabricated in hydrogen atmosphere. According to the Ellingham diagram, the dissociation reaction of moisture, Ni þ H 2 O! NiO þ H 2 ; ð2þ occurs when the partial pressures ratio of H 2 O and H 2, P H2 O=P H2, is more than approximately 2: 1 2. It can be

5 2124 H. Onishi, S.-K. Hyun and H. Nakajima.4 4. Conclusion Oxygen content (mass%) We studied the effect of hydrogen partial pressure in the atmosphere on the fabrication of lotus-type porous nickel. The pore diameter and porosity of lotus-type porous nickel gradually decreased as hydrogen partial pressure was increased up to a point. However, when hydrogen was further added to the atmosphere, the pore diameter and porosity increased while the number of pores decreased dramatically. As the result of the fabrication under various pressures, the hydrogen partial pressure at the border was.5 MPa. REFERENCES Fig. 8 Dependence of oxygen content in the matrix on the partial pressure of hydrogen during fabrication (total pressure:.8 MPa). explained that dissociation reaction of moisture did not occur under P H2 > :5 MPa since P H2 O=P H2 might be smaller than approximately 2: 1 2. Further investigation into details is required. 3.3 Oxygen content The specimen was hewed from an ingot of lotus-type porous nickel by a fine cutter in order to prevent oxidation. The oxygen content in the matrix as well as the porosity and pore diameter depend on the P H2 ranging between to.6 MPa. Furthermore, a very small amount of oxygen was contained in the matrix when the P H2 was equal to or greater than.6 MPa as shown in Fig. 8. It is believed that oxygen is generated by the dissociation of moisture in the mold. Consequently, when the P H2 was not less than approximately.5 MPa, lotus-type porous nickel was fabricated utilizing the hydrogen only in the atmosphere. 1) L. J. Gibson and M. F. Ashby: Cellular Solids, Cambridge Univ. Press, Cambridge ) J. Banhart: Prog. Mater. Sci. 46 (21) ) J. Barhart and D. Weaire: Phys. Today 55 (22) ) L. V. Boiko, V. I. Shapovalov and E. A. Chernykh: Metallurgiya 346 (1991) ) H. Nakajima: Mater. Integration 12 (1999) ) H. Nakajima: The Production & Technique 51 (1999) ) H. Nakajima: Boundary 15 (1999) ) H. Nakajima: Funct. Mater. 2 (2) ) H. Nakajima: J. High Temp. Mater. 26 (2) ) H. Nakajima, S. K. Hyun, K. Ohashi, K. Ota and K. Murakami: Colloid. Surface. A 179 (21) ) S. Yamamura, Y. Shiota, K. Murakami and H. Nakajima: Mater. Sci. Eng. A 318 (21) ) S. K. Hyun and H. Nakajima: Mater. Trans. 43 (22) ) S. K. Hyun, K. Murakami and H. Nakajima: Mater. Sci. Eng. A 299 (21) ) S. K. Hyun and H. Nakajima: Mater. Sci. Eng. A 34 (23) ) H. Mizugai: Undergraduate Thesis, Engineering department, Osaka Electro-Communication Univ. (22). 16) S. Yamamura: Master s Thesis, Graduate School of Engineering, Osaka Univ. (21). 17) Y. Suematsu, S. K. Hyun and H. Nakajima: J. Japan Inst. Metals 68 (24)

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