Development of New High-Purity Alumina

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1 Development of New High-Purity Alumina Sumitomo Chemical Co., Ltd. Basic Chemicals Research Laboratory Shinji FUJIWARA Yasuaki TAMURA Hajime MAKI Norifumi AZUMA Yoshiaki TAKEUCHI Sumitomo s high-purity alumina has been manufactured by the method of hydrolysis of aluminum alkoxide since 1981, and the present production capacity is 1500t/Y. High-purity alumina is used in areas such as displays, energy, automobiles, semiconductors and computers and demand for it is growing steadily. In this paper, a general view of recent applications for high-purity alumina is introduced, and our newlydeveloped high-purity alumina products are also described. Al2O IC t/Y t/Y 1) 10) 11) AACH 12) 13) 14) Fig

2 Al + 3ROH / Al (OR)3 + 3/2H2 (1) 2Al (OR)3 +4H2O / Al2O3 H2O + 6ROH (2) Al2O3 H2O / Al2O3 + H2O (3) Fig. 1 ROH H2O Al Metal Alkoxide Synthesis Hydrolysis Hydrated Alumina Calcination Processing High Purity Alumina Manufacturing process of High Purity Alumina by alkoxide method Boehmite γ, δ, θ- Al2O3 -Al2O3 -Al2O3 nm -Al2O Al2O3 -Al2O3 -Al2O3 15) 18) 18), 19) 20), 21) -Al2O3 -Al2O3 Table 1 Character of Sumitomo s high purity alumina AKP-20 AKP-30 AKP-50 AKP-3000 AKP-G008 AKP-G015 HIT-50 Crystal Form Purity (%) Particle Size (µm) Loose Bulk Density (g/cm 3 ) BET Surface Area (m 2 /g) Impurity Level Si (ppm) Na (ppm) Mg (ppm) Cu (ppm) Fe (ppm) 0.4 ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 8 20 θ 5 < 0.1 ~ 80 ~ 8 8 γ 5 < 0.1 ~ 150 ~ 8 8 > ~ 0.25~ 6 ~

3 22), 23) Table 1 Fig. 2 24) In Situ Chemical Vapor Deposition -Al2O3 µm Fig. 3 (1) AKP-30 (2) AKP-3000 Fig. 3 SEM image of Sumicorundum 10µm Fig. 2 1µm 1µm (3) AKP-G015 (4) HIT µm 0.25µm SEM and TEM images of Sumitomo s high purity alumina Al2O3 -Al2O Rajendran 25) -Al2O nm -Al2O3 (1) 70nm (2) 50nm (3) 30nm 100nm Fig. 4 TEM images of Sumitomo s nano-sized -Al2O3 powders 2007-

Krell Ma 26) 28) 0.1µm Diaspore -Al2O3 950 50nm -Al2O3 -Al2O3 -Al2O3 Fig.

33) -Al2O3 AKQ-10 2.0g/cm 3 -Al2O3 Table 2 Fig.

4 Krell Ma 26) 28) 0.1µm Diaspore -Al2O nm -Al2O3 -Al2O3 -Al2O3 Fig. 4 Verneuil γ -Al2O3 EFG Edge-defined Film-fed Growth LED Light Emitting Diode 29) LED LED 30) LEDGaN 3-5 GaNGaN 31) -Al2O Mo -Al2O3 32) 2mm AKQ-10 Czochralski 33) -Al2O3 AKQ g/cm 3 -Al2O3 Table 2 Fig. 5 -Al2O3 -Al2O3 Table 2 Character of -Al2O3 for sapphire single crystal Crystal Form Purity (%) Loose Bulk Density (g/cm 3 ) BET Surface Area (m 2 /g) Impurity Level Si (ppm) Na (ppm) Mg (ppm) Cu (ppm) Fe (ppm) Ca (ppm) AKQ-10 1 ~ ~ 3 ~ High Density New Alumina 2 1 (1) AKQ-10 (2) High Density New Alumina Fig. 5 1mm SEM images of -Al2O3 for sapphire single crystal 2007-

PDP Plasma Display Panel PDP 34) 147nm Xe172nm Xe VUV 254nm BaMgAl10O17 : Eu 2+ BAM PDP VUV 35) BAM Ba Mg Eu 36) 38) 39) 5 40) 41) 42) Fired Density (g/cm 3 ) 4.00 3.80 3.60 3.40 3.

5 PDP Plasma Display Panel PDP 34) 147nm Xe172nm Xe VUV 254nm BaMgAl10O17 : Eu 2+ BAM PDP VUV 35) BAM Ba Mg Eu 36) 38) 39) 5 40) 41) 42) Fired Density (g/cm 3 ) Fig. 6 Powder A (particle size : 0.5µm) Powder B (particle size : 0.4µm) Powder C (particle size : 0.2µm) Powder D (particle size : 0.1µm) Temperature ( C) Sintering behavior of Sumitomo s high purity alumina powders A/F Air fuel ratio sensor A/F Fig. 7 1µm Microstructure of Powder D (MgO = 500ppm addition) sintered body at 1300 C 2007-

6 -Al2O3 Fig. 6 Fig. 7 -Al2O3 24) 43) -Al2O3 PETPEN 48) Fig. 8 Fe C -Al2O3 100nm 49) -Al2O3 Magnetic Recording Tape Fig. 8 Magnetic Layer Non-Magnetic Layer Base film Back coating Layer Magnetic Head Magnetic Recording System -Al2O3 Particle Magnetic Particle Binder Non-Magnetic Particle -Al2O3 1 -Al2O3 HITFig ) 47) -Al2O3 CMP Chemical Mechanical Polishing 2 -Al2O3 Ma 26), 27) -Al2O Al2O g/cm

7 3 -Al2O CH4 + H2O / 3H2 + CO (4) Fig. 9 -Al2O3 γ - Al2O3 Pore Volume (cc/g) Fig. 10 Powder B (particle size : 0.4µm) Powder C (particle size : 0.2µm) Powder D (particle size : 0.1µm) Nano-Al2O3 (particle size : 50nm) Pore Radius (nm) Pore size distribution of high purity alumina powder compacts 16nm -Al2O3 H2 separation Layer (SiO2, Zeolite) Intermediate Layer (γ-al2o3) Porous Tube (-Al2O3) Fig. 9 H2 H2, CO Structure of Hydrogen separation element γ - Al2O3 -Al2O3 -Al2O3 1/5 Krell Ma 28) -Al2O nm 40 -Al2O nm -Al2O3 γ -Al2O3 2 50nm Al2O3 50) -Al2O3 Fig. 10 -Al2O3 -Al2O3 CO 1),,,, 2, 59 (1980). 2),,, 2 (5), 23 (1982). 3),,,, 58 (3), 106 (1984). 4),,,, 1984 (6), 63. 5), FC, 3 (7), 9 (1985). 6),,, 48, 173 (1985)

8 7) H.Kadokura, and M.Hama, New Materials New Processes, 3, 335 (1985). 8),, !, 4 (1993). 9),,, 29 (8), 659 (1994). 10),, 36 (4), 248 (2001). 11),, 17 (9), 764 (1982). 12),, 4, 100 (1983). 13),,,,, 6 (6), 461 (1971). 14),,,, 21, 540 (1972). 15) M.Kumagai, and G.L.Messing, J.Am.Ceram.Soc., 67 (11), C-230 (1984). 16) M.Kumagai, and G.L.Messing, J.Am.Ceram.Soc., 68 (9), 500 (1985). 17) J.L.McArdle, and G.L.Messing, J.Am.Ceram.Soc., 76 (1), 214 (1993). 18) R.B.Bagwell, and G.L.Messing, J.Am.Ceram.Soc., 82 (4), 825 (1999). 19) H.Yanagida, G.Yamaguchi, and J.Kubota,, 74 (12), 371 (1966). 20),,, 10, 175 (1989). 21) P.Burtin, J.P.Brunelle, M.Pijolat, and M.Soustelle, Appl.Catal., 34, 225 (1987). 22), (1999). 23), (2004). 24),,,,,,,,,,, FC, 24 (4), 153 (2006). 25) S.Rajendran, J.Mater.Sci., 29, 5664 (1994). 26) A.Krell, and H.Ma, NanoStructured Materials, 11 (8), 1141 (1999). 27) H.Ma, and A.Krell, Key Engineering Materials, , 43 (2002). 28) A.Krell, and H.Ma, J.Am.Ceram.Soc., 86 (2), 241 (2003). 29), (2000). 30) JLEDS Technical Report, 1 (2005). 31), FC, 22 (6), 163 (2004). 32), (2005). 33), (2006). 34),, (2006), p ),, 41 (8), 593, (2006). 36), (2004). 37),, (2004). 38), (2001). 39),,, Matsushita Technical Journal, 47 (4), 323 (2001). 40),,,,, No.27-02, p.11 (2002). 41), (1997). 42), (1999). 43), FC, 23 (1), 12 (2005). 44) TDK, (1987). 45), (1999). 46), (1991). 47), (1994). 48),,,,, FUJIFILM RESEARCH & DEVELOP- MENT, 48, 76 (2003). 49),,,,,, FUJIFILM RESEARCH & DEVELOP- MENT, 48, 71 (2003). 50), (2005)

9 PROFILE Shinji FUJIWARA Norifumi AZUMA Yasuaki TAMURA Yoshiaki TAKEUCHI Hajime MAKI 2007-

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