# Fileset [fgm-2003-1-172.xlsx](https://mdr.nims.go.jp/filesets/b264d340-7b8f-4be5-8e9a-31dc6dbb0fdc/download) ## Creator National Institute for Materials Science ## Rights ## Other metadata [Proceedings of the 15th Symposium on Functionally Gradient Materials (FGM 2003 in Sapporo) (pp.1-172)](https://mdr.nims.go.jp/datasets/ae6b0a98-1324-4f8c-a9bc-53b2d70e036d) ## Fulltext Sheet1 BookTitle_j BookTitle_e Volume/Issue Issueddate Page Title_j Title_e AuthorList_j AuthorList_e Abstract Language 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 1-4 水熱ホットプレス法によるチタンとハイドロキシアパタイトセラミックス接合に及ぼす圧力,反応時間の影響 Effects of pressure and reaction time on the Bonding of Hydroxyapatite Ceramics and Titanium by the Hydrothermal Hot-pressing Method 小野木伯薫、田中雅明、橋田俊之/東北大院・工・破制研, 細井和幸/白石工業(株) Takamasa ONONKI, Masa-aki TANAKA, Toshiyuki HASHIDA/Fracture Research Institute, Grad. Sch. of Eng., Tohoku Univ., Sendai, 980-8579, Japan. Kazuyuki HOSOI/Shiraishi Kogyo Kaisha Ltd., Amagasaki, 660-0085, Japan. Solidification of hydroxyapatite (HA) and its bonding with titanium (Ti) were simultaneously achieved by using a hydrothermal hot-pressing (HHP) method at the low temperature as low as 150 deg.C. A mixture of calcium hydrogen phosphate dehydrate and calcium hydroxide was used as a starting material powder for solidifying HA. 3-point bending tests were conducted to obtain an estimate of the fracture toughness for the HA/Ti interface. Application of pressures greater than 20MPa was necessary for bonding, and the interface strength increased with the increasing applied pressure. However, the degree of HA formation was lower when the pressure was increased. Excessively long term HHP treatment was shown to be ineffective for the bonding and there was an optimal treatment time. The optimal pressure and treatment time for bonding were estimated to be 40MPa and 12h, respectively. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 5-9 天然・人工気孔を有する傾斜機能アパタイトと硬組織誘導 Hard Tissue Induction using Functionally Graded Apatite with Natural and Artificial pores 村田勝,佐々木智也,田崎純一,有末眞/北海道医療大・歯.　赤澤敏之/道工試・材料技術部.　菅野亨,小林正義/北見工大・化学システム工学科 Masaru MURATA, Tomoya SASAKI,Junichi TAZAKI, Makoto ARISUE/School of Dentistry, Health Science University of Hokkaido, Japan. Toshiyuki AKAZAWA/Department of Materials Technology, Hokkaido Industrial Research Institute, Japan. Tohru KANNO, Masayoshi KOBAYASHI/Department of Chemical System Engineering, Kitami institute of Technology, Japan. A unique biomimetic material, functionally graded calcium phosphate (HAp), was developed and its efficacy as a carrier for recombinant human bone morphogenetic protein-2 (rhBMP-2) was evaluated histologically. The HAp was prepared as a random composite of cattle spongy bone with stepwise sintering and HNO3-etching, and precipitation derived from minerals in cortical bone. The time-course of bone induction by rhBMP-2(5 micro gram) and HAp block (3*3*3mm) was investigated in the subcutaneous tissue of 4 weeks-old Wistar rats. Histological examination showed that the surface and bulk degradation of the HAp was found and the absorption of the HAp, adsorbing body fluid, was accelerated as induced bone matured. These results indicate that the HAp is a novel type of biointegrated materials as to be absorbed from the outside and the inside, and completely replaced by new bone. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 10-15 カーボンナノチューブの固化とハイドロキシアパタイト被覆 Consolidation of Multi-Walled Carbon Nanotube and Hydroxyapatite Coating 大森守,大久保昭/東北大・金研.　大坪誠,田路和幸,橋田俊之/東北大院・工 Mamoru OMORI, Akira OKUBO/Tohoku University, Institute for Materials Research, Sendai, Japan. Makoto OTUBO, Kazuyuki TOHJI, Toshiyuki HASHIDA/Tohoku University, Graduate school of Engineering, Sendai, Japan. The multi-walled carbon nanotube(MWNT) was coated with phenol resin and consolidated at 1000-1600 deg.C at 120MPa in a vacuum by the spark plasma system(SPS). The bulk density was between 1.67g/cm3 and 1.74g/cm3 for the MWNTs consolidated at 1000-1400 deg.C. Young's modulus was 11.1 GPa for the MWNT consolidated at 1200 deg.C and 3.05GPa for the MWNT consolidated at 1000 deg.C. The consolidated MWNT was put in the suspension made of 6CaHPO4'2H2O and 4Ca(OH)2. The coated compounds were heated at 1000 deg.C at 120MPa in a vacuum by SPS and resulted in the hydroxyapatite film on the consolidated MWNT. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 16-21 rhBMP-2/FRIOS Algipore 複合体による硬組織形成誘導 Hard tissue formation by rhBMP-2/FRIOS Algipore composite 小林文人,小池俊之,斉藤隆史/北海道医療大　　別所和久/京大大学院・医 F.Kobayashi, T.Koike, M.Ogawa, T. Saito/Health Sciences University of Hokkaido, School of Dentistry. K.Bessho/Kyoto University, Graduate School of Medicine. The purposes of this study were to determine if Algipore, calcified algae-derived porous hydroxyapatite, that has a pore size of 10-30 micro meter, porosity of over 65%, and a very large surface area of 50m2/g, is an effective carrier for BMP in heterotopic and orthotopic hard tissue formation, and to investigate the possibility of clinical applications of BMP/Algipore composite in pulp-conservative therapy. Five microgram of E.coli-derived recombinant human. BMP-2 variant(rhBMP-2) was combined with Algipore 0.3-0.5(particle size of 0.3-0.5mm) or Algipore 0.5-1.0(particle size of 0.5-1.0mm). Each sample was implanted subcutaneously in 4-week-old Wistar rat. The samples were harvested 1, 2, and 3 weeks after implantation. Then, biochemical and histological analyses were performed in each sample.At 3-week(3 weeks after implantation), dry weight of rhBMP-2/Algipore 0.3-0.5 increased 2.2 times more than that before implantation. For rhBMP-2/Algipore 0.5-1.0, it was 1.8 time. An ALPase activity of rhBMP-2/Algipore 0.3-0.5 showed a high peak at 1-week, then it decreased quickly whereas rhBMP-2/Algipore0.5-1.0 showed a peak at 2-week. In histological analysis, rhBMP-2/Algipore found to induce a great volume of bone and marrow formations compared with control groups(Algipore alone).From above results, it was suggested that rhBMP-2/Algipore composite that possesses biocompatibility could be the effective bio-material for hard tissue formation. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 22-27 カーボンナノチューブ,ナノ・マイクロ微粒子に対する生体反応 Pathobiological Response of Carbon nano-tubes and Micro/nano particles 田村一央,　高師則行,　赤坂司,　ロスカ・イオシフ,　宇尾基弘,　戸塚靖則,　亘理文夫/北大院・歯.　田路和幸/東北大院・工. Kazuchika TAMURA, Noriyuki TAKASHI, Tskasa AKASAKA, Rosca IOSIF, Motohiro UO, Yasunori TOTSUKA, Fumio WATARI/Hokkaido University, Graduate School of Dental Medicine, Sapporo, Hokkaido, Japan. Kazuyuki Tohji/Tohoku University, Industrial Research Institute, Sendai, Miyagi, Japan. The cytotoxicity of micro/nano particles in Ti, TiO2 and carbon nanotube was investigated by in vitro biochemical analyses using human neutrophils. The particles smaller and larger than the neutrophils were used to determine the relationship between cell and particle size with respect to cytotoxicity. As the particle size decreased, the cell survival rate decreased and, with the good corresponding relation to this, the value of lactate dehydrogenase(LDH), which is the indication of cell disruption, was increased. The release of superoxide anion showed the increasing tendency. Proinflammatory cytokines were detected distinctly for 3 micro meters or smaller particles and very little in more than 10 micro meters, which is closely related to the phagocytosis by neutrophils. ICP elemental analysis showed that the dissolution from Ti particles was below detection limit. Micro and nano particles stimulated the cell reactions according to the results of the human neutrophil functional tests. As the particle size was smaller, the inflammation was pronounced. The fine particles less than 3 micro meters caused distinctly the inflammation in the surrounding tissue. All these results indicated that the cytotoxicity was induced due to the physical size effect of particles, which is different from the ionic dissolution effect. The clinical phenomenon confirmed the result obtained in vitro cell tests. The neutrophils stimulated by fine particles may cause the inflammatory cascade and harm the surrounding tissue. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 28-33 牛骨由来生体吸収性傾斜機能アパタイトの作成とそのキャラクタリゼーション Preparation and Characterization of Bio-absorbable and Functionally Graded Apatites Originated from Cattle Bone 赤澤敏之,板橋孝至/道工試・材料技術部村田勝,佐々木智也,田崎純一,有末眞/道医療大・歯学部小林正義,菅野亨/北見工大・化学システム工学科 Toshiyuki AKAZAWA,Takashi ITABASHI/Hokkaido Insdustrial Research Institute, Department of Materials Technology, Sapporo, Hokkaido, JapanMasaru MURATA, Tomoya SASAKI, Junichi TAZAKI,Makoto ARISUE/Health Sciences University of Hokkaido, Faculty of Dentistry, Sapporo, Hokkaido, JapanMasayoshi KOBAYASHI, Tohru KANNO/kitami institute of Technology, Department of Chemical System Engineering, Kitami, Hokkaido, Japan Bio-absorbable and functionally graded apatite(fg-HAp) ceramics with 100-600 micro meters pore sizes and 60-80% porosities, were prepared using calcined cattle bones by a complete or partial dissolution-precipitation method. Crystallinity and grain size gradations of hydroxyapatite were optimally designed. Recombinant human bone morphogenetic protein(rhBMP-2) was added to the fg-HAp ceramics, and the two ceramics prepared were implanted to the subcutaneous tissue of rats. For the fg-HAp ceramics, body fluid was well invaded into the micropores, and many giant cells were observed. For the rhBMP-2/fg-HAp ceramics, permeation and diffusion of body fluid and active bone formation were recognized. Accordingly, the rhBMP-2/fg-HAp ceramics were found to be one of biomimetic materials, which gave faster bio-absorption and osteoinduction. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 34-39 バイオ用カーボンナノファイバーの開発 Development of carbon nanofibers for biomedical uses 佐藤義倫,畠山力三/東北大院・工秋本結輝,大坪誠,田路和幸/東北大院・環境科学 Yoshinori SATO, Rikizo HATAKEYAMA/Tohoku University, Graduate School of Engineering, Sendai, Miyagi,JapanYuki AKIMOTO, Makoto OHTSUBO, Kazuyuki TOHJI/Tohoku University, Graduate school of Enviromental Studies, Sendai, Japan Cone-stacked carbon nanofibers were simply cut and well dispersed in water using sonication in a mixture of concentrated H2SO4 and HNO3 in order to use them as the biomaterials. The "cut" cone-stacked carbon nanofibers were characterized by SEM, TEM, XRD, and FT-IR measurements. Carbon nanofibers were easily cut into 400-nanometer to 1.5-micrometer lengths. The resulting cut nanofibers formed a stable solution in water without the help of surfactants. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 40-45 放電プラズマ焼結法で作製した窒化チタン/アパタイト系傾斜機能型インプラントの物性と生体適合性 Evaluation of properties and biocompatibility of titanium nitride/apatite functionally graded implants fabricated by spark plasma sintering 近藤秀臣,横山敦郎,川崎貴生/北大院・歯・有床義歯補綴宇尾基弘,亘理文夫/北大院・歯・歯科理工 Hideomi Kondo, Atsuro Yokoyama, Takao Kawasaki, Motohiro Uo, Fumio Watari/Graduate school of Dental Medicine, Hokkaido University, Sapporo Titanium nitride/hydroxyapatite functionally graded implant(TiN/HAP) was successfully fabricated by spark plasma sintering method (SPS) and the properties were investigated. The functionally graded materials(FGMs) with the concentration from TiN at one end to HAP at the other were prepared by sintering at 1100 and 1200 deg.C. under the pressure of 150MPa. The Brinell hardness was around 60, nearly uniform for the whole range of composition. After 2 and 8 weeks implantation in diaphysis of femur of rat there was very little inflammation and the new bone was formed around the sample. By use of TiN instead of Ti, the decomposition of HAP during sintering process could be suppressed and the successful sintering of FGMs and mechanical properties could be successfully attained. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 46-51 マイクロアークを用いた表面溶融によるチタンの窒化 Nitriding of Titanium Surface by Micro-arc Melting 有田大,松浦清隆,工藤昌行/北海道大学宮本鉄生/大阪大学 Hiroshi Arita,Kiyotaka Matsuura,Masayuki Kudoh/Hokkaido University,Sapporo,Hokkaido 060-8628 JapanYoshinari Miyamoto/Osaka University, Ibaraki, Osaka 567-0047,Japan A surface of a titanium block was melted in an atmosphere of pure nitrogen using 3D Micro Welder that was designed by the present authors. The surface was nitrided to a depth of 90 to 260micro meters depending on the arc current of 6 to 24A. The concentration of nitrogen in the nitrided layer was approximately 50at% at the surface and it decreased as the distance from the surface increased. A TiN layer was formed at the surface, and beneath the TiN layer, a dual phase layer of TiN and alpha-Ti was formed. And the nitrided layer which has a depth of 130-260micro meters was obtained in a line. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 52-57 純チタンと歯科用貴金属合金のレーザー溶接 Laser welding of titanium and dental precious alloys 岩崎佳治,大川昭治,赤坂司,宇尾基弘,亘理文夫/北大院・歯・理工 Kenji IWASAKI,Shoji OHKAWA,Thukasa AKASAKA, Motohiro UO,Fumio WATARI/Hokkaido University, Graduate School of Dental Medicine. Sapporo, Hokkaido, Japan We examined performance of laser welding between titanium and two dental alloys of Ag-Pd-Cu-Au and Au-Pd-Pt. Design of the weld was but joint with and without groove weld, using filler materials of Ti and Au-Pt-Ru. Tensile breaking loads and hardness of joining part welds were measured. Microstructures and fractures surfaces of the welds were observed. Elemental distribution of the welds was analyzed by a EPMA. Tensile fracture force of welds of dissimilar metals without groove weld was lower than ones of welds between the similar metal. That was because there were welding cracks and elemental heterogeneousness in the welds. But the fracture forces of dissimilar metals-welds increased by the groove weld. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 58-63 3次元マイクロ溶接によるTi系材料の自由造形に関する研究 Study on Freeform Fabrication of Titanium Metal System by 3-Dimensional Micro Welding 寺久保匡志,桐原聡秀,宮本鉄生/阪大接合研松浦清隆,工藤昌行/北大・工 Masayuki TERAKUBO, Soshu KIMIHARA, Yoshinari MIYAMOTO/Osaka University, Joining and Welding Research Institute, Ibaraki, Osaka, JapanKiyotaka MATSUURA,Masayuki KUDOH/Hokkaido University,Sapporo,Hokkaido,Japan 3-Dimensional Micro Welding was developed as a new freeform fabrication method of refractory metals, alloys and intermetallics which is a combined processing TIG welding and rapid prototyping. The preliminary freeforming of titanium metal system was investigated. Titanium beads were formed by discharging micro arc beam to the tip of a titanium wire which was fed automatically under computer control. Each bead was joined well to the titanium substrate except for microcracks of about 20-micro meter in length appeared at the edge part of bead near the interface. Grid patterns of titanium beads and pin objects were successfully fabricated using the automatic control program. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 64-68 All-in-One Adhesiveにおける象牙質接着海面の形態学的解析 Morphological Analyses of the Bonding Interaction Zone in All-in-One Adhesives 吉田英史,宇野滋,堀稔,野田坂佳伸,加我正行/北大院・歯 Eiji YOSHIDA,Shigeru UNO, Minoru HORI, Yoshinobu NODASAKA, Masayuki KAGA/Hokkaido University, Graduate School of Dental Medicine, Sapporo, Hokkaido, Japan Objective: To evaluate the effect of difference of curing lamps on quality of the composite-to-dentin adhesion mediated with all-in-one adhesive systems. Materials and Methods: AQ Bond Plus(AQP: Sun Medical) and i Bond(iB: Heraeus-Kulzer) were used for all-in-one systems as well as Linerbond two sigma(LB: Kuraray) for a reference. Irradiation condition to the adhesives were the instructed period with a Halogen lamp(HL: Optilux 501), and 30 or 60 sec with a blue LED lamp(LED: Radius). Microhardness of the adhesives polymerized on the flat dentin surfaces(MH) was measured immediately after polymerization by an indentation method, n=5 for each condition. Microtensile bond strength to flat human dentin(MTBS) was also measured after 24-hours' storage in water. The debonded surfaces were observed in SEM to access the quality of the bonding interfaces. Results and Discussion: For AQP and iB, both MH and MTBS generated with LED were lower than those with HL. For LB, however, there was no influence of the irradiation conditions on MH and MTBS. SEM observation revealed that the hybrid zone was poorly polymerized when the adhesives were cured with LED. These findings suggested that two all-in-one adhesives used might contain some photo-initiators which could not excite with LED. Poor polymerization of the adhesive results in the instable bonding interface. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 69-74 rhBMP-2の培養ヒト歯髄細胞から象牙芽細胞への分化に対する影響 Effects of rhBMP-2 on differentiation of human dental pulp cells into odontoblasts 小川真史,小林文人,斎藤隆史/北医療大・歯別所和久/京大・医 Masafumi OGAWA, Fumito KOBAYASHI, Takashi SAITO/Health Sciences University of Hokkaido, School of Dentistry, Tobetsu, Hokkaido, JapanKazuhisa BESSHO/Kyoto University, Graduate School of Medicine, Kyoto, Japan Biological reconstruction of lost substance of teeth by carieses is one of final object in dental domain. Recently, reconstruction of bone and teeth with tissue engineering has been drawn attention. As the material that promotes forming hard tissue passively, BMP is given. The purpose of this study is to analyze the ability that BMP promote the differentiation from dental pulp cells to odontoblasts. To investigate the ability of BMP for differentiation, we observed cell's shape and measured the number and ALP activity of cells. Further, after cells reached confluent, rhBMP-2 at concentration of 0, 10, 100, 1000 ng/ml was added to the cells with serum-free medium. We collected the cells and examined the expression of mRNAs related to the formation of dentin by a quantitative PCR method using LightCycler. There was few difference in the number and shape of the cells between the group BMP added and BMP-free, but the group BMP added indicated more than twice of the value of ALP activity compared with that of BMP-free.rhBMP-2 promoted the expression of mRNAs related to the formation of dentin by a quantitative PCR method using LightCycler. These results show that rhBMP-2 has a possibility for the promotion of differentiation of human dental pulp cells into odontoblasts. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 75-80 数値計算力学によるバイオマテリアルの傾斜機能の評価 Modeling Simulation of Graded Function in Biomaterials 浅岡憲三/徳島大・歯 Kenzo ASAOKA/The University of Tokushima, School of Dentistry, Tokushima, Japan Modeling simulation was applied to estimate the service life of dental titanium implant. Retrieved pure titanium screw in the dental implant system was analyzed by fractography technique. The change that took place in the microstructure during function in oral cavity was examined. It was reasonable to suspect whether hydrogen absorption is the most essential factor on delayed fracture of the broken screw, that is, grain refinement layer by hydrogen absorption was observed. The thickness of the hydride layer was about 100 micro meters. Theoretical distributions of the hydrogen concentration were computed for an infinite cylinder model using Fick's differential equation, and compared with the thickness of the hydride layer in retrieved screw. Diffusion constant of hydrogen in titanium was estimated. The process of fracture formation in a biological environment was discussed. The absorbed hydrogen is suspected to be from hydrogen ion in biological fluid, by galvanic current and by repassivation of titanium oxide surface film for abrasion. It is concluded that modeling simulation is helpful in understanding of delayed fracture of medical titanium devices. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 81-86 細孔反応法で作製した繊維強化複合材料における繊維/母相間の組織傾斜 Graded Microstructure at Fiber/Matrix Interface in FRM Fabricated by the Reaction at Narrow Holes Method 渡辺義見/信州大学・繊維学部後藤岳志/信州大学大学院生・工業系研究科 Yoshimi WATANABE/Shinsyu University, Faculty of Textile Science and Technology, Ueda, Nagano, JapanTakeshi GOTO/Shinsyu University,Graduate School of Science and Technology,Ueda, Nagano, Japan A nickel-aluminides fiber/nickel composite was fabricated by the reaction at narrow holes(RANH) method, which is a novel method to fabricate an intermetallic compound fiber/metal matrix composite. Narrow holes were drilled in the nickel matrix, and then metal aluminum fibers were inserted into these holes. The specimens were heated at 800-1200 deg.C. in an argon atmosphere to obtain molten aluminum in the holes. Then the reaction of mNi+nAl -> NimAln should be caused in the narrow holes. During the reaction, the aluminum maintaining its fiber shape surrounded by the nickel matrix was replaced by intermetallic compound of NimAln, so that graded microstructure was formed at fiber/matrix interface. For the specimens heat-treated at 1200 deg.C, the hardness was gradually distributed, although for the specimens heat-treated at 1000 deg.C, stepwise hardness profiles were found. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 87-92 乳化溶剤蒸発法による生分解性高分子微粒子形成のメカニズム Mechanism of biodegradable polymer microparticle formation by emulsification solvent evaporation method Iossif Daniel ROSCA/Department of Polymer Science, Polytechnic University Bucharest, RomaniaFumio WATARI, Motohiro UO, Tsukasa AKASAKA,Kazuchika TAMURA/Hokkaido University, Graduate School of Dental Medicine, Sapporo, Hokkaido, Japan Iossif Daniel ROSCA/Department of Polymer Science, Polytechnic University Bucharest, RomaniaFumio WATARI, Motohiro UO, Tsukasa AKASAKA,Kazuchika TAMURA/Hokkaido University, Graduate School of Dental Medicine, Sapporo, Hokkaido, Japan This study elucidates different aspects of microparticle formation and encapsulation mechanism in single emulsion solvent evaporation method through observing the transformation of the initial microdroplet into the final hard microparticle by optical microscopy and laser diffractometry. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 93-98 天然機能性材料のイオン応答性ゲル化を利用した除法性液剤の開発 Development of sustained release liquid dosage forms using anionic responsible gelation of natural functional materials 久保亘,　渡辺秀樹,　宮崎正三/北海道医療大・薬David Attwood/マンチェスター大・薬 Wataru KUBO, Hideki WATANABE, Shozo MIYAZAKI/Health Science University of Hokkaido, Faculty of Pharmaceutical Sciences, Ishikari Thobetsu, Hokkaido, JapanDavid ATTWOOD/University of Manchester, School of Pharmacy and Pharmaceutical Sciences, Manchester, UK The purpose of this study was to evaluate the potential for the oral sustained delivery of paracetamol(acetaminophen) of two formulations with in situ gelling properties. Oral administration of aqueous solutions of either gellan gum(1.0%w/v) or sodium alginate(1.5%w/v) containing calcium ions in complexed form resulted in the formation of gel depots in rabbit stomachs as a consequence of the release of the calcium ions in the acidic environment. In vitro studies demonstrated diffusion-controlled release of paracetamol from the gels over a period of 6h. The bioavailability of paracetamol from the gels formed in situ in the stomachs of rabbits following oral administration of the liquid formulations was similar to that of a commercially available suspension. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 99-104 酸化物磁性ナノ粒子の合成と医療応用の検討 Synthesis and Medical Applications of Oxide Magnetic Nanoparticles 渥美崇,B.ジャヤデワン,田路和幸/東北院・環境 Takashi ATSUMI, Balachandran JAYADEVAN, Kazuyuki TOHJI/TOHOKU University, Graduate School of Environmental Studies, Sendai, Miyagi, Japan It is considered that magnetic nanoparticles, such as magnetite could be used for biomedical applications. Actually, magnetite particles are being used as a contrast medium in magnetic resonance imaging, in the hyperthermia treatment of cancer and in drug delivery. Magnetite beads are used for the purification of DNA or virus. The size and size distribution of magnetic nanoparticles are very important factors for the biomedical applications. We have synthesized Fe3O4 particles, with the average size of 10 and 40nm, by using the coprecipitation process. To synthesize particles larger than 40nm oxidation method is considered. Using the oxidation method, we have successfully synthesized CoFe2O4 particles with a good control over particle size in the range of 15 to 110nm. This expertise will be used to prepare magnetite particles with average sizes larger than 40nm. The application of 40nm magnetite particles for the development of a new type of sentinel lymph node detection technique is also reported. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 105-110 アメロゲニンの骨髄細胞の分化に対する影響 Effects of Amelogenin on Differentiation of Bone Marrow Cells 泉川昌宣,　小川真史,　豊田将吾,　小池俊之,　小林文人,　斎藤隆史/北医療大・歯 Masanobu Izumikawa, Masafumi Ogawa, Shogo Toyota, Toshiyuki Koike, Fimito Kobayashi, Takashi Saito/Department of Oprative Dentistry and Endodontology, School of Dentistry, Health Sciences University of Hokkaido, Tobetu, Hokkaido, Japan The purpose of this study was to examine the effects of amelogenin on differentiation of bone marrow stromal cells including multipotent cells, to clarify the usefulness of stromal cells and amelogenin, enamel matrix protein, in tissue engineering. Bone marrow stromal cells were isolated from 7 week-old F344 rat femur by following the method of Maniatopoulos et al. The cells were srimulated by amelogenin (0, 10, 100 and 1000ng/ml). Quantitative RT-PCR was performed with LightCycler (Roche Diagnostics, Germany) using the double-stranded DNA dye SYBR Green I to examin the mRNA levels, BMP-2, BMP-4, osteonectin(ONN), osteopontin(OPN), osteocalcin(OCN), Type I collagen, dentin matrix protein-1(DMP-1), and dentin sialophosphoprotein(DSPP). Amelogenin of 100ng/ml up-regulated mRNA expressions of BMP-4, and OCN, and DSPP compared with the control. Amelogenin of 1000ng/ml up-regulated mRNA expressions of BMP-2, ONN, amelogenin of 1000ng/ml, up-regulated mRNA expressions of OPN, Type I collagen and DMP-1. ALPase activity was enhanced by amelogenin of 100ng/ml. Some nodules observed in the cultured cells with amelogenin of 100ng/ml was stained by von Kossa at Day-11. In this study, it was suggested that amelogenin differentiated stromal marrow cells into osteo- or dentino-genetic cells. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 111-115 絹繊維への水酸アパタイト被覆 Hydroxyapatite Coating on Silk Fabric 平井伸治,　嶋影和宜/室工大・工横井慎也/室工大・院（現,　トステム（株））玉田靖/農業生物資源研究所 Shinji HIRAI, Kazuyoshi SHIMAKAGE/Muroran Institute of Technology, Department of Materials Science and Engineering, Muroran, JapanShinya YOKOI/Muroran Institute of Technology, Graduate Student, Muroran, JapanYasushi TAMADA/National Institute of Agrobiological Science, Tsukuba, Japan Hydroxyapatite coatings on silk fabric were attempted by a sol-gel process combined with ultraviolet(UV) irradiation at ambient temperature after dipping/withdrawing a substrate into/from the sol.The sol-gel coated silk fabric had low cytotoxicity which was similar to uncoated silk fabric. In addition, Though the sol-gel coated silk fabric had lower cell adhesion of mouse fibroblast than uncoated silk fabric, its adhesion was improved by the autoclave sterilization. The coating on silk fabric induces bonelike apatite formation onto its surface from a simulated body fluid. The wound healing effect of sol-gel coated silk fabric as wound dressing were similar to that of commercial silicon gauze. As the results of blood coagulation test if sol-gel coated silk fabric using rat plasma, activated partial thromboplastin time(APTT) tended to shorten without shortening prothrombin time(PT). Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 116-121 糖鎖によるカーボンナノチューブの表面修飾 Carbohydrate Coating of Carbon Nanotubes 赤坂司,亘理文夫/北大院・歯佐藤義倫,田路和幸/東北大・環境科学 Tsukasa AKASAKA, Fumio WATARI/Hokkaido University, Graduate School of Dental Medicine, Sapporo, Hokkaido, JapanYoshinori SATO, Kazuyuki TOHJI/Tohoku, Graduate School of Environmental Studies, Sendai, Miyagi, Japan We have demonstrated that multi-walled carbon nanotubes(MWCNTs) coated with a carbohydrate-carrying polymer for use as biological recognition signaling molecile can be easily prepared by a non-covalent method via hydrophobic interactions. Fluorescence observation by confocal laser scanning microscopy showed that the carbohydrate-carrying polymer was uniformly and densely localized along needle shape of the MWCNT. To evaluate biological recognition affinity, interactions of the MWCNT with lectins were examined by binding tests. The resultant MWCNT was found to acquire a selective binding affinity to the corresponding lectin without a nonspecific interaction. On the other hand, a bare MWCNT nonspecifically interacted with lectins. These results showed that a MWCNT coated with a carbohydrate-carrying polymer has biological recognition signals. Modification of a CNT with various carbohydrate chains will be a useful protocol for molecular designs of biomaterials, nanoarchitecture, and biosensors. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 122-126 液中基盤加熱法によりチタン基板上に形成したHA薄膜の構造と溶解性 Structure and Dissolution Behavior of the HA Thin Formed on Ti Substrate by Thermally Induced Liquid-Phase Deposition Method 遠藤一彦,大野弘機/北医療大・歯田村誠/北医療大・医療科学センター Kazuhiko ENDO, Hiroki OHNO/Health Sciences University of Hokkaido, School of Dentistry, Ishikari-Tobetsu, Hokkaido, JapanMakoto TAMURA/Health Sciences University of Hokkaido, Institute of Medical Science, Sapporo, Hokkaido, Japan Thermally induced liquid-phase deposition method was employed to produce a crystalline hydroxyapatite (HA) film on titanium substrate in metastable calcium phosphate solution. A 100*10*0.02 mm**3 titanium foil was employed as a substrate. Prior to HA coating, the substrate was immersed in 5M NaOH solution at 60 deg.C for 24 h. The temperature of the substrate was kept constant at 60 deg.C for 3 h by electrically heated with DC power souce in the solution. The X-ray deffractogram indicated that the deposited film on the titanium substrate was composed of HA. The thickness of the HA coatings was approximately 7 micro meter. In a saline solution (pH5.8), the deposited HA gradually dissolved and pH of the solution increased due to the released hydroxyl ions and phosphate ions. These results suggest that a HA film may play an important role in enhancement of bone formation around the implant. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 127-132 X線分析顕微鏡の生体内金属材料及び周囲組織分析への応用 Application of X-ray Scanning Analytical Microscope for the Analysis of Tissue Implanted Metals and Surrounding Tissues 宇尾基弘,赤坂司,Rosca Iosif Daniel,亘理文夫/北大院・歯学研究科・歯科理工学講座 Motohiro UO, Tsukasa AKASAKA, Rosca Iosif DANIEL, Fumio WATARI/Hokkaido University, Sapporo, Hokkaido, Japan The soft tissue implanted with various metals were investigated with X-ray scaning analytical microscope(XSAM) and compared with histlogical observation. The clear dissolution images of Ni was obtained with XSAM and the severe tissue damage was observed in the dissolved areas. In comparison with electron-probe micro analysis(EPMA), XSAM provided clearer mapping images for heavier elements. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 133-138 ハイドロタルサイト－バイオナノハイブリッドの合成 Syntheses of Bio-nanohybridized Hydrotalcite 千葉淳,武田隆史,田村紘基,吉川信一/北大院・工 Jun CHIBA, Takashi TAKADA, Hiroki TAMURA, Shinichi KIKKAWA/Graduatedd School of Engineering, Hokkaido University, Sapporo 060-8628, Japan. Adenosine triphosphate(ATP) intercalated hydrotalcite was obtained by two preparation methods; the anion exchange reaction of hydortalcite with nitrate ions in the interlayer(LDH-NO3) and the coprecipitation of mixed magnesium and aluminum hydroxide in the presence of ATP. Layer stacking was less perfect in the latter product than the former in spite of the comparable amounts of intercalated ATP. Green fluorescent protein was also introduced into hydrotalcite. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 139-144 銀粉末を含む電気伝導性皮膜及び絶縁性高分子膜に覆われたNafionゲルの機械的性質 Mechanical Performance of Nafion Gels Coated with an Electrically Conductive and a Polymeric Insulating Composite 玉川浩久,野方文雄/岐阜大・工学部 Hirohisa TAMAGAWA, Fumio NOGATA/Depertment of Human and Information Systems, Faculty of Engneering, Gifu University, Japan Nafion has been known for its exhibition of rapid and large bending upon applying low voltage such as 1V. It shows possibility of development of a practical Nafion actuator, but its realization is found to be difficult so far. There are some serious defficultied to reach that goal. About Nafion, especially (i) low force generation and (ii) low durability are the typical problems to be overcome. The generated force can be improved to some extent by, forming thicker metal plating layers on both the surfaces of Nafion. However, the metal plating layers are easy to come off from the Nafion surfaces, so the durability of such Nafion is not enough. To overcome these difficulties, the electrically conductive and insulating polymer coatings were applied on the Nafion surfaces and the investigation on its mechanical characteristics was conducted. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 145-150 磁性流体とPVAによるソフトアクチュエータの基礎研究 Fundamental study of soft actuator with magnetic fluid and PVA 坂東幹生,小島洋一郎,見藤歩,蘇武栄治,田島勲/苫小牧工業高等専門学校 Mikio BANDO, Yohichiro KOJIMA, Ayumi MITOH, Eiji SOBU and isao TAJIMA/Tomakomai National College of Technology, Tomakomai, Hokkaido, Japan This paper deals with a kind of actuator consisting of polyvinyl alcohol(PVA) gel mixed with a magnetic fluid and is called as a soft actuator. In this research, 5% PVA gel was produced and the characteristics of the soft actuator were measured against static magnetic field, load, repetition response and response speed. The soft actuator was able to raise and lower weights from 10 to 100g. Now we are trying to apply this actuator, for development of a peristalsis pump. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 151-156 酸化チタン傾斜機能タイルの製作 Production of titanium dioxie functionally graded tile 鈴木秀幸,内田敬久,内田悦行,林二一/愛知工大・工 Hideyuki SUZUKI, Yoshihisa UCHIDA, Yoshiyuki UCHIDA, Niichi HAYASHI/Aichi Institute of Technology, Toyota, Aichi, Japan Development of TiO2-kaolin functionally graded material(FGM) which has photocatalytic effect with high bending strength has been reported. To improve the mechanical properties, Korean kaolin was selected as a binder. The FGMs were manufactured by a progressive lamination method using vacuum filtration. By this method, it is easy to control the thickness of the FGM. The results showed that the photocatalytic effect was found to drop drastically at 900 deg.C, since crystalline changes from anatase type to rutile type at more than 900 deg.C. High photocatalytic effect was observed at 0.1 MPa compression pressure. However, a bending strength of the FM increased with increasing compression pressure. Therefore, it is necessary to optimize the manufacturing conditions. Based on the optimal design of conditions, the FGM was developed for air purification. This FGM has high photocatalytic effect with good mechanical properties, such as 15% NOx reduction efficiency without defect in the material. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 157-162 単層カーボンナノチューブ焼結体の機械的特性に及ぼす不純物の影響 Effect of Impurities on Mechanical Properties of SWNT Solids Prepared by Spark Plasma Sintering 山本剛,高橋亨,橋田俊之/東北大・工大坪誠,佐藤義倫,田路和幸/東北大・環境大森守/東北大・金研 Go YAMAMOTO, Toru TAKAHASHI, Toshiyuki HASHIDA /Fracture Research Institute, Tohoku University, Sendai 980-8579, JapanMakoto OHTSUBO, Yoshinori SATO, Kazuyuki TOHJI /Graduate School of Environmental studies, Tohoku University, Sendai 980-8579, JapanMamoru OHMORI /Institute for Materials Research, Tohoku University, Sendai 980-8579, Japan In this paper, a spark plasma sintering(SPS) method was employed to solidify single-walled carbon nanotubes(SWNTs) only, and the effect of impurities on the mechanical properties of the SWNT solids was examined using a small punch(SP) testing method. The SWNTs were prepared by an arc discharge method, and then purified using oxidation and chemical processes. The compaction pressure and the temoerature used in the SPS method were 120MPa, and 1000deg.C, respectively. It was shown that the SWNT solids produced from the purified SWNTs gave higher fracture strength compared to the one prepared from the raw-soot(nearly 33MPa), with the maximum strength value being 47MPa. On the other hand, the Young' modulus was insensitive to the purification process. SEM, XRD and Raman spectroscopy cbservations indicated that the raw-soot included lager amount of the impurities such as metal particles and amorphous carbon than that for the purified SWNTs. Thus, the purification and removal of the impurities are expected to be effective for improving the fracture strength property of SWNT solids. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 163-166 マイクロアークを用いた表面溶融によるニオブの窒化 Nitriding of Niobium Surface by Micro-arc Melting 高橋孝一,松浦清隆,工藤昌行/北海道大学宮本欽生/大阪大学 Koichi Takahashi, Kiyotaka Matsuura, Masayuki Kudoh / Hokkaido University, Sapporo, Hokkaido 060-8628, JapanYoshinari Miyamoto / Osaka University, Ibaraki, Osaka 567-0047, Japan A surface of a niobium plate was melted using a metal arc heat source in an atmosphere of pure nitrogen in order to nitride the surface. The melting depth of the niobium plate was approximately 60 micro meter when an arc current was 24A. A thin continuous Nb2N layer was formed on the surface of the melted part, and beneath the layer, fine Nb2N particles were dispersed in the melted part. The Vickers hardness was approximately 600 in the Nb2N layer and 350 to 450 in the Nb2N dispersed layer. Japanese 2003年度　傾斜機能材料論文集　＜FGM2003 in Sapporo＞　 Proceedings of the 15th Symposium on Functionally Gradient Materials 25 2004-07-15 167-172 コンポジットレジン修復と歯質接着の進歩 Current Progress of Dental Resin Composite and Tooth Adhesion 佐野英彦,井上哲,小城賢一/北海道大学大学院歯学研究科 Hidehiko Sano, Satoshi Inoue, Ken-ichi Koshiro / Hokkaido University, Graduate School of Dental Medicine, Sapporo, Japan The two fold of mechanism of tooth adhesion made it possible for clinical use of adhesive restorations within an oral environment. One of the mechanisms is chemical bonding between functional monomers and hydroxyapatite. This mechanism is very effective for enamel and dentin. The other is micromechanical interlocking. For enamel adhesion, combination of micromechanical interlocking and chemical adhesion works very well and provides durable bond in vivo. Dentin adhesion is still challenging because we have to rely on the relatively weak link between resin and collagen fibrils that degrades over time. Current progress of the self-etching technology that partially demineralizes superficial dentin and preserves hydroxyapatite crystals on the collagen fibrils has a potential to solve this problem. Current dentin adhesives employing self-etching technology create "Functionally Graded Material" at the adhesive interface confirming more durable and stronger bond than conventional dentin adhesives that create laminate structure between resin and dentin. Japanese