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A metallic chelate of ethylenediaminetetraacetic acid (EDTA) is usually represented as a discrete complex by coordination number (CN) 6. On the other hand, it has been elucidated in the cations of heavier group 14 elements (heavy tetrels) chelated by EDTA that they have various binding modes from monomeric structures to coordination polymers from X-ray crystallographic studies. Some of them were systematized in reviews; however, they uncover the whole heavy tetrels-EDTA complexes. Hence, the reported crystal structures of heavy tetrels-EDTA complexes with different counter cations and/or (pseudo)halogens, 3 of Ge(IV)-, 2 of Sn(II)-, 5 of Sn(IV)-, and 21 of Pb(IV)-EDTA (CN 5-8), are briefly summarized herein for showing a variety of bonding modes existing in the heavy tetrels-EDTA chelates., 長崎大学大学院工学研究科研究報告, 53(100), pp.55-62; 2023

Magnesium (Mg) has the lowest density among practical metals and has excellent specific stiffness and strength characteristics. Carbon nanotube (CNT) reinforced Mg matrix composites have been attracting much attention as an effective material composing light-weight structures in automobile and aerospace industries. However, CNT fibers tend to be intricately entangled with each other, which lead to exhibit unexpected low mechanical properties of the composites. In this study, CNT reinforced Mg composites have been fabricated using powder metallurgical techniques with spark plasma sintering (SPS) methods. CNTs have been subjected to ultrasonic treatment and mixed with fine powder of ZrO_2 to obtain uniform dispersion of CNTs in Mg matrix. In addition, metals with low melting points have been added to fill voids and cracks around CNTs. Three-point bending test results demonstrated that CNT/ Mg composites with both low melting point metal, Sn, and fine powders, ZrO_2, exhibited the highest maximum bending stresses among the composites and pure Mg. Flexural modulus have been also highly improved.

Since 2002, we have been researching and developing a method for generation EUV light by irradiating a tin droplet with a laser beam. We believe the double pulse lasers irradiation scheme, in which the droplet is irradiated with a pre-pulse laser beam and a pulse CO_2 laser beam, and the debris mitigation by magnetic field are keys for industrial EUV light source system. In our experimental tool, we have investigated and optimized the droplet behavior and observed effect of the double pulse lasers irradiation scheme. The double-pulse method can improve conversion efficiency by 3.7% by increasing ionization rate of the droplet (93%). The pulse CO_2 laser energy absorption rate into the droplet is 68% at optimized pre-pulse laser setting. Also the 98% of ions were captured by our mitigation technique. Our scheme is also tested on the proto type of the industrial system. No ion signal was observed by Faraday cup on the collector mirror. It is expected our scheme will achieve high power and long time operation in industrial use.

The purpose of this study is to find out the effect of thermal environmental improvement by solar insulating on the RC construction in Okinawa. Insulating paint becomes the insulating material of the temperature. The paint is a wall surface and the roof surface, setting is simple. It could be proposed as a good system which improved the indoor thermal environment on the existent houses. I compare the water save the cooling effect of the roof this time with the sprinkling. I want to clarify the effect. Water save, and there is a large number of presentation of the results of the study about the sprinkling effect. It is revealed that I lower load of the heat on the roof of the building. The paint which I used together with heat cover block from this experiment is effective. Water save and the sprinkling are heat cover block and about the same performance the water which they expected by water-cooled action. It became clear by this experiment. Water has enough, and calcium carbonate which is new material is s weak point of the sprinkling. It is the roof materials that can overcome hygiene and maintenance.

Anode properties of Sn films on macroporous (m-) metal films (Sn(N)/m-M films, N: condition of electrolytic deposition, S (10 mA cm-2, 2 min) or L (2 mA cm-2, 10 min), M: Co or Ni) for secondary lithium-ion batteries have been investigated. Sn(N)/m-M films were fabricated as follows. First, polymethylmethacrylate (PMMA) microspheres (ca. 800 nm in diameter) as a macropore template were stacked on a Cu foil by dip-coating. m-Co or m-Ni film was obtained after electrolytic deposition on the PMMA template film in a constituent metal sulfate aqueous solution and subsequent removal of PMMA microspheres in acetone. Thereafter, Sn was electrochemically deposited on m-Co or m-Ni at condition of S or L, and then it was heat-treated at 200℃ for 20 h in vacuo. First discharge capacity of 4 kinds of Sn(N)/m-M films obtained (550~750 mA h g-1) was lower than that of the pure Sn film without m-M (ca. 900 mA h g-1). However, charge-discharge characteristics of their anodes were drastically improved by the introduction of m-M, and the Sn(L)/m-Co film showed the largest discharge capacity (ca. 600 mA h g-1 even at 30th discharge) among the films tested., 長崎大学工学部研究報告 Vol.39(73), pp.8-14; 2009

金沢大学大学院自然科学研究科（工学系）, TiN and TiCN thin films are used as antiwear layer on parts such as metal cutting tools. It is reported that the thin films that are deposited ceramics and metals have preferred orientation, and that the residual stresses generate by the difference in the coefficients of thermal expansion between the thin films and the substrate. Tools coated with TiN and TiCN films are heated to high temperature during service due to the frictional heat. Under this condition, the texture and the residual stress should change due to the heat. In the material engineering, it is well known that the residual stress in the material affects the mechanical strength of the industrial products. The purpose of this study is to examine the effect of the residual stress on the mechanical strength of TiN and TiCN thin films having preferred orientation. In this study, speciments that are deposited TiN and TiCN respectively by Physical Vapor Deposition (PVD) were annealed in a furnace at temperature of 573K, 798K, 843K and 893K. Using X-ray diffraction technique, the crystallite orientation was evaluated by the pole figure and the crystallite orientation distribution function (ODF). The films exhibited {111} fiber texture. After that, the residual stress of thin films was measured using CoKα radiation with the two-exposure method at Ψ=39°and 75°. Since the relationship between the mechanical strength and the residual stress has not been revealed about the thin film materials, the effect of the residual stress on the mechanical strength of the TiN and TiCN thin films having preferred orientation was investigated by the dynamic hardness (DH) and the scratch test. As a result, although the ODF little changed due to the heat treatment, the residual compressive stress relaxed at higher temperatures than 573K. As for the hardness of thin films, the residual stress did not affect the hardness. However, the residual stress influenced the behavior of the scratch test. The abrasive wear and the micro cracks were decreased by highly residual compressive stress.

TiN-TiAl ceramics/intermetallic composites containing no additives were hot-pressed from a mixture of TiN, Ti and Al powders containing 5 up to 100massl%TiAl (5, 20, 40, 60, 80, 100mass%TiAl), which were formed from a reaction between Ti and Al. Hot-pressing was conducted at 1000℃ for 7.2 ks under a pressure of 13.9 MPa in an Ar gas atmosphere. The mechanical and electrical properties were examined as a function of compositional change from 5 to 100mass%TiAl. TiN-TiAl composites containing 60～100mass%TiAl had a relative density of 67.3～71.1%, bulk density of 2380～2830kg m^, Vickers hardness of 506～2771MPa, flexural strength of 50～123MPa, Young's modulus of 45.9～82.4GPa, and electrical conductivity of 606～778k S・m^. The sufficient densification was not necessarily performed because the reaction from Ti and Al to TiAl phase was not completed by the use of coase Ti and Al powders.

Ti-Al-N films were deposited using an activated reactive evaporation (ARE) method with single vapor source of Ti-Al alloys. Oxidation behaviors of Ti-Al-N films were investigated in dry air in the temperature range from 673K to 1173K. Oxidation layers of the films were characterized by XRD, EPMA, XPS and TEM. The results are summarized as follows. (1) The oxidation characteristics of Ti-Al-N films improved more than 200 degrees camparing that of TiN film and the oxidation resistance of Ti-Al-N films increase with an increase of Al content in the films. (2) Ti-Al-N films obtained by an ARE method had a cubic B1 structure. Ti atoms in the films were substituted by Al atoms. (3) TiN films changed directly to TiO_2 in high temperature oxidation and no Ti-O-N compounds were observed at the interface. (4) TiO_2 and Al_2O_3 compounds were observed after oxidation of the Ti-Al-N films and Ai_2O_3 enriched at the surface of the films. This is the reason that the Ti-Al-N films show a good resistance to the oxidation at the high temperature.

高純度かつ高品位の材料を得るためには、材料加工にとって試料と容器の濡れ性は、特に微小重力(マイクロG)環境下では、重要な因子である。SiO2容器への濡れ性に及ぼすSn、Ge、およびGaSb試料の精製処理による効果を1GおよびマイクロG環境下で検討した。処理は真空加熱、水素ガス中加熱および塩素ガス雰囲気中での加熱溶融を行った。試料と容器の濡れ挙動は精製処理の各種類ごとに変化した。(1)塩素ガス雰囲気中での加熱溶融は、Sn試料に対してSiO2容器への濡れ性を改善するのに効果があった。(2)Sn試料については、試料と容器の濡れ性は表面酸化物層の厚さと関連がある。(3)水素ガス雰囲気中での加熱はGeおよびGaSb試料に対する濡れ性を改善するのに効果があった。, A sample/container wettability is an important factor for material processing, especially in microgravity (micro-g) environment, to get high purity and high quality materials. The effect of refining treatment of Sn, Ge and GaSb samples on wettability to SiO2 container was investigated both in 1-g and micro-g environment. The treatments were heating in vacuum, heating in H2 gas and heating/melting in Cl2 gas atmosphere. The sample/container wetting behavior was changed for each kind of refining treatments. (1) The heating/melting in Cl2 gas atmosphere was effective to improve the wettability to SiO2 container for Sn sample. (2) The sample/container wettability was related to the thickness of the surface oxide layers for Sn sample. (3) The heating in H2 gas atmosphere was effective to improve the wettability for Ge and GaSb samples., 資料番号: AA0000741005, レポート番号: NASDA-TMR-960024

微小重力下における、濡れ挙動の温度依存性評価、および濡れ挙動におよぼす精製処理効果の確認のため、MU-300型機のパラボリックフライトによる航空機実験を行った。実験装置としては新たに設計製作したものを用いた。以下の結果が得られた。(1)Sn溶湯と石英容器では、マイクロg下での濡れ性の温度依存性は、地上の場合と同様にきわめて小さい。(2)精製処理の違いによるマイクロg下での濡れ挙動の変化を明確に確認した。(3)Cu溶湯の濡れ挙動を明確に観察できた。, In order to estimate temperature dependence of wettability, and to confirm effect of purification treatment on the wettability, microgravity experiments were conducted via parabolic flight of MU-300 aircraft. Experimental apparatus used was newly designed and constructed. The following results were obtained: (1) as on the ground, temperature dependence of wettability under micro g is very small for molten Sn and quartz wessel; (2) difference in wettability under micro g which is caused by that in purification treatment was clearly confirmed; and (3) wetting behavior of molten Cu was definitely observed., 資料番号: AA0000736005, レポート番号: NASDA-TMR-960019

高純度・高品質の材料処理において、材料と容器の濡れ性は、とくに微小重力(マイクロg)環境下では重要な因子である。Sn、Bi、Geの精製処理の、SiO2容器に対する濡れ性への効果について、1gおよびマイクロgの両環境下で実験調査を行った。酸(HCl)による原材料の前処理をして、真空下、H2およびCl2雰囲気中で処理を行った。精製処理の違いによる材料と容器の濡れ挙動に次のような差異が観察された。(1)SnおよびBiにおける材料と容器の濡れ挙動は表面酸化層の厚みに関係がある。(2)原材料の前処理は濡れ性改善に効果がある。(3)GeのCl2雰囲気中での濡れ挙動は温度(1,280-1,370K)の影響が、特にマイクロg環境下で大きい。宇宙実験に向けて、航空機実験による、材料と容器の各組み合わせにおける濡れ性改善のための最適精製処理条件のスクリーニングは重要である。, A sample/container wettability is an important factor for material processing, especially in microgravity (micro g) environment, to get high purity and high quality materials. The effect of refining treatment of Sn, Bi and Ge samples on wettability to SiO2 container was investigated both in 1 g and micro g environment. The treatments were conducted in vacuum, in H2 gas, and in Cl2 gas atmosphere including pretreatment of raw materials by acid (HCl). The sample/container wetting behavior was changed for each kind of refining treatments: (1) the sample/container wettability was related to the thickness of the surface oxide layers for Sn and Bi samples; (2) the pretreatment of raw materials was effective to improve the wettability; and (3) the wetting behavior of Ge sample in Cl2 gas atmosphere was depended on the temperature (1,280-1,370 K) especially in a micro g environment. For the experiments in space, it is important to screen the most suitable refining treatment for improvement of wettability for each combination of sample and container by aircraft experiments., 資料番号: AA0000738002, レポート番号: NASDA-TMR-960021

A TiN-Al_2O_3 composite powder was synthesized by the floating-type fluidized- bed CVD. Al_2O_3 particles were floated in an N_2/NH_3 gas mixture, and TiCl_4 was fed to deposit TiN. The composite powders obtained and the ceramics were examined by an electron probe microanalyzer (EPMA). The TiN content in the composite powder was controlled by the flow rate of carrier gas of TiCl_4. It was deduced that the composite powder was formed by deposition of fine TiN particles onto Al_2O_3 particle surfaces, aggregating to about 3μm. Ceramic from the composite powder containing 12.5 wt% TiN was conductive. Its microstructure suggested that TiN was uniformly dispersed as compared with mechanical mixing.