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報告書

溶融鉛ビスマス共晶合金中における9Cr-1Mo鋼の腐食抑制のための適切な酸素濃度の検討

小松 篤史

JAEA-Research 2021-019, 24 Pages, 2022/05

JAEA-Research-2021-019.pdf:1.53MB

溶融鉛ビスマス共晶合金(LBE)中における材料の腐食速度を低減するには、酸素濃度を調整することが重要とされており、過去の報告を見ると約10$$^{-7}$$$$sim$$10$$^{-5}$$wt%程度に酸素濃度を調整していることが多い。しかし、どの程度の濃度が最適と明言されているわけではなく、この濃度範囲内であっても激しく腐食したとの報告もある。本研究では9Cr-1Mo鋼を例にとり、酸化被膜中およびLBE中の拡散を考慮した腐食モデルを作成し、腐食モデルから推定される腐食抑制策について検討を行った。また、LBE中における9Cr-1Mo鋼の腐食を低減しつつ、流れのあるループ環境における低温部での流路閉塞を防止するための最適酸素濃度の算出を試みた。その結果、LBE中における9Cr-1Mo鋼の腐食形態は、酸化被膜厚さと拡散層厚さの比や、LBE中の鉄濃度、温度等により変化し、その成膜挙動から、緻密被膜生成、沈殿被膜生成、被膜溶解の三つに分類した。腐食を抑制するには、緻密被膜生成条件を維持できるように酸素濃度を調整することが重要であり、そのためにはLBEに浸漬する前に10$$^{-7}$$m程度以上の予備酸化被膜をつける必要がある。従来報告でよく用いられる約10$$^{-7}$$$$sim$$10$$^{-5}$$wt%という酸素濃度は、酸化被膜がある程度成長した場合の最適酸素濃度であり、被膜が薄い場合は、より高い酸素濃度が必要になると推察された。

論文

Steam oxidation of silicon carbide at high temperatures for the application as accident tolerant fuel cladding, an overview

Pham, V. H.; 倉田 正輝; Steinbrueck, M.*

Thermo (Internet), 1(2), p.151 - 167, 2021/09

Since the nuclear accident at Fukushima Daiichi Nuclear Power Station in 2011, a considerable number of studies have been conducted to develop accident tolerant fuel (ATF) claddings for safety enhancement of light water reactors. Among many potential ATF claddings, silicon carbide is one of the most promising candidates with many superior features suitable for nuclear applications. In spite of many potential benefits of SiC cladding, there are some concerns over the oxidation/corrosion resistance of the cladding, especially at extreme temperatures (up to 2000$$^{circ}$$C) in severe accidents. However, the study of SiC steam oxidation in conventional test facilities in water vapor atmospheres at temperatures above 1600$$^{circ}$$C is very challenging. In recent years, several efforts have been made to modify existing or to develop new advanced test facilities to perform material oxidation tests in steam environments typical of severe accident conditions. In this article, the authors outline the features of SiC oxidation/corrosion at high temperatures, as well as the developments of advanced test facilities in their laboratories, and, finally, give some of the current advances in understanding based on recent data obtained from those advanced test facilities.

論文

Oxidation kinetics of silicon carbide in steam at temperature range of 1400 to 1800$$^{circ}$$C studied by laser heating

Pham, V. H.; 永江 勇二; 倉田 正輝; Bottomley, D.; 古本 健一郎*

Journal of Nuclear Materials, 529, p.151939_1 - 151939_8, 2020/02

AA2019-0197.pdf:1.61MB

 被引用回数:7 パーセンタイル:81.95(Materials Science, Multidisciplinary)

As expected for accident tolerant fuels, investigation of steam oxidation for silicon carbide under the conditions beyond design basis accident scenarios is needed. Many studies focused on steam oxidation of SiC at temperatures up 1600$$^{circ}$$C have been conducted and reported in the literature. However, behavior of SiC in steam at temperatures above 1600$$^{circ}$$C still remains unclear. To complete this task, we have designed and manufactured a laser heating facility for steam oxidation at extreme temperatures. With the facility, we report the first results on the steam oxidation behavior of SiC at temperatures range of 1400-1800$$^{circ}$$C for short term exposure of 1-7 h under atmospheric pressure. Based on the mass change of SiC samples, parabolic oxidation rate and linear volatilization rate were calculated. The oxidation layer appears to be maintained at 1800$$^{circ}$$C in steam, but the bubble formation phenomenon suggests other volatilization reactions may limit its life.

論文

Oxidation of silicon carbide in steam studied by laser heating

Pham, V. H.; 永江 勇二; 倉田 正輝; 古本 健一郎*; 佐藤 寿樹*; 石橋 良*; 山下 真一郎

Proceedings of International Nuclear Fuel Cycle Conference / Light Water Reactor Fuel Performance Conference (Global/Top Fuel 2019) (USB Flash Drive), p.670 - 674, 2019/09

Silicon carbide (SiC) has recently attracted much attention as a potential material for accident tolerant fuel cladding. To investigate the performance of SiC in severe accident conditions, study of steam oxidation at high temperatures is necessary. However, the study focusing on steam oxidation of SiC at temperatures above 1600$$^{circ}$$C is still certainly limited due to lack of test facilities. With the extreme oxidation/corrosion environment in steam at high temperatures, current refractory materials such as alumina and zirconia would not survive during the tests. Application of laser heating technique could be a great solution for this problem. Using laser heating technique, we can localize the heat and focus them on the test sample only. In this study, we developed a laser heating facility to investigate high-temperature oxidation of SiC in steam at temperature range of 1400-1800$$^{circ}$$C for 1-7 h. The oxidation kinetics is then being studied based on the weight gain and observation on cross-sectioned surface of tested sample using field emission scanning electron microscope. Off-gas measurement of hydrogen (H$$_{2}$$) and carbon monoxide (CO) generated during the test is also being conducted via a sensor gas chromatography. Current results showed that the SiC sample experienced a mass loss process which obeyed paralinear laws. Parabolic oxidation rate constant and linear volatilization rate constant of the process were calculated from the mass change of the samples. The apparent activation energy of the parabolic oxidation process was calculated to be 85 kJ.mol$$^{-1}$$. The data of the study also indicated that the mass change of SiC under the investigated conditions reached to its steady stage where hydrogen generation became stable. Above 1800$$^{circ}$$C, a unique bubble formation on sample surface was recorded.

論文

Effect of re-oxidation rate of additive cations on corrosion rate of stainless steel in boiling nitric acid solution

入澤 恵理子; 山本 正弘; 加藤 千明; 本岡 隆文; 伴 康俊

Journal of Nuclear Science and Technology, 56(4), p.337 - 344, 2019/04

 被引用回数:0 パーセンタイル:0.01(Nuclear Science & Technology)

The boiling nitric acid solution containing highly oxidizing cations dissolved from the spent nuclear fuels corrodes stainless steels because of the nobler corrosion potential and their fast reduction rate. The cations themselves are re-oxidized to higher oxidizing states in a bulk solution after the corrosion reaction. In this paper, the re-oxidation rate constants of typical cations, such as Cr, V, Pu, and Np, were analyzed, and discussed about the effect on time dependencies of the corrosion rate. It was indicated that the cations with a large re-oxidation rate constant, such as Np, could keep the corrosion rate at high level continuously for the long immersion duration.

論文

Improvements in drill-core headspace gas analysis for samples from microbially active depths

宮川 和也; 奥村 文章*

Geofluids, 2018, p.2436814_1 - 2436814_11, 2018/10

 被引用回数:2 パーセンタイル:12.26(Geochemistry & Geophysics)

地下深部の炭化水素ガスの濃度組成や同位体組成を調べる事により、炭化水素ガスの起源や長期的な流体移動に関する知見が得られる。地上からのボーリング孔を用いてガス採取を行う場合によく用いられる方法として、ボーリングのカッティングスあるいはコアに吸着したガスをサンプル容器のヘッドスペースに追い出して分析する方法がある。しかしながら、この方法により得られた結果は、しばしば大きなばらつきを示す。本研究では、上述の手法により採取・分析した結果を、地下施設を利用して得られた結果と比較し、ばらつきの原因が試料の採取・保管方法に起因することを明らかにし、正しい値を得るための要点を指摘した。

論文

Oxidation and reduction behaviors of a prototypic MgO-PuO$$_{2-x}$$ inert matrix fuel

三輪 周平; 逢坂 正彦

Journal of Nuclear Materials, 487, p.1 - 4, 2017/04

 被引用回数:4 パーセンタイル:45.14(Materials Science, Multidisciplinary)

MgOを母材としたPuO$$_{2-x}$$含有イナートマトリックス原型燃料の酸化還元挙動を熱分析により調べ、MgO-PuO$$_{2-x}$$試料の酸化還元速度を実験的に決定した。MgO-PuO$$_{2-x}$$試料の酸化還元速度はPuO$$_{2-x}$$試料に比べ低くなった。また、高い酸素分圧条件において、MgO-PuO$$_{2-x}$$試料の定比からのO/Pu比の変化はPuO$$_{2-x}$$試料に比べ小さくなることがわかった。これより、MgOを母材にすることによりイナートマトリックス燃料からの酸素供給及び放出が抑制されることがわかり、被覆管酸化等の観点で懸念となる高い酸素ポテンシャルを有するマイナーアクチニド酸化物の母材としてMgOが有効であることがわかった。

論文

Corrosion test of HTGR graphite with SiC coating

Chikhray, Y.*; Kulsartov, T.*; Shestakov, V.*; Kenzhina, I.*; Askerbekov, S.*; 角田 淳弥; 植田 祥平; 柴田 大受; 坂場 成昭; Abdullin, Kh.*; et al.

Proceedings of 8th International Topical Meeting on High Temperature Reactor Technology (HTR 2016) (CD-ROM), p.572 - 577, 2016/11

高温ガス炉(HTGR)に用いられる黒鉛について、耐腐食性を有するSiC被覆の適用は重要な課題である。本研究は、高密度のIG-110黒鉛にSiCを傾斜被覆した材料について、1673Kまでの温度で蒸気との化学反応の結果を示したものである。100Paの蒸気との反応に関する実験では、SiC酸化のパッシブ反応により表面にSiO$$_{2}$$膜が形成されることを確認した。また、1Paの蒸気とのアクティブ反応では、表面に様々なカーボン複合材が形成されることを確認した。

論文

In situ X-ray diffraction study of the oxide formed on alloy 600 in borated and lithiated high-temperature water

渡邉 真史*; 米澤 利夫*; 菖蒲 敬久; 城 鮎美; 庄子 哲雄*

Corrosion, 72(9), p.1155 - 1169, 2016/09

 被引用回数:0 パーセンタイル:0.01(Materials Science, Multidisciplinary)

In situ X-ray diffraction (XRD) measurements of the oxide film formed on Alloy 600 in borated and lithiated high-temperature water were conducted to demonstrate a capability to investigate rapid changes in oxide films during transient water chemistry conditions. In the presence of dissolved hydrogen (DH) = 30 cm$$^{3}$$/kg [H$$_{2}$$O] and dissolved oxygen (DO) $$<$$ 0.06 ppm, only spinel oxides were detected and no significant NiO peak was found even after 1,220 h exposure. By contrast, once the DO was increased to 8 ppm, a NiO peak grew rapidly. Within 7 h, the amount of NiO became comparable to that of spinel oxide. However, when DO was decreased again below 0.3 ppm and DH was increased up to 30 cm$$^{3}$$/kg [H$$_{2}$$O], the ratio of NiO to spinel did not change during 10 h. Thus, the rate of dissolution of NiO in DH = 30 cm$$^{3}$$/kg water seemed to be lower than the growth rate of NiO in high DO conditions.

論文

The Effect of crystal textures on the anodic oxidization of zirconium in a boiling nitric acid solution

加藤 千明; 石島 暖大; 上野 文義; 山本 正弘

Journal of Nuclear Science and Technology, 53(9), p.1371 - 1379, 2016/09

AA2015-0626.pdf:1.2MB

 被引用回数:2 パーセンタイル:23.29(Nuclear Science & Technology)

硝酸水溶液でジルコニウムの応力腐食割れに関して、ジルコニウムの陽極酸化に及ぼす結晶配向の影響を調査した。酸化ジルコニウム膜の成長挙動は、脱不動態化電位(1.47V vs. SSE)で、劇的に変化した。1.5Vでは、酸化皮膜は速く成長し、その平均皮膜厚さは電荷量に比例して増加した。酸化皮膜は周期的な3乗則に従った成長挙動を示した。周期的な3乗則に従った成長挙動への遷移前では、酸化皮膜の成長挙動に結晶配向の影響を及ぼさなかった。しかし、皮膜成長の遷移後は、酸化皮膜の平均皮膜厚さと厚い酸化皮膜の下に生じたき裂は結晶配向の影響を受けた。(0002)面が配向している圧延面では、その平均皮膜厚さは減少し、皮膜内のき裂により皮膜の剥離が生じた。(0002)面に垂直面である圧延方向面では、厚い酸化皮膜の下には、圧延方向に深く進展したき裂が観察された。き裂は酸化物層の中をジルコニウム母材の(0002)面に沿って進展した。酸化物層は、ひも状の酸化ジルコニウムとジルコニウム水素化物からなり、ひも状の酸化ジルコニウムは、単斜晶ZrO$$_{2}$$に加えて斜方晶ZrO$$_{2}$$を含んでいた。外部応力が無い条件でき裂が発生・進展した機構の1つの仮定として、(0002)面に析出した水素化物の酸化と、その後に生じる斜方晶ZrO$$_{2}$$から単斜晶ZrO$$_{2}$$への相変態がその原因の一つと考えられた。

論文

Corrosion of 9-12Cr ferritic-martensitic steels in high-temperature CO$$_{2}$$

Rouillard, F.*; 古川 智弘

Corrosion Science, 105, p.120 - 132, 2016/04

 被引用回数:70 パーセンタイル:97.2(Materials Science, Multidisciplinary)

9-12Crフェライト・マルテンサイト系鋼を対象に、1-250barの圧力条件下の高温CO$$_{2}$$中にて最長8000時間の腐食研究を実施した。その結果、ブレークアウェイ酸化と呼称される腐食挙動は観察されなかった。9Cr鋼は、12Cr鋼に比較して高い酸化成長挙動および浸炭が生じていた。CO$$_{2}$$圧力が増加した場合においても高温酸化成長挙動はほとんど変化しなかったにも関わらず、浸炭速度は増加する傾向を示した。2種の12Cr鋼は異なった腐食形態を示し、その影響として、ガスの構成、鋼中微量元素または試験片最終表面処理の影響が考えられた。本研究では酸化と浸炭を考慮した腐食メカニズムを提案する。

論文

Activation and control of visible single defects in 4H-, 6H-, and 3C-SiC by oxidation

Lohrmann, A.*; Castelletto, S.*; Klein, J. R.*; 大島 武; Bosi, M.*; Negri, M.*; Lau, D. W. M.*; Gibson, B. C.*; Prawer, S.*; McCallum, J. C.*; et al.

Applied Physics Letters, 108(2), p.021107_1 - 021107_4, 2016/01

 被引用回数:31 パーセンタイル:82.7(Physics, Applied)

Creation and characterisation of single photon emitters near the surface of 4H- and 6H-silicon carbide bulk substrates and 3C-SiC epitaxially grown on silicon substrates were investigated. These single photon emitters can be created and stabilized by thermal annealing in an oxygen atmosphere at temperatures above 550 $$^{circ}$$C. Hydrofluoric acid (HF) treatment is shown to effectively annihilate the emission from defects and to restore an optically clean surface. However, the emission from the defects can be obtained after re-oxidation above 550 $$^{circ}$$C. By measuring using standard confocal microscopy techniques, the excited state lifetimes for the emitters are found to be in the nanosecond regime in all three polytypes, and the emission dipoles are aligned with the lattice.

論文

The Effect of oxidation and crystal phase condition on the ballooning and rupture behavior of Zircaloy-4 cladding tube-under transient-heating conditions

成川 隆文; 天谷 政樹

Journal of Nuclear Science and Technology, 53(1), p.112 - 122, 2016/01

 被引用回数:4 パーセンタイル:42.19(Nuclear Science & Technology)

In order to investigate the effect of oxidation and crystal phase condition on the ballooning and rupture behaviors of cladding tube under simulated loss-of-coolant-accident (LOCA) conditions, laboratory-scale experiments were performed in which internally pressurized non-irradiated Zircaloy-4 (Zry-4) cladding specimens were heated to burst in steam and argon gas conditions. Values of the maximum circumferential strain were normalized by dividing them by engineering hoop stress at the time of rupture. The dependence of the normalized value on burst temperature and the relationship between the normalized value and the length, width and area of rupture opening were evaluated. The correlation between the normalized value and the burst temperature suggested that the fraction of the $$beta$$ phase in Zry-4 cladding specimens affected the strain in the specimens and the oxidation of specimens suppressed the amount of ballooning of the specimens. The relationship between the normalized value and the length, width and area of rupture opening indicated that the length, width and area of rupture opening depended on the crystal phase condition in Zry-4 cladding specimens irrespective of atmosphere in the case of the heating rate of $$sim$$3 K/s.

論文

Upgrade in catalytic activity of hydrophobic platinum catalysts by irradiation with electron beams

岩井 保則

Fusion Engineering and Design, 98-99, p.1796 - 1799, 2015/10

 被引用回数:4 パーセンタイル:37.88(Nuclear Science & Technology)

疎水性白金触媒は水蒸気-水素間水素同位体交換反応やトリチウム酸化の用途にて核融合分野で広く使用されている。疎水性触媒の触媒活性は空気中の水蒸気や水ミストのほかに燃焼反応により生成する水にもほとんど影響されない特徴を持つ。一般的に疎水性触媒は多孔性の疎水性高分子に白金を担持することで作成される。日本はスチレンジビニルベンゼンを疎水性高分子とした疎水性白金触媒をトリチウム水処理システムに採用してきた実績を有する。システム規模低減のためには触媒活性の可能な限りの向上が必要である。二種類の疎水性白金触媒を電子線で照射した場合のトリチウム酸化性能の変化を精査した。両方の触媒とも線量の増加とともに疎水性触媒の触媒活性は向上し、500から1000kGyにて総括反応速度係数はピーク値を示し、それ以降の線量では徐々に低下することを見出した。総括反応速度係数のピーク値は未照射の6倍の値を示した。スチレンジビニルベンゼンは放射線に対する耐久性が強く、この程度の線量では機械的強度に影響はなく、簡易に触媒活性を向上可能な有力な方法であることを見出した。

論文

Corrigendum to "Real time observation of oxygen chemisorption states on Si(001)-2$$times$$1 during supersonic oxygen molecular beam irradiation"

寺岡 有殿; 吉越 章隆

Applied Surface Science, 346, P. 580, 2015/08

 被引用回数:0 パーセンタイル:1.75(Chemistry, Physical)

We have performed experiments on surface chemical reactions using a supersonic O$$_{2}$$ molecular beam. Translational kinetic energy values of the O$$_{2}$$ molecules have been estimated by calculations. I had made a mistake in the calculations. We had calculated the translational kinetic energy with gas constant R = 1.134$$times$$10$$^{-4}$$ eV/K. However, R = 8.617$$times$$10$$^{-5}$$ eV/K is correct. Consequently, the correct translational kinetic energy values can be obtained by multiplying those in the published article by a factor of 0.76. Even if they are corrected, conclusions and the points of arguments are as they are except the translational kinetic energy values themselves.

論文

Corrigendum to "Si 2p and O 1s photoemission from oxidized Si(001) surfaces depending on translational kinetic energy of incident O$$_{2}$$ molecules"

寺岡 有殿; 吉越 章隆

Applied Surface Science, 343, P. 212, 2015/07

 被引用回数:0 パーセンタイル:1.75(Chemistry, Physical)

We have performed experiments on surface chemical reactions using a supersonic O$$_{2}$$ molecular beam and O$$_{2}$$ gas. Translational kinetic energy values of the O$$_{2}$$ molecules have been estimated by calculations. I had made a mistake in the calculations. We had calculated the translational kinetic energy with gas constant R = 1.134$$times$$10$$^{-4}$$ eV/K. However, R = 8.617$$times$$10$$^{-5}$$ eV/K is correct. Consequently, the correct translational kinetic energy values can be obtained by multiplying those in the published article by a factor of 0.76. Even if they are corrected, conclusions and the points of arguments are as they are except the translational kinetic energy values themselves.

論文

Corrigendum to "Coexistence of passive and active oxidation for O$$_{2}$$/Si(001) system observed by SiO mass spectrometry and synchrotron radiation photoemission spectroscopy"

寺岡 有殿; 盛谷 浩右*; 吉越 章隆

Applied Surface Science, 343, P. 213, 2015/07

 被引用回数:0 パーセンタイル:1.75(Chemistry, Physical)

We have performed experiments on surface chemical reactions using a supersonic O$$_{2}$$ molecular beam. Translational kinetic energy values of the O$$_{2}$$ molecules have been estimated by calculations. I had made a mistake in the calculations. We had calculated the translational kinetic energy with gas constant R = 1.134$$times$$10$$^{-4}$$ eV/K. However, R = 8.617$$times$$10$$^{-5}$$ eV/K is correct. Consequently, the correct translational kinetic energy values can be obtained by multiplying those in the published article by a factor of 0.76. Even if they are corrected, conclusions and the points of arguments are as they are except the translational kinetic energy values themselves.

論文

Corrigendum to "Commissioning of surface chemistry end-station in BL23SU of SPring-8"

寺岡 有殿; 吉越 章隆

Applied Surface Science, 339, P. 158, 2015/06

We have performed experiments on surface chemical reactions using a supersonic O$$_{2}$$ molecular beam. Translational kinetic energy values of the O$$_{2}$$ molecules have been estimated by calculations. I had made a mistake in the calculations. We had calculated the translational kinetic energy with gas constant R = 1.134$$times$$10$$^{-4}$$ eV/K. However, R = 8.617$$times$$10$$^{-5}$$ eV/K is correct. Consequently, the correct translational kinetic energy values can be obtained by multiplying those in the published article by a factor of 0.76. Even if they are corrected, conclusions and the points of arguments are as they are except the translational kinetic energy values themselves.

論文

Intergranular oxidation within crevice of austenitic stainless steel in high temperature water

相馬 康孝; 加藤 千明; 上野 文義

Proceedings of 23rd International Conference on Nuclear Engineering (ICONE-23) (DVD-ROM), 8 Pages, 2015/05

高温高圧水中(温度288$$^{circ}$$C,圧力8.5MPa,溶存酸素濃度32ppm,導電率1.2$$pm$$0.2$$mu$$S(25$$^{circ}$$Cにおける値))に浸漬(500h)した低炭素オーステナイトステンレス鋼のすき間内において粒界酸化が発生した。粒界酸化はすき間の開口部から一定の距離を有し、かつすき間幅が比較的小さい特定の箇所で発生した。粒界酸化部ではFeとNi成分が選択溶解し、Crリッチな酸化物が形成した。粒界酸化の最大浸食深さは500hで約50$$mu$$mであった。粒界酸化部周辺で形成された表面酸化皮膜層を電位-pH図を以て熱力学的に解析したところ、環境のpHは約3.2から3.4と推定された。粒界酸化部が起きた箇所に小型のセンサーを挿入し、すき間内の局所的な溶液導電率を測定した。測定した導電率を理論的に求めた導電率-pHの関係と比較した。その結果、すき間内ではバルクに比べ約100倍の導電率を示し、それに対応するpHは約3.5であった。以上の結果から、すき間内では溶液の酸性化が起き、それにより粒界酸化が発生したものと推定された。

論文

Erratum; Precise control of Si(001) initial oxidation by translational kinetic energy of O$$_{2}$$ molecules

寺岡 有殿; 吉越 章隆

Japanese Journal of Applied Physics, 54(3), P. 039204_1, 2015/03

 被引用回数:2 パーセンタイル:77.82(Physics, Applied)

We have performed experiments on surface chemical reactions using a supersonic O$$_{2}$$ molecular beam and O$$_{2}$$ gas. Translational kinetic energy values of the O$$_{2}$$ molecules have been estimated by calculations. We have noticed a mistake in the calculations. We had calculated the translational kinetic energy with gas constant $$R$$ = 1.134$$times$$10$$^{-4}$$ eV/K. However, $$R$$ = 8.617$$times$$10$$^{-5}$$ eV/K is correct. Consequently, the correct translational kinetic energy values can be obtained by multiplying those in the published article by a factor of 0.76. Even if they are corrected, conclusions and the points of arguments are as they are except the translational kinetic energy values themselves.

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