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論文

Temperature-dependent deformation behavior of dual-phase medium-entropy alloy; In-situ neutron diffraction study

Gu, G. H.*; Jeong, S. G.*; Heo, Y.-U.*; Harjo, S.; Gong, W.; Cho, J.*; Kim, H. S.*; 他4名*

Journal of Materials Science & Technology, 223, p.308 - 324, 2025/07

 被引用回数:0 パーセンタイル:0.00(Materials Science, Multidisciplinary)

Face-centered cubic (FCC) equi-atomic multi-principal element alloys (MPEAs) exhibit excellent mechanical properties from cryogenic to room temperatures. At room temperature, deformation is dominated by dislocation slip, while at cryogenic temperatures (CTs), reduced stacking fault energy enhances strain hardening with twinning. This study uses in-situ neutron diffraction to analyze the temperature-dependent deformation behavior of Al$$_{7}$$(CoNiV)$$_{93}$$, a dual-phase (FCC/BCC) medium-entropy alloy (MEA). At liquid nitrogen temperature (LNT), deformation twinning in the FCC matrix leads to additional strain hardening through the dynamic Hall-Petch effect, giving the appearance of improved strengthening at LNT. In contrast, BCC precipitates show dislocation slip at both 77 K and 298 K, with temperature-dependent lattice friction stress playing a significant role in strengthening. The study enhances understanding of deformation behaviors and provides insights for future alloy design.

論文

Unusual low-temperature ductility increase mediated by dislocations alone

Naeem, M.*; Ma, Y.*; Tian, J.*; Kong, H.*; Romero-Resendiz, L.*; Fan, Z.*; Jiang, F.*; Gong, W.; Harjo, S.; Wu, Z.*; et al.

Materials Science & Engineering A, 924, p.147819_1 - 147819_10, 2025/02

 被引用回数:0 パーセンタイル:0.00(Nanoscience & Nanotechnology)

Face-centered cubic (fcc) medium-/high-entropy alloys (M/HEAs) typically enhance strength and ductility at cryogenic temperatures via stacking faults, twinning, or martensitic transformation. However, in-situ neutron diffraction on VCoNi MEA at 15 K reveals that strain hardening is driven solely by rapid dislocation accumulation, without these mechanisms. This results in increased yield strength, strain hardening, and fracture strain. The behavior, explained by the Orowan equation, challenges conventional views on cryogenic strengthening in fcc M/HEAs and highlights the role of dislocation-mediated plasticity at low temperatures.

論文

Martensitic transformation and shape memory effect in Mn-rich Cu-Mn-Al alloys

伊東 達矢; Xu, S.*; Xu, X.*; 大森 俊洋*; 貝沼 亮介*

Shape Memory and Superelasticity, 9 Pages, 2025/00

The microstructure, crystal structures, cold workability, and martensitic transformation temperatures of several Cu$$_{100-{it x}-{it y}}$$Mn$$_{it x}$$Al$$_{it y}$$ (40 $$leq$$ ${it x}$ $$leq$$ 55; 10 $$leq$$ ${it y}$ $$leq$$ 13; at%) alloys were analyzed. For the first time, martensitic transformation was revealed Mn-rich Cu-Mn-Al alloys. The surface relief of the martensite phase reversibly appeared and disappeared during cooling and heating, along with small thermal hysteresis, implying a thermoelastic transformation. The crystal structures of the parent and martensite phases are B2 and 2M(BCT), respectively, with c$/a being approximately 1.35. Cold workability improves with decreasing Al content, exhibiting a trend similar to that observed for previously reported Cu-rich Cu-Al-Mn shape memory alloys. The martensitic transformation temperatures decrease with increasing Al content and increase with increasing Mn content. These results are consistent with the stability trends of the parent body-centered cubic phase in the phase diagram at high temperature. The shape memory effect with a recovery strain of 1.3% was observed in a 5.0% pre-stretched Cu$_{39}$$Mn$$_{50}$$Al$$_{11}$$ (at%) sample. This alloy demonstrates moderate cold workability and cost-effectiveness, exhibiting potential as an alternative for conventional shape memory alloys in various applications.

論文

Enhanced cryogenic mechanical properties of heterostructured CrCoNi multicomponent alloy; Insights from ${it in situ}$ neutron diffraction

Naeem, M.*; Ma, Y.*; Knowles, A. J.*; Gong, W.; Harjo, S.; Wang, X.-L.*; Romero Resendiz, L.*; 他6名*

Materials Science & Engineering A, 916, p.147374_1 - 147374_8, 2024/11

 被引用回数:2 パーセンタイル:67.89(Nanoscience & Nanotechnology)

Heterostructured materials (HSMs) improve the strength-ductility trade-off of alloys, but their cryogenic performance under real-time deformation is unclear. We studied heterostructured CrCoNi medium-entropy alloy via ${it in situ}$ neutron diffraction at 77 K and 293 K. A significant mechanical mismatch between fine and coarse grains led to an exceptional yield strength of 918 MPa at 293 K, increasing to 1244 MPa at 77 K with a uniform elongation of 34%. This strength-ductility synergy at 77 K is attributed to high dislocation pile-up density, increased planar faults, and martensitic transformation. Compared to homogeneous alloys, HSMs show promise for enhancing cryogenic mechanical performance in medium-/high-entropy alloys.

論文

高圧中性子回折実験のためのダイヤモンドアンビルセルの開発

町田 真一*; 服部 高典; 中野 智志*; 佐野 亜沙美; 舟越 賢一*; 阿部 淳*

高圧力の科学と技術, 34(3), p.134 - 142, 2024/09

J-PARC物質・生命科学実験施設PLANETビームラインにおいて、高圧中性子回折実験用ダイヤモンドアンビルセル(DAC)を開発した。高圧発生には円錐形状で支持されたダイヤモンドアンビルを用いた。その結果、69.4GPaまでのD$$_2$$O氷の中性子データを得ることに成功した。また、中性子回折測定に適したガスケット材料を検討した。11種類の合金を試験し、SUS304, Inconel718, M2052 (73Mn-20Cu-5Ni-2Fe, at%)合金が優れた性能を示した。特にM2052ヌルマトリクス合金は、入射ビームがガスケットに当たることが避けられない中性子回折実験に有用であることが実証された。われわれは、D$$_2$$O氷に対して少なくとも43.3GPaまでリートベルト解析が可能な中性子回折プロファイルを得ることができた。

論文

Antiferromagnetism and phase stability of CrMnFeCoNi high-entropy alloy

Zhu, L.*; He, H.*; Naeem, M.*; Sun, X.*; Qi, J.*; Liu, P.*; Harjo, S.; 中島 健次; Li, B.*; Wang, X.-L.*

Physical Review Letters, 133(12), p.126701_1 - 126701_6, 2024/09

 被引用回数:1 パーセンタイル:53.15(Physics, Multidisciplinary)

It has long been suspected that magnetism could play a vital role in the phase stability of multi- component high-entropy alloys. However, the nature of the magnetic order, if any, has remained elusive. Here, by using elastic and inelastic neutron scattering, we demonstrate evidence of antiferromagnetic order below $$sim$$80 K and strong spin fluctuations persisting to room temperature in a single-phase face-centered cubic (fcc) CrMnFeCoNi high-entropy alloy. Despite the chemical complexity, the magnetic structure in CrMnFeCoNi can be described as $$gamma$$-Mn-like, with the magnetic moments confined in alternating (001) planes and pointing toward the $$langle$$111$$rangle$$ direction. Combined with first-principles calculation results, it is shown that the antiferromagnetic order and spin fluctuations help stabilized the fcc phase in CrMnFeCoNi high-entropy alloy.

論文

Anomalous dislocation response to deformation strain in CrFeCoNiPd high-entropy alloys with nanoscale chemical fluctuations

Ying, H.*; Yang, X.*; He, H.*; Yan, A.*; An, K.*; Ke, Y.*; Wu, Z.*; Tang, S.*; Zhang, Z.*; Dong, H.*; et al.

Scripta Materialia, 250, p.116181_1 - 116181_7, 2024/09

 被引用回数:1 パーセンタイル:47.38(Nanoscience & Nanotechnology)

Nanoscale chemical fluctuations and their effect on the deformation behavior of CrFeCoNi-based high-entropy alloys (HEAs) were investigated using small-angle scattering and in situ neutron diffraction measurements. Small-angle scattering results demonstrated the presence of nano ($$>$$10 nm) chemical fluctuations in the as-prepared CrFeCoNiPd HEAs, which was attributed to the negative mixing of enthalpy and the significant atomic radius difference between Pd and the constituent elements in the CrFeCoNi-based alloys. Subsequent tensile tests demonstrated that the yield and tensile strengths of the as-prepared CrFeCoNiPd HEA surpass those of the as-prepared CrMnFeCoNi HEA. Neutron diffraction data analysis revealed an anomalous response of dislocation evolution with the strain.

論文

Anisotropic creep property related to non-spherical shape of mechanically alloyed powder of oxide dispersion strengthened F82H

酒瀬川 英雄; 中島 基樹*; 加藤 太一朗*; 野澤 貴史*; 安堂 正己*

Materials Today Communications (Internet), 40, p.109659_1 - 109659_8, 2024/08

 被引用回数:1 パーセンタイル:41.44(Materials Science, Multidisciplinary)

酸化物分散強化型鋼鋼のナノメートルサイズの酸化物粒子はクリープ強度の向上に対して重要な役割を持つ。以前の研究では旧粉末境界という焼結前に機械的合金粉末の表面であった組織因子に注目した。その結果、より小さなサイズの粉末で製作され微細な旧粉末境界を持つ酸化物分散強化型鋼は、より大きなサイズの粉末で製作され粗大な旧粉末境界を持つ酸化物分散強化型鋼よりも、短いクリープ寿命を示すことを確かめた。これより、機械的合金粉末の大きさがクリープ強度特性に影響を及ぼすことを明らかとなった。本研究では非球状である機械的合金粉末の形状がクリープ強度特性に及ぼす影響に注目した。このような形状がクリープ強度特性に異方性を生じさせる可能性が考えられたからである。ここでは異なった切り出し方位を持つ試験片に対してスモールパンチクリープ試験を実施することで異方性に注目した。これより、クリープ寿命は試験片の切り出し方位によって変化することを確かめて、形状がクリープ強度特性に及ぼす影響を明らかとした。

論文

Multi-modal 3D image-based simulation of hydrogen embrittlement crack initiation in Al-Zn-Mg alloy

比嘉 良太*; 藤原 比呂*; 戸田 裕之*; 小林 正和*; 海老原 健一; 竹内 晃久*

Materials Transactions, 65(8), p.899 - 906, 2024/08

 被引用回数:0 パーセンタイル:0.00(Materials Science, Multidisciplinary)

Al-Zn-Mg合金では、水素(H)によって機械的特性が著しく劣化することから、そのような合金の強度を向上させるためには、水素脆化(HE)と呼ばれるこの現象を抑制することが不可欠である。粒界破壊(IGF)は主にHE発生時に観察されるため、HEを抑制するためにはIGFの発生挙動を理解する必要がある。通常、応力、ひずみ、H濃度の不均一な分布は、多結晶材料におけるIGFの発生に影響を与える。本研究では、X線イメージング技術により得られた多結晶体の3次元微細構造データをもとに作成した3次元イメージベースモデルを用いた結晶塑性有限要素法とH拡散解析によるシミュレーションから、実際の破壊領域における応力、ひずみ、H濃度の分布を調べた。そして、シミュレーション結果とX線CTによる引張試験試料のその場観察を組み合わせ、実際のき裂発生挙動における応力、ひずみ、H濃度の分布を調べ、粒界き裂の発生条件を検討した。その結果、結晶塑性に起因する粒界垂直応力が粒界き裂の発生を支配することが明らかになった。一方、応力による内部Hの蓄積はき裂発生にほとんど影響しないことがわかった。

論文

Mechanical properties of base metal and heat-affected zone in friction-stir-welded AA6061-T6 at ultra-low temperature of 20 K

Nguyen, T.-D.*; Singh, C.*; Kim, Y. S.*; Han, J. H. *; Lee, D.-H.*; Lee, K.*; Harjo, S.; Lee, S. Y.*

Journal of Materials Research and Technology, 31, p.1547 - 1556, 2024/07

 被引用回数:2 パーセンタイル:0.00(Materials Science, Multidisciplinary)

This study investigates the mechanical properties of a friction-stir-welded (FSW) AA6061-T6 aluminum alloy at ultra-low temperature (ULT) of 20 K. In-situ neutron diffraction and orientation imaging microscopy were employed to compare the tensile deformation behavior of the base metal (BM) and heat-affected zone (HAZ) in the FSW aluminum plate. The results demonstrate that compared to room-temperature (RT), ULT induces a significant improvement in tensile strength and ductility in both the BM and HAZ. The enhanced mechanical properties in BM at ULT result from a more homogeneous deformation than occurs at RT. On the other hand, HAZ at ULT exhibits an even lower yield strength than at RT, but the strain hardening rate (SHR) is the most significant among the alloys, leading to a tensile strength of 346 MPa and the highest ductility of 46.8%. The lowest yield strength corresponds to the lowest-hardness zones in HAZ, caused by dissolved/coarsened precipitates during the FSW process.

論文

マルチピークを用いた応力評価

Harjo, S.; Gong, W.; 川崎 卓郎

日本材料学会第58回X線材料強度に関するシンポジウム講演論文集, p.51 - 54, 2024/07

In-situ neutron diffraction was used to study tensile deformation in an extruded AZ31 alloy. The aim was to validate existing methods and develop new ones for stress evaluation in magnesium alloys. Results showed varied increases in lattice strains among grains, posing challenges for conventional procedures. A new method, considering grain volume fraction and multiple orientations, proved highly accurate. When simultaneous hk.l peaks weren't available, the 12.1 peak was recommended for stress evaluation, showing a linear relationship with applied stress throughout deformation.

論文

マルチモーダル化したマグネシウム合金の変形中の構成相・組織の挙動

Harjo, S.; Gong, W.; 相澤 一也; 山崎 倫昭*; 川崎 卓郎

日本材料学会第58回X線材料強度に関するシンポジウム講演論文集, p.58 - 60, 2024/07

The experiment and analysis procedures for a sample exhibiting multimodal structures were outlined. The sample, a Mg$$_{97}$$Zn$$_1$$Y$$_2$$ alloy, initially comprised two phases: the HCP $$alpha$$ matrix ($$alpha$$Mg) and the long-period stacking ordered phase (LPSO), constituting approximately 25% of the volume. Through hot extrusion at 623 K with an extrusion ratio (R) of 5.0, the alloy was rendered multimodal. Specifically, at an R value of 5.0, dynamic recrystallization occurred partially within the $$alpha$$Mg phase, resulting in a bimodal microstructure. This microstructure consisted of a deformed $$alpha$$Mg component and a recrystallized $$alpha$$Mg component. An analysis employing Electron Backscatter Diffraction (EBSD) data facilitated multimodal characterization, enabling successful determination of stresses within the individual $$alpha$$Mg components, as well as the LPSO phase stress.

論文

The Precipitation and redistribution of alloying element in Zircaloy-4 cladding tube oxidized in high-temperature steam

天谷 政樹

High Temperature Corrosion of Materials, 101(3), p.455 - 469, 2024/06

 被引用回数:0 パーセンタイル:0.00(Metallurgy & Metallurgical Engineering)

Zirconium (Zr)-based alloys are widely used as fuel cladding material for light water reactors. Under a loss-of-coolant accident (LOCA) condition, the oxidation of fuel cladding by high-temperature steam induces the degradation of mechanical properties of the cladding and would affect the integrity of fuel rods and/or assemblies, etc., during LOCA. In this study, the distribution of the elements (zirconium, oxygen, tin, iron and chromium) in Zircaloy-4 cladding specimens oxidized in the temperature range of $$sim$$1350- $$sim$$1700 K in steam was analyzed along the radial direction of the specimens by using SEM/EPMA, and the cause of element distribution in the specimens was discussed in consideration of the morphology of precipitates in the specimens and hypothesized phase diagrams related to the elements contained in the specimens. The form of the particles precipitated and the comparison between SEM/EPMA results and hypothesized phase diagrams of Zr-Sn-O system suggested that the liquefaction of tin-rich material and/or Zr-(Fe,Cr) compounds occurred during the oxidation test. The results obtained indicate that Zircaloy-4 cladding tubes would start melting at the melting point of tin-oxide and the eutectic point of Zr-(Fe,Cr)compounds, which is much lower than the melting point of Zr, $$alpha$$-Zr(O), or zirconium oxide (ZrO$$_{2}$$).

論文

変形その場パルス中性子回折実験により高強度マグネシウム合金の強度増加機構を解明

Harjo, S.

Isotope News, (793), p.13 - 16, 2024/06

高強度マグネシウム(Mg)合金の高温押出加工による大幅な強度増加の機構を引張変形その場中性子回折実験によってどのように解明したかについて紹介する。高温押出加工の条件により組織が複雑化し、構成相それぞれの組織からの強度への寄与について解説する。

論文

薄膜の垂直磁気異方性

高梨 弘毅; 関 剛斎*

まぐね, 19(3), p.100 - 106, 2024/06

薄膜の垂直磁気異方性は、磁気記録のみならずスピントロニクスにおいても重要な役割を果たしている。本解説記事では、垂直磁気異方性に関して、磁気多層膜、規則合金膜、希土類遷移金属アモルファス合金多層膜、不均一膜やグラニュラー膜など、垂直磁化を持つ具体例を示しながら、基礎からこれまでの研究、そして最近の研究動向を概説する。それぞれの具体例について、構造対称性の破れによる界面磁気異方性、ひずみによる磁気弾性異方性、バルクの結晶磁気異方性、原子の方向性規則配列などの垂直磁気異方性の物理的起源を議論する。

論文

Contributions of multimodal microstructure in the deformation behavior of extruded Mg alloys containing LPSO phase

萩原 幸司*; 眞山 剛*; 山崎 倫昭*; Harjo, S.; 徳永 透子*; 山本 和輝*; 杉田 三佳*; 青山 海琳*; Gong, W.; 西本 宗矢*

International Journal of Plasticity, 173, p.103865_1 - 103865_21, 2024/02

 被引用回数:13 パーセンタイル:98.17(Engineering, Mechanical)

The unique control mechanisms of the plastic deformation of two-phase extruded alloy composed of Mg and long-period stacking ordered (LPSO) phase were clarified by comparison with those of other Mg solid-solution alloys, focusing on the question of why do the Mg/LPSO two-phase alloys exhibit both large elongation and high strength? The stress-strain curves for each grain in the alloys could be imaginary estimated using neutron diffraction analysis during the tensile test. The results demonstrate that the deformation behaviors of the worked and recrystallized grains are significantly different in all the Mg-extruded alloys owing to the strong plastic anisotropy in Mg with hexagonal close-packed (hcp) structure. Therefore, the deformation behavior is controlled by a composite-like deformation mechanism, even in single-phase Mg solid-solution alloys.

報告書

健全性崩壊をもたらす微生物による視認不可腐食の分子生物・電気化学的診断及び抑制技術の開発(委託研究); 令和4年度英知を結集した原子力科学技術・人材育成推進事業

廃炉環境国際共同研究センター; 物質・材料研究機構*

JAEA-Review 2023-031, 101 Pages, 2024/01

JAEA-Review-2023-031.pdf:24.47MB

日本原子力研究開発機構(JAEA)廃炉環境国際共同研究センター(CLADS)では、令和4年度英知を結集した原子力科学技術・人材育成推進事業(以下、「本事業」という。)を実施している。本事業は、東京電力ホールディングス株式会社福島第一原子力発電所(1F)の廃炉等をはじめとした原子力分野の課題解決に貢献するため、国内外の英知を結集し、様々な分野の知見や経験を、従前の機関や分野の壁を越えて緊密に融合・連携させた基礎的・基盤的研究及び人材育成を推進することを目的としている。平成30年度の新規採択課題から実施主体を文部科学省からJAEAに移行することで、JAEAとアカデミアとの連携を強化し、廃炉に資する中長期的な研究開発・人材育成をより安定的かつ継続的に実施する体制を構築した。本研究は、令和2年度に採択された研究課題のうち、「健全性崩壊をもたらす微生物による視認不可腐食の分子生物・電気化学的診断及び抑制技術の開発」の令和2年度から令和4年度分の研究成果について取りまとめたものである。本研究では、微生物が関与して誘起・加速する金属材料の腐食(微生物鉄腐食)に関して、加速検査試験片、オンサイト遺伝子検査などの革新的な診断技術を開発、1Fで想定される微生物腐食の発生・進行条件の洗い出しを行い、水質や環境コントロールによって微生物腐食を防ぐ方法を提案することを目的とした。具体的な研究成果として、微生物腐食反応の加速技術を材料と細菌集積の2つの方向から実現し、採水によるオンサイト加速試験の要素技術開発を行なった。さらに、局所的に激しい腐食を行う細菌の単離に成功し、新しい微生物腐食の抑止技術へと繋がる成果が得られた。さらに、これらの成果の大部分は、春に博士課程に進学した2人の修士課程の学生によって達成されたもので有り、高い学際性を持つリーダー人材の育成に貢献した。

論文

Probing deformation behavior of a refractory high-entropy alloy using ${it in situ}$ neutron diffraction

Zhou, Y.*; Song, W.*; Zhang, F.*; Wu, Y.*; Lei, Z.*; Jiao, M.*; Zhang, X.*; Dong, J.*; Zhang, Y.*; Yang, M.*; et al.

Journal of Alloys and Compounds, 971, p.172635_1 - 172635_7, 2024/01

 被引用回数:1 パーセンタイル:13.75(Chemistry, Physical)

The grain orientation-dependent lattice strain evolution of a (TiZrHfNb)$$_{98}$$$$N_2$$ refractory high-entropy alloy (HEA) during tensile loading has been investigated using ${it in situ}$ neutron diffraction. The equivalent strain-hardening rate of each of the primary $$<hkl>$$-oriented grain families was found to be relatively low, manifesting the macroscopically weak work-hardening ability of such a body-centered cubic (BCC)-structured HEA. This finding is indicative of a dislocation planar slip mode that is confined in a few single-slip planes and leads to in-plane softening by high pile-up stresses.

論文

Magnetic layer thickness influence on magnetoelastic properties anisotropy in Co$$_{2}$$Fe$$_{0.4}$$Mn$$_{0.6}$$Si heusler alloy thin films

Nabialek, A.*; Chumak, O.*; 関 剛斎*; 高梨 弘毅; Baczewski, L. T.*; Szymczak, H.*

IEEE Transactions on Magnetics, 59(11), p.2501405_1 - 2501405_5, 2023/11

 被引用回数:2 パーセンタイル:32.34(Engineering, Electrical & Electronic)

The anisotropic magnetoelastic (ME) properties of epitaxial Co$$_{2}$$Fe$$_{0.4}$$Mn$$_{0.6}$$Si(CFMS) Heusler alloy thin films with thicknesses ranging from 8 to 100 nm were investigated using the strain-modulated ferromagnetic resonance (SMFMR) technique. The calculation of the first cubic magnetocrystalline (MC) constant ${it K}$ $$_{1}$$ and the two cubic ME constants ${it b}$ $$_{1}$$ and ${it b}$ $$_{2}$$ was carried out assuming the cubic symmetry of the magnetic layer. A significant negative perpendicular MC anisotropy, of the order of 10$$^{5}$$ J/m$$^{3}$$, was also observed. The investigated parameters were found to be dependent on the thickness of the magnetic layer. The thinnest magnetic layers showed the strongest cubic MC anisotropy and the weakest anisotropy of ME properties. These findings highlight the importance of considering the magnetic layer thickness when evaluating the anisotropy in the ME properties of Heusler alloy thin films.

論文

Direct observation of concentration fluctuations in Au-Si eutectic liquid by small-angle neutron scattering

坂口 佳史*; 高田 慎一; 川北 至信; 藤村 由希; 近藤 啓悦

Journal of Physics; Condensed Matter, 35(41), p.415403_1 - 415403_11, 2023/10

 被引用回数:0 パーセンタイル:0.00(Physics, Condensed Matter)

It is well-known that eutectic gold-silicon (Au-Si) alloys exhibit anomalous melting point depression, which is more than 1000 $$^{circ}$$C from the melting point of elemental Si (1414 $$^{circ}$$C). The melting point depression in eutectic alloys is generally explained in terms of a decrease of the free energy by mixing. However, it is difficult to understand the anomalous melting point depression only from the stability of the homogeneous mixing. Some researchers suggest that there are concentration fluctuations in the liquids, where the atoms are inhomogeneously mixed. In this paper, we measure the small-angle neutron scattering (SANS) of Au$$_{81.4}$$Si$$_{18.6}$$ (eutectic composition) and Au$$_{75}$$Si$$_{25}$$ (off-eutectic composition) at temperatures from room temperature to 900 $$^{circ}$$C in both solid and liquid states to observe such concentration fluctuations directly.

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