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High pressure neutron diffraction on WAND2 with a Paris-Edinburgh press 巴黎-爱丁堡压机在WAND2上的高压中子衍射
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-08-02 DOI: 10.1080/08957959.2022.2062242
M. Donnelly, Y. Wu, E. Kroll, J. Molaison, M. Frontzek, B. Haberl
ABSTRACT The Paris-Edinburgh press is a widely available, highly adaptable pressure cell commonly used while collecting neutron scattering data. Here, we detail the use of the VX3 and VX5 Paris-Edinburgh presses on the Wide-Angle Neutron Diffractometer (WAND ) at the High Flux Isotope Reactor at Oak Ridge National Laboratory. We first give a detailed overview of the instrument setup and alignment capabilities used at WAND . We then demonstrate the high pressure capabilities through three examples. The first example focuses on diffraction data obtained from a lithium-diamond mixture to 10 GPa with the use of single toroidal cubic boron nitride anvils. Other examples include the room temperature compressions of germanium (up to 16 GPa) and the mineral malachite with double toroidal sintered diamond anvils. This work thereby represents the first studies above 10 GPa at the High Flux Isotope Reactor and opens the door for future user experiments at these elevated pressures.
巴黎-爱丁堡出版社是一种广泛使用的,高度适应性的压力电池,通常用于收集中子散射数据。在这里,我们详细介绍了VX3和VX5巴黎-爱丁堡压机在橡树岭国家实验室高通量同位素反应堆的广角中子衍射仪(WAND)上的使用。我们首先给出了仪器设置和校准能力在WAND使用的详细概述。然后,我们通过三个例子来演示高压能力。第一个例子着重于使用单环面立方氮化硼砧从10 GPa的锂-金刚石混合物中获得的衍射数据。其他的例子包括锗(高达16 GPa)的室温压缩和矿物孔雀石与双环形烧结金刚石砧。因此,这项工作代表了高通量同位素反应堆在10 GPa以上的第一次研究,并为未来在这些高压力下的用户实验打开了大门。
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引用次数: 0
Resistively heated, high pressure, membrane and screw driven diamond anvil cell 电阻加热,高压,膜和螺旋驱动金刚石砧细胞
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-07-02 DOI: 10.1080/08957959.2020.1789619
M. Santoro, Ahmed Hajeb, F. Gorelli
ABSTRACT High temperature is of paramount importance in high pressure science. One of the leading tools in this respect is the resistively heated diamond anvil cell (DAC), where the heat is provided by small heaters, positioned close to the diamond/gasket/sample region (internally heated DAC, IHDAC) or by wrapping the DAC body into bigger heaters (externally heated DAC, EHDAC). Although IHDACs can reach sample temperatures higher than 1000 K, they are difficult to handle and the heater/diamond/gasket/sample region may be affected by strong thermal gradients potentially hindering accurate temperature measurements. Here we present a novel EHDAC, which overcomes these issues by uniquely joining: (i) high mechanical precision for multi-Mbar, (ii) high temperature alloys for operating to 1000 K, (iii) membrane or screw driven, easily switchable between each other, (iv) operation into a vacuum chamber, (v) uniform temperature, (vi) facile handling, and (vii) possibility to add internal heaters for achieving even higher temperatures.
摘要高温在高压科学中至关重要。这方面的领先工具之一是电阻加热的金刚石砧座电池(DAC),其中热量由靠近金刚石/垫圈/样品区域的小加热器提供(内部加热的DAC,IHDAC),或通过将DAC主体包裹到更大的加热器中(外部加热的DAC、EHDAC)。尽管IHDAC可以达到高于1000的样本温度 K、 它们很难处理,并且加热器/金刚石/垫圈/样品区域可能受到可能阻碍精确温度测量的强热梯度的影响。在这里,我们提出了一种新的EHDAC,它通过独特的连接克服了这些问题:(i)多Mbar的高机械精度,(ii)工作到1000的高温合金 K、 (iii)薄膜或螺杆驱动,彼此之间易于切换,(iv)进入真空室的操作,(v)均匀的温度,(vi)易于操作,以及(vii)添加内部加热器以实现更高温度的可能性。
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引用次数: 6
Toward an international practical pressure scale: A proposal for an IPPS ruby gauge (IPPS-Ruby2020) 迈向国际实用压力表:IPPS红宝石压力计(IPPS-Ruby2020)的建议
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-07-02 DOI: 10.1080/08957959.2020.1791107
Guoyin Shen, Yanbin Wang, A. Dewaele, Christine Wu, D. Fratanduono, J. Eggert, S. Klotz, K. Dziubek, P. Loubeyre, O. V. Fat’yanov, P. Asimow, T. Mashimo, R. Wentzcovitch
ABSTRACT At the 26th AIRAPT conference in 2017, a task group was formed to work on an International Practical Pressure Scale (IPPS). This report summarizes the activities of the task group toward an IPPS ruby gauge. We have selected three different approaches to establishing the relation between pressure (P) and ruby R1-line shift (Δλ) with three groups of optimal reference materials for applying these approaches. Using a polynomial form of the second order, the recommended ruby gauge (referred as Ruby2020) is expressed by: , where λ0 is the wavelength of the R1-line near 694.25 nm at ambient condition. In June of 2020, the Executive Committee of AIRAPT endorsed the proposed Ruby2020. We encourage high-pressure practitioners to utilize Ruby2020 within its applicable pressure range (up to 150 GPa), so that pressure data can be directly compared across laboratories and amended consistently as better scales emerge in the future.
在2017年第26届AIRAPT会议上,成立了一个国际实用压力标(IPPS)工作组。本报告总结了工作组为实现IPPS红宝石标准所开展的活动。我们选择了三种不同的方法来建立压力(P)和红宝石r1线位移(Δλ)之间的关系,并使用三组最佳参考材料来应用这些方法。采用二阶多项式形式,将推荐的红宝石量规(Ruby2020)表示为:,其中λ0为环境条件下r1线694.25 nm附近的波长。2020年6月,AIRAPT执行委员会批准了Ruby2020提案。我们鼓励高压从业者在其适用的压力范围内(高达150 GPa)使用Ruby2020,这样压力数据可以直接在实验室之间进行比较,并在未来出现更好的刻度时不断修改。
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引用次数: 114
X-ray diffraction and Raman spectra of merrillite at high pressures 高压下镁铝石的x射线衍射和拉曼光谱
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-07-02 DOI: 10.1080/08957959.2020.1798945
Muhua Jia, Xin Hu, Y. Liu, Sheng Jiang, Xiang Wu, S. Zhai
ABSTRACT The compressibility and effect of pressure on the vibrations of merrillite, Ca9NaMg(PO4)7, were studied by using diamond anvil cell at room temperature combined with in-situ synchrotron X-ray diffraction and Raman spectroscopy up to about 18 and 15 GPa, respectively. The pressure-volume data was fitted by a third-order Birch–Murnaghan equation of state to determine the isothermal bulk modulus as K0  = 87.2(32) GPa with pressure derivative K0′ = 3.2(4). If K0′ = 4, the isothermal bulk modulus was obtained as 81.6(10) GPa. The axial compressibility was estimated and an axial elastic anisotropy exists since a-axis is less compressible than the c-axis. The Raman frequencies of all observed modes for merrillite continuously increase with pressure, and the pressure dependences of stretching modes (v 3 and v 1) are larger than those of the bending modes (v 4 and v 2) and external modes. The isothermal mode Grüneisen parameters and intrinsic anharmonicity of merrillite were also calculated.
摘要:利用金刚石砧池,结合原位同步加速器x射线衍射和拉曼光谱,在室温下研究了Ca9NaMg(PO4)7的可压缩性和压力对其振动的影响。采用三阶Birch-Murnaghan状态方程拟合压力-体积数据,得到等温体积模量K0 = 87.2(32) GPa,压力导数K0′= 3.2(4)。当K0′= 4时,等温体积模量为81.6(10)GPa。估计了轴向压缩性,由于a轴比c轴可压缩性小,因此存在轴向弹性各向异性。各模态的拉曼频率随压力的增加而不断增加,且拉伸模态(v3和v1)的压力依赖性大于弯曲模态(v4和v2)和外模态。计算了梅里石的等温模式grisen参数和本征非调和性。
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引用次数: 2
Boron-doped diamond synthesized by chemical vapor deposition as a heating element in a multi-anvil apparatus 在多砧装置中用化学气相沉积法合成硼掺杂金刚石作为加热元件
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-07-02 DOI: 10.1080/08957959.2020.1789618
Longjian Xie, A. Yoneda, Zhaodong Liu, K. Nishida, T. Katsura
ABSTRACT We tested boron-doped diamond (BDD) synthesized by chemical vapor deposition (CVD) as a heating element in a multi-anvil apparatus. We succeeded in manufacturing BDD into a tubular shape by laser cutting and electric discharging machining. The BDD tube shaped by the electric discharging machining was contaminated by discharging electrode materials (Mo and W), which affected the heating performance. The laser-cut BDD tube has a clean surface and, therefore, had a good heating performance. We succeeded in generating temperature as high as 2670 K at a pressure around 30 GPa with laser-cut heater. Heating reproducibility was confirmed through repeated heating and cooling cycles. The recovered sample shows that a higher temperature generation above 2670 K was prevented by eutectic melting of ZrO2 thermal insulator and Al2O3 sample. Owing to the commercial availability with a reasonable price, CVD–BDD heaters are more practical than a high-pressure synthesized BDD heaters for wide applications.
摘要在多砧实验装置中对化学气相沉积(CVD)合成的掺硼金刚石(BDD)作为加热元件进行了测试。通过激光切割和放电加工,成功地将BDD加工成管状。放电加工成型的BDD管受到放电电极材料(Mo和W)的污染,影响了加热性能。激光切割的BDD管表面干净,因此具有良好的加热性能。我们成功地利用激光切割加热器在30 GPa左右的压力下产生了高达2670 K的温度。通过反复加热和冷却循环,确认了加热的再现性。回收样品表明,ZrO2绝缘体和Al2O3样品的共晶熔化阻止了2670 K以上高温的产生。由于CVD-BDD加热器的商业化和合理的价格,在广泛的应用中比高压合成BDD加热器更实用。
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引用次数: 2
Static compression of rare earth metal holmium to 282 GPa 稀土金属钬的静态压缩至282 GPa
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-07-02 DOI: 10.1080/08957959.2020.1790552
Christopher S. Perreault, Y. Vohra
ABSTRACT The phase transitions and equation of state measurements were carried out on rare earth metal Holmium (Ho) to 282 GPa using toroidal diamond anvils thereby doubling the pressure range to which it has been studied previously. The first set of experiment employed standard beveled diamond anvils utilizing copper as an x-ray pressure standard to 217 GPa. The second set of experiment employed toroidal diamond anvils utilizing platinum as an x-ray pressure standard to 282 GPa. The recently proposed 16-atom orthorhombic structure (oF16) appeared to be stable between 103 and 282 GPa. The scaled axial ratio (c/a) shows a narrow range of variation of 1.58 ± 0.05 for the five known crystalline phases of Ho to 282 GPa. The experimental equation of state of Ho is presented up to a threefold volume compression V/Vo = 0.322.
摘要对稀土金属钬(Ho)到282的相变和状态方程进行了测量 GPa使用环形金刚石砧,从而将之前研究的压力范围扩大了一倍。第一组实验采用了标准的斜切金刚石砧,将铜作为x射线压力标准,达到217 GPa。第二组实验采用了环形金刚石砧,将铂作为x射线压力标准,达到282 GPa。最近提出的16原子正交结构(oF16)似乎在103到282之间是稳定的 GPa。标度轴向比(c/a)的变化范围很窄,为1.58 ± Ho至282的五个已知晶相为0.05 GPa。给出了Ho在三倍体积压缩V/Vo下的实验状态方程 = 0.322。
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引用次数: 6
Practical effects of pressure-transmitting media on neutron diffraction experiments using Paris–Edinburgh presses 传压介质对巴黎-爱丁堡压机中子衍射实验的实际影响
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-06-25 DOI: 10.1080/08957959.2020.1782899
T. Hattori, A. Sano‐Furukawa, S. Machida, K. Ohuchi, H. Kira, J. Abe, K. Funakoshi
ABSTRACT To understand the practical effects of pressure-transmitting media (PTM) on neutron diffraction using Paris–Edinburgh presses, diffraction patterns of MgO were collected to approximately 20 GPa using PTMs of Pb, AgCl, 4:1 methanol–ethanol (ME) mixture with and without heating, N2, and Ar. Hydrostaticity in the sample chamber estimated from the MgO 220 peak width improves in the order of Pb, AgCl, Ar, ME mixture, N2, and the heated ME mixture. Unlike previous results using diamond anvil cells, the unheated ME mixture is superior to Ar even after freezing, probably due to the cup on the anvil face. Considering these results and the sizable coherent scattering of Ne, which would show good hydrostaticity, we conclude that the ME mixture (preferably the heated one) is the best PTM in neutron experiments up to 20 GPa, while Ar can be substituted when a sample is reactive to alcohols.
摘要为了了解压力传输介质(PTM)对巴黎-爱丁堡压机中子衍射的实际影响,收集了大约20个MgO的衍射图 使用Pb、AgCl、4:1甲醇-乙醇(ME)混合物在加热和不加热、N2和Ar的情况下的PTM的GPa。根据MgO 220峰宽估计的样品室中的静水压按Pb、AgCl、Ar、ME混合物、N2和加热的ME混合物的顺序提高。与之前使用金刚石砧座细胞的结果不同,即使在冷冻后,未加热的ME混合物也优于Ar,这可能是由于砧座表面上的杯状物。考虑到这些结果和Ne的相当大的相干散射,这将显示出良好的流体静力学,我们得出结论,在高达20的中子实验中,ME混合物(最好是加热的混合物)是最好的PTM GPa,而当样品与醇反应时,Ar可以被取代。
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引用次数: 2
Refrigerated shelf-life evaluation of high pressure processed, raw and sous vide cooked lobster 高压加工龙虾、生龙虾和生龙虾的冷藏保质期评估
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-06-16 DOI: 10.1080/08957959.2020.1774753
S. Humaid, D. Nayyar, J. Bolton, B. Perkins, D. Skonberg
ABSTRACT High pressure processing (HPP) and sous vide may increase the shelf-life of high value seafood products without the use of additives. This study investigated the effects of 150MPa or 350MPa for 10min on microbial, sensory, and physicochemical qualities of raw and subsequently sous vide cooked (65°C) lobster tails during 28 days of refrigerated storage. Raw lobster pressurized at 350MPa or sous vide cooked maintained significantly lower microbial counts, total volatile base nitrogen, and biogenic amine levels. Due to off-odors, 90% and 60% of sensory respondents rejected the control and 150MPa raw samples, respectively, by day 7, while 70% rated the 350MPa samples as still acceptable on day 28. For cooked lobster, only 20% of the respondents rejected any samples by day 28. Moderate HPP conditions were effective in extending refrigerated shelf-life of vacuum-packaged raw lobster tails. However, HPP pretreatment did not contribute to additional shelf-life extension for sous vide cooked products.
摘要高压加工(HPP)和真空处理可以在不使用添加剂的情况下延长高价值海鲜产品的保质期。本研究调查了在冷藏28天期间,150MPa或350MPa持续10分钟对生龙虾尾和随后经冷藏(65°C)的龙虾尾的微生物、感官和理化性质的影响。生龙虾在350MPa的压力下加压或真空烹饪,可以显著降低微生物计数、总挥发性碱氮和生物胺水平。由于异味,90%和60%的感官受访者在第7天分别拒绝了对照和150MPa的原始样本,而70%的人在第28天认为350MPa的样本仍然可以接受。对于煮熟的龙虾,只有20%的受访者在第28天拒绝接受任何样本。适度的HPP条件有效地延长了真空包装生龙虾尾的冷藏保质期。然而,HPP预处理并没有延长冷藏产品的保质期。
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引用次数: 20
Development of a high pressure stirring cell up to 2 GPa: a new window for chemical reactions and material synthesis 高达2gpa的高压搅拌池的开发:化学反应和材料合成的新窗口
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-06-05 DOI: 10.1080/08957959.2020.1775200
Ying-Jui Hsu, A. Gordeeva, M. Antlauf, U. Häussermann, O. Andersson
ABSTRACT A new method for stirring under high pressure conditions has been developed and tested. The key component is a Teflon cell assembly equipped with magnetic stirring function, which is capable to operate across a wide pressure range, up to at least 2 GPa, in a large volume press. The setup enables adjustable stirrer rotation rate and detection of stirring in a sample, e.g. to observe liquid–solid phase transitions at high pressure. The viscosity limit of stirring is ca. 500 times that of water at room temperature (i.e. ∼500 mPas). Moreover, we show that zinc oxide nanoparticles hydrothermally synthesized at 0.5 GPa and 100°C under stirring conditions show an order of magnitude smaller size (100 nm) compared to those synthesized under non-stirring conditions (1 μm). The wide pressure range for stirring of viscous media opens interesting possibilities to produce novel materials via hydrothermal synthesis and chemical reactions.
开发并测试了一种在高压条件下搅拌的新方法。关键部件是一个具有磁力搅拌功能的聚四氟乙烯电池组件,该组件能够在宽压力范围内运行,最高可达2 GPa,在大容量印刷机中。该设置能够调节搅拌器转速并检测样品中的搅拌,例如在高压下观察液固相转变。搅拌的粘度极限约为室温下水粘度的500倍(即~500 mPas)。此外,我们发现氧化锌纳米颗粒在0.5 GPa和100°C在搅拌条件下显示出较小尺寸(100 nm)与在非搅拌条件下合成的那些(1 μm)。粘性介质搅拌的宽压力范围为通过水热合成和化学反应生产新型材料开辟了有趣的可能性。
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引用次数: 2
Compression of CsCl and CsBr in the megabar range CsCl和CsBr在兆巴范围内的压缩
IF 2 4区 物理与天体物理 Q3 PHYSICS, MULTIDISCIPLINARY Pub Date : 2020-06-03 DOI: 10.1080/08957959.2020.1774754
A. Dewaele
ABSTRACT The quasi-hydrostatic compression of cesium chloride and cesium bromide has been measured with X-ray diffraction up to 141 GPa at 300 K. A cubic to orthorhombic transition, with a ≥10% distortion of lattice parameters, is evidenced in CsBr around 60 GPa. A smaller distortion (∼1.5%) appears in CsCl at the same pressure, followed by a likely transition to a lower symmetry phase which starts at 134 GPa. P−V compression curves yield equation of state parameters in line with those of other B2 alkali halides.
摘要用X射线衍射测量了氯化铯和溴化铯的准流体静力压缩,压缩系数高达141 300时的GPa K.CsBr在60左右证明了晶格参数畸变≥10%的立方向正交转变 GPa。在相同压力下,CsCl中出现较小的畸变(~1.5%),随后可能从134开始过渡到较低的对称相 GPa。P−V压缩曲线产生的状态方程参数与其他B2碱金属卤化物的状态方程一致。
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引用次数: 2
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