Feng Yejun, Jaramillo R, Wang Jiyang, Ren Yang, Rosenbaum T F
The Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, USA.
Rev Sci Instrum. 2010 Apr;81(4):041301. doi: 10.1063/1.3400212.
Condensed matter experiments at high pressure accentuate the need for accurate pressure scales over a broad range of temperatures, as well as placing a premium on a homogeneous pressure environment. However, challenges remain in diamond anvil cell technology, including both the quality of various pressure transmitting media and the accuracy of secondary pressure scales at low temperature. We directly calibrate the ruby fluorescence R1 line shift with pressure at T=4.5 K using high-resolution x-ray powder diffraction measurements of the silver lattice constant and its known equation of state up to P=16 GPa. Our results reveal a ruby pressure scale at low temperatures that differs by 6% from the best available ruby scale at room T. We also use ruby fluorescence to characterize the pressure inhomogeneity and anisotropy in two representative and commonly used pressure media, helium and methanol:ethanol 4:1, under the same preparation conditions for pressures up to 20 GPa at T=5 K. Contrary to the accepted wisdom, both media show equal levels of pressure inhomogeneity measured over the same area, with a consistent DeltaP/P per unit area of +/-1.8 %/(10(4) microm(2)) from 0 to 20 GPa. The helium medium shows an essentially constant deviatoric stress of 0.021+/-0.011 GPa up to 16 GPa, while the methanol:ethanol mixture shows a similar level of anisotropy up to 10 GPa, above which the anisotropy increases. The quality of both pressure media is further examined under the more stringent requirements of single crystal x-ray diffraction at cryogenic temperature. For such experiments we conclude that the ratio of sample-to-pressure chamber volume is a critical parameter in maintaining sample quality at high pressure, and may affect the choice of pressure medium.
高压下的凝聚态物质实验凸显了在广泛温度范围内精确压力标度的必要性,同时也对均匀压力环境提出了很高要求。然而,金刚石对顶砧技术仍存在挑战,包括各种压力传递介质的质量以及低温下二级压力标度的准确性。我们利用银晶格常数的高分辨率X射线粉末衍射测量及其已知的状态方程,在T = 4.5 K下直接校准了红宝石荧光R1线随压力的变化,压力范围可达P = 16 GPa。我们的结果表明,低温下的红宝石压力标度与室温下最佳可用的红宝石标度相差6%。我们还利用红宝石荧光来表征两种具有代表性且常用的压力介质——氦气和甲醇:乙醇4:1——在T = 5 K、压力高达20 GPa的相同制备条件下的压力不均匀性和各向异性。与普遍看法相反,在相同面积上测量时,两种介质显示出相同水平的压力不均匀性,从0到20 GPa,每单位面积的ΔP/P一致为±1.8 %/(10⁴ 微米²)。氦介质在高达16 GPa时显示出基本恒定的偏应力0.021±0.011 GPa,而甲醇:乙醇混合物在高达10 GPa时显示出类似水平的各向异性,高于此压力各向异性增加。在低温下单晶X射线衍射的更严格要求下,对两种压力介质的质量进行了进一步研究。对于此类实验,我们得出结论,样品与压力腔体积之比是在高压下保持样品质量的关键参数,并且可能影响压力介质的选择。