岩石内应力的X射线-中子散射测量方法

岩石内应力的储存和释放对深地资源和能源开发具有重要约束。矿物晶格间距的动态变化是揭示岩石内应力演化的重要指示。X射线衍射法是当前获取矿物晶体结构的主要手段,可以准确测定矿物的特征衍射峰。但是,对于具有复杂结构和矿物组成的岩石,X射线在穿透过程中携带的统计信息,难以反映矿物晶格间距的细节特征。中子射线的能量高、穿透深度大,且与原子核反应,因而能更准确地刻画矿物元素位置和结构细节,但中子的波长较长、校准困难,结果具有不确定性,导致中子射线在岩石内应力研究中未能发挥应有作用。在分析X射线、中子技术优势和固有局限的基础上,提出了岩石内应力的X射线-中子衍射测量方法,重点剖析了该方法的基本原理,提出了该方法的关键技术与研究前景。得出了如下结论:利用X射线在确定岩石矿物晶格参数的优势,结合加热处理等技术,可实现岩石矿物无应力条件下晶格间距的标定; 采用中子衍射技术可精确测量岩石矿物的衍射偏移峰,实现岩石内应力深度轮廓的精准刻画; 结合X射线与中子的优势,可实现岩石内应力绝对值的精确测量。提出的技术手段有利于揭示岩石内应力的微观储存和释放过程,以及长期存留的物质条件和物理力学机制,并有望为岩石矿物组成和微观结构研究提供一种新的技术方案。     

Room-temperature equation of state of Li<Subscript>2</Subscript>VOSiO<Subscript>4</Subscript> up to 8.5 GPa

High-pressure single-crystal X-ray diffraction measurements of lattice parameters of the compound Li₂VOSiO₄, which crystallises with a natisite-type structure, has been carried out to a pressure of 8.54(5) GPa at room temperature. Unit-cell volume data were fitted with a second-order Birch-Murnaghan EoS (BM-EoS), simultaneously refining V ₀ and K ₀ using the data weighted by the uncertainties in V. The bulk modulus is K ₀ = 99(1) GPa, with K′ fixed to 4. Refinements of third order equations-of-state yielded values of K′ that did not differ significantly from 4. The compressibility of the unit-cell is strongly anisotropic with the c axis (K ₀(c) = 49.7 ± 0.5 GPa) approximately four times more compressible than the a axis (K ₀(a) = 195 ± 3 GPa).     

斜方辉石的反演畴结构对其衍射效应的影响

斜方辉石内部存在着众多的相邻间呈反演关系的(100)晶畴。这些晶畴的存在使斜方辉石的K为奇数的okl衍射之强度明显减弱,且参与衍射的晶畴的数目越多,其减弱的程度也就越大。这一现象在一定程度上掩盖了斜方辉石P2_(1ca)的真实对称性。与X射线衍射相比,利用电子衍射来研究斜方辉石的空间群类型具有明显的优越性。     

From geometry to dynamics of microstructure: using boundary lengths to quantify boundary misorientations and anisotropy

The microstructure of a quartzite experimentally deformed and partially recrystallised at 900 °C, 1.2 GPa confining pressure and strain rate 10⁻⁶/s was investigated using orientation contrast and electron backscatter diffraction (EBSD). Boundaries between misoriented domains (grains or subgrains) were determined by image analysis of orientation contrast images. In each domain, EBSD measurements gave the complete quartz lattice orientation and enabled calculation of misorientation angles across every domain boundary. Results are analysed in terms of the boundary density, which for any range of misorientations is the boundary length for that range divided by image area. This allows a more direct comparison of misorientation statistics between different parts of a sample than does a treatment in terms of boundary number.The strain in the quartzite sample is heterogeneous. A 100×150 μm low-strain partially recrystallised subarea C was compared with a high-strain completely recrystallised subarea E. The density of high-angle (>10°) boundaries in E is roughly double that in C, reflecting the greater degree of recrystallisation. Low-angle boundaries in C and E are produced by subgrain rotation. In the low-angle range 0–10° boundary densities in both C and E show an exponential decrease with increasing misorientation. The densities scale with exp(−θ/λ) where λ is approximately 2° in C and 1° in E; in other words, E has a comparative dearth of boundaries in the 8–10° range. We explain this dearth in terms of mobile high-angle boundaries sweeping through and consuming low-angle boundaries as the latter increase misorientation through time. In E, the density of high-angle boundaries is larger than in C, so this sweeping would have been more efficient and could explain the relative paucity of 8–10° boundaries.The boundary density can be generalised to a directional property that gives the degree of anisotropy of the boundary network and its preferred orientation. Despite the imposed strain, the analysed samples show that boundaries are not, on average, strongly aligned. This is a function of the strong sinuosity of high-angle boundaries, caused by grain boundary migration. Low-angle boundaries might be expected, on average, to be aligned in relation to imposed strain but this is not found.Boundary densities and their generalisation in terms of directional properties provide objective measures of microstructure. In this study the patterns they show are interpreted in terms of combined subgrain rotation and migration recrystallisation, but it may be that other microstructural processes give distinctive patterns when analysed in this fashion.     

电子背散射衍射和傅里叶变换红外光谱结合测量橄榄石的原位含水量

橄榄石的含水量对上地幔的物理化学性质具有重要影响。傅里叶变换红外光谱（简称FTIR） 是目前最常用的测量名 义上无水矿物含水量的方法。由于矿物中红外光谱的吸收系数是各向异性的,理论上应使用偏振光来测量橄榄石的含水 量,但是该方法需要把橄榄石颗粒分离出来进行定向,非常费时。前人大多使用非偏振光来测量薄片中多个橄榄石的含水 量,并使用Paterson （1982） 的校正方法计算样品中橄榄石的平均含水量。非偏振光的使用忽略了颗粒定向造成的影响,会 低估橄榄石的含水量。上地幔橄榄石常发育晶格优选定向,为快速准确地获得橄榄石的原位含水量,该文将电子背散射衍 射技术（EBSD） 与FTIR 相结合,提出测量薄片中橄榄石含水量的新方法。首先使用Bell 等（2003） 的红外偏振光实验结 果,通过橄榄石[100]、[010]和[001]方向的含水量吸收系数建立一个椭球体。然后使用EBSD 测量某一颗粒在薄片中的取 向,根据欧拉角计算该方向的含水量吸收系数Ws,再根据Beer-Lambert 公式获得该颗粒的含水量。对加拿大Slave 克拉通 Muskox 金伯利岩携带的石榴橄榄岩中橄榄石的含水量研究表明,该方法可用于测量显微尺度的橄榄石原位含水量分布,为 橄榄石含水量与组构关系的研究提供基础资料。     

Estimating the settling velocity of bioclastic sediment using common grain‐size analysis techniques

Most techniques for estimating settling velocities of natural particles have been developed for siliciclastic sediments. Therefore, to understand how these techniques apply to bioclastic environments, measured settling velocities of bioclastic sedimentary deposits sampled from a nearshore fringing reef in Western Australia were compared with settling velocities calculated using results from several common grain‐size analysis techniques (sieve, laser diffraction and image analysis) and established models. The effects of sediment density and shape were also examined using a range of density values and three different models of settling velocity. Sediment density was found to have a significant effect on calculated settling velocity, causing a range in normalized root‐mean‐square error of up to 28%, depending upon settling velocity model and grain‐size method. Accounting for particle shape reduced errors in predicted settling velocity by 3% to 6% and removed any velocity‐dependent bias, which is particularly important for the fastest settling fractions. When shape was accounted for and measured density was used, normalized root‐mean‐square errors were 4%, 10% and 18% for laser diffraction, sieve and image analysis, respectively. The results of this study show that established models of settling velocity that account for particle shape can be used to estimate settling velocity of irregularly shaped, sand‐sized bioclastic sediments from sieve, laser diffraction, or image analysis‐derived measures of grain size with a limited amount of error. Collectively, these findings will allow for grain‐size data measured with different methods to be accurately converted to settling velocity for comparison. This will facilitate greater understanding of the hydraulic properties of bioclastic sediment which can help to increase our general knowledge of sediment dynamics in these environments.     

High-pressure X-ray and Raman study of a ferrian magnesian spodumene

The high-pressure behaviour of a synthetic P2₁/c ferrian magnesian spodumene, ^M2 (Li_0.85Mg_0.09Fe²⁺ _0.06)^M1(Fe³⁺ _0.85Mg_0.15)Si₂O₆, has been investigated using in situ single-crystal X-ray diffraction and Raman spectroscopy. No phase transition has been observed within the pressure range investigated. The isothermal equation of state up to 7 GPa was determined. V₀, K_T0 and K, simultaneously refined with a Murnaghan equation of state, are: V₀= 415.66(7) ų, K_T0=83(1) GPa and K=9.6(6). The magnitudes of the principal unit-strain coefficients were calculated and their ratios 1:2:3=1.00:1.85:2.81 at P=6.83 GPa indicate a very strong anisotropy. Monitoring of the intensity of b-type reflections (h+k= 2n+1) confirms that from room conditions up to 7 GPa the primitive lattice is maintained. Raman spectra have been collected up to 7.4 GPa. No change in the number of observed vibrational modes occurs in the pressure range investigated. At high frequency, the Raman doublet relative to the Si–O–Si vibrations of the two distinct tetrahedral chains is a broad band at room pressure, however, the frequency difference between the two modes increases with increasing pressure.Operating system: Windows NT