Electron Diffraction Patterns of Plesiotwinning of Fe-Illite

1 Introduction Micas are a series of layer silicates (phyllosilicates). Many clay minerals, such as muscovite, celadonite, illite, phengite, belong to the mica series and possess the same basic crystallographic symmetries. Illite is a kind of micas whose unit structure consists of one octahedral sheet in between two opposing tetrahedral sheets. These sheets form a basic 2:1 layer that is linked by interlayer cations. Mica twinnings and twin laws (Donnay et al., 1964; Rieder, 1970) have been …     

用于同位素测年的自生伊利石分离纯化流程探索

沉积岩中自生矿物与碎屑矿物的分离问题是制约沉积岩定年的主要问题之一.本文以浙江和川西地区的粘土矿物为例,介绍了沉积岩中自生伊利石与碎屑矿物的一般分离过程,具体包括悬浮液的制备过程、高速离心机的条件实验和8个样品的分级实验,确定了较佳的分级参数,并对分级后的各级别进行了X-射线衍射(XRD)分析.X-射线衍射结果表明,随着粒度的减小,各种杂质的含量都在逐渐减少,在小于0.2 μm的粒级中,已检测不出石英、钾长石、钠长石、方解石、白云石等杂质的存在,其中有3个产品的成岩混层含量达到100%,,说明本次实验的分离纯化流程是比较成功的.综合考虑粒度和自生伊利石的纯度,一般情况下,以0.1~0.2 μm粒级的产品用于Ar-Ar和K-Ar测年较合适.但在实际进行年龄分析时,一定要先进行XRD和透射电镜分析,只有确定其成岩混层I/S的含量近100%(至少在95%以上)及混层中S的含量小于25%时,才可用于Ar-Ar和K-Ar年龄测定.     

吉林省东部石炭-二叠系伊利石的成因标志

吉林东部石炭-二叠系主要是一套泥质岩石, 其详细深入的矿物学工作尚不多见。利用JSM-6700F场发射电镜及INCA能谱仪,研究了伊利石的显微形貌和微区成分。采用D/max-2500 X-射线衍射仪,研究了伊利石的结晶度、多型和b₀值。结果表明:研究区伊利石结晶度变化于0.26~0.77,平均值为0.44;伊利石（白云母）多型有3种类型,分别为1M_d型、1M_d+2M₁混合型和2M₁型;伊利石（白云母）b₀值为8.996~9.045,平均值为9.007Å。石炭系伊利石结晶度变化于0.26~0.50,平均值为0.35,主要呈2M₁多型,b₀平均值为9.011Å,主要是低级近变质带的产物;二叠系伊利石结晶度变化于0.26~0.50,平均值为0.42,主要为1M_d+2M₁混合型多型,b₀平均值为9.004Å,主要为晚期成岩带的产物。     

Illite Crystallinity Mapping of Very Low Grade Metamorphism of Triassic Metapelites in the Zoigê Area, Western China

X-ray diffraction methods for estimating the metamorphic grade of diagenetic, anchizone and epizone in metapelites are reviewed and applied to samples from a 7000?m+ borehole in western China and surface samples from the surrounding Zoigê area. Kübler’s illite crystallinity (IC) measurements provide more consistent results than calculated values of percentage of illite in the I/S mixed layers and percentage of I/S mixed layers. Down-borehole IC values display a typical burial metamorphic relationship between stratigraphic level and IC. A method for preparing very low grade metamorphic maps is described, and isograds plotted on a regional geological map at selected values of IC, delineating a high temperature diagenetic zone, an anchizone, and an epizone. The map shows that IC values are controlled by stratigraphic level in the north of the study area (i.e. burial metamorphism), and proximity to an igneous intrusive body in the south (i.e. contact metamorphism).     

天津蓟县二维纳米级伊利石研究

天津蓟县中元古界串岭沟组上部黑色页岩产有丰富的伊利石,其矿物组合仅为石英和伊利石,是重要的可利用伊利石资源。运用化学成分分析和XRD方法确定出伊利石含量为64％～70％。由Scherrer方程计算的平均c^*轴方向厚度为12nm,平均6轴方向长度为167nm,结合伊利石的片状生长习性,可确定串岭沟组上部黑色页岩所产伊利石为二维纳米级伊利石,具有重要的纳米属性。化学成分分析表明,黑色页岩所产伊利石具有0．75的层间电荷和二八面体为主的二八-三八面体的过渡类型八面体结构特点。对数正态粒度大小的分布特征表明黑色页岩中的伊利石经历了由成核→等体积转移→最终长大的Ostwald成熟效应。     

浙江渡船头“伊利石”应属绢云母

渡船头云母状矿物长期以来被称为“伊利石”,近期经过X射线衍射(XRD)、红外光谱(IR)、差热分析(DTA)、电子显微镜(EM)观察及化学组成等研究后显示:这种呈薄鳞片状、粒度很细(一般小于5μm)、结晶度高的矿物,其d(002)=9.95?,为2M多型,出现特征的3625cm~(-1)、3450cm~(-1)、1020cm~(-1)、935cm~(-1)、825cm~(-1)、799cm~(-1)、755cm~(-1)、543cm~(-1)、480cm~(-1)红外吸收和40—70℃、106.4—111.2℃两弱吸热谷及630—670℃强吸热谷;矿物MgO小于0.25%,结构中八面体Mg~(2+)量小于0.03,以Al~(3+)和Fe~(3+)为主,八面体电荷为-0.052—+0.048/O_(10)(OH)_2,K_2O一般大于9%。上述这些均表明,渡船头“伊利石”应属绢云母。     

蒙脱石、高岭石、伊利石对重金属离子吸附容量的实验研究

在pH=4,t=23℃和微量浓度条件下,不改变离子浓度,通过增加吸附液体积进而增加体系中重金属离子含量的方法进行了蒙脱石、伊利石、高岭石对Cu2+、Pb2+、Zn2+、Cd2+、Cr3+等重金属离子吸附容量的实验研究,结果表明,3种矿物吸附容量大小顺序为蒙脱石>伊利石>高岭石,与其阳离子交换容量密切相关.Cu-蒙脱石和Cr-蒙脱石的X射线衍射结果表明,Cu2+、Cr3+通过离子交换作用进入了蒙脱石的层间.同一矿物对不同重金属离子也有不同的吸附容量蒙脱石Cr3+>Cu2+>Zn2+>Cd2+>Pb2+;高岭石Cr3+>Pb2+>Zn2+>Cu2+>Cd2+;伊利石Cr3+>Zn2+>Cd2+>Cu2+>Pb2+.     

Illite/smectite transformation in detrital glaucony during burial diagenesis of sandstone: A study from Siri Canyon – Danish North Sea

Detrital glaucony in the Palaeogene glauconitic sandstones in Siri Canyon, Danish North Sea, has been analysed from 15 exploration wells by X‐ray diffraction, electron microprobe and scanning electron microscopy. These sandstones consist of mixed‐layer illite/smectite and have a large variability in chemical composition and structure. In the most shallow wells (ca 1700 m), the glaucony is rich in Fe and consists of mixed‐layer illite/smectite with random‐interstratification (R = 0). In the depth interval from 1700 to 2000 m, the composition changes as Si is incorporated. The structure changes to ordered R = 1. Further increase in burial leads to the loss of Fe. Ordered R = 3 mixed‐layer illite/smectite is recognized from burial depths of 2200 m. The proportion of illite in illite/smectite mixed layers increases only slightly with depth and temperature. Although the structural changes generally are associated with chemical changes, they can also take place isochemically when the detrital glaucony is tightly embedded in earlier cement, which prevented chemical exchange. The glaucony transformation in the Siri Canyon sandstones partly reflects a supply of Si and partly significant loss of Fe. Thus, the glaucony transformation relates to the general diagenesis of the host sandstone. These sandstones are cemented by microquartz at an early stage, followed by precipitation of Fe‐rich grain‐coating berthierine or chlorite.     

福建宁德下洋伊利石矿矿床地质特征及成因探讨

宁德下洋伊利石矿呈脉状产出,贮存于晚侏罗世南园组火山碎屑岩石中,共发现有3个矿体。矿石可分为石英一伊利石型及叶蜡石伊利石型。矿体受北东向断裂控制,由火山碎屑岩经过热液交代形成。     

Suitability of Mn‐ and Fe‐Rich Reference Materials for Microanalytical Research

Manganese‐ and iron‐rich materials are of major geoscientific and economic interest, many of which contain microscopic features that provide valuable information. To obtain accurate results, a homogeneous microanalytical reference material for calibration is needed. Several researchers have used the Mn‐ and Fe‐rich RMs, JMn‐1, NOD‐A‐1, NOD‐P‐1 and FeMn‐1, for this purpose; therefore, they were tested in this study to determine their suitability for microanalysis. Their homogeneity was investigated by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) with two different types of lasers (nano‐ and femtosecond), with spot and line scan analyses and with different operating parameters, such as spot size, pulse repetition rate and fluence. As the established manganese nodule RMs revealed inhomogeneities for picogram to microgram test portions, we also investigated the new synthetic Fe‐ and Mn‐rich RM, FeMnOx‐1. FeMnOx‐1 was found to be homogeneous for large (ø 40 μm: 2% RSD repeatability) and small (ø 8–10 μm: 10% RSD repeatability) spot sizes. This homogeneity is in the range of the homogeneous NIST SRM 610 and GSE‐1G reference glasses. Furthermore, FeMnOx‐1 revealed a large‐scale homogeneity within uncertainties of a few per cent, using test portions in the ng range, when measuring four individual mounts of this material.     

A Practical Method for Accurate Measurement of Trace Level Fluorine in Mg‐ and Fe‐Bearing Minerals and Glasses Using Electron Probe Microanalysis

Fluorine plays an important role in magmatic and hydrothermal processes, but due to its low abundance in geological samples determining F is difficult by electron probe microanalysis. By using a W‐Si multi‐layered pseudocrystal as the diffraction crystal instead of thallium acid phthalate (TAP), count rates were considerably higher, which however introduced spectral interferences between FKα and FeLα and MgKβ lines when normal integral mode is applied. In this study, we developed a protocol using a W‐Si multi‐layered pseudocrystal for measuring accurately trace level F in both minerals and glasses. First, we used differential mode with an optimised PHA (pulse height analysis) setting in signal processing, instead of normal integral mode, which completely eliminated the second‐order MgKβ line. Second, the overlap of the first‐order FeLα on FKα peak, which cannot be filtered by modifying the PHA setting, was calibrated quantitatively using F‐free minerals and silicate glasses. Applying this two‐step method, F was determined in a number of reference glasses, as well as in glasses synthesised from powders of the rock reference materials AC‐E, GS‐N and DR‐N. Our data are consistent within error with F concentrations determined by other methods, demonstrating the reliability of this method.     

叶腊石微结构及其晶体结构缺陷的高分辨透射电镜分析

采用场发射扫描电镜（FE-SEM）、高分辨透射电镜（HRTEM）结合选区电子衍射（SAED）、X射线粉晶衍射（XRD）及X射线荧光光谱（XRF）等对浙江青田叶腊石的微结构特征进行较系统的研究。结果表明：①粉晶X射线衍射证实青田叶腊石具有典型的单斜晶系特征,该结论与叶腊石粉体选区电子衍射结果吻合,且其伴生矿为石英。②叶腊石微晶体呈＂复式板片＂构型,且＂复式＂板片中薄片厚度约为8±2 nm。③在高能电子束辐照下,叶腊石矿物颗粒形貌及晶格结构发生明显的改变,且由此产生晶格膨胀,并最终形成非晶态。     

Kübler Index and K-Ar Ages of Illite in the Yinshan Polymetallic Deposit, Jiangxi Province, South China: Analyses and Implications

Abstract. The Yinshan polymetallic deposit is a hydrothermal vein-type deposit closely related to Late Jurassic felsic-inter-mediate volcanic-subvolcanic activity in Jiangxi Province, South China. Illite is a major alteration mineral observed in the deposit. Our study shows that the Kübler index of the illite has a close relation to ore-forming fluids of different stages of hydrothermal alteration and mineralization. The early Pb-Zn-Ag mineralization dated at 130–136 Ma is characterized by relatively low water/rock ratios and diffusive fluid movement within phyllite, whereas the later Cu-Au-S mineralization at 122 -125 Ma was accompanied by higher water/rock ratios and localized fluid flow through fractures and channels. Illite formed in the early Pb-Zn-Ag mineralization stage contains swelling layers while the illite formed in the later Cu-Au-S mineralization stage has no swelling layers but was associated with intensive chloritization. The last stage of mineralization (at 104 Ma) was minor and did not produce significant amounts of illite.     

Ultra‐high temperature metamorphism recorded in Fe‐rich olivine‐bearing migmatite from the Khondalite Belt,North China Craton

We document the first occurrence of Fe‐rich olivine‐bearing migmatitic metapelite in the Khondalite Belt, North China Craton. Petrological analyses revealed two exotic assemblages of orthopyroxene+spinel+olivine and orthopyroxene+spinel+cordierite. Phase relation modelling suggests that these assemblages are diagnostic of ultra‐high temperature (UHT) metamorphism in the Fe‐rich system, with temperatures from 1,000 to 1,050°C at 0.6 GPa. U–Th–Pb SIMS analyses on zircon reveal a similar age of c. 1.92 Ga for the olivine‐bearing migmatite and an adjacent gabbronoritic intrusion that is therefore identified as the heat source for the UHT metamorphism. These results, coupled with additional analysis of the famous Tuguiwula sapphirine‐bearing granulite, lead to a re‐appraisal of the P–T path shape and heat source for the UHT metamorphism. We suggest that UHT metamorphism, dated between 1.92 and 1.88 Ga, across the whole Khondalite belt, proceeded from a clockwise P–T evolution with an initial near‐isobaric heating path at ~0.6–0.8 GPa, and a maximum temperature of 1,050°C followed by a cooling path with minor decompression to ~0.5 GPa. Considering our results and previous works, we propose that the orogenic crust underwent partial melting at temperature reaching 850°C and depth of ~20 to ~30 km during a period of c. 30 Ma, between 1.93 and 1.90 Ga. During this time span, the partially molten crust was continuously intruded by mafic magma pulses responsible for local greater heat supply and UHT metamorphism above 1,000°C. We propose that the UHT metamorphism in the Khondalite belt is not related to an extensional post‐collisional event, but is rather syn‐orogenic and associated with mafic magma supplies.     

Illite Crystallinity Mapping of Very Low Grade Metamorphism of Triassic Metapelites in the Zoig(e) Area,Western China

X-ray diffraction methods for estimating the metamorphic grade of diagenetic,anchizone and epizone in metapelites are reviewed and applied to samples from a 7000 m+ borehole in western China and surfac...     

黑硼锡镁矿孪晶的电子衍射分析

黑硼锡镁矿是1985年在我国发现的一种新矿物,微孪晶特别发育,其电子衍射斑点往往具规律的分裂现像。用选区电子衍射获得[010]、[141]和[121]定向带轴电子衍射斑点分裂图,经矩阵分析,确定两套斑点分裂是由其呈挛晶结构关系所致,孪晶面为(101),属于面律孪晶,这种孪晶的微形貌由明场像(BF)得到证实。根据不同取向的电子衍射图,确定该矿物属单斜晶系,a_0=10.7,b_0=3.01,c_0=5.39,β=94.5°。上述挛晶结构特征及其晶体学数据与X射线单晶研究结果有很好的可比性。     

焉耆盆地包裹体特征和伊利石测年对油气成藏期次的指示

焉耆盆地侏罗系储层中流体包裹体主要分布于三工河组和八道湾组,其均一温度多为101～110 ℃和121～130 ℃,组分中的正构烷烃碳数呈双峰态,前主峰碳为nC₁₈或C₂₀,后主峰碳为nC₂₆或nC₂₇。这些特征指示盆地在侏罗纪中晚期发生两次成藏作用;而储层中自生伊利石同位素测年同样指示了博湖坳陷北部凹陷油气的两次成藏时期,即中晚侏罗世（142.26～183.15 Ma）和白垩纪（75.07～142.26 Ma）。南部凹陷和本布图构造带的油气成藏期分别为中侏罗世、中晚侏罗世-早白垩世,同时纵向上在同一构造带内,K-Ar年龄随埋深增加而变大,反映油气自构造低部位向高部位逐渐充注运移和调整。     

应用流体包裹体和自生伊利石测年重构鄂尔多斯盆地侏罗系油藏烃类充注史

中生界侏罗系是鄂尔多斯盆地重要的石油勘探与开发目的层之一,侏罗系油藏受前侏罗纪古地貌影响较为显著。本文通过流体包裹体特征分析、均一化温度测定和包裹体丰度（GOI）分析、定量颗粒荧光（QGF、QGF-E）研究以及储集层自生伊利石K-Ar定年等实验方法和手段的应用,对鄂尔多斯盆地侏罗系油气包裹体特征进行了精细描述及定量化分析研究,揭示了侏罗系油藏形成时间、充注过程及油气包裹体与油气运移、成藏的关系。研究结果表明：侏罗系油藏存在晚期充注,早期充注少或油藏遭受调整,早期生成的烃类现今仅以沥青的形式赋存,现今烃类流体主要为晚期成藏的产物。侏罗系石油大规模充注期为（108.3±2.0）~（116.5±2.0）Ma（早白垩世中期）,具有垂向运移聚集的特点。鄂尔多斯盆地侏罗系油藏早期受岩性和构造双重控制,晚期构造活动调整了油气藏的形态及局部富集。侏罗系在晚期成藏过程中没有形成过叠合连片的大规模的油藏,只在局部构造上形成规模较小的“小而肥”的独立油藏。     

Provenance Study of Fe–Ti Oxide Minerals in the Quaternary Sediments in Yichang Area and Its Implication of Formation Time of the Yangtze Three Gorges, China

The Three Gorges are considered to be critical to understand the formation of Yangtze River. Recent research results suggest that the Yangtze Three Gorges was created during the Quaternary but the exact time is debatable. Fe–Ti oxide minerals are seldom used to study sediment provenance, expecially using scanning electron microscopy(SEM), and energy dispersive spectrometer(EDS). In this study, the provenance of Quaternary sediments in Yichang area, which is located to the east of the Yangtze Three Gorges, was investigated by using SEM and EDS to research Fe–Ti oxides. The Panzhihua vanadium titanomagnetite and Emeishan basalt outcrop are located to the west of the Three Gorges. Further, the materials from them are observed in the Quaternary sediments of Yichang area. Fe–Ti oxide minerals from the Huangling granite are observed in the Yunchi and Shanxiyao Formations, which were formed before 0.75 Ma B.P., whereas Fe–Ti oxide minerals from the Huangling granite, Panzhihua vanadium titanomagnetite, and Emeishan basalt are observed in the riverbed and fifth-terrace sediments of the Yangtze River, which were formed after 0.73 Ma B.P.. Thus, we can infer that the Three Gorges formed after the deposition of the Shanxi Formation and before the fifth-terrace; i.e., 0.75–0.73 Ma B.P..     

Study of the Stacking Sequences of an Irregular Mixed—Layer Illite / Smectite (I / S) Clay Mineral1

Abstract There are two aspects in the study of irregular mixed—layer clay minerals: one is the kinds and ratios of their basic structural unit layers and the other is the junction probabilities of the unit layers. Irregular mixed—layer illite / smectite clay minerals (I / S) are widespread in nature. While studying the clay minerals from the Permian—Triassic (P / T) boundary bed, the authors found that I / S clay minerals are developed in all P / T boundary clay layers in areas from the northwest to southeast of China. Systematic mineralogical studies of the I / S clay minerals from Hunan, Hubei, Sichuan and Zhejiang were made by means of X—ray, infrared spectroscopic, electron microscopic and chemical analyses and a deepened study of the stacking sequences of their structural unit layers was conducted by the MacEwan one—dimentional direct Fourier transform. It was found that the stacking of the illite and smectite crystal layers along the c axis can be derived from Fibonacci sequences. Hence, the authors propose that such I / S clay minerals are possessed of two—dimentional crystal lattice and one—dimentional quasicrystal lattice.