U-Th-Pb副矿物的原地原位测年微束分析方法比较与微区晶体化学研究

系统地对比分析了各种微束分析技术在原地原位测年中的优势和局限性,并对近年发展的微区原位化学测年技术(EPMA)和质子激发X射线微探针分析技术(μ-PIXE)进行了探讨.阐明了矿物微区晶体化学研究的各种方法及其对实现精确原地原位测年的重要性.介绍了北大别黄土岭麻粒岩锆石测定点的晶体化学特征,应用激光剥蚀微探针-感应耦合等离子体质谱(LAM-ICPMS)技术对其进行了锆石的U-Pb表面年龄的测定,结果表明该岩石的麻粒岩相变质发生在2.050 Ga前,锆石来源为多源区.     

离子探针锆石U-Pb定年

锆石是大型离子探针U-Pb定年技术应用最早和最广的矿物,离子探针U-Pb定年可以有效获取粒径微小锆石或具有复杂环带结构的锆石中不同区域的年龄信息。文中以Cameca IMS 1280型离子探针为例,对离子探针锆石U-Pb定年原理、仪器分析流程、数据校正方法和数据误差分析等多方面进行综述,并总结了近年来离子探针锆石U-Pb定年技术新进展。     

锆石地球化学特征及地质应用研究综述

介绍并对比了用于锆石等副矿物测试的离子探针、激光探针、电子探针、质子探针等几种微区原位测试技术各自的特点.锆石U-Pb定年实现了对同一锆石颗粒内部不同成因的锆石域进行原位年龄的分析,给出了有关寄主岩石的源岩、地质演化历史等重要信息,为地质过程的精细年龄框架的建立提供了有效的途径.锆石微量元素、同位素特征是译解岩石来源和成因的指示器.锆石Hf同位素已成功地用于地球早期历史、岩浆来源、壳幔相互作用、区域大陆地壳增长的研究等;锆石氧同位素组成能有效地约束壳幔相互作用和示踪岩浆来源等.     

中-浅正变质岩锆石SHRIMP法与TIMS法测年结果不一致处理——以滇东南南温河花岗岩为例

变质岩中的锆石大多遭受变质热事件的改造,但中-浅变质岩一般不甚发育新生锆石或变质增生边,不易通过现有的锆石测年技术获得该岩石的变质年龄。中-浅正变质岩的锆石为岩浆锆石与变质增生锆石的混合物,其U-Pb同位素组成可以采用二端元混合模式来表达。利用同位素稀释法(TIMS)可以获得混合锆石U-Pb年龄及对应的同位素组成;结合CL等内部结构分析,利用离子探针法(SHRIMP)可以获得岩浆锆石U-Pb年龄及对应的同位素组成,进而推算出变质增生锆石U-Pb年龄对应的同位素组成。在对滇东南南温河花岗岩锆石U-Pb年代学的研究中,我们发现同一样品的SHRIMP与TIMS U-Pb法测年结果不一致,根据上式推算出后期主变质年龄约为230 Ma,与前人利用其它测年方法获得的结果基本一致,符合研究区主变质期为印支期的区域地质背景。该方法为中-浅正变质岩年代学研究提供了一种新思路。     

区域变质岩系锆石U-Pb法年龄低值解释问题

锆石U-Pb法以其矿物母体封闭性好等特点是岩石测年的优选方法之一,特别是对于变质岩石年龄的测定被广泛采用.区域变质岩系中的锆石普遍具有环边结构,内核是变质原岩(如辉长岩、闪长岩)形成时就存在的锆石,环边是变质过程中新生的锆石.对环边锆石U-Pb法测定所获得的同生变质岩石的年龄值,常存在较大的变化范围.例如Ames等采用锆石U-Pb法所获的大别山变质榴辉岩的年龄为(208.6±2.4)Ma[1],刘贻灿等用同样方法获得该区榴辉岩年龄为(230±6.0)Ma[2].这种差值的产生,如非测试误差,一般认为它反映变质过程不同阶段的年龄.高值为变质峰期的年龄,低值为退变质时期的年龄.然而,对于低值应为退变质期年龄的解释迄今尚缺乏Zr的地球化学论据,变质新生的环边锆石Zr的来源及其可运移性能的研究,是揭示U-Pb法年龄差值原因的关键.     

U-Pb同位素测年新方法——激光烧蚀等离子体质谱法直接测定探针片中锆石和磷灰石年龄

通过实验研究,笔者确定了激光烧蚀等离子体质谱法直接测定探针片中锆石、磷灰石U-Pb同位素年龄的流程,包括样品制备、矿物成因分析、仪器测试条件和测试过程。该方法最大的优势在于,可在探针片上确定测年矿物的共生组合及地质意义,将测得的年龄与特定地质事件,如变质事件、热液事件等相联系,对年龄数据给予合理的地质解释。利用此方法对一些岩石中的锆石、磷灰石在探针片上进行了测试,与用传统单矿物制靶方法测试的结果在误差范围内一致,表明在探针片上进行含铀矿物原地原位U-Pb测年是完全可行的。     

碧溪岭岩体中石榴橄榄岩的锆石显微结构及离子探针定年

对碧溪岭岩体中石榴橄榄岩的锆石进行了BSE和CL显微结构分析，并在此基础上用离子探针进行了锆石微区U－Pb定年。锆石CL图像显示其有明显的核边结构，核部具岩浆锆石，边部是变质增生锆石的特征。结合锆石的外形特征认为，边部的变质锆石是在超高压变质作用中重结晶形成的。离子探针分析结果在一致曲线图中构成不一致线，得到上下交点 年龄分别为824±39Ma和254±38Ma。结合CL图像认为上交点824±39Ma的年龄代表其原岩形成年龄，下交点254±38Ma为基超高压变质作用的年龄。另有少量较年龄的捕虏晶锆石，可能来自岩浆上升过程中同化混染的围岩。     

阿尔金江尕勒萨依榴辉岩和围岩锆石LA ICP MS微区原位定年及其地质意义

阿尔金江尕勒萨依榴辉岩及其直接围岩——石榴子石黑云母片麻岩锆石的阴极发光图像、微区原位LA-ICP-MS微量元素分析研究表明,榴辉岩锆石内部结构比较均匀,少数颗粒保留斑杂状残核;位于锆石斑杂状残核测点的重稀土相对富集,Th/U比值多大于0.4,为岩浆锆石的特征;位于锆石边部与内部结构均匀颗粒上的测点显示HREE近平坦型或弱亏损型的稀土配分模式,显示了与石榴石平衡共生的变质锆石特征;而石榴子石黑云母片麻岩的锆石具有核-幔-边结构,核部为碎屑锆石,幔部则为与石榴石平衡共生的变质锆石。LA-ICP-MS微区定年获得榴辉岩的变质年龄为(493±4.3)Ma,其原岩形成年龄为(754±9)Ma;石榴子石黑云母片麻岩的变质年龄为(499±27)Ma。榴辉岩的变质年龄滞后于其原岩的形成年龄约250Ma,并且榴辉岩与其直接围岩副片麻岩的变质年龄几乎完全一致,充分表明该超高压榴辉岩的形成是陆壳深俯冲作用的产物。     

东喜马拉雅构造结墨脱地区晚三叠世深熔作用的锆石U-Pb年代限定

东喜马拉雅构造结是研究青藏高原构造演化的关键地区。本文对东构造结墨脱地区的混合岩化片麻岩中的锆石进行了LA-ICP-MS微区微量元素分析及U-Pb定年。阴极发光(CL)图像揭示多数锆石具有明显的核-边结构特征,核部为原岩残留核,外形表现出晶棱圆化、港湾状等特征;而边部是混合岩化深熔作用变质过程中形成的新生变质锆石,并且具有典型岩浆锆石的环带特征。微量元素分析显示,锆石不同微域的微量元素含量不同,锆石核部含量明显高于边部(如:元素Th、U、Nb、Ta及Th/U比值),这一结果与深熔熔体和残留相之间的平衡关系有关。锆石U-Pb定年结果显示12个原岩锆石分析点给出的206Pb/238U年龄为516~1826 Ma,其中有6个分析点的年龄值相对集中在911~1330 Ma,表明该混合岩化片麻岩的原岩可能主要形成在这个年龄区间;14个变质锆石分析点给出了206Pb/238U年龄加权平均结果为216.7±3.2 Ma(MSWD=3.9),这一年龄代表拉萨地体在晚三叠世发生深熔作用,与区域上拉萨地体东南缘发生变质事件的时间一致。     

锆石微区原位同位素和微量元素测定的新进展

文章简述了二次离子探针质谱(SIMS)、激光剥蚀等离子体质谱(LA-ICP-MS)和激光剥蚀多接受等离子体质谱(LA-MC-ICP-MS)等3种锆石微区原位同位素和微量元素测定方法的原理和优缺点;针对U-Pb定年、铪同位素、锂同位素、多种元素的同时测定,以及仪器改进、测试方法创新、标样研发等方面的新进展进行了评述。     

Baddeleyite and zircon U-Pb ages of the ultramafic rocks in Chigu Tso area,Southeastern Tibet and their constraints on the timing of Comei Large Igneous Province

A suite of ultramafic and mafic rocks developed in the Chigu Tso area, eastern Tethyan Himalaya. Baddeleyite and zircon U-Pb ages acquired by SIMS and LA-ICP-MS from olivine pyroxenite rocks in the Chigu Tso area are 138.9±3.0 Ma and 139.0±1.9 Ma, respectively. These two Early Cretaceous ages are similar with the ages of the more abundant mafic rocks in the eastern Tethyan Himalaya, indicating that this suite of ultramafic and mafic rocks in the Chigu Tso area should be included in the outcrop area of the Comei Large Igneous Province (LIP). These ultramafic rocks provide significant evidence that the involvement of mantle plume/hot spot activities in the formation of the Comei LIP. Baddeleyite U-Pb dating by SIMS is one reliable and convenient method to constrain the formation time of ultramafic rocks. The dating results of baddeleyite and zircon from the olivine pyroxenite samples in this paper are consistent with each other within analytical uncertainties, suggesting that baddeleyite and zircon were both formed during the same magmatic process. The consistency of baddeleyite U-Pb ages in the Chigu Tso area with zircon U-Pb ages for a large number of Early Cretaceous mafic rocks in the eastern Tethyan Himalaya further support that zircon grains from such mafic rocks yielding Early Cretaceous ages are also magmatic in origin.     

黄陵野马洞基性岩脉中锆石的U-Pb年龄和Hf同位素组成

采用激光剥蚀-等离子质谱(LA-ICP-MS)分析技术测定野马洞基性岩脉中锆石的U-Pb年龄和Hf同位素组成,以探讨黄陵地区TTG片麻岩原岩的形成及变质时间、是否存在比崆岭群更古老的地壳等问题。野马洞辉绿岩脉(1850 Ma)侵入TTG片麻岩,并从TTG片麻岩中捕获了大量捕掳晶锆石。捕掳晶锆石岩浆结晶核部的U-Pb年龄分别为2842 Ma、2900 Ma和2949 Ma,指示TTG花岗岩体为复式岩体,其至少经历了2949 Ma、2900 Ma和2842 Ma三期岩浆作用。捕掳晶锆石变质边部的U-Pb年龄为2557 Ma,指示TTG花岗岩体转变为TTG片麻岩,是"水月寺运动"及其构造热事件共同作用的结果,其变形变质的时间为2557～2511 Ma。捕掳晶锆石的εHf(t)为-9.85～0.89、平均值为-4.07,亏损地幔模式年龄TDM为3.6～3.2 Ga,指示黄陵地区存在比崆岭群(3.2 Ga)更古老的陆壳。     

Unravelling the protracted U-Pb zircon geochronological record of high to ultrahigh temperature metamorphic rocks: Implications for provenance investigations

The assessment of detrital zircon age records is a key method in basin analysis, but it is prone to several biases that may compromise accurate sedimentary provenance investigations. High to ultrahigh temperature (HT-UHT) metamorphism (especially if T > 850 °C) is herein presented as a natural cause of bias in provenance studies based on U-Pb detrital zircon ages, since zircon from rocks submitted to these extreme and often prolonged conditions frequently yield protracted, apparently concordant, geochronological records. Such age spreading can result from disturbance of the primary U-Pb zircon system, likewise from (re)crystallization processes during multiple and/or prolonged metamorphic events. In this contribution, available geochronological data on Archean, Neoproterozoic and Palaeozoic HT-UHT metamorphic rocks, acquired by different techniques (SIMS and LA-ICP-MS) and showing distinct compositions, are reassessed to demonstrate HT-UHT metamorphism may result in modes and age distributions of unclear geological meaning. As a consequence, it may induce misinterpretations on U-Pb detrital zircon provenance analyses, particularly in sedimentary rocks metamorphosed under such extreme temperature conditions. To evaluate the presence of HT-UHT metamorphism-related bias in the detrital zircon record, we suggest a workflow for data acquisition and interpretation, combining a multi-proxy approach with: (i) in situ U-Pb dating coupled with Hf analyses to retrieve the isotopic composition of the sources, and (ii) the integration of a petrochronological investigation to typify fingerprints of the HT-UHT metamorphic event. The proposed workflow is validated in the investigation of one theoretical and one natural example allowing a better characterization of the sedimentary sources, maximum depositional ages, and the tectonic setting of the basin. Our workflow allows to the appraisal of biases imposed by HT-UHT metamorphism and resulting disturbances in the U-Pb detrital zircon record, particularly for sedimentary rocks that underwent HT-UHT metamorphism and, finally, suggests ways to overcome these issues.     

LA-ICP-MS锆石微区U-Pb定年方法及不同束斑直径对年龄结果的影响作用探讨

利用自然资源部古地磁与古构造重建重点实验室新引进的GeoLas HD型193nm ArF准分子激光剥蚀系统和Agilent 7900型四极杆电感耦合等离子质谱仪,成功建立了LA-ICP-MS锆石微区U-Pb定年及微量元素分析测试方法。以标准锆石91500为外标,在32 μm束斑直径、5.0 J/cm2能量密度和5 Hz剥蚀频率等实验条件下,对Ple?ovice、Temora1和Qinghu锆石标样开展了U-Pb定年实验,所测年龄结果与各标样推荐值在误差范围允许的条件下一致,并且Ple?ovice年龄结果在不同时间段内保持稳定。同时对未知年龄样品11-5开展了不同实验室测年结果对比研究,所测结果与中国地质大学(武汉)地质过程与矿产资源国家重点实验室所测年龄在误差允许范围内一致。以NIST SRM 610为外标,29Si为内标,分析测试了锆石91500和NIST SRM 612标准样品的微量元素含量,实验测试结果与推荐值一致。在此基础上探索总结了不同剥蚀斑束直径对U-Pb年龄结果的影响,认为在同样的能量密度和剥蚀频率条件下,16~44 μm的剥蚀直径可以获取可靠的锆石U-Pb年龄,但32~44 μm相比16~24 μm小斑束直径所测得的年龄更加精准。      

柴北缘大陆深俯冲板片折返过程中的深熔作用研究

柴北缘锡铁山地区长英质（花岗）片麻岩普遍经历了不同程度的部分熔融作用,常见新生的花岗质浅色体呈层状、脉状或网络状分布于长英质片麻岩中,并显示出混合岩化的特征。岩相学观察结果显示长英质片麻岩保留了关键的深熔作用显微结构证据:（1）石榴石内部发育有钾长石、石英和斜长石组成的矿物包裹体;（2）长石颗粒边界出现由石英+钾长石±斜长石±白云母组成的楔形矿物集合体;（3）云母颗粒边界发育尖锐的、不规则的微斜长石,而且云母边界溶蚀明显,形成锯齿状不规则的边界;（4）石英、斜长石或钾长石颗粒边界发育圆珠状（stringofbeads）结构,而且颗粒边界或三联点中尖锐状微斜长石与周围矿物的形成较小的二面角。阴极发光图像和锆石U-Pb定年结果表明花岗质浅色体中的锆石具有明显的核、幔、边三层结构,而且具有明显不同的年龄结果。发光较强的继承性锆石岩浆核部的²⁰⁶Pb/²³⁸U年龄约为~910Ma,而且具有高的Th/U比值;弱发光的变质锆石幔的²⁰⁶Pb/²³⁸U年龄结果约为~450Ma。新生的锆石增生边中等程度发光,并发育震荡环带和较低的Th/U比值,与世界典型地区混合岩中深熔锆石的特征十分相似,其²⁰⁶Pb/²³⁸U年龄结果为432±3Ma。野外关系、显微结构特征和年代学的研究结果显示柴北缘锡铁山地区花岗质浅色体可能是其寄主岩石长英质片麻岩在折返到高压麻粒岩相条件下深熔作用的产物,而且白云母的脱水熔融是引发岩石发生深熔作用的主要机制。柴北缘地区已有的资料综合研究表明,大陆深俯冲板片在俯冲/碰撞和折返过程中可能经历了多重深熔作用。     

The 3.98–3.63 Ga zircons as indicators of major processes operating in the ancient continental crust of the east Antarctic shield (Enderby Land)

This study presents new results on zircons from the enderbite-charnockite rocks of Enderby Land, East Antarctica. U-Pb age of 3981 ± 8 Ma (SIMS SHRIMP II), which was first obtained for a protolith of massive enderbites from Aker Peaks, eastern Napier Mts, suggests that the existence of sialic crust in the study area at 4 Ga. Although there was only one magmatic zircon (of 150 grains analyzed) in the study area known with the oldest age, its significance cannot be overestimated, since it may indirectly evidence the existence of an Early Archean crustal block with a minimum age of 4 Ga, which extends for over 300 km across Enderby Land from its western to eastern part. Based on the U-Pb systematics, REE and trace element distributions in zircons from charnockite and enderbite gneisses, high-aluminous gneisses, and basic granulites, we first revealed that an early high-temperature metamorphic event accompanied by the emplacement of granodiorite intrusions occurred in the vicinity of Aker Peaks at 3620–3630 Ma. Although the 2850–3050 metamorphic overprints are clearly observed in some other areas of Enderby Land and are widely considered to be of critical importance on a regional scale, their metamorphic signatures are apparently absent from the U-Pb systematics of the studied zircon, thus suggesting the presence of similar old zircons in the study area. At the same time, all samples in this study record a 2480–2550 Ma granulite-amphibolite facies overprint represented as new zircon growths or recrystallization of earlier phases.     

二次离子质谱第四纪锆石年代学:台湾金瓜石英安岩定年

高精度第四纪年代学是第四纪研究的基础,对了解地球演化和发展非常关键。大型二次离子质谱(SIMS)锆石U-Th-Pb定年方法,集高空间分辨率、高精度、高效率和近无损分析等优势于一体,可以提取矿物微区中记录的丰富地质信息,在第四纪年代学研究中具有很大的应用潜力。文中对SIMS第四纪锆石原位微区年龄测定的基本原理、分析校正方法进行介绍,并报道我们测定台湾第四纪金瓜石英安岩锆石U-Pb年龄的结果((1.166±0.020)Ma)。     

Micro-Analytical Zircon and Monazite U-Pb Isotope Dating by Laser Ablation-Inductively Coupled Plasma-Quadrupole Mass Spectrometry

In this study we evaluated the capability of a 213 nm laser ablation system coupled to a quadrupole-based ICP-MS in delivering accurate and precise U-Pb ages on zircons and monazites. Four zircon samples ( ca. 50 Ma to ca. 600 Ma) and four monazite samples ( ca. 30 Ma to ca. 1390 Ma) of known ages were analysed utilising laser ablation pits with diameters of 20 μm and 60 μm. Instrument mass bias and laser induced time-dependent elemental fractionation were corrected for by calibration against a matrix-matched reference material. Tera-Wasserburg plots of the calculated U-Pb data were employed to assess, and correct for, common Pb contributions. The results indicated that the LA-ICP-MS technique employed in this study allowed precise and accurate U-Pb isotope dating of zircon and monazite on sample areas 20 μm in diameter. At this spot size, the precisions achieved for single spot ²⁰⁶Pb/²³⁸U ages, were better than 5% (2s) for monazites and zircons with ages down to 30 Ma and 50 Ma, respectively. The precisions reported are comparable to those generally reported in SIMS and LA-MC-ICP-MS U-Pb isotope determinations.     

阿拉善地块东部早古生代(约420 Ma)变质事件的发现及其地质意义:来自独居石与锆石U-Pb定年的新证据

前寒武纪变沉积岩系是阿拉善地块重要组成部分,准确测定其原岩成岩时代和变质时代,对于进一步认识阿拉善地块起源、形成、演化与亲缘性具有十分重要的科学意义.本文对阿拉善地块东部阿拉坦敖包地区德尔和通特组含蓝晶石石榴云母石英片岩开展了系统的野外地质调查、岩相学观察和同位素年代学研究.碎屑锆石U-Pb定年和野外地质调查表明,阿拉坦敖包地区德尔和通特组和祖宗毛道组碎屑锆石年龄介于3 306~1 146 Ma,并以出现中元古代锆石年龄（1 800~1 100 Ma）高频区为特征,最小一组碎屑锆石年龄约为1 123 Ma,结合区域上它们被约900 Ma花岗质片麻岩侵入的野外关系,阿拉坦敖包地区德尔和通特组与祖宗毛道组变沉积岩系的沉积时代被限定在1 123~900 Ma之间,为一套中元古代晚期?新元古代早期陆缘沉积建造,具有亲华北板块的特点.此外,变质独居石和变质锆石U-Pb定年和微量元素分析表明,阿拉坦敖包地区德尔和通特组含蓝晶石泥质片岩中发育大量变质独居石,它们具有典型变质独居石的稀土元素配分模式（轻稀土元素强烈富集而重稀土元素强烈亏损）,其加权平均年龄为419±3 Ma（MSWD=7.1,n=40）,类似地,一个锆石变质边也记录了406±7 Ma的206Pb/238U年龄.这些变质年龄被解释为阿拉善地块东部阿拉坦敖包地区德尔和通特组含蓝晶石石榴云母石英片岩遭受早古生代末角闪岩相变质?变形作用的时代,可能是阿拉善地块与周缘微陆块早古生代末碰撞造山作用的响应.      

苏鲁地体超高压矿物的三维空间分布

采用激光拉曼技术,配备电子探针和阴极发光测试,确认苏鲁地体大多数花岗质片麻岩,所有类型片麻岩、斜长角闪岩、蓝晶石英岩和大理岩的锆石中均隐藏以柯石英为代表的超高压包体矿物组合。其中花岗质片麻岩典型超高压包体矿物为柯石英±多硅白云母;副片麻岩为柯石英+石榴子石+绿辉石、柯石英±石榴子石+硬玉+多硅白云母+磷灰石、柯石英+多硅白云母±磷灰石;斜长角闪岩为柯石英+石榴子石+绿辉石±金红石;蓝晶石英岩为柯石英+蓝晶石+金红石+磷灰石、柯石英+蓝晶石+多硅白云母+金红石;大理岩为柯石英+透辉石、柯石英+橄榄石。表明苏鲁地体由榴辉岩及其围岩所组成的巨量陆壳物质曾普遍发生深俯冲,并经历了超高压变质作用。锆石的矿物包体分布特征及相应的阴极发光图像研究表明,在同一样品中,锆石的成因特征存在明显差异。有的锆石显示继承性(碎屑)锆石的核(core)、超高压变质的幔(mantle)和退变质的边(rim);有的锆石则具有超高压的核、幔和退变质的边;而有的锆石却记录了深俯冲的核、超高压的幔和退变质的边。标志着苏鲁超高压变质带各类岩石副矿物锆石均具有十分复杂的结晶生长演化历史。因此,在充分研究锆石中矿物包体性质、分布特征以及相应阴极发光图像的基础上,采用SHRIMP离子探针技术,在锆石晶体的不同