云贵高原及邻区次生氧化锰矿晚新生代大规模成矿作用及其构造和古气候意义
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摘要
云贵高原及邻区分布有大量的次生氧化锰矿床,这些矿床是我国优质锰矿石的重要来源之一。对次生氧化锰矿床矿物学、地球化学、4OAr/39Ar同位素年代学的研究是理解区域化学风化、矿床次生富集过程及富集机理的重要内容和关键所在。次生氧化锰矿不仅是极好的古气候和古环境信息载体,而且其形成之后的保存程度又与区域构造活动性及地貌演化过程紧密相关。因此,对云贵高原次生氧化锰矿床进行系统的矿物学、地球化学和年代学研究不仅有助于了解次生锰矿床的成矿过程和成矿机理,而且可以查明矿床的剥蚀程度、为深部矿产资源评价提供依据,同时还可以提供区域地壳活动、地貌形成和演化和新生代古气候特征等方面的重要信息,具有重要的理论和实际意义。
本论文选取云贵高原及邻区具有代表性的8个氧化锰矿床为研究对象,包括巴夜、老厂鹤庆、遵义、东湘桥、下雷、二塘和荔浦锰矿。在详细野外观察及系统采样的基础上,利用X射线荧光光谱(XRF)和电感耦合等离子体质谱(ICP-MS)对锰矿石的主量和微量元素进行准确分析,进而应用光学显微镜、扫描电子显微镜(SEM)、X-射线粉晶衍射(XRD)、电子显微探针(EMP)、激光剥蚀ICP-MS及矿物热重分析(TGA)等手段对氧化锰矿物的晶体结构、矿物形貌、结晶程度、矿物化学成分等进行综合研究,最后选取其中6个矿床开展系统和全面的40Ar/39Ar年代学研究,获得了一大批高精度的年龄数据。
以上研究表明,云贵高原及邻区氧化锰矿床的矿物组成主要为：隐钾锰矿、锰钡矿、锰铅矿、软锰矿、恩苏塔矿、斜方锰矿、锂锰矿、黑锌锰矿、钙锰矿等。其中软锰矿在风化过程中相当稳定,存在于所有氧化锰矿床中;其次是隐钾锰矿、锰钡矿、锂锰矿、恩苏塔矿。XRD分析可对光学性质很接近的隐钾锰矿、斜方锰矿、恩苏塔矿和锂锰矿进行有效鉴定,因为这些矿物有其特征的衍射峰值：隐钾锰矿6.95A、4.9A；斜方锰矿4.08A、2.53A；恩苏塔矿3.95A、2.34A；锂锰矿9.56A、4.74A。TGA与XRD分析表明云南巴夜锰矿床中隐钾锰矿衍射峰强、含水低,加热至450～750℃时缓慢地脱羟基；相反,老厂和遵义锰矿的隐钾锰矿衍射峰弱、含水较高,在600℃时迅速地脱羟基。这种脱羟基温度的差异反映了不同矿床氧化锰矿物结晶程度的差异,同时为后续年代学研究提供了充分的理论基础和依据。对氧化锰矿物的形貌观察表明：具1×1或1×2隧道结构的氧化锰矿物以柱状或粒状晶形为主,如软锰矿、斜方锰矿、恩苏塔矿；具2×2隧道结构的氧化锰矿物主要为长柱状和针状晶形,如隐钾锰矿和锰钡矿；具2×3或3×3隧道结构的氧化锰矿物主要为针状和纤维状晶形,如钙锰矿；具有层状结构的锰矿物呈片状晶形,如锂锰矿、黑锌锰矿。氧化锰矿物的形貌不仅受控于矿物晶体结构,而且还受生长空间的影响。
对矿石组成和结构构造的研究表明,氧化锰矿的形成过程实际上就是Mn与A1、Fe、Ca等元素在风化过程中发生强烈分离的过程。当铁氧化物和锰氧化物共存时,有害元素P主要赋存在铁氧化物中,因此,制定合理的矿物分选流程将铁氧化物从锰矿石和铁锰矿石中分离可以显著降低P的含量,提高锰矿石的质量。氧化锰矿石的稀土元素(REE)分析表明,鹤庆氧化锰的矿石REE含量(25.76～45.5ppm)、球粒陨石标准化配分模式与矿区的菱锰矿和硅质岩一致,而与玄武岩和泥岩存在显著差别,表明鹤庆氧化锰矿是由菱锰矿及硅质岩矿胚层风化形成。老厂锰矿石的REE含量(270.22～1942.9ppm)和球粒陨石标准化配分模式与老厂地区石炭系火山岩相似,REE含量随结核减小而增加,并与Mn的含量呈负相关,与Fe、Si、P等元素呈正相关,与Ce异常呈正相关。另外,矿石中含Ag、Pb、Zn等元素强烈富集,含量分别可达1790g/t、0.4%和7.56%,表明老厂氧化锰矿的形成很可能与老厂铅锌银矿关系密切；Mn和其他金属元素来自老厂铅锌银矿床及含锰碳酸岩蚀变岩的化学风化。
除Mn以外,Mo、Co、Ni、V、As、Zn、Cd、Pb、Cu、Ba等在氧化锰矿石中也不同程度地富集,并经常达到综合回收利用水平。由于这些元素易于进入氧化锰矿物的晶格中或被氧化锰矿物吸附,因此,可作为氧化锰矿找矿的重要地球化学标志。广西荔浦矿床中Ni的含量最高,平均达0.13%;湖南东湘桥锰矿床的Co含量最高,平均0.024%。Co主要赋存在锂锰矿、锰钡矿-隐钾锰矿固溶体和隐钾锰矿中；Ni在隐钾锰矿和锂锰矿中的含量分别可达3%和2%。SEM、EMP和XRD分析均未发现Co和Ni的独立矿物,说明这些元素自氧化锰矿物中以吸附或类质同像的形式存在。这些富Co、Ni的氧化锰矿床均与二叠系孤峰组热水沉积成因的含锰硅质岩有关,反映了矿胚层对氧化锰矿伴生有益元素的控制。Cu、Pb在云南老厂锰矿床的平均含量很高,分别为0.07%和0.16%；Zn在老厂和鹤庆锰矿床的平均中含量为1.38%和0.61%；Cu在广西二塘和湖南东湘桥锰矿的平均含量可达0.1%。单矿物电子探针分析结果表明Cu主要分布在锂锰矿、恩苏塔矿、锰铅矿或锰钡矿-隐钾锰矿的固溶体矿物中；Pb则赋存在锰铅矿或锰铅矿-锰钡矿的固溶体中；Zn主要存在于黑锌锰矿中,少部分在锰钡矿-隐钾锰矿的固溶体、恩苏塔矿中。值得注意的是,Ag在老厂锰矿的含量极高(336～1790g/t),其中以5cm左右的锰结核中含Ag最高。当结核直径小于5cm时,Ag与Mn具有正相关性；当结核大于5cm时,Ag与Mn具负相关性,因而可根据锰结核的粒级分布粗略评估银的经济价值。同样,锰矿石中无独立银矿物的存在,Ag常呈分散状分布于锰铅矿中,其赋存状态为类质同象或吸附。
利用激光阶段加热技术对云贵高原和邻区6个氧化锰矿共136个单矿物颗粒进行了40Ar/39Ar定年,获得一大批高精度的年代学数据,初步揭示了云贵高原及邻区氧化锰矿的年代学格架。激光阶段加热40Ar/39Ar同位素分析共获得五种特征的表观年龄谱,分别是平坦状年龄谱、反冲型年龄谱、阶梯状年龄谱、跳跃式年龄谱和马鞍形年龄谱。平坦状年龄谱表明样品结晶较好、样品中无过剩氩、无老矿物的污染、样品在照射过程中也没有发生39Ar的反冲丢失。反冲型年龄谱说明样品在中子反应堆中接收快中子照射时发生过部分39Ar的反冲,但反冲强度不大,多数情况下仍然给出了较好的年龄结果。阶梯状年龄谱说明样品中有大量形成于不同时期的氧化锰环带或存在不同期次的矿物,这些环带和不同世代的矿物具有不同的热稳定性,因而在激光阶段加热时于不同的温度区间释气并形成阶梯状年龄谱。跳跃式年龄谱同样是样品中存在多个环带或多世代矿物的反映,但这些环带或矿物的热稳定性可能是动荡变化的。马鞍形年龄谱反映样品中存在少量的原生老矿物的污染。在所分析的136个矿颗粒中,约85%的样品给出了很好的坪年龄或似坪年龄,其中云南巴夜锰矿的年龄为6.5～0.03.03Ma,老厂锰矿的年龄为9.5～4.3Ma,贵州遵义锰矿的年龄为13.1～0.1Ma,广西二塘锰矿的年龄为11.0～4.1Ma,下雷锰矿的年龄为11.9～0.1Ma,湖南东湘桥锰矿的年龄为9.1～4.2Ma。本文研究结果并结合前人获得的华南氧化锰矿年龄数据表明,云贵高原和邻区氧化锰矿的次生富集至少始于早中新世(-23Ma),大规模富集成矿时间集中在中中新世(13～15Ma),晚中新世(5-8Ma),上新世(3.5、2.4-2.8Ma)和更新世(1.2Ma、0.8Ma、0.5Ma)。氧化锰矿的成矿时代分布反映云贵高原和华南地区温暖潮湿的古气候至少在早中新世就已出现并一直持续到更新世,这种气候条件促进了区域大面积的红土型风化和氧化锰矿大规规模表生富集成矿。早中新世的氧化锰矿次生富集与东亚夏季风的起源时间基本吻合,而中中新世、晚中新世、上新世界、更新世各时间段的大规模表生成矿作用则反映了东亚夏季风的强化,这与华南大量陆相盆地中的沉积物、南海及印度洋的深海沉积物、以及黄土堆积等的研究结果一致。华南地区晚新生代大规模区域化学风化与成矿年代学研究的初步结果显示大陆区域化学风化可能并不具有全球性,而主要受区域古气候和构造等因素的控制。
云南次生氧化锰矿的年龄最老为晚中新世(9-5Ma),且晚中新世氧化锰矿均遭到强烈剥蚀,但在地势较低地方还有部分残留;原地的次生氧化锰矿年龄一般为晚上新世以后(3.4,2.8～2.4,1.2～0.8,0.5Ma),表明云南高原在晚中新世至早上新世经历了强烈的隆升,晚上新世后则为周期性的隆升。黔北高原遵义氧化锰矿年代学研究表明矿床次生富集开始于13Ma,表明黔北高原在晚中新世以来相对稳定。本文研究发现云贵高原氧化锰矿的年龄与其高程存在显著的正相关性,据此计算出云南巴夜地区晚上新世以来的剥蚀率为～30m/Ma,明显大于黔北高原的剥蚀速率<3.2m/Ma,反映了滇西南地区3Ma以来隆升剧烈,而黔北高原从晚中新世以来构造隆升剥蚀较弱。云贵高原及其邻区氧化锰矿年龄表现为从东至西依次减小：广东新榕锰矿为23.5～2.06Ma,广西南部钦州-防城锰矿带为17.5～4.7Ma,桂西南下雷锰矿11.3～0.3Ma,广西北部二塘锰矿9.8～4.1Ma,；湖南东湘桥锰矿10.23～4.19Ma,贵州遵义锰矿13.1～0.1Ma,云南巴夜锰矿6.8～0.08Ma,云南老厂锰矿床9.5～4.3Ma。氧化锰矿的这种年龄分布特征反映早中新世以来云贵高原和华南地区地壳稳定性和隆升剥蚀程度的差异：与青藏高原邻近的云南地区和桂西南地区经历了较强的隆升,因此早期化学风化和表生成矿的记录未能有效保存下来。氧化锰矿年龄分布的空间变化还为这类矿床的区域矿产潜力评价提供了重要信息。
云贵高原及邻区氧化锰矿床的矿物学、地球化学、年代学研究表明次生氧化锰矿物的富集主要为三种机制：(1)对含锰碳酸盐和锰硅酸盐的直接交代形成氧化锰矿；(2)锰离子直接从风化溶液中沉淀充填于裂隙或空洞中；(3)先前形成氧化锰矿物再经溶解、沉淀富集。氧化锰矿床的形成主要受含锰岩系、气候条件、地质构造、地形地貌及次生富集持续时间等因素的控制：云贵高原及邻区广泛分布的含锰矿胚层及中新世以来温暖潮湿的古气候条件是矿床大规模成矿的基础；次生氧化锰矿年代学研究表明氧化锰矿的生长速率十分缓慢,一般均小于100mm/Ma,因此中新世以来长期的、大规模化学风化有利于形成具有工业价值的氧化锰矿；次生氧化锰矿床年龄分布呈现出由西至东逐渐年轻,反映了构造稳定性对矿床保存的控制；云贵高原氧化锰矿床一般分布于低缓的山坡,这种地形地貌有利于氧化锰矿的保存。
Supergene Mn-oxide deposits are widely distributed in Yunnan-Guizhou Plateau, and have been a major source of high grade Mn-oxide ore. Mineralogy, geochemistry, and40Ar/39Ar geochronology of supergene Mn-oxide deposits are crucial in understanding the secondary mineralization, chemical weathering processes, and the enrichment of associated elements (Ag, Co, Ni, Zn etc.). Precise age constraints of the supergene Mn-oxide deposits not only provide insights into the timing, rates, and processes of supergene Mn mienralization, but also shed lisghts on the paceloclimatic and tectonic conditions and geomorphological evolution that control the formation, distribution, and preservation of the Mn-oxide ores.
In this study, I chose8representative Mn-oxide deposits (Baye, Laochang, Heqing, Zunyi, Dongxiangqiao, Xialei, Ertang, Lipu) from Yunnan, Guizhou, Guangxi, and Hunan Provinces to carry out detailed mineralogical, geochemical, and geochronological investigations. These studies rely on the identification and selection of suitable samples in the field; the characterization of mineral paragenesis by optical microscopy; the determination of fine-scale mineral chemistry and paragenesis though scan electron microscopy (SEM) and electron microprobe analysis (EMPA); the determination of the physico-chemical properties (mineral structure, crystallinity, and thermal stability) of the Mn-oxide minerals through X-ray diffraction (XRD) and thermo-gravimetric analysis (TGA); the characterization of the major and trace geochemistry of Mn-oxides ores by X ray fluorescence and Inductively coupled plasma mass spectrometry (ICP-MS); and precise40Ar/39Ar dating of K-bearing Mn-oxide minerals using a noble gas mass-spectrometer (Mass Analyser Products215-50:Map215-50).
The Mn-oxide deposits investigated consist mainly of cryptomelane, hollandite, coronadite, pyrolusite, nsutite, ramsdellite, lithiophorite, chalcophanite, and todorokite, witgh pyrolusite and cryptomelane being the most common phases. Cryptomelane, ramsdellite, nsutite and lithiophorite are difficultly recognized under optical microscopy, as then have very similar optical properties. These minerals, however, can be readily recognized by XRD studies because each mineral has distrinct diffraction patterns. TGA analysis of cryptomelane from the Baye deposit shows that this mineral subjects to significant but slow dehydroxylation at between450and750℃, whereas dehydroxylation of cryptomelane from the Zunyi and Laochan deposits ocurred rapidly at ca.600℃. This indicates that cryptomelane in Baye is better crystallized and has lower water contents compared to that of the Zunyi and Laochan deposit. Crystal forms of the Mn-oxide minerals with tunnel structures (1×1,1×2,2×2,2×3,3×3) are acicular and columnar, while the Mn-oxides with layer structures commonly display plate and sheet crystal morphology. The crystal morphologies of Mn-oxide minerals are obviously controlled by the mineral structures and space availability during mineral growth.
Geochemcal data of Mn-oxides ores reveal that Mn was completely seprated from Al, Fe, and P during lateritic weathering and supergene enrichment of Mn-oxide ores. Al and Fe commonly form the residual minerals at the top of weathering profile. Whenever Fe-oxides and Mn-oxides coexist, P is always preferentially fractionated into Fe-oxides such as goethite and hematite. Mo, Co, Ni, V, As, Zn, Cd, Pb, Cu, Ba, and Sr are also enriched in Mn-oxide ores, and can be used as fingerprinter elemenets in geochemical exploration of Mn-oxide deposits. The Heqing Mn deposit (Yunnan) contains25.76-45.5ppm REE and has chondrite-normalized REE patterns similar to the rhodochrosite and siliceous rocks in the mine and surroundings, but are distinctly different from the Triassic basalts and mud stones. This indicates that Mn-oxides were derived from weathering of rhodochrosite and siliceous rocks. The Laochang Mn-oxide deposit (Yunnan) have REE contents and chondrite-normalized REE patterns compatible with Carboniferous volcanic rocks, and the REE contents show positive relationship with Fe, Si, P, and Ce#, and negative correlations with grain size of Mn-oxide nodules and contents of Mn. These observations indicate that the volcanic rocks are the most likely source of Mn-oxide ores. On the other hand, Mn-oxide ores in the Laochang deposit contain Ag, Pb, and Zn up to1790g/t,0.4%, and7.56%, respectively, clearly indicating that these elements and Mn were provided by weathering the Laochang Ag-Pb-Zn deposits in proximity to the Mn-oxide deposits.
Co and Ni are notably high in the Baye, Er'tang, Dongxiangqiao, and Lipu Mn-oxide deposits, with values enough for recovery. Nickel content is up to0.13%at Lipu, whereas the average content of Co is0.024%at the Dongxiangqiao deposit. Cobalt and Ni are mainly enriched in lithiophorite, hollandite-cryptomelane solid solution, and cryptomelane. The contents of Ni are up to3%in cryptomelane and2%in lithiophorite. The Co-and Ni-enriched Mn-oxide ores are commonly associated with cherts of the Permian Gufeng Formation, indicating that protores have direct control on supergene Mn mineralization and enrichement of other trace elements. Copper and Pb are high in the Laochan Mn-oxide deposit, up to0.07%and0.16%, respectively. The concentration of Zn in the Heqing and Laochan deposits are up to1.38%and0.61%, respectively. The Cu contents are up to0.1%in the Ertang and Dongxiangqia deposits. Copper is mainly hosted in lithiophorite, nsutite, coronadite, and hollandite-cryptomelane solid solutions; Pb is enriched in coronadite and hollandite-coronadite solid solution; and Zn is present in chalcophanite, hollandite-cryptomelane solid solutions, and nsutite. It is noteworthy that Ag is unusually enriched in the Laochan Mn deposit, ranging from336to1790g/t. There is a positive relationship between Ag and Mn in Mn-oxide nodules are <5cm in diameter; but these elementsare negatively correlated in nodules>5cm in diameter.X-ray mapping shows that distribution of Ag is consistent with coronadite, indicating that it occrs mainly as substitution for the Pb lattice site is adsorbed on mineral surfaces. The supergene Mn oxide deposits of the Yunnan-Guizhou Plateau were formed by three principal mechanisms:(1) replacement of hypogene Mn-silicates and Mn-carbonates by Mn-oxides,(2) precipitation of tetravalent manganese directly from weathering solution to form cavity-and fracture-fillings, and (3) dissolution and re-precipitation or previous Mn-oxides by reducing, organic batter-enriched solutions. The formation of Mn-oxide deposits are controlled by Mn-protore, paleoclimate, tectonism, geomorphonology, and duration of mineralization.
40Ar/39Ar laser incremental heating analysis of136K-Mn oxide grains collected from8deposits provides the first numerical constraints on the timing and history of supergene Mn enrichment. These samples yield five types of age spectra:(1) well-defined flat plateau,(2) left-deviated spectra,(3) staircase spectra,(4) rugged spectra, and (5) saddle-shaped spectra. The well-defined flat spectra suggest that the grains analyzed are well crystallized, cotain no excess argon and old contamination, and lack39Ar loss by recoil. The left-deviated spectra are an indicative of39Ar recoil due to irradiation. However, whenever the recois occurred, it seems that only the outer parts of the crystals were affected and plateau or pseudo-plateau may still be obtained. The staircase spectra are best interpreted as presence of multiple growth bands in the grains, with individual bands having distinct thermal stability and thus releasuing their gases at different temperatures. Variable thermal stabilities of multiple banded Mn oxides or generations in the grains may explain the rugged spectra. If old, hypogene minerals are contained in the grain, a saddle-shaped spectrum may occur.
More than85%of the136grains yield well-developed plateau or pseudo plateau ages. The Baye and Laochang Mn-oxide deposit in Yunnan were dated at6.5～0.03Ma and9.5～4.3Ma, respectively, whereas the Zunyi Mn-oxide deposit in Guizhou yield ages ranging from13.1to0.1Ma. The Ertang and Xialei deposits in Guangxi recorded weathering and supergene mineralization events in the11.0to4.1Ma and11.9to0.1Ma intervals, respectively. Simialr ages are also obtained in the Dongxiangqiao deposit, southern Hunan Provinc, which are9.1～4.2Ma. The dating results form this study, when combined with previous data in South China, reveal that weathering and Mn-oxide precipitation commenced at least in early Miocene (～23Ma), and experienced several periods of intensification at mid-Miocene (13～15Ma), late Miocene (5-8Ma), Pliocene (3.5,2.4-2.8Ma), and Pleistocene (1.2,0.8,0.5Ma). This indicates that warm and humid climatic conditions conducive to supergene mineralization prevailed during the Neogene. The geochronological results of Mn-oxide are consistent with the evolution of Summer Asia Monsoon, which commenced in the early Miocene and were strengthened at mid-Miocene, late Miocene, late Pliocene, and Pleistocene. The climatic conditions inferred from weathering geochronology is consistent with the records of sedimentary and fossil floral and fauna associations from inland, deep ocean sediments from South China sea and Indian Ocean, and North China loess.
The oldest supergene Mn-oxides (ca.5-9Ma) in the Yunnan plateau have been eroded, transported, and redeposited on flat slopes and low relie landscape, while in situ Mn-oxides yield the ages between ca.3Ma to present. This demonstrates that the Yunnan plateau experienced significant uplift during the late Miocene to early Pliocene. The ages of Mn-oxides at different erosion surfaces decrease with the elevation, indicating repeated uplift of the Yunnan plateau during the Pleistocene. In northern Guizhou, the uppermost level of weathering profile yielded40Ar/39Ar ages in the range of11-13Ma, demonstrating relatively stable tectonism in northern Guizhou compared to the Yunnan plateau. This is also consistent with the erosion rates calculated from the Mn-oxide ages vs. elevation, which show the erosion rate at Baye (30m/Ma) is much higher than the value obtained from Zunyi (3.2m/Ma). In combination with40Ar/39Ar ages of Mn oxide deposits in south China, the present data show that Mn-oxide deposits become progressively younger from east to west:23.5to2.06Ma for the Xingrong deposit in western Guangdong province,17.5to4.7Ma for the Qianzhou-Fangcheng Mn belt in southern Guangxi,11.3to0.3Ma for the Xialei deposit in SW Guangxi Province,9.8to4.1Ma for the Ertang deposit in northern Guangxi,10.23to4.19Ma for the Dongxiangqiao deposit in southern Hunan Province,13.1to0.1Ma for the Zunyi deposit in northern Guizhou Province,9.5to4.3Ma for the Laochan deposit in NW Yunan Province, and6.8to0.08Ma for the Baye deposit in southern Yunnan Province,. The distribution of Mn-oxide ages demonstrate a fundamental control of tectonic stability on the preservation of weathering records and supergene Mn ores.
本论文选取云贵高原及邻区具有代表性的8个氧化锰矿床为研究对象,包括巴夜、老厂鹤庆、遵义、东湘桥、下雷、二塘和荔浦锰矿。在详细野外观察及系统采样的基础上,利用X射线荧光光谱(XRF)和电感耦合等离子体质谱(ICP-MS)对锰矿石的主量和微量元素进行准确分析,进而应用光学显微镜、扫描电子显微镜(SEM)、X-射线粉晶衍射(XRD)、电子显微探针(EMP)、激光剥蚀ICP-MS及矿物热重分析(TGA)等手段对氧化锰矿物的晶体结构、矿物形貌、结晶程度、矿物化学成分等进行综合研究,最后选取其中6个矿床开展系统和全面的40Ar/39Ar年代学研究,获得了一大批高精度的年龄数据。
以上研究表明,云贵高原及邻区氧化锰矿床的矿物组成主要为：隐钾锰矿、锰钡矿、锰铅矿、软锰矿、恩苏塔矿、斜方锰矿、锂锰矿、黑锌锰矿、钙锰矿等。其中软锰矿在风化过程中相当稳定,存在于所有氧化锰矿床中;其次是隐钾锰矿、锰钡矿、锂锰矿、恩苏塔矿。XRD分析可对光学性质很接近的隐钾锰矿、斜方锰矿、恩苏塔矿和锂锰矿进行有效鉴定,因为这些矿物有其特征的衍射峰值：隐钾锰矿6.95A、4.9A；斜方锰矿4.08A、2.53A；恩苏塔矿3.95A、2.34A；锂锰矿9.56A、4.74A。TGA与XRD分析表明云南巴夜锰矿床中隐钾锰矿衍射峰强、含水低,加热至450～750℃时缓慢地脱羟基；相反,老厂和遵义锰矿的隐钾锰矿衍射峰弱、含水较高,在600℃时迅速地脱羟基。这种脱羟基温度的差异反映了不同矿床氧化锰矿物结晶程度的差异,同时为后续年代学研究提供了充分的理论基础和依据。对氧化锰矿物的形貌观察表明：具1×1或1×2隧道结构的氧化锰矿物以柱状或粒状晶形为主,如软锰矿、斜方锰矿、恩苏塔矿；具2×2隧道结构的氧化锰矿物主要为长柱状和针状晶形,如隐钾锰矿和锰钡矿；具2×3或3×3隧道结构的氧化锰矿物主要为针状和纤维状晶形,如钙锰矿；具有层状结构的锰矿物呈片状晶形,如锂锰矿、黑锌锰矿。氧化锰矿物的形貌不仅受控于矿物晶体结构,而且还受生长空间的影响。
对矿石组成和结构构造的研究表明,氧化锰矿的形成过程实际上就是Mn与A1、Fe、Ca等元素在风化过程中发生强烈分离的过程。当铁氧化物和锰氧化物共存时,有害元素P主要赋存在铁氧化物中,因此,制定合理的矿物分选流程将铁氧化物从锰矿石和铁锰矿石中分离可以显著降低P的含量,提高锰矿石的质量。氧化锰矿石的稀土元素(REE)分析表明,鹤庆氧化锰的矿石REE含量(25.76～45.5ppm)、球粒陨石标准化配分模式与矿区的菱锰矿和硅质岩一致,而与玄武岩和泥岩存在显著差别,表明鹤庆氧化锰矿是由菱锰矿及硅质岩矿胚层风化形成。老厂锰矿石的REE含量(270.22～1942.9ppm)和球粒陨石标准化配分模式与老厂地区石炭系火山岩相似,REE含量随结核减小而增加,并与Mn的含量呈负相关,与Fe、Si、P等元素呈正相关,与Ce异常呈正相关。另外,矿石中含Ag、Pb、Zn等元素强烈富集,含量分别可达1790g/t、0.4%和7.56%,表明老厂氧化锰矿的形成很可能与老厂铅锌银矿关系密切；Mn和其他金属元素来自老厂铅锌银矿床及含锰碳酸岩蚀变岩的化学风化。
除Mn以外,Mo、Co、Ni、V、As、Zn、Cd、Pb、Cu、Ba等在氧化锰矿石中也不同程度地富集,并经常达到综合回收利用水平。由于这些元素易于进入氧化锰矿物的晶格中或被氧化锰矿物吸附,因此,可作为氧化锰矿找矿的重要地球化学标志。广西荔浦矿床中Ni的含量最高,平均达0.13%;湖南东湘桥锰矿床的Co含量最高,平均0.024%。Co主要赋存在锂锰矿、锰钡矿-隐钾锰矿固溶体和隐钾锰矿中；Ni在隐钾锰矿和锂锰矿中的含量分别可达3%和2%。SEM、EMP和XRD分析均未发现Co和Ni的独立矿物,说明这些元素自氧化锰矿物中以吸附或类质同像的形式存在。这些富Co、Ni的氧化锰矿床均与二叠系孤峰组热水沉积成因的含锰硅质岩有关,反映了矿胚层对氧化锰矿伴生有益元素的控制。Cu、Pb在云南老厂锰矿床的平均含量很高,分别为0.07%和0.16%；Zn在老厂和鹤庆锰矿床的平均中含量为1.38%和0.61%；Cu在广西二塘和湖南东湘桥锰矿的平均含量可达0.1%。单矿物电子探针分析结果表明Cu主要分布在锂锰矿、恩苏塔矿、锰铅矿或锰钡矿-隐钾锰矿的固溶体矿物中；Pb则赋存在锰铅矿或锰铅矿-锰钡矿的固溶体中；Zn主要存在于黑锌锰矿中,少部分在锰钡矿-隐钾锰矿的固溶体、恩苏塔矿中。值得注意的是,Ag在老厂锰矿的含量极高(336～1790g/t),其中以5cm左右的锰结核中含Ag最高。当结核直径小于5cm时,Ag与Mn具有正相关性；当结核大于5cm时,Ag与Mn具负相关性,因而可根据锰结核的粒级分布粗略评估银的经济价值。同样,锰矿石中无独立银矿物的存在,Ag常呈分散状分布于锰铅矿中,其赋存状态为类质同象或吸附。
利用激光阶段加热技术对云贵高原和邻区6个氧化锰矿共136个单矿物颗粒进行了40Ar/39Ar定年,获得一大批高精度的年代学数据,初步揭示了云贵高原及邻区氧化锰矿的年代学格架。激光阶段加热40Ar/39Ar同位素分析共获得五种特征的表观年龄谱,分别是平坦状年龄谱、反冲型年龄谱、阶梯状年龄谱、跳跃式年龄谱和马鞍形年龄谱。平坦状年龄谱表明样品结晶较好、样品中无过剩氩、无老矿物的污染、样品在照射过程中也没有发生39Ar的反冲丢失。反冲型年龄谱说明样品在中子反应堆中接收快中子照射时发生过部分39Ar的反冲,但反冲强度不大,多数情况下仍然给出了较好的年龄结果。阶梯状年龄谱说明样品中有大量形成于不同时期的氧化锰环带或存在不同期次的矿物,这些环带和不同世代的矿物具有不同的热稳定性,因而在激光阶段加热时于不同的温度区间释气并形成阶梯状年龄谱。跳跃式年龄谱同样是样品中存在多个环带或多世代矿物的反映,但这些环带或矿物的热稳定性可能是动荡变化的。马鞍形年龄谱反映样品中存在少量的原生老矿物的污染。在所分析的136个矿颗粒中,约85%的样品给出了很好的坪年龄或似坪年龄,其中云南巴夜锰矿的年龄为6.5～0.03.03Ma,老厂锰矿的年龄为9.5～4.3Ma,贵州遵义锰矿的年龄为13.1～0.1Ma,广西二塘锰矿的年龄为11.0～4.1Ma,下雷锰矿的年龄为11.9～0.1Ma,湖南东湘桥锰矿的年龄为9.1～4.2Ma。本文研究结果并结合前人获得的华南氧化锰矿年龄数据表明,云贵高原和邻区氧化锰矿的次生富集至少始于早中新世(-23Ma),大规模富集成矿时间集中在中中新世(13～15Ma),晚中新世(5-8Ma),上新世(3.5、2.4-2.8Ma)和更新世(1.2Ma、0.8Ma、0.5Ma)。氧化锰矿的成矿时代分布反映云贵高原和华南地区温暖潮湿的古气候至少在早中新世就已出现并一直持续到更新世,这种气候条件促进了区域大面积的红土型风化和氧化锰矿大规规模表生富集成矿。早中新世的氧化锰矿次生富集与东亚夏季风的起源时间基本吻合,而中中新世、晚中新世、上新世界、更新世各时间段的大规模表生成矿作用则反映了东亚夏季风的强化,这与华南大量陆相盆地中的沉积物、南海及印度洋的深海沉积物、以及黄土堆积等的研究结果一致。华南地区晚新生代大规模区域化学风化与成矿年代学研究的初步结果显示大陆区域化学风化可能并不具有全球性,而主要受区域古气候和构造等因素的控制。
云南次生氧化锰矿的年龄最老为晚中新世(9-5Ma),且晚中新世氧化锰矿均遭到强烈剥蚀,但在地势较低地方还有部分残留;原地的次生氧化锰矿年龄一般为晚上新世以后(3.4,2.8～2.4,1.2～0.8,0.5Ma),表明云南高原在晚中新世至早上新世经历了强烈的隆升,晚上新世后则为周期性的隆升。黔北高原遵义氧化锰矿年代学研究表明矿床次生富集开始于13Ma,表明黔北高原在晚中新世以来相对稳定。本文研究发现云贵高原氧化锰矿的年龄与其高程存在显著的正相关性,据此计算出云南巴夜地区晚上新世以来的剥蚀率为～30m/Ma,明显大于黔北高原的剥蚀速率<3.2m/Ma,反映了滇西南地区3Ma以来隆升剧烈,而黔北高原从晚中新世以来构造隆升剥蚀较弱。云贵高原及其邻区氧化锰矿年龄表现为从东至西依次减小：广东新榕锰矿为23.5～2.06Ma,广西南部钦州-防城锰矿带为17.5～4.7Ma,桂西南下雷锰矿11.3～0.3Ma,广西北部二塘锰矿9.8～4.1Ma,；湖南东湘桥锰矿10.23～4.19Ma,贵州遵义锰矿13.1～0.1Ma,云南巴夜锰矿6.8～0.08Ma,云南老厂锰矿床9.5～4.3Ma。氧化锰矿的这种年龄分布特征反映早中新世以来云贵高原和华南地区地壳稳定性和隆升剥蚀程度的差异：与青藏高原邻近的云南地区和桂西南地区经历了较强的隆升,因此早期化学风化和表生成矿的记录未能有效保存下来。氧化锰矿年龄分布的空间变化还为这类矿床的区域矿产潜力评价提供了重要信息。
云贵高原及邻区氧化锰矿床的矿物学、地球化学、年代学研究表明次生氧化锰矿物的富集主要为三种机制：(1)对含锰碳酸盐和锰硅酸盐的直接交代形成氧化锰矿；(2)锰离子直接从风化溶液中沉淀充填于裂隙或空洞中；(3)先前形成氧化锰矿物再经溶解、沉淀富集。氧化锰矿床的形成主要受含锰岩系、气候条件、地质构造、地形地貌及次生富集持续时间等因素的控制：云贵高原及邻区广泛分布的含锰矿胚层及中新世以来温暖潮湿的古气候条件是矿床大规模成矿的基础；次生氧化锰矿年代学研究表明氧化锰矿的生长速率十分缓慢,一般均小于100mm/Ma,因此中新世以来长期的、大规模化学风化有利于形成具有工业价值的氧化锰矿；次生氧化锰矿床年龄分布呈现出由西至东逐渐年轻,反映了构造稳定性对矿床保存的控制；云贵高原氧化锰矿床一般分布于低缓的山坡,这种地形地貌有利于氧化锰矿的保存。
Supergene Mn-oxide deposits are widely distributed in Yunnan-Guizhou Plateau, and have been a major source of high grade Mn-oxide ore. Mineralogy, geochemistry, and40Ar/39Ar geochronology of supergene Mn-oxide deposits are crucial in understanding the secondary mineralization, chemical weathering processes, and the enrichment of associated elements (Ag, Co, Ni, Zn etc.). Precise age constraints of the supergene Mn-oxide deposits not only provide insights into the timing, rates, and processes of supergene Mn mienralization, but also shed lisghts on the paceloclimatic and tectonic conditions and geomorphological evolution that control the formation, distribution, and preservation of the Mn-oxide ores.
In this study, I chose8representative Mn-oxide deposits (Baye, Laochang, Heqing, Zunyi, Dongxiangqiao, Xialei, Ertang, Lipu) from Yunnan, Guizhou, Guangxi, and Hunan Provinces to carry out detailed mineralogical, geochemical, and geochronological investigations. These studies rely on the identification and selection of suitable samples in the field; the characterization of mineral paragenesis by optical microscopy; the determination of fine-scale mineral chemistry and paragenesis though scan electron microscopy (SEM) and electron microprobe analysis (EMPA); the determination of the physico-chemical properties (mineral structure, crystallinity, and thermal stability) of the Mn-oxide minerals through X-ray diffraction (XRD) and thermo-gravimetric analysis (TGA); the characterization of the major and trace geochemistry of Mn-oxides ores by X ray fluorescence and Inductively coupled plasma mass spectrometry (ICP-MS); and precise40Ar/39Ar dating of K-bearing Mn-oxide minerals using a noble gas mass-spectrometer (Mass Analyser Products215-50:Map215-50).
The Mn-oxide deposits investigated consist mainly of cryptomelane, hollandite, coronadite, pyrolusite, nsutite, ramsdellite, lithiophorite, chalcophanite, and todorokite, witgh pyrolusite and cryptomelane being the most common phases. Cryptomelane, ramsdellite, nsutite and lithiophorite are difficultly recognized under optical microscopy, as then have very similar optical properties. These minerals, however, can be readily recognized by XRD studies because each mineral has distrinct diffraction patterns. TGA analysis of cryptomelane from the Baye deposit shows that this mineral subjects to significant but slow dehydroxylation at between450and750℃, whereas dehydroxylation of cryptomelane from the Zunyi and Laochan deposits ocurred rapidly at ca.600℃. This indicates that cryptomelane in Baye is better crystallized and has lower water contents compared to that of the Zunyi and Laochan deposit. Crystal forms of the Mn-oxide minerals with tunnel structures (1×1,1×2,2×2,2×3,3×3) are acicular and columnar, while the Mn-oxides with layer structures commonly display plate and sheet crystal morphology. The crystal morphologies of Mn-oxide minerals are obviously controlled by the mineral structures and space availability during mineral growth.
Geochemcal data of Mn-oxides ores reveal that Mn was completely seprated from Al, Fe, and P during lateritic weathering and supergene enrichment of Mn-oxide ores. Al and Fe commonly form the residual minerals at the top of weathering profile. Whenever Fe-oxides and Mn-oxides coexist, P is always preferentially fractionated into Fe-oxides such as goethite and hematite. Mo, Co, Ni, V, As, Zn, Cd, Pb, Cu, Ba, and Sr are also enriched in Mn-oxide ores, and can be used as fingerprinter elemenets in geochemical exploration of Mn-oxide deposits. The Heqing Mn deposit (Yunnan) contains25.76-45.5ppm REE and has chondrite-normalized REE patterns similar to the rhodochrosite and siliceous rocks in the mine and surroundings, but are distinctly different from the Triassic basalts and mud stones. This indicates that Mn-oxides were derived from weathering of rhodochrosite and siliceous rocks. The Laochang Mn-oxide deposit (Yunnan) have REE contents and chondrite-normalized REE patterns compatible with Carboniferous volcanic rocks, and the REE contents show positive relationship with Fe, Si, P, and Ce#, and negative correlations with grain size of Mn-oxide nodules and contents of Mn. These observations indicate that the volcanic rocks are the most likely source of Mn-oxide ores. On the other hand, Mn-oxide ores in the Laochang deposit contain Ag, Pb, and Zn up to1790g/t,0.4%, and7.56%, respectively, clearly indicating that these elements and Mn were provided by weathering the Laochang Ag-Pb-Zn deposits in proximity to the Mn-oxide deposits.
Co and Ni are notably high in the Baye, Er'tang, Dongxiangqiao, and Lipu Mn-oxide deposits, with values enough for recovery. Nickel content is up to0.13%at Lipu, whereas the average content of Co is0.024%at the Dongxiangqiao deposit. Cobalt and Ni are mainly enriched in lithiophorite, hollandite-cryptomelane solid solution, and cryptomelane. The contents of Ni are up to3%in cryptomelane and2%in lithiophorite. The Co-and Ni-enriched Mn-oxide ores are commonly associated with cherts of the Permian Gufeng Formation, indicating that protores have direct control on supergene Mn mineralization and enrichement of other trace elements. Copper and Pb are high in the Laochan Mn-oxide deposit, up to0.07%and0.16%, respectively. The concentration of Zn in the Heqing and Laochan deposits are up to1.38%and0.61%, respectively. The Cu contents are up to0.1%in the Ertang and Dongxiangqia deposits. Copper is mainly hosted in lithiophorite, nsutite, coronadite, and hollandite-cryptomelane solid solutions; Pb is enriched in coronadite and hollandite-coronadite solid solution; and Zn is present in chalcophanite, hollandite-cryptomelane solid solutions, and nsutite. It is noteworthy that Ag is unusually enriched in the Laochan Mn deposit, ranging from336to1790g/t. There is a positive relationship between Ag and Mn in Mn-oxide nodules are <5cm in diameter; but these elementsare negatively correlated in nodules>5cm in diameter.X-ray mapping shows that distribution of Ag is consistent with coronadite, indicating that it occrs mainly as substitution for the Pb lattice site is adsorbed on mineral surfaces. The supergene Mn oxide deposits of the Yunnan-Guizhou Plateau were formed by three principal mechanisms:(1) replacement of hypogene Mn-silicates and Mn-carbonates by Mn-oxides,(2) precipitation of tetravalent manganese directly from weathering solution to form cavity-and fracture-fillings, and (3) dissolution and re-precipitation or previous Mn-oxides by reducing, organic batter-enriched solutions. The formation of Mn-oxide deposits are controlled by Mn-protore, paleoclimate, tectonism, geomorphonology, and duration of mineralization.
40Ar/39Ar laser incremental heating analysis of136K-Mn oxide grains collected from8deposits provides the first numerical constraints on the timing and history of supergene Mn enrichment. These samples yield five types of age spectra:(1) well-defined flat plateau,(2) left-deviated spectra,(3) staircase spectra,(4) rugged spectra, and (5) saddle-shaped spectra. The well-defined flat spectra suggest that the grains analyzed are well crystallized, cotain no excess argon and old contamination, and lack39Ar loss by recoil. The left-deviated spectra are an indicative of39Ar recoil due to irradiation. However, whenever the recois occurred, it seems that only the outer parts of the crystals were affected and plateau or pseudo-plateau may still be obtained. The staircase spectra are best interpreted as presence of multiple growth bands in the grains, with individual bands having distinct thermal stability and thus releasuing their gases at different temperatures. Variable thermal stabilities of multiple banded Mn oxides or generations in the grains may explain the rugged spectra. If old, hypogene minerals are contained in the grain, a saddle-shaped spectrum may occur.
More than85%of the136grains yield well-developed plateau or pseudo plateau ages. The Baye and Laochang Mn-oxide deposit in Yunnan were dated at6.5～0.03Ma and9.5～4.3Ma, respectively, whereas the Zunyi Mn-oxide deposit in Guizhou yield ages ranging from13.1to0.1Ma. The Ertang and Xialei deposits in Guangxi recorded weathering and supergene mineralization events in the11.0to4.1Ma and11.9to0.1Ma intervals, respectively. Simialr ages are also obtained in the Dongxiangqiao deposit, southern Hunan Provinc, which are9.1～4.2Ma. The dating results form this study, when combined with previous data in South China, reveal that weathering and Mn-oxide precipitation commenced at least in early Miocene (～23Ma), and experienced several periods of intensification at mid-Miocene (13～15Ma), late Miocene (5-8Ma), Pliocene (3.5,2.4-2.8Ma), and Pleistocene (1.2,0.8,0.5Ma). This indicates that warm and humid climatic conditions conducive to supergene mineralization prevailed during the Neogene. The geochronological results of Mn-oxide are consistent with the evolution of Summer Asia Monsoon, which commenced in the early Miocene and were strengthened at mid-Miocene, late Miocene, late Pliocene, and Pleistocene. The climatic conditions inferred from weathering geochronology is consistent with the records of sedimentary and fossil floral and fauna associations from inland, deep ocean sediments from South China sea and Indian Ocean, and North China loess.
The oldest supergene Mn-oxides (ca.5-9Ma) in the Yunnan plateau have been eroded, transported, and redeposited on flat slopes and low relie landscape, while in situ Mn-oxides yield the ages between ca.3Ma to present. This demonstrates that the Yunnan plateau experienced significant uplift during the late Miocene to early Pliocene. The ages of Mn-oxides at different erosion surfaces decrease with the elevation, indicating repeated uplift of the Yunnan plateau during the Pleistocene. In northern Guizhou, the uppermost level of weathering profile yielded40Ar/39Ar ages in the range of11-13Ma, demonstrating relatively stable tectonism in northern Guizhou compared to the Yunnan plateau. This is also consistent with the erosion rates calculated from the Mn-oxide ages vs. elevation, which show the erosion rate at Baye (30m/Ma) is much higher than the value obtained from Zunyi (3.2m/Ma). In combination with40Ar/39Ar ages of Mn oxide deposits in south China, the present data show that Mn-oxide deposits become progressively younger from east to west:23.5to2.06Ma for the Xingrong deposit in western Guangdong province,17.5to4.7Ma for the Qianzhou-Fangcheng Mn belt in southern Guangxi,11.3to0.3Ma for the Xialei deposit in SW Guangxi Province,9.8to4.1Ma for the Ertang deposit in northern Guangxi,10.23to4.19Ma for the Dongxiangqiao deposit in southern Hunan Province,13.1to0.1Ma for the Zunyi deposit in northern Guizhou Province,9.5to4.3Ma for the Laochan deposit in NW Yunan Province, and6.8to0.08Ma for the Baye deposit in southern Yunnan Province,. The distribution of Mn-oxide ages demonstrate a fundamental control of tectonic stability on the preservation of weathering records and supergene Mn ores.
引文
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