2021, Vol. 37
2. 中国地质调查局天津地质矿产研究所, 天津 300170;
3. 江西省地质矿产勘查开发局九一二大队, 鹰潭 335001
2. Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China;
3. 912 Party of Jiangxi Bureau of Geology and Mineral Exploration, Yingtan 335001, China
钨作为亲石元素，在地幔熔融和硅酸岩岩浆演化过程中，表现出高度不相容的性质，最终导致W在地壳中(约1×10-6)相对于地幔(约13×10-9~16×10-9)显著富集(Rudnick and Gao, 2003)；而铜作为亲硫元素，与钨表现出截然不同的地球化学性质，相对于主要起源于地壳的钨元素，铜更可能起源于地幔(Richards, 2015)，俯冲洋壳(毛景文等, 2014; mungall, 2002; sun et al., 2015)或加厚地壳底部的硫化物堆晶体(Chiaradia, 2014; Hou et al., 2015)。钨、铜的矿化作用常与中酸性、酸性花岗质岩浆活动密切相关，但二者在花岗质岩浆演化过程中却表现出明显不同的地球化学性质：铜在花岗质岩浆中的富集需要岩浆具有高氧逸度，并且岩浆热液流体越早出溶，越有利于铜在残余岩浆体系中的富集(Candela, 1992; Jugo et al., 2005)；钨在花岗质岩浆的演化过程中主要呈W6+存在，为稳定的不相容元素(Fonseca et al., 2014; O'Neill et al., 2008)，因而氧逸度对花岗质岩浆体系中钨的富集没有明显的控制作用(Blevin and Chappell, 1992)，岩浆热液流体越晚出溶，越有利于钨在残余岩浆热液体系中的富集(Meinert, 1993; Newberry and Swanson, 1986)。钨、铜的成矿岩浆源区不同和岩浆演化过程中元素地球化学行为不同，暗示着同一花岗质岩浆活动不大可能同时导致大规模的钨、铜矿化作用。例如，在我国华南地区，中晚侏罗世古太平洋板块俯冲过程中形成了一系列沿东南沿海地区分布的铜矿床，而晚侏罗世则在弧后伸展带形成了一系列钨锡矿床(Yuan et al., 2007, 2019; Hu and Zhou, 2012; Hu et al., 2012a, b; Mao et al., 2021; 袁顺达等, 2012a, b)。
值得注意的是，近年来的地质勘探工作在长江中下游地区斑岩-矽卡岩型铜多金属矿带南侧的江南钨矿带上，发现了多个钨铜共生的矽卡岩-斑岩型钨矿床(图 1)。例如，大湖塘矿区石门寺矿床中，WO3金属量达74万吨，铜金属量达40万吨(项新葵等, 2013)；朱溪矿床中WO3金属量达344万吨，而铜金属量达11万吨(Ouyang et al., 2019)，并且紧邻朱溪钨矿床还存在一个矿石中发育明显白钨矿矿化的小型铜矿床(图 2，Song et al., 2019)。鉴于朱溪矿床中“钨铜共生”现象明显，并且这种钨铜密切共生的成矿现象在国际上也是罕见现象(蒋少涌等, 2015)，朱溪矿床“钨铜共生”的地质特征已经引起了矿床学研究者的关注。准确厘定成矿时代是成矿机制研究的基础，对于朱溪钨矿化时代，前人研究一致表明该矿床中钨成矿时代约为150Ma(Pan et al., 2017; Song et al., 2019; 于全等, 2018)，与朱溪成矿相关的S型花岗岩形成时代吻合(Chen et al., 2016; Song et al., 2018b; Zhang et al., 2020; 刘经纬等, 2017)。值得注意的是，由朱溪成矿相关岩浆高度演化产生的残余岩浆遭受灰岩混染时形成的含白钨矿钙长岩内，低氧逸度条件才能形成的富Mn钛铁矿(Feenstra and Peters, 1996)广泛存在，而磁铁矿却完全缺失(Song et al., 2018a)；并且朱溪矿床成矿相关岩体内含有S型花岗岩的特征矿物——岩浆成因白云母(Song et al., 2018b)；由此说明朱溪成矿相关岩浆为壳源的还原性岩浆，显然不可能提供大量高氧逸度条件下才能富集成矿的铜元素(Ishihara, 1981)。
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图 1 江南钨矿带及长江中下游斑岩矽卡岩铜-金-钼-铁多金属成矿带矿床分布图(据Mao et al., 2017修改) 1-中侏罗统-白垩系沉积岩和火山岩；2-石炭系-下三叠统层状海相碎屑岩和碳酸盐岩，中三叠统-上三叠统近海相碎屑岩；3-石炭世中酸性侵入体；4-侏罗世中酸性侵入体；5-江南古陆：新元古代浅变质岩及沉积岩；6-新元古代中酸性侵入体；7-新元古代蛇绿岩；8-河流湖泊；9-钨矿床；10-锡矿床；11-铜矿床；12-金矿床；13-铅锌矿床；14-铁矿床 Fig. 1 Distribution of the Middle-Lower Yangtze River porphyry-skarn Cu-Au-Mo-Fe ore belt (YRB) in the north and the Jiangnan tungsten belt (JNB) in the south (modified after Mao et al., 2017) 1-Middle Jurassic to Cretaceous sedimentary and volcanic rocks; 2-Cambrian to Early Triassic marine clastic and carbonate rocks, and Middle Triassic to Early Jurassic paralic clastic rocks; 3-Cretaceous granitoids; 4-Jurassic granitoids; 5-Jiangnan Massif: Neoproteroizoic epimetamorphic and sedimentary rocks; 6-Neoproterozoic granite; 7-Neoproterozoic ophiolite; 8-river and lake; 9-W deposit; 10-Sn deposit; 11-Cu deposit; 12-Au deposit; 13-Pb-Zn deposit; 14-Fe deposit |
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图 2 朱溪钨-铜矿床地质简图(据陈国华等, 2012修改) 1-第四系沉积物；2-晚侏罗世煌斑岩脉；3-二叠系碎屑岩；4-二叠系碳酸盐岩；5-石炭系灰岩；6-石炭系白云岩；7-新元古代片岩夹火山岩；8-新元古代花岗斑岩；9-断裂构造；10-勘探线及编号；11-河流；12-钻孔 Fig. 2 Geological map of the Zhuxi W-Cu deposit (modified after Chen et al., 2012) 1-Quaternary sediments; 2-Late Jurassic lamprophyre dykes; 3-Permian detrital rock; 4-Permian carbonate; 5-Carboniferous carbonate; 6-Carboniferous dolomite; 7-Proterozoic phyllite intercalated with volcanic rocks; 8-Neoproterozoic granite porphyry; 9-fault; 10-exploration line and its serial number; 11-river; 12-drill hole |
前人对朱溪矿床中铜的成矿时代也进行了研究。例如，Pan et al. (2017)对浅部(786~1192m)的硫化物脉中的辉钼矿进行了Re-Os定年，获得了145.1±1.5Ma的等时线年龄；Song et al. (2019)对浅部(991.8m)浸染状铜矿石中与黄铜矿紧密共生的榍石进行了原位U-Pb定年工作，在Tera-Wasserburg谐和图解上获得下交点年龄为149±2.6Ma；Ouyang et al. (2019)对深部(2099m)蚀变花岗岩中与黄铜矿共生的白云母进行40Ar-39Ar年龄测定，获得了147.39±0.94Ma的坪年龄。虽然这些研究工作说明朱溪矿床中在大规模钨矿化发生过程中伴随着铜矿化作用；但是，这些研究工作所获得的成矿时代并不能限定朱溪矿床中主要铜矿体的形成时代，因为朱溪矿床中的铜矿化主要发生在新元古代浅变质岩与古生代碳酸盐岩的不整合面附近的钨铜矿体中(1200~1800m，图 3)。此外，朱溪矿床中还存在形成时代早于成钨岩体的花岗闪长岩脉(~160Ma; 贺晓龙等, 2018)，该类偏中性的花岗闪长岩脉更可能在成因上与铜矿化作用相关。为此，要客观揭示朱溪矿床中的“钨铜共生”机制，急需精确限定朱溪矿床深部不整合面附近钨(铜)矿体的铜矿化时代。
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图 3 朱溪钨-铜矿床42线勘探线剖面图(据王先广等, 2014修改) 1-第四系；2-晚侏罗世黑云母二长花岗岩；3-晚侏罗世细粒花岗岩；4-晚侏罗世花岗斑岩；5-三叠系碎屑岩；6-二叠系碎屑岩；7-二叠系碳酸盐岩；8-石炭系灰岩；9-石炭系白云岩；10-新元古代片岩夹火山岩；11-矽卡岩；12-大理岩；13-钨矿体；14-钨铜矿体；15-蚀变花岗岩内浸染状钨矿体；16-铜矿体；17-钻孔 Fig. 3 Cross section showing the tungsten and copper mineralization of No.42 exploration line of the Zhuxi deposit (modified after Wang et al., 2014) 1-Quaternary; 2-Late Jurassic biotite monzogranite; 3-Late Jurassic fine-grained granite; 4-Late Jurassic granite porphyry; 5-Triassic detrital rocks; 6-Permian detrital rocks; 7-Permian carbonate rocks; 8-Carboniferous limestone; 9-Carboniferous dolomite; 10-Proterozoic phyllite intercalated with volcanic rocks; 11-skarn; 12-marble; 13-tungsten orebody; 14-tungsten-copper orebody; 15-disseminated tungsten orebody in altered granite; 16-copper orebody; 17-drill hole |
本研究针对朱溪矿床深部不整合面附近形成的似层状钨(铜)矿体中与黄铜矿紧密共生的磷灰石、白钨矿，开展了精细的原位微区分析测试。计划以宏观、微观地质证据为基础，结合白钨矿、磷灰石的地球化学特征，以期揭示似层状钨(铜)矿体中白钨矿、黄铜矿是否为同一热液流体结晶形成，论证该热液流体成因上是否与朱溪矿床成矿相关岩浆形成的高分异残余岩浆密切相关。拟通过似层状钨(铜)矿体中磷灰石的原位U-Pb同位素定年工作，精确限定朱溪矿床中最重要的铜矿化作用的形成时代，厘定朱溪矿床中“钨铜共生”的特殊地质现象是否为同期形成。
1 成矿地质背景朱溪矿床位于江南钨矿带，该矿带是过去十年确定的一个世界级钨矿带，探明资源量达606万吨(毛景文等, 2020; Mao et al., 2019)。江南钨矿带上出露的地层由前寒武纪基底和显生宙盖层组成(图 1)。前寒武纪基底分布于阳兴-常州断裂以南，由中元古代的田里片岩，早元古代双溪钨群火山碎屑岩，以及中-新元古代沉积岩和蛇绿岩混杂体组成(Ye et al., 2007; Zhao et al., 2011)；并且前寒武纪基底由一个明显的不整合面划分为2个低绿片岩相变质序列(Wang et al., 2012; Zhao and Cawood, 2012)。前人对出露于不同区域的不整合面之下的前寒武基底有着不同的命名，如安徽省南部和江西省东北部的溪口群，江西省北部和东北部的双桥山群，湖南省北部的冷家溪群，桂州东北部的梵净山群以及广西省北部的四堡群(Zhao and Cawood, 2012)；其中，双桥山群广泛分布于江南古陆中部(图 1)，主要由千枚岩和变质火山岩组成，部分地区保留了原始的沉积构造，并且沉积物粒度向上逐渐变粗(Mao et al., 2017)。位于不整合面之上的前寒武纪基底(南华系)的形成伴随南华盆地的发育，如分布于湖南省的板溪群，广西省北部的丹洲群以及江西省的登山群；南华系主要由砂岩、板岩、砾岩、泥质岩及少量碳酸盐岩、细碧岩和火山碎屑岩组成(Wang et al., 2007)。传统认为不整合面之下的前寒武纪基底由中元古代变质地层组成，但是近年来的锆石U-Pb同位素研究证明这些地层形成于新元古代中期(Zhao and Cawood, 2012)。这些不整合面之下的前寒武纪基底早期沉积于活动大陆边缘，并在扬子和华夏板块拼合过程中发生强烈地褶皱变形；而不整合面之上的变质基底形成于碰撞后的伸展盆地中，仅发生微弱的变形(Wang and Li, 2003; Wang et al., 2007; Zhao et al., 2011)。因此，江南古陆前寒武基底中的不整合面的形成时间代表了扬子与华夏板块的拼合时间(Wang et al., 2007)。相对于广泛出露于江南钨矿带上的前寒武变质基底，上覆的显生宙地层零星地分布在江南古陆周围(图 1)，这些地层包括志留系到上三叠统的海相碎屑岩和碳酸盐岩，中三叠统到下侏罗统的近海碎屑岩，中-上侏罗统的沉积岩和火山岩，以及在一系列北东向展布的陆内拉分盆地内沉积的白垩系红色砂岩(Mao et al., 2017)。
江南古陆内的岩浆活动以中酸性花岗质岩浆活动为主，并且花岗质侵入体主要形成于晋宁运动和燕山运动期。例如，位于江南古陆西南部的新元古代摩天岭、元宝山和本洞花岗质侵入体(870~740Ma)，位于江南古陆中部的九岭花岗质侵入体(828~819Ma)，以及位于江南古陆东北部的许村、歙县和休宁花岗质侵入体(838~823Ma)(Li et al., 2003; Wu et al., 2006; 宋昊等, 2015)。这些新元古代花岗质岩体主要由含堇青石的过铝质花岗质侵入体组成(Wang et al., 2014)。燕山期的花岗质侵入体可以进一步划分为两组，第一组主要侵位于149~136Ma(Chen et al., 2016; Huang and Jiang, 2014; Mao et al., 2015, 2017; Pan et al., 2018; Song et al., 2012, 2018b; Zhang et al., 2020, 2021; Zhu et al., 2014; 陈雪霏等, 2013; 孔志岗等, 2018; 李岩等, 2014; 秦燕等, 2010; 王先广等, 2015)，主要由二长花岗岩和一些花岗闪长岩、碱性花岗岩组成，这些侵入体属于准铝质到过铝质的高钾钙碱性花岗岩。燕山期第二组花岗质侵入体主要侵位于129~102Ma(Dai et al., 2018; Zhao et al., 2017; 胡正华等, 2018)，主要由具有过铝质特征的二长花岗岩组成。根据成矿年代学研究，江南古陆钨矿带上的钨矿床主要与燕山期第一组花岗质侵入体(149~136Ma)密切相关(Huang and Jiang, 2014; Zhu et al., 2014; Chen et al., 2016; Mao et al., 2017; Pan et al., 2017; Su et al., 2018; Song et al., 2018b)；但也有一些钨矿化作用与燕山期第二组花岗质侵入体相关，如香炉山矽卡岩钨矿床(Dai et al., 2018)和近年来新发现的东坪石英脉型钨矿床(胡正华等, 2018)。
2 矿床地质特征朱溪矿区内出露的地层由前寒武变质基底和古生代沉积岩盖层组成，变质基底主要为新元古代双桥山群的千枚岩、板岩和杂砂岩，而变质基底之上的盖层从下至上(图 2、图 3)包括：(1)石炭系白云岩，主要由灰色白云岩和白云质灰岩组成；(2)石炭系灰岩，主要由灰色-浅灰色灰岩组成；(3)二叠系碳酸盐岩，主要由深灰色灰岩组成，并在其底部出现一层石英细砂岩作为与石炭系碳酸盐岩的分界标志；(4)二叠系碎屑岩，主要由泥岩和以砂岩为夹层的白云岩、硅质灰岩组成；(5)三叠系碎屑岩，主要由泥质碳酸盐岩、细砾岩、岩屑石英砂岩组成。地质勘探显示石炭系白云岩、灰岩和二叠系碳酸盐岩都发生了明显的钨矿化作用。
朱溪矿区地表出露的岩脉以煌斑岩脉为主，仅在地表见花岗斑岩小范围的出现(图 2)。然而，地质勘探揭示朱溪床中主要出现三种类型的花岗质侵入体(图 3)：(1)黑云母二长花岗岩，主要出现于地表以下2000m的深部，是朱溪矿区内最主要的花岗质侵入体。黑云母花岗岩主要由石英(~40vol.%)、钾长石(~27vol.%)、斜长石(~23vol.%)、黑云母(~5vol.%)、白云母(~3vol.%)，及锆石、磷灰石、钛铁矿等副矿物(~2vol.%)组成，其中锆石和磷灰石通常呈矿物包裹体包裹于黑云母中，而钛铁矿则常呈粒状被石英和长石包裹。(2)细粒花岗岩，主要以岩脉形式出现于地表以下400m至2000m的深度，并且主要由石英(~43vol.%)、钾长石(~20vol.%)、斜长石(~28vol.%)、黑云母(~2vol.%)、白云母(~4vol.%)，及锆石、磷灰石、钛铁矿、金红石等副矿物(~3vol.%)组成。(3)花岗斑岩，以脉体形式主要出现于地表以下800m至1800m的深度，斑晶含量约为15vol.%，由~13vol.%石英和~2vol.%白云母组成，基质主要由石英(~45vol.%)、白云母(~35vol.%)、黄铁矿(~3vol.%)及锆石、磷灰石(~2vol.%)等副矿物组成。除了这些常见的长英质岩体(脉)外，朱溪矿床中还出现了两类形成与高分异残余岩浆密切相关的罕见岩脉，分别为含白钨矿钙长岩脉和含白钨矿钠长岩脉(Song et al., 2018a, 2021)。
根据成矿元素组合，朱溪矿床的矿化类型可以分为钨矿化和铜矿化，并且以钨矿化为主(图 3)。值得注意的是黄铜矿通常和白钨矿共生(图 3、图 4k-n)，即使是紧邻朱溪钨矿床的朱溪铜矿(地表小型铜矿床)中的块状铜矿石也见大量粒状白钨矿被黄铜包裹(Song et al., 2019)。此外，仅有少量不含或仅含少量白钨矿的铜矿体出现在浅部，但以白钨矿为主(几乎不含黄铜矿)的钨矿体却在朱溪矿床中广泛出现。同时，根据矿石类型，朱溪矿床中可以识别出以下三种主要的钨矿化类型(Song et al., 2019)。
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图 4 朱溪矿床代表性矿石手标本(a、c、f、i、k、m)及微观地质特征照片(b、d、e、g、h、j、l、n)(据Song et al., 2019) (a)热液矿脉穿插钙质大理岩；(b)白钨矿和白云母、萤石、石英紧密共生；(c)蚀变花岗岩发生浸染状矿化；(d)蚀变花岗中长石发生强烈蚀变；(e)白钨矿和黄铜矿紧密共生；(f)脉状矽卡岩矿石；(g)脉状石榴石矽卡岩与大理岩接触带微观地质特征；(h)白钨矿呈粒状与石榴石紧密共生；(i)块状矽卡岩矿石；(j)白钨矿呈粒状生长于辉石、石榴石粒间；(k)块状钨铜矿石；(l)白钨矿与磁黄铁矿、黄铜矿、自然铋、辉铋矿紧密共生；(m)钨铜矿脉穿插蛇纹石化白云质大理岩；(n)黄铜矿、白钨矿、蛇纹石紧密共生(a、c、f、i、k、m：荧光灯下拍摄；b、g、j：透射光；d、h：正交偏光；e、l、m：反射光.手标本与显微照片对应关系: a-b; c-d, e; f-g, h; i-j; k-l; m-n). Ap-磷灰石；Bis-辉铋矿；Cal-方解石；Ccp-黄铜矿；Fl-萤石；Grt-石榴石；Mbl-大理岩；Ms-白云母；Pl-斜长石；Po-磁黄铁矿；Pyx-辉石；Qz-石英；Sch-白钨矿；Srp-蛇纹石 Fig. 4 Photograph (under ultraviolet light, a, c, f, i, k, m) and representative transmitted (b, g, j), perpendicular polarized (d, h) and reflected (e, l, n) photomicrographs of the different ore of the Zhuxi deposit (after Song et al., 2019) (a) veined W ore superimposed on calcic marble; (b) scheelite is intergrown with fluorite and muscovite at the contact zone of veined ore and marble; (c) disseminated W and Cu mineralization occurred in the altered granites; (d) scheelite, muscovite, quartz and completely altered plagioclase in the altered granite; (e) scheelite coexisting with chalcopyrite and apatite in the altered granite; (f) veined garnet skarn superimposed on the calcic marble; (g) contact zone of the veined garnet skarn with calcic marble; (h) scheelite coexisting with garnet and calcite in the center of the veined garnet skarn; (i) pyroxene-garnet skarn formed in the magnesian marble; (j) scheelite occurring as interstitial grains between garnet and pyroxene; (k) massive Cu (W) ore hosted in the Carboniferous dolomite; (l) chalcopyrite coexisting with pyrrhotite, sphalerite, bismuthine, native bismuth and scheelite; (m) veined Cu (W) ore superimposed on serpentine in the dolomitic marble; (n) chalcopyrite coexisting with pyrrhotite, scheelite, calcite and serpentine (correspondence between the hand specimen and the photomicrographs: a-b; c-d, e; f-g, h; i-j; k-l; m-n). Ap-apatite; Bis-bismuthinite; Cal-calcite; Ccp-chalcopyrite; Fl-fluorite; Grt-garnet; Mbl-marble; Ms-muscovite; Pl-plagioclase; Po-pyrrhotite; Pyx-pyroxene; Qz-quartz; Sch-scheelite; Srp-serpentine |
(1) 热液脉型矿化：该类型矿化主要呈以石英+白钨矿+白云母+萤石组合的细脉穿插在二叠系灰岩或钙质矽卡岩中(图 3、图 4a, b)，这些热液矿脉的宽度可以从0.2cm变化到大于10cm。
(2) 蚀变花岗岩型矿化：这些花岗岩主要侵位于石炭纪灰岩和二叠纪碳酸盐岩中(图 3)，蚀变花岗岩中的斜长石几乎完全被蚀变交代，仅保留了外形(图 4c, d)，并且白钨矿、黄铜矿呈浸染状分布在这些蚀变花岗岩中(图 4a)；可见白钨矿、黄铜矿与白云母、萤石紧密共生(图 4e)。
(3) 矽卡岩型矿化：该类型矿化是朱溪矿床中最重要的矿化类型，根据矿体形态可以进一步细分为层状矽卡岩矿体和脉状矽卡岩矿体。层状矽卡岩矿体中，几乎所有的碳酸盐岩都完全遭受交代作用而形成矽卡岩，这些矽卡岩中绝大部分发生以钨为主的矿化作用，并且白钨矿在石榴石和辉石的粒间间隙中生长(图 4i, j)，并伴随着一些磁黄铁矿的结晶。同时，在层状矽卡岩和内矽卡岩中出现了一些透镜状的W(Cu)矿体，在这些W(Cu)矿体中，白钨矿和黄铜矿、磁黄铁矿、闪锌矿、辉铋矿及自然铋共生(图 3、图 4k, l)。在脉状矽卡岩发育的地层中，碳酸盐岩部分或完全转变为大理岩，并且被矽卡岩脉所穿插，矽卡岩脉和大理岩之间有着十分清晰的界线(图 4f, m)。此外，脉状矽卡岩中，白钨矿通常和石榴石一起在脉状矽卡岩的中部结晶(图 4f-h)。
3 样品准备及测试方法首先磨制加厚探针片(~300μm)，通过显微镜下观察，选取代表性的磷灰石和白钨矿颗粒在中国地质科学院矿产资源研究所电子探针实验室进行背散色(BSE)图像拍摄，明确这些矿物的内部结构。尽管BSE图像显示白钨矿颗粒内部成分均一，没有分带特征；但是，前人研究表明，即使BSE图像下均一的白钨矿颗粒，通常在CL图像下也会显示出不均匀的特征(Poulin et al., 2016)。为此，本研究在中国地质科学院地质研究所自然资源部大陆动力学重点实验室对待分析的白钨矿进行阴极发光图像(CL)拍摄，进一步通过CL图像来更好地观察白钨矿的内部结构。如图 5所示，磷灰石(图 5f)和白钨矿(图 5h)分别在BSE图像和CL图像中均表现出相对均一的特征，没有明显的分带特征。在明确矿物内部结构的基础上，选取合适的点位进行电子探针、LA-ICP-MS微量元素、LA-MC-ICP-MS U-Pb同位素测试分析。
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图 5 朱溪矿床深部似层状钨(铜)矿体代表性矿石手标本和微观地质特征图像 (a)白钨矿、黄铜矿共生呈脉状穿入大理岩化白云岩中(荧光灯下拍摄)；(b、c)磷灰石呈自形粒状被大片黄铜矿包裹，并可见少量黄铜矿被自形磷灰石包裹；(d)黄铜矿沿白钨矿颗粒边缘呈不规则状、脉状生长；(e)自形粒状磷灰石被黄铜矿和白钨矿包裹；(f)被黄铜矿包裹的磷灰石的背散射(BSE)图像；(g)半自形粒状的粗粒白钨矿；(h)半自形粒状的粗粒白钨矿的阴极发光(CL)图像. (b)-(e), (g)为反射光图像 Fig. 5 Photograph (under ultraviolet light, a) and representative reflected (b-e, g), backscattered electron (f) and cathodoluminescence (h) photomicrographs of the stratiform-like ore of the Zhuxi deposit (a) scheelite and chalcopyrite superimposed on the marbleized dolomite in the form of veins; (b, c) the euhedral apatite grains are surrounded chalcopyrite, and a small amount of chalcopyrite is enclosed by apatite grains; (d) chalcopyrite grows irregularly and vein-like along the edges of scheelite grains; (e) the euhedral apatite grains are wrapped by chalcopyrite and scheelite; (f) the Backscatter (BSE) image of apatite wrapped by chalcopyrite; (g) the euhedral and subhedral coarse-grained scheelite; (h) the cathodoluminescence (CL) image for the euhedral and subhedral coarse-grained scheelite |
磷灰石微量元素测试分析在中国地质大学(北京)科学研究院LA-ICP-MS实验室完成，所用仪器为连接New Wave 193ss激光剥蚀系统的Agilent 7500a型质谱仪。实验过程中，激光剥蚀束斑直径约为50μm，可控激光能量8.5J/cm2，采集时间为45s，以He为载气，流量为0.98L/min。激光剥蚀方式为单点方式，激光器工作频率为10Hz。电感耦合等离子体质谱仪的冷却气为氮气，流量为15L/min，辅助器为氩气，流量为1.15L/min。测试每5个未知点后，进行一次NISTsRM 610测试。为增强能量的稳定性，整个激光剥蚀路径以Ar气作为载体(1.13L/min)。Ti、Zr、Nb、Hf、Ta、206Pb、208Pb、Th和U的计数时间为40ms，207Pb的计数时间为20ms，204Pb的计数时间为100ms，其他元素的计数时间为20ms。微量元素处理过程选用NISTsRM 610玻璃作为外标，磷灰石的43Ca含量(根据电子探针测试的平均CaO含量计算)作为内标，并使用GLITTER软件(Griffin et al., 2008)进行处理。
白钨矿微量元素微区原位测试分析工作在中国地质科学院国家地质实验测试中心内完成，测试方法采用激光剥蚀电感耦合等离子质谱仪(LA-ICP-MS)。使用仪器为Thermo Element Ⅱ单接收四极杆等离子质谱仪，配合激光剥蚀系统为New Wave UP-213。实验采用He作为剥蚀物质的载气，激光波长213nm、激光束斑直径为50μm、脉冲频率10Hz、能量0.176mJ、密度23~25J/cm2，测试过程中首先遮挡激光束进行空白背景采集15s，然后进行样品连续剥蚀采集45s，停止剥蚀后继续吹扫15s清洗进样系统，单点测试分析时间75s。等离子质谱测试参数为冷却气流速(Ar)15.55L/min；辅助气流速(Ar)0.67L/min；载气流速(He)0.58L/min；样品气流速0.819L/min，射频发生器功率1205W。大部分元素检测限设定为0.1×10-6以下，运行精度 < 10%。微量元素处理过程选用NISTsRM 610玻璃作为外标，白钨矿的43Ca含量(根据电子探针测试的单个样品平均CaO含量计算)作为内标，并使用GLITTER软件(Griffin et al., 2008)进行处理。
磷灰石微区原位LA-MC-ICP-MS U-Pb同位素定年在中国地质调查局天津地质调查中心实验测试室完成。所用仪器为Neptune多接收电感耦合等离子体质谱仪，激光剥蚀系统为UP193 ArF准分子激光器，采用的波长为193nm，脉冲宽度为5ns。测试过程中激光剥蚀束斑为55μm、激光频率为8Hz、激光能量密度为10J/cm2。采用磷灰石标准OtterLake对分析过程中的U、Pb同位素分馏进行校正(Barfod et al., 2005; Chew et al., 2011)，采用NISTsRM 610玻璃作为外标计算磷灰石的U、Pb含量，数据处理采用ICPMSDataCal程序(Liu et al., 2010)和Isoplot程序(Ludwig, 2003)进行分析和作图。详细的分析过程见周红英等(2012)。
4 测试结果电子探针测试数据如表 1示，白钨矿和磷灰石的主要成分组成CaO、P2O5、WO3含量较为均一，白钨矿具有相对较低的MoO3含量(0.45%~0.59%)，而磷灰石具有富F(1.75%~2.31%)而贫Cl(≤0.01%)的特征。
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表 1 朱溪矿床深部似层状钨(铜)矿体白钨矿、磷灰石电子探针成分测试结果(wt%) Table 1 EPMA chemical composition (wt%) of the scheelite and apatite from the deep seated stratiform-like W(Cu) ore of the Zhuxi tungsten deposit |
LA-ICP-MS微量元素数据如表 2所示，白钨矿的稀土元素含量整体较低，并且变化不大(∑REE：1.69×10-6~13.72×10-6)，而磷灰石的稀土含量变化较大(∑REE：0.61×10-6~77.02×10-6)。但是白钨矿和磷灰石具有一致的正Eu异常(2.04~7.24和1.65~29.92)和负Ce异常(0.43~0.54和0.19~0.51)(图 6)。
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表 2 朱溪矿床深部似层状钨(铜)矿体白钨矿、磷灰石LA-ICP-MS稀土元素测试结果(×10-6) Table 2 LA-ICP-MS chemical composition (×10-6) of the scheelite and apatite from the deep seated stratiform-like W(Cu) ore of the Zhuxi tungsten deposit |
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图 6 朱溪矿床深部似层状钨(铜)矿体及含白钨矿钠长岩所含白钨矿(a)和磷灰石(b)球粒陨石标准化稀土元素配分模式曲线图(标准化值据Boynton, 1984) 钠长岩所含白钨矿、磷灰石数据来源于Song et al. (2021) Fig. 6 Chondrite-normalized REE patterns of scheelite (a) and apatite (b) grains from the stratiform-like W(Cu) ore and the scheelite-bearing albitite of the Zhuxi tungsten deposit (normalization values after Boynton, 1984) Data of scheelite and apatite in the scheelite-bearing albitite from Song et al. (2021) |
如表 3所示，磷灰石原位LA-MC-ICP-MS U-Pb同位素测试结果表明本研究所测试的磷灰石颗粒的U含量为30×10-6~345×10-6，平均值为102×10-6，具有较高的U含量，确保了所测试磷灰石颗粒具有较高含量的放射性成因Pb，能获取可靠的磷灰石结晶年龄。测试结果显示这些所测试的磷灰石的U-Pb同位素组成在Tera-Wasserburg谐和图解上的下交点年龄为150.2±2.4Ma(图 7)。
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表 3 朱溪矿床深部似层状钨(铜)矿体磷灰石原位LA-MC-ICP-MS U-Pb同位素测试结果 Table 3 In situ LA-ICP-MS U-Pb dating results for the apatite from the deep seated stratiform-like W(Cu) ore of the Zhuxi tungsten deposit |
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图 7 朱溪矿床似层状钨(铜)矿体所含磷灰石LA-ICP-MS U-Pb定年结果 Fig. 7 LA-MC-ICP-MS U-Pb age for apatite grains from the stratiform-like W(Cu) ore of the Zhuxi tungsten deposit |
从手标本可以看出朱溪深部似层状钨(铜)矿体中黄铜矿和白钨矿呈脉状穿入大理岩化的白云岩中(图 5a)，镜下显示白钨矿和黄铜矿虽然共生(图 5b-d)，但是可见黄铜矿沿白钨矿裂隙生长(图 5d)。为此，这些似层状钨(铜)矿体中钨、铜是否为同期形成，并且与前人研究朱溪矿床已报道的成岩、成矿时代(~150Ma)是否一致，需要进一步研究厘定。如图 6所示，尽管似层状钨(铜)矿体中的白钨矿和磷灰石的稀土配分曲线变化较大，但二者整体上具有近于一致的配分模式。鉴于稀土元素性质相似，并且白钨矿与磷灰石在空间上紧密共生，说明白钨矿和磷灰石是从同一热液体系结晶形成。同时，白钨矿和磷灰石均表现出明显一致的负Ce异常(0.43~0.54和0.19~0.51；表 2)，同样说明空间上共生的白钨矿和磷灰石结晶于相同的热液体系；而且白钨矿和磷灰石均表现出明显的正Eu异常(2.04~7.24和1.65~29.92；表 2)，说明白钨矿和磷灰石结晶的体系中Eu呈Eu2+与Ca2+发生了显著的替代作用，进一步指示白钨矿和磷灰石均结晶于还原体系。此外，白钨矿、钼钨钙矿是一个连续的固溶体系列的两个端元，在氧化条件下容易形成富含钼钙矿(CaMoO4)的白钨矿，而在还原条件下则有利于形成纯的白钨矿和辉钼矿(Hsu and Galli, 1973)。因此，白钨矿中的Mo含量可以反映成矿流体中白钨矿结晶时的氧化还原条件变化。例如，在Skrytoe还原型矽卡岩钨矿床中的白钨矿的Mo含量十分低(通常为0.001%~0.05%，很少有超过0.2%)(Soloviev and Kryazhev, 2017)，而Kara氧化型的矽卡岩钨矿中的白钨矿却具有中等含量的Mo(~3% MoO3)(Zaw and Singoyi, 2000)。为此，朱溪似层状钨(铜)矿体中白钨矿具有较低的MoO3含量(0.45%~0.59%；表 1)，同样说明白钨矿结晶时的热液体系氧逸度较低。
此外，鉴于稀土元素族各种元素地球化学行为十分相似、通常具有共同变化的特点，似层状钨(铜)矿体中的白钨矿和磷灰石与朱溪成矿相关岩浆极端分异情况下产生的残余岩浆(已经达到流体饱和)结晶的含白钨矿钠长岩(Song et al., 2021)中的白钨矿(图 6a)和磷灰石(图 6b)具有相似的稀土配分曲线，暗示似层状钨(铜)矿体的形成在成因上与高分异残余岩浆释放的热液流体密切相关。值得注意的是，朱溪钠长岩中的磷灰石相对于似层状钨(铜)矿体中的磷灰石具有显著较高的稀土含量，同时显示出明显的负Eu异常；这种现象很可能是由于钠长岩中磷灰石结晶晚于富钠斜长石的结晶，而富钠斜长石的大量结晶导致了残余岩浆体系中稀土元素的富集和Eu元素的亏损，进而导致钠长岩中晚期结晶的磷灰石继承了这种稀土元素组成特征。此外，朱溪矿床高分异残余岩浆(流体)遭受灰岩混染时形成的含白钨矿钙长岩中含有大量高度还原条件下才能形成的富Mn钛铁矿(MnO含量：6.6%~8.3%; Song et al., 2018a)，这种还原条件下显然不利于Cu元素的富集成矿。基于上述论述，似层状钨(铜)矿体中的钨、铜矿化虽然是由同一热液体系导致，但是钨来源于高分异的残余岩浆热液流体，而铜更可能是来自残余岩浆热液流体对朱溪矿区基底地层——双桥山群中铜元素的萃取活化。
5.2 磷灰石微区原位LA-MC-ICP-MS U-Pb定年对似层状钨(铜)矿体铜矿化作用的限定不同于钼、锡矿化作用，可以直接选用矿石矿物来限定成矿时代(Mao et al., 1999; Yuan et al., 2008, 2011)，岩浆热液作用形成的铜矿化通常选用与富铜矿物紧密共生、并且适合定年的辉钼矿或副矿物来间接地精确限定其成矿时代。值得注意的是，适合定年的副矿物需要满足以下条件(Romer and Öhlander, 1994)：①直接与矿化作用紧密相关；②广泛出现在矿化过程中；③能采用U-Pb定年成功地限定矿物形成时代。对于还原型钨矿床(不含Mo)，磷灰石是一种比较理想的定年矿物。首先，不含Mo的矽卡岩钨矿通常与过铝质的S型花岗岩相关，磷灰石在该类花岗质岩浆中的溶解度随铝饱和指数的增大而增大(Wolf and London, 1994)，因此，还原型矽卡岩钨矿床的成矿相关岩体出溶的流体中必然含大量的P元素，从而在矿化过程中形成大量磷灰石；例如，除朱溪矿床外，俄罗斯还原型钨矿(不含Mo)——Skrytoe矿床的矿石中磷灰石含量高达5%~40%(Soloviev and Kryazhev, 2017)。其次，S型花岗岩的源区通常为经历过地表风化作用的变质沉积物，具有明显较高U含量(Bea and Montero, 1999)，而U为不相容元素，必然在部分熔融作用过程中选择性地优先进入到熔体中(Cuney and Barbey, 2014)，并且在岩浆形成后的演化过程中U会在残余岩浆中不断富集(Cuney, 2009; Linnen et al., 2014)；而钨矿化作用通常与岩浆演化最晚阶段形成的高分异岩脉相关(Yuan et al., 2018)；因而，还原型钨矿床成矿相关岩浆演化晚期必然出溶具有高U含量的岩浆热液流体。例如，朱溪矿床中残余岩浆(流体)遭受灰岩混染时形成的含白钨矿钙长岩中可见磷灰石与晶质铀矿紧密共生(Song et al., 2018a)。此外，磷灰石原位U-Pb定年方法已经十分成熟，广泛用于成岩、成矿时代的限定(Li et al., 2012; Zhang et al., 2021; 周红英等, 2012)。
如图 5显示，黄铜矿不仅包裹着大量自形粒状的磷灰石(图 5b, c, e, f)，而磷灰石中同样包裹着少量黄铜矿(图 5b, c)，说明黄铜矿与磷灰石为同期形成。为此，通过磷灰石的原位U-Pb定年，可以间接地精确限定该类矿石中铜的矿化时代。该类矿石形成于古生代碳酸盐岩与新元古代浅变质岩不整合接触面附近，代表着朱溪矿床中最为重要的铜矿化作用。这些磷灰石在Tera-Wasserburg谐和图解上的下交点年龄(150.2±2.4Ma)与前人研究获得的朱溪矿床成岩、成矿时代(~150Ma)近于一致(Pan et al., 2017, 2018; Song et al., 2018b, 2019; Zhang et al., 2020)，进一步说明朱溪矿床中钨、铜为同期矿化。朱溪矿区内出现的新元古代含铜花岗斑岩(万浩章等, 2015)和(或)地层中的基性火山岩夹层可能为朱溪矿区内在晚侏罗世发生的铜矿化作用提供成矿物质。例如，江南古陆钨矿带东延的浙江平水地区发育着新元古代的块状硫化物Cu-Zn矿床(Chen et al., 2015)，说明区域新元古代地层中存在着富含硫化物的火山岩夹层。此外，Sun et al. (2018)对江南钨矿带与朱溪矿床近于同期形成的石门寺钨(铜)矿床成矿相关岩体的氧逸度，以及黄铜矿的微量元素、S-Pb-Nd同位素进行了研究，结果表明石门寺的成矿相关岩体为还原性的S型花岗岩，不利于大规模的Cu成矿作用，矿床形成过程中Cu元素很可能来自于双桥山群中局部富集Cu的岩层。因此，在晚侏罗世的岩浆活动过程中，朱溪矿区内新元古代的含铜花岗斑岩和(或)地层中的基性火山岩夹层中的铜元素可能会被萃取出来进入成矿热液流体，并伴随白钨矿的结晶而再次沉淀。朱溪矿床中这种可能的“钨铜共生”的成矿机制与我国华南个旧矿集区“锡铜共生”的成矿机制类似：尽管卡房矿区的Cu-Sn矿石的形成与同一岩浆热液系统密切相关，但是铜的来源可能是作为矿体围岩的三叠纪玄武岩，而锡则可能来源于白垩纪花岗质侵入体(Cheng et al., 2012)。值得注意的是朱溪矿床中0.11Mt的铜相对于3.44Mt的WO3资源量是微不足道的，相对于朱溪矿床中巨量的钨，岩浆热液流体对基底双桥山群地层中铜元素的萃取，便能导致朱溪矿床“钨铜共生”的特殊地质现象的形成。
6 结论朱溪矿床深部似层状钨(铜)矿体中的白钨矿和黄铜矿是从同一热液流体结晶形成，该热液流体成因上与朱溪矿床成矿相关岩浆高程度结晶分异后形成的残余岩浆热液流体相关。
朱溪矿床深部似层状钨(铜)矿体中的铜矿化时代为150.2±2.4Ma，与朱溪矿床的钨矿化时代及成钨岩体的成岩时代近于一致。
致谢 野外考察及样品采集得到孔志岗博士、谢涛、康川、魏锦、许杰辉等工程师的热心帮助；电子探针测试得到中国地质科学院矿产资源研究所电子探针室的陈振宇研究员、陈小丹助理研究员的帮助；白钨矿阴极发光图像拍摄得到中国地质科学院地质研究所施彬老师的帮助；LA-ICP-MS微量元素测试得到中国地质大学(北京)苏犁教授、张红雨博士和中国地质科学院国家测试中心赵令浩博士、孙东阳老师的帮助；磷灰石LA-MC-ICP-MS U-Pb年龄测试得到中国地质调查局天津地质调查中心周红英高级工程师的帮助；两位审稿人对文章提出了诸多宝贵意见；在此一并表示衷心感谢！
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