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Volume 25 Issue 3
May  2023
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Article Contents
Abstract
1.   样品与测试方法
2.   结果与讨论
3.   结论
References
Related Articles
SHI Yujing, CHEN Tao, ZHENG Jinyu, LI Xingtong, ZHANG Qian. Mineralogical Characteristic of Garnet Containing Sheaf-like Inclusion from Huanggangliang Deposit, Inner Mongolia[J]. Journal of Gems & Gemmology, 2023, 25(3): 7-15. DOI: 10.15964/j.cnki.027jgg.2023.03.002
Citation: SHI Yujing, CHEN Tao, ZHENG Jinyu, LI Xingtong, ZHANG Qian. Mineralogical Characteristic of Garnet Containing Sheaf-like Inclusion from Huanggangliang Deposit, Inner Mongolia[J]. Journal of Gems & Gemmology, 2023, 25(3): 7-15. DOI: 10.15964/j.cnki.027jgg.2023.03.002
shu

Mineralogical Characteristic of Garnet Containing Sheaf-like Inclusion from Huanggangliang Deposit, Inner Mongolia

  • 1.

    Gemmological Institute, China University of Geosciences, Wuhan 430074, China

  • 2.

    Hubei Gems and Jewelry Engineering Technology Research Center, Wuhan 430074, China

  • 3.

    School of Earth Sciences, China University of Geosciences, Wuhan 430074, China

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  • Received Date: February 13, 2023
    Graphical Abstract
    • Abstract
  • There are various types of inclusions in garnet. In this study, garnets containing sheaf-like inclusions from the Huanggangliang deposit, Inner Mongolia, were examined by conventional mineralogical tests, electron microprobe (EPMA), Raman spectrometer, infrared spectrometer (IR), ultraviolet-visible absorption spectrometer, scanning electron microscope (SEM) and X-ray energy spectrometer, to investigate the mineralogical characteristics of these garnet samples and their sheaf-like inclusions. The chemical composition analysis indicated that these garnet samples are andradite, which contain impurity elements including Mn, Ti, Mg and Cr.Raman spectra also indicated that these samples are andradite. Such garnets are dark brown - brown yellow. UV-Vis absorption spectra showed that the electron transition of Fe3+ between the energy levels of 6A1g→4A1g 4Eg produces a blue-violet absorption peak at 438 nm, which indicates that the colour is mainly caused by Fe3 +. The absorption peak in the IR spectra is related to the vibration of [SiO4]4- and Fe3+. The shift of absorption peaks in different samples is caused by the small amount of grossularite and spessartite. The sheaf-like inclusions in the samples are mainly light brown, some are distributed in hexagonal inclusions, others are radial and fan-shaped, and a few are filamentous. The results of SEM indicated that cross sections of the sheaf-like inclusions are mostly approximately circular, rectangular or triangular hollow channels and the longitudinal section is long strip; partly filled with quartz and galena. Al-rich zonation is found in hexagonal inclusions.
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  • 蛋白石是一种非晶态或微晶的含水二氧化硅矿物，其化学成分为SiO2·nH2O。根据外观特征可以将蛋白石粗分为三大类: 具有变彩效应的贵蛋白石，透明-半透明、体色黄-红色的火蛋白石，以及没有变彩、不透明的普通蛋白石[1-3]。Jones和Segnit[4]根据X射线衍射特征建立了蛋白石的矿物学分类，将其分为Opal-C型(相对有序的α-方石英为主，少量有鳞石英)、Opal-CT型(无序排列的α-方石英、α-鳞石英混杂堆积为主)和Opal-A型(高度无序，近无定形)三种类型。

    蛋白石是一种用于珠宝首饰的宝贵原料，为了满足对蛋白石不断增长的需求，许多国家都在尝试合成蛋白石[5]。1964年Gasrin和Darragh等[6]从钠的硅酸盐中得到胶体的SiO2微细小球体，通过沉降、干燥，再将其粘结，制成合成蛋白石。1968年，Stober[6]进一步发展和优化了这种方法，但问题在于未找到一种很好的固化方法，导致早期的合成蛋白石的硬度和强度都很小。20世纪70年代，法国的Pierre Gilson等[6-8]采用乙醇水解―自发沉降―粘结渗透技术首次成功合成了蛋白石。80年代后期，获得吉尔森合成蛋白石生产权的日本大阪Nakazumi晶体实验室也开展可合成蛋白石的研发工作，并以Inamori合成蛋白石冠名[9]。自1993年以来，俄罗斯Dubna人工蛋白石应用研究中心一直潜心研究宝石级人工蛋白石(欧泊)的工艺技术，其人工蛋白石的新品种相继出现在珠宝市场上[8-10]。

    目前珠宝市场上存在诸多不同制造商生产的合成蛋白石，包括吉尔森合成蛋白石、Kyocera/Inamori合成蛋白石和一些俄罗斯人工蛋白石等[8, 11]，对多种类型合成蛋白石宝石学特征的细致研究将有助于为实验室准确、快速、无损鉴别合成蛋白石提供可行性依据。本文在前人的研究基础上，采用超景深显微镜、傅里叶变换红外光谱(FTIR)、显微激光拉曼光谱(Raman)、紫外-可见吸收光谱(UV-Vis)、激光诱导击穿光谱(LIBS)、X射线荧光光谱(EDXRF)等测试技术，对一类合成粉色蛋白石样品的宝石学特征、谱学特征及颜色成因予以探讨。

    1.1   样品特征

    实验样品选取合成粉色蛋白石原料2件，编号为SOpal-1、SOpal-2(图 1)。肉眼观察，样品呈浅粉色，整体分布较均匀，局部可见颜色富集，样品表面可见白色、浅黄色矿物，玻璃光泽，透明，无变彩，折射率(点测)1.14~1.42，密度2.16~2.20 g/cm3，样品SOpal-1在长、短波紫外光下呈荧光惰性，样品SOpal-2在短波紫外灯下呈弱-中等的黄色荧光，长波下呈强黄色荧光(表 1)。

    Figure  1.  Synthetic pink opal samples
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    Table  1.  Basic gemmological characteristics of the synthetic pink opal samples
    样品号 颜色 光泽 透明度 折射率(点测) 密度/g·cm-3 紫外荧光
    SOpal-1 粉色 玻璃光泽 透明 1.41 2.20 惰性
    SOpal-2 粉色 玻璃光泽 透明 1.42 2.16 SW：弱―中等，黄色；LW：强，黄色
     | Show Table
    DownLoad: CSV

    1.2   测试方法

    红外光谱测试采用Thermo ScientificTM NicoletTM iS50型傅立叶变换红外光谱仪，测试环境为室温25℃，相对湿度40%，反射法测试条件：扫描范围400~4 000 cm-1，扫描次数32次，分辨率8 cm-1，分束器KBr；透射法测试条件：扫描范围400~6 000 cm-1，扫描次数32次，分辨率4 cm-1，分束器KBr；近红外扫描范围4 000~12 000 cm-1，分束器为CaF2。背景扫描次数均为32次。

    激光拉曼光谱测试采用Renishaw in Via型激光共焦显微拉曼光谱仪，测试条件：532 nm激光器和785 nm激光器，光栅1 800 I/mm和1 200 I/mm, 物镜50倍, 输出功率10 mW, 最佳分辨率为1 cm-1, 曝光时间10 s, 信号叠加2次扫描, 测试范围100~2 000 cm-1。

    激光诱导击穿光谱测试采用美国TSI公司生产的ChemRevealTM LIBS台式激光诱导击穿光谱仪，测试条件：能量100%，重复频率1.0 Hz，激光斑束直径50 μm，采集波长范围200~1 000 nm。

    X射线荧光光谱测试采用美国赛默飞世尔科技公司生产的Thermo ScientificTM ARLTMQUANT’X型X射线荧光光谱仪，靶材为Rh，薄铍窗(50 μm)，准直器1 mm，氛围真空，测试范围0~40 keV。

    紫外-可见吸收光谱测试采用广州标旗电子科技有限公司生产的GEM-3000紫外-可见分光光谱仪，测试条件：积分时间150 s，平均次数10次，平滑宽度2，测试范围400~1 000 nm。

    2.1   放大观察

    使用VHX-2000型超景深显微镜对样品进行放大观察发现，样品原料表面可见白色矿物，白色矿物与蛋白石交界处可见浅黄色矿物(图 2a)。样品内部可见细微分散的微纳米级粉红色固相包裹体(图 2b)，进一步放大观察发现其外观可呈球状、椭球状，且在反射光下表面呈金属光泽(图 2c)。利用VHX-2000型超景深显微镜内部自带软件测量，较大颗粒的固相包裹体直径可达170 μm(图 2d)。

    Figure  2.  Digital micrographs of the synthetic pink opal samples: (a) white and pale yellow minerals on the surface of sample SOpal-2, 150×; (b) finely dispersed solid inclusions in sample SOpal-1, 200×; (c) dense distribution of spherical mineral inclusions in sample SOpal-1, 300×; (d) dense distribution of spherical and ellipsoidal mineral inclusions in sample SOpal-2 with the diameter up to 170 μm, 200×
    DownLoad: Full-Size Img PowerPoint

    2.2   红外光谱分析

    前人研究表明[12-13]，在400~2 000 cm-1内，蛋白石主要有3个强谱带，分别位于470、790、1 100 cm-1附近，其中470 cm-1与Si—O—Si弯曲振动有关，790 cm-1与Si—O—Si对称伸缩振动有关，1 100 cm-1与Si—O—Si反对称伸缩振动有关。根据Adamo，Curtis等[12-13]的研究表明，红外光谱是区分Opal-A型、Opal-CT型及Opal-C型蛋白石的一种替代方法，其中位于470、790 cm-1附近的吸收峰与蛋白石的结晶程度有关，完全非结晶质蛋白石(Opal-A型)的特征吸收峰分别位于466~472 cm-1及796~800 cm-1，同时具有550 cm-1附近弱吸收峰；含一定结晶度的蛋白石(Opal-CT型)的特征吸收峰分别位于472~477 cm-1及788~792 cm-1；而主要由相对有序的α-方石英，少量鳞石英组成的蛋白石(Opal-C型)则以475~481 cm-1和793~794 cm-1，以及620 cm-1附近较弱吸收峰为特征。

    红外光谱反射法测试结果(图 3)显示，2件测试样品的红外最强吸收峰位于1 080~1 111 cm-1附近，次强峰位于451~470 cm-1，还具有799~806 cm-1附近弱的吸收谱峰和1 245 cm-1附近弱的肩峰，但未见明显的550 cm-1及620 cm-1附近弱吸收峰(具体峰位归属见表 2)。结果表明，该2件测试样品的类型并非Opal-A型及Opal-C型，应介于Opal-A与Opal-CT之间，且与Opal-A型蛋白石较为接近。

    Figure  3.  Infrared reflectance spectra of the synthetic pink opal samples: (a) diffuse reflection method(K-K); (b) attenuation total reflection method (ATR)
    DownLoad: Full-Size Img PowerPoint
    Table  2.  Peak assignments of the synthetic pink opal samples in mid-infrared and near-infrared spectra
    峰位/cm-1 归属
    451~470 δ(Si—O—Si)
    799~806 νs(Si—O—Si)
    1 080~1 111 νas(Si—O—Si)
    3 674 νs(OH)
    4 523 νs(OH)+ δ(SiOH)
    7 224 2νs(OH)
     | Show Table
    DownLoad: CSV

    红外光谱透射法测试结果(图 4)显示，该类合成欧泊具有7 224、4 523、3 674、2 662、2 266 cm-1附近的一组特征红外吸收谱峰，其中与ν(OH)伸缩振动有关的强吸收峰位于3 674 cm-1附近，由OH合频振动与倍频振动所致的特征吸收峰分别位于4 523、7 224 cm-1附近[14-15]。参考前人研究结果表明[9]，该类合成蛋白石与俄罗斯人工蛋白石的红外透射光谱特征基本吻合。

    Figure  4.  Infrared transmission spectra of the synthetic pink opal samples: (a) NIR, 10 000~6 000 cm-1; (b) Mid-IR, 6 000~2 000 cm-1
    DownLoad: Full-Size Img PowerPoint

    2.3   拉曼光谱分析

    据Sodo，Ostroumov等[16-19]的研究表明，蛋白石通常在200~600 cm-1范围内表现出由Si—O—Si弯曲振动产生的强拉曼信号，拉曼谱带较宽指示了蛋白石的结晶程度较差。同时，200~600 cm-1范围内最高峰值的位置可以用于区分Opal-A型蛋白石(430 cm-1)和Opal-CT型蛋白石(335 cm-1)。

    拉曼光谱测试结果(图 5a)显示，样品在100~2 000 cm-1内显示不同类型的Si—O振动峰，其在200~600 cm-1范围内的最大值位于(420±5) cm-1附近，同时具有由Si—O—Si对称伸缩振动和非对称伸缩振动所致的799 cm-1和1 057 cm-1附近的次强拉曼谱峰。结果表明该2件测试样品的类型较为接近Opal-A型蛋白石，与前文红外光谱结果相吻合。

    Figure  5.  Raman spectra of the synthetic pink opal samples: (a)sample SOpal-1 and SOpal-2; (b) white and light yellow minerals in sample SOpal-2
    DownLoad: Full-Size Img PowerPoint

    对样品SOpal-2表面白色、浅黄色矿物进行拉曼光谱测试，结果(图 5b)显示229 cm-1和417 cm-1附近强且尖锐的拉曼谱峰以及781 cm-1和1 076 cm-1的次拉曼谱峰，与RRUFF拉曼光谱数据库中美国宝石学院的方石英(RRUFF ID: R060648)标准谱峰相吻合。表明样品在合成过程中由于条件、环境及时间等因素的影响，存在部分SiO2胶体逐渐向结晶态转化，形成方石英。

    2.4   化学成分分析

    2.4.1   激光诱导击穿光谱分析

    采用激光诱导击穿光谱技术对2件样品中的元素进行等离子体激发测试，得到波长在200~900 nm的等离子光谱图(图 6)。由于测试结果中谱线复杂，数量较多，因此选取强度较强的特征谱线进行定性分析，结果显示2件样品所含元素种类基本一致，除了主量元素Si外，还含有Na、Mg、K、Ca、Cu等元素。值得注意的是，在测试中检测到了C、N、O等元素的存在，但因无法判定其是因受测试环境条件的影响(如空气)，还是样品在合成过程中的残留物所致，故在此处未进行深入探讨。

    Figure  6.  LIBS spectra of the synthetic pink opal samples: (a) 200~50 nm; (b) 500~900 nm
    DownLoad: Full-Size Img PowerPoint
    2.4.2   X射线荧光光谱分析

    X射线荧光光谱测试结果(表 3，图 7)显示，样品的SiO2含量达97.581%~98.352%，此外还分别含有0.287%~0.497%的Na2O，0.112%~0.326%的MgO，0.895%~1.507%的Al2O3，0.011%~0.026%的K2O，0.003%~0.015%的CaO，0.079%~0.244%的Cu2O。结合激光诱导击穿光谱测试结果分析，样品中Na、Mg、Al、K、Ca等元素并非致色元素，而Fe元素的含量极低，约0.000 5%~0.000 8%，对颜色的贡献有限，因此该类合成粉色蛋白石的颜色成因应与Cu元素有关。

    Table  3.  EDXRF data of the synthetic pink opal samples
    样品号 含量(%)
    Na2O MgO Al2O3 SiO2 K2O CaO FeOT Cu2O
    SOpal-1 测试点1 0.497 0.326 1.378 97.581 0.022 0.003 0.000 7 0.091
    测试点2 0.287 0.239 1.507 97.597 0.018 0.005 0.000 8 0.244
    测试点3 0.495 0.295 1.080 97.838 0.026 0.015 — 0.149
    SOpal-2 测试点1 0.390 0.165 0.895 98.352 0.014 0.003 0.000 5 0.079
    测试点2 0.400 0.240 1.281 97.834 0.013 0.004 0.000 6 0.127
    测试点3 0.290 0.112 1.111 98.265 0.011 0.005 — 0.106
    注：FeOT为全铁质量百分数；“—”代表该元素质量分数低于仪器检出限。
     | Show Table
    DownLoad: CSV
    Figure  7.  XRF spectrum of inclusions in the synthetic pink opal sample SOpal-2
    DownLoad: Full-Size Img PowerPoint

    为了进一步探讨该类合成蛋白石内部固相矿物包裹体的化学成分，对出露表面的包裹体进行元素定性测试，结果显示其主要含有Cu元素(图 7)，合理推测该类合成蛋白石内部的固相矿物包裹体应为铜的某种化合物。

    2.5   紫外-可见吸收光谱分析

    紫外-可见吸收光谱测试(图 8)显示，2件样品均具有570 nm附近的特征吸收峰。据前人[20-22]研究发现，随着形态(如立方体、八面体、球体等)和颗粒大小(如纳米级、微米级等)的变化，固体Cu2O颗粒的外观可呈现不同色调和饱和度的红色(如红、紫红、暗红等)，且通常Cu2O的微纳米颗粒在可见光范围内具有570 nm(直接带隙能Eg ≈ 2.17 eV)附近的最强吸收峰。因此，结合化学成分分析，进一步指示该类合成欧泊的颜色与元素Cu有关，且应主要由铜的氧化物(主要为Cu2O)等矿物颗粒细微分散所致。

    Figure  8.  UV-Vis absorption spectra of the sythetic pink opal samples
    DownLoad: Full-Size Img PowerPoint

    本文揭示了一种合成蛋白石的宝石学及谱学特征，探讨了其致色机理，可以为实验室准确、快速、无损鉴别该类合成蛋白石提供可行性参考依据。通过测试分析，主要得出以下结论。

    (1) 该类合成粉色蛋白石的外观呈粉色，玻璃光泽，透明，无变彩，折射率(点测)1.41~1.42，密度2.16~2.20 g/cm3，放大观察内部可见不同红色调球状、椭球状的微纳米级固相包裹体，直径可达170 μm。

    (2) 红外光谱与拉曼光谱特征显示合成粉色蛋白石的类型应介于Opal-A型与Opal-CT型之间，且与Opal-A型蛋白石较为接近；红外透射光谱显示其具有7 224、4 523、3 674、2 662、2 266 cm-1附近的一组特征红外吸收谱峰，与俄罗斯合成蛋白石较为吻合。

    (3) 化学成分分析与紫外-可见吸收光谱结果表明，该类合成粉色蛋白石的SiO2含量达97.581%~98.352%，此外还含有Na2O(0.287%~0.497%)、MgO(0.112%~0.326%)、Al2O3(0.895%~1.507%)、K2O(0.011%~0.026%)、CaO(0.003%~0.015%)以及Cu2O(0.079%~0.244%)；其颜色主要是由铜的氧化物(主要为Cu2O)等矿物颗粒细微分散所致，并在可见光范围内产生570 nm附近的特征吸收峰。

    感谢中国地质大学(武汉)珠宝学院职教中心徐丰舜老师提供样品。

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