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作者简介:

赵志强(1990—),男,2016年硕士毕业于西北大学文化遗产学院,馆员,E-mail:zhaozq301@163.com

中图分类号:K876.3

文献标识码:A

文章编号:1005-1538(2020)05-0051-08

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目录contents

    摘要

    为研究湖南桃源县战国楚墓出土彩绘陶器的组成结构及保存现状,采用能量色散X射线荧光光谱法(EDXRF)、扫描电镜-能谱法(SEM-EDS)、X射线衍射法(XRD)和激光拉曼光谱法(LRS)等手段对陶器胎体成分、表面彩绘、金属涂层等进行分析检测。结果表明:这批彩绘陶器胎体成分相近,为普通易熔黏土。彩绘陶器表面的红色颜料为朱砂(HgS),黑色颜料为炭黑(C)。在彩绘陶壶、陶鼎和陶敦表面发现金属涂层装饰,通过扫描电镜能谱和X射线衍射分析,确定涂层为单质锡,属于锡涂陶的范畴。同时红外光谱测试显示锡层内面棕黑色物质为生漆,可能混合其他胶结材料。以上结果为研究战国时期彩绘陶器,特别是锡涂陶的制作工艺及发展提供了新的资料。

    Abstract

    In order to study the composition, structure and status of preservation of polychrome potteries excavated from a Chu tomb of the Warring States period in Taoyuan County, Hunan Province, we used energy dispersive X-ray fluorescence (EDXRF) spectrometry, scanning electron microscopy-energy dispersive spectrometry (SEM-EDS), X-ray diffraction (XRD) and laser Raman spectrometry (LRS), etc. to analyze the chemical compositions of pottery bodies and pigments on pottery surfaces and metal coatings. The chemical compositions of pottery bodies, which are made from fusible clay, are similar. The red pigment on pottery surfaces is cinnabar (HgS) and the black is carbon black (C). According to the SEM-EDS and XRD analyses, a layer of tin, as a typical decoration, was identified on pottery surfaces. By Fourier transform infrared (FTIR) spectrometry, the black material on the inner side of the tin layer is mainly lacquer, along with other types of binding materials. This paper provides new data for future research on the craftsmanship and development of tin-decorated pottery during the Warring States period.

    关键词

    战国楚墓彩绘陶组成结构锡层

  • 0 引言

  • 彩绘陶是指在器物表面饰以彩绘纹饰的陶器。与彩陶制作方法不同,彩绘陶是在陶器烧成后使用各类矿物颜料施彩,由于颜料未经烧制,容易剥落。作为我国陶瓷史上具有代表性的品种,彩绘陶早在新石器时代就已出现[1]。此后延续较长时间,是一类珍贵的考古实物资料,长期以来一直受到众多研究人员的关注[2-4]。

  • 2018年10月,湖南省文物考古研究所在位于湖南桃源县的打锣岗抢救性发掘了一座战国晚期楚墓,墓葬出土陶豆、陶鼎、陶壶、陶敦、陶罐等陶制品。在初步清理过程中,发现陶壶、陶鼎和陶敦表面部分区域有黑色涂层,局部可见金属箔片。为探究这批彩绘陶器的胎体成分、颜料种类和金属箔片属性,利用X射线荧光光谱仪等仪器对彩绘陶器进行取样分析,希望以此来了解它们的化学组成和工艺特征,同时也为后续彩绘陶器的保护修复提供科学依据。

  • 1 实验部分

  • 样品信息

  • 桃源打锣岗墓葬出土的这几件彩绘陶器,器表为灰色或褐色,胎体颜色多是灰色或红灰相杂,此外陶土原料多未经淘洗,放大观察下,部分器物残块的断面可见细小砂粒。彩绘陶器形包括豆、壶、鼎、敦,仅陶壶保存相对完整。彩绘颜色有红、黑两种,大多脱落严重。陶器样品概况见表1。通过对陶壶和碎块的观察,发现陶鼎、陶壶和陶敦表面有黑色涂层,涂层主要分布在器物两弦纹或凸棱之间,而不是整体覆盖。部分样品照片见图1。

  • 表1 彩绘陶器基本情况

  • Table 1 Description of the analysed painted potteries

  • 图1 桃源战国墓葬出土部分器物照片

  • Fig.1 Appearances of some samples from the Warring States period tomb in Taoyuan County

  • 1.2 实验仪器

  • 1)X射线荧光光谱仪。美国Thermo Fisher ARL QUANT’X型,铑(Rh)靶X-射线光管,输入电压4~50 V,测试电流自动调节;电制冷硅漂移探测器,元素检测范围为Na(11)~U(92);其中轻元素为真空环境下测试,每个点的测试时间为400 s。胎体成分检测使用国家土壤标样GSS5、GSS7、GSS8、GSS9、GSS12、GSS17、GSS18、GSS20、GSS25,利用测试软件内置的基本参数法建立陶瓷胎体的定量分析方法。

  • 2)扫描电镜-能谱仪。扫描电镜为ZEISS EVO MA 10,二次电子和背散射电子像分辨率3.0 nm@30 kV、4.0 nm@30 kV,工作电压20 kV;能谱仪为Bruke X Flash Detector 6|30型,能谱测试时间60 s,样品测试前均进行喷金处理。

  • 3)X射线衍射仪。日本理学Rigaku Ultima-IV X射线多晶粉末衍射仪,测试电压40 kV,电流40 mA,纵向限制狭缝10 mm,测试速度为10°/min。

  • 4)激光拉曼光谱仪。Renishaw生产invia拉曼光谱分析仪(配Leica显微镜)。半导体激光器(514 nm),物镜放大倍数为100倍,信息采集时间为10 s,累加次数1~3次。测试时将颜料置于载玻片上,用无水乙醇浸润、搅拌,在显微镜下选择需要分析的样品区域。

  • 5)傅立叶变换红外光谱仪。Nicoleti S10,DTGS检测器,测试范围4000~400 cm-1,背景扫描次数32,样品扫描次数32,分辨率4 cm-1,检测方法为KBr压片投射光谱法。

  • 1.3 实验结果

  • 1.3.1 XRF分析结果

  • 测试时以陶块样品的断面部位为准,其中M1-5和M1-6陶豆胎体和彩绘层之间有一层灰色物质,触感较为细腻,也一并进行测试。M1-1因保存完整,故未进行检测。样品的成分数据如表2所示,仅列出常量元素含量。

  • 表2 彩绘陶器胎体的成分数据

  • Table 2 Chemical composition of pottery bodies(%)

  • 1.3.2 SEM-EDS分析结果

  • 本次实验的样品主要包括陶器表面红色和黑色颜料小残块,及起翘或者剥落的涂层残片。能谱结果见表3(限于篇幅仅列出8种重要元素),部分样品的SEM照片见图2和图3。

  • 1.3.3 XRD分析结果

  • 为检测金属涂层的化学组成,分析了M1-2陶壶表面脱落的金属涂层残片。XRD结果显示涂层主要成分为单质锡,同时存在锡的氧化物SnO(图4)。

  • 表3 样品能谱分析结果

  • Table 3 EDS results(%)

  • 图2 M1-5红色和黑色颜料SEM照片

  • Fig.2 SEM images of the red and black pigments of M1-5

  • 图3 M1-7金属涂层SEM照片

  • Fig.3 SEM images of the metal coating of M1-7

  • 图4 M1-2样品金属涂层的XRD图谱

  • Fig.4 XRD pattern of the metal coating of M1-2

  • 1.3.4 LRS实验结果

  • 在能谱测试结果的基础上,利用激光拉曼光谱仪对M1-1、M1-5和M1-63件样品中的黑色和红色颜料进行检测。结果表明红色颜料均出现同一晶体特征峰,黑色颜料拉曼谱图亦是如此,具体如图5和图6所示。

  • 图5 M1-1红色颜料拉曼谱图

  • Fig.5 Raman spectrum of the red pigment of M1-1

  • 图6 M1-5黑色颜料拉曼谱图

  • Fig.6 Raman spectrum of the black pigment of M1-5

  • 1.3.5 FTIR实验结果

  • EDS测试结果显示锡层内面棕黑色物质含有相对较高的碳(C),如M1-3涂层内面棕黑色物质的C含量为28.18%,M1-7的为38.21%,疑为有机物残留,故刮取金属涂层与胎体之间的这类棕黑色物质(图7),采用红外光谱进行分析验证。实验共测试4个样品,其红外光谱图基本一致,如图8所示:样品均在3438 cm-1附近有一吸收峰,应为酚羟基的伸缩振动;2926 cm-1和2854 cm-1附近的双肩吸收峰为-CH2-的伸缩振动。结合近年来发表的古代漆膜红外光谱数据[5-6],推测棕黑色物质为老化后的漆层。

  • 图7 锡层下方棕黑色物质

  • Fig.7 Brownish black substance under the Sn layer

  • 图8 棕黑色物质红外光谱图

  • Fig.8 FTIR spectrum of the brownish black sample

  • 2 数据分析与讨论

  • 2.1 陶器化学组成

  • 表2列出了彩绘陶器的成分数据(除M1-1),可以看出,不同器型的陶器胎体在原料上差别不大,成分特征较为一致。其中SiO2含量在64%~68%之间,Al2O3为20%~25%,Fe2O3的含量在3.3%~6.5%,熔剂氧化物的含量在11%左右,属于普通易熔黏土。另外,关于陶豆胎体上的灰色物质,断面可看出它与胎体有明显的分层(图9)。这类灰色物质触感细腻,结构更为致密,成分数据也显示灰色层与陶豆胎体成分存在差异,其Al2O3含量在16%左右,SiO2约为75%,Fe2O3为2.5%左右。较之陶胎成分数据,灰色物质具有较低含量的Fe2O3、Al2O3和较高含量的SiO2,可能经过淘洗加工,作为打底材料。

  • 图9 M1-5陶豆断面外观照片

  • Fig.9 Cross section of Sample M1-5

  • 2.2 颜料的物相组成

  • 图2和表3为颜料的微观结构照片和能谱数据,能谱数据显示红色颜料(M1-1、M1-5和M1-6)有Hg和S元素。图5为红色颜料的拉曼光谱图,在254.1 cm-1、286.3 cm-1和347.8 cm-1处有明显的拉曼峰值,为朱砂(HgS)的拉曼特征峰[7],这与能谱测试数据一致。黑色颜料的能谱数据显示其C含量相对较高,M1-1为23.26%,M1-5的含量是29.62%。图6为黑色颜料的拉曼光谱,光谱中位于1361 cm-1和1597 cm-1附近的两个宽峰属于无定形碳的特征峰[8],因此黑色颜料为炭黑。

  • 2.3 陶器的“锡涂”工艺

  • “锡陶”一词是根据马王堆一、三号汉墓遣策中的记载而命名的,释读为“锡涂”[9]。“锡涂”,顾名思义,是将金属锡附着于物体之上。关于锡涂工艺,李建毛先生[9]认为陶器锡涂采用沉浸法热镀,即将陶器浸入锡液之中取出,使附着的锡与空气中的O2反应生成银白色的SnO2保护膜。王宜飞[10]则通过陶器锡涂工艺的模拟试验,即按照沉浸法热镀锡、锡汞齐镀锡和锡箔粘接的方法进行操作,结果表明马王堆汉墓出土锡涂陶采用的是贴锡工艺。因此,“锡涂陶”不能笼统地概括为一类使用镀锡方法制作的陶器,其锡涂方法还应包括贴锡工艺。桃源打锣岗的这几件彩绘陶器,EDS和XRD结果表明彩绘陶器上金属涂层的锡含量高达63.89%,主要成分以单质锡为主,还含有锡的氧化物SnO。图3为锡层的SEM照片(M1-7),锡层表面可见明显褶皱和龟裂纹,应是在粘接锡箔时产生。利用超景深显微镜的尺寸测量功能,测得锡箔厚度约11 μm(图10),与马王堆汉墓出土锡涂陶涂层厚度接近[10]。同时,红外光谱显示锡箔内面的棕黑色物质为生漆,若采用镀锡的方法进行“锡涂”,熔融状态下的锡液势必会造成生漆底层的劣化起翘,以上特征说明这几件彩绘陶极大可能采用的是常温贴锡工艺,即在陶器之上使用胶粘剂粘接锡箔,至于生漆中是否添加其他胶结材料,还需要进一步分析验证。

  • 根据目前的考古研究资料,锡涂陶主要见于商代晚期至东汉时期。战国时期的锡涂陶大多出自于楚墓,器形以仿铜陶礼器为主,如长沙子弹库战国楚墓[11-12]、湖北江陵太晖观20号战国楚墓[13]、河南信阳城阳城遗址战国楚墓[14]和山东沂源战国墓[15],另外湖北荆门黄付庙楚墓也似有出土[16-17];两汉时期有马王堆汉墓[18-19]、长沙伍家岭西汉墓[20]、安徽霍山西汉墓[21]和陕西咸阳渭城区东汉墓[22]。锡涂陶从其出土地点及数量来看,以长沙居多。需要指出的是,不同时空背景下的锡涂陶器在工艺特征方面仍有一定的区别。本研究提及彩绘陶器和马王堆汉墓陶器的锡涂方式均为贴锡工艺,锡层上方不施彩绘,但也存在差异:桃源出土的这批陶器锡层均只分布在局部区域,而马王堆汉墓锡涂方式为整体覆盖。同时也注意到信阳城阳城遗址战国楚墓出土的锡涂陶是使用锡做底层,其上再施彩绘[14];而山东沂源战国墓锡涂陶和陕西咸阳渭城区东汉墓锡涂陶器使用的是镀锡工艺[15,22]。以上研究结果说明了陶器锡涂工艺的多样性。

  • 另外,也发现保存下来的锡涂陶表面锡层多已氧化成黑色的SnO,且锡层脱落严重。因此,在后续的保存过程中应通过控制环境的温湿度和光照等条件,避免病害进一步加剧。与此同时,锡涂陶的这种外观特性,导致它容易与普通陶器混淆,易被忽略,但作为我国古陶瓷发展历程中的特殊产物,应引起必要的关注。

  • 图10 锡层照片

  • Fig.10 Appearance of Sn layer

  • 结论

  • 对湖南桃源县出土战国时期彩绘陶器的科学检测发现:这批彩绘陶器的胎体成分特征一致,属于易熔黏土;彩绘陶器表面的红色颜料为朱砂,黑色颜料为炭黑;SEM-EDS和XRD分析表明陶鼎、陶壶和陶敦表面金属涂层的化学成分为单质锡和氧化亚锡,其中氧化亚锡为单质锡氧化后生成。4件样品表面装饰锡层的彩绘陶礼器属于锡涂陶的范畴;红外光谱显示锡层内面的棕黑色物质为生漆。已有研究表明,热镀锡的方法无法在陶器表面形成均一的涂层,且熔融状态下的锡液势必会造成生漆层的劣化起翘。因此,本研究的几件彩绘陶器锡涂方式极大可能采用的是常温贴锡工艺。

  • 通过与河南信阳城阳城遗址战国楚墓、山东沂源战国墓、马王堆汉墓和陕西咸阳渭城区东汉墓出土锡涂陶的比较,对不同时空背景下锡涂陶器的制作特征进行探讨,表明了陶器锡涂工艺的多样性。值得一提的是,桃源打锣岗墓葬出土彩绘陶器的时代为战国晚期,长沙子弹库楚墓为战国中期中晚段,马王堆一~三墓为西汉初期。湖南不同时期均有锡涂陶的出土,说明锡涂陶的制作在该地区存在一定的延续性,桃源出土的这几件彩绘锡涂陶器也为研究其制作工艺和发展提供了新的资料。

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