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Zhang X.-M.,Peking University | Wei X.-N.,Peking University | Lei Y.,The Palace Museum | Cheng X.-L.,Center for Conservation of National Museum of China | Zhou Y.,Silk Museum of China
Guang Pu Xue Yu Guang Pu Fen Xi/Spectroscopy and Spectral Analysis | Year: 2010

Dye analysis is important to the understanding of fabric color degradation and technical development of ancient printing and dyeing. In the present study, thin layer chromatography and Raman spectroscopy were used for the analysis of blue dyes from 6 silk fabric of Tang dynasty and decorative painting of Jian Fu Gong, Forbidden City. The applicability of these two methods in the cultural heritages was also studied. The results indicate that all these blue substances are indigo; indigo was not only used as dye in ancient fabrics, but also as pigment in decorative painting of historic building, so it is used widely. Both analytic methods have advantages and disadvantages; Raman spectroscopy is nondestructive analysis; thin layer chromatography needs small amount of sample, but could give more information.

Liu W.,Tsinghua University | Xie Z.,Tsinghua University | Zhang X.,Qingdao University | Jia C.,The Palace Museum | And 3 more authors.
Advances in Applied Ceramics | Year: 2016

In this study, we have made a comprehensive investigation on the optimisation of the compositions of polyethylene glycol (PEG)/polymethyl methacrylate (PMMA) binder system for water debinding. An orthogonal test was designed, and L9(33) table was chosen to investigate the influence of the molecular weight of low molecular PEG (L-PEG), high molecular PEG (H-PEG) and the percentage of L-PEG in PEGs on flaws of the injection moulded compacts after water debinding. In addition, the ratio of PMMA content to PEG content on flaws is also investigated. Four regions were defined as high stress region, safe debinding region, low binder removal rate region and unavailable injection region respectively. It is believed that our work could provide comprehensive and convincing principles for the manufacturing of injection moulded ceramic parts via water debinding. © 2016 Institute of Materials, Minerals and Mining.

Duan H.,Key Scientific Research Base of Ancient Ceramics the Palace Museum | Ji D.,Key Scientific Research Base of Ancient Ceramics the Palace Museum | Ding Y.,Key Scientific Research Base of Ancient Ceramics the Palace Museum | Wang G.,The Palace Museum | And 3 more authors.
Microchemical Journal | Year: 2016

Longquan celadon is one of the most valuable treasures in Chinese ceramic history. Representative products are Ge ware (Ge meaning elder brother, black body celadon) and Di ware (Di meaning younger brother, gray body celadon) of the Song Dynasty (960-1279. A.D.). In this study, Ge and Di ware shards excavated from Wayaoyang kiln site in Longquan were collected and studied. Chemical and crystallite composition, microstructure, body and glaze thickness, firing temperature and glaze reflectance spectrum were observed and examined. Differences in raw materials and manufacturing technology between Ge and Di ware were studied. Based on the results and historical background, it was speculated that some Ge wares from Wayaoyang kiln site might be the test products of jade-like black body celadon for the imperial court. © 2015 Elsevier B.V.

Liu W.,Tsinghua University | Yang X.,Changsha University of Science and Technology | Xie Z.,Tsinghua University | Jia C.,The Palace Museum | Wang L.,Tsinghua University
Journal of the European Ceramic Society | Year: 2012

In this work, we adopt a combination of low molecular weight PEG (L-PEG) and high molecular weight PEG (H-PEG) as water-soluble binder to fabricate injection-moulded ceramic parts with large section. The mechanism of the combination of PEGs removal was proposed for the first time. Defect-free near gear parts with large-sized-section (thickness - 16. mm) were successfully fabricated through water extraction (15. h) followed by rapid thermal pyrolysis (4.5. h). It solves the difficulty of fabricating injection-moulded ceramic parts with large section and our approach is energy saving and high-efficiency as compared with conventional thermal debinding. The results demonstrate that our approach of partially water-debinding followed by rapid thermal pyrolysis could solve the problems of conventional thermal debinding, providing an effective route for the production of injection moulded ceramic parts with large section. © 2012 Elsevier Ltd.

PubMed | The Palace Museum, Wuhan University and Friedrich - Schiller University of Jena
Type: | Journal: Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy | Year: 2015

Two kinds of enamels, including Chinese cloisonn wares from Fuwang chamber and gourd-shaped painted enamels decorations from the Forbidden City, in the Imperial Palace of China, are investigated by micro-Raman spectroscopy in combination with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and energy-dispersive X-ray fluorescence (EDXRF) in order to examine and analyze the composition of the glaze layer in each case. In this study the excitation is employed with either a NIR laser (785 nm) or a red laser (632.8 nm) in order to effectively eliminate the interference of background fluorescence and resonance effect. We have identified that the major matrix ingredients of the cloisonn wares are lead-based potash-lime silicate glasses while lead-potash silicate glass matrix is the main constituent for the painted enamels. Eight different colored areas of glaze layer also have been discussed in detail due to the distinct colors including turquoise, deep blue, yellow, white, red, pink, deep green and pale green. Their identification based on Raman data will be useful with regard to rapid and on site analysis and the restoration of the enamel decorations.

Zi M.,CAS Shanghai Institute of Applied Physics | Zi M.,University of Chinese Academy of Sciences | Wei X.,CAS Shanghai Institute of Applied Physics | Yu H.,CAS Shanghai Institute of Applied Physics | And 2 more authors.
He Jishu/Nuclear Techniques | Year: 2015

Background: Confocal micro-X-ray method is a sensitive tool for analysis of three dimensional (3D) elemental composition and chemical species, and has many important applications in the research fields such as geology, archaeology, environment, biology and materials sciences. Purpose: Confocal micro-X-ray method was established at BL15U in Shanghai Synchrotron Radiation Facility (SSRF) and applied to study the stratified structure of some kind of paints in the Forbidden City. Methods: By the combination of pollycapillary half lens and K-B mirrors, a confocal micro volume is formed by the overlapped foci of these two focusing optics. The confocal system had a depth resolution of about 31.5 μm at 8.04 keV and can be used to perform the confocal micro X-ray fluorescence (Micro-XRF) and confocal micro X-ray absorption fine structure (Micro-XAFS) experiments. Results: A typical structure of Doucai with three glaze layers has been disclosed by the confocal Micro-XRF. The chemical information of Fe inside the paint was obtained by confocal Micro-XAFS. Conclusion: The confocal micro-X-ray facility is indicated to be a powerful tool for 3D analysis of fine arts samples. ©, 2015, Science Press. All right reserved.

Zhao D.,Northwest University, China | Huang J.,Northwest University, China | Song J.-R.,The Palace Museum | Zhong Y.-T.,Northwest University, China | And 2 more authors.
Chemical Research in Chinese Universities | Year: 2012

N-(2,3-Dimethyl-phenyl)-N'-(methoxyl formyl)thiourea was synthesized by the reacting of 2,3-dimethylaniline, potassium thiocyanate(KSCN) and methyl chloroformate(ClCOOCH 3). Single crystal was obtained by slowly evaporation solvent at room temperature. The structure was characterized by elemental analysis, IR and X-ray crystalography. The compound crystallized: a triclinic system with space group Pi, a=0.83440(12) nm, b=0.89113(13) nm, c=0.93015(13) nm, a=76.548(2)o, ß=63.906(2)o, γ=82.538(2)o, V=0.60379(15) nm 3, Z=2, D c=1.311 mg/m 3, F(000)=252, μ=0.256 mm -1, R 1=0.0379, wR 2=0.0919. The specific heat capacity of the title compound was determined by a Micro-DSC method, and the specific heat capacity was 1.25 J.g -1.K -1 at 298.15 K. Thermodynamic functions, relative to those at the standard temperature of 298.15 K, were calculated via thermodynamic relationship. The thermal behavior of the title compound under a non-isothermal condition was studied by differential scanning calorimetry/ thermogravimetric(DSC/TG) method. There was an obvious endothermic peak in the DSC curve, the peak temperature was 479.43 K. The compound mass loss was 89.94% observed from the TG curve.

Chen M.,Northwest University, China | Song J.-R.,The Palace Museum | Ma H.-X.,Northwest University, China
Hanneng Cailiao/Chinese Journal of Energetic Materials | Year: 2016

The geometrical structures, front orbit energy and enthalpies of formation (ΔHf) of thirty kinds of 1, 2, 4, 5-tetrazine derivatives were studied by using DFT-wB97/6-31+G** method. On this basis, the detonation parameters of the derivatives were estimated by Kamlet-Jacobs equation. The bond dissociation energy of the title compounds was analyzed. The thermodynamic properties of part of the title compounds at different temperatures from 200 K to 800 K were calculated by statistical thermodynamics. The detonation performances and stability of 1, 2, 4, 5-tetrazine derivatives were compared. Results show that their ΔHf are between 920.46 and 2610.45 kJ·mol-1and the detonation velocities are between 7.69 and 9.31 km·s-1. -NO2 and -N=N-is not conducive to increase the stability of the derivatives. The values of standard molar heat capacity cp, standard molar entropy Sm and standard molar enthalpy Hm gradually increase with the temperature. i2 (3-(5-Nitro-1, 2, 3, 4-tetrazol)-6-nitro-1, 2, 4, 5-tetrazine), ii2 (3-(azo-5-nitro-1, 2, 3, 4-tetrazol)-6-nitro-1, 2, 4, 5-tetrazine) and iv2 (3, 6-azo-bis (5-nitro-1, 2, 3, 4-tetrazol)-1, 2, 4, 5-tetrazine) may be considered as potential candidates for energetic materials. © 2016, Editorial Board of Chinese Chinese Journal of Energetic Materials. All right reserved.

Ma C.,Northwest University, China | Huang J.,Northwest University, China | Zhong Y.T.,Northwest University, China | Xu K.Z.,Northwest University, China | And 2 more authors.
Bulletin of the Korean Chemical Society | Year: 2013

Two new high-nitrogen energetic compounds ZTO·2H2O and ZTO(phen)·H2O have been synthesized (where ZTO = 4,4-azo-1,2,4-triazol-5-one and phen = 1,10-phenanthroline). The crystal structure, elemental analysis and IR spectroscopy are presented. Compound 1 ZTO·2H2O crystallizes in the orthorhombic crystal system with space group Pnna and compound 2 ZTO(phen)·H2O in the triclinic crystal system with space group P-1. In ZTO(phen)·H2O, there is intermolecular hydrogen bonds between the -NH group of ZTO molecule (as donor) and N atom of phen molecule (as acceptor). Thermal decomposition process is studied by applying the differential scanning calorimetry (DSC) and thermo thermogravimetric differential analysis (TG-DTG). The DSC curve shows that there is one exothermic peak in ZTO·2H2O and ZTO(phen) ·H2O, respectively. The critical temperature of thermal explosion (Tb) for ZTO·2H2O and ZTO(phen)·H2O is 282.21 °C and 195.94 °C, respectively. Copyright © 2005 KCSNET.

PubMed | The Palace Museum and CAS Institute of Remote Sensing
Type: | Journal: Applied spectroscopy | Year: 2016

Spectral analysis is one of the main non-destructive techniques used to examine cultural relics. Hyperspectral imaging technology, especially on the shortwave infrared (SWIR) band, can clearly extract information from paintings, such as color, pigment composition, damage characteristics, and painting techniques. All of these characteristics have significant scientific and practical value in the study of ancient paintings and other relics and in their protection and restoration. In this study, an ancient painting, numbered Gu-6541, which had been found in the Forbidden City, served as a sample. A ground-based SWIR imaging spectrometer was used to produce hyperspectral images with high spatial and spectral resolution. Results indicated that SWIR imaging spectral data greatly facilitates the extraction of line features used in drafting, even using a single band image. It can be used to identify and classify mineral pigments used in paintings. These images can detect alterations and traces of daub used in painting corrections and, combined with hyperspectral data analysis methods such as band combination or principal component analysis, such information can be extracted to highlight outcomes of interest. In brief, the SWIR imaging spectral technique was found to have a highly favorable effect on the extraction of line features from drawings and on the identification of colors, classification of paintings, and extraction of hidden information.

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