化学气相沉积法再生钻石的实验室检测特征研究
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摘要
再生钻石是使用化学气相沉积法(CVD)以天然钻石为基底再生长合成钻石层,得到具有整体外观的钻石产品。由于再生钻石含有天然钻石的氮杂质信息,传统的合成钻石排查方法和检测流程已不再适用于再生钻石的检测。本文对实验室检出的一颗再生钻石进行了详尽的宝石学测试分析,以建立再生钻石的最佳检测方案。结果显示:常规的显微观察、钻石仪器排查以及红外光谱测试都不能将再生钻石检出。DiamondViewTM多方位发光图像观察该样品呈现清晰的发光分层现象,上层为红色荧光与蓝绿色磷光,下层为深蓝色荧光与惰性磷光;红外透射光谱分区域定点扫描样品上层为IIa型钻石,下层为Ia型钻石;紫外可见吸收光谱分析和光致发光光谱测试显示样品同时具有N3和高浓度[Si-V]-缺陷。综合判定该样品亭部的下半部分为天然钻石,亭部的上半部分和冠部为CVD合成钻石,CVD层厚度约740μm。作为我国首例报道的再生钻石,与国外已报道的同类型样品相比,该样品中分层界限不可见,且合成层厚度呈现明显增长。研究认为,应用多方位发光图像分析及光谱测试技术是再生钻石检测的关键。
BACKGROUND: Overgrowth diamond refers to the product of thick CVD synthetic diamond layer grown on a natural diamond with the whole appearance. Since overgrown diamonds contain information on the nitrogen impurities of natural diamonds,traditional synthetic diamond screening methods and testing procedures are no longer applicable to the detection of overgrown diamonds.OBJECTIVE: To gemologically test an overgrowth diamond sample in order to investigate the full identification features and to propose the optimum detection strategy.METHODS: Minspecting,screening instruments testing,UV-Vis/FTIR/PL spectra examinations,as well as fluorescence and phosphorescence observation under deep UV excitation are carried out.RESULTS: The sample cannot be identified by traditional microscopic observation,diamond instrument screening,and infrared spectra measurement. The sample has a distinct boundary that is separated by different luminescence under DiamondViewTM. The upper layer displays red fluorescence and greenish blue phosphorescence,while the lower layer shows deep blue fluorescence and no phosphorescence. Infrared spectroscopic analysis shows that the upper layer is type IIa and the lower layer is type Ia diamond. The UV-Vis absorption and photoluminescence spectra confirmed the coexistence of N3 centers and a high level of [Si-V]-defects in the diamond.CONCLUSIONS: It was confirmed that the lower part of the sample is natural and the upper part of the sample is CVD synthetic layer with a thickness around 740μm. The first overgrowth diamond reported domestically was compared to the same type of samples reported abroad. The existence of a boundary are missing and the thickness of the CVD layer increased significantly in this sample. The innovative application of the multidirectional luminescence imaging and spectroscopic analyses is the key to laboratory testing of overgrowth diamond.
BACKGROUND: Overgrowth diamond refers to the product of thick CVD synthetic diamond layer grown on a natural diamond with the whole appearance. Since overgrown diamonds contain information on the nitrogen impurities of natural diamonds,traditional synthetic diamond screening methods and testing procedures are no longer applicable to the detection of overgrown diamonds.OBJECTIVE: To gemologically test an overgrowth diamond sample in order to investigate the full identification features and to propose the optimum detection strategy.METHODS: Minspecting,screening instruments testing,UV-Vis/FTIR/PL spectra examinations,as well as fluorescence and phosphorescence observation under deep UV excitation are carried out.RESULTS: The sample cannot be identified by traditional microscopic observation,diamond instrument screening,and infrared spectra measurement. The sample has a distinct boundary that is separated by different luminescence under DiamondViewTM. The upper layer displays red fluorescence and greenish blue phosphorescence,while the lower layer shows deep blue fluorescence and no phosphorescence. Infrared spectroscopic analysis shows that the upper layer is type IIa and the lower layer is type Ia diamond. The UV-Vis absorption and photoluminescence spectra confirmed the coexistence of N3 centers and a high level of [Si-V]-defects in the diamond.CONCLUSIONS: It was confirmed that the lower part of the sample is natural and the upper part of the sample is CVD synthetic layer with a thickness around 740μm. The first overgrowth diamond reported domestically was compared to the same type of samples reported abroad. The existence of a boundary are missing and the thickness of the CVD layer increased significantly in this sample. The innovative application of the multidirectional luminescence imaging and spectroscopic analyses is the key to laboratory testing of overgrowth diamond.
引文
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[8] Wang W,Johnson P,Moe K S,et al. CVD synthetic diamonds from gemesis corp[J]. Gems&Gemology,2012,48(2):80-97.
[9] Moses T M,Reinitz I M,Johnson M L,et al. A contribution to understanding the effect of blue fluorescence on the appearance of diamonds[J]. Gems&Gemology,1997,33(4):244-259.
[10] Shigley J E,Breeding C M. Optical defects in diamond:A quick reference chart[J]. Gems&Gemology,2013,49(2):107-111.
[11] Tang S,Su J,Lu T J,et al. A melee-size CVD synthetic diamond in pearl and diamond jewelry[J]. Gems&Gemology,2017,53(3):382.
[12] Wang W,Moses T,Linares R,et al. Gem-quality synthetic diamonds grown by the chemical vapor deposition method[J]. Gems&Gemology,2003,39(4):268-283.
[13] Eaton-Magana S,Shigley J E. Observations on CVDgrown synthetic diamonds:A review[J]. Gems&Gemology,2016,52(3):222.
[14]宋中华,兰延,沈美冬,等. NGTC实验室发现未揭示的CVD合成钻石鉴定特征研究[J].宝石和宝石学杂志,2012,14(4):30-34.Song Z H,Lan Y,Shen M D,et al. Identification characteristics of undisclosed CVD synthetic diamonds found recently by NGTC[J]. Journal of Gems and Gemmology,2012,14(4):30-34.
[15] Collins A T. Colour centers in diamond[J]. Journal of Gemmology,1982,18:35-75.
[16] Collins A T. The colour of diamond and how it may be changed[J]. Journal of Gemmology,2001,27:341-359.
[17] Collins A T,Stanley M,Woods G S. Nitrogen isotope effects in synthetic diamonds[J]. Journal of Physics D:Applied Physics,1987,20(7):969-974.
[18] Collins A T. Intrinsic and extrinsic absorption and luminescence in diamond[J]. Physica B:Condensed Matter,1993,185(1-4):284-296.
[19] Collins A T,Kanda H,Burns R C. The segregation of nickel-related optical centers in the octahedral growth sectors of synthetic diamond[J]. Philosophical Magazine B,1990,61(5):797-810.
[20] Tang S,Song Z H,Lu T J,et al. Two natural type IIa diamonds with strong phosphorescence and Ni-related defects[J]. Gems&Gemology,2017,53(4):476-478.
[21] Song Z H,Lan Y,Shen M D,et al. Identification characteristics of undisclosed CVD synthetic diamonds found recently by NGTC[J]. Journal of Gems and Gemmology,2012,14(4):30-34.
[22]宋中华,魏华,田晶.钻石辨假[M].北京:文化出版社,2017.Song Z H,Wei H,Tian J. Identification of Diamonds[M]. Beijing:Cultural Development Press,2017.
[23] Fisher D,Spits R A. Spectroscopic evidence of GE POL HPHT-treated natural type IIa diamonds[J]. Gems&Gemology,2000,36(1):42-49.
[24]宋中华,陆太进,苏隽,等.利用吸收和发光光谱技术分析高温高压天然富氢钻石的鉴定特征[J].岩矿测试,2018,37(1):64-68.Song Z H,Lu T J,Su J,et al. Identification of HPHTtreated hydrogen-rich diamonds by optical absorption and photo luminescence spectroscopy techniques[J].Rock and Mineral Analysis,2018,37(1):64-69.
[2] Yacobi B G,Lebens J,Vahala K J,et al. Preferential incorporation of defects in monocrystalline diamond films[J]. Diamond&Related Materials,1993,2(2-4):92-99.
[3] Eaton-Magana S. Long-term durability of CVD synthetic film on natural diamond[J]. Gems&Gemology,2014,50(2):152.
[4] Moe K J,Johnson P,D’Haenens-Johansson U,et al.A synthetic diamond overgrowth on a natural diamond[J]. Gems&Gemology,2017,53(2):237-239.
[5] Serov R,Shelementiev Y,Serova A. Hybrid Diamonds:Natural Diamonds Overgrown with CVD Synthetic[C]//The Proceedings of 35th International Geological Congress. 2017:51-53.
[6] Christopher M,Breeding,Shigley J E. The‘type’classification system of diamonds and its importance in gemology[J]. Gems&Gemology,2009,45(2):96-111.
[7]宋中华,陆太进,苏隽,等.无色-近无色高温高压合成钻石的谱图特征及其鉴别方法[J].岩矿测试,2016,35(5):496-504.Song Z H,Lu T J,Su J,et al. The spectral characteristics and identification techniques forcolorless and nearcolorless HPHT synthetic diamonds[J]. Rock and Mineral Analysis,2016,35(5):496-504.
[8] Wang W,Johnson P,Moe K S,et al. CVD synthetic diamonds from gemesis corp[J]. Gems&Gemology,2012,48(2):80-97.
[9] Moses T M,Reinitz I M,Johnson M L,et al. A contribution to understanding the effect of blue fluorescence on the appearance of diamonds[J]. Gems&Gemology,1997,33(4):244-259.
[10] Shigley J E,Breeding C M. Optical defects in diamond:A quick reference chart[J]. Gems&Gemology,2013,49(2):107-111.
[11] Tang S,Su J,Lu T J,et al. A melee-size CVD synthetic diamond in pearl and diamond jewelry[J]. Gems&Gemology,2017,53(3):382.
[12] Wang W,Moses T,Linares R,et al. Gem-quality synthetic diamonds grown by the chemical vapor deposition method[J]. Gems&Gemology,2003,39(4):268-283.
[13] Eaton-Magana S,Shigley J E. Observations on CVDgrown synthetic diamonds:A review[J]. Gems&Gemology,2016,52(3):222.
[14]宋中华,兰延,沈美冬,等. NGTC实验室发现未揭示的CVD合成钻石鉴定特征研究[J].宝石和宝石学杂志,2012,14(4):30-34.Song Z H,Lan Y,Shen M D,et al. Identification characteristics of undisclosed CVD synthetic diamonds found recently by NGTC[J]. Journal of Gems and Gemmology,2012,14(4):30-34.
[15] Collins A T. Colour centers in diamond[J]. Journal of Gemmology,1982,18:35-75.
[16] Collins A T. The colour of diamond and how it may be changed[J]. Journal of Gemmology,2001,27:341-359.
[17] Collins A T,Stanley M,Woods G S. Nitrogen isotope effects in synthetic diamonds[J]. Journal of Physics D:Applied Physics,1987,20(7):969-974.
[18] Collins A T. Intrinsic and extrinsic absorption and luminescence in diamond[J]. Physica B:Condensed Matter,1993,185(1-4):284-296.
[19] Collins A T,Kanda H,Burns R C. The segregation of nickel-related optical centers in the octahedral growth sectors of synthetic diamond[J]. Philosophical Magazine B,1990,61(5):797-810.
[20] Tang S,Song Z H,Lu T J,et al. Two natural type IIa diamonds with strong phosphorescence and Ni-related defects[J]. Gems&Gemology,2017,53(4):476-478.
[21] Song Z H,Lan Y,Shen M D,et al. Identification characteristics of undisclosed CVD synthetic diamonds found recently by NGTC[J]. Journal of Gems and Gemmology,2012,14(4):30-34.
[22]宋中华,魏华,田晶.钻石辨假[M].北京:文化出版社,2017.Song Z H,Wei H,Tian J. Identification of Diamonds[M]. Beijing:Cultural Development Press,2017.
[23] Fisher D,Spits R A. Spectroscopic evidence of GE POL HPHT-treated natural type IIa diamonds[J]. Gems&Gemology,2000,36(1):42-49.
[24]宋中华,陆太进,苏隽,等.利用吸收和发光光谱技术分析高温高压天然富氢钻石的鉴定特征[J].岩矿测试,2018,37(1):64-68.Song Z H,Lu T J,Su J,et al. Identification of HPHTtreated hydrogen-rich diamonds by optical absorption and photo luminescence spectroscopy techniques[J].Rock and Mineral Analysis,2018,37(1):64-69.
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