litosphereЛитосфераLITHOSPHERE (Russia)1681-90042500-302XA.N. Zavaritsky Institute of Geology and Geochemistry10.24930/1681-9004-2024-24-2-347-363litosphere-2067Research ArticleСтатьиArticlesОпределение внутренней структурной неоднородности природного алмаза: методические аспекты использования конфокальной спектроскопии комбинационного рассеяния света с анализом поляризацииDetermination of the internal structural heterogeneity of natural diamond: Methodological aspects of using confocal Raman spectroscopy with polarization analysisБогдановаЛ. И.BogdanovaL. I.

620110, г. Екатеринбург, ул. Академика Вонсовского, 15

Louisa I. Bogdanova

15 Academician Vonsovsky st., Ekaterinburg 620110

bogdanovalouisa@gmail.comЩаповаЮ. В.ShchapovaYu. V.

620110, г. Екатеринбург, ул. Академика Вонсовского, 15

Yuliya V. Shchapova

15 Academician Vonsovsky st., Ekaterinburg 620110

СушанекЛ. Я.SushanekL. Y.

620110, г. Екатеринбург, ул. Академика Вонсовского, 15

Lev Y. Sushanek

15 Academician Vonsovsky st., Ekaterinburg 620110

ВасильевЕ. А.VasilievE. A.

199106, г. Санкт-Петербург, Васильевский остров, 21 линия, 2

Evgenii A. Vasiliev

2 21st Line, Vasilyevsky Island, Saint Petersburg 199106

 

ВотяковС. Л.VotyakovS. L.

620110, г. Екатеринбург, ул. Академика Вонсовского, 15

Sergey L. Votyakov

15 Academician Vonsovsky st., Ekaterinburg 620110

Институт геологии и геохимии им. академика А.Н. Заварицкого УрО РАНРоссияA.N. Zavaritsky Institute of Geology and Geochemistry, UB RASRussian FederationСанкт-Петербургский горный университет императрицы Екатерины IIРоссияEmpress Catherine II Saint Petersburg Mining UniversityRussian Federation202407052024242347363Copyright © Богданова Л.И., Щапова Ю.В., Сушанек Л.Я., Васильев Е.А., Вотяков С.Л., 20242024Богданова Л.И., Щапова Ю.В., Сушанек Л.Я., Васильев Е.А., Вотяков С.Л.Bogdanova L.I., Shchapova Y.V., Sushanek L.Y., Vasiliev E.A., Votyakov S.L.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.lithosphere.ru/jour/article/view/2067

Цель. В работе представлено описание методических приемов исследования внутренней структурной неоднородности кристаллов природного алмаза, основанных на использовании конфокальной спектроскопии комбинационного рассеяния света с анализом поляризации, в том числе с угловым разрешением, при высоком спектральном (0.5–0.6 см–1) и пространственном (1 мкм) разрешении. Результаты. Параметры колебательной моды F2g в алмазе (положение, ширина, интенсивность, форма, в том числе доля гауссова и лоренцева вкладов в уширение) определяются суперпозиционным влиянием ряда факторов, в числе которых тип и содержание структурных напряжений, деформаций, различных типов дефектов, а также ориентировка кристаллографических осей кристалла относительно направлений падающего и рассеянного лучей и направлений их электрических векторов поляризации. Реализованная аналитическая процедура включает в себя следующее: 1) анализ кристаллографической ориентировки образца в системе координат спектрометра и возможных разориентировок его фрагментов с погрешностью ≈8–15°; 2) визуализацию распределения структурных напряжений, деформаций, двойников, примесных дефектов и их ассоциатов на основе картирования поверхности образцов по спектральным параметрам колебательной моды F2g; 3) получение статистических характеристик внутренней структурной неоднородности образцов на основе диаграмм частоты встречаемости спектральных параметров при их статистически значимом количестве (≈103): унимодальности (уни-, бимодальные распределения), ширины распределений (от ≈0.1 до ≈0.6 см–1 для FWHMcorr и от ≈0.04 до ≈0.6 см–1 для положения линии). Апробация методических приемов выполнена на примере двух синтетических CVD монокристаллов алмаза, допированных азотом и бором; возможность типизации природных образцов по статистическим характеристикам внутренней неоднородности рассмотрена на примере образцов из кимберлитовых трубок Якутии и из россыпей Западного Приуралья. Выводы. Отработан ряд методических приемов определения внутренней структурной неоднородности кристаллов природного алмаза, основанных на конфокальной спектроскопии комбинационного рассеяния света с анализом поляризации, и показана возможность использования статистических характеристик неоднородности в качестве одного из типоморфных признаков коренного источника алмазов; предложенные диаграммы перспективно использовать для сопоставления и типизации образцов.

Aim. To describe a technique for studying the internal structural heterogeneity of natural diamond crystals, based on confocal Raman spectroscopy with polarization analysis, including angular resolution, at high spectral (0.5–0.6 cm–1) and spatial (1 μm) resolution. Results. The parameters of the F2g vibrational mode in diamond (position, width, intensity, shape, including the Gaussian and Lorentzian contributions to the broadening) are determined by the superposition influence of a number of factors, including the type and content of structural stresses, deformations, various types of defects, as well as orientation of crystallographic axes of the crystal relative to the directions of incident and scattered rays and the directions of their electric polarization vectors. The proposed analytical technique includes: (1) analysis of the crystallographic orientation of the sample in the spectrometer coordinate system and possible misorientations of its fragments with an error of ≈8–15°; (2) visualization of the distribution of structural stresses, deformations, twins, impurity defects and their associates based on sample surface mapping by spectral parameters of the F2g vibration mode; (3) obtaining statistical characteristics of the internal structural heterogeneity of the samples based on diagrams of spectral parameter frequency with a statistically significant number (≈103): unimodality (uni-, bimodal distributions) and distribution dispersion (from ≈0.1 to ≈0.6 cm–1 for width and from ≈0.04 to ≈0.6 cm–1 for line position). The procedure was tested using two synthetic CVD diamond single crystals doped with nitrogen and boron. The possibility of typification of natural samples by statistical characteristics of internal heterogeneity is considered using the example of samples from kimberlite pipes of Yakutia and placers of the Western Cis-Urals. Conclusions. A method for determining the internal structural heterogeneity of natural diamond crystals based on confocal Raman spectroscopy with polarization analysis is proposed. The possibility of using statistical characteristics of heterogeneity as a typomorphic feature of the original diamond source is demonstrated. The proposed diagrams are promising for sample comparison and typification.

алмазкомбинационное рассеяние светаспектроскопияструктурная неоднородностьтипоморфизмdiamondRaman spectroscopystructural heterogeneitytypomorphismРабота выполнена в ЦКП “Геоаналитик” ИГГ УрО РАН в рамках государственного задания ИГГ УрО РАН, тема № 123011800012-9 (80%). Образцы для исследования из россыпей Западного Приуралья предоставлены Е.А. Васильевым в рамках выполнения работ по гранту РНФ 21-77-20026 (20%). Авторы благодарны Д.А. Зедгенизову, Н.В. Губанову за предоставление образцов из кимберлитов и И.В. Клепикову за предоставление синтетических образцов. Авторы благодарны Г.Б. Михалевскому за получение катодолюминесцентных изображений образцов и Н.С. Чебыкину за измерение карты обратно-рассеянных электронов одного из кристаллов.The work was carried out using the “Geoanalitik” shared research facilities of the IGG UB RAS within the framework of the State Assignment of the IGG UB RAS No. 123011800012-9 (80%). Diamond samples from Western Ural deposits were provided by E.A. 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