Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment

Deuterium is accumulated by defects in nitrogen-implanted silicon (Si:N). This effect is investigated for Si:N processed at HT ≤ 1400 K, also under enhanced hydrostatic pressure, HP ≤ 1.1 GPa. Si:N was prepared from Czochralski grown silicon by N₂⁺ implantation at E = 140 keV with nitrogen doses, DN...

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Datum:	2010
Hauptverfasser:	Misiuk, A., Barcz, A., Ulyashin, A., Prujszczyk, M., Bak-Misiuk, J., Formanek, P.
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Veröffentlicht:	Донецький фізико-технічний інститут ім. О.О. Галкіна НАН України 2010
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spelling	irk-123456789-693282014-10-12T03:01:45Z Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment Misiuk, A. Barcz, A. Ulyashin, A. Prujszczyk, M. Bak-Misiuk, J. Formanek, P. Deuterium is accumulated by defects in nitrogen-implanted silicon (Si:N). This effect is investigated for Si:N processed at HT ≤ 1400 K, also under enhanced hydrostatic pressure, HP ≤ 1.1 GPa. Si:N was prepared from Czochralski grown silicon by N₂⁺ implantation at E = 140 keV with nitrogen doses, DN = 1–1.8•10¹⁸ cm⁻². Si:N was subsequently processed in RF deuterium plasma to prepare Si:N,D. Si:N and Si:N,D were investigated by Transmission Electron Microscopy (TEM), X-ray and Secondary Ion Mass Spec- trometry (SIMS) methods, also after additional annealing at 723 K. In heavily implanted Si:N (DN = 1.8•1010¹⁸ cm⁻²), plasma treatment leads to deuterium pile up to сD1 = 2•10²¹ cm⁻³ at a depth, d = 50 nm, while, at d = 80–250 nm, deuterium concentration is practically constant with сD2 = 1•10²¹ cm⁻³. This suggests dominating accumulation of deuterium within the bubble-containing areas. Determination of deuterium depth profiles in Si:N,D can reveal implantation- and processing-induced defects. В работе рассмотрены эффекты влияния обработки температурным отжигом (до 1400 K) и гидростатическим давлением (до 1.1 GPa) на дефектный состав SOI-структур (silicon-on-insulator) на основе образцов Si:N – материала, широко используемого в полупроводниковых технологиях. Были получены новые данные, свидетельствующие об образовании скрытых дефектосодержащих слоев в образцах кремния, имплантированного азотом, и подвергнутых обработке высокими температурами и давлениями. Такие структуры становятся центрами абсорбции дейтерия из плазмы – его накопление и распределение внутри образца зависят от микроструктуры материала. Таким образом, показано, что обработка в дейтериевой плазме с дальнейшим определением концентрационных профилей по глубине образца может быть полезной для оценки микроструктуры У роботі розглянуто ефекти впливу обробки температурним відпалом (до 1400 K) і гідростатичним тиском (до 1.1 GPa) на дефектний склад SOI-структур (silicon-oninsulator) на основі зразків Si:N – матеріалу, широко використовуваного в напівпровідникових технологіях. Було отримано нові дані, що свідчать про утворення прихованих дефектовміщуючих шарів в зразках кремнію, імплантованого азотом, підданих обробці високими температурами та тиском. Такі структури стають центрами абсорбції дейтерію з плазми – його накопичення і розподіл усередині зразка залежать від мікроструктури матеріалу. Таким чином, показано, що обробка в дейтерієвій плазмі з подальшим визначенням концентраційних профілів по глибині зразка може бути корисною для оцінки мікроструктури Si:N-зразка, особливо зважаючи на потенційну застосовність в SOI-технологіях. 2010 Article Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment / A. Misiuk, A. Barcz, A. Ulyashin, M. Prujszczyk, J. Bak-Misiuk, P. Formanek // Физика и техника высоких давлений. — 2010. — Т. 20, № 4. — С. 53-59. — Бібліогр.: 4 назв. — рос. 0868-5924 PACS: 61.05.pp, 61.43.Gt, 61.72.–y, 62.50.+p, 68.37.Og http://dspace.nbuv.gov.ua/handle/123456789/69328 en Физика и техника высоких давлений Донецький фізико-технічний інститут ім. О.О. Галкіна НАН України
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language	English
description	Deuterium is accumulated by defects in nitrogen-implanted silicon (Si:N). This effect is investigated for Si:N processed at HT ≤ 1400 K, also under enhanced hydrostatic pressure, HP ≤ 1.1 GPa. Si:N was prepared from Czochralski grown silicon by N₂⁺ implantation at E = 140 keV with nitrogen doses, DN = 1–1.8•10¹⁸ cm⁻². Si:N was subsequently processed in RF deuterium plasma to prepare Si:N,D. Si:N and Si:N,D were investigated by Transmission Electron Microscopy (TEM), X-ray and Secondary Ion Mass Spec- trometry (SIMS) methods, also after additional annealing at 723 K. In heavily implanted Si:N (DN = 1.8•1010¹⁸ cm⁻²), plasma treatment leads to deuterium pile up to сD1 = 2•10²¹ cm⁻³ at a depth, d = 50 nm, while, at d = 80–250 nm, deuterium concentration is practically constant with сD2 = 1•10²¹ cm⁻³. This suggests dominating accumulation of deuterium within the bubble-containing areas. Determination of deuterium depth profiles in Si:N,D can reveal implantation- and processing-induced defects.
format	Article
author	Misiuk, A. Barcz, A. Ulyashin, A. Prujszczyk, M. Bak-Misiuk, J. Formanek, P.
spellingShingle	Misiuk, A. Barcz, A. Ulyashin, A. Prujszczyk, M. Bak-Misiuk, J. Formanek, P. Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment Физика и техника высоких давлений
author_facet	Misiuk, A. Barcz, A. Ulyashin, A. Prujszczyk, M. Bak-Misiuk, J. Formanek, P.
author_sort	Misiuk, A.
title	Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment
title_short	Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment
title_full	Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment
title_fullStr	Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment
title_full_unstemmed	Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment
title_sort	defects in high temperature and high pressure processed si:n revealed by deuterium plasma treatment
publisher	Донецький фізико-технічний інститут ім. О.О. Галкіна НАН України
publishDate	2010
url	http://dspace.nbuv.gov.ua/handle/123456789/69328
citation_txt	Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment / A. Misiuk, A. Barcz, A. Ulyashin, M. Prujszczyk, J. Bak-Misiuk, P. Formanek // Физика и техника высоких давлений. — 2010. — Т. 20, № 4. — С. 53-59. — Бібліогр.: 4 назв. — рос.
series	Физика и техника высоких давлений
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fulltext	Физика и техника высоких давлений 2010, том 20, № 4 © A. Misiuk, A. Barcz,, A. Ulyashin, M. Prujszczyk, J. Bak-Misiuk, P. Formanek, 2010 PACS: 61.05.pp, 61.43.Gt, 61.72.–y, 62.50.+p, 68.37.Og A. Misiuk1, A. Barcz1,2, A. Ulyashin3, M. Prujszczyk1, J. Bak-Misiuk2, P. Formanek4 DEFECTS IN HIGH TEMPERATURE AND HIGH PRESSURE PROCESSED Si:N REVEALED BY DEUTERIUM PLASMA TREATMENT 1Institute of Electron Technology Al. Lotnikow 46, 02-668 Warsaw, Poland E-mail: misiuk@ite.waw.pl 2Institute of Physics, PAS Al. Lotnikow 32/46, 02-668 Warsaw, Poland 3SINTEF, P.O. Box 124 Blindern NO-0314 Oslo, Norway 4Technical University Dresden, Institut fűr Strukturphysik, 010602 Dresden, Germany Deuterium is accumulated by defects in nitrogen-implanted silicon (Si:N). This effect is investigated for Si:N processed at HT ≤ 1400 K, also under enhanced hydrostatic pres- sure, HP ≤ 1.1 GPa. Si:N was prepared from Czochralski grown silicon by N2 + implan- tation at E = 140 keV with nitrogen doses, DN = 1–1.8·1018 cm–2. Si:N was subsequently processed in RF deuterium plasma to prepare Si:N,D. Si:N and Si:N,D were investigated by Transmission Electron Microscopy (TEM), X-ray and Secondary Ion Mass Spec- trometry (SIMS) methods, also after additional annealing at 723 K. In heavily implanted Si:N (DN = 1.8·1018 cm–2), plasma treatment leads to deuterium pile up to сD1 = 2·1021 cm–3 at a depth, d = 50 nm, while, at d = 80–250 nm, deuterium concentration is practically constant with сD2 = 1·1021 cm-3. This suggests dominating accumulation of deuterium within the bubble-containing areas. Determination of deuterium depth profiles in Si:N,D can reveal implantation- and processing-induced defects. Keywords: Cz–Si, implantation, nitrogen, high temperature, high pressure, deuterium plasma, defect, gettering Introduction Silicon-on-insulator structures (SOI) prepared from nitrogen-implanted single crystalline silicon (Si:N) present usually the dislocated SiNx/Si interface and may contain nitrogen-filled bubbles formed within the buried SiNx layer [1]. Enhanced temperature (HT) and hydrostatic pressure (HP) applied at process- ing of Si:N affect its microstructure and can improve quality of the SiNx/Si inter- faces [2]. Физика и техника высоких давлений 2010, том 20, № 4 54 As it has been stated earlier for self-implanted silicon, the buried defect region, cre- ated by implantation, can getter hydrogen in-diffused from hydrogen plasma [3]. This effect is now investigated for the Si:N samples, preliminary processed at HT–HP. Bas- ing on our earlier results, the treatment in deuterium (hydrogen isotope) plasma has been considered as a tool helpful in revealing the defects in such structures. Experimental Details concerning preparation of the Si:N structures are presented in Table. Table Investigated Si:N samples, prepared by N2 + implantation at ≤ 350 K into (001) oriented Czochralski grown silicon (Cz–Si) with interstitial oxygen concentration, c0 = 9·1017 cm–3 Sample Energy E, keV Dose D (calculated for atomic nitrogen), 1018 cm–2 N2 + projected range Rp, nm A 140 1.0 180 B 140 1.8 180 After ion implantation the Si:N samples were processed for 5 h at HT up to 1400 K under hydrostatic Ar pressure HP ≤ 1.1 GPa. Structure of the HT–HP processed Si:N samples was determined by TEM and X-ray methods. To introduce deuterium, the as-implanted and processed Si:N samples were subsequently treated for 2 h at 530 K in RF deuterium plasma in Plasma Enhanced Chemical Vapour Deposition (PECVD) reactor [3]. In what follows, the plasma- treated Si:N samples are labelled as Si:N,D. SIMS was used to determine the nitrogen, deuterium and oxygen depth profiles in Si:N,D. The mentioned depth distributions were also determined after anneal- ing the Si:N,D samples for 1 h at 723 K under 105 Pa. Results and discussion Upon annealing the amorphous (aSi) defect layers produced by implantation of N2 + at D ≥ 1·1018 cm–2 are subjected to Solid Phase Epitaxial Re-growth (SPER). Layers or/and precipitates composed of stoichiometric (Si3N4) or substoichi- ometric (SiNx) nitride were formed within the buried damaged areas (Fig. 1). Annealing under 105 Pa as well as the HT–HP treatment of Si:N at up to 1400 K do not result in complete SPER, so processed Si:N is composed of the areas with different microstructure. As confirmed also by X-ray measurements, nitrogen-filled bubbles are present near Rp after processing ([4], Fig. 1). The plasma treatment leads, first of all, to accumulation of deuterium near the sample surface. In the case of as-implanted BSi:N samples, the near-surface deuterium peak has been detected at a depth, d = 50 nm with cD1 = 2·1021 cm–3, while, at d = 80–250 nm the deute- rium content remains almost constant, with cD2 = 1·1021 cm–3 (compare [2]). Физика и техника высоких давлений 2010, том 20, № 4 55 Processing of ASi:N at 1070 K results in the formation of N-enriched zone near Rp. Interstitial oxygen atoms always present in Cz-Si are also gettered at this defect-containing area. As follows from the oxygen depth profile (Fig. 2), sub- stantial part of oxygen in-diffused from the sample surface covered by thin SiO2 film is produced at the plasma treatment. The strongest deuterium accumulation is observed just within this near-surface area, at about 20 nm depth. Just this area contains numerous defects introduced by plasma etching itself. Processing of ASi:N at 1270 K resulted in the formation of N-enriched plateau at d = 100–300 nm, containing about 20 at.% of nitrogen. This suggests almost uniform distribution of implanted nitrogen, in the form of sub-stoichiometric Si3Nx. Deuterium introduced by the plasma treatment is accumulated mainly at the bottom Si3Nx/Si boundary thus suggesting strong affinity of deuterium just to defects created at this place (Fig. 3). Fig. 2. SIMS depth profiles of nitrogen, oxygen and deuterium in ASi:N,D, prepared from ASi:N (DN = 1018 cm–2) processed for 5 h at 1070 K under 1.1 GPa Fig. 3. SIMS depth profiles of nitrogen and deuterium in ASi:N,D, prepared from ASi:N processed for 5 h at 1270 K under 1.1 GPa Fig. 1. Cross-sectional TEM image of ASi:N processed at 1400 K under 1.1 GPa. Si:N consists of sub-layers of different microstructure. Very top layer is amor- phous with mosaic-like polycrystallites just below it. Big pores (bubbles) are ob- served near Rp. aSi layers containing Si nanocrystallites are visible on both sides 50 nm Физика и техника высоких давлений 2010, том 20, № 4 56 Deuterium accumulation in BSi:N,D is more pronounced than that in ASi:N,D. The deuterium profiles in the near-surface area of BSi:N,D prepared from BSi:N processed at 1270 K are similar to these in BSi:N,D prepared from the as- implanted BSi:N sample but сD2 decreased to 4·1020 and 3·1020 cm–3 after proc- essing under 105 Pa and 1.1 GPa, respectively [2]. The BSi:N,D samples prepared from BSi:N processed at 1400 K indicate a lowered D accumulation. Deuterium concentration exhibits minimum near Rp and the maximum at a d ≈ 250 nm (compare Fig. 4). A lot of deuterium is still retained, especially in the BSi:N,D samples, after their subsequent annealing at 723 K under 105 Pa (Fig. 4). And so the BSi:N,D sample, prepared from as-implanted BSi:N, and annealed at 723 K, still indicates сD1 = 6·1020 cm–3 at d = 50 nm, while, at d = 150 nm, сD2 equals to about 7·1020 cm–3 (Fig. 4). Accumulated deuterium is strongly bonded to defects also in the BSi:N,D samples prepared from Si:N processed at higher temperatures and finally annealed at 723 K (Fig. 5). Fig. 4. SIMS depth profiles of nitrogen, oxygen and deuterium in BSi:N,D, prepared from as-implanted BSi:N (DN = 1.8·1018 cm–2) and finally annealed at 723 K Fig. 5. SIMS depth profiles of nitrogen, oxygen and deuterium in BSi:N,D, prepared from BSi:N processed for 5 h at 1270 K under 105 Pa and finally annealed at 723 K Also the BSi:N,D sample prepared from BSi:N processed for 5 h at 1400 K under 105 Pa, indicated, after annealing at 723 K, high deuterium concentration at the very sample surface (сD ≈ 2·1021 cm–3). At d = 100–200 nm this concentration is equal to about 3·1020 cm–3. As seen in TEM patterns, the very top layer of Si:N is composed of the polycrystalline-like material (compare Fig. 1). In effect of its presence, one can observe sometimes a specific artefact: massive in-diffusion of deuterium as well Физика и техника высоких давлений 2010, том 20, № 4 57 as in-diffusion and re-distribution of other admixing atoms, especially in the case of BSi:N prepared by heavy nitrogen implantation (Fig. 6). In the case of Si:N structures pre- pared by ion implantation, the forma- tion of aSi area takes place near Rp. Most of implanted nitrogen atoms are contained within this area. Upon an- nealing, nitrogen-containing aSi is subjected to SPER. The processed Si:N samples indicate the presence of buried SiNx layer con- taining numerous nitrogen-filled bubbles. The deuterium plasma treatment of Si:N with different microstructure induced by specific HT–HP processing, results in hydrogen accumulation at the surface and within the buried defect layers. Deuterium concentration is the highest at the near-surface areas of the Si:N,D samples, especially in the ones prepared from as-implanted or relatively low- temperature-processed Si:N. This means that plasma deuterization itself intro- duces a lot of defects within the near-surface sample areas. In spite of relatively low temperature (T ≈ 530 K) and short time of plasma treatment (2 h), a remark- able in-diffusion and subsequent gettering of deuterium within the deeper placed damaged layers has been observed. In the case of BSi:N,D, prepared by heavy nitrogen implantation, the deuterium concentration profiles correspond roughly to these of nitrogen, suggesting a spe- cial role of N2-filled bubbles (Fig. 1) in deuterium accumulation. A release of about 50% of deuterium after annealing of Si:N,D (prepared from as-implanted Si:N) at 723 K may suggest some D–N bonding. Enhanced pressure applied during preparation of the Si:N samples affects strongly their microstructure and thus in-diffusion and depth profiles of deuterium after plasma treatment. The deuterium depth distribution depends crucially on the implanted nitrogen dose (Figs 3 and 5). Conclusions New data concerning the formation of buried defect-containing layers in silicon implanted with nitrogen and subjected to the post-implantation high temperature (pressure) processing are reported. Such structures absorb deuterium from deute- rium plasma; the deuterium accumulation and distribution within the samples are dependent on the sample microstructure. Specific character of SPER and of deuterium interaction with defects in as-implan- ted and processed Si:N has been confirmed. Determination of the deuterium depth Fig. 6. SIMS depth profiles of nitrogen, oxygen and deuterium in BSi:N,D, prepared from BSi:N processed for 5 h at 1270 K under 1.1 GPa and finally annealed at 723 K Физика и техника высоких давлений 2010, том 20, № 4 58 profiles in Si:N,D, also subjected to additional anneals, can contribute to revealing the implantation-induced and other structural defects in the SOI-like and similar structures prepared from Si:N. This means that the deuterium plasma treatment with subsequent determination of depth concentration profiles of deuterium may be helpful in evaluating the Si:N sample microstructure, especially in view of potential applicability for SOI tech- nology. 1. I.V. Antonova, A. Misiuk, C.A. Londos, J. Appl. Phys. 99, 033506 (2006). 2. A. Misiuk, A. Ulyashin, A. Barcz, P. Formanek, Solid State Phen. 156-158, 319 (2010). 3. A.G. Ulyashin, J.S. Christinsen, B.G. Svensson, R. Kogler, W. Skorupa, Nucl. In- strum. Meth. Phys. Res. B253, 126 (2006). 4. J. Bak-Misiuk, I.V. Antonova, A. Misiuk, P. Formanek, P. Romanowski, Phys. Status Solidi C6, 1580 (2009). A. Misiuk, A. Barcz, A. Ulyashin, M. Prujszczyk, J. Bak-Misiuk, P. Formanek ДЕФЕКТИ В Si:N, ОБРОБЛЕНОМУ ПРИ ВИСОКИХ ТЕМПЕРАТУРАХ І ТИСКАХ, ЩО ВИЯВЛЯЮТЬСЯ ВНАСЛІДОК ТРАВЛЕННЯ В ДЕЙТЕРІЄВІЙ ПЛАЗМІ У роботі розглянуто ефекти впливу обробки температурним відпалом (до 1400 K) і гідростатичним тиском (до 1.1 GPa) на дефектний склад SOI-структур (silicon-on- insulator) на основі зразків Si:N – матеріалу, широко використовуваного в напівпровідникових технологіях. Було отримано нові дані, що свідчать про утво- рення прихованих дефектовміщуючих шарів в зразках кремнію, імплантованого азотом, підданих обробці високими температурами та тиском. Такі структури ста- ють центрами абсорбції дейтерію з плазми – його накопичення і розподіл усередині зразка залежать від мікроструктури матеріалу. Таким чином, показано, що обробка в дейтерієвій плазмі з подальшим визначенням концентраційних профілів по гли- бині зразка може бути корисною для оцінки мікроструктури Si:N-зразка, особливо зважаючи на потенційну застосовність в SOI-технологіях. Ключові слова: Cz–Si, імплантація, азот, висока температура, високий тиск, дей- терієва плазма, дефект, газопоглинання A. Misiuk, A. Barcz, A. Ulyashin, M. Prujszczyk, J. Bak-Misiuk, P. Formanek ДЕФЕКТЫ В Si:N, ОБРАБОТАННОМ ПРИ ВЫСОКИХ ТЕМПЕРАТУРАХ И ДАВЛЕНИЯХ, ПРОЯВЛЯЮЩИЕСЯ В РЕЗУЛЬТАТЕ ТРАВЛЕНИЯ В ДЕЙТЕРИЕВОЙ ПЛАЗМЕ В работе рассмотрены эффекты влияния обработки температурным отжигом (до 1400 K) и гидростатическим давлением (до 1.1 GPa) на дефектный состав SOI- Физика и техника высоких давлений 2010, том 20, № 4 59 структур (silicon-on-insulator) на основе образцов Si:N – материала, широко исполь- зуемого в полупроводниковых технологиях. Были получены новые данные, свиде- тельствующие об образовании скрытых дефектосодержащих слоев в образцах кремния, имплантированного азотом, и подвергнутых обработке высокими темпе- ратурами и давлениями. Такие структуры становятся центрами абсорбции дейтерия из плазмы – его накопление и распределение внутри образца зависят от микро- структуры материала. Таким образом, показано, что обработка в дейтериевой плаз- ме с дальнейшим определением концентрационных профилей по глубине образца может быть полезной для оценки микроструктуры Si:N-образца, особенно ввиду потенциальной применимости в SOI-технологиях. Ключевые слова: Cz–Si, имплантация, азот, высокая температура, высокое давление, дейтериевая плазма, дефект, газопоглощение

Defects in high temperature and high pressure processed Si:N revealed by deuterium plasma treatment

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