Structural transformation of implanted diamond layers during high temperature annealing

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Abstract

In the recent years graphitization of ion-beam induced amorphous layers became the basic tool for device fabrication in diamond. The etchable graphitic layers can be removed to form free-standing membranes into which the desired structures can be sculpted using FIB milling. The optical properties of the devices fabricated using this method are assumed on the model of sharp diamond–air interface. The real quality of this interface could depend on degree of graphitization of the amorphous damage layers after annealing. In the present work the graphitization process was studied using conventional and analytical TEM. It was found that annealing at 550 °C results in a partial graphitization of the implanted volume with formation of the nano-crystalline graphitic phase sandwiched between layers of tetrahedral amorphous carbon. Annealing at 1400 °C resulted in complete graphitization of the amorphous layers. The average size of graphite nano-crystals did not exceed 5 nm with predominant orientation of c-planes normal to the sample surface.

Introduction

The progress in the fabrication of synthetic diamond has resulted in increasing number of its potential applications. Single crystal diamond has also attracted enormous interest as a solid state platform for quantum information processing. Nitrogen-vacancy (N-V) color centers in diamond show remarkable quantum properties such as long coherence times and single spin readout, and can be used as qubits in a quantum computer architecture [1], [2], [3]. In order to take advantage of these properties, it is highly desirable to fabricate photonic components in diamond at the micro and even nano-scale level. In a previous work we demonstrated the ability of fabricating three-dimensional structures in diamond at the micro-scale level using lift-out method [4]. MeV ion implantation was used to create a buried damage layer which transformed into a graphite-like layer upon high temperature thermal annealing. The graphitic layer can be selectively etched to form a free-standing membrane into which the desired structures can be sculpted using focused ion beam (FIB) milling. Ion implantation with tens of keV ion energy [5] or multiple energy implantation techniques [6] when combined with FIB milling allows device fabrication in diamond at the micro- and nano-scale. The modeling of the optical properties of the devices fabricated using this method [4], [5], [6], [7], [8] are based on the assumption of a sharp diamond–air interface. The real quality of this interface could depend on many factors, for example, on the degree of graphitization of the amorphous damage layers after annealing. Kalish et al. [9] reported complete graphitization of the implanted layer in diamond after a 20 min annealing at 600 °C. However, a recent study [10] using high-resolution electron microscopy (HREM) revealed the presence of a transition area with pockets of crystalline diamond in the graphite matrix near surface, after high temperature vacuum annealing of implanted layer in diamond. Thus, the real quality of the diamond surface after chemical removal of graphitic layer can be far from ideal. In the present work the processes of the ion-beam-induced amorphisation and graphitisation in diamond were studied using cross-sectional conventional and analytical TEM. The graphitisation of the amorphized layers was carried out at annealing temperatures of 550 °C and 1400 °C.

Section snippets

Experimental

Synthetic (0 0 1) diamond samples produced by Sumitomo Inc. were implanted at room temperature with He+ ions to a fluence range of 3 × 1016–10 × 1016 cm−2. The energy of the He+ ions was 0.5 MeV or 2 MeV. The ion implantation with ion energy of 0.5 MeV was performed through a mask, (a copper TEM mesh grid). Thus, the latter sample contains implanted areas separated by unimplanted areas screened during implantation by grid bars. The 0.5 MeV implantation was chosen to create the damage layer in diamond much

Results and discussions

The interaction of the energetic ions with the diamond substrate initiates a sequence of displacement events that leads to the production of lattice defects (vacancies and interstitials) and, at sufficiently high fluences, to the crystalline-to-amorphous (c–a) transformation of the irradiated volume [4], [6]. The amorphous damage layer after 0.5 MeV He+ ion implantation is clearly visible in the bright-field TEM image in Fig. 1a due to absence of the diffraction contrast or long-range order in

Conclusions

High-fluence MeV He+ ion implantation in diamond results in the formation of a large number of lattice defects with corresponding distortion of the diamond lattice and formation of the buried amorphous layer. The thermal annealing at moderate temperature (550 °C) resulted in a partial graphitization of the implanted volume and in the formation of the nano-crystalline graphitic phase which is sandwiched between layers of tetrahedral amorphous carbon. Selected area diffraction and dark field

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