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Identification of dislocations in synthetic Chemically Vapor Deposited diamond single crystals Alexandre Tallaire, Thierry Ouisse, Arthur Lantreibecq, Robin Cours, Marc Legros, Hakima Bensalah, Julien Barjon, Vianney Mille, Ovidiu Brinza, and Jocelyn Achard Cryst. Growth Des., Just Accepted Manuscript • DOI: 10.1021/acs.cgd.6b00053 • Publication Date (Web): 30 Mar 2016 Downloaded from http://pubs.acs.org on April 2, 2016

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Crystal Growth & Design

Identification of dislocations in synthetic Chemically Vapor Deposited diamond single crystals Alexandre Tallaire■*, Thierry Ouisse▲, Arthur Lantreibecq●, Robin Cours●, Marc Legros●, Hakima Bensallah○, Julien Barjon○, Vianney Mille■, Ovidiu Brinza■, Jocelyn Achard■ ■ LSPM-CNRS, Université Paris 13, 99 avenue JB Clément 93430 Villetaneuse, France ▲ LMGP-CNRS, Université Grenoble Alpes, 3 Parvis Louis Néel, 38016 Grenoble Cedex 1, France ● CEMES-CNRS, 29 rue Jeanne Marvig, 31055 Toulouse Cedex, France ○ GEMaC-CNRS, Université de Versailles Saint Quentin en Yvelines, 45 avenue des Etats Unis, 78035 Versailles Cedex, France KEYWORDS:

diamond,

dislocations,

CVD,

transmission

electron

microscopy,

cathodoluminescence, etching, birefringence microscopy

ABSTRACT: High purity chemically vapor deposited (CVD) diamond single crystals are now widely available. However the reduction of dislocations in this material still remains an important challenge that will strongly condition its adoption in areas such as optics, electronics and spintronics where these defects have a disastrous effect on the properties. In this work we report on a methodology that allows a complete identification of the type, density and

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distribution of dislocations in a high-quality CVD single crystal. A good agreement between all characterization techniques was established. When the surface is adequately prepared, a simple plasma etching allows evidencing 2 main dislocation types: 45° mixed and edge, the latter one being dominant with a density of around 4.5×104 cm-2. This investigation paves the way to the development of a quick and simple process to analyze dislocations towards getting a better understanding of their impact on the material properties and eventually elaborate strategies to eliminate them.


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Introduction

In the past decade, strong improvements in the crystalline quality and purity of Chemically Vapor Deposited (CVD) diamond films have been achieved1. Millimeter-thick single crystal CVD plates with an area close to 1 cm² have been demonstrated2 although their availability still remains limited. The high transparency and thermal conductivity of CVD diamond can be exploited into optical and thermal applications in which diamond is used as a transparent active media for lasers3 or as a heat sink for cooling down electronic devices4. Luminescent defects in high isotopic purity diamond such as the Nitrogen-Vacancy (NV) center can also be harnessed as highly sensitive magnetometers5 or as long coherence qubits for quantum information processing6. Besides, single crystal diamond is regarded as the ultimate wide band-gap material for power electronics7. For all these applications, wider availability of large-area high-quality CVD films is highly sought after to unlock the outstanding potential of diamond. As the purity and size of the material have increased, the presence of extended defects has started to focus more attention. The stress induced by dislocations is for example responsible for birefringence, which is of importance when diamond optics are to be developed for Raman lasers8 or X-ray beams9. The presence of dislocations can also affect stress surrounding luminescent defects and induce a widening of the electron spin resonance5 or undesirable background luminescence. Finally, dislocations are responsible for current leakage of high power electronic devices, especially when high current densities and high area contacts are considered10. In particular a certain type of defects is believed to act as a “killer” for those applications11. To achieve an optimal performance it has become urgent to develop strategies aiming at reducing their occurrence.


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Dislocations tend to proceed in a direction parallel to the epitaxial growth direction (commonly ) leading to so-called threading dislocations (TD). Their density in a CVD single crystal can vary from a few 103 cm-2 up to 107 cm-2 depending on the quality of the initial diamond seed and its surface, as well as the chosen growth conditions12-13. It has been shown experimentally and theoretically that TDs in CVD-grown diamond generally lie in the {100} slip system while {111} would be the expected gliding plane. Screw, 60°, 45° mixed and edge dislocations have all been observed14-15 or theoretically modeled16-17 in diamond. However, the last two types are believed to be dominant in CVD-grown diamond18. Analyzing and identifying dislocations in diamond remains a difficult but necessary task. Different characterization techniques provide complementary information at scales spanning from millimeters down to nanometers. Dislocations can be revealed by plasma etching19-20, or the stress that surrounds them can be imaged in a birefringence microscope21-22. Low temperature cathodoluminescence (CL) can also allow visualizing dislocations since they behave as efficient recombination centers for free excitons23. Other heavier techniques can allow a direct identification of the type and Burgers vector of dislocations such as X-ray topography with a synchrotron beam (XRT)24-25 or Transmission Electron Microscopy (TEM)26. However they rely on bulky equipments and cannot be carried out in a systematic fashion. Although a few very recent studies that aim at visualizing dislocations in diamond by etching have been published27-28, we propose here to combine plasma etching with birefringence imaging, CL and TEM. We eventually demonstrate a complete identification of dislocation type, direction and density without having to rely on more complicated techniques by establishing an unambiguous correlation between etch-pit and dislocation type. Bringing together those techniques to assess TDs in diamond, remains quite challenging, but the converging results


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demonstrated here break ground to a possible simple and precise way to count and sort dislocations in synthetic CVD diamonds. Experimental methods The procedure used to study dislocations in CVD diamond is summarized in Fig. 1. Each processing step (S1 to S7) and characterization conditions are further detailed in the additional supporting information section provided as a separate file. Briefly, a thick film is homoepitaxially grown by plasma assisted CVD (S1) before being detached from its substrate and polished into a 4×4×0.4 mm3 freestanding plate (S2). The polished surface was then uniformly etched by ICP (Inductively Coupled Plasma). This step was found to be crucial to assess the correct value of the TD content in the bulk crystal. It removes the subsurface damage and therefore avoids the appearance of etch-pits developed from polishing-related defects after the plasma reveal step (S4)28. To facilitate the spatial localization of dislocations, a tungsten grid that consists of an array of 250×250 µm² squares was deposited on the surface by lithography and sputtering (S3). Different characterizations techniques were then successively carried out and the results confronted to each other. The sample was first observed under crossed polarizers to assess its birefringence (Fig. 1d). It was then etched using a H2/O2 (98/2) plasma for 10 minutes (S4) in order to reveal dislocations in the form of inverted pyramidal shape etch-pits (EP). A full map of EP size and distribution could be established by acquiring 3D images with a laser microscope (Fig. 1e). By using a Focused Ion Beam (FIB), lamellae were then prepared and thinned down around selected EP (S5) and later observed by TEM (Fig. 1f). It should be noted that prior to FIB preparation, a further 10 min H2/O2 plasma etching step was performed in order to increase the size of EPs to be cut. Eventually the sample was re-polished and ICP etched in order to remove


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EP and residual damage (S6). CL images were finally acquired at a wavelength of 235 nm and a temperature of 80 K on selected regions (Fig. 1g). For the sake of clarity, results of the different characterization techniques are compared and discussed in the following part without necessarily following the chronological order with which they were carried out.

Figure 1. Procedure used to study dislocations in a synthetic CVD plate. Results and discussion At first we consider surface observation after H2/O2 plasma etching before confronting the results to those obtained with other characterization techniques. The produced EPs were found to be isolated with no groups aligned along grooves or polishing lines. This indicates that the ICP etching treatment performed after polishing was successful in removing subsurface damage. In fact previous experiments performed without this step could not lead to any correspondence between EP and birefringence patterns (see figure 3 in the separate supporting information file). The laser microscopy measurements revealed two main families of inverted pyramidal EPs: large ones (L) and small ones (S) as illustrated in Fig. 2a. Large EPs with a width of 8-10 µm appear


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dark on the image (dashed blue circle). They exhibit a rather octagonal shape (Fig. 2b) and are distributed with a low density on the sample of around 1×103 cm-2. On the other hand, small EPs have a square shape and are found with a density of about 5×104 cm-2. This value is a reasonably good estimate of the dislocation density usually measured for good quality CVD diamond films. Interestingly, while the vast majority of small EPs have a depth in the range 0.5-1 µm (shallow type Ss, green, Fig. 2d), a smaller number shows a slightly larger width and are clearly much deeper (1.5-1.8µm) (deep type Sd, red circle, Fig. 2c) even though this is not immediately evident from the image. This is highlighted in the statistical distribution of around 100 different small EPs in 36 square areas of the grid and plotted in Fig. 2e and 2f. The 2 main populations are clearly distinguished especially when comparing their depth.

Figure 2. Laser microscope observation of the CVD diamond surface after H2/O2 plasma etching (a). Three different EP types are evidenced: (b) large (L), (c) small-deep (Sd) and (d) small-


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shallow (Ss). The width and depth distribution for around 100 small EPs is also given in the graphs (e) and (f). In an attempt to establish a correspondence between EPs and defect type, images of the different square areas of the grid after etching were confronted to the birefringence microscopy images acquired before etching. The results are presented in Fig. 3 for a region containing only small EPs where Sd are circled in red. It is striking that a perfect match between the features labeled D1 to D9 and 4D’s and the EPs could be made. There were no unassigned small EPs or birefringent patterns. For better clarity each single birefringence pattern is shown with a suited contrast in the insets of Fig. 3. The proximity of other dislocations and the long-range residualstress in the CVD plate make it difficult to identify with certainty all dislocations and their Burgers vector using this technique21. However, the amplitude of the stress field is in good agreement with single dislocations having unitary burger vectors. While small EPs (Ss and Sd) gave rise to a similar birefringence pattern, large EPs (L, not visible in this figure) did not lead to any contrast at all. This suggests that either they are not related to an extended defect or that the Burgers vector of their dislocation is perpendicular to the (001) plane (screw dislocation) making them invisible in birefringence. The birefringence technique is thus a simple way to accurately assess the real dislocation density in a CVD diamond crystal providing a freestanding plate can be observed in transmission. However the high dislocation density and large background stress complicate the identification of the dislocation type and does not allow differentiating between extended defects leading to shallow and deep EPs.


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Figure 3. Comparison of an area of the CVD plate after etching (top/grey color) and birefringence image before etching (bottom). Etch-pits of the Ss-type and Sd-type (red circle) are labeled D1 to D9. Four dislocations of the Ss type that cannot be resolved individually are also black circled as 4D’s. The insets show each birefringence pattern with an optimized contrast. To establish a correspondence between EP and defect type, images of the different square areas of the grid after etching were also confronted to CL images acquired at 235 nm after repolishing the surface. The optical, SEM and CL images are shown in Fig. 4a-c for 2 different regions. A perfect match was again found between EPs and the dark spots visible in CL images at 235 nm: 100% of 160 Ss EPs were associated to a CL black dot. Reciprocally, we could not


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detect any dark spot which were not associated with an etch-pit. This confirms that dislocations are efficient recombination centers for free excitons. As illustrated in Fig. 4c, it is not possible to distinguish between Ss and Sd EP type from the CL contrast, both leading to an almost similar dark spot. However, CL images of exciton recombination appear as a promising and nondestructive method to count unitary dislocations emerging at the surface just after diamond growth, i.e. without the need of preparing a polished freestanding CVD plate (birefringence), neither etching the diamond, nor extracting a thin lamellae (TEM).

Figure 4. (a) Laser microscope images of two regions (A and B) showing both Ss and Sd EPs (circled in red). (b) SEM images of the same regions after polishing and ICP etching. (c) CL images at 235 nm recorded simultaneously with SEM images. The dislocation lines emerging at the surface produce dark spots in the CL images.


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In order to unambiguously identify the type of dislocation involved in the different EPs, we eventually turned to TEM analysis on a selected number of EPs. Fig. 5a-c illustrates the procedure used to isolate 3 Sd EPs in a thin FIB lamella. Several lamellae were cut around large EPs but they failed to reveal the presence of a dislocation line (Fig. 5d) which is in agreement with the absence of visible birefringence previously described. This suggests that this type of EP may not be dislocation-related. Instead they could originate from inclusions that are common defects in CVD diamond. This is supported by the fact that a flat pit is found at the bottom of the lamella in Fig. 5d. Another possibility is an artifact during H2/O2 plasma etching. In fact the presence of foreign metallic or inorganic particles at the surface of the sample could locally enhance the diamond etching rate leading to the appearance of these deep features. A similar process with Ni or Co particles was intentionally developed recently29. On the other hand all lamellae prepared around Sd or Ss EPs led to the appearance of a clear contrast corresponding to a threading dislocation line along the direction. From the invisibility criterion obtained by tilting the sample, the Burgers vector could be determined for all Sd and Ss EPs. It was found to lie along the and directions, corresponding to 45° mixed and edge dislocations respectively (Fig. 5e and 5f). Therefore although TEM is a rather heavy technique that cannot be carried out in a systematic fashion, it allowed clearly identifying the different EP types and can be correlated with previous characterizations. The results obtained are summarized in Tab. 1.


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Figure 5. (a-c) FIB preparation of a thin lamella containing 3 aligned type Sd EPs. TEM observation and identification of (d) type L EP: no dislocation, (e) type Sd EP: 45° mixed dislocation and (f) type Ss: edge dislocation. The diffraction vector (g), burgers vector (b) and line direction (L) are indicated on the images. Etchpits

Description Large/

Type L

deep

Type

Small/

Sd

deep Small/

Type Ss

shallow

Width

Depth

Density -2

Proportion

Birefrin-

CL

Dislocation

(µm)

(µm)

(cm )

(%)

gence

in TEM

8-10

3-5

1×103

2

No

n.m.

No

3-4

1.5-2

2×103

4

Yes

Dark spot

45° mixed

2-3

0.5-1

4.5×104

94

Yes

Dark spot

Edge

Table 1. Summary of the results obtained with the different characterization techniques indicating the correspondence between EPs and dislocation type as well as the overall density. (n.m. not measured) Conclusion


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In summary, a high-quality CVD synthetic diamond plate was characterized with a set of complimentary techniques in order to investigate the nature and density of dislocations that it contains. Thanks to an adapted ICP etching treatment of the surface, the correct content of bulk extended defects can be assessed without any overlap with features originating from subsurface polishing damage. An almost perfect correlation was found between birefringence, CL and etching. Indeed, all cross-shape patterns in birefringence and dark spots in CL were assigned to etch-pits although it was not possible to clearly distinguish between different dislocation types using these techniques. Plasma etching has revealed 3 different etch-pits: large, small-deep and small-shallow. The latter type represented around 94 % of the total amount of EPs. These were subsequently assigned to 45° mixed and edge threading dislocations respectively with a line (i.e. along the growth direction) by TEM. This is consistent with other reports in which these 2 types of dislocations were found to be dominating in CVD films15,18. Interestingly, the largest EPs did not lead to any birefringence contrast and were not assigned to a dislocation in TEM. This indicates that they are probably either due to an artifact during etching or to localized defects such as inclusions but most likely not a dislocation. Further analysis is needed though to fully determine their origin. This investigation paves the way to the development of a quick and simple process to determine the nature, density and spatial distribution of dislocations in CVD synthetic films. A simple plasma etching followed by microscope observation appears as a powerful technique. The correspondence between etch-pit shape and density with the dislocations observed in TEM indicates that etching can be used without the need to rely on heavy equipment. Since these defects constitute one of the main issues towards developing efficient electronic and optic


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components based on this material, the method presented here could accelerate the characterization and counting of threading dislocations in artificial diamonds, helping finding processing routes to bypass or eliminate them.

Acknowledgements C. Vilar is acknowledged for help with the SEM/CL measurements at GEMaC. Supporting Information Description Full experimental details for substrate fabrication and preparation including UV images of the diamond plates Description of the characterization techniques and conditions used for etching, birefringence, TEM and CL An illustration of the birefringence set-up Comparison of etching and birefringence when no ICP step is used This material is available free of charge via the Internet at http://pubs.acs.org. AUTHOR INFORMATION Corresponding Author * [email protected] Author Contributions The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript.


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Funding Sources This work was financially supported by French ANR projects: CROISADD (No. ANR-11ASTR-020), HIRIS (No. ANR-12-BS09-0001) and MONODIAM-HE (No. ANR-12-BS050014) as well as the French National Research Agency under the "Investissement d'Avenir" program reference No. ANR-10-EQPX-38-01 – MIMETIS. REFERENCES (1) Tallaire, A.; Achard, J.; Silva, F.; Brinza, O.; Gicquel, A., Comptes Rendus Physique 2013, 14, 169-184. (2) Yamada, H.; Chayahara, A.; Mokuno, Y.; Umezawa, H.; Shikata, S.-i.; Fujimori, N., Applied Physics Express 2010, 3 (5), 051301. (3) Reilly, S.; Savitski, V. G.; Liu, H.; Gu, E.; Dawson, M. D.; Kemp, A. J., Optics Letters 2015, 40, (6), 930-933. (4) Trejo, M.; Jessen, G. H.; Chabak, K. D.; Gillespie, J. K.; Crespo, A.; Kossler, M.; Trimble, V.; Langley, D.; Heller, E. R.; Claflin, B.; Walker, D. E.; Poling, B.; Gilbert, R.; Via, G. D.; Hoelscher, J.; Roussos, J.; Ejeckam, F.; Zimmer, J., physica status solidi (a) 2010, 208, 439-444. (5) Rondin, L.; Tetienne, J.-P.; Hingant, T.; Roch, J.-F.; Maletinsky, P.; Jacques, V., Reports on Progress in Physics 2014, 77, (5), 056503. (6) Wrachtrup, J.; Jelezko, F., Journal of Physics: Condensed Matter 2006, 18, (21), S807. (7) Umezawa, H.; Nagase, M.; Kato, Y.; Shikata, S., Diamond and Related Materials 2012, 24, (0), 201-205.


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(18) Martineau, P.; Gaukroger, M.; Khan, R.; Evans, D., Physica Status Solidi C 2009, 6, (8), 1953-1957. (19) Khokhryakov, A. F.; Palyanov, Y. N., Journal of Crystal Growth 2006, 293, (2), 469-474. (20) Achard, J.; Silva, F.; Brinza, O.; Bonnin, X.; Mille, V.; Issaoui, R.; Kasu, M.; Gicquel, A., physica status solidi (a) 2009, 206, (9), 1949-1954. (21) Pinto, H.; Jones, R., Journal of Physics: Condensed Matter 2009, 21, (36), 364220. (22) Le, H. T. M.; Ouisse, T.; Chaussende, D.; Naamoun, M.; Tallaire, A.; Achard, J., Crystal Growth & Design 2014, 14, 5761-5766. (23) Tallaire, A.; Barjon, J.; Brinza, O.; Achard, J.; Silva, F.; Mille, V.; Issaoui, R.; Tardieu, A.; Gicquel, A., Diamond and Related Materials 2011, 20, (7), 875-881. (24) Kato, Y.; Umezawa, H.; Yamaguchi, H.; Shikata, S., Japanese Journal of Applied Physics 2012, 51, 090103. (25) Burns, R. C.; Chumakov, A. I.; Connell, S. H.; Dube, D.; Godfried, H. P.; Hansen, J. O.; Hartwig, J.; Hoszowska, J.; Masiello, F.; Mkhonza, L.; Rebak, M.; Rommevaux, A.; Setshedi, R.; Vaerenbergh, P. V., Journal of Physics: Condensed Matter 2009, 21, (36), 364224. (26) Araújo, D.; Alegre, M. P.; García, A. J.; Navas, J.; Villar, M. P.; Bustarret, E.; Volpe, P. N.; Omnès, F., Diamond and Related Materials 2011, 20, (3), 428-432. (27) Ichikawa, K.; Kodama, H.; Suzuki, K.; Sawabe, A., Thin Solid Films 2016, 600, 142-145. (28) Tsubouchi, N.; Mokuno, Y.; Shikata, S., Diam. & Relat. Mat. 2015, In press


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Table of content/Synopsis

Identification of dislocations in synthetic Chemically Vapor Deposited diamond single crystals A. Tallaire, T. Ouisse, A. Lantreibecq, R. Cours, M. Legros, H. Bensallah, J. Barjon, V. Mille, O. Brinza, J. Achard

Threading dislocations in CVD diamond were investigated by etching, CL, birefringence and TEM. All results were consistent and allowed assessing dislocation density, distribution and type. Shallow and deep etch-pits were found to be associated with edge and 45° mixed dislocations respectively with densities of 4.5×104 and 2×103 cm-2 indicating that this technique can be quickly carried out to reveal dislocation content without the need to rely on heavier techniques.

For table of contents use only


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Figure 1 252x138mm (96 x 96 DPI)


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254x190mm (96 x 96 DPI)



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254x190mm (96 x 96 DPI)


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1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


254x190mm (96 x 96 DPI)



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Figure 5 247x143mm (96 x 96 DPI)


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Identification of Dislocations in Synthetic ... - ACS Publications

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