Influence of CVD diamond growth conditions on nitrogen incorporation

Accepted Manuscript Influence of CVD diamond growth conditions on nitrogen incorporation

M.A. Lobaev, A.M. Gorbachev, S.A. Bogdanov, A.L. Vikharev, D.B. Radishev, V.A. Isaev, V.V. Chernov, M.N. Drozdov PII: DOI: Reference:

S0925-9635(16)30590-8 doi: 10.1016/j.diamond.2016.12.011 DIAMAT 6778

To appear in:

Diamond & Related Materials

Received date: Accepted date:

28 October 2016 15 December 2016

Please cite this article as: M.A. Lobaev, A.M. Gorbachev, S.A. Bogdanov, A.L. Vikharev, D.B. Radishev, V.A. Isaev, V.V. Chernov, M.N. Drozdov , Influence of CVD diamond growth conditions on nitrogen incorporation. The address for the corresponding author was captured as affiliation for all authors. Please check if appropriate. Diamat(2016), doi: 10.1016/j.diamond.2016.12.011

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ACCEPTED MANUSCRIPT Influence of CVD diamond growth conditions on nitrogen incorporation M.A. Lobaev1, A.M. Gorbachev1, S.A. Bogdanov1, A.L. Vikharev1, D.B. Radishev1, V.A. Isaev1, V.V. Chernov1, M.N. Drozdov2 1 Institute of Applied Physics RAS, Nizhny Novgorod, Russia 2 Institute for Physics of Microstructures RAS, Nizhny Novgorod, Russia

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Abstract. Nitrogen incorporation during the process of CVD diamond synthesis was studied at different growth conditions: nitrogen flow, substrate temperature, methane content. High nitrogen concentration >1019 cm-3 was obtained using (100)-oriented HPHT substrates. We also demonstrated the growth of the ultra-thin nitrogen doped delta layers with peak nitrogen concentration ~1019 cm-3 and thickness ~ 3 nm. It is shown, that nitrogen delta doping allows the creation of high-density NV-center ensembles with nanometer-precision depth control.

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Keywords: CVD diamond growth, nitrogen incorporation, delta doping

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1. Introduction CVD diamond is regarded as one of the most attractive wide-bandgap material for the next generation of high-power and high-frequency electronic devices, and also have promising applications in biology, quantum information processing and ultrasensitive magnetometry [1]. In comparison with HPHT-grown diamond, CVD diamond layers have much lower impurity content, which is crucial for many up-to-date technological applications, such as high power electronics or quantum information processing. Modern CVD technology allows obtaining epitaxial diamond layers of high crystalline perfection with controlled impurity content. The most frequent and extensively studied impurity in diamond is nitrogen. It is found in natural and HPHT-grown diamond, causing a yellow color in nitrogen-rich samples. CVD growth also easily incorporates nitrogen impurities from the gas phase. Nitrogen impurities are usually found in CVD diamond as substitutional nitrogen, nitrogen-vacancy centers and nitrogen-vacancy-hydrogen defects [2]. Nitrogen additions are often used in CVD diamond growth and are known to increase the growth rate [3-5], thereby reducing production costs and significantly reducing deposition time for such time-consuming applications as diamond windows for high power radiation sources [6, 7]. Also nitrogen doped CVD diamonds with nitrogen vacancy centers (NV-centers) are now considered as the most promising solid-state media for the realization of component base for quantum information processing due to the unique properties of NV-center electronic transitions, which allow initialization and read-out of it`s spin state [8]. Thus, the study of nitrogen impurities in CVD grown diamond is important for many applications and the investigation of nitrogen incorporation dependence on the growth conditions is crucial for further development of CVD technology. In this work, we investigated nitrogen incorporation at different CVD growth conditions. The dependence of nitrogen impurity concentration in the grown diamond layers and diamond growth rate on substrate temperature, methane content and nitrogen amount in the gas phase was extensively studied. Nitrogen impurity content was determined by SIMS method. We investigated the method of controlled creation of NV-centers in diamond using delta-doping, which in contrast to the method of ion implantation does not produce lattice defects and allows controlling the depth of the NV-center to within a few nanometers. CVD method allows producing single-crystal diamond of high crystalline perfection with a low content of impurities that does not vary from sample to sample. Due to the absence of lattice damage, as in the case of ion implantation, NV-centers produced by delta-doping have better spin properties.

2. Experimental

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CVD diamond growth of nitrogen-doped layers was performed in the novel CVD reactor (Figure 1). The main features of the reactor are: 1) rapid gas switching; 2) laminar gas flow; 3) axial symmetric resonant mode – symmetric discharge; 4) slow growth of diamond (40-100 nm/h without nitrogen addition). We achieve rapid gas switching from one input gas to another by a home-made electronic switch. The residence time of our reactor is approximately 5 s. This reactor was initially designed for boron delta doping, and was described in our previous work [9]. The reactor is also capable for the growth of delta-layers doped with any other impurities, such as nitrogen.

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Figure 1. Scheme of the novel 2.45 GHz MPACVD reactor for diamond delta doping: (1) quartz tube; (2) substrate holder; (3) plasma; (4) cylindrical cavity; (5) 2.45 GHz magnetron; (6) rectangular waveguide; (7) gas feeding system, (8) gas pumping system; (9) control system.

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It is well-known, that incorporation of impurities during CVD diamond growth is highly dependent on the substrate orientation, and could also be affected by the misorientation angle. In order to eliminate the influence of substrate, each of the experiment was performed on one sample, varying growth conditions in a one growth process, resulting in the growth of multiple thin nitrogen-doped layers. Our reactor is capable to vary all of the growth conditions separately during a one growth process. For the temperature variation in a one process the substrate heater was used. The growth was performed under the following conditions: pressure 40 Torr, hydrogen flow 950 sccm, methane flow 0.7-1.7 sccm. Nitrogen flow was varied from 1 to 8 sccm. The growth conditions for all samples are summarized in Table 1. Type IIa HPHT diamond (100)-oriented substrates from New Diamond Technologies [10], 3.5×3.5×0.5 mm3, were used for the nitrogen-doped CVD diamond layers growth. The substrates were pre-treated by ICP plasma in order to get rid of the defects introduced during the polishing procedure [11]. ICP etching up to 5 μm depth did not change the surface roughness but allowed to eliminate polishing damages. It should be noted, that similar substrate pretreatment was studied in some previous works [12, 13]. SIMS was used to measure the nitrogen concentration in the grown diamond samples. The time-of-flight secondary ion mass spectrometer TOF.SIMS-5 by ION-TOF (Münster, Germany) was used for the depth profiling and a Talysurf CCI 2000 interferometer was used to measure the depths of the etching craters for normalization of the analysis depth scale. The instrument operates in dual beam mode employing 1 keV Cs+ ions for sputtering and 25 keV Bi+ ions for probing with 45° of incidence for both ion beams. The SIMS nitrogen measurements were quantitatively calibrated using a nitrogen ion-implanted HPHT single crystal “test” diamond, having the implanted nitrogen concentration equal to 1020 сm–3. SIMS profiles were used also for the determination of the growth rate in each of the growth regime.

ACCEPTED MANUSCRIPT Photoluminescence of the grown samples was measured using micro-Raman system with laser excitation wavelength of 514 nm. Measurements were performed at liquid nitrogen temperature.

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Table 1. Growth conditions Sample Hydrogen flow, sccm Sample 1 950

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3. Results and discussion

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3.1 Nitrogen doped delta-layer growth Controllable creation of NV centers during nitrogen doped delta-layer growth is a promising technology for the precise positioning of NV centers with nanometer resolution. In comparison with the creation of NV centers by ion implantation, delta doping does not produce lattice damage and therefore NV center created by delta doping will have longer spin coherence times. The most exciting applications of NV centers require location of a delta-layer within a few nanometers under the surface and also any surface defects could led to the deterioration of NV center properties, therefore the quality of surface preparation become a very important issue in this field. In the experiments on delta-doped growth we paid much attention to substrate polishing and the subsequent ICP treatment, which eliminate polishing damage. All of the prepared surfaces have very low roughness: Ra < 0.3 nm for all samples, while the best prepared samples have Ra ~ 0.1 nm. Figure 2a shows the substrate surface image obtained by the white light interferometer after surface preparation. Figure 2b shows the sample surface after CVD growth (CVD layer thickness ~100 nm).

Figure 2. Data from the interferometer ZYGO NewView 7300: (a) substrate surface after preparation. Ra=0.087 nm; (b) sample surface after CVD diamond growth of 100 nm, Ra=0.160 nm.

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Creation of surface-proximate NV centers with long spin coherence times still remains a challenge. Several groups have used nitrogen delta doping for the creation of near-surface NV center ensembles for ultrasensitive magnetometry applications [14-17]. However, in most of these works (except the work [14]), the real profile of delta layer is not provided, therefore it is not possible to understand what is the real thickness of the delta layer and how sharp the edges are. In a typical MPACVD reactor, even after turning off the N2 input flow, nitrogen remains inside the plasma for a fairly long period of time and keeps incorporating into the diamond surface. Therefore, ultra-thin nitrogen doped layers with sharp interfaces are not easily obtained in a typical reactor. In our novel reactor, rapid gas switching and laminar gas flow are specially designed for the synthesis of ultra-sharp interfaces. For the ability of nanometer-scale depth control it is crucial to know the real profile of nitrogen impurities, as it determines the distribution of NV centers. In our work, we studied the distribution of nitrogen in the delta layer by SIMS. The obtained SIMS profile of the nitrogen-doped delta layer is shown in Figure 3. In the work [14] the SIMS profile of thin nitrogen doped layers was also shown (see Figure S2, supplementary material in online version), demonstrating the peak nitrogen concentration ~ 3·1016 cm-3. In our work, the peak nitrogen concentration of 1.3·1019 cm-3 was obtained (Sample 4). High nitrogen concentration is favorable for the control of sharpness of the interface using SIMS. The width of the SIMS profile, shown in Figure 3 is about 3 nm. The profile of such a thin layer is influenced by a SIMS depth resolution function, which width is about 1 nm.

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Figure 3. SIMS profile of nitrogen doped delta-layer (thickness ~ 3 nm). Sample 4.

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3.2 Nitrogen incorporation efficiency We studied nitrogen incorporation dependence on N2 flow using Sample 1. For this experiment, ultra-thin (1-3 nm) nitrogen doped delta layers were not necessary, since thicker layers provide better accuracy of the growth rate estimate from the SIMS profile. On the other hand, the doped layers should not be too wide in order to be able to do SIMS profiling of the structure with multiple layers. We used nitrogen doped layers with thickness about 60-80 nm. Figure 4 shows the obtained SIMS profile of the Sample 1. Total CVD layer thickness is about 600 nm, showing Ra<0.5 nm.

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Figure 4. SIMS profile of the Sample 1. Four nitrogen doped layers was grown at nitrogen flows 1, 2, 4 and 8 sccm. Methane flow 1.4 sccm.

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All the doped layers were grown in nitrogen-rich growth regime: nitrogen to carbon ratio in the gas phase was higher than unity in this experiment. Nitrogen incorporation efficiency, defined as (N/C)diamond/(N/C)gas could be calculated using our data, presented in Figure 5. In our growth regime, nitrogen incorporation efficiency is equal to 8·10-6. Reported in literature values of nitrogen incorporation efficiency varies in the range 10-4-10-5 [18, 19].

Figure 5. (a) Average nitrogen concentration dependence on nitrogen flow. Methane flow 1.4 sccm. (b) Growth rate dependence on nitrogen flow. Sample 1.

As can be seen from Figure 5, the growth rate is saturated at nitrogen flow higher than 4 sccm, while nitrogen incorporation does not show any evidence of saturation up to 8 sccm N2 flow. It should be noted, that nitrogen concentrations obtained in our experiments are higher, than in most works, done using (100) substrates. For example, in the work [20] the solubility limit of nitrogen for (100)-orientation was determined as 10 ppm (1 ppm = 1.77·1017 cm-3). In our work we have an order higher nitrogen concentrations. However, the growth regime in the work [20] was significantly different in comparison to our growth conditions: the growth rate was about 6 m/h, while our experiments were performed at much slower growth. Another possible explanation of the increased nitrogen incorporation could be the influence of misorientation angle, which was not systematically studied yet.

ACCEPTED MANUSCRIPT There were only few reports in literature on the CVD growth of highly nitrogen-doped diamond layers. In the recent work [21], nitrogen-doped CVD diamond layers with concentration of nitrogen impurities ~1019 cm-3 was achieved, which is similar to the highest nitrogen concentration obtained in our work, however, in contrast to our work, the growth was performed on (111)-oriented substrates, which is known for much easier impurity incorporation. In our work we used only (100) substrates. Highly nitrogen doped diamond layers are desirable for the creation of high-density NV ensembles. In the work [22], highly nitrogen doped HPHT diamond (with nitrogen concentration ~100 ppm) was used for the creation of such ensembles. The results of our work show, that such ensembles could be obtained by CVD growth in nitrogen-rich gas mixtures even on (100)-oriented substrates.

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3.3 Substrate temperature effect on nitrogen incorporation Investigation of substrate temperature influence on nitrogen incorporation was performed using another Sample 2. The methane flow was fixed to 1.4 sccm in this experiment.

Figure 6. (a) Average nitrogen concentration dependence on substrate temperature. Methane flow 1.4 sccm. (b) Growth rate dependence on substrate temperature. Sample 2.

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Figure 6a shows the linear dependence of nitrogen concentration in diamond on the substrate temperature: lower temperatures lead to higher nitrogen incorporation. Nitrogen concentration decreased by approximately a factor of 4 with the increase of substrate temperature from 750 to 900 oC. Figure 6b presents the growth rate dependence on the substrate temperature, showing a maximum at 850 oC. Similar behavior was observed in the recent work [23], studied the dependence of photoluminescense intensity of NV-centers created during the CVD synthesis on substrate temperature. 3.4 Nitrogen incorporation dependence on the methane flow Investigation of nitrogen incorporation on the methane flow was performed using the Sample 3. Nitrogen flow was fixed to 4 sccm in this experiment. The results of this experiment are presented in Figure 7.

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Figure 7. (a) Average nitrogen concentration dependence on the methane flow. Nitrogen flow 4 sccm. (b) Growth rate dependence on the methane content. Sample 3.

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It is interesting to note, that this experiment shows almost no dependence of nitrogen incorporation on the methane content. Although the growth rate is monotonically increased from 0.14 to 0.4 m/h with increasing methane from 0.7 to 1.7 sccm, the rate of nitrogen incorporation also increases, so the resulting nitrogen concentration in diamond depends only on N2 flow.

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3.5 NV center photoluminescence Although we have achieved high nitrogen concentrations in our CVD grown diamond layers, the SIMS measurement can not confirm the existence of NV centers formed during the CVD growth, because SIMS data reflects mainly the substitutional nitrogen. However, it is important to know, do we really have the creation of NV centers in our layers. In order to clarify this question, we investigated the grown samples using photoluminescence spectroscopy. For example, photoluminescence spectrum of the Sample 1 is shown in Figure 8. The photoluminescence of the sample was studied before CVD growth (Figure 8a) and after growth (Figure 8b). The figure shows the absence of NV centers in the HPHT substrate and their appearance after CVD growth, showing both NV0 and NV- photoluminescence. The total thickness of the nitrogen doped region (4 doped layers) is about 300 nm (see Figure 4). The sample has not been irradiated by electron or ion beams for the creation of vacancies, so the Figure 8b demonstrates the photoluminescence of as-grown NV centers.

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Figure 8. Photoluminescence spectrum (77 K) of the Sample 1: (a) before growth; (b) after growth.

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4. Conclusion In this work, we investigated nitrogen incorporation during CVD diamond growth at different growth conditions. The influence of substrate temperature, methane content and nitrogen flow on the nitrogen incorporation was extensively studied. In order to eliminate the influence of substrate, each of the experiment was performed on one sample, varying the growth conditions in the one growth process. The grown nitrogen doped layers were investigated by SIMS and photoluminescence spectroscopy. Nitrogen incorporation efficiency in our growth regime was determined as 8·10-6. Moreover, we succeeded in fabrication of ultra-thin nitrogen doped delta layers with peak nitrogen concentration ~1019 cm-3 and thickness ~ 3 nm. The SIMS profile of such ultra-thin nitrogen doped layer with high peak concentration is demonstrated for the first time. Such ultra-thin nitrogen-doped layers could be used for the creation of high-density NV center ensembles, which are highly desirable for ultra-sensitive magnetometry applications. Due to the absence of lattice damage, as in the case of ion implantation, NV-centers produced by delta-doping are expected to have better spin properties.

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5. Acknowledgements The study was performed by a grant from the Russian Science Foundation (Project № 16-1900163). The authors are grateful to A.V. Kolyadin (New Diamond Technology Ltd., St. Petersburg) for manufacture of HPHT substrates required for the experiments, to M.P. Dukhnovsky (JSC "RPC "Istok" named after Shokin") for assistance in calibration of SIMS measurement. 6. References [1] Ricardo S. Sussman, CVD Diamond for Electronic Devices and Sensors, Wiley, 2009. [2] S. J. Charles, J. E. Butler, B. N. Feygelson, M. E. Newton, D. L. Carroll, J. W. Steeds, H. Darwish, C.-S. Yan, H. K. Mao, and R. J. Hemley, Characterization of nitrogen doped chemical vapor deposited single crystal diamond before and after high pressure, high temperature annealing, Phys. Status Solidi A 201(11), (2004), 2473–2485. [3] W. Muller-Sebert, E. Worner, F. Fuchs, C. Wild, P. Koidl, Nitrogen induced increase of growth rate in chemical vapor deposition of diamond, Appl. Phys. Lett. 68, (1996), 759-760. [4] A. Chayahara, Y. Mokuno, Y. Horino, Y. Takasu, H. Kato, H. Yoshikawa, N. Fujimori, The effect of nitrogen addition during high-rate homoepitaxial growth of diamond by microwave plasma CVD, Diam. Relat. Mater. 13, (2004), 1954-1958.

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Novelty Influence of CVD diamond growth conditions on nitrogen incorporation and demonstration of 3 nm thick delta layer with nitrogen concentration ~ 1019 cm-3 on (100)-oriented HPHT substrate.

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Graphical abstract

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Nitrogen incorporation dependence on CVD growth conditions was investigated. High nitrogen concentration >1019 cm-3 was achieved on (100) HPHT substrates. Nitrogen doped delta layers with thickness of 3 nm were obtained.

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