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Abstract
Gem-sized single crystals of diamond have been produced by very high growth rate microwave plasma chemical vapor deposition (CVD) and found to exhibit remarkable mechanical properties. The as-grown material has extremely high fracture toughness, and treatment by high-pressure/high-temperature annealing produces crystals that have exceptionally high intrinsic hardness. The annealing appears to induce a novel work hardening of CVD single-crystal diamond. (C) 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Abstract
A 820 micron thick single crystal diamond layer epitaxially grown on a single crystal diamond seed (high pressure, high temperature grown synthetic) by microwave plasma chemical vapor deposition with added nitrogen is characterized by an array of analytical techniques before and after annealing the material at high pressures and temperatures. The most striking result is the conversion of the initially dark colored, highly absorbing CVD layer to clear, transparent material after a 1 hour anneal at 7 GPa and 2200 degreesC. IR absorption in the region of the CH stretching modes, 2800 to 3107 cm(-1) shows a remarkable sharpening and persistence of the observed modes. IR absorption in the one-phonon region also indicates the presence of significant concentrations of ionized single substitutional nitrogen in the as grown material. EPR indicates a concentration of neutral single substitutional nitrogen at lattice sites of ca. I ppm, and this changes by less then 30% when annealed at temperatures up to 2200 degreesC. EPR also detects 0.1 ppm of the negatively charged nitrogen-vacancy-hydrogen complex in the as grown diamond, but this anneals out by 1900 degreesC, the negatively charged nitrogen-vacancy complex is below the EPR detection limit in these samples of about 0.1 ppm. Photoluminescence detects the presence of neutral and negatively charged nitrogen-vacancy complexes in the as grown material, and the formation of new, unassigned bands principally in the 800 to 900 nm region. The total detected nitrogen concentration in the sample is ca. 1.5 ppm. (C) 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Abstract
The synthesis of large single-crystal diamonds by chemical vapor deposition (CVD) at high growth rate has opened a new era for applications of the material. Large and thick single crystals can now be produced at very high growth rates, and the mechanical properties, chemistry, and optical and electronic properties of the material can be tuned over a wide range. The single crystals can have extremely high fracture toughness exceptionally high hardness following high-pressure/high-temperature annealing. CVD single-crystal diamonds will make possible a new generation of high-pressure-temperature experimentation to study Earth and planetary materials and should enable a variety of other new scientific and technological applications.
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Abstract
The detailed correlation of results from two dissimilar experimental techniques, transmission electron microscopy and micro-photoluminescence spectroscopy, has allowed us to obtain direct evidence of the interaction between linear and point defects in diamond as both 388.9 nm and 379 nm optical centers were found to be strongly related to dislocations. (c) 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Abstract
The correlation of TEM imaging and micro-photoluminescence studies of electron irradiated areas of diamond, developed in Bristol, has been extended to new optical centres and defects. In this paper, we show new evidence of the interaction of point defects with dislocations and grain boundaries in diamond. Optical centres at 518.6 and 518.8 nm are directly correlated with dislocations and an optical centre at 519.1 nm was correlated with a grain boundary. (c) 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Abstract
We report on the first observation of stimulated Raman scattering (SRS) in single crystal diamond synthesized by chemical vapor deposition (CVD). An efficiency of 45% of energy conversion from the pumping Nd3+:Y3Al5O12 laser radiation to all Stokes and anti-stokes components is achieved. This makes single crystal CVD diamond an attractive chi((3)) nonlinear crystalline material as a Raman laser converter.
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Abstract
Single crystal diamond produced by chemical vapor deposition (CVD) at very high growth rates (up to 150 mu m/h) has been successfully annealed without graphitization at temperatures up to 2200 degrees C and pressures <300 torr. Crystals were annealed in a hydrogen environment by using microwave plasma techniques for periods of time ranging from a fraction of minute to a few hours. This low-pressure/high-temperature (LPHT) annealing enhances the optical properties of this high-growth rate CVD single crystal diamond. Significant decreases are observed in UV, visible, and infrared absorption and photoluminescence spectra. The decrease in optical absorption after the LPHT annealing arises from the changes in defect structure associated with hydrogen incorporation during CVD growth. There is a decrease in sharp line spectral features indicating a reduction in nitrogen-vacancy-hydrogen (NVH-) defects. These measurements indicate an increase in relative concentration of nitrogen-vacancy (NV) centers in nitrogen-containing LPHT-annealed diamond as compared with as-grown CVD material. The large overall changes in optical properties and the specific types of alterations in defect structure induced by this facile LPHT processing of high-growth rate single-crystal CVD diamond will be useful in the creation of diamond for a variety of scientific and technological applications.
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Abstract
Single crystals of diamond up to 18 mm in thickness have been grown by microwave plasma assisted chemical vapor deposition at gas pressures of up to 350 torr. Growth rates of up to 165 mu m/h at 300 torr at high power density have been achieved. The processes were evaluated by optical emission spectroscopy. The high-quality single-crystal diamond grown at optimized conditions was characterized by UV-visible absorption and photoluminescence spectroscopy. The measurements reveal a direct relationship between residual absorption and nitrogen content in the gas chemistry. Fabrication of high quality single-crystal diamond at higher growth rates should be possible with improved reactor design that allows still higher gas synthesis pressures.
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Abstract
There have been important advances in microwave plasma chemical vapor deposition (MPCVD) of large single-crystal CVD diamond at high growth rates and applications of this diamond. The types of gas chemistry and growth conditions, including microwave power, pressure, and substrate surface temperatures, have been varied to optimize diamond quality and growth rates. The diamond has been characterized by a variety of spectroscopic and diffraction techniques. We have grown single-crystal CVD diamond over ten carats and above 1 cm in thickness at growth rates of 50-100 mu m/h. Colorless and near colorless single crystals up to two carats have been produced by further optimizing the process. The nominal Vickers fracture toughness of this high-growth rate diamond can be tuned to exceed 20 MPa m(1/2) in comparison to 5-10 MPa m(1/2) for conventional natural and CVD diamond. Post-growth high-pressure/ high-temperature (HPHT) and low-pressure/high-temperature (LPHT) annealing have been carried out to alter the optical, mechanical, and electronic properties. Most recently, single-crystal CVD diamond has been successfully annealed by LPHT methods without graphitization up to 2200 degrees C and < 300 Torr for periods of time ranging from a fraction of minute to a few hours. Significant changes observed in UV, visible, infrared, and photoluminescence spectra are attributed to changes in various vacancy centers and extended defects. (C) 2008 Elsevier B.V. All rights reserved.
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