Inclusions in large diamond single crystals at different temperatures of synthesis

The inclusions in large diamond single crystals have effects on its ultimate performance, which restricts its industrial applications to a great extent. Therefore, it is necessary to study the inclusions systematically. In this paper, large diamond single crystals with different content values of inclusions are synthesized along the(100) surface by the temperature gradient method(TGM) under 5.6 GPa at different temperatures. With the synthetic temperature changing from 1200?C to 1270?C,the shapes of diamonds change from plate to low tower, to high tower, even to steeple. From the microscopic photographs of the diamond samples, it can be observed that with the shapes of the samples changing at different temperatures, the content values of inclusions in diamonds become zero, a little, much and most, correspondingly. Consequently, with the temperature growing from low to high, the content values of inclusions in crystals increase. The origin of inclusions is explained by the difference in growth rate between diamond crystal and its surface. The content values of inclusions in diamond samples are quantitatively calculated by testing the densities of diamond samples. And the composition and inclusion content are analyzed by energy dispersive spectroscopy(EDS) and x-ray diffraction(XRD). From contrasting scanning electron microscopy(SEM) photographs, it can be found that the more the inclusions in diamond, the more imperfect the diamond surface is.

Growth characteristics of type IIa large single crystal diamond with Ti/Cu as nitrogen getter in FeNi–C system

High-quality type IIa large diamond crystals are synthesized with Ti/Cu as nitrogen getter doped in an FeNi–C system at temperature ranging from 1230℃to 1380℃and at pressure 5.3–5.9 GPa by temperature gradient method.Different ratios of Ti/Cu are added to the Fe Ni–C system to investigate the best ratio for high-quality type IIa diamond.Then,the different content of nitrogen getter Ti/Cu(Ti:Cu=4:3)is added to this synthesis system to explore the effect on diamond growth.The macro and micro morphologies of synthesized diamonds with Ti/Cu added,whose nitrogen concentration is determined by Fourier transform infrared(FTIR),are analyzed by optical microscopy(OM)and scanning electron microscopy(SEM),respectively.It is found that the inclusions in the obtained crystals are minimal when the Ti/Cu ratio is 4:3.Furthermore,the temperature interval for diamond growth becomes narrower when using Ti as the nitrogen getter.Moreover,the lower edge of the synthesis temperature of type IIa diamond is 25℃higher than that of type Ib diamond.With the increase of the content of Ti/Cu(Ti:Cu=4:3),the color of the synthesized crystals changes from yellow and light yellow to colorless.When the Ti/Cu content is 1.7 wt%,the nitrogen concentration of the crystal is less than 1 ppm.The SEM results show that the synthesized crystals are mainly composed by(111)and(100)surfaces,including(311)surface,when the nitrogen getter is added into the synthesis system.At the same time,there are triangular pits and dendritic growth stripes on the crystal surface.This work will contribute to the further research and development of high-quality type IIa diamond.

Effect of FeS doping on large diamond synthesis in FeNi-C system

The large single-crystal diamond with FeS doping along the （111） face is synthesized from the FeNi-C system by the temperature gradient method （TGM） under high-pressure and high-temperature （HPHT）. the effects of different FeS additive content on the shape, color, and quality of diamond are investigated. It is found that the （111） face of diamond is dominated and the （100） face of diamond disappears gradually with the increase of the FeS content. At the same time, the color of the diamond crystal changes from light yellow to gray-green and even gray-yellow. The stripes and pits corrosion on the diamond surface are observed to turn worse. The effects of FeS doping on the shape and surface morphology of diamond crystal are explained by the number of hang bonds in different surfaces of diamond. It can be shown from the test results of the Fourier transform infrared （FTIR） spectrum that there exists an S element in the obtained diamond. The N element content values in different additive amounts of diamond are calculated. The XPS spectrum results demonstrate that our obtained diamond contains S elements that exist in S-C and S-C-O forms in a diamond lattice. This work contributes to the further understanding and research of FeS-doped large single-crystal diamond characterization.

Synthesis and Characteristics of Type Ib Diamond Doped with NiS as an Additive

Large diamond single crystals doped with NiS are synthesized under high pressure and high temperature. It is found that the effects on the surface and shape of the synthesized diamond crystals are gradually enhanced by increasing the NiS additive amount. It is noted that the synthesis temperature is necessarily raised to 1280℃ to realize the diamond growth when the additive amount reaches 3.5% in the synthesis system. The results of Fourier transform infrared spectroscopy(FTIR) demonstrate that S is incorporated into the diamond lattice and exists in the form of C–S bond. Based on the FTIR results, it is found that N concentration in diamond is significantly increased, which are ascribed to the NiS additive. The analysis of x-ray photoelectron spectroscopy shows that S is present in states of C–S, S–O and C–S–O bonds. The relative concentration of S compared to C continuously increases in the synthesized diamonds as the amount of additive NiS increases. Additionally,the electrical properties can be used to characterize the obtained diamond crystals and the results show that diamonds doped with NiS crystals behave as n-type semiconductors.