Diamond crystals with low nitrogen concentration were synthesized from the Fe-Ni-C system with Ti additive at high pressure and high temperature (HPHT) in a china-type cubic high pressure apparatus (CHPA). The synthes...Diamond crystals with low nitrogen concentration were synthesized from the Fe-Ni-C system with Ti additive at high pressure and high temperature (HPHT) in a china-type cubic high pressure apparatus (CHPA). The synthesis pressure range was 4.8-5.2 GPa, and the temperature range was 1420-1600 K. The lowest synthesis pressure for diamond fell first and then rose with the increase of Ti additive. The color, shape, surface morphology and nitrogen impurity concentration of the synthesized diamond crystals were characterized using optical microscopy (OM), scanning electron microscopy (SEM) and micro Fourier transform infrared (FTIR) spectrometry. The results show that the Ti additive has significant effects on color, growth rate, crystal shape, surface morphology and nitrogen impurity con- centration of the synthesized diamond crystals. The color of diamond crystals synthesized without Ti additive is yellow, while that with Ti additive becomes light and nearly colorless. The growth rate without Ti additive is higher than that with Ti additive. The crystal shapes of as-grown diamond crystals vary with the increase of Ti additive. The {111} crystal faces become dominant and some {311} crystal faces appear with the increase of Ti additive. The concentration of nitrogen impurity in diamond crystals without Ti additive is higher than that with Ti additive.展开更多
In this work, under pressure 5.4 GPa and temperature 1250-1400°C, large gem-diamond single crystals with perfect shape and different content of additive boron were synthesized using temperature gradient method. H...In this work, under pressure 5.4 GPa and temperature 1250-1400°C, large gem-diamond single crystals with perfect shape and different content of additive boron were synthesized using temperature gradient method. High-purity boron powders were added as boron source into the graphite powder, and the effects of additive boron on crystal growth habit were investigated in detail. The relationship between the growth rate and the amount of additive boron was studied. The scanning electron microscopy was employed to study the morphology of boron-doped diamond crystals. Raman spectroscopy and Hall measurements were used to investigate the crystal structures and the carrier concentration, respectively. The results show that with the increase of the content of boron added into graphite powder, the crystal growth rate and the carrier concentration increase firstly, and decrease afterwards, and the zone-center phonon line at 1332 cm 1 has small shift to lower energy. The defects occur on the crystal surface when excessive boron is added in the synthesis system.展开更多
In this paper, crystal growth instability of diamond was studied in a Fe-Ni-C system at high temperature-high pressure (HPHT). As any other crystal grown from solution, the flat or smooth growth interface of the diamo...In this paper, crystal growth instability of diamond was studied in a Fe-Ni-C system at high temperature-high pressure (HPHT). As any other crystal grown from solution, the flat or smooth growth interface of the diamond crystal is highly sensitive to growth conditions. The growth front interface should be of great importance to understand the diamond growth process. The presence of cellular growth interface by transmission electron microscopy indicated that there existed a narrow constitutional supercooling zone in front of the growth interface. Several parallel layers with cellular interface by TEM directly suggested that the diamond grows from the solution of carbon in the molten catalyst layer by layer, which is in accordance with the result obtained by scanning electron microscopy in this paper. Impurities are trapped by rapidly advancing growth layers during the diamond growth and they impose a great effect on the growth front stability. As the growth front interface approaches the impurity particle to a distance of about 10-5~10-7 cm, appreciable molecular forces begin to operate between them, and the impurity particle is trapped as the growth rate reaches a critical value. As a result, the driving force for crystallization under the impurity particles becomes smaller, the front buckles under the particle. An impurity naturally reduces the growth rate to a different extent.展开更多
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 o...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.展开更多
基金Supported by the National Natural Science Foundation of China (Grant Nos. 50572032 and 50731006)
文摘Diamond crystals with low nitrogen concentration were synthesized from the Fe-Ni-C system with Ti additive at high pressure and high temperature (HPHT) in a china-type cubic high pressure apparatus (CHPA). The synthesis pressure range was 4.8-5.2 GPa, and the temperature range was 1420-1600 K. The lowest synthesis pressure for diamond fell first and then rose with the increase of Ti additive. The color, shape, surface morphology and nitrogen impurity concentration of the synthesized diamond crystals were characterized using optical microscopy (OM), scanning electron microscopy (SEM) and micro Fourier transform infrared (FTIR) spectrometry. The results show that the Ti additive has significant effects on color, growth rate, crystal shape, surface morphology and nitrogen impurity con- centration of the synthesized diamond crystals. The color of diamond crystals synthesized without Ti additive is yellow, while that with Ti additive becomes light and nearly colorless. The growth rate without Ti additive is higher than that with Ti additive. The crystal shapes of as-grown diamond crystals vary with the increase of Ti additive. The {111} crystal faces become dominant and some {311} crystal faces appear with the increase of Ti additive. The concentration of nitrogen impurity in diamond crystals without Ti additive is higher than that with Ti additive.
文摘In this work, under pressure 5.4 GPa and temperature 1250-1400°C, large gem-diamond single crystals with perfect shape and different content of additive boron were synthesized using temperature gradient method. High-purity boron powders were added as boron source into the graphite powder, and the effects of additive boron on crystal growth habit were investigated in detail. The relationship between the growth rate and the amount of additive boron was studied. The scanning electron microscopy was employed to study the morphology of boron-doped diamond crystals. Raman spectroscopy and Hall measurements were used to investigate the crystal structures and the carrier concentration, respectively. The results show that with the increase of the content of boron added into graphite powder, the crystal growth rate and the carrier concentration increase firstly, and decrease afterwards, and the zone-center phonon line at 1332 cm 1 has small shift to lower energy. The defects occur on the crystal surface when excessive boron is added in the synthesis system.
基金This work was supported by the National Natural Science Foundation of China (Grant. No 59631060).
文摘In this paper, crystal growth instability of diamond was studied in a Fe-Ni-C system at high temperature-high pressure (HPHT). As any other crystal grown from solution, the flat or smooth growth interface of the diamond crystal is highly sensitive to growth conditions. The growth front interface should be of great importance to understand the diamond growth process. The presence of cellular growth interface by transmission electron microscopy indicated that there existed a narrow constitutional supercooling zone in front of the growth interface. Several parallel layers with cellular interface by TEM directly suggested that the diamond grows from the solution of carbon in the molten catalyst layer by layer, which is in accordance with the result obtained by scanning electron microscopy in this paper. Impurities are trapped by rapidly advancing growth layers during the diamond growth and they impose a great effect on the growth front stability. As the growth front interface approaches the impurity particle to a distance of about 10-5~10-7 cm, appreciable molecular forces begin to operate between them, and the impurity particle is trapped as the growth rate reaches a critical value. As a result, the driving force for crystallization under the impurity particles becomes smaller, the front buckles under the particle. An impurity naturally reduces the growth rate to a different extent.
基金Project supported by the National Natural Science Foundation of China(Grant No.51772120)the Project for Key Science and Technology Research of Henan Province,China(Grant Nos.162102210275 and 172102210283)+1 种基金the Key Scientific Research Project in Colleges and Universities of Henan Province,China(Grant Nos.18A430017 and 17A430020)the Professional Practice Demonstration Base for Professional Degree Graduate in Material Engineering of Henan Polytechnic University,China(Grant No.2016YJD03)
文摘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.
