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Journal Articles

Hydrogenation of silicon-bearing hexagonal close-packed iron and its implications for density deficits in the inner core

Mori, Yuichiro*; Kagi, Hiroyuki*; Aoki, Katsutoshi*; Takano, Masahiro*; Kakizawa, Sho*; Sano, Asami; Funakoshi, Kenichi*

Earth and Planetary Science Letters, 634, p.118673_1 - 118673_8, 2024/05

https://doi.org/10.1016/j.epsl.2024.118673

To investigate silicon effects on the hydrogen-induced volume expansion of iron, neutron diffraction and X-ray diffraction experiments were conducted to examine hcp-Fe$$_{0.95}$$Si$$_{0.05}$$ under high pressures and high temperatures. Neutron diffraction experiments were performed on the deuterated hcp-Fe$$_{0.95}$$Si$$_{0.05}$$ at 13.5 GPa and 900 K, and at 12.1 GPa and 300 K. By combining the P-V-T equation of state of hcp-Fe$$_{0.95}$$Si$$_{0.05}$$, present results indicate that the hydrogen-induced volume expansion of hcp-Fe$$_{0.95}$$Si$$_{0.05}$$ is 10% greater than that of pure hcp iron. Using the obtained values, we estimated the hydrogen content that would reproduce the density deficit in the inner core, which was 50% less than that without the effect of silicon. Possible hydrogen content, $$x$$, in the inner core and the outer core was calculated to be 0.07 and 0.12-0.15, respectively, when reproducing the density deficit of the inner core with hcp-Fe$$_{0.95}$$Si$$_{0.05}$$Hx.

Journal Articles

Deuterium content and site occupancy in iron sulfide at high pressure and temperature determined using in situ neutron diffraction measurements

Abeykoon, S.*; Howard, C.*; Dominijanni, S.*; Eberhard, L.*; Kurnosov, A.*; Frost, D. J.*; Boffa Ballaran, T.*; Terasaki, Hidenori*; Sakamaki, Tatsuya*; Suzuki, Akio*; et al.

Journal of Geophysical Research; Solid Earth, 128(9), p.e2023JB026710_1 - e2023JB026710_17, 2023/09

https://doi.org/10.1029/2023JB026710
 Times Cited Count：0 Percentile：0.01(Geochemistry & Geophysics)

Small amounts of iron sulphide minerals are found in most rocks from the Earth's mantle and as inclusions trapped in natural diamonds. Hydrogen may dissolve into iron sulphide minerals under high pressures and temperature, but is most likely lost once pressure and temperature are removed. In this study, we determined deuterium contents in iron sulphide, held under high pressure and temperature conditions, using neutron diffraction measurements with 6-ram multi-anvil press at PLANET, J-PARC. Deuterium contents in iron sulphide were measured at high-P, up to 11.4 GPa and high-T to 1300 K in in situ neutron diffraction experiments. The total deuterium content increases with both P and T. The results are used to estimate hydrogen contents of iron sulphide minerals in the deep continental lithospheric mantle, which are found to be in the range 1700-2700 ppm. This corresponds to approximately 2-3 ppm of hydrogen in the bulk mantle.

Journal Articles

Hydrogen occupation and hydrogen-induced volume expansion in Fe$$_{0.9}$$Ni$$_{0.1}$$D$$_x$$ at high $$P-T$$ conditions

Shito, Chikara*; Kagi, Hiroyuki*; Kakizawa, Sho*; Aoki, Katsutoshi*; Komatsu, Kazuki*; Iizuka, Riko*; Abe, Jun*; Saito, Hiroyuki*; Sano, Asami; Hattori, Takanori

American Mineralogist, 108(4), p.659 - 666, 2023/04

https://doi.org/10.2138/am-2022-8348
 Times Cited Count：1 Percentile：64.83(Geochemistry & Geophysics)

The phase relation and crystal structure of Fe$$_{0.9}$$Ni$$_{0.1}$$H$$_x$$ (D$$_x$$) at high pressures and temperatures up to 12 GPa and 1000 K were clarified by in-situ X-ray and neutron diffraction measurements. Under $$P-T$$ conditions of the present study, no deuterium atoms occupied tetragonal ($$T$$) sites of face-centered cubic (fcc) Fe$$_{0.9}$$Ni$$_{0.1}$$D$$_x$$ unlike fcc FeH$$_x$$(D$$_x$$). The deuterium-induced volume expansion per deuterium $$v_mathrm{D}$$ was determined as 2.45(4) $AA$^3$$ and 3.31(6) $AA$^3$$ for fcc and hcp phases, respectively, which were significantly larger than the corresponding values for FeD$$_x$$. The $$v_mathrm{D}$$ value slightly increased with increasing temperature. This study suggests that only 10% of nickel in iron drastically changes the behaviors of hydrogen in metal. Assuming that $$v_mathrm{D}$$ is constant regardless of pressure, the maximum hydrogen content in the Earth's inner core is estimated to be one to two times the amount of hydrogen in the oceans.

Journal Articles

Magnetic and structure transition of Mn$$_{3-x}$$Fe$$_x$$O$$_4$$ solid solutions under high-pressure and high-temperature conditions

Yamanaka, Takamitsu*; Hirao, Naohisa*; Nakamoto, Yuki*; Mikouchi, Takashi*; Hattori, Takanori; Komatsu, Kazuki*; Mao, H.-K.*

Physics and Chemistry of Minerals, 49(10), p.41_1 - 41_14, 2022/10

https://doi.org/10.1007/s00269-022-01215-4
 Times Cited Count：0 Percentile：0.02(Materials Science, Multidisciplinary)

Magnetic and crystal structure of Mn$$_{3-x}$$Fe$$_x$$O$$_4$$ solid solutions under high-PT conditions are investigated by neutron diffraction and synchrotron M${"o}$ssbauer spectroscopy. The ferrimagnetic-paramagnetic transition and tetragonal-cubic transition of Mn$$_2$$FeO$$_4$$ spinel occur at 100$$^circ$$C and 180$$^circ$$C, respectively, suggesting both the transitions are not coupled. The structure transition temperature decreases with pressure. M${"o}$ssbauer experiments and neutron diffraction revealed that the Fe$$^{2+}$$ occupancy in tetrahedral site increases increase with pressure, suggesting Mn$$_2$$FeO$$_4$$ phase approaches inverse spinel. Magnetic structure refinement clarified paramagnetic and ferrimagnetic structure of MnFe$$_2$$O$$_4$$ and Mn$$_2$$FeO$$_4$$. These spinels transform into high-pressure orthorhombic phases at 18.4 and 14.0 GPa, respectively, indicating lower transition pressure with increasing Mn content.

Journal Articles

Effects of potential on the electrical conductivity of a solution within a crevice of stainless steel in high-temperature water

Soma, Yasutaka; Komatsu, Atsushi; Ueno, Fumiyoshi

Corrosion, 78(6), p.503 - 515, 2022/06

https://doi.org/10.5006/3187
 Times Cited Count：0 Percentile：0(Materials Science, Multidisciplinary)

The effects of electrochemical potential (ECP) on water chemistry within a crevice are of critical importance for understanding stress corrosion cracking (SCC) of Fe-Cr-Ni alloys in high temperature water. In this study, the effects of ECP on the electrical conductivity of a solution within a Type-316L stainless steel crevice ($$sigma$$$$_{crev}$$) have been studied in 288$$^{circ}$$C and 8 MPa water containing 10 ppb Cl$$^{-}$$ as major anionic species. In situ measurements of $$sigma$$$$_{crev}$$ in a rectangular crevice with a gap of 15 $$mu$$m and a depth of 23 mm have been conducted using small sensors installed at different crevice depths. An increase in ECP from -0.49 V (vs. standard hydrogen electrode) to -0.12 V resulted in an increase in $$sigma$$$$_{crev}$$ from 12 $$mu$$Scm$$^{-1}$$ to 160 $$mu$$Scm$$^{-1}$$ at a distance of 21 mm from the crevice mouth. The increase in $$sigma$$$$_{crev}$$ reached a maximum at about 0.15 V (about 300 $$mu$$Scm$$^{-1}$$) and then tended to decrease with increasing potential. Finite element model analysis taking into account the electrochemical reaction quantitatively reproduced this behavior. It is considered that Cl$$^{-}$$ is the major anionic species transported into the crevice at relatively low potentials, and that $$sigma$$$$_{crev}$$ increases monotonically with increasing ECP. On the other hand, when ECP exceeds around 0 V, a sufficient amount of HCrO$$_{4}$$$$^{-}$$ generated by transpassive dissolution also transported into the gap. Since this chemical species is highly oxidizing, unlike Cl, it is assumed that it reacts with metal cations to oxidize and precipitate them, thereby lowering conductivity.

Journal Articles

Electrochemical behavior of Fe-Cr-Ni alloys in simulated crevice condition in high temperature water

Soma, Yasutaka; Kato, Chiaki

Zairyo To Kankyo 2022 Koenshu (CD-ROM), p.219 - 220, 2022/05

It is important to understand the electrochemical properties of stainless steel in environment created within crevice of stainless steel in high temperature water (crevice environment). This is because acidification and concentration of impurity ions occur in the crevice environment and this is common inside the stress corrosion crack. In this study, we reproduced the crevice environment in bulk scale and investigated mainly the effect of Cr concentration on the electrochemical properties of Fe-Cr-Ni alloys. Polarization curves of Fe-20Ni-xCr (x=16.4, 23, 26) were measured in water with a temperature of 288$$^{circ}$$C, a Cl concentration of 2$$times$$10$$^{-4}$$ mol/dm$$^{-3}$$, a pH value of about 4.5, and a dissolved hydrogen concentration of 10 ppb. The peak currents of active dissolution (at -400 mV) and passive current density (at -50 mV) for specimens with Cr concentrations x = 16.4, 23, and 26% were approximately 13.8, 15.9, 10.0 $$mu$$Acm$$^{-2}$$, and 18.4, 8.5, 8.5 $$mu$$Acm$$^{-2}$$, respectively. Although the current values of x=26 were slightly lower in both cases, it was concluded that there was no clear dependence of the polarization curve on Cr concentration in this environment.

Journal Articles

Behavior of light elements in iron-silicate-water-sulfur system during early Earth's evolution

Iizuka, Riko*; Goto, Hirotada*; Shito, Chikara*; Fukuyama, Ko*; Mori, Yuichiro*; Hattori, Takanori; Sano, Asami; Funakoshi, Kenichi*; Kagi, Hiroyuki*

Scientific Reports (Internet), 11(1), p.12632_1 - 12632_10, 2021/06

https://doi.org/10.1038/s41598-021-91801-3
 Times Cited Count：3 Percentile：32.31(Multidisciplinary Sciences)

The Earth's core consist of Fe-Ni alloy with some light elements (H, C, O, Si, S etc.). Hydrogen (H) is the most abundant element in the universe and one of the promising candidates. In this study, we have investigated the effects of sulfur(S) on hydrogenation of iron-hydrous silicate system containing saturated water in the ideal composition of the primitive Earth. We observed a series of phase transitions of Fe, dehydration of the hydrous mineral, and formation of olivine and enstatite with increasing temperature. The FeS formed as the coexisting phase of Fe under high-pressure and temperature condition, but its unit cell volume did not increase, suggesting that FeS is hardly hydrogenated. Recovered samples exhibited that H and S can be incorporated into solid Fe, which lowers the melting temperature as Fe(H$$_{x}$$)-FeS system. No detection of other light elements (C, O, Si) in solid Fe suggests that they dissolve into molten iron hydride and/or FeS in the later process of Earth's core-mantle differentiation.

Journal Articles

Pressure effect on isotope fractionation factor

Sano, Asami; Ito, Shoichi*; Suzumura, Akimasa*; Ueno, Yuichiro*; Yagi, Hikaru*; Inoue, Toru*; Kawazoe, Takaaki*

Koatsuryoku No Kagaku To Gijutsu, 30(2), p.85 - 94, 2020/10

https://doi.org/10.4131/jshpreview.30.85

Minerals and rocks exhibit various isotope compositions depending on their origins and histories. In interpreting their isotopic variations, the equilibrium isotope fractionation factor is a key because it depends on the environment parameters such as temperature. Recent studies have shown that the effect of pressure on the isotope fractionation, which was considered negligible compared to temperature, is significant under the conditions of the Earth's interior. In this article we review recent advances in experimental studies to determine the isotope fractionation of iron and hydrogen at high pressure over several GPa, discussing their issues and future perspectives.

Journal Articles

Crystal and magnetic structures of double hexagonal close-packed iron deuteride

Saito, Hiroyuki*; Machida, Akihiko*; Iizuka, Riko*; Hattori, Takanori; Sano, Asami; Funakoshi, Kenichi*; Sato, Toyoto*; Orimo, Shinichi*; Aoki, Katsutoshi*

Scientific Reports (Internet), 10, p.9934_1 - 9934_8, 2020/06

https://doi.org/10.1038/s41598-020-66669-4
 Times Cited Count：3 Percentile：15.07(Multidisciplinary Sciences)

Neutron powder diffraction profiles were collected for iron deuteride (FeDx) while the temperature decreased from 1023 to 300 K for a pressure range of 4-6 GPa. The $$varepsilon$$' deuteride with a double hexagonal close-packed (dhcp) structure, which coexisted with other stable or metastable deutrides at each temperature and pressure condition, formed solid solutions with a composition of FeD$$_{0.68(1)}$$ at 673 K and 6.1 GPa and FeD$$_{0.74(1)}$$ at 603 K and 4.8 GPa. Upon stepwise cooling to 300 K, the D-content x increased to a stoichiometric value of 1.0 to form monodeuteride FeD$$_{1.0}$$. In the dhcp FeD$$_{1.0}$$ at 300 K and 4.2 GPa, dissolved D atoms fully occupied the octahedral interstitial sites, slightly displaced from the octahedral centers in the dhcp metal lattice, and the dhcp sequence of close-packed Fe planes contained hcp-stacking faults at 12%. Magnetic moments with 2.11 $$pm$$ 0.06 B/Fe-atom aligned ferromagnetically in parallel on the Fe planes.

Journal Articles

Hexagonal close-packed iron hydride behind the conventional phase diagram

Machida, Akihiko*; Saito, Hiroyuki*; Hattori, Takanori; Sano, Asami; Funakoshi, Kenichi*; Sato, Toyoto*; Orimo, Shinichi*; Aoki, Katsutoshi*

Scientific Reports (Internet), 9(1), p.12290_1 - 12290_9, 2019/08

https://doi.org/10.1038/s41598-019-48817-7
 Times Cited Count：25 Percentile：83.96(Multidisciplinary Sciences)

Hexagonal close-packed iron hydride, hcp FeHx, is absent from the conventional phase diagram of the Fe-H system, although hcp metallic Fe exists stably over extensive temperature ($$T$$) and pressure ($$P$$) conditions, including those corresponding to the Earth's inner core. ${{it In situ}}$ X-ray and neutron diffraction measurements at temperatures ranging from 298 to 1073 K and H pressures ranging from 4 to 7 GPa revealed that the hcp hydride was formed for FeH$$_{x}$$ compositions when $$x < 0.6$$. Hydrogen atoms occupied the octahedral interstitial sites of the host metal lattice both partially and randomly. The hcp hydride exhibited a H-induced volume expansion of 2.48(5) $AA $^{3}$$/H-atom, which was larger than that of the face-centered cubic (fcc) hydride. The hcp hydride showed an increase in $$x$$ with $$T$$, whereas the fcc hydride showed a corresponding decrease. The present study provides guidance for further investigations of the Fe-H system over an extensive $$x$$-$$T$$-$$P$$ region.

Journal Articles

In-situ measurement of electrical conductivity of solution within crevice of stainless steel in high temperature and high purity water

Soma, Yasutaka; Komatsu, Atsushi; Ueno, Fumiyoshi

Zairyo To Kankyo, 67(9), p.381 - 385, 2018/09

https://doi.org/10.3323/jcorr.67.381

In-situ measurement of electrical conductivity of solution within crevice of SUS316L stainless steel in 288$$^{circ}$$C water has been conducted with newly developed electrochemical sensor system. The sensor measures local electrical conductivity of crevice solution beneath the electrode ($$kappa$$$$_{crev}$$) with electrochemical impedance method. The sensors were installed at different positions within tapered crevice of SUS316L stainless steel. The crevice specimen with the sensors were immerged into 288$$^{circ}$$C, 8 MPa, pure oxygen saturated high purity water for 100 h. $$kappa$$$$_{crev}$$ at a position with crevice gap of $$approx$$59.3$$mu$$m was 8-11$$mu$$S/cm, least deviate from conductivity of 288$$^{circ}$$C pure water (4.4$$mu$$S/cm) and no localized corrosion occurred. On the contrary, $$kappa$$$$_{crev}$$ at a position with crevice gap of $$approx$$4.4$$mu$$m increased with time and showed maximum value of $$approx$$1600$$mu$$S/cm at 70 h. Localized corrosion occurred in the vicinity of this position. Thermodynamic equilibrium calculation showed $$kappa$$$$_{crev}$$ of 1600$$mu$$S/cm being equivalent to pH of 3 to 3.7. It can be concluded that acidification occurred in tight crevice even under high purity bulk water and resulted in localized corrosion.

Journal Articles

Localized corrosion in crevice of SUS316 stainless steel in oxygenated high temperature and high purity water

Soma, Yasutaka; Ueno, Fumiyoshi

Zairyo To Kankyo, 67(5), p.222 - 228, 2018/05

https://doi.org/10.3323/jcorr.67.222

Localized corrosion in crevice of SUS316 stainless steel after immersion in 288$$^{circ}$$C high purity water with dissolved oxygen concentration of 32 ppm for 100 h was analyzed. Two different types of localized corrosion initiated on grain boundary and inclusions. The former initiated on grain boundary and oxide grown into grain matrix. The oxidized area showed duplex structure composed of microcrystalline FeCr$$_{2}$$O$$_{4}$$ and island-shaped residual metals. The latter initiated on inclusions containing Ca and S and microcrystalline FeCr$$_{2}$$O$$_{4}$$ grown into metal matrix. These localized corrosion occurred selectively in oxygen depleted area indicated formation of macroscopic corrosion cell with the corroded area as anode and surrounding oxygenated area as cathode.

Journal Articles

Effect of dissolved gas on mechanical property of sheath material of mineral insulated cables under high temperature and pressure water

Takeuchi, Tomoaki; Nakano, Hiroko; Uehara, Toshiaki; Tsuchiya, Kunihiko

Nuclear Materials and Energy (Internet), 9, p.451 - 454, 2016/12

https://doi.org/10.1016/j.nme.2016.06.018
 Times Cited Count：1 Percentile：10.71(Nuclear Science & Technology)

no abstracts in English

Journal Articles

Electrical conductivity and potential response within crevice of stainless steel in high temperature water under cyclic deaerated and aerated condition

Soma, Yasutaka; Kato, Chiaki; Ueno, Fumiyoshi

Fushoku Boshoku Kyokai Dai-63-Kai Zairyo To Kankyo Toronkai Koenshu, p.253 - 256, 2016/10

Contribution of corrosion to advance of stress corrosion cracking (SCC) of stainless steel in high temperature water must be assessed because serious corrosion can be found within SCC of light water reactors. The corrosion took the form of both intergranular and grain-matrix attack indicate aggressive corrosion condition was formed in the crevice of the SCC. We have investigated the crevice environment electrochemically and found that local electrical conductivity of the crevice solution at satisfactory narrow crevice gap having more than 100 times higher than that of bulk solution. In this research we assessed effect of cyclic deaerated and aerated bulk solution to the crevice environment. The result showed that electrical conductivity of the crevice solution under the deaerated bulk solution increased more than 10times by injection of pure oxygen suggest that the dissolved oxygen caused aggressive corrosion condition within the crevice.

JAEA Reports

Performance test of ex-core high temperature and high pressure water loop test equipment (Contract research)

Nakano, Hiroko; Uehara, Toshiaki; Takeuchi, Tomoaki; Shibata, Hiroshi; Nakamura, Jinichi; Matsui, Yoshinori; Tsuchiya, Kunihiko

JAEA-Technology 2015-049, 61 Pages, 2016/03

JAEA-Technology-2015-049.pdf:14.7MB

In Japan Atomic Energy Agency, we started a research and development so as to monitor the Nuclear Plant Facilities situations during a severe accident, such as a radiation-resistant monitoring camera under a severe accident, a radiation resistant in-water transmission system for conveying the information in-core and a heat-resistant signal cable. As part of advance in a heat-resistant signal cable, we maintained to ex-core high-temperature and pressure water loop test equipment which can be simulated conditions of BWRs and PWRs for evaluation reliability and property of construction sheath materials. This equipment consists of Autoclave, water conditioning tank, water pump, high-pressure metering pump, preheater, heat exchanger and pure water purification equipment. This report describes the basic design and the results of performance tests of construction machinery and tools of ex-core high-temperature and pressure water loop test equipment.

Journal Articles

True Boundary for the formation of homoleptic transition-metal hydride complexes

Takagi, Shigeyuki*; Iijima, Yuki*; Sato, Toyoto*; Saito, Hiroyuki; Ikeda, Kazutaka*; Otomo, Toshiya*; Miwa, Kazutoshi*; Ikeshoji, Tamio*; Aoki, Katsutoshi*; Orimo, Shinichi*

Angewandte Chemie; International Edition, 54(19), p.5650 - 5653, 2015/05

https://doi.org/10.1002/anie.201500792
 Times Cited Count：32 Percentile：68.44(Chemistry, Multidisciplinary)

Journal Articles

Design and performance of high-pressure PLANET beamline at pulsed neutron source at J-PARC

Hattori, Takanori; Sano, Asami; Arima, Hiroshi*; Komatsu, Kazuki*; Yamada, Akihiro*; Inamura, Yasuhiro; Nakatani, Takeshi; Seto, Yusuke*; Nagai, Takaya*; Utsumi, Wataru; et al.

Nuclear Instruments and Methods in Physics Research A, 780, p.55 - 67, 2015/04

https://doi.org/10.1016/j.nima.2015.01.059
 Times Cited Count：75 Percentile：99.01(Instruments & Instrumentation)

PLANET is a time-of-flight (ToF) neutron beamline dedicated to high-pressure and high-temperature experiments. The large six-axis multi-anvil high-pressure press designed for ToF neutron diffraction experiments enables routine data collection at high pressures and high temperatures up to 10 GPa and 2000 K, respectively. To obtain clean data, the beamline is equipped with the incident slits and receiving collimators to eliminate parasitic scattering from the high-pressure cell assembly. The high performance of the diffractometer for the resolution ($$Delta$$ $$d$$/$$d$$ $$sim$$ 0.6%) and the accessible $$d$$-spacing range (0.2-8.4 ${AA}$) together with low-parasitic scattering characteristics enables precise structure determination of crystals and liquids under high pressure and temperature conditions.

Journal Articles

Six-axis multi-anvil press for high-pressure, high-temperature neutron diffraction experiments

Sano, Asami; Hattori, Takanori; Arima, Hiroshi*; Yamada, Akihiro*; Tabata, Satoshi*; Kondo, Masahiro*; Nakamura, Akihiro*; Kagi, Hiroyuki*; Yagi, Takehiko*

Review of Scientific Instruments, 85(11), p.113905_1 - 113905_8, 2014/11

https://doi.org/10.1063/1.4901095
 Times Cited Count：42 Percentile：84.25(Instruments & Instrumentation)

We developed a six-axis multi-anvil press, ATSUHIME, for high-pressure and high-temperature in situ time-of-flight neutron powder diffraction experiments. The press has six orthogonally oriented hydraulic rams that operate individually to compress a cubic sample assembly. Experiments indicate that the press can generate pressures up to 9.3 GPa and temperatures up to 2000 K using a 6-6-type cell assembly, with available sample volume of about 50 mm $$^{3}$$. Using a 6-8-type cell assembly, the available conditions expand to 16 GPa and 1273 K. Combination of the six-axis press and the collimation devices realized high-quality diffraction pattern with no contamination from the heater or the sample container surrounding the sample. This press constitutes a new tool for using neutron diffraction to study the structures of crystals and liquids under high pressures and temperatures.

Journal Articles

Recent progress on solution chemistry of actinides studied by time-resolved laser-induced fluorescence spectroscopy

Kimura, Takaumi; Kirishima, Akira*; Arisaka, Makoto

Kidorui, (47), p.43 - 56, 2005/11

no abstracts in English

Journal Articles

Synthesis of Al$$_{x}$$Ga$$_{1-x}$$N and InN crystals under high pressures

Saito, Hiroyuki; Utsumi, Wataru; Kaneko, Hiroshi*; Aoki, Katsutoshi

Proceedings of Joint 20th AIRAPT - 43rd EHPRG International Conference on High Pressure Science and Technology (CD-ROM), 4 Pages, 2005/06

We have performed synthesis studies of various III-V nitrides crystals, key materials for optoelectronic and high-power/frequency devices, using a cubic-anvil-type large volume high-pressure apparatus combined with in situ X-ray diffraction. Polly-crystallines of Al$$_{x}$$Ga$$_{1-x}$$N alloys covering a composition range of 0 $$leq$$ x $$leq$$ 1 were synthesized by a solid-phase reaction under high pressure. In situ X-ray diffraction profiles were measured to observe the alloying process, which started at around 800$$^{circ}$$C under 6.0 GPa. Single crystal of Al$$_{0.1}$$Ga$$_{0.9}$$N was also successfully obtained by slow cooling of its melt from 2400$$^{circ}$$C at 6.5 GPa. For InN, its phase diagram was determined under high P-T conditions up to 20GPa and 2000$$^{circ}$$C based on the in situ observations, which demonstrates that 19GPa and 1900$$^{circ}$$C are needed for its congruent melting.

74 (Records 1-20 displayed on this page)