Near-normal incident infrared reflectivity spectra of （100） MgAl2O4 spinel single crystal have been measured at different temperatures in the frequency region between 50 and 6000 cm^-1. Eight infrared-active phonon ...Near-normal incident infrared reflectivity spectra of （100） MgAl2O4 spinel single crystal have been measured at different temperatures in the frequency region between 50 and 6000 cm^-1. Eight infrared-active phonon modes are identified, which are fitted with the factorized form of the dielectric function. The dielectric property and optical conductivity of the MgAl2O4 crystal are analysed. From TO/LO splitting, the effective Szigeti charges and Born effective charges at different temperatures are calculated for studying the ionicity and the effect of polarization. Based on the relationship between the （LO-TO）1 splitting, which represents the transverse and longitudinal frequencies splitting of the highest energy phonon band in the reflectivity spectrum, and the ionic-covalent parameter, the four main phonon modes are assigned. MgA1204 can be considered as a pure ionic crystal and its optical characters do not change with decreasing temperature, so it may be used as a suitable substrate for high-Tc superconducting thin films.展开更多
Superconducting La1.937Sr0.063CuO4 crystals grown by the travelling-solvent floating-zone technique were thermally treated under various temperatures and oxygen pressures for moderately adjusting the oxygen content. T...Superconducting La1.937Sr0.063CuO4 crystals grown by the travelling-solvent floating-zone technique were thermally treated under various temperatures and oxygen pressures for moderately adjusting the oxygen content. The response of intrinsic electronic property of the crystals to the change of hole density in La2-xSrxCuO4 in the vicinity of the magic doping of x= 1/16 （= 0.0625） is studied in detail by magnetic measurements under various fields up to 1 T. It is found that when the superconducting critical temperature （Tc） increases with the oxygen content, there appears also a new subtle electronic state that can be detected from the differential curves of diamagnetic susceptibility dx/dT of the crystal sample. In contrast with the intrinsic state, the new subtle electronic state is very fragile under the magnetic fields. Our results indicate that a moderate change in oxygen doping does not significantly modify the intrinsic electronic state originally existing at the magic doping level.展开更多
The transmittance (T) and the reflectance (R) were measured for (TMA)2ZnCl4 single crystals and hence the absorption coefficient (α), extinction coefficient (Kex.), refractive index (n), real and im-aginary dielectri...The transmittance (T) and the reflectance (R) were measured for (TMA)2ZnCl4 single crystals and hence the absorption coefficient (α), extinction coefficient (Kex.), refractive index (n), real and im-aginary dielectric constants (ε', ε") of (TMA)2ZnCl4 crystals were calculated as a function of photon energy. The analysis of the spectra behavior of the absorption coefficient in the absorption region revealed indirect transition. The dispersion of the refractive index is discussed in terms of the sin-gle oscillator Wemple-DiDomenico model. The single oscillator energy (E0), the dispersion energy (Ed), the lattice dielectric constant (εL) and the ratio of free charge carrier concentration to the ef-fective mass (N/m*) were estimated. The FTIR spectra were recorded to study the functional groups of the as grown and annealed samples.展开更多
The 1-azido-2-chloro-4-nitrobenzene was prepared by nucleophilic substitution between 2-chloro-4-nitro-1-(trifluoromethylsulfinyl)benzene and sodium azide, and its structure was characterized by NMR spectrum and X-ray...The 1-azido-2-chloro-4-nitrobenzene was prepared by nucleophilic substitution between 2-chloro-4-nitro-1-(trifluoromethylsulfinyl)benzene and sodium azide, and its structure was characterized by NMR spectrum and X-ray single-crystal diffraction. It crystallizes in the monoclinic system, space group P21/n, Z = 8 and Mr = 198.57. A cultivation process of the single crystal of unstable aryl azide was provided. The group of trifluoromethyl sulfinyl was found for the first time to be a new excellent leaving group of aromatic nucleophilic substitution reactions.展开更多
A solar-blind photodetector is fabricated on single crystal Ga_2O_3 based on vertical structure Schottky barrier diode. A Cu Schottky contact electrode is prepared in a honeycomb porous structure to increase the ultra...A solar-blind photodetector is fabricated on single crystal Ga_2O_3 based on vertical structure Schottky barrier diode. A Cu Schottky contact electrode is prepared in a honeycomb porous structure to increase the ultraviolet(UV) transmittance.The quantum efficiency is about 400% at 42 V. The Ga_2O_3 photodetector shows a sharp cutoff wavelength at 259 nm with high solar-blind/visible(= 3213) and solar-blind/UV(= 834) rejection ratio. Time-resolved photoresponse of the photodetector is investigated at 253-nm illumination from room temperature(RT) to 85.8℃. The photodetector maintains a high reversibility and response speed, even at high temperatures.展开更多
We report a reproducible approach in preparing high-quality overdoped Bi2 Sr2 CaCu2 08＋δ （Bi2212） single crystals by annealing Bi2212 crystals in high oxygen pressure followed by a fast quenching. In this way, hig...We report a reproducible approach in preparing high-quality overdoped Bi2 Sr2 CaCu2 08＋δ （Bi2212） single crystals by annealing Bi2212 crystals in high oxygen pressure followed by a fast quenching. In this way, high-quality overdoped and heavily overdoped Bi2212 single crystals are obtained by controlling the annealing oxygen pressure. We find that, beyond a limit of oxygen pressure that can achieve most heavily overdoped Bi2212 with a Tc N63 K, the annealed Bi2212 begins to decompose. This accounts for the existence of the hole-doping limit and thus the Tc limit in the heavily overdoped region of Bi2212 by the oxygen annealing process. These results provide a reliable way in preparing high-quality overdoped and heavily overdoped Bi2212 crystals that are important for studies of the physical properties, electronic structure and superconductivity mechanism of the cuprate superconductors.展开更多
The compound described as [Cu(OH)2(H2O)2(4-C5H4NCOOH)2] in Chin. J. Struct. Chem., 2001, 20: 478-480 is instead the compound [Cu(H2O)4(4-C5H4NCOO)2], whose crystal structure has already been published elsewhere.
The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determin...The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.展开更多
The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been conf...The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS （ESI） and single-crystal X-ray diffraction. （R）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867（2）, b = 8.4087（2）, c = 14.325（6） A^°, β = 117.59（2）°, Z = 4, V = 1266.9（6） A^°3, Dc = 1.307 g/cm^3, F（000） = 528, μ（MoKα） = 0.097 mm-1, R = 0.0453 and wR = 0.1237; （S）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647（17）, b = 8.7034（17）, c = 9.5479（19） A^°, α = 105.33（3）, β = 100.95（3）, γ = 105.14（3）°, Z = 2, V = 614.1（2） A^°3, Dc = 1.348 g/cm^3, F（000） = 264, μ（MoKα） = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.展开更多
By using Tb407 and MoO3 as starting materials, ferroelectric Tb2（MoO4）3 crystal was grown by the Czochralski method. The as-grown crystal was pale green color, transparent and crack-free. X-ray powder diffraction （...By using Tb407 and MoO3 as starting materials, ferroelectric Tb2（MoO4）3 crystal was grown by the Czochralski method. The as-grown crystal was pale green color, transparent and crack-free. X-ray powder diffraction （XRPD）, transmission spectrum, dielectric constant and polarization-electric field （P-E） hysteresis loop measurements were performed to characterize the crystal. The XRPD confirmed the as-grown crystal to be Tb2（MoO4）3. The transmission spectrum of the crystal showed that its transmittance in the entire visible and most near-infrared region was more than 70% except for an absorption peak around 486 nm. Obvious dielectric anomaly could be observed at low frequencies with increasing temperature through the dielectric constant measurement and the Curie temperature of Tb2（MoO4）3 crystal was determined to be 162.3℃ The unsaturated P-E hysteresis loops indicated that it was difficult for the ferroelectric domains in Tb2（MoO4）3 crystal to array regularly with repeated switching of the electric field.展开更多
Experiments performed on the grwth of mixed crystals of rare earth tartrates (Y1-xSmx)2 (C4H4O6)3.zH2O (0≤x≤1) from silica gels at 35~40℃ and 25~30℃ employing single-diffusion technique. are discussed. The crysta...Experiments performed on the grwth of mixed crystals of rare earth tartrates (Y1-xSmx)2 (C4H4O6)3.zH2O (0≤x≤1) from silica gels at 35~40℃ and 25~30℃ employing single-diffusion technique. are discussed. The crystals maintain spherulitic morphology, irrespective of the value of x, concentration of upper and lower reactants, gel pH, gel age and gel temperature. Formation Of Liesegang rings in this system is a temperature dependent phenomenon. It is shown that with the increase of the value of x the system passes from Liesegangring phenomenon to singlezone phenomenon. Operative mechanism of crystallization in the higher (35~40℃) and lower temperature ranges (25~30℃) is explained. Seeded growth experiments indicate the possibility of increasing the size of the spherulites in the gel medium展开更多
The formation of macrostep during high-temperature phase of barium meta-borate （^-BaB204） single crystal growth has been investigated by both optical in-situ observation system and atomic force microscopy （AFM）. T...The formation of macrostep during high-temperature phase of barium meta-borate （^-BaB204） single crystal growth has been investigated by both optical in-situ observation system and atomic force microscopy （AFM）. The in- si$u observation results demonstrate that the critical linear size of growing facet exceeding the size that the macrostep generates is significantly anisotropic. The critical linear sizes are around 280 ~m and 620 ~m for {1010} and （T010} planes, respectively. AFM study illustrates that macrostep train with a height of 150 nm^200 nm is one typical morphological feature of the as-grown crystal surface. The riser of each macrostep consists of several straight and parallel sub-steps, indicating the occurrence of step bunching. Additionally, triangular sub-steps with heights of several nanometers on the treads of the macrosteps are found to be another typical feature of surface morphology, which implies a microscopically competitive bunching of sub-steps between various crystallographic orientations.展开更多
The compound （SiCl3）2Fe（CO）4 was synthesized and structurally characterized by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P2 1/n with α = 8.287（2）, b = 9.829（2）, c = 9.042（2...The compound （SiCl3）2Fe（CO）4 was synthesized and structurally characterized by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P2 1/n with α = 8.287（2）, b = 9.829（2）, c = 9.042（2） A, β = 96.19（3）°, V= 732.2（3） A^3, C4Cl6FeO4Si2, Mr = 436.77, Z = 2, Dc = 1.981 g/cm^3, F（000） = 424, μ（MoKα） = 2.282 mm^-1, the final R = 0.048 and wR = 0.164 for 1109 observed reflections （I 〉 2σ（I））. The crystal structure of （SiCl3）2Fe（CO）4 reveals that the Si（l）- Fe-Si（l）^a sequence is linear and perpendicular to the Fe（CO）4 cross-shaped plane.展开更多
Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3...Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.展开更多
The title compound, Cs 2[Mg(CO 3) 2(H 2O) 4], was synthesized by the dropwise addition of an aqueous solution of Mg(NO 3) 2 to a stirred aqueous Cs 2CO 3/CsHCO 3 solution. A colorless needle shaped crystal was formed ...The title compound, Cs 2[Mg(CO 3) 2(H 2O) 4], was synthesized by the dropwise addition of an aqueous solution of Mg(NO 3) 2 to a stirred aqueous Cs 2CO 3/CsHCO 3 solution. A colorless needle shaped crystal was formed by slow evaporation. The crystal structure was established on the basis of the single crystal X ray diffraction data. Cs 2[Mg(CO 3) 2(H 2O) 4] crystallized in the orthorhombic space group Pbca (No. 61) with a =0.658 4(1) nm, b =1.257 9(1) nm, c =1.301 3(1) nm, \{ V =1.077 8 nm 3, Z =4, D x=2.971 g·cm -3 , μ =69.20 cm -1 , F (000)=888, T =298 K, final R =0.029 and R w=0.024 for 1 037 observed reflections. The crystal consists of Cs + cations and the complex trans [Mg(CO 3) 2(H 2O) 4] 2- anions with each Mg atom coordinated by the six oxygens of two carbonate groups and four water molecules [ d (Mg_O)=0.203 6(4), 0.207 4(4), 0.213 4(4) nm]. The complex trans [Mg(CO 3) 2(H 2O) 4] 2- anions are arranged in a strongly compressed bcc pattern. A 3D network was formed through the intermolecular hydrogen bonds. The Cs + cations are located in cavities, each being surrounded by nine oxygens of five complex anions with d (Cs_O)=0.306 1-0.348 8 nm. The CO 2- 3 group reveals a lowering of D 3h symmetry due to site and coordination effects, but not any observable deviation from co planarity [ d (C_O)=0.127 2(6), 0.127 5(7) , 0.130 5(6) nm and O_C_O=119.6(5)°, 120.1(5)°, 120.4(5)°].展开更多
基金Project supported by the National Natural Science Foundation of China （Grant No 10474128） and Chinese Academy of Sciences.
文摘Near-normal incident infrared reflectivity spectra of （100） MgAl2O4 spinel single crystal have been measured at different temperatures in the frequency region between 50 and 6000 cm^-1. Eight infrared-active phonon modes are identified, which are fitted with the factorized form of the dielectric function. The dielectric property and optical conductivity of the MgAl2O4 crystal are analysed. From TO/LO splitting, the effective Szigeti charges and Born effective charges at different temperatures are calculated for studying the ionicity and the effect of polarization. Based on the relationship between the （LO-TO）1 splitting, which represents the transverse and longitudinal frequencies splitting of the highest energy phonon band in the reflectivity spectrum, and the ionic-covalent parameter, the four main phonon modes are assigned. MgA1204 can be considered as a pure ionic crystal and its optical characters do not change with decreasing temperature, so it may be used as a suitable substrate for high-Tc superconducting thin films.
基金Project supported by the Ministry of Science and Technology of China (973 project Grant No 2006CB0L0302)the National Natural Science Foundation of China (Grant No 10574149)Chinese Academy of Sciences (Grant No KJCX2-SW-W18)
文摘Superconducting La1.937Sr0.063CuO4 crystals grown by the travelling-solvent floating-zone technique were thermally treated under various temperatures and oxygen pressures for moderately adjusting the oxygen content. The response of intrinsic electronic property of the crystals to the change of hole density in La2-xSrxCuO4 in the vicinity of the magic doping of x= 1/16 （= 0.0625） is studied in detail by magnetic measurements under various fields up to 1 T. It is found that when the superconducting critical temperature （Tc） increases with the oxygen content, there appears also a new subtle electronic state that can be detected from the differential curves of diamagnetic susceptibility dx/dT of the crystal sample. In contrast with the intrinsic state, the new subtle electronic state is very fragile under the magnetic fields. Our results indicate that a moderate change in oxygen doping does not significantly modify the intrinsic electronic state originally existing at the magic doping level.
文摘The transmittance (T) and the reflectance (R) were measured for (TMA)2ZnCl4 single crystals and hence the absorption coefficient (α), extinction coefficient (Kex.), refractive index (n), real and im-aginary dielectric constants (ε', ε") of (TMA)2ZnCl4 crystals were calculated as a function of photon energy. The analysis of the spectra behavior of the absorption coefficient in the absorption region revealed indirect transition. The dispersion of the refractive index is discussed in terms of the sin-gle oscillator Wemple-DiDomenico model. The single oscillator energy (E0), the dispersion energy (Ed), the lattice dielectric constant (εL) and the ratio of free charge carrier concentration to the ef-fective mass (N/m*) were estimated. The FTIR spectra were recorded to study the functional groups of the as grown and annealed samples.
文摘The 1-azido-2-chloro-4-nitrobenzene was prepared by nucleophilic substitution between 2-chloro-4-nitro-1-(trifluoromethylsulfinyl)benzene and sodium azide, and its structure was characterized by NMR spectrum and X-ray single-crystal diffraction. It crystallizes in the monoclinic system, space group P21/n, Z = 8 and Mr = 198.57. A cultivation process of the single crystal of unstable aryl azide was provided. The group of trifluoromethyl sulfinyl was found for the first time to be a new excellent leaving group of aromatic nucleophilic substitution reactions.
基金Project supported by National Key Research and Development Plan of China(Grant Nos.2016YFB0400600 and 2016YFB0400601)the National Natural Science Foundation of China(Grant Nos.61574026,11675198,61774072,and 11405017)+2 种基金the Natural Science Foundation of Liaoning Province,China(Grant Nos.201602453 and 201602176)China Postdoctoral Science Foundation Funded Project(Grant No.2016M591434)the Dalian Science and Technology Innovation Fund(Grant No.2018J12GX060)
文摘A solar-blind photodetector is fabricated on single crystal Ga_2O_3 based on vertical structure Schottky barrier diode. A Cu Schottky contact electrode is prepared in a honeycomb porous structure to increase the ultraviolet(UV) transmittance.The quantum efficiency is about 400% at 42 V. The Ga_2O_3 photodetector shows a sharp cutoff wavelength at 259 nm with high solar-blind/visible(= 3213) and solar-blind/UV(= 834) rejection ratio. Time-resolved photoresponse of the photodetector is investigated at 253-nm illumination from room temperature(RT) to 85.8℃. The photodetector maintains a high reversibility and response speed, even at high temperatures.
基金Supported by the National Natural Science Foundation of China under Grant Nos 11190022,11334010 and 11534007the National Basic Research Program of China under Grant No 2015CB921000the Strategic Priority Research Program(B)of Chinese Academy of Sciences under Grant No XDB07020300
文摘We report a reproducible approach in preparing high-quality overdoped Bi2 Sr2 CaCu2 08＋δ （Bi2212） single crystals by annealing Bi2212 crystals in high oxygen pressure followed by a fast quenching. In this way, high-quality overdoped and heavily overdoped Bi2212 single crystals are obtained by controlling the annealing oxygen pressure. We find that, beyond a limit of oxygen pressure that can achieve most heavily overdoped Bi2212 with a Tc N63 K, the annealed Bi2212 begins to decompose. This accounts for the existence of the hole-doping limit and thus the Tc limit in the heavily overdoped region of Bi2212 by the oxygen annealing process. These results provide a reliable way in preparing high-quality overdoped and heavily overdoped Bi2212 crystals that are important for studies of the physical properties, electronic structure and superconductivity mechanism of the cuprate superconductors.
文摘The compound described as [Cu(OH)2(H2O)2(4-C5H4NCOOH)2] in Chin. J. Struct. Chem., 2001, 20: 478-480 is instead the compound [Cu(H2O)4(4-C5H4NCOO)2], whose crystal structure has already been published elsewhere.
基金Supported by the Central University Basic Scientific Research Fund of Hunan University (2009)the Key Scientific and Technological Project of Changsha, Hunan Province (No. 0901077-31)
文摘The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.
基金supported by the National Natural Science Foundation of China(No.31572042)Natural Science Foundation of Heilongjiang Province(B201303)the Research Science Foundation in Technology Innovation of Harbin(No.2015RAYXJ010)
文摘The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS （ESI） and single-crystal X-ray diffraction. （R）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867（2）, b = 8.4087（2）, c = 14.325（6） A^°, β = 117.59（2）°, Z = 4, V = 1266.9（6） A^°3, Dc = 1.307 g/cm^3, F（000） = 528, μ（MoKα） = 0.097 mm-1, R = 0.0453 and wR = 0.1237; （S）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647（17）, b = 8.7034（17）, c = 9.5479（19） A^°, α = 105.33（3）, β = 100.95（3）, γ = 105.14（3）°, Z = 2, V = 614.1（2） A^°3, Dc = 1.348 g/cm^3, F（000） = 264, μ（MoKα） = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.
基金supported by the National Natural Science Foundation of China (50590401)
文摘By using Tb407 and MoO3 as starting materials, ferroelectric Tb2（MoO4）3 crystal was grown by the Czochralski method. The as-grown crystal was pale green color, transparent and crack-free. X-ray powder diffraction （XRPD）, transmission spectrum, dielectric constant and polarization-electric field （P-E） hysteresis loop measurements were performed to characterize the crystal. The XRPD confirmed the as-grown crystal to be Tb2（MoO4）3. The transmission spectrum of the crystal showed that its transmittance in the entire visible and most near-infrared region was more than 70% except for an absorption peak around 486 nm. Obvious dielectric anomaly could be observed at low frequencies with increasing temperature through the dielectric constant measurement and the Curie temperature of Tb2（MoO4）3 crystal was determined to be 162.3℃ The unsaturated P-E hysteresis loops indicated that it was difficult for the ferroelectric domains in Tb2（MoO4）3 crystal to array regularly with repeated switching of the electric field.
文摘Experiments performed on the grwth of mixed crystals of rare earth tartrates (Y1-xSmx)2 (C4H4O6)3.zH2O (0≤x≤1) from silica gels at 35~40℃ and 25~30℃ employing single-diffusion technique. are discussed. The crystals maintain spherulitic morphology, irrespective of the value of x, concentration of upper and lower reactants, gel pH, gel age and gel temperature. Formation Of Liesegang rings in this system is a temperature dependent phenomenon. It is shown that with the increase of the value of x the system passes from Liesegangring phenomenon to singlezone phenomenon. Operative mechanism of crystallization in the higher (35~40℃) and lower temperature ranges (25~30℃) is explained. Seeded growth experiments indicate the possibility of increasing the size of the spherulites in the gel medium
基金supported by the Young Scientists Fund of the National Natural Science Foundation of China (Grant No. 50802105)
文摘The formation of macrostep during high-temperature phase of barium meta-borate （^-BaB204） single crystal growth has been investigated by both optical in-situ observation system and atomic force microscopy （AFM）. The in- si$u observation results demonstrate that the critical linear size of growing facet exceeding the size that the macrostep generates is significantly anisotropic. The critical linear sizes are around 280 ~m and 620 ~m for {1010} and （T010} planes, respectively. AFM study illustrates that macrostep train with a height of 150 nm^200 nm is one typical morphological feature of the as-grown crystal surface. The riser of each macrostep consists of several straight and parallel sub-steps, indicating the occurrence of step bunching. Additionally, triangular sub-steps with heights of several nanometers on the treads of the macrosteps are found to be another typical feature of surface morphology, which implies a microscopically competitive bunching of sub-steps between various crystallographic orientations.
基金supported by the 863 Project (2006 A03Z219)Natural Science Foundation of Jiangsu Province (BK2007199)+2 种基金Foundation for "Liu Da Ren Cai" of Jiangsu Province (06-E-021)State Postdoctoral Foundation of China (No. 2006040932)the Postdoctoral Foundation of Jiangsu Province (No. 0602008B)
文摘The compound （SiCl3）2Fe（CO）4 was synthesized and structurally characterized by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P2 1/n with α = 8.287（2）, b = 9.829（2）, c = 9.042（2） A, β = 96.19（3）°, V= 732.2（3） A^3, C4Cl6FeO4Si2, Mr = 436.77, Z = 2, Dc = 1.981 g/cm^3, F（000） = 424, μ（MoKα） = 2.282 mm^-1, the final R = 0.048 and wR = 0.164 for 1109 observed reflections （I 〉 2σ（I））. The crystal structure of （SiCl3）2Fe（CO）4 reveals that the Si（l）- Fe-Si（l）^a sequence is linear and perpendicular to the Fe（CO）4 cross-shaped plane.
基金Project supported by China National Climbing plan and National Nature Science Foundation
文摘Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.
文摘The title compound, Cs 2[Mg(CO 3) 2(H 2O) 4], was synthesized by the dropwise addition of an aqueous solution of Mg(NO 3) 2 to a stirred aqueous Cs 2CO 3/CsHCO 3 solution. A colorless needle shaped crystal was formed by slow evaporation. The crystal structure was established on the basis of the single crystal X ray diffraction data. Cs 2[Mg(CO 3) 2(H 2O) 4] crystallized in the orthorhombic space group Pbca (No. 61) with a =0.658 4(1) nm, b =1.257 9(1) nm, c =1.301 3(1) nm, \{ V =1.077 8 nm 3, Z =4, D x=2.971 g·cm -3 , μ =69.20 cm -1 , F (000)=888, T =298 K, final R =0.029 and R w=0.024 for 1 037 observed reflections. The crystal consists of Cs + cations and the complex trans [Mg(CO 3) 2(H 2O) 4] 2- anions with each Mg atom coordinated by the six oxygens of two carbonate groups and four water molecules [ d (Mg_O)=0.203 6(4), 0.207 4(4), 0.213 4(4) nm]. The complex trans [Mg(CO 3) 2(H 2O) 4] 2- anions are arranged in a strongly compressed bcc pattern. A 3D network was formed through the intermolecular hydrogen bonds. The Cs + cations are located in cavities, each being surrounded by nine oxygens of five complex anions with d (Cs_O)=0.306 1-0.348 8 nm. The CO 2- 3 group reveals a lowering of D 3h symmetry due to site and coordination effects, but not any observable deviation from co planarity [ d (C_O)=0.127 2(6), 0.127 5(7) , 0.130 5(6) nm and O_C_O=119.6(5)°, 120.1(5)°, 120.4(5)°].
