Diamond crystals were synthesized with different doping proportions of N-H-O at 5.5 GPa-7.1 GPa and 1370℃-1450℃. With the increase in the N-H-O doping ratio, the crystal growth rate decreased, the temperature and pr...Diamond crystals were synthesized with different doping proportions of N-H-O at 5.5 GPa-7.1 GPa and 1370℃-1450℃. With the increase in the N-H-O doping ratio, the crystal growth rate decreased, the temperature and pressure conditions required for diamond nucleation became increasingly stringent, and the diamond crystallization process was affected. [111] became the dominant plane of diamonds;surface morphology became block-like;and growth texture,stacking faults, and etch pits increased. The diamond crystals had a two-dimensional growth habit. Increasing the doping concentration also increased the amount of N that entered the diamond crystals as confirmed via Fourier transform infrared spectroscopy. However, crystal quality gradually deteriorated as verified by the red-shifting of Raman peak positions and the widening of the Raman full width at half maximum. With the increase in the doping ratio, the photoluminescence property of the diamond crystals also drastically changed. The intensity of the N vacancy center of the diamond crystals changed, and several Ni-related defect centers, such as the NE1 and NE3 centers, appeared. Diamond synthesis in N-H-O-bearing fluid provides important information for deepening our understanding of the growth characteristics of diamonds in complex systems and the formation mechanism of natural diamonds, which are almost always N-rich and full of various defect centers. Meanwhile, this study proved that the type of defect centers in diamond crystals could be regulated by controlling the N-H-O impurity contents of the synthesis system.展开更多
By temperature gradient method under high pressure and high temperature (HPHT), with NiMnCo alloy as the solvent metal, at diamond-stable region of about 5.4 GPa and 1500 K, metastable regrown graphite crystals of d...By temperature gradient method under high pressure and high temperature (HPHT), with NiMnCo alloy as the solvent metal, at diamond-stable region of about 5.4 GPa and 1500 K, metastable regrown graphite crystals of different morphology were synthesized. With B as an additive incorporated into the NiMnCo-C system, metastable regrown graphite crystals of sphere-like shape were firstly obtained under HPHT. If the growth system does not contain B, sheet-like regrown graphite crystals, most with regular hexagonal morphology, are grown upwards and standing vertically in the metal solvent. When B additive of 1.0 wt pct was added into carbon source (graphite powder), all metastable regrown graphite crystals took on the habit of regular sphere-like morphology, and were grown by a spiral layer growth mechanism.展开更多
For the growth of large synthetic diamond crystals by temperature gradient method (TGM), the grit sizes of seed crystals have great effects on the growth rate and quality of large grown crystals. Because of the limi...For the growth of large synthetic diamond crystals by temperature gradient method (TGM), the grit sizes of seed crystals have great effects on the growth rate and quality of large grown crystals. Because of the limited area of seed surfaces, the maximum diffusion flux of carbon source, which could be absorbed by the seed, is related to the seed size. And with increasing the seed sizes, the growth rates also increase markedly. However, the seed sizes should be lower than a certain value, which determines the crystal quality directly. For example, with NiMnCo alloy as the metal solvent, when the seed size increases from 0.5 to 1.8 mm, the growth rate increases greatly from about 1.1 to 3.2 mg/h; when the size is beyond 2.0 mm, more and more metal inclusions would be incorporated into the grown crystals, and the crystal quality is destroyed heavily. Finite element analysis (FEA) shows that, due to the special assembly of growth cell, the diffusion of carbon source in the metal solvent is very inhomogeneous, which could be substantiated directly by the appearances and shapes of large grown crystals and the remains of carbon source. And this inhomogeneous diffusion of carbon source would be very harmful to the growth of large diamond crystals, especially when large-size seed crystals are used.展开更多
The temperature in the high-pressure high-temperature(HPHT) synthesis is optimized to enhance the thermoelectric properties of high-density Zn O ceramic, Zn_(0.98)Al_(0.02)O. X-ray diffraction, scanning electron micro...The temperature in the high-pressure high-temperature(HPHT) synthesis is optimized to enhance the thermoelectric properties of high-density Zn O ceramic, Zn_(0.98)Al_(0.02)O. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy show that HPHT can be utilized to control the crystal structure and relative density of the material.High pressure can be utilized to change the energy band structure of the samples via changing the lattice constant of samples, which decreases the thermal conductivity due to the formation of a multi-scale hierarchical structure and defects. The electrical conductivity of the material reaches 6×10^(4) S/m at 373 K, and all doped samples behave as n-type semiconductors. The highest power factor(6.42 μW·cm^(-1)·K^(-2)) and dimensionless figure of merit(z T = 0.09) are obtained when Zn_(0.98)Al_(0.02)O is produced at 973 K using HPHT, which is superior to previously reported power factors for similar materials at the same temperature. Hall measurements indicate a high carrier concentration, which is the reason for the enhanced electrical performance.展开更多
By doping titanium hydride(TiH2) into boron carbide(B4C), a series of B4C + x wt% TiH2(x = 0, 5, 10, 15, and 20)composite ceramics were obtained through spark plasma sintering(SPS). The effects of the sintering temper...By doping titanium hydride(TiH2) into boron carbide(B4C), a series of B4C + x wt% TiH2(x = 0, 5, 10, 15, and 20)composite ceramics were obtained through spark plasma sintering(SPS). The effects of the sintering temperature and the amount of TiH2 additive on the microstructure, mechanical and electrical properties of the sintered B4C-TiB2 composite ceramics were investigated. Powder mixtures of B4C with 0–20 wt% TiH2 were heated from 1400℃ to 1800℃ for 20 min under 50 MPa. The results indicated that higher sintering temperatures contributed to greater ceramic density. With increasing TiH2 content, titanium diboride(TiB2) formed between the TiH2 and B4C matrix. This effectively improved Young’s modulus and fracture toughness of the composite ceramics, significantly improving their electrical properties: the electrical conductivity reached 114.9 S·cm-1 at 1800℃ when x = 20. Optimum mechanical properties were obtained for the B4C ceramics sintered with 20 wt% TiH2, which had a relative density of 99.9±0.1%, Vickers hardness of 31.8 GPa,and fracture toughness of 8.5 MPa·m1/2. The results indicated that the doping of fine Ti particles into the B4C matrix increased the conductivity and the fracture toughness of B4C.展开更多
Phase transition generates rapid changes of transport parameters and poor mechanical property,and thus restricts the application of thermoelectric materials.AgBiSe_(2) exhibits cubic phase at above 580 K with high-sym...Phase transition generates rapid changes of transport parameters and poor mechanical property,and thus restricts the application of thermoelectric materials.AgBiSe_(2) exhibits cubic phase at above 580 K with high-symmetry structure and low lattice thermal conductivity,indicating the potentiality of high thermoelectric performances.In this work,the cubic structure of AgBiSe_(2) was achieved at ambient conditions by alloying with PbS,enhancing the configurational entropy at both cationic and anionic sites.The cubic structure was rather stable after several measurement cycles.Nb substitution at cationic sites effectively reduced band gap,and increased both carrier concentration and effective mass.All samples exhibited relatively low lattice thermal conductivity(0.68-0.34 W/(m·K))in the temperature range of 300-773 K,due to the nanoscale inhomogeneity and the random distribution of multiple species at some atomic sites.A maximum zT of 0.65 at 773 K was obtained for(Ag_(0.99)Nb_(0.01)BiSe_(2))_(0.8)(PbS)_(0.2) sample.The entropy-driven structural stabilization is a promising strategy to achieve stable structure for practical thermoelectric applications.展开更多
We present the work about the initiative fabrication of multi-scale hierarchical TiO2-x by our strategy,combining high pressure and high temperature(HPHT)reactive sintering with appropriate ratio of coarse Ti to nanos...We present the work about the initiative fabrication of multi-scale hierarchical TiO2-x by our strategy,combining high pressure and high temperature(HPHT)reactive sintering with appropriate ratio of coarse Ti to nanosized TiO_(2).Ubiquitous lattice defects engineering has also been achieved in our samples by HPHT.The thermoelectric performance was significantly enhanced,and rather low thermal conductivity(1.60 W m^(-1)K^(-1))for titanium oxide was reported here for TiO1.76.Correspondingly,a high dimensionless figure of merit(zT)up to 0.33 at 700℃was realized in it.As far as we know,this value is an enhancement of 43%of the ever best result about nonstoichiometric TiO_(2)and the result is also exciting for oxide thermoelectric materials.The moderate power factor,the significantly reduced thermal conductivity and the remarkable synergy between electrical properties and thermal conductivity are responsible for the excellent thermoelectric performance.We develop a facile strategy for preparing multi-scale hierarchical TiO_(2-x)and its superior ability to optimize thermoelectric performance has been demonstrated here.展开更多
Due to elimination of horizontal and vertical tails,flying wing aircraft has poor longitudinal and directional dynamic characteristics.In addition,flying wing aircraft uses drag rudders for yaw control,which tends to ...Due to elimination of horizontal and vertical tails,flying wing aircraft has poor longitudinal and directional dynamic characteristics.In addition,flying wing aircraft uses drag rudders for yaw control,which tends to generate strong three-axis control coupling.To overcome these problems,a flight control law design method that couples the longitudinal axis with the lateraldirectional axes is proposed.First,the three-axis coupled control augmentation structure is specified.In the structure,a‘‘soft/hard"cross-connection method is developed for three-axis dynamic decoupling and longitudinal control response decoupling from the drag rudders;maneuvering turn angular rate estimation and subtraction are used in the yaw axis to improve the directional damping.Besides,feedforward control is adopted to improve the maneuverability and control decoupling performance.Then,detailed design methods for feedback and feedforward control parameters are established using eigenstructure assignment and model following technique.Finally,the proposed design method is evaluated and compared with conventional method by numeric simulations.The influences of control derivatives variation of drag rudders on the method are also analyzed.It is demonstrated that the method can effectively improve the dynamic characteristics of flying wing aircraft,especially the directional damping characteristics,and decouple the longitudinal responses from the drag rudders.展开更多
Bulk materials Ba_(8)Ga_(16)In_(x)Ge_(30-x)(x=0.5,1.0,1.5)were prepared by High-Pressure and High-Temperature(HPHT)method and the crystal structure has been confirmed by X-ray diffraction and cell refinement.The actua...Bulk materials Ba_(8)Ga_(16)In_(x)Ge_(30-x)(x=0.5,1.0,1.5)were prepared by High-Pressure and High-Temperature(HPHT)method and the crystal structure has been confirmed by X-ray diffraction and cell refinement.The actual In composition was much lower than the starting composition,and lattice constants increased with the increase of substitution.As the temperature increased,the Seebeck coefficient and electrical resistivity increased first and then decreased,while the thermal conductivity was the opposite,which leads to significant enhancement on thermoelectric properties of the clathrates.The substitution of indium elements decreased the seebeck coefficient and electrical resistivity,and also changed the microstructure of the compounds.A minimum thermal conductivity of 0.84Wm^(-1)1K^(-1)was obtained,and a good ZT value of 0.52 was achieved.The grain boundaries and lattice defects generated by high pressure can effectively scatter phonons of different frequencies,which reduce the lattice thermal conductivity.展开更多
Polycrystalline Cu_(2)Se bulk materials were synthesized by high-pressure and high-temperature(HPHT)technique.The effects of synthetic temperature and pressure on the thermoelectric properties of Cu_(2)Se materials we...Polycrystalline Cu_(2)Se bulk materials were synthesized by high-pressure and high-temperature(HPHT)technique.The effects of synthetic temperature and pressure on the thermoelectric properties of Cu_(2)Se materials were investigated.The results indicate that both synthetic temperature and pressure determine the microstructure and thermoelectric performance of Cu2Se compounds.The increase of synthetic temperature can effectively enhance the electrical conductivity and decrease the lattice thermal conductivity.A two-fold improvement in the power factor is obtained at synthetic temperature of 1000℃ compared to that obtained at room temperature.All b-Cu2Se samples exhibit low and temperatureindependent lattice thermal conductivity ranging from 0.3 to 0.5 Wm^(-1)K^(-1) due to the intrinsic superionic feature and the abundant lattice defects produced at high pressure.A maximum zT of 1.19 at 723 K was obtained for the sample synthesized at 3 GPa and 1000℃.These findings indicate that HPHT technology is an efficient approach to synthesize Cu_(2)Se-based bulk materials.展开更多
基金Project supported by the National Natural Science Foundation of China (Grant Nos. 51772120, 11604246, 51872112, and 11804305)the Project of Jilin Science and Technology Development Plan (Grant No. 20180201079GX)+1 种基金the Fundamental Research Funds for the Central Universities, the Natural Science Foundation of Chongqing, China (Grant No. cstc2019jcyj-msxm X0391)the Science and Technology Research Program of Chongqing Municipal Education Commission (Grant No. KJQN201901405)。
文摘Diamond crystals were synthesized with different doping proportions of N-H-O at 5.5 GPa-7.1 GPa and 1370℃-1450℃. With the increase in the N-H-O doping ratio, the crystal growth rate decreased, the temperature and pressure conditions required for diamond nucleation became increasingly stringent, and the diamond crystallization process was affected. [111] became the dominant plane of diamonds;surface morphology became block-like;and growth texture,stacking faults, and etch pits increased. The diamond crystals had a two-dimensional growth habit. Increasing the doping concentration also increased the amount of N that entered the diamond crystals as confirmed via Fourier transform infrared spectroscopy. However, crystal quality gradually deteriorated as verified by the red-shifting of Raman peak positions and the widening of the Raman full width at half maximum. With the increase in the doping ratio, the photoluminescence property of the diamond crystals also drastically changed. The intensity of the N vacancy center of the diamond crystals changed, and several Ni-related defect centers, such as the NE1 and NE3 centers, appeared. Diamond synthesis in N-H-O-bearing fluid provides important information for deepening our understanding of the growth characteristics of diamonds in complex systems and the formation mechanism of natural diamonds, which are almost always N-rich and full of various defect centers. Meanwhile, this study proved that the type of defect centers in diamond crystals could be regulated by controlling the N-H-O impurity contents of the synthesis system.
基金supported by the National Natural Science Foundation of China under grant No.50172018the Foundation of He nan Educational Committee undergrant No.2009A430014the Open Research Fund Program of State Key Laboratory of Superhard Materials of Jilin University under grant No.200801
文摘By temperature gradient method under high pressure and high temperature (HPHT), with NiMnCo alloy as the solvent metal, at diamond-stable region of about 5.4 GPa and 1500 K, metastable regrown graphite crystals of different morphology were synthesized. With B as an additive incorporated into the NiMnCo-C system, metastable regrown graphite crystals of sphere-like shape were firstly obtained under HPHT. If the growth system does not contain B, sheet-like regrown graphite crystals, most with regular hexagonal morphology, are grown upwards and standing vertically in the metal solvent. When B additive of 1.0 wt pct was added into carbon source (graphite powder), all metastable regrown graphite crystals took on the habit of regular sphere-like morphology, and were grown by a spiral layer growth mechanism.
基金supported by the National Natural Science Foundation of China under grant No.50172018.
文摘For the growth of large synthetic diamond crystals by temperature gradient method (TGM), the grit sizes of seed crystals have great effects on the growth rate and quality of large grown crystals. Because of the limited area of seed surfaces, the maximum diffusion flux of carbon source, which could be absorbed by the seed, is related to the seed size. And with increasing the seed sizes, the growth rates also increase markedly. However, the seed sizes should be lower than a certain value, which determines the crystal quality directly. For example, with NiMnCo alloy as the metal solvent, when the seed size increases from 0.5 to 1.8 mm, the growth rate increases greatly from about 1.1 to 3.2 mg/h; when the size is beyond 2.0 mm, more and more metal inclusions would be incorporated into the grown crystals, and the crystal quality is destroyed heavily. Finite element analysis (FEA) shows that, due to the special assembly of growth cell, the diffusion of carbon source in the metal solvent is very inhomogeneous, which could be substantiated directly by the appearances and shapes of large grown crystals and the remains of carbon source. And this inhomogeneous diffusion of carbon source would be very harmful to the growth of large diamond crystals, especially when large-size seed crystals are used.
基金Project supported by the National Natural Science Foundation of China(Grant No.51171070)the Project of Jilin Science and Technology Development Plan,China(Grant No.20170101045JC)。
文摘The temperature in the high-pressure high-temperature(HPHT) synthesis is optimized to enhance the thermoelectric properties of high-density Zn O ceramic, Zn_(0.98)Al_(0.02)O. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy show that HPHT can be utilized to control the crystal structure and relative density of the material.High pressure can be utilized to change the energy band structure of the samples via changing the lattice constant of samples, which decreases the thermal conductivity due to the formation of a multi-scale hierarchical structure and defects. The electrical conductivity of the material reaches 6×10^(4) S/m at 373 K, and all doped samples behave as n-type semiconductors. The highest power factor(6.42 μW·cm^(-1)·K^(-2)) and dimensionless figure of merit(z T = 0.09) are obtained when Zn_(0.98)Al_(0.02)O is produced at 973 K using HPHT, which is superior to previously reported power factors for similar materials at the same temperature. Hall measurements indicate a high carrier concentration, which is the reason for the enhanced electrical performance.
基金Project supported by the National Natural Science Foundation of China(Grant Nos.11704340 and 11804305)the Scientific and Technology Project in Henan Province,China(Grant No.202102210198).
文摘By doping titanium hydride(TiH2) into boron carbide(B4C), a series of B4C + x wt% TiH2(x = 0, 5, 10, 15, and 20)composite ceramics were obtained through spark plasma sintering(SPS). The effects of the sintering temperature and the amount of TiH2 additive on the microstructure, mechanical and electrical properties of the sintered B4C-TiB2 composite ceramics were investigated. Powder mixtures of B4C with 0–20 wt% TiH2 were heated from 1400℃ to 1800℃ for 20 min under 50 MPa. The results indicated that higher sintering temperatures contributed to greater ceramic density. With increasing TiH2 content, titanium diboride(TiB2) formed between the TiH2 and B4C matrix. This effectively improved Young’s modulus and fracture toughness of the composite ceramics, significantly improving their electrical properties: the electrical conductivity reached 114.9 S·cm-1 at 1800℃ when x = 20. Optimum mechanical properties were obtained for the B4C ceramics sintered with 20 wt% TiH2, which had a relative density of 99.9±0.1%, Vickers hardness of 31.8 GPa,and fracture toughness of 8.5 MPa·m1/2. The results indicated that the doping of fine Ti particles into the B4C matrix increased the conductivity and the fracture toughness of B4C.
基金supported by the National Natural Science Foundation of China(Nos.12004342,12274372,12274373,12204419,12104408,12004341)the Scientific and technological Project in Henan Province of China(Nos.222102230018 and 232102231052).
文摘Phase transition generates rapid changes of transport parameters and poor mechanical property,and thus restricts the application of thermoelectric materials.AgBiSe_(2) exhibits cubic phase at above 580 K with high-symmetry structure and low lattice thermal conductivity,indicating the potentiality of high thermoelectric performances.In this work,the cubic structure of AgBiSe_(2) was achieved at ambient conditions by alloying with PbS,enhancing the configurational entropy at both cationic and anionic sites.The cubic structure was rather stable after several measurement cycles.Nb substitution at cationic sites effectively reduced band gap,and increased both carrier concentration and effective mass.All samples exhibited relatively low lattice thermal conductivity(0.68-0.34 W/(m·K))in the temperature range of 300-773 K,due to the nanoscale inhomogeneity and the random distribution of multiple species at some atomic sites.A maximum zT of 0.65 at 773 K was obtained for(Ag_(0.99)Nb_(0.01)BiSe_(2))_(0.8)(PbS)_(0.2) sample.The entropy-driven structural stabilization is a promising strategy to achieve stable structure for practical thermoelectric applications.
基金This work was supported by the National Natural Science Foundation of China(Grant No.51171070)the Project of Jilin Science and Technology Development Plan(20170101045JC)Graduate Innovation Fund of Jilin University(Project No.2016065).
文摘We present the work about the initiative fabrication of multi-scale hierarchical TiO2-x by our strategy,combining high pressure and high temperature(HPHT)reactive sintering with appropriate ratio of coarse Ti to nanosized TiO_(2).Ubiquitous lattice defects engineering has also been achieved in our samples by HPHT.The thermoelectric performance was significantly enhanced,and rather low thermal conductivity(1.60 W m^(-1)K^(-1))for titanium oxide was reported here for TiO1.76.Correspondingly,a high dimensionless figure of merit(zT)up to 0.33 at 700℃was realized in it.As far as we know,this value is an enhancement of 43%of the ever best result about nonstoichiometric TiO_(2)and the result is also exciting for oxide thermoelectric materials.The moderate power factor,the significantly reduced thermal conductivity and the remarkable synergy between electrical properties and thermal conductivity are responsible for the excellent thermoelectric performance.We develop a facile strategy for preparing multi-scale hierarchical TiO_(2-x)and its superior ability to optimize thermoelectric performance has been demonstrated here.
基金supported by the Fundamental Research Funds for the Central Universities of China(No.:YWF-19-BJ-J-322)。
文摘Due to elimination of horizontal and vertical tails,flying wing aircraft has poor longitudinal and directional dynamic characteristics.In addition,flying wing aircraft uses drag rudders for yaw control,which tends to generate strong three-axis control coupling.To overcome these problems,a flight control law design method that couples the longitudinal axis with the lateraldirectional axes is proposed.First,the three-axis coupled control augmentation structure is specified.In the structure,a‘‘soft/hard"cross-connection method is developed for three-axis dynamic decoupling and longitudinal control response decoupling from the drag rudders;maneuvering turn angular rate estimation and subtraction are used in the yaw axis to improve the directional damping.Besides,feedforward control is adopted to improve the maneuverability and control decoupling performance.Then,detailed design methods for feedback and feedforward control parameters are established using eigenstructure assignment and model following technique.Finally,the proposed design method is evaluated and compared with conventional method by numeric simulations.The influences of control derivatives variation of drag rudders on the method are also analyzed.It is demonstrated that the method can effectively improve the dynamic characteristics of flying wing aircraft,especially the directional damping characteristics,and decouple the longitudinal responses from the drag rudders.
基金This workwas financially supported by National Natural Science Foundation of China(51171070)the Project of Jilin Science and Technology Development Plan(20170101045JC).
文摘Bulk materials Ba_(8)Ga_(16)In_(x)Ge_(30-x)(x=0.5,1.0,1.5)were prepared by High-Pressure and High-Temperature(HPHT)method and the crystal structure has been confirmed by X-ray diffraction and cell refinement.The actual In composition was much lower than the starting composition,and lattice constants increased with the increase of substitution.As the temperature increased,the Seebeck coefficient and electrical resistivity increased first and then decreased,while the thermal conductivity was the opposite,which leads to significant enhancement on thermoelectric properties of the clathrates.The substitution of indium elements decreased the seebeck coefficient and electrical resistivity,and also changed the microstructure of the compounds.A minimum thermal conductivity of 0.84Wm^(-1)1K^(-1)was obtained,and a good ZT value of 0.52 was achieved.The grain boundaries and lattice defects generated by high pressure can effectively scatter phonons of different frequencies,which reduce the lattice thermal conductivity.
基金the National Natural Science Foundation of China(No.11704340,11804305 and 51171070)the Project of Jilin Science and Technology Development Plan(Project No.20170101045JC)+1 种基金the China Postdoctoral Science Foundation(No.2017M620303 and 2017M622360)the Key Research Project of Higher Education Institution of Henan Province(No.19A140006).
文摘Polycrystalline Cu_(2)Se bulk materials were synthesized by high-pressure and high-temperature(HPHT)technique.The effects of synthetic temperature and pressure on the thermoelectric properties of Cu_(2)Se materials were investigated.The results indicate that both synthetic temperature and pressure determine the microstructure and thermoelectric performance of Cu2Se compounds.The increase of synthetic temperature can effectively enhance the electrical conductivity and decrease the lattice thermal conductivity.A two-fold improvement in the power factor is obtained at synthetic temperature of 1000℃ compared to that obtained at room temperature.All b-Cu2Se samples exhibit low and temperatureindependent lattice thermal conductivity ranging from 0.3 to 0.5 Wm^(-1)K^(-1) due to the intrinsic superionic feature and the abundant lattice defects produced at high pressure.A maximum zT of 1.19 at 723 K was obtained for the sample synthesized at 3 GPa and 1000℃.These findings indicate that HPHT technology is an efficient approach to synthesize Cu_(2)Se-based bulk materials.