This paper adopted the hydrothermal method to prepare tungsten oxide(WO_(3))nanorod films and studied the effects of precursor solution concentration(0.02,0.03,0.06 mol/L peroxytungstic acid)and annealing temperature(...This paper adopted the hydrothermal method to prepare tungsten oxide(WO_(3))nanorod films and studied the effects of precursor solution concentration(0.02,0.03,0.06 mol/L peroxytungstic acid)and annealing temperature(200,300,400℃)on their electrochromic properties.The microstructure characterization of WO_(3) films were performed using scanning electron microscope(SEM),X-ray diffraction(XRD),and transmission electron microscope(TEM),and their electrochromic properties were tested by combining an electrochemical workstation with an ultraviolet-visible spectrophotometer.The results showed that the precursor solution concentration directly affected the thickness(290,560,990 nm)and microstructure of WO_(3) films,significantly impacting their electrochromic properties.However,the annealing temperature had a negligible effect.As the precursor solution concentration increased,the optical modulation of WO_(3) films gradually decreased,reaching 51.1%,43.8%,and 35.1%,respectively.The switching time first increased and then stabilized,with coloring times of 7.3,7.7,and 7.7 s,respectively,and bleaching times of 3.8,6.5,and 6.5 s,respectively.The coloration efficiency gradually increased but the increase was relatively small,reaching 41.8,44.4,and 44.8 cm^(2)/C,respectively.Moreover,the cycling stability of WO_(3) films was poor,with the ratios of the final value of optical modulation to the initial value 0.33,0.26,and 0.34,respectively.Additionally,there were bigger differences in the bleached state transmittance,while the colored state transmittance showed smaller variations.However,the former has better cycling stability than the latter.In summary,to obtain better electrochromic properties,the thickness of WO_(3) films should not exceed 290 nm.展开更多
ZnO is a highly significant II-VI semiconductor known for its excellent optoelectronic properties,making it widely applicable and promising for use in light-emitting devices,solar cells,lasers,and photodetectors.The m...ZnO is a highly significant II-VI semiconductor known for its excellent optoelectronic properties,making it widely applicable and promising for use in light-emitting devices,solar cells,lasers,and photodetectors.The methods for preparing ZnO are diverse,and among them,the hydrothermal method is favored for its simplicity,ease of operation,and low cost,making it an optimal choice for ZnO single-crystal growth.Most studies investigating the effects of different hydrothermal experimental parameters on the morphology and performance of ZnO nano-materials typically focus on only 2—3 variable parameters,with few examining the impact of all possible experimental parameter changes on ZnO nano-mate-rials.The principles of the hydrothermal method and its advantages in nano-material preparation were briefly introduced in this article.The detailed discussion on the influence of various experimental parameters on the preparation of ZnO nano-materials was provided,which including reaction materials,Zn^(2+)/OH^(-)ratio,reaction time and temperature,additives,experimental equipment,and annealing conditions.The review co-vers how different experimental parameters affect the morphology and performance of the materials,as well as how different rare earth doping elements influence the performance of ZnO nano-materials.It is hoped that this work will contribute to future research on the hydrothermal synthesis of nano-materials.展开更多
The fly ash from waste incineration poses a serious threat to human health due to its high content of dioxins.Hydrothermal treatment is an efficient and clean method on the decomposition and detoxifying of fly ash.To ...The fly ash from waste incineration poses a serious threat to human health due to its high content of dioxins.Hydrothermal treatment is an efficient and clean method on the decomposition and detoxifying of fly ash.To study the degradation mechanism of dioxins,this paper uses molecular dynamics(MD)to simulate the hydrothermal reaction process of polychlorinated dibenzo-p-dioxins(PCDDs)under different conditions,and the degradation mechanism of PCDDs is obtained.The results show that the degradation of PCDDs includes two pathways:the first pathway is the substitution of Cl groups by hydroxyl groups to form low-chlorine substitution products through direct hydrogenation,and the second pathway is the formation of non-toxic benzene ring structures accompanied by the cleavage of C—O bonds.The two degradation pathways of PCDDs well explain the changes in toxicity before and after the hydrothermal treatment of fly ash,which is consistent with experimental results.This study provides theoretical guidance for the harmless treatment process of fly ash via hydrothermal method.展开更多
High purity ZrSiO4 powders were prepared using zirconium oxychloride and tetraethoxysilane as raw materials by the microwave-hydrothermal method at 160-200 ℃ for 30 min, in which NaF was added as mineralizer to promo...High purity ZrSiO4 powders were prepared using zirconium oxychloride and tetraethoxysilane as raw materials by the microwave-hydrothermal method at 160-200 ℃ for 30 min, in which NaF was added as mineralizer to promote the crystallization of zircon. The phase composition and microstructure of synthesized ZrSiO4 powders were investigated in detail. The results show that: the microwave-hydrothermal method greatly reduces the synthesis temperature of ZrSiO4 to 160 ℃, 30 min. The synthesized ZrSiO4 powders have small particle size and high stability up to 950 ℃. The synthesis mechanism of ZrSiO4 by microwave hydrothermal s process was also discussed.展开更多
SnO2 nanoparticles with the average particle size of 5-30 nm were synthesized using SnCl4·5H2O as the precursor and NH3·H2O as the mineralizing agent by hydrothermal method.In the case of 1 kg/batch producti...SnO2 nanoparticles with the average particle size of 5-30 nm were synthesized using SnCl4·5H2O as the precursor and NH3·H2O as the mineralizing agent by hydrothermal method.In the case of 1 kg/batch production,the effects of synthesis conditions including solution concentration,reaction temperature,pressure,time and pH value on the grain size,particle morphology and crystal structure of SnO2 were systematically studied.The particles were characterized by X-ray diffraction（XRD） and transmission electron microscopy（TEM）.The results show that,the particle size can be well controlled in the range of 5-30 nm by adjusting the processing parameters such as reaction temperature and time when the crystal structure and particle morphology remain unchanged.The previous reports,the unusual dependences of the grain size of SnO2 on reaction temperature and time were found.The mechanism for such abnormal grain growth behavior was tentatively elucidated.展开更多
Fluorescence imaging techniques represent essential tools in in vitro,preclinical,and clinical studies.In this study,an improved one-step hydrothermal method to synthesize citric acid(CA)modifiedα-NaYbF_(4):2%Er^(3+)...Fluorescence imaging techniques represent essential tools in in vitro,preclinical,and clinical studies.In this study,an improved one-step hydrothermal method to synthesize citric acid(CA)modifiedα-NaYbF_(4):2%Er^(3+)nanocrystals was proposed.The introduction of various doping ions into NaYbF_(4):2%Er^(3+)and the different valence states of the same ions affect both the crystal size and upconversion luminesce nce.There fore,we investigated the upconversion luminesce nce enha ncement of NaYbF_(4):2%Er^(3+)by ion doping and find that the upconversion luminescence intensity of the upconversion nanoparticles(UCNPs)co-doped with 5 mol%Fe^(2+)ions shows the greatest enhancement,especially for red emission at654 nm.Furthermore,HeLa cells incubated with UCNPs allow for imaging with strong red upconversion emission detectio n.Confocal laser scanning microscope(CLSM)fluorescent images of HeLa cells indicate that NaYbF_(4):2%Er/5%Fe^(2+)leads to a clear outline and improves visualization of the cell morphology.In addition,the CA coated NaYbF_(4):2%Er^(3+)/5%Fe^(2+)nanoparticles and NaYbF_(4):2%Er^(3+)/5%Fe^(2+)show low cytotoxicity in HeLa cells.Organ imaging reveals the efficiency of these UCNPs to analyze the lungs,liver,and spleen.Together,these results indicate that the Cit-NaYbF_(4):2%Er^(3+)/5%Fe^(2+)UCNPs are efficient nanoprobes for fluorescence molecular to mography.展开更多
Hydrothermal method was used to synthesize nanoscale particles of MnZn ferrites. The crystallites were characterized by XRD, TEM and SEM. The effects of the reaction time, temperature and additives on the product were...Hydrothermal method was used to synthesize nanoscale particles of MnZn ferrites. The crystallites were characterized by XRD, TEM and SEM. The effects of the reaction time, temperature and additives on the product were investigated. Crystallization process would be carried out above 160 ℃ for 5 h or more, higher temperature can reduce the reaction time. Additives were used to remove impurities such as Fe 2O 3, ZnMnO 3.10～15 nm pure slightly agglomerated MnZn ferrite crystallites with a narrow grain size distribution were obtained.展开更多
LiCoPO4 micron-rods with an average diameter of about 500 nm and length of about 5 μm were synthesized by dispersant-aided hydrothermal method. Poly(n-vinylpyrrolidone) (PVP) was used as dispersant in the hydrotherma...LiCoPO4 micron-rods with an average diameter of about 500 nm and length of about 5 μm were synthesized by dispersant-aided hydrothermal method. Poly(n-vinylpyrrolidone) (PVP) was used as dispersant in the hydrothermal method. The starting solution and the concentration of dispersant have significant influences on the morphology of LiCoPO4,and the electrochemical performance is improved via controlling the particle size and morphology by the hydrothermal method. The cell using smaller particle LiCoPO4 as cat...展开更多
pH value is a key factor in the preparation of nano-sized TiO2 with hydrothermal method. Using Ti（SO4）2 as the titanium source, H2O2 as the complexing agent, NaOH and HCl as the pH value regulator, nano- sized TiO2 ...pH value is a key factor in the preparation of nano-sized TiO2 with hydrothermal method. Using Ti（SO4）2 as the titanium source, H2O2 as the complexing agent, NaOH and HCl as the pH value regulator, nano- sized TiO2 powder with various morphologies and sizes was synthesized. Changes in morphology, size and phase type with pH values of samples were characterized by X-ray diffraction （XRD） and transmission electron micro- scopy （TEM） measurements. Results show that under the present preparation conditions, TiO2 powder is an anatase phase with pH value less than 11, but is more likely to be a brookite phase with pH value more than 11. With the increase in pH value from 1 to 11 in hydrothermal envi- ronment, nano-sized anatase TiO2 gradually grows up in all directions. {001 }, { 101 } and { 100} groups of crystal plane are the exposed crystal planes of nano-sized anatase TiO2 for the （004）, （101） and （200） facets found in high-reso- lution TEM image. The photocatalytic performance of nano-sized TiO2 with different morphologies was com- pared by measuring their photocatalytic degradation rates for methylene blue under ultraviolet light. Results show that anatase TiO2 prepared under the alkalescenthydrothermal environment （pH = 9, 11） has a better pho- tocatalytic degrading performance. Different sizes and phases of nanoscaled TiO2 powders with different photo- catalytic performances can be prepared by the control of pH value of hydrothermal solutions.展开更多
Nanocrystal of upconversion （UC） phosphor Ho^3＋, Tm^3＋ , and Yb^3＋ co-doped NaYF4 was prepared by the hydrothermal method in the presence of the complexing agent EDTA. Under 980 nm diode laser excitation, the imp...Nanocrystal of upconversion （UC） phosphor Ho^3＋, Tm^3＋ , and Yb^3＋ co-doped NaYF4 was prepared by the hydrothermal method in the presence of the complexing agent EDTA. Under 980 nm diode laser excitation, the impact of different concentrations of Ho^3＋ ion on the UC luminescence intensity was discussed. The law of luminescence intensity versus pump power shows that the 474 nm blue emission, 538 nm green emission, and 642 nm red emission are all due to the two-photon process, while the 450 nm blue emission is a three-photon process. The UC mechanism and processes were also analyzed. The sample was characterized by transmission electron microscopy （TEM） and X-ray diffraction （XRD）. The result shows that Ho^3＋ ,Tm^3＋ , and Yb^3＋ co-doped NaYF4 prepared by the hydrothermal method exhibits a hexagonal nanocrystal.展开更多
In this paper,the TiO_2 nanotubes were synthesized by hydrothermal method using a 10 mol/L NaOH aqueous solution at 150℃. The structure of prepared materials was characterized by X-ray diffraction（XRD）,transmission...In this paper,the TiO_2 nanotubes were synthesized by hydrothermal method using a 10 mol/L NaOH aqueous solution at 150℃. The structure of prepared materials was characterized by X-ray diffraction（XRD）,transmission electron microscopy（TEM）. scanning electron microscope（SEM） and Brunauer-Emmett-Teller（BET）.The prepared TiO_2 nanotubes were used to prepare thick film gas sensors and the gas sensing properties to various gases were tested.Results show the prepared TiO_2 nanotube gas sensors responses to ethanol under dry condition at 450℃.This could be attributed to the fact that it had high porous morphology and a higher pore volume,which can promote the diffusion of ethanol deep inside the films and improve the sensor response. Moreover,the gas sensor made with nanotubes exhibit high selective response towards ethanol gas compared with H_2,CO,acetone.展开更多
The semiconductor TiO_(2)is the most important photocatalyst for the degradation of pollutants.Anatase TiO_(2)has a large band gap of 3.2 eV that requires powerful UV light to initiate the photocatalytic reactions.Man...The semiconductor TiO_(2)is the most important photocatalyst for the degradation of pollutants.Anatase TiO_(2)has a large band gap of 3.2 eV that requires powerful UV light to initiate the photocatalytic reactions.Many modifịcation methods such as metal ion doping,composite semiconductors and metal layer modification have been used to extend the light absorption of the catalyst to the visible light region but have little effect[1~4].Surface sensitization with dyes[5]is not practical in application as most dyes self-degrade easily.Therefore,the preparation of TiO_(2)with good wavelength response in the visible light region and high photocatalytic activity for pollutant degradation using natural sunlight is an important goal in TiO_(2)photocatalysis.展开更多
Highly dispersed carbon microspheres(CMSs)derived from D-xylose were successfully synthesized under hydrothermal conditions and followed by further carbonization,in which F127 was used as a soft template.As-synthesize...Highly dispersed carbon microspheres(CMSs)derived from D-xylose were successfully synthesized under hydrothermal conditions and followed by further carbonization,in which F127 was used as a soft template.As-synthesized products were characterized by scanning electron microscopy(SEM),transmission electron microscopy(TEM),flourier transform infrared spectroscopy(FT-IR),thermal gravimetric(TG)and X-ray diffraction(XRD).The results showed that the morphology and structure of the CMSs prominently depended on the stirring speed during hydrothermal reaction.The resultant CMSs principally had non-porous structure without stirring and had a very smooth surface.When the stirring speed increased to 200 rpm,the synthesized mesoporous carbon microspheres at 220?C for 24 h(CMSs-5)had a uniform size distribution of 1–1.4μm and a specific surface area of 452 m^2/g.Nevertheless,with further increasing to 400 rpm,as-fabricated carbon products were mostly amorphous with a low degree of sphericity.Results demonstrated that the diameter of the products decreased with the increase of stirring speed.Furthermore,the sphericity product yield of CMSs reduced with the increase of stirring speed.XRD result showed that all the obtained samples contained partial graphite phase.In addition,a formation mechanism was proposed that involved polymerization product as the precursors for microsphere formation.The controllable and green strategy may provide a great convenience to study properties and applications of carbon microspheres.展开更多
NaTaONcatalysts were synthesized by a hydrothermal（H） and a solid-state（S） methods in this study.The H-and S-NaTaONsamples were characterized by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, trans...NaTaONcatalysts were synthesized by a hydrothermal（H） and a solid-state（S） methods in this study.The H-and S-NaTaONsamples were characterized by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, transmission electron microscopy（TEM）, UV–visible（UV–vis） diffuse reflectance spectroscopy, and photoluminescence（PL） spectroscopy. The XRD patterns of the H-and S-samples showed peaks indexed to the pure phase of perovskite NaTaOand minor peaks assignable to TaNat various synthesis temperatures. Substitution of oxygen by nitrogen ions causes the light absorption of the H-and S-NaTaONsamples to be extended to the 600–650 nm region, thus making the samples visible-light active. The NaTaONsamples exhibited photocatalytic activity for Hand Oevolution from aqueous methanol and silver nitrate solutions under visible-light irradiation. The UV–vis and PL spectra of the Hand S-catalysts revealed the presence of cationic vacancies and reduced metallic species, which acted as recombination centers. These results demonstrated that the preparation method plays a critical role in the formation of defect states, thereby governing the photocatalytic activity of the NaTaONcatalysts.展开更多
Monodisperse spherical SiO2 particles were successfully synthesized in 2-propanol-H2O-NH3 system by the microwave hydrothermal method using ammonia as catalyst. To investigate the influences on the size of spherical S...Monodisperse spherical SiO2 particles were successfully synthesized in 2-propanol-H2O-NH3 system by the microwave hydrothermal method using ammonia as catalyst. To investigate the influences on the size of spherical SiO2 particles, factors such as ammonia concentration, reaction temperature, stirring intensity and reactants mol ratio have been studied. The orthogonal experiments were carried out. The as-prepared SiO2 particles were characterized by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, Fourier transform infrared spectroscopy （FTIR） and differential thermal analysis （DTA）. The results indicated that the size of SiO2 particles increased greatly with the increase in ammonia concentration, temperature and reactants mol ratio, but increased slightly with the increase in stirring intensity. Monodisperse spherical Si02 particles were amorphous with perfect sphere and uniform size. Hydroxyl was detected in SiO2. Kinetic parameters were calculated, and finally the reaction rate equation of dehydrated hydroxyl was obtained.展开更多
Hydro-sodalites are zeolitic materials with a wide variety of applications.Fly ash is an abundant industrial solid waste,rich in silicon and aluminum,from which hydro-sodalite can be synthesized.However,traditional hy...Hydro-sodalites are zeolitic materials with a wide variety of applications.Fly ash is an abundant industrial solid waste,rich in silicon and aluminum,from which hydro-sodalite can be synthesized.However,traditional hydrothermal synthesis methods are complex and cannot produce high-purity products.Therefore,there is a demand for processing routes to obtain high-purity hydro-sodalites.In the present study,high-purity hydro-sodalite(90.2 wt%)was prepared from fly ash by applying a hydrothermal method to a submolten salt system.Samples were characterized by powder X-ray diffraction(XRD),scanning electron microscopy(SEM),thermogravimetry and differential thermal analysis(TG–DTA),and Fourier transform infrared spectroscopy(FTIR)to confirm and quantify conversion of the raw material into the product phase.Purity of the samples prepared with an H2O/Na OH mass ratio of 1.5 and an H2O/fly ash mass ratio of 10 was calculated and the conversion process of the product phase was studied.Crystallinity of the product was influenced more by the Na OH concentration,less by the H2O/fly ash mass ratio.The main reaction process of the system is that the Si O ions produced by dissolution of the vitreous body in the fly ash and Na+ions in the solution reacted on the destroyed mullite skeleton to produce hydro-sodalite.This processing route could help mitigate processing difficulties,while producing high-purity hydro-sodalite from fly ash.展开更多
The europium ions doped MMoO4 （M=Sr, Ba） nanophosphors were successfully synthesized via a facile hydrothermal method using isopropanol. The relationship between phosphor crystalline phase, morphology, photohtminesc...The europium ions doped MMoO4 （M=Sr, Ba） nanophosphors were successfully synthesized via a facile hydrothermal method using isopropanol. The relationship between phosphor crystalline phase, morphology, photohtminescent properties and hexadecyl trimethyl ammonium bromide （CTAB） concentration, pH value in precursor solution was investigated. The results indi- cated that the morphology and photoluminescent properties were strongly influenced by CTAB concentration and pH value in precursor solution. In SrMoO4：Eu3＋ hosts, the phosphor surface tended to become smoother as the concentration of CTAB was increased; while particles tended to agglomerate as increasing pH value. The relative intensity ratio of charge transfer band to Eu3＋ characteristic emission peaks of MMoO4：Eu3＋ （M=Sr, Ba） was changed as CTAB concentration and pH value changed. The emission spectra of MMoO4：Eu3＋ （M=Sr, Ba） could be adjusted by CTAB concentration and pH value due to their impacts on the structure. It was im- portant that the different morphologies and photoluminescent properties of MMoO4：Eu3＋ （M=Sr, Ba） could be obtained by the facile hydrothermal method and modulated by changing CTAB concentration and pH value.展开更多
Silicon is one of the most promising anode materials for lithium-ion batteries(LIBs), but it suffers from pulverization and hence poor cycling stability due to the large volume variation during lithiation/delithiation...Silicon is one of the most promising anode materials for lithium-ion batteries(LIBs), but it suffers from pulverization and hence poor cycling stability due to the large volume variation during lithiation/delithiation. The core-shell structure is considered as an effective strategy to solve the expansion problem of silicon-based anodes. In this paper, the double-shell structured Si@SnO_(2) @C nanocomposite with nano-silicon as the core and SnO_(2) , C as the shells is synthesized by a facile hydrothermal method.Structural characterization shows that Si@SnO_(2) @C nanocomposite is composed of crystalline Si, crystalline SnO_(2) and amorphous C, and the contents of them are 42.1wt%, 37.8 wt% and 20.1 wt%, respectively. Transmission electron microscope(TEM) observations confirm the double-shell structure of Si@SnO_(2) @C nanocomposite, and the thicknesses of the SnO_(2) and C layers are 20 and 7 nm. The Si@SnO_(2) @C electrode exhibits a high initial discharge capacity of 2777 mAh·g^(-1)at 100 mA·g^(-1)and an excellent rate capability of 340 mAh·g^(-1)at 1500 mA·g^(-1). The outstanding capacity retention is 50.2% after 300 cycles over a potential of 0.01 to 2.00 V(vs. Li/Li+) at 500 mA·g^(-1). The resistance of solid electrolyte interphase(SEI) film(Rf) and charge transfer resistance(Rct) of Si@SnO_(2) @C are 7.68and 0.82 Ω, which are relatively smaller than those of Si@C(21.64 and 2.62 Ω). It is obviously seen that the SnO_(2) shell can reduce the charge transfer resistance, leading to high ion and electron transport efficiency in the Si@SnO_(2) @C electrode. The incorporation of SnO_(2) shell is attributed to the enhanced rate capability and cycling performance of Si@SnO_(2) @C nanocomposite.展开更多
High quality potassium hexatitanate whiskers were hydrothermally synthesized in one step under moderate temperature and pressure conditions. Effects of the titanium source and reaction conditions on the hydrothermal r...High quality potassium hexatitanate whiskers were hydrothermally synthesized in one step under moderate temperature and pressure conditions. Effects of the titanium source and reaction conditions on the hydrothermal reaction rate, product phase component, and morphology of whiskers were investigated. The results show that the reactivity of hydrated titania, anatase TiO2, and rutile TiO2 with KOH decreases in turn, and with hydrated titania as titanium source, it is difficult to obtain potassium hexatitanate whiskers with good morphology. In contrast, uniform potassium hexatitanate whiskers with a length of 10-20 μm and a diameter of 200-700 nm were obtained using anatase TiO2 as titanium source. The investigation demonstrates that the initial KOH concentration, annealing temperature and time, molar ratio of K2O/TiO2, etc. significantly affect the morphology of the as-synthesized whiskers. The optimized synthesis condition is as follows： anatase as a titanium source 10 wt.% KOH solution; annealing temperature and time of 300℃ and 5 h, respectively; K2O/TiO2 molar ratio of 5, etc. A rhombic potassium hexatitanate was prepared under the optimum condition and the whisker grew along the [110] direction. The reaction mechanism was discussed.展开更多
The Ni(OH)2/SiO2 binary colloid was prepared using Ni(NO3)2.6H2O and (C2H5O)4SiO4 as starting materials and was used to form NiO/SiO2. composite powder by hydrothermal method and desiccant method in open air respectiv...The Ni(OH)2/SiO2 binary colloid was prepared using Ni(NO3)2.6H2O and (C2H5O)4SiO4 as starting materials and was used to form NiO/SiO2. composite powder by hydrothermal method and desiccant method in open air respectively. Multi-walled carbon nanotubes (MWCNTs) were synthesized respectively by chemical vapor deposition using the NiO/SiO2 catalyst prepared by different methods. The phase and morphology of the catalysts and the morphology, output yield and purity of MWCNTs were compared by XRD, TEM and SEM. The results show that the catalyst powder prepared by hydrothermal method, compared with that by desiccant method, is smaller, better dispersion and has stronger catalytic activity. Pure MWCNTs with smaller tube diameter and narrow range could be obtained at a high yield using that NiO/SiO2 powder prepared by hydrothermal method as catalyst.展开更多
基金the National Natural Science Foundation of China(No.52272009)the Henan Provincial Science and Technology Research Project(No.242102230151)+1 种基金the Henan Provincial University Science and Technology Innovation Team(No.25IRTSTHN009)the Key Scientific Research Projects of Colleges and Universities in Henan Province(Nos.24B560021,25B560020,25B560023)。
文摘This paper adopted the hydrothermal method to prepare tungsten oxide(WO_(3))nanorod films and studied the effects of precursor solution concentration(0.02,0.03,0.06 mol/L peroxytungstic acid)and annealing temperature(200,300,400℃)on their electrochromic properties.The microstructure characterization of WO_(3) films were performed using scanning electron microscope(SEM),X-ray diffraction(XRD),and transmission electron microscope(TEM),and their electrochromic properties were tested by combining an electrochemical workstation with an ultraviolet-visible spectrophotometer.The results showed that the precursor solution concentration directly affected the thickness(290,560,990 nm)and microstructure of WO_(3) films,significantly impacting their electrochromic properties.However,the annealing temperature had a negligible effect.As the precursor solution concentration increased,the optical modulation of WO_(3) films gradually decreased,reaching 51.1%,43.8%,and 35.1%,respectively.The switching time first increased and then stabilized,with coloring times of 7.3,7.7,and 7.7 s,respectively,and bleaching times of 3.8,6.5,and 6.5 s,respectively.The coloration efficiency gradually increased but the increase was relatively small,reaching 41.8,44.4,and 44.8 cm^(2)/C,respectively.Moreover,the cycling stability of WO_(3) films was poor,with the ratios of the final value of optical modulation to the initial value 0.33,0.26,and 0.34,respectively.Additionally,there were bigger differences in the bleached state transmittance,while the colored state transmittance showed smaller variations.However,the former has better cycling stability than the latter.In summary,to obtain better electrochromic properties,the thickness of WO_(3) films should not exceed 290 nm.
文摘ZnO is a highly significant II-VI semiconductor known for its excellent optoelectronic properties,making it widely applicable and promising for use in light-emitting devices,solar cells,lasers,and photodetectors.The methods for preparing ZnO are diverse,and among them,the hydrothermal method is favored for its simplicity,ease of operation,and low cost,making it an optimal choice for ZnO single-crystal growth.Most studies investigating the effects of different hydrothermal experimental parameters on the morphology and performance of ZnO nano-materials typically focus on only 2—3 variable parameters,with few examining the impact of all possible experimental parameter changes on ZnO nano-mate-rials.The principles of the hydrothermal method and its advantages in nano-material preparation were briefly introduced in this article.The detailed discussion on the influence of various experimental parameters on the preparation of ZnO nano-materials was provided,which including reaction materials,Zn^(2+)/OH^(-)ratio,reaction time and temperature,additives,experimental equipment,and annealing conditions.The review co-vers how different experimental parameters affect the morphology and performance of the materials,as well as how different rare earth doping elements influence the performance of ZnO nano-materials.It is hoped that this work will contribute to future research on the hydrothermal synthesis of nano-materials.
基金financially supported by the Science and Technology Innovation Program of Hunan Province(2024AQ2008)。
文摘The fly ash from waste incineration poses a serious threat to human health due to its high content of dioxins.Hydrothermal treatment is an efficient and clean method on the decomposition and detoxifying of fly ash.To study the degradation mechanism of dioxins,this paper uses molecular dynamics(MD)to simulate the hydrothermal reaction process of polychlorinated dibenzo-p-dioxins(PCDDs)under different conditions,and the degradation mechanism of PCDDs is obtained.The results show that the degradation of PCDDs includes two pathways:the first pathway is the substitution of Cl groups by hydroxyl groups to form low-chlorine substitution products through direct hydrogenation,and the second pathway is the formation of non-toxic benzene ring structures accompanied by the cleavage of C—O bonds.The two degradation pathways of PCDDs well explain the changes in toxicity before and after the hydrothermal treatment of fly ash,which is consistent with experimental results.This study provides theoretical guidance for the harmless treatment process of fly ash via hydrothermal method.
基金National Nature Science Foundation of China (51072109)
文摘High purity ZrSiO4 powders were prepared using zirconium oxychloride and tetraethoxysilane as raw materials by the microwave-hydrothermal method at 160-200 ℃ for 30 min, in which NaF was added as mineralizer to promote the crystallization of zircon. The phase composition and microstructure of synthesized ZrSiO4 powders were investigated in detail. The results show that: the microwave-hydrothermal method greatly reduces the synthesis temperature of ZrSiO4 to 160 ℃, 30 min. The synthesized ZrSiO4 powders have small particle size and high stability up to 950 ℃. The synthesis mechanism of ZrSiO4 by microwave hydrothermal s process was also discussed.
基金Project(2006AA03Z413) supported by the Hi-tech Research and Development Program of China
文摘SnO2 nanoparticles with the average particle size of 5-30 nm were synthesized using SnCl4·5H2O as the precursor and NH3·H2O as the mineralizing agent by hydrothermal method.In the case of 1 kg/batch production,the effects of synthesis conditions including solution concentration,reaction temperature,pressure,time and pH value on the grain size,particle morphology and crystal structure of SnO2 were systematically studied.The particles were characterized by X-ray diffraction（XRD） and transmission electron microscopy（TEM）.The results show that,the particle size can be well controlled in the range of 5-30 nm by adjusting the processing parameters such as reaction temperature and time when the crystal structure and particle morphology remain unchanged.The previous reports,the unusual dependences of the grain size of SnO2 on reaction temperature and time were found.The mechanism for such abnormal grain growth behavior was tentatively elucidated.
基金Project supported by the Natural Science Basic Research Program of Shaanxi Province(2021JZ-43)the Key Program for International Science and Technology Cooperation Projects of Shaanxi Province(2018KWZ-08)+2 种基金the National Key Research and Development Program of China(2019YFC1520904)the Scientific Research Plan of Shannxi Provincial Education Department,China(18JK0780)Ningxia Natural Fund(2023AAC03338)。
文摘Fluorescence imaging techniques represent essential tools in in vitro,preclinical,and clinical studies.In this study,an improved one-step hydrothermal method to synthesize citric acid(CA)modifiedα-NaYbF_(4):2%Er^(3+)nanocrystals was proposed.The introduction of various doping ions into NaYbF_(4):2%Er^(3+)and the different valence states of the same ions affect both the crystal size and upconversion luminesce nce.There fore,we investigated the upconversion luminesce nce enha ncement of NaYbF_(4):2%Er^(3+)by ion doping and find that the upconversion luminescence intensity of the upconversion nanoparticles(UCNPs)co-doped with 5 mol%Fe^(2+)ions shows the greatest enhancement,especially for red emission at654 nm.Furthermore,HeLa cells incubated with UCNPs allow for imaging with strong red upconversion emission detectio n.Confocal laser scanning microscope(CLSM)fluorescent images of HeLa cells indicate that NaYbF_(4):2%Er/5%Fe^(2+)leads to a clear outline and improves visualization of the cell morphology.In addition,the CA coated NaYbF_(4):2%Er^(3+)/5%Fe^(2+)nanoparticles and NaYbF_(4):2%Er^(3+)/5%Fe^(2+)show low cytotoxicity in HeLa cells.Organ imaging reveals the efficiency of these UCNPs to analyze the lungs,liver,and spleen.Together,these results indicate that the Cit-NaYbF_(4):2%Er^(3+)/5%Fe^(2+)UCNPs are efficient nanoprobes for fluorescence molecular to mography.
文摘Hydrothermal method was used to synthesize nanoscale particles of MnZn ferrites. The crystallites were characterized by XRD, TEM and SEM. The effects of the reaction time, temperature and additives on the product were investigated. Crystallization process would be carried out above 160 ℃ for 5 h or more, higher temperature can reduce the reaction time. Additives were used to remove impurities such as Fe 2O 3, ZnMnO 3.10～15 nm pure slightly agglomerated MnZn ferrite crystallites with a narrow grain size distribution were obtained.
文摘LiCoPO4 micron-rods with an average diameter of about 500 nm and length of about 5 μm were synthesized by dispersant-aided hydrothermal method. Poly(n-vinylpyrrolidone) (PVP) was used as dispersant in the hydrothermal method. The starting solution and the concentration of dispersant have significant influences on the morphology of LiCoPO4,and the electrochemical performance is improved via controlling the particle size and morphology by the hydrothermal method. The cell using smaller particle LiCoPO4 as cat...
基金financially supported by the National Natural Science Foundation of China (Nos.51302322 and 21373273)the Open-End Fund for the Valuable and Precision Instruments of Central South University (No.CSUZC201613)+1 种基金the Open Foundation of Guangdong Provincial Key Laboratory for Technology and Application of Metal Toughening,Guangdong Institute of Materials and Processing (No.GKL201605)the Education Reform Project of Central South University (No.2016jy03)
文摘pH value is a key factor in the preparation of nano-sized TiO2 with hydrothermal method. Using Ti（SO4）2 as the titanium source, H2O2 as the complexing agent, NaOH and HCl as the pH value regulator, nano- sized TiO2 powder with various morphologies and sizes was synthesized. Changes in morphology, size and phase type with pH values of samples were characterized by X-ray diffraction （XRD） and transmission electron micro- scopy （TEM） measurements. Results show that under the present preparation conditions, TiO2 powder is an anatase phase with pH value less than 11, but is more likely to be a brookite phase with pH value more than 11. With the increase in pH value from 1 to 11 in hydrothermal envi- ronment, nano-sized anatase TiO2 gradually grows up in all directions. {001 }, { 101 } and { 100} groups of crystal plane are the exposed crystal planes of nano-sized anatase TiO2 for the （004）, （101） and （200） facets found in high-reso- lution TEM image. The photocatalytic performance of nano-sized TiO2 with different morphologies was com- pared by measuring their photocatalytic degradation rates for methylene blue under ultraviolet light. Results show that anatase TiO2 prepared under the alkalescenthydrothermal environment （pH = 9, 11） has a better pho- tocatalytic degrading performance. Different sizes and phases of nanoscaled TiO2 powders with different photo- catalytic performances can be prepared by the control of pH value of hydrothermal solutions.
基金Project supported bythe Key Laboratory of Rare Earth Chemistry and Physics ,ChangchunInstitute of Applied Chemistry ,Chinese Academy of Sciences (R020202K)
文摘Nanocrystal of upconversion （UC） phosphor Ho^3＋, Tm^3＋ , and Yb^3＋ co-doped NaYF4 was prepared by the hydrothermal method in the presence of the complexing agent EDTA. Under 980 nm diode laser excitation, the impact of different concentrations of Ho^3＋ ion on the UC luminescence intensity was discussed. The law of luminescence intensity versus pump power shows that the 474 nm blue emission, 538 nm green emission, and 642 nm red emission are all due to the two-photon process, while the 450 nm blue emission is a three-photon process. The UC mechanism and processes were also analyzed. The sample was characterized by transmission electron microscopy （TEM） and X-ray diffraction （XRD）. The result shows that Ho^3＋ ,Tm^3＋ , and Yb^3＋ co-doped NaYF4 prepared by the hydrothermal method exhibits a hexagonal nanocrystal.
基金supported by the Chinese Ministry of Science and Technology 973 Program(No. 2006CB705604)Science and Technology Commission of Shanghai Municipality(No.09XD 1401800)+1 种基金the National Natural Science Foundation(No.50578090)Shanghai Leading Academic Discipline Project(No.S30109)
文摘In this paper,the TiO_2 nanotubes were synthesized by hydrothermal method using a 10 mol/L NaOH aqueous solution at 150℃. The structure of prepared materials was characterized by X-ray diffraction（XRD）,transmission electron microscopy（TEM）. scanning electron microscope（SEM） and Brunauer-Emmett-Teller（BET）.The prepared TiO_2 nanotubes were used to prepare thick film gas sensors and the gas sensing properties to various gases were tested.Results show the prepared TiO_2 nanotube gas sensors responses to ethanol under dry condition at 450℃.This could be attributed to the fact that it had high porous morphology and a higher pore volume,which can promote the diffusion of ethanol deep inside the films and improve the sensor response. Moreover,the gas sensor made with nanotubes exhibit high selective response towards ethanol gas compared with H_2,CO,acetone.
基金Supported by the Education Department of Zhejiang Province(20030625)SRF for ROCS,SEM(2003-14)the National Natural Science Foundation of China(50272059).
文摘The semiconductor TiO_(2)is the most important photocatalyst for the degradation of pollutants.Anatase TiO_(2)has a large band gap of 3.2 eV that requires powerful UV light to initiate the photocatalytic reactions.Many modifịcation methods such as metal ion doping,composite semiconductors and metal layer modification have been used to extend the light absorption of the catalyst to the visible light region but have little effect[1~4].Surface sensitization with dyes[5]is not practical in application as most dyes self-degrade easily.Therefore,the preparation of TiO_(2)with good wavelength response in the visible light region and high photocatalytic activity for pollutant degradation using natural sunlight is an important goal in TiO_(2)photocatalysis.
基金supported financially by the Outstanding Youth Science Fund of Shaanxi Province(No.2018JC-028)the fund of Beijing Key Laboratory of Quality Evaluation Technology for Hygiene and Safety of Plastics,Beijing Technology and Business University(No.51772243)+1 种基金the Innovation Team Plan of Shaanxi Province(No.2017KCT-17)the National Natural Science Foundation of China(No.51772243).
文摘Highly dispersed carbon microspheres(CMSs)derived from D-xylose were successfully synthesized under hydrothermal conditions and followed by further carbonization,in which F127 was used as a soft template.As-synthesized products were characterized by scanning electron microscopy(SEM),transmission electron microscopy(TEM),flourier transform infrared spectroscopy(FT-IR),thermal gravimetric(TG)and X-ray diffraction(XRD).The results showed that the morphology and structure of the CMSs prominently depended on the stirring speed during hydrothermal reaction.The resultant CMSs principally had non-porous structure without stirring and had a very smooth surface.When the stirring speed increased to 200 rpm,the synthesized mesoporous carbon microspheres at 220?C for 24 h(CMSs-5)had a uniform size distribution of 1–1.4μm and a specific surface area of 452 m^2/g.Nevertheless,with further increasing to 400 rpm,as-fabricated carbon products were mostly amorphous with a low degree of sphericity.Results demonstrated that the diameter of the products decreased with the increase of stirring speed.Furthermore,the sphericity product yield of CMSs reduced with the increase of stirring speed.XRD result showed that all the obtained samples contained partial graphite phase.In addition,a formation mechanism was proposed that involved polymerization product as the precursors for microsphere formation.The controllable and green strategy may provide a great convenience to study properties and applications of carbon microspheres.
基金the financial support from the Ministry of Science and Technology,Taiwan(MOST 104-2218-E-033-006-MY2)
文摘NaTaONcatalysts were synthesized by a hydrothermal（H） and a solid-state（S） methods in this study.The H-and S-NaTaONsamples were characterized by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, transmission electron microscopy（TEM）, UV–visible（UV–vis） diffuse reflectance spectroscopy, and photoluminescence（PL） spectroscopy. The XRD patterns of the H-and S-samples showed peaks indexed to the pure phase of perovskite NaTaOand minor peaks assignable to TaNat various synthesis temperatures. Substitution of oxygen by nitrogen ions causes the light absorption of the H-and S-NaTaONsamples to be extended to the 600–650 nm region, thus making the samples visible-light active. The NaTaONsamples exhibited photocatalytic activity for Hand Oevolution from aqueous methanol and silver nitrate solutions under visible-light irradiation. The UV–vis and PL spectra of the Hand S-catalysts revealed the presence of cationic vacancies and reduced metallic species, which acted as recombination centers. These results demonstrated that the preparation method plays a critical role in the formation of defect states, thereby governing the photocatalytic activity of the NaTaONcatalysts.
基金supported by the National Basic Research Program of China (Grant No.2007CB613603)
文摘Monodisperse spherical SiO2 particles were successfully synthesized in 2-propanol-H2O-NH3 system by the microwave hydrothermal method using ammonia as catalyst. To investigate the influences on the size of spherical SiO2 particles, factors such as ammonia concentration, reaction temperature, stirring intensity and reactants mol ratio have been studied. The orthogonal experiments were carried out. The as-prepared SiO2 particles were characterized by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, Fourier transform infrared spectroscopy （FTIR） and differential thermal analysis （DTA）. The results indicated that the size of SiO2 particles increased greatly with the increase in ammonia concentration, temperature and reactants mol ratio, but increased slightly with the increase in stirring intensity. Monodisperse spherical Si02 particles were amorphous with perfect sphere and uniform size. Hydroxyl was detected in SiO2. Kinetic parameters were calculated, and finally the reaction rate equation of dehydrated hydroxyl was obtained.
基金financially supported by the National Natural Science Foundation of China (No. 51474028)the National Key Research and Development Program of China (No. 2017YFC0210301)+1 种基金China Postdoctoral Science Foundation (No. 2017M621034)the Science and Technology Benefiting Citizens Program of Ningbo, China (No. 2015C50058)
文摘Hydro-sodalites are zeolitic materials with a wide variety of applications.Fly ash is an abundant industrial solid waste,rich in silicon and aluminum,from which hydro-sodalite can be synthesized.However,traditional hydrothermal synthesis methods are complex and cannot produce high-purity products.Therefore,there is a demand for processing routes to obtain high-purity hydro-sodalites.In the present study,high-purity hydro-sodalite(90.2 wt%)was prepared from fly ash by applying a hydrothermal method to a submolten salt system.Samples were characterized by powder X-ray diffraction(XRD),scanning electron microscopy(SEM),thermogravimetry and differential thermal analysis(TG–DTA),and Fourier transform infrared spectroscopy(FTIR)to confirm and quantify conversion of the raw material into the product phase.Purity of the samples prepared with an H2O/Na OH mass ratio of 1.5 and an H2O/fly ash mass ratio of 10 was calculated and the conversion process of the product phase was studied.Crystallinity of the product was influenced more by the Na OH concentration,less by the H2O/fly ash mass ratio.The main reaction process of the system is that the Si O ions produced by dissolution of the vitreous body in the fly ash and Na+ions in the solution reacted on the destroyed mullite skeleton to produce hydro-sodalite.This processing route could help mitigate processing difficulties,while producing high-purity hydro-sodalite from fly ash.
基金Project supported by the Nation Natural Science Foundation of China(51562025)Graduate Student Innovation Special Funds(YC2016-S085)
文摘The europium ions doped MMoO4 （M=Sr, Ba） nanophosphors were successfully synthesized via a facile hydrothermal method using isopropanol. The relationship between phosphor crystalline phase, morphology, photohtminescent properties and hexadecyl trimethyl ammonium bromide （CTAB） concentration, pH value in precursor solution was investigated. The results indi- cated that the morphology and photoluminescent properties were strongly influenced by CTAB concentration and pH value in precursor solution. In SrMoO4：Eu3＋ hosts, the phosphor surface tended to become smoother as the concentration of CTAB was increased; while particles tended to agglomerate as increasing pH value. The relative intensity ratio of charge transfer band to Eu3＋ characteristic emission peaks of MMoO4：Eu3＋ （M=Sr, Ba） was changed as CTAB concentration and pH value changed. The emission spectra of MMoO4：Eu3＋ （M=Sr, Ba） could be adjusted by CTAB concentration and pH value due to their impacts on the structure. It was im- portant that the different morphologies and photoluminescent properties of MMoO4：Eu3＋ （M=Sr, Ba） could be obtained by the facile hydrothermal method and modulated by changing CTAB concentration and pH value.
基金financially supported by GRINM Science and Technology Innovation Fund (Nos. 2020DY0109 and 57222001)the Opening Project Fund of Materials Service Safety Assessment Facilities (No. MSAF-2021-001)Guangdong High Level Innovation Research Institute (No. 2021B0909050001)。
文摘Silicon is one of the most promising anode materials for lithium-ion batteries(LIBs), but it suffers from pulverization and hence poor cycling stability due to the large volume variation during lithiation/delithiation. The core-shell structure is considered as an effective strategy to solve the expansion problem of silicon-based anodes. In this paper, the double-shell structured Si@SnO_(2) @C nanocomposite with nano-silicon as the core and SnO_(2) , C as the shells is synthesized by a facile hydrothermal method.Structural characterization shows that Si@SnO_(2) @C nanocomposite is composed of crystalline Si, crystalline SnO_(2) and amorphous C, and the contents of them are 42.1wt%, 37.8 wt% and 20.1 wt%, respectively. Transmission electron microscope(TEM) observations confirm the double-shell structure of Si@SnO_(2) @C nanocomposite, and the thicknesses of the SnO_(2) and C layers are 20 and 7 nm. The Si@SnO_(2) @C electrode exhibits a high initial discharge capacity of 2777 mAh·g^(-1)at 100 mA·g^(-1)and an excellent rate capability of 340 mAh·g^(-1)at 1500 mA·g^(-1). The outstanding capacity retention is 50.2% after 300 cycles over a potential of 0.01 to 2.00 V(vs. Li/Li+) at 500 mA·g^(-1). The resistance of solid electrolyte interphase(SEI) film(Rf) and charge transfer resistance(Rct) of Si@SnO_(2) @C are 7.68and 0.82 Ω, which are relatively smaller than those of Si@C(21.64 and 2.62 Ω). It is obviously seen that the SnO_(2) shell can reduce the charge transfer resistance, leading to high ion and electron transport efficiency in the Si@SnO_(2) @C electrode. The incorporation of SnO_(2) shell is attributed to the enhanced rate capability and cycling performance of Si@SnO_(2) @C nanocomposite.
文摘High quality potassium hexatitanate whiskers were hydrothermally synthesized in one step under moderate temperature and pressure conditions. Effects of the titanium source and reaction conditions on the hydrothermal reaction rate, product phase component, and morphology of whiskers were investigated. The results show that the reactivity of hydrated titania, anatase TiO2, and rutile TiO2 with KOH decreases in turn, and with hydrated titania as titanium source, it is difficult to obtain potassium hexatitanate whiskers with good morphology. In contrast, uniform potassium hexatitanate whiskers with a length of 10-20 μm and a diameter of 200-700 nm were obtained using anatase TiO2 as titanium source. The investigation demonstrates that the initial KOH concentration, annealing temperature and time, molar ratio of K2O/TiO2, etc. significantly affect the morphology of the as-synthesized whiskers. The optimized synthesis condition is as follows： anatase as a titanium source 10 wt.% KOH solution; annealing temperature and time of 300℃ and 5 h, respectively; K2O/TiO2 molar ratio of 5, etc. A rhombic potassium hexatitanate was prepared under the optimum condition and the whisker grew along the [110] direction. The reaction mechanism was discussed.
基金This work was supported in part by NSF of Guangdong Province,the Most Important Items of the Tenth Five-Year Plan of Guangdong Provincethe Project of Science and Technology Program of Guangdong Province+1 种基金the Project of Science and Technology Program of Guangzhou Citythe Maoming Science Technology Fund of Guangdong Province.
文摘The Ni(OH)2/SiO2 binary colloid was prepared using Ni(NO3)2.6H2O and (C2H5O)4SiO4 as starting materials and was used to form NiO/SiO2. composite powder by hydrothermal method and desiccant method in open air respectively. Multi-walled carbon nanotubes (MWCNTs) were synthesized respectively by chemical vapor deposition using the NiO/SiO2 catalyst prepared by different methods. The phase and morphology of the catalysts and the morphology, output yield and purity of MWCNTs were compared by XRD, TEM and SEM. The results show that the catalyst powder prepared by hydrothermal method, compared with that by desiccant method, is smaller, better dispersion and has stronger catalytic activity. Pure MWCNTs with smaller tube diameter and narrow range could be obtained at a high yield using that NiO/SiO2 powder prepared by hydrothermal method as catalyst.
