Effect of fuel type on the aminolysis synthesis of CrN powders from combustion synthesis precursors

CrN nanopowders were synthesized by the aminolysis method by using the low temperature combustion synthesis (LCS) precursor derived from the mixed solution of chromium nitrate and alanine, or urea, or glycine, or citric acid. Effects of fuel type on the particle size and morphology of precursors and their corresponding aminolysis powders were studied in detail. It was found that the use of different types of fuel in solution, had a significant effect on the particle size and morphology of precursors and their corresponding aminolysis powders. Moreover, the optimized fuel type (glycine) yielded the precursor with high specific surface area and reactivity. The characteristics of aminolysis powders were found similar to those of their corresponding precursor. The CrN powders derived from glycine and synthesized at 750?°C for 6?h were comprised of well-distributed spherical particles, exhibiting high specific surface area (32.5?m²/g) with an average size of 30–50?nm.     

Direct combustion synthesis of SiC powders

In this study, we examine the possibility to direct combustion synthesize SiC powders from elements using four reactant combinations (Si and graphite; Si and carbon black; ground Si and carbon black; both Si and carbon black ground) under two reacting environments (heated by an oxy-acetylene torch in air, and heated by tungsten coils in vacuum). The experimental results showed that high-purity SiC product with no oxide present was obtained if pellet, made of Si and carbon black, was burned by an oxy-acetylene torch in air. Also, ground reactant particles yielding deteriorated effect on product conversion is also discussed.     

Gas-phase synthesis of AlN powders from AlCl3-NH3-N2

Aluminium nitride powders were synthesized by the gas-phase reaction of AlCl₃-NH₃-N₂ system. The yield of AlN powders from AlCl₃ and their crystallinity increased as the reaction temperature and the mole ratio of NH₃/AlCl₃ were increased. AlN powders were also formed outside the reactor and their crystallinity was amorphous. The yield of AlN powders was as high as 80% when the reactor temperature was 1000 °C and the mole ratio of NH₃/AlCl₃ was 8. Most of the HCl by-product was recovered as NH₄Cl outside the reactor. Powder characteristics, such as shape, size distribution and crystallinity, were also studied.     

尿素对以硝酸铝和葡萄糖为原料合成氮化铝粉末反应过程中相变及反应速率的影响

以硝酸铝(Al(NO3)3·9H2O)和葡萄糖(C6H12O6·H2O)为原料,利用碳热还原法制备氮化铝粉末,研究了尿素对前驱物的制备及前驱物氮化反应的影响,研究发现添加尿素合成的前驱物和未添加尿素合成的前驱物在氮化反应过程中相变和反应速率存在较大差异。在没有添加尿素合成的前驱物的氮化反应过程中,出现了γ-Al2O3、α-Al2O3、AlON和AIN相,该前驱物的反应速率慢,完全氮化需要在1600℃下才能完成。对于添加尿素合成的前驱物而言,在其氮化反应过程中仅出现了γ-Al2O3和AIN相,没有α-Al2O3和AlON的生成,AIN直接由γ-Al2O3氮化生成,该前驱物的氮化反应速率快,氮化反应温度低,在1400℃下即可实现完全氮化。分析讨论了两种前驱物的氮化反应速率不同的主要原因,并利用XRD、SEM等分析方法对粉末进行了表征。     

The influence of Yb doping on the upconversion luminescence of Pr in aluminum oxide based powders prepared by combustion synthesis

The effect of ytterbium (Yb³⁺) doping on the upconversion (UC) emission of praseodymium (Pr³⁺) doped in aluminum oxide based powders prepared by combustion synthesis is reported for near-infrared excitation (λ = 980 nm). Our experimental results show that the crystalline structure and the UC emission changes with the Yb³⁺ concentration. The sample containing only Pr³⁺ (1.0 wt.%) did not show any UC signal and the UC emission profiles of the samples containing Pr³⁺ (1.0 wt.%) and Yb³⁺ (0.5, 2.0 wt.%) are quite different. The sample containing 0.5 wt.% of Yb³⁺ has five emission lines in the visible range associated to Pr³⁺ 4f–4f transitions, ³P₀ → ³H₄ (497 nm), ³P₀ → ³H₅ (525 and 550 nm), ³P₀ → ³H₆ (620 nm) and ³P₀ → ³F₂ (650 nm). We believe that the UC process has its origin in energy transfer from Yb³⁺ ions to Pr³⁺ ions in Pr_0.83Al_11.83O₁₉ phase. The sample containing 2.0 wt.% of Yb³⁺ has only one emission line in the visible range peaked at 507 nm which we believe has its origin in cooperative UC emission due to excited Yb³⁺ pairs in YbAlO₃ phase. The samples containing Yb³⁺ also present UC emission lines in the near-infrared which are assigned to intrinsic lattice defects.     

Aqueous combustion synthesis and characterization of ZnO powders

New organic fuels (β-alanine, valine, zinc acetate and acrylamide) have been successfully tested for the preparation of nanocrystalline ZnO powders via aqueous combustion synthesis. In all cases, ZnO resulted directly from the combustion process and no subsequent annealing was required. Properties of the as-prepared ZnO powders were investigated and it was found that morphology, specific surface area, crystallite size and cumulative volume of pores are determined by the used fuel. A correlation has been found between the total volume of generated gases, adiabatic temperature, the amount of ZnO and the characteristics of the resulting powders. Largest surface area (42.0 m² g⁻¹) and smallest ZnO crystallite size (21 nm) were obtained for acrylamide.     

溶剂对溶胶-凝胶燃烧法合成YAG粉体的影响

以Y(NO3)3.6H2O、Al(NO3)3.9H2O和柠檬酸为原料,分别以去离子水和无水乙醇为溶剂,采用溶胶-凝胶燃烧法合成YAG粉体。借助FT-IR、XRD、SEM等分析仪器研究了溶胶-凝胶燃烧法合成YAG粉体的过程,重点讨论了前躯体溶液不同溶剂对溶胶-凝胶燃烧法合成过程及合成产物的影响。结果表明:去离子水和无水乙醇对合成的YAG粉体的形貌和分散性有重要的影响。     

A facile synthesis of CuInS2 nanoparticles from molecular single source precursors

CuInS2 nanoparticles have been synthesized via solvent thermolysis of novel bimetallic complexes of the general formula [(Ph3P)2CuIn(S2COR)4] (where R = CH3; C2H5; C(CH3)2); and [(Ph3P)2CuIn(SCH2CH2S)2]. These complexes have been prepared by the reactions of Na/KS2COR and NaSCH2CH2SNa with InCl3 and [(Ph3P)2CuNO3] in methanol, respectively. Solvent thermolyses of these complexes were carried out in ethylene glycol at 196 degrees C for different time periods. The nanoparticles obtained were characterized extensively by techniques like powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction, and X-ray photoelectron spectroscopy. The optical band gap of the nanoparticles was determined by diffuse reflectance spectroscopy (DRS).     

工艺参数对低温燃烧合成钛酸钡粉体的影响

低温燃烧合成(LCS)钛酸钡粉体的工艺是一种能够直接在低温合成四方相纳米钛酸钡粉的方法。在硝酸盐和柠檬酸体系中,以推进剂化学为理论依据,实验得出各反应物间的最佳摩尔配比,考察了前驱体溶液pH值等对反应过程和最终产物的影响。应用X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)等对粉体的结构、形貌进行了分析。结果在300℃点火生成晶粒度在100nm左右无杂质相的四方相钛酸钡粉。     

Mechanical-activation-assisted combustion synthesis of SiC powders with polytetrafluoroethylene as promoter

Mechanical-activation-assisted combustion synthesis of SiC has been conducted with polytetrafluoroethylene (PTFE) as promoters. The mechanical activation of the Si-C reactants with the addition of NH₄Cl as process controlling agent during the high-energy attrition milling could substantially decrease the content of PTFE promoter, which is needed for inducing the Si-C combustion reaction. Ultra-fine β-SiC powders with spherical particles were synthesized at PTFE content as low as 6 wt.%. The combustion synthesized SiC powders have a narrow particle size distribution in the range of 0.5-1 μm.     

煅烧工艺对溶液燃烧合成超细ZrO2粉末的影响

以硝酸锆-尿素为原料,采用溶液燃烧合成(SCS)法制备了超细ZrO2粉末,着重研究了后续煅烧处理对合成的ZrO2粉末结构、尺寸和团聚程度的影响.结果表明,利用SCS法可以合成超细ZrO2粉末,对之进一步进行煅烧处理,可明显降低合成产物中残留有机物的含量,并改善合成粉末的分散性;在700℃煅烧1.0h的条件下,可以获得分散性好,粒径小(＜200nm)的ZrO2粉末.     

In situ synthesis of nanostructured carbon reinforcement in aluminum powders

A novel approach was developed to obtain uniformly dispersed nanostructured carbon reinforcement in aluminum matrix composite powders. This process involves in situ synthesis of carbon nanoflakes (CNFs) with thickness of 30-50 nm on the surface of aluminum powders through Friedel-Crafts alkylation of benzene under its supercritical conditions, at 300 °C and 5.7 MPa with benzene and C₂Cl₆ as carbon sources, and AlCl₃ as catalyst. In this process, all the reactants and catalyst are in gaseous state, which play an important role in inducing homogeneous reaction and dispersion of the CNFs. Meanwhile, Al powders play an important role in inducing the morphology of the CNFs by providing the heterogeneous nucleation sites.     

Preparation and dielectric properties of B-doped SiC powders by combustion synthesis

The SiC(B) solid solution powders were synthesized via combustion reaction of Si/C system in Ar atmosphere, using boron powder as the dopant and polytetrafluoroethylene as the chemical activator, which were investigated by X-ray diffraction (XRD), scanning electronic microscope (SEM) and Raman spectra. Results show that the prepared powders are C-enriched SiC with C antisites and sp² carbon defects in which the sp² carbon is transformed to the sp³ carbon due to boron doping. The electric permittivities of the prepared powders were determined in the frequency range of 8.2-12.4 GHz. The dielectric real part ?′ and dielectric loss tan δ of undoped powder have maximum values (?′ = 5.5-5.3, tan δ = 0.23-0.20), and decrease with increasing boron content. The mechanism of dielectric loss by doping has been discussed.     

Comparison between two combustion routes for the synthesis of nanocrystalline SnO2 powders

Two nitrate–citrate gel combustion routes for the synthesis of nanocrystalline SnO₂ powders were compared. Metallic tin and tin dichloride were used as raw materials. The combustion process was more intense for the metallic tin route, resulting in smaller crystallite size (10.5 nm) and higher specific surface area (49.4 m²/g). The presence of chloride ions in powders obtained by the tin dichloride route was also studied.     

Effect of the composition of starting yttrium aluminum hydroxide sols on the properties of yttrium aluminum garnet powders

A technique has been developed for the synthesis of yttrium aluminum garnet sols aggregationstable in water as a dispersion medium. Depending on the type of precursor used, the temperature of yttrium aluminum garnet formation varies from 900°C to 1100°C. We have obtained yttrium aluminum garnet nanopowders with an average particle size from 40 to 300 nm, depending on the aluminum yttrium hydroxide hydrosol synthesis procedure and annealing temperature.     

工艺条件对低温燃烧/水热法合成纳米羟基磷灰石的影响

以Ca(NO3)2·4H2O、(NH4)2HPO4和柠檬酸为原料,浓硝酸为溶剂,NH4NO3为助燃剂,采用低温燃烧/水热法能够快速合成羟基磷灰石纳米粉体.通过对不同工艺条件下得到的试样进行XRD、SEM等分析,研究了柠檬酸和NH4NO3的加入量对燃烧反应的影响,以及水热处理的温度和时间对水热反应的影响.研究结果表明,选择合理的工艺条件能够快速合成高纯度的羟基磷灰石纳米粉体.     

pH值对溶胶凝胶-燃烧合成纳米晶LaMnO_3粉末的影响

以硝酸镧、硝酸锰和柠檬酸为原料,采用溶胶凝胶燃烧合成技术制备了超细LaMnO3粉末。借助XRD、DTA、SEM、FT-IR等分析仪器研究了溶胶凝胶-燃烧合成技术合成超细LaMnO3粉末的过程,着重讨论了前驱体溶液不同pH值对溶胶凝胶燃烧合成过程及合成产物的影响。结果发现,采用溶胶凝胶燃烧合成技术能合成纳米晶的LaMnO3粉末,随前驱体溶液pH值增加,燃烧反应速率增加,合成粉体的平均晶粒尺寸随pH值增加而减小。通过控制前驱体溶液pH值能一步合成超细LaMnO3颗粒(粒径200nm)。     

反应物量对燃烧合成Ni-Zn铁氧体粉的影响

为探讨燃烧合成法制备Ni0.4Zn0.6Fe2O4粉末工业化放大合成的可行性,研究不同反应物量对燃烧合成制备的Ni0.4Zn0.6Fe2O4粉体及烧结后产物的物相、微观形貌及磁性能的影响,对终产物进行XRD、SEM和EDS分析,对样品经行磁性能测试.结果表明:Fe-Fe2O3-Zn O-Ni O体系燃烧合成过程是以扩散-溶解-析出机制进行的,燃烧反应在非平衡条件下进行,燃烧产物的主要物相为Ni-Zn铁氧体,其中存在Zn O及一些铁的氧化物的杂质,产物经热处理后物相全部转变为尖晶石结构;随着反应物量的增加,产物颗粒尺寸增大,均匀度增加,反应物量的增加对产物的磁性能影响不大;随着反应物量的增加,饱和磁化强度逐渐增加,矫顽力基本不变,反应物量为1 500 g时制备的产品磁性能最佳,具有较高的饱和磁化强度Ms=63.72 emu/g和较低的矫顽力Hc=15.61 Oe.