Carbothermal synthesis of Si3N4 powders using a combustion synthesis precursor

Si₃N₄ powders were synthesized by a carbothermal reduction method using a SiO₂ + C combustion synthesis precursor derived from a mixed solution consisting of silicic acid (Si source), polyacrylamide (additive), nitric acid (oxidizer), urea (fuel), and glucose (C source). Scanning electron microscopy (SEM) micrographs showed that the obtained precursor exhibited a uniform mixture of SiO₂ + C composed of porous blocky particles up to ～20 μm. The precursor was subsequently calcined under nitrogen at 1200–1550°C for 2 h. X-ray diffraction (XRD) analysis revealed that the initial reduction reaction started at about 1300°C, and the complete transition of SiO₂ into Si₃N₄ was found at 1550°C. The Si₃N₄ powders, synthesized at 1550°C, exhibit a mixture phase of α- and β-Si₃N₄ and consist of mainly agglomerates of fine particles of 100–300 nm, needle-like crystals and whiskers with a diameter of about 100 nm and a length up to several micrometers, and a minor amount of irregular-shaped growths.     

Reaction mechanism for in-situ β-SiAlON formation in Fe3Si-Si3N4-Al2O3 composites

In this work, Fe₃Si-Si₃N₄-Al₂O₃ composites were prepared at 1300℃ in an N₂ atmosphere using fused corundum and tabular alumina particles, Al₂O₃ fine powder, and ferrosilicon nitride (Fe₃Si-Si₃N₄) as raw materials and thermosetting phenolic resin as a binder. The effect of ferrosilicon nitride with different concentrations (0wt%, 5wt%, 10wt%, 15wt%, 20wt%, and 25wt%) on the properties of Fe₃Si-Si₃N₄-Al₂O₃ composites was investigated. The results show that the apparent porosity varies between 10.3% and 17.3%, the bulk density varies from 2.94 g/cm3 and 3.30 g/cm3, and the cold crushing strength ranges from 67 MPa to 93 MPa. Under the experimental conditions, ferrosilicon nitride, whose content decreases substantially, is unstable; part of the ferrosilicon nitride is converted into Fe₂C, whereas the remainder is retained, eventually forming the ferrosilicon alloy. Thermodynamic assessment of the Si₅AlON₇ indicated that the ferrosilicon alloy accelerated the reactions between Si₃N₄ and α-Al₂O₃ fine powder and that Si in the ferrosilicon alloy was nitrided directly, forming β-SiAlON simultaneously. In addition, fused corundum did not react directly with Si₃N₄ because of its low reactivity.     

Improvement of oxidation resistance of Nb–Ti–Si based alloys with additions of Al,Cr and B at different temperatures

The effects of Cr,Al and B addition on the microstructure and high-temperature oxidation behaviors(at 1200,1250 and 1300℃) of Nb-Ti-Si based alloys were investigated.The results showed that the addition of Cr stabilized α-Nb₅ Si₃,while Al promoted the formation of β-Nb₅ Si₃ and adding B promoted the formation of γ-Nb₅ Si₃.Among the three elements,Al and Cr were beneficial to oxidation resistance at 1200℃,and B was favorable to the...     

The first observation of Mo5+ in the passivation layer of Mo2N

Molybdenum nitride powder with S_g of 115 m² · g¹ (passivated) has been prepared by a temperature programmed reaction of MoO₃in H₂/N₂ mixture. It exhibited high catalytic activity in CO oxidation at low temperature. XPS, EPR and LRS studies have shown the existence of mixed valence states of Mo ions, especially Mo⁵⁺ ion (g(tT=1.932,g||=1.892) observed for the first time, in the passivation layer of molybdenum nitride. A surface Superoxide species, O₂ (g = 2.001, Raman band 1 124 cm¹), was found to be produced accompanying the transformation of Mo⁵⁺/Mo⁴⁺ redox pair. Evidence has been given to suggest that this surface superoxide might be responsible for CO oxidation over Mo₂N catalyst.     

Microstructure and improved mechanical properties of ultrafine-grained Mo-12Si-8.5B (at.%) alloys with addition of ZrB2

Multi-hierarchical Mo-12Si-8.5B-x Zr B_2(x=0,0.5,1.0,1.5,2.5 wt%)alloys consisting of three ultrafine-grained(UFG,0.47–0.81μm)phases of Mo_5Si B_2(T2),Mo_3Si and Mo solid solution(α-Mo)were prepared by mechanical alloying following hot pressing.Microstructure observations showed that the intermetallic phases(Mo_3Si and T2)distributed dispersedly in the continuousα-Mo matrix associated with the homogeneously embedded nanoscaled particles(10–225 nm)in the grain interiors and at the grain boundaries.The Mo-12Si-8.5B-x Zr B_2alloys exhibited monotonically increasing compressive strength to 3.13 GPa with increasing content of Zr B_2,and the fracture toughness increased about 27%and reached at 11.5 MPa m~(1/2)at 1.0 wt%Zr B_2,rendering the Mo-12Si-8.5B-1.0 wt%Zr B_2alloy possessing the best combined mechanical properties of high strength and high toughness.The underlying reason for the superior mechanical properties of the Mo-12Si-8.5B-x Zr B_2alloys is that the dispersedly distributed nanosized particles in the UFG multi-phased-matrix can not only effectively block the dislocation motion to increase the strength but also store the dislocations to increase the strain hardening ability during mechanical deformation.     

Joining of Si3N4 ceramic using PdCo(Ni SiB)–V system brazingfi ller alloy and interfacial reactions

The wettability of V-active PdCo-based alloys on Si3N4ceramic was studied with the sessile drop method. And the alloy of Pd50.0–Co33.7–Ni4.0–Si2.0–B0.7–V9.6(wt%),was developed for Si3N4ceramic joining in the present investigation. The rapidly-solidified brazing foils were fabricated by the alloy Pd50.0–Co33.7–Ni4.0–Si2.0–B0.7–V9.6. The average room-temperature three-point bend strength of the Si3N4/Si3N4joints brazed at 1453 K for 10 min was 205.6 MPa,and the newly developed braze gives joint strengths of 210.9 MPa,206.6 MPa and 80.2 MPa at high temperatures of 973 K,1073 K and 1173 K respectively. The interfacial reaction products in the Si3N4/Si3N4joint brazed at 1453 K for10 min were identified to be VN and Pd2Si by XRD analysis. Based on the XEDS analysis result,the residual brazing alloy existing at the central part of the joint was verified as Co-rich phases,in which the concentration of element Pd was high up to 18.0–19.1 at%. The mechanism of the interfacial reactions was discussed. Pd should be a good choice as useful alloying element in newer high-temperature braze candidates for the joining of Si-based ceramics.     

Si3N4/AlN对Sialon/刚玉复合材料组织和性能的影响

以棕刚玉,Al,Si,Al2O3为原料,利用一步工艺合成了Sialon/刚玉复合材料·研究了Si3N4/AlN复合添加剂对复合材料组织、性能以及复合材料中N含量的影响·研究结果表明:材料中N含量随着Si3N4/AlN复合添加剂的增加而增加,材料的强度随着Si3N4/AlN复合添加剂的增加呈现出先升高后降低的变化趋势;当氮化温度超过1330℃,氮化时间超过8h后,添加Si3N4/AlN的材料中N含量基本上达到饱和值,添加Si3N4/AlN可以降低Sialon相的合成温度;1230～1280℃是一个重要的前期氮化温度,添加Si3N4/AlN的材料在该温度可完成整个氮化反应的94 2%,早期对Al,...     

Influence of B source materials on the synthesis of TiB2-Al2O3 nanocomposite powders by mechanical alloying

An Al2O3-TiB2 nanocomposite was successfully synthesized by ball milling of Al, TiO2 and two B source materials of B2O3 （system （1）） and H3BO3 （system （2））. Phase identification of the milled samples was examined by Xray diffraction. The morphology and microstructure of the milled powders were monitored by scanning electron microscopy and transmission electron microscopy. It was found that the formation of this composite was completed after 15 and 30 h of milling time in systems （1） and （2）, respectively. More milling energy was required for the formation of this composite in system （2） due to the lubricant properties of HaBO3 and also its decomposition to HBO2 and B2O3 during milling. On the basis of X-ray diffraction patterns and thermodynamic calculations, this composite was formed by highly exothermic mechanically induced self-sustaining reactions （MSR） in both systems. The MSR mode took place around 9 h and 25 h of milling in systems （1） and （2）, respectively. At the end of milling （15 h for system （1） and 30 h for system （2）） the grain size of about 35-50 nm was obtained in both systems.     

TEM observation on nucleation of Ca α-Sialon

Ca α -Sialon compacts pressurelessly-sintered to the intermediate temperature (1 450℃) were investigated with TEM for an overall composition Ca_1.8Si_6.6Al_5.4O_1.8N_14.2. It was found that in most cases, the newly-formed α -Sialon grains had no epitaxial orientation relationship with the Si₃N₄ particles; only occasionally heteroepitaxial nucleation of α -Sialon on α -Si₃N₄ was detected. Further EDAX analysis revealed a much higher Ca concentration in the non-epi- taxially nucleated α -Sialon than in the heteroepitaxially nucleated α -Sialon. Thus a possible correlation between the concentration of metal cations in the α -Sialon structure and the nucleation mechanism has been proposed, i.e. α -Sialon compositions with higher Ca concentration show a stronger trend of non-epitaxial nucleation.     

The preparation and characterization of amorphous SiCN thin films

Radio Frequency plasma enhanced Chemical Vapor Deposition (RF CVD) using N₂, SiH₄ and C₂H₄ as the reaction sources was used to prepare amorphous ternary Si _x C _y N _z thin films. The chemical states of the C, Si and N atoms in the films were characterized by X-ray photoelectron spectroscopy (XPS) and Fourier Transform Infrared Spectroscopy (FTIR). The refractive indexn, extinction coefficientk and optical band gapE _opt of the thin films were investigated by UV-visible spectrophotometer and spectroscopic ellipsometer. The results show that a complex chemical bonding network rather than a simple mixture of Si₃N₄, SiC, CN _x and a-C etc., may exist in the ternary thin films. Then's of the films are within the range of 1. 90–2. 45, andE _opt's of all samples are within the range of 2. 71–2. 86 eV. Foundation item: Supported by the National Natural Science Foundation of China (19975035) Biography: Li Jin-chai (1946-), male, Professor, research direction: novel functional materials films & ion beam modification of materials.     

Effect of reinforcement content on the adhesive wear behavior of Cu10Sn5Ni/Si3N4 composites produced by stir casting

The main objective of this paper was to fabricate Cu10Sn5Ni alloy and its composites reinforced with various contents of Si₃N₄ particles (5wt%, 10wt%, and 15wt%) and to investigate their dry sliding wear behavior using a pin-on-disk tribometer. Microstructural examinations of the specimens revealed a uniform dispersion of Si₃N₄ particles in the copper matrix. Wear experiments were performed for all combinations of parameters, such as load (10, 20, and 30 N), sliding distance (500, 1000, and 1500 m), and sliding velocity (1, 2, and 3 m/s), for the alloy and the composites. The results revealed that wear rate increased with increasing load and increasing sliding distance, whereas the wear rate decreased and then increased with increasing sliding velocity. The primary wear mechanism encountered at low loads was mild adhesive wear, whereas that at high loads was severe delamination wear. An oxide layer was formed at low velocities, whereas a combination of shear and plastic deformation occurred at high velocities. The mechanism at short sliding distances was ploughing action of Si₃N₄ particles, which act as protrusions; by contrast, at long sliding distances, direct metal-metal contact occurred. Among the investigated samples, the Cu/10wt% Si₃N₄ composite exhibited the best wear resistance at a load of 10 N, a velocity of 2 m/s, and a sliding distance of 500 m.     

Fe包覆Si3N4金属陶瓷相反应热力学分析

研究非均相沉淀-热还原法制备Fe包覆α-Si3N4复合粉末常压烧结界面反应特性,并进行热力学分析.研究结果表明:在1 600℃下烧结时,α-Si3N4部分转变为β-Si3N4,Fe相消失,转而生成FeSi化合物;在1700℃下烧结时,α-Si3N4基本转变为β-Si3N4,FeSi化合物消失,Fe相重新出现;在烧结过程中,FeSi化合物或Fe晶粒发生明显长大,呈圆球状分布在Si3N4晶粒之间,实验结果可通过热力学分析进行解释.     

球磨时间对Mo_2FeB_2基金属陶瓷组织和力学性能的影响

以Mo、FeB、Cr、Ni、Fe粉末以及少量的C粉为原料,采用行星球磨法对其球磨后烧结制备Mo2FeB2基金属陶瓷,利用扫描电镜观察球磨粉及其烧结试样的组织形貌,并测定烧结试样的孔隙度、硬度和抗弯强度,研究原料粉末球磨时间对Mo2FeB2基金属陶瓷组织和力学性能的影响。结果表明,随着球磨时间的增加,粉末粒度逐渐变小,Mo2FeB2基金属陶瓷的孔隙度明显降低,其硬度和抗弯强度明显增大,晶粒也随之细化;球磨30h原料粉末所制Mo2FeB2基金属陶瓷的综合性能最优,其硬度(HRA)达到90.2,抗弯强度达到1850MPa。     

Morphology of α-Si3N4 in Fe–Si3N4 prepared via flash combustion

The state and formation mechanism ofα-Si3N4 in Fe–Si3N4 prepared by flash combustion were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results indicate thatα-Si3N4 crystals exist only in the Fe–Si3N4 dense areas. When FeSi75 particles react with N2, which generates substantial heat, a large number of Si solid particles evaporate. The prod-uct between Si gas and N2 is a mixture ofα-Si3N4 andβ-Si3N4. At the later stage of the flash combustion process,α-Si3N4 crystals dissolve and reprecipitate asβ-Si3N4 and theβ-Si3N4 crystals grow outward from the dense areas in the product pool. As the temperature decreases, the α-Si3N4 crystals cool before transforming into β-Si3N4 crystals in the dense areas of Fe–Si3N4. The phase composition of flash-combustion-synthesized Fe–Si3N4 is controllable through manipulation of the gas-phase reaction in the early stage and theα→βtrans-formation in the later stage.     

Structural investigation and luminescent properties of BaZr(BO<Subscript>3</Subscript>)2:Eu<Superscript>3+</Superscript> phosphors containing Si

Si⁴⁺-doped BaZr(BO₃)₂:Eu³⁺ phosphors are prepared by a conventional solid-state reaction. The influence of Si⁴⁺ addition on the charge transfer state of Eu³⁺-O^2– and photoluminescence (PL) properties of BaZr(BO₃)₂:Eu³⁺ are discussed. Room temperature PL spectra indicated that efficient emission is obtained by Si doping. Increased values for the peak-peak ratio (PPR) of BaZr(BO₃)₂:Eu³⁺ at higher Si doping concentrations implied that the Eu³⁺ ion is located in a more asymmetric environment in BaZr_0.8Si_0.2(BO₃)₂:Eu³⁺ than in the undoped samples. The Judd-Ofelt parameters Ω_λ (λ=2,4) were calculated from the PL data, giving results that were consistent with those from the PPR. The maximum radiative quantum efficiency was achieved at a Si doping concentration of 20 mol%.     

机械合金化-热处理制备V5Si3材料

[目的]为了获得V/Si类化合物基本结构和性能,拟合成V/Si系金属间化合物V_5Si_3。[方法]采用V粉和Si粉作原料,按照原子比V∶Si=5∶3进行称量,通过机械合金化与热处理制备V_5Si_3,再利用XRD,SEM/EDS等方法对球磨粉体试样和热处理试样的物相组成、微观形貌和微区成分进行分析与表征,并测量其抗压性能和硬度。[结果]V/Si粉体经过球磨后颗粒度减小,逐渐非晶化,最终得到以原子比V∶Si=5∶3结合的非晶态物质;经过热处理,非晶态结构转变为V_5Si_3晶体。[结论]随着热处理温度的升高,晶体结晶度提高,材料的抗压强度和显微硬度增加,抗压强度达到640 MPa,显微硬度最高为656 MPa。     

The microstructure evolution and phase transformation behavior of a β-solidifying γ-TiAl alloy during creep

The microstructural evolution and creep behavior of the Ti-43.5Al–4Nb–1Mo-0.1B alloy have been investigated by scanning electron microscope(SEM) and transmission electron microscope(TEM). The excellent creep property was obtained with a fully lamellar(FL) microstructure containing the least grain boundary β_o phase(GB-β_o).TEM results revealed that after creep testing the α₂→βophase transformation was observed in the FL microstructure. The formation βophase is asso...     

Effect of trace Zn, P and Mg additions on microstructure and mechanical properties of Nb-Si-Ti alloys

The effects of Zn,P and Mg additions on the microstructure and mechanical properties of Nb-22Ti-3Si alloys were studied. The phases of Nbss and Nb_3Si presented in Nb-22Ti-3Si(AC1),Nb-22Ti-3Si-0.2Zn(AC2) and Nb-22Ti-3Si-0.2Mg alloys(AC3). The Nb-22Ti-3Si-0.2P(AC4) alloy consisted of Nbss,Nb_3Si network and eutectic cell of Nbss/α-Nb_5Si_3.By the addition of Zn,the Nb_3Si network was broken and the volume fraction of Nbss increased from 92%to 96%.The values of fracture toughness of the alloy AC2 at ambien...     

Solidification microstructure and phase constitution of Fe-7.5%Mo-16.5%Si ternary quasiperitectic alloy

Solidification of Fe-7.5%Mo-16.5%Si ternary quasiperitectic alloy is investigated by using differential scanning calorimetry (DSC) and drop tube containerless processing techniques.The primary phase is identified as R (Fe5Mo3Si2) and the quasiperitectic phases are τ1 (Fe5MoSi4) and Fe3Si.With the decrease of droplet diameter, the cooling rate and undercooling of the droplets in-crease rapidly.The experiment result indicates that the solidification microstructure is composed of remnant primary phase, qua-sip...     

Microstructures and mechanical properties of directionally solidified multi-element Nb-Si alloy

Nb-Si system in-situ composites with nominal composition of Nb-21Ti-16Si-7Cr-3Al-2Hf(mole fraction,%) were prepared by directional solidification technology in an optical floating zone furnace at the growth rates of 3,5,8 and 12 mm/h.The microstructures and mechanical properties were investigated as a function of the growth rate.The results show that the solidification microstructures consist of Nb solid solution(Nbss),α-Nb_5Si_3 andβ-Nb_5Si_3.Silicides with high aspect ratio grow continuously and straig...