Si3N4粉粒度对振荡压力烧结Si3N4陶瓷的影响

为了提高Si₃N₄陶瓷的烧结致密度,采用振荡压力烧结工艺分别在1 745和1 775℃制备了Si₃N₄陶瓷,主要研究了Si₃N₄粉的粒度（平均粒径分别为0.4、2.0、2.3μm）对Si₃N₄陶瓷的显微结构和性能的影响。结果显示：1)在两种温度的振荡压力烧结工艺下,由三种不同粒度的Si₃N₄粉制备的Si₃N₄陶瓷的相对密度都很大,为99.65%～99.86%,彼此相差很小。2)由平均粒径为0.2μm的Si₃N₄粉在1 745℃烧结制备的试样的微观结构最均匀,其β-Si₃N₄晶粒平均长径比、抗弯强度和维氏硬度均最大,分别达到5.0、（1 364±65） MPa和（15.72±0.8） GPa;由平均粒径为2.3μm的Si₃     

Sn/Si3N4复合镀层中纳米Si3N4含量测定方法的比较

采用电熔解法溶解Sn/Si3N4复合镀层,以紫外可见分光光度法测定了镀层中纳米Si3N4的含量,并与传统酸溶解及重量法对比。结果表明,电解法在10 min内使镀层完全溶解且在测定波长448 nm处纳米Si3N4溶液的吸光度值与其浓度在10～200 mg/L范围保持良好的线性关系,该方法简单,省时,误差小,回收率98.5%～100%。     

Si3N4粉体表面化学分析及表面改性

Si3N4陶瓷是一种重要的结构陶瓷,本文着重阐述了Si3N4粉体的表面分析方法,以及为了提高固相体积分数而进行的Si3N4粉体表面改性方面的进展.     

导电 Si3N4 基复相陶瓷研究进展

Si_3N_4陶瓷具有优异的力学性能和导热性能,然而其固有的高硬度和脆性极大地限制了其加工性能。通过添加导电相改善Si3N4陶瓷的导电性能可实现对Si_3N_4陶瓷的电火花加工。添加的导电相主要包括钛基化合物(TiN、TiC、TiC N、TiB_2)、锆基化合物(Zr B_2、Zr N)和MoSi_2等导电陶瓷以及碳纳米管(CNT)、碳纳米纤维(CNF)、石墨烯纳米片(GNP)等导电碳基纳米材料。本论文详细回顾了Si_3N_4基导电陶瓷的研究进展,并对今后Si_3N_4基导电陶瓷的发展趋势进行了展望。     

Microstructure and reaction phases in Si3N4/Si3N4 joint brazed with Cu–Pd–Ti filler alloy

Si₃N₄ ceramic was self-jointed using a filler alloy of Cu–Pd–Ti, and the microstructure of the joint was analyzed. By using a filler alloy of Cu76.5Pd8.5Ti15 (at.%), a high quality Si₃N₄/Si₃N₄ joint was obtained by brazing at 1100–1200 °C for 30 min under a pressure of 2 × 10⁻³ MPa. The microstructure of the Si₃N₄/Si₃N₄ joint which was observed by EPMA, XRD and TEM, and the results indicated that a reaction layer of TiN existed at the interface between Si₃N₄ ceramic and filler alloy. The center of the joint was Cu base solid solution containing Pd, and some reaction phases of TiN, PdTiSi and Pd₂Si found in the Cu [Pd] solid solution.     

基于激光切割的Si3N4陶瓷断裂韧性测试方法

提出一种采用激光切割技术在Si3N4陶瓷表面预制微小切口,并结合SENB法测定陶瓷材料断裂韧性的新方法。利用连续激光束在陶瓷表面加工出切口,在三点弯曲实验前后分别运用激光共聚焦显微镜(LSCM)和扫描电镜(SEM)测量切口宽度和深度,而后计算陶瓷材料断裂韧性。在此基础上分析激光输出功率P、激光辐照光斑直径D和激光切割速率Vw与材料断裂韧性值的内在联系。结果表明:输出的激光能量密度达到陶瓷切割加工阈值后,光束在试件表面制得对应切口;切口深宽比为4.3～4.8时测得的Si3N4陶瓷断裂韧性值具有较高精度。     

Si3N4-TiN陶瓷氧化模型

氮化硅-氮化钛陶瓷的氧化行为是建立在对其微观结构的观察,对这种氧化模型现象进行了描述,并对其氧化动力学模型进行研究。当温度<1 000℃,只有TiN相被氧化。此氧化过程是由氧气通过TiO2扩散来控制的,由氧化动力学抛物线方程来描述。超过1 000℃的过程是非常复杂的,那是因为同时发生Si3N4和TiN相的两种氧化反应。三种氧化模型都被清晰的扩散机理所控制,是接连发生的。第1步,Si3N4和TiN相被独立的氧化,它们分别被氧化为SiO2和TiO2相。Si3N4的氧化是由氧通过SiO2扩散控制的,而TiN的氧化由钛通过TiO2扩散所控制。第2步,TiN的氧化被氧通过TiO2扩散控制,而通过SiO2被氧化形成Si3N4。第3步,TiN和Si3N4的氧化由氧通过二氧化硅层扩散控制。动力学方程可以由这三种氧化模型的任意一种决定。     

B4C对Si3N4/Si2N2O结合SiC材料抗热震性能的影响

首先以Si粉、SiO₂微粉为原料，先在700℃空气气氛处理，然后在1 400℃氮气气氛下合成Si₂N₂O,研究了B₄C添加量(外加质量分数分别为0、1.0%、2.0%、3.0%、4.0%)对Si₂N₂O合成效果的影响。然后根据B₄C最优加入量，先在700℃空气气氛保温5 h,然后在1 400℃氮气气氛保温5 h制备了Si₃N₄/Si₂N₂O结合SiC试样。采用1 300℃风冷5次后试样的抗折强度保持率评价其抗热震性，分析了热震前后试样的物相组成和显微结构。结果表明：1)合成Si₂N₂O的B₄C最优添加量为3%(w);在700℃空气处理时，B₄C优先和气氛中O₂反应生成液相B₂O₃,为1 400℃氮...     

Microstructure evolution of Si3N4/Si3N4 joint brazed with Ag–Cu–Ti + SiCp composite filler

The Si₃N₄ ceramic was brazed by Ag–Cu–Ti + SiCp composite filler (p = particle) prepared by mechanical mixing. Effects of the content of Ti and SiC particles on microstructure of the joint were investigated. A reliable Si₃N₄/Si₃N₄ joint was achieved by using Ag–Cu–Ti + SiCp composite filler at 1173 K for 10 min. A continuous and compact reaction layer, with a suitable thickness, forms at the Si₃N₄/braze interface. The SiC particles react with Ti in the brazing layers, forming Ti₃SiC₂ thin layers around the SiC particles themselves and Ti₅Si₃ small particles in the Ag[Cu] and Cu[Ag] based solid solution. The higher content of SiC particles in the filler (≥10 vol%) depresses interfacial bonding strength between the Si₃N₄ substrate and composite brazing layer due to the thinner reaction layer and the bad fluidity of the filler. The Ti₃SiC₂ → TiC + Ti₅Si₃ reaction occurs when Ti concentration around SiC particles in the filler increases.     

Synthesizing high α-phase Si3N4 powders containing sintering additives

Fine grain α-phase silicon nitride (Si₃N₄) ceramic powders were produced via carbothermic reduction of colloidal SiO₂, which contained pre-mixed additives of sintering aids primarily consisting of oxides such as MgO and Y₂O₃. The powders that were pre-mixed in the starting reactants were chosen based on the final powder composition and on type and amount of the secondary phases desired for sintering. After synthesizing, powder properties were examined using standard characterization techniques (XRD, SEM, BET, etc). This technique of ceramic synthesis has advantages in providing nitride-based ceramic powders, which contain secondary in situ phases that are distributed as sintering additives. Silicon nitride ceramic powders synthesized using this method might therefore be readily sintered because the homogeneously distributed sintering additives were present in the starting materials. In this work, the processing parameters are described in terms of the synthesis conditions.     

ZrSiO4对Si3N4结合SiC制品强度和抗氧化性的影响

研究了硅酸锆(ZrSiO     

TiN/Si3N4复合材料的磁控溅射制备及其电性能研究

利用直流反应磁控溅射法在Si3N4陶瓷基体上制备了TiN导电薄膜。采用X射线衍射仪(XRD)、扫描电镜(SEM)和电子能谱(EDS)对薄膜的物相组成以及表面形貌进行分析,表明TiN薄膜均匀,且与基体有较强的附着力。采用SZ82型四探针测试仪对薄膜进行了方阻随厚度变化的分析,表明薄膜的厚度对薄膜的电性能有很大的影响。     

用硅灰合成无碳Si3N4/SiC纳米粉末

用机械与同步热激活法首次从废硅灰中合成无碳Si3N4/SiC纳米粉末。通过这种新方法可在1 465℃形成晶粒尺寸小至45nm的Si3N4/SiC纳米粉末。为了合成无碳Si3N4/SiC纳米粉末,研究了两种不同方法移除纳米粉末中游离碳的有效性。这两种方法分别使用氢气和空气。研究发现,虽然使用氢气时Si3N4和SiC是稳定的,但是这种方法不是很有效。相比之下,使用空气移除游离碳是有效的。游离碳除去后立即停止使用空气,Si3N4/SiC纳米粉末也会有少量被氧化。本文提供了明确的途径将硅灰有效合成无碳Si3N4/SiC纳米粉末。     

Si3N4陶瓷材料高温力学性能和断裂行为定量化实验研究

陶瓷构件常常服役于高温极端环境，易发生脆性断裂破坏。然而，关于陶瓷材料定量化的高温微观断裂研究报道较少。本文基于硅钼棒加热技术开展了Si₃N₄陶瓷材料高温维氏压痕实验，测试了惰性环境下，材料从室温至1200℃间的维氏硬度和断裂韧性，定量化表征了典型温度下的裂纹偏转和穿沿晶行为。研究表明：Si₃N₄陶瓷材料的维氏硬度、断裂韧性和杨氏模量在高温下有一定的降低，实验温度下的沿晶裂纹比例远大于穿晶裂纹比例，而裂纹偏转角分布随温度的变化不大。     

Paper derived SiC–Si3N4 ceramics for high temperature applications

Biomorphic Si₃N₄–SiC ceramics have been produced by chemical vapour infiltration and reaction technique (CVI-R) using paper preforms as template. The paper consisting mainly of cellulose fibres was first carbonized by pyrolysis in inert atmosphere to obtain carbon bio-template, which was infiltrated with methyltrichlorosilane (MTS) in excess of hydrogen depositing a silicon rich silicon carbide (Si/SiC) layer onto the carbon fibres. Finally, after thermal treatment of this Si/SiC precursor ceramic in nitrogen-containing atmosphere (N₂ or N₂/H₂), in the temperature range of 1300–1450 °C SiC–Si₃N₄ ceramics were obtained by reaction bonding silicon nitride (RBSN) process. They were mainly composed of SiC containing α-Si₃N₄ and/or β-Si₃N₄ phases depending on the nitridation conditions. The SiC–Si₃N₄ ceramics have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and Raman spectroscopy. Thermal gravimetric analysis (TGA) was applied for the determination of the residual carbon as well as for the evaluation of the oxidation behaviour of the ceramics under cyclic conditions. The bending strength of the biomorphic ceramics was related to their different microstructures depending on the nitridation conditions.     

Dielectric properties of Cf–Si3N4 sandwich composites prepared by gelcasting

C_f–Si₃N₄ sandwich composites were prepared by gelcasting using α-Si₃N₄ powder, SiC-coated carbon fibers and sintering additives as starting materials. The microstructure and composition, dielectric properties of C_f–Si₃N₄ sandwich composites were investigated. SEM and EDS analysis results reveal that the SiC interphase could effectively overcome incompatibility between carbon fiber and silicon nitride matrix under the condition of pressure-less sintering at 1700 °C. The investigation of microwave absorbing property reveals that, compared with the Si₃N₄ ceramics, both the real (ε?$\epsilon ?$) and imaginary (ε??$\epsilon ??$) permittivity of C_f–Si₃N₄ sandwich composites show strong frequency dispersion characteristics at X-band. Microwave absorption ability of the C_f–Si₃N₄ sandwich composites are significantly enhanced compared with pure Si₃N₄ ceramic, and the reflection loss gradually decreases from −3.5 dB to −14.4 dB with the increase of frequency, while the pure Si₃N₄ ceramic keeps at −0.1 dB. Particularly, the relationship between permittivity of C_f–Si₃N₄ sandwich composites and frequency at X-band has been established through an equivalent RC circuit model. Results showed that both ε?$\epsilon ?$ and ωε??$\omega \epsilon ??$ are inversely proportional to the frequency square ω²${\omega }^2$, and the predicted results agree quite well with the measured data.     

研磨时间对Si3N4纳米复合材料烧结动力学的影响

采用20MPa的等静压与2MPa的气体压力烧结法制备了由多层纳米管增强的氮化硅复合材料。为了保证多层纳米管的良好分散性,在粉料混合物的制备过程中采用了高效的立式球磨机进行研磨。监测了在高能研磨期间的粉状颗粒的形态与显微结构的变化。研究发现,研磨时间通过影响纳米级填充物的分散和降解以及陶瓷主体的相转化,从而对纳米复合材料的结构和机械性能都产生了复杂的影响。     

低温热压制备半透明α/βSi3N4复相陶瓷

以α-Si3N4粉为原料、MgSiN2粉为烧结助剂,在1563℃热压1h制备出半透明α/βSi3N4复相陶瓷。X射线衍射分析结果表明,半透明α/βSi3N4复相陶瓷由85%(质量分数,下同)α-Si3N4和15%β-Si3N4组成。半透明α/βSi3N4复相陶瓷具有和Mg-α-SiAlON陶瓷相似的透光性质,样品厚度为0.42mm,其透过率随波长增加而增大,波长在3.3μm处透过率最大,达到66%,在2.0～4.5μm波长范围,透过率保持在50%以上,随后透过率迅速降低,在5.0μm处截止。     

纳米Si3N4/ACM复合材料的力学性能和硫化性能研究

采用大分子表面处理剂LMPB-g-KH570对纳米Si₃N₄表面进行修饰。利用共混技术制备了纳米Si₃N₄/ACM复合材料。利用RPA-8000、SEM、TEM等测试技术,对纳米复合材料的微观结构和性能进行了分析和评价。结果表明,大分子表面改性剂能有效改善复合材料的微观界面结构,促进纳米Si₃N₄在橡胶基体中的有效分散,橡胶硫化性能得到改善,力学性能得到提高。添加2.0份改性纳米Si₃N₄/ACM复合材料,胶料正硫化时间减少38 s,拉伸强度提高24.8%,撕裂强度提高3.39%。