BN含量对多孔BN/Si3N4陶瓷结构和性能的影响

以氮化硅(Si₃N₄)为基体, 氮化硼(BN)为添加剂, 叔丁醇为溶剂, 采用凝胶注模成型与无压烧结工艺(温度为1750 ℃、保温时间为1.5 h、流动N₂气氛), 成功制备出具有一定强度和低介电常数的多孔BN/Si₃N₄陶瓷。在浆料中初始固相含量固定为15%体积分数的基础上, 研究了BN含量对多孔Si₃N₄陶瓷材料的气孔率、物相组成及显微结构的影响, 分析了抗弯强度、介电常数与结构之间的关系。结果表明, 通过改变BN含量可制备出气孔率为55.1%~66.2%的多孔Si₃N₄陶瓷; 多孔BN/Si₃N₄复合陶瓷的介电常数随着BN含量的增加而减小, 为3.39~2.25; 抗弯强度随BN含量提高而有所下降, BN质量分数为2.5%时, 抗弯强度最高, 为(74.8±4.25) MPa。     

籽晶添加对氮化硅陶瓷显微结构与力学性能的影响

以不同配比的Y₂O₃-Al₂O₃为烧结助剂, 通过添加3wt%的单分散β-Si₃N₄籽晶, 采用气压烧结制备了氮化硅陶瓷, 并对所得材料的相组成、密度、室温和高温力学性能及显微结构进行了研究. 结果表明: 不同烧结助剂配比的α-Si₃N₄粉体在1800℃保温2 h即全部转化为β-Si₃N₄, 且各烧结体的相对密度都达到了97%以上. 在6wt%Y₂O₃和4.5wt%Al₂O₃为烧结助剂时, 添加3wt%籽晶的样品其室温强度和1200℃高温强度分别提高了20%和16%, 断裂韧性提高了8%.     

High temperature strength and oxidation behaviour of hot-pressed silicon nitride-disilicate ceramics

Twelve different silicon nitride-disilicate ceramics have been fabricated by hot-pressing Si3N4 with the oxides of Y, Yb, Ho, Dy, Er, Sm, Ce, Lu, La, Pr, Gd, and Sc that are used as sintering additives. The high temperature strength and oxidation behaviour of the hot-pressed ceramics were investigated and correlated with the cationic radii of the oxide additives. The flexural strength at 1200°C increased, from 666 MPa for Si3N4-La2Si2O7 to 965 MPa for Si3N4-Sc2Si2O7 which is correlated with a decreasing cationic radius of the oxide additive. The weight gain during oxidation at 1400°C for 192 h in air decreased, from 0.8732 mg cm-2 for a Si3N4-Sm2Si2O7 ceramic to 0.1089 mg cm-2 for a Si3N4-Sc2Si2O7 ceramic, which is a function of the decreasing cationic radius of the oxide additive. This revised version was published online in November 2006 with corrections to the Cover Date.     

以YbH2-MgO体系为烧结助剂制备高热导率高强度氮化硅陶瓷

以YbH2-MgO体系为烧结助剂,采用两步法烧结制备了高热导率高强度氮化硅陶瓷,研究了YbH2-MgO对氮化硅致密化行为、相组成、微观形貌、热导率和抗弯强度的影响.在预烧结阶段,YbH2在还原SiO2的同时原位生成了Yb2O3,进而形成"缺氧–富氮"液相.该液相不仅有利于晶粒的生长,更有利于阻碍晶格氧的生成,相较于Yb...     

碳热还原-反应烧结法制备多孔氮化硅陶瓷

以廉价的二氧化硅、炭黑和硅粉为起始原料, 利用碳热还原-反应烧结法制备了高气孔率、孔结构均匀的多孔氮化硅陶瓷, 考察了原料中硅粉含量对多孔氮化硅陶瓷微观组织和力学性能的影响。XRD分析表明烧结后的试样成分除了少量的α-Si₃N₄相和晶间相Y₂Si₃O₃N₄外, 其余都是β-Si₃N₄相; SEM分析显示微观组织由棒状β-Si₃N₄晶粒和均匀的孔组成。通过改变硅粉的含量, 制备了不同气孔率, 力学性能优异的多孔氮化硅陶瓷。     

反应烧结法制备高强度多孔氮化硅陶瓷

以硅粉(Si)为起始原料, 氧化钇(Y₂O₃)为烧结助剂, 利用干压成型工艺制备出不同气孔率的多孔硅坯体, 通过反应烧结得到高强度多孔氮化硅(Si₃N₄)陶瓷. 研究了Y₂O₃添加量在不同升温制度下对于氮化率的影响, 以及1500~1750℃后烧结对多孔材料强度的影响. 结果表明: 添加9%Y₂O₃的样品具有较高的氮化率, 主要是Y₂O₃与Si粉表面的SiO₂在较低的温度下反应生成了Y₅Si₃O₁₂N. 在不同的反应条件下可得到气孔率为30%~50%, 强度为160~50MPa的样品. 在1750、 0.5MPaN₂气压下对样品进行后处理, α-Si₃N₄完全转变成柱状β-Si₃N₄, 晶型转变有利于强度提高,气孔率为46%的多孔Si₃N₄其强度可达140MPa.     

Preparation of zirconium pyrophosphate bonded silicon nitride porous ceramics

Abstract

A new method for preparing high bending strength porous silicon nitride ceramics with controlled porosity was developed using a pressureless sintering technique, using zirconium pyrophosphate as a binder. The fabrication process was described in detail and the sintering mechanism of porous ceramics was analysed by an X-ray diffraction method. The microstructure and mechanical properties of the porous Si₃N₄ ceramics were investigated, as a function of the content of ZrP₂O₇. The resultant porous silicon nitride ceramics sintered at low temperature (1000 and 1100°C) showed fine micropore structure and a high bending strength. Porous silicon nitride ceramics with porosity of 34–47%, a bending strength of 40–114 MPa and a Young's modulus of 20–50 GPa were obtained.     

SiC_W含量对SiC_W/Si_3N_4复合陶瓷力学及高温微波性能影响

以α-Si_3N_4粉、β-SiC_W为原料,Al_2O_3、Y_2O_3为烧结助剂,采用凝胶注模工艺制备了SiC_W/Si_3N_4复合陶瓷材料,烧结温度为1 650℃,保温1.5h。研究了SiC_W加入含量对SiC_W/Si_3N_4复合陶瓷的微观结构、力学及常温/高温微波吸收性能的影响。结果表明:随着SiC_W含量的增加,SiC_W/Si_3N_4复合陶瓷的抗弯强度和断裂韧性都有先増后减的趋势,当含量为10wt%时,抗弯强度达到最大值505MPa,断裂韧性达9.515MPa·m1/2。常温介电常数在SiC_W含量为10wt%时,实部达最大值12,在12GHz最大吸收值为-21dB。高温介电常数随着SiC_W含量的增加有先增后减的趋势,在含量为10wt%时,实部达到最大值12.5。相比于纯Si_3N_4陶瓷,当SiC_W含量为10wt%时,SiC_W/Si_3N_4复合陶瓷在11.7GHz左右最大吸收可达-27dB,有效吸收频带(小于-5dB)为11.2~12.3GHz。     

氮气压力对多孔氮化硅陶瓷显微组织和力学性能的影响

以α-Si₃N₄为原料, Y₂O₃为烧结助剂, 在三种不同的氮气压力(0.12、0.32和0.52 MPa)下烧结制备了多孔氮化硅陶瓷。研究了氮气压力对氮化硅的烧结行为、显微组织和力学性能的影响, 分别通过SEM观察显微组织并统计晶粒的长径比, 通过XRD对物相进行分析, 并对烧结试样进行三点弯曲强度测试。随着氮气压力的提高, 多孔陶瓷的线收缩率降低、气孔率提高, 这是由于低熔点的液相中N含量随氮气压力的提升而增加, 导致了液相粘度提高, 抑制陶瓷致密化。随着氮气压力的提高, 组织中的棒状β-Si₃N₄生长良好, 晶粒长径比增大, 其原因是高的液相粘度抑制了β-Si₃N₄形核, 有利于β-Si₃N₄生长。由于β-Si₃N₄棒状晶的作用, 陶瓷弯曲强度随氮气压力的升高得到改善, 但是气孔率的升高降低陶瓷的强度。在0.52 MPa的氮气压力下烧结的多孔陶瓷气孔率达58%, 弯曲强度为140 MPa。     

氮化硅复合陶瓷的制备及其显微结构分析

以Si3N4、SiC为原料,Y2O3、Al2O3、MgO为助剂,在1500℃氮气气氛下采用无压烧结的方式进行烧结。利用SEM和XRD观察分析了材料的组织结构和物相组成,研究了材料的配方、制备工艺和烧结性能之间的关系。结果表明,当SiC含量为5％时,烧结体的空隙率为22．9％,抗弯强度为395MPa,显微结构均匀、晶粒细小。     

烧结温度对包混/复合添加工艺制备多孔SiC陶瓷性能的影响

采用包混工艺合成了核壳结构的先驱体粉体,并引入一定量Al2O3、SiO2和Y2O3复合添加剂,通过成型、炭化和烧结工艺制备了多孔碳化硅陶瓷;分析了样品的物相、表面形貌、孔隙率、热导率、热膨胀系数、抗弯强度和抗热震性能。结果表明,在较低的烧结温度下制得了多孔碳化硅陶瓷,在1650℃烧结的多孔碳化硅陶瓷综合性能较好。     

原位反应结合多孔Si3N4陶瓷的制备及其介电性能

以氮化硅(Si₃N₄)和氧化铝(Al₂O₃)为起始原料, 利用原位反应结合技术制备Si₃N₄多孔陶瓷. 研究烧结温度和保温时间对Si₃N₄多孔陶瓷的微观结构、力学性能以及介电性能的影响. 结果表明: 烧结温度在1350℃以下, 保温时间<4h时, 随着烧结温度的升高, 保温时间的延长, 样品的强度和介电常数增大; 但条件超出这个范围, 结果刚好相反; 物相分析表明多孔陶瓷主要由Si3N4和Al₂O₃以及Si₃N₄氧化生成的SiO₂(方石英)组成. 所制备的多孔Si₃N₄陶瓷的气孔率范围为25.34%～48.86%, 抗弯强度为34.77～127.85MPa, 介电常数为3.0～4.6, 介电损耗约为0.002.     

Oxide and interface characteristics of oxidized silicon oxynitride ceramics – an investigation by electron microscopy

Hot-isostatically pressed silicon oxynitride (Si2N2O) ceramics free from sintering aids were oxidized in 1 atm dry oxygen at 1100 and 1300°C. The structural and chemical characteristics of the oxide and the nature of the oxide–Si2N2O interface were determined using cross-sectional transmission electron microscopy in conjunction with small-probe energy dispersive X-ray analysis and selected-area electron diffraction. Oxidation of Si2N2O resulted in the formation of amorphous SiO2. The oxide–Si2N2O interface was chemically abrupt. The interface was very flat when parallel to low-index, high atomic density Si2N2O crystal planes but became notably undulated if oriented to high index, low atomic density planes. About 6 vol% residual SiO2 phase was present in the bulk of the Si2N2O ceramics. Current results have provided an important baseline for the understanding of the oxidation behaviour of Si2N2O. © 1998 Kluwer Academic Publishers     

用碳热还原法制备多孔氮化硅陶瓷

以廉价的二氧化硅和活性碳为起始粉料, 用碳热还原法制备了高气孔率, 孔结构均匀的多孔氮化硅陶瓷.考察了二氧化硅粉末粒径对多孔氮化硅陶瓷微观组织和力学性能的影响. 借助X射线衍射(XRD), 扫描电子显微(SEM)和三点弯曲法对多孔氮化硅陶瓷的微观组织和力学性能进行了研究. XRD分析表明在烧结后的试样中, 除了微量的α-Si₃N₄相和晶界结晶相Y₈Si₄N₄O₁₄外, 其余的都是β-Si₃N₄相; SEM分析显示多孔氮化硅陶瓷是由柱状β-Si₃N₄晶粒和均匀的孔组成, 通过改变二氧化硅的粒径, 制备了不同孔隙率, 力学性能优异的多孔氮化硅陶瓷.     

Si<Subscript>3</Subscript>N<Subscript>4</Subscript>/TiN composites produced from TiO<Subscript>2</Subscript>-Modified Si<Subscript>3</Subscript>N<Subscript>4</Subscript> powders

Si₃N₄/TiN composites have been produced by hot pressing at temperatures from 1600 to 1800°C in a nitrogen atmosphere, using silicon nitride powders prepared by self-propagating high-temperature synthesis and surface-modified with titanium dioxide nanoparticles. We examined the effect of TiO₂ content on the microstructure, phase composition, and mechanical strength of the ceramics. It is shown that titanium nitride can be formed by the reaction Si₃N₄ + TiO₂ → TiN + NO + N₂O + 3Si. The Si₃N₄/TiN composites containing 5–20% TiN have a low density, high porosity, and a bending strength of 60 MPa or lower. In Si₃N₄/TiN ceramics produced using calcium aluminates as sintering aids, the silicon nitride grains are densely packed, which ensures an increase in strength to 650 MPa.     

反应烧结制备Si3N4/SiC复相陶瓷及其力学性能研究

以两种不同配比Y₂O₃/Al₂O₃ (A, 2:3; B, 3:1, 总量15 wt%)为烧结助剂, 通过添加不同质量分数的SiC粉体,反应烧结制备了高强度的氮化硅/碳化硅复相陶瓷。并对材料的相组成、相对密度、显微结构和力学性能进行了分析。结果表明: 在1700℃保温2 h情况下, 烧结助剂A 与B对应的样品中α-Si₃N₄相全部转化为β-Si₃N₄; 添加5wt% SiC, 烧结助剂A对应样品的相对密度达到最大值94.8%, 且抗弯强度为521.8 MPa, 相对于不添加SiC样品的抗弯强度(338.7 MPa)提高了约54.1%。SiC能有效改善氮化硅基陶瓷力学性能, 且Si₃N₄/SiC复相陶瓷断裂以沿晶断裂方式为主。     

氮化硅-铼嬗变模拟靶材的制造和性能研究

采用无压烧结的方法(在1550℃保温3小时)添加5wt.％MgO,5wt.％Y2Oa和不同含量的Re制造出了Si3N4-Re嬗变模拟靶材.研究了Re含量的不同对嬗变靶材致密度和抗弯强度的影响,并通过物相分析,显微组织和断口形貌观察对相关机理进行了分析.     

无压烧结制备氧氮化硅陶瓷

以β－Si3N4和ＳiO2粉末为原料,以ＭgAl2O4为烧结添加剂,通过无压烧结制备出致密的Ｓi2N2O陶瓷材料,所得材料由柱状Ｓi2N2O颗粒和少量β－Si3N4颗粒复合组成,研究了烧结温度对材料显微结构的影响,发现材料的断裂大部分是穿晶断裂。     

Effect of Si3N4 Addition on the Mechanical Properties, Microstructures, and Wear Resistance of Ti-6Al-4V Alloy

In order to improve the wear resistance of Ti-6Al-4V, different amounts of Si3N4 powder were added into the alloy powder and sintered at 1250℃. Porous titanium alloy with higher wear resistance was successfully fabricated. At sintering temperature, reaction took place and a new hard phase of Ti5Si3 formed. The mechanical properties of the fabricated alloys with different amounts of Si3N4 addition were investigated. The hardness of Ti-6Al-4V, which is the index of wear resistance, was increased by the addition of Si3N4. Amounts of Si3N4 addition have very significant influences on hardness and compressive strength. In present study,titanium alloy with 5 wt pct Si3N4 addition has 62% microhardness and 45% overall bulk hardness increase,respectively. In contrast, it has a 16.4% strength reduction. Wear resistance was evaluated by the weight loss during wear test. A new phase of Ti5Si3 was detected by electron probe microanalyzer （EPMA） and X-ray diffraction （XRD） method. The original Si3N4 decomposed during sintering and transformed into titanium silicide. Porous structure was achieved due to the sintering reaction.     

凝胶注模成型制备高性能氮化硅陶瓷(Ⅰ) 助烧剂包覆氮化硅粉料对材料性能的影响

用无机盐共沉淀法在氮化硅颗粒表面包覆一层纳米级的钇铝氧化物后,粉料的分散性大大提高,可用来制备固相体积分数为50%的悬浮体,利用凝胶注模成型和气压烧结制备了氮化硅陶瓷,与机械混合加入助烧剂相比,采用包覆法加入助烧剂能明显提高氮化硅陶瓷的抗弯强度和韦泊尔模数。