烧结温度对Ｓｉ３Ｎ４显微结构及性能的影响

基于凝胶分子造孔机理,通过提高凝胶注模工艺中有机单体含量,制备微多孔氮化硅陶瓷,研究了烧结温度对Si3N4微多孔陶瓷烧结体的显微结构、强度、气孔率、孔径等方面的影响.结果表明,温度升高有利于β-Si3N4晶相的生成,烧结温度为1 680℃时,氮化硅陶瓷烧结体中α-Si3N4和β-Si3N4并存,当烧结温度为1 730和1 780℃时,氮化硅陶瓷烧结体的晶相全部为β-Si3N4;陶瓷烧结体的孔径均<1μm,而且孔径分布范围较窄、较均匀;随着烧结温度的提高,陶瓷烧结体的强度单调上升而气孔率下降.     

浆料固相含量对多孔氮化硅陶瓷结构和性能的影响

以琼脂糖作为凝胶物质,采用凝胶注模工艺制备了多孔氮化硅陶瓷,通过改变浆料的固相含量,制备了不同性能的多孔氮化硅陶瓷.结果表明,随着浆料的固相含量从35vol％增加到45vol％,材料的气孔率从57.6％减小至40.8％,弯曲强度从96 MPa增加到178 MPa;大量的长棒状β-Si3N4晶粒从孔壁上生长出来,将气孔填充,其生长方式为溶解-沉淀-析出与气-液-固两种生长机制协同作用的结果.长棒状的氮化硅晶须和恰当的界面结合强度是多孔氮化硅陶瓷具有较高强度的主要原因.     

预烧结对反应烧结多孔氮化硅陶瓷性能的影响

研究了预烧结对反应烧结多孔氮化硅陶瓷的介电性能和力学性能的影响。通过添加30wt%的成孔剂颗粒,制备出孔隙率在55%左右的具有宏观球形孔的多孔氮化硅陶瓷。反应烧结前,在低于硅熔点的温度下,对多孔硅坯体进行不同温度和不同时间的预烧。结果表明,随着预烧结温度的增高和时间的加长,反应烧结后烧结体的强度明显提高,介电常数ε′和介电损耗tanδ都有小幅度的增加。在硅粉中添加5wt%Y2O3 5wt%Al2O3进行预烧,可以减小反应烧结后试样的ε′,并且随预烧结时间的增加而减小。     

烧结助剂含量对多孔氮化硅结构及性能的影响

以氮化硅为原料,以叔丁醇为溶剂,采用凝胶注模成型工艺和无压烧结工艺(17500C、保温1.5h、流动氮气气氛),制备出具有高强度和高气孔率的多孔氮化硅.在浆料中初始固相含量固定为15%体积分数的基础上,研究了烧结助剂含量对多孔氮化硅的气孔率、孔径尺寸分布、物相组成及显微结构的影响,分析了弯曲强度与结构之间的关系.结果表明,通过改变烧结助剂含量,所制备的多孔氮化硅的气孔率为52%-65%;气孔尺寸呈单峰分布,均匀性好,平均孔径为0.82-1.05μm;弯曲强度为64.4-193.5 MPa,且随烧结助剂含量增加呈先增大后减少,在烧结助剂含量为7.5%质量分数时达到最大值(193.5±10.1)MPa.     

有序多孔氧化铝陶瓷微观结构研究

利用扫描电镜(SEM)对模板法制备的有序多孔氧化铝陶瓷的微观结构特征、孔隙结构和晶粒生长进行了研究.结果表明:通过模板法制备的多孔氧化铝陶瓷孔结构均匀、排列有序,孔洞内部相互连通;随着料氧化铝浆固相体积的增加,多孔陶瓷的孔隙率相应降低;孔洞边缘没有出现晶粒的异常生长,与发泡法制备的多孔陶瓷相比,烧结致密度更高.     

氮化硅短纤维多孔材料制备与性能研究

以氮化硼为烧结助剂,采用抽滤成型方法制备氮化硅短纤维多孔材料。通过氮化硼和氮化硅纤维的氧化过程分析,确定了最佳烧结制度。对不同氮化硼含量材料的微观结构、压缩及介电性能进行了测试分析。结果表明:在1 200℃时,氮化硼氧化增重达20%,氮化硅纤维表面明显氧化;随着氮化硼含量的增加,氮化硅纤维粘结明显,粘结点主要成分为二氧化硅和硼硅酸盐,氮化硅短纤维多孔材料的ε随着密度的增加从1. 36增加到1. 62,tanδ从7. 8×10~(-4)增加到9. 5×10~(-4),材料10%压缩应变下的压缩强度从0. 58 MPa提升到2. 03 MPa。     

真空中多孔氮化硅的高温弯曲强度

研究了高温真空环境下多孔(气孔率>50%)氯化硅陶瓷的弯曲强度,并进行了初步分析.结果表明,多孔氮化硅陶瓷在真空中的高温强度随温度上升而降低,由于没有氧化作用,晶界玻璃相在高温下的软化成为影响其强度的主要因素.     

三维网络碳化硅多孔陶瓷的制备

以中间相沥青添加55%(质量分数,下同)的Si粉混合物为原料,制备了含Si的炭泡沫模板。在高温反应烧结炉中,氩气气氛下1500℃保温1～6h,结合反应烧结工艺制备了碳化硅多孔陶瓷。利用扫描电子显微镜(SEM)和X射线衍射分析仪(XRD)对碳化硅多孔陶瓷的微观形貌、物相组成进行了观察,并对熔融Si与C的反应机理进行了探讨。结果表明:碳化硅多孔陶瓷的微观结构与炭泡沫模板的微观结构一致,烧结温度1500℃下,随着保温时间的延长,多孔陶瓷的弯曲强度先增大后减小,而孔隙率先减小后增大;在保温4h的条件下制备的碳化硅多孔陶瓷主要由β-SiC相组成,最大弯曲强度为26.2MPa,对应的孔隙率为45%。内部熔融的Si与外部熔融的Si同时与C反应生成SiC,最后两者结合在一起形成致密的SiC多孔陶瓷。     

具有三维网络结构的莫来石纤维多孔隔热材料的制备及性能研究

本文针对以模压法制备的莫来石纤维隔热材料内部莫来石纤维易形成层状排列的缺点,通过向浆料中引入聚丙烯酰胺(CPAM)的方法来增加浆料的黏度,从而提高纤维的悬浮稳定性,进而制备出具有三维网络结构的莫来石纤维隔热材料。研究了CPAM浓度对莫来石纤维多孔隔热材料的显微结构以及各项物理性能的影响规律。试验结果表明,随着CPAM浓度的增加,试样内部纤维的三维搭接结构越发明显,试样的气孔率逐渐增大,密度和热导率随之减小。但样品的强度随着CPAM的加入呈先增大后减小趋势。当CPAM的浓度为质量分数0.62%时,所制备出的样品的密度为0.382g/cm3、热导率为0.069W/(m·K),且强度呈现最大值0.64MPa。     

多孔氮化硅高温氧化特性分析

采用TG-DSC、XRD、SEM、ICP 等分析手段,对某一典型多孔氮化硅样品进行4 个不同温度点的

静态和微动态连续氧化试验,最高氧化温度为1 400℃。结果表明:多孔氮化硅在0. 1 MPa 静态空气气氛下,

800℃之前,氧化反应非常微弱,800℃以上可见明显的氧化反应,1 000℃以上氧化反应加剧,增重速率加快,并

优先发生在表面与外部孔壁处,之后再发生在样品的内部孔隙处,氧化反应受界面处的化学动力学控制,以被

动氧化为主,主要生成物是SiO2,属吸热反应。当生成的SiO2 将氮化硅表面和孔壁处覆盖时,在其界面处,随

着温度的进一步升高或时间的延长,会生成Si2N2O,且需要注意防范样品可能出现脆性断裂情况。此外,同等

温度下,动态氧化气氛将加速氮化硅的氧化,特别是多孔和粉末状样品。

     

氮化硅的氧化机制研究

研究了氮化硅的氧化机制以及被动氧化至主动氧化的转捩温度,并结合试验结果做了分析。结果表明氮化硅在高温下极易炸裂,在被动氧化机制下生成氮气和SiO2薄膜,转捩温度和碳化硅材料基本一致。     

氮化硅高温透波材料的研究现状和展望

从氮化硅的晶体结构出发,介绍了氮化硅陶瓷优良的性能,综述了近年来氮化硅透波纤维和氮化硅基透波复合材料的研究进展,并对现有氮化硅高温透波材料体系存在的问题及其未来的发展趋势作了展望.     

Grinding performance evaluation of porous composite-bonded CBN wheels for Inconel 718

For high-efficiency grinding of difficult-to-cut materials such as titanium and nickel alloys, a high porosity is expected and also a sufficient mechanical strength to satisfy the function.However, the porosity increase is a disadvantage to the mechanical strength. As a promising pore forming agent, alumina bubbles are firstly induced into the abrasive layer to fabricate porous cubic boron nitride（CBN） wheels. When the wheel porosity reaches 45%, the bending strength is still high up to 50 MPa with modified orderly pore distribution. A porous CBN wheel was fabricated with a total porosity around 30%. The grinding performance of the porous composite-bonded CBN wheel was evaluated in terms of specific force, specific grinding energy, and grinding temperature, which were better than those of the vitrified one under the same grinding conditions. Compared to the vitrified CBN wheel, clear straight cutting grooves and less chip adhesion are observed on the ground surface and there is also no extensive loading on the wheel surface after grinding.     

Effect of Counterface Material on Friction and Wear Behavior of Ni-Cr-W-Al-Ti-MoS_2 Composites

Ni-Cr-W-Al-Ti-MoS2 self-lubricating composites were prepared through the powder metallurgy (P/M) method. Their friction properties were investigated by a pin-on-disk tribometer in the range from the room temperature to 600 ℃. Alumina, silicon nitride and nickel-iron-sulfide alloys were selected as the counterface materials. Results indicate that the lowest friction coefficients under 0.22 can be obtained at 600 ℃ when rubbed against alumina. When rubbed against nickel-iron-sulfide alloys, are presented the lowest wear rates in the magnitude of 10-6 mm3/N·m, one order of magnitude lower than those when rubbed against ceramics. In the case of three rubbing pairs, the wear rates of the composite containing MoS2 present themselves inversely proportional to friction coefficients. With alumina ceramics used as a counterface, transfer films and glaze layers will form on the contact surface playing a main role in lubrication at high temperatures. However, when silicon nitride and nickel-iron-sulfide alloy are used, the lubricating transfer films appear not to be promi-nent.     

凝胶注模氧化铝陶瓷坯体的结构与表征

研究了凝胶注模氧化铝陶瓷坯体的密度、强度、空隙率分布及微观结构等特征。结果表明,影响凝胶注模陶瓷坯片密度的因素主要有:料浆的固含量、单体含量、单体和胶联剂的比值。随着料浆固含量的提高,坯片的抗弯强度呈下降趋势,坯片内部的孔隙率降低,从平均孔隙度为110nm降为90nm,而且均为单峰分布。凝胶注模成型的陶瓷坯片在干燥后,坯片强度优于注射成型、流延成型等传统成型方式。     

利用电化学方法制备有序多孔硅阵列

采用电化学刻蚀的方法，在自制的电解槽中制备n型〈100〉晶向多孔硅条状阵列。通过扫描电子显微镜对生成的多孔硅进行形貌观察，并对多孔硅条状阵列的生长速率与形貌进行了初步的理论分析和实验研究。实验结果表明，多孔硅的生长速率主要由临界电流密度决定，多孔硅生成初始阶段产生锥形刻痕的原因是初始电流密度比较小，加大电流密度可以消除刻痕。多孔硅分又是由孔间距远远大于自由电荷区而产生的，而深槽中出现分立小孔的原因是反应产生的氢气阻碍了阳极氧化的进行。本实验结果对开展多孔硅进一步的研究工作具有指导意义。     

Characteristics of Disorder and Defect in Hydrogenated Amorphous Silicon Nitride Thin Films Containing Silicon Nanograins

The hydrogenated amorphous silicon nitride (SiNx) thin films embedded with nano-structural silicon were prepared and the micro-structures at the interface of silicon nano-grains/SiNx were identified by the optical absorption and Raman scattering measurements. Characterized by the exponential tail of optical absorption and the band-width of the Raman scattering TO mode, the disorder in the interface region increases with the gas flow ratio increasing. Besides, as reflected by the sub-gap absorption coefficients, the density of interface defect states decreases, which can be attributed to the structural mismatch in the interface region and also the changes of hy-drogen content in the deposited films. Additional annealing treatment results in a significant increase of defects and degree of disorder, for which the hydrogen out-diffusion in the annealing process would be responsible.     

A novel bolometer for infrared and millimeter-wave astrophysics

We are developing a novel bolometer which uses a fine mesh to absorb radiation. The filling factor of the mesh is small, providing a small heat capacity and a low geometric cross-section to cosmic rays. The mesh is patterned from a free-standing silicon nitride membrane and is thermally isolated by long radial legs of silicon nitride. A thin metallic film evaporated on the mesh absorbs radiation by matching the surface impedance to that of free space. A neutron transmutation doped germanium thermistor attached to the center of the mesh detects the temperature increase from absorbed radiation. The low thermal conductivity and heat capacity of silicon nitride provide improved performance in low background applications. We discuss the theoretical limits of the performance of these devices. We have tested a device at 300 mK with an electricalNEP=4×10^–17 W Hz^–1/2 and a time constant =40 ms.