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Post-sintering of reaction-bonded silicon nitride 反应键合氮化硅烧结后的研究
Pub Date : 1979-07-01 DOI: 10.1016/0390-5519(79)90015-2
A. Giachello , P. Popper

Reaction-bonded silicon nitride, RBSN, may be used as the starting material for a post-densification process carried out at about 1800°C in nitrogen at atmospheric pressure. The sintering aids used are similar to those employed in hot pressing and pressureless sintering (e.g. MgO, Y2O3). They may be added to the silicon powder before nitridation or, in the case of MgO, by diffusing the vapour into preformed RBSN. High densities (98.5% theoretical) have been achieved accompanied by a shrinkage of only 6.2%. The strength at R.T. was about 1000 MN/m2; the strength at H.T. depends on devitrification. The process thus offers complex components to be formed by injection moulding, with strength values after sintering similar to those of hot-pressed silicon nitride.

反应键合氮化硅(RBSN)可用作在大气压力下约1800℃的氮气中进行后致密化过程的起始材料。所用的助烧剂类似于热压和无压烧结中使用的助烧剂(例如MgO, Y2O3)。它们可以在氮化之前添加到硅粉中,或者在MgO的情况下,通过将蒸汽扩散到预成型的RBSN中。高密度(理论上的98.5%)已经实现,同时只有6.2%的收缩。瞬时强度约为1000 MN/m2;高温的强度取决于脱硝作用。因此,该工艺提供了通过注塑成型的复杂部件,烧结后的强度值与热压氮化硅相似。
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引用次数: 34
Effect of data scatter on apparent thermal stress failure mode of brittle ceramics 数据散射对脆性陶瓷表观热应力破坏模式的影响
Pub Date : 1979-07-01 DOI: 10.1016/0390-5519(79)90019-X
G. Ziegler , D.P.H. Hasselman
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引用次数: 2
On the fracture strength of tape-casted alumina substrates 胶带浇注氧化铝基材的断裂强度
Pub Date : 1979-07-01 DOI: 10.1016/0390-5519(79)90018-8
C. Fiori, G. Fusaroli, A. Krajewski, P. Vincenzini
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引用次数: 3
Effect of titanate additions on sintering temperature of Al2O3 钛酸盐添加量对Al2O3烧结温度的影响
Pub Date : 1979-07-01 DOI: 10.1016/0390-5519(79)90017-6
G. Wroblewska

The effect of small additions of magnesium titanate, calcium titanate, strontium titanate, and barium titanate on the sintering temperature of aluminum oxide was investigated. The dependence of linear shrinkage and density on sintering temperature and dopant concentration and type was studied. X-ray analysis, microscopic examination, and electron microprobe analysis indicate that sintering occurred through a liquid phase and that Ti4+ diffused into the Al2O3 grains. When CaTiO3, SrTiO3, and BaTiO3 were added, the compounds 3CaO · Al2O3, SrO · 6Al2O3, and BaO · 6Al2O2 were formed. The sintering temperature was reduced to 1500°C by adding less than 2 mol% of magnesium, calcium, strontium, or barium titanate.

研究了钛酸镁、钛酸钙、钛酸锶和钛酸钡的添加量对氧化铝烧结温度的影响。研究了线收缩率和密度与烧结温度、掺杂剂浓度和类型的关系。x射线分析、显微检查和电子探针分析表明,烧结是通过液相进行的,Ti4+扩散到Al2O3晶粒中。当添加CaTiO3、SrTiO3和BaTiO3时,形成3CaO·Al2O3、SrO·6Al2O3和BaO·6Al2O2化合物。通过加入低于2mol %的镁、钙、锶或钛酸钡,烧结温度降至1500℃。
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引用次数: 1
Mechanisms of hot pressing of magnesium oxide powders 氧化镁粉末热压成型机理研究
Pub Date : 1979-04-01 DOI: 10.1016/0390-5519(79)90033-4
R. Pampuch

Estimation of the rate controlling mechanisms of mass transport during the initial, Intermediate and a portion of the final stage of hot pressing of powder compacts by an adequate application of the theory of creep of non-porous polycrystals at elevated temperature is first discussed and their significance for understanding of the relations between powder characteristics and their densification during hot pressing stressed. Review of recent developments of the creep theory indicates that if intraparticle (intracrystallite) i.e. dislocation mechanisms are acting to a negligible extent only, the steady-state strain rate ϵ, should be controlled entirely either by boundary reactions (emission/absorption of point defects at sources and sinks, e.g. at boundary line-defects) or by diffusion between sources and sinks (Nabarro-Herring and/or Coble creep). An analysis has been made in these terms of ϵ observed with well characterised MgO powders, having a rather uniform crystallite size, during hot pressing at 775–975K under loads of PA = 60–295 MPa. Two types of powders, obtained by thermal decomposition of Mg(OH)2 at different temperatures, have been studied, namely i. powders constituted by well-annealed fine crystallites (d = 28–56 nm) showing no lattice microstrains, and ii. powders constituted by fine crystallites (25–45 nm) showing appreciable microstrains of the lattice and, consequently, a high density of the line defects. Experimental determination of the stress sensitivity, n, particle sensitivity, m, and true activation energy for creep, Qc, has shown that the data correspond very closely to ϵsPA2d in the first, and to ϵsPAd3 in the second case, respectively. The first situation is expected for strain rates controlled by boundary reactions while the second for the ones controlled by Coble creep, respectively. The different rate-controlling mechanisms enable to explain rationally the different densifications obtained under comparable conditions of hot pressing with the two types of MgO powders.

本文首先讨论了利用高温下无孔多晶蠕变理论对粉末压坯热压初期、中期和部分最终阶段的质量输运速率控制机制的估计,及其对理解热压应力下粉末特性与其致密化之间关系的意义。对蠕变理论最新发展的回顾表明,如果颗粒内(晶内)即位错机制仅在可忽略的程度上起作用,则稳态应变率λ应该完全由边界反应(源和汇点缺陷的发射/吸收,例如在边界线缺陷处)或源和汇之间的扩散(Nabarro-Herring和/或Coble蠕变)控制。在PA = 60-295 MPa的载荷下,在775-975K的热压过程中,用表征良好的MgO粉末观察到的,具有相当均匀的晶粒尺寸,在这些条件下进行了分析。研究了在不同温度下由Mg(OH)2热分解得到的两种粉末,即由退火良好的细晶(d = 28 ~ 56 nm)组成的粉末,没有晶格微应变;由细晶(25-45 nm)组成的粉末显示出明显的晶格微应变,因此具有高密度的线缺陷。对应力敏感性n、颗粒敏感性m和蠕变真活化能Qc的实验测定表明,第一种情况下的数据与ϵs∝PA2d非常接近,第二种情况下的数据与ϵs∝PAd3非常接近。由边界反应控制的应变率出现第一种情况,由Coble蠕变控制的应变率出现第二种情况。不同的速率控制机制可以合理地解释两种MgO粉末在热压条件下获得的不同密度。
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引用次数: 7
Observations on the grain-boundary of Al2O3 bicrystals Al2O3双晶晶界的观察
Pub Date : 1979-04-01 DOI: 10.1016/0390-5519(79)90028-0
O. Maruyama, W. Komatsu ∗

The grain-boundary thickness of alumina bicrystals, fabricated without the aid of sintering additives and pressure, was measured with an optical microscope. The thickness was 500 to 550 Å and independent of the tilt angle. Impurities segregated at the grain-boundary and the surface of the same sample was studied with an ion microanalyser. The segregation of Ca and Si at both interfaces was noticeable but that of Mg was not. The thickness of the segregation region for both interfaces was 600 to 800 Å. The spheroidization of tubular voids into pores at the grain-boundary was controlled by surface diffusion. Discussion of the fabrication process of the bicrystal in terms of initial sintering kinetics concluded that the process was controlled by the surface diffusion.

用光学显微镜测量了在没有烧结添加剂和压力的情况下制备的氧化铝双晶的晶界厚度。厚度为500到550 Å,与倾斜角度无关。用离子微量分析仪研究了同一样品在晶界和表面分离的杂质。Ca和Si在两个界面处的偏析明显,而Mg的偏析不明显。两个界面的偏析区厚度均为600 ~ 800 Å。管状孔洞在晶界处球化成孔隙受表面扩散控制。从初始烧结动力学的角度讨论了双晶的制备过程,得出该过程受表面扩散控制的结论。
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引用次数: 15
Effects of strain energy on precipitate morphology in MgO 应变能对MgO中沉淀形态的影响
Pub Date : 1979-04-01 DOI: 10.1016/0390-5519(79)90029-2
A.F. Henriksen, W.D. Kingery

Differences between the morphology of MgFe2O4 precipitates, which form octahedra with {111} habit planes and grow into dendritic forms propagating along 〈100〉; MgCr2O4 and MgAl2O4, which assume plate-like morphology with a {100} habit plane; and Sc2O3, which precipitates as randomly oriented platelets, are discussed in terms of the differences in strain energy associated with exsolution of the phases in MgO. The strain energy effects, which occur both during nucleation and subsequent growth, provide a rational explanation of the observed behavior.

MgFe2O4析出相形态的差异,形成具有{111}习性面的八面体,沿< 100 >方向生长为枝晶;MgCr2O4和MgAl2O4,呈{100}习惯面片状;和Sc2O3,沉淀为随机取向的片状,讨论了在MgO中相的析出相关的应变能差异。应变能效应发生在成核和随后的生长过程中,为观察到的行为提供了合理的解释。
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引用次数: 7
Fabrication of stabilized ZrO2 by hot petroleum drying method 石油热干燥法制备稳定ZrO2
Pub Date : 1979-04-01 DOI: 10.1016/0390-5519(79)90030-9
Su-il Pyun

A series of MgO- and CaO- partially and fully-stabilized ZrO2 bodies were produced from sulfate and acetate powders using a wet chemical drying method (“ hot petroleum drying method ”). The optimum sintering conditions for powders produced from sulfates and acetates were found: calcining at 1200°C for 2–5 h, followed by sintering for 5 h at 1600°C. This drying process proved to be a very effective method for preparing stabilized ZrO2 without conventional ceramic process of mixing, milling, and granulating.

用湿式化学干燥法(“热石油干燥法”)从硫酸盐和醋酸盐粉末中制备了一系列MgO-和CaO-部分和完全稳定的ZrO2体。确定了硫酸盐和醋酸酯粉末的最佳烧结条件:在1200℃下煅烧2-5 h,然后在1600℃下烧结5 h。事实证明,这种干燥工艺是制备稳定ZrO2的一种非常有效的方法,无需传统的陶瓷混合、研磨和造粒工艺。
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引用次数: 1
Transparent hot-pressed alumina 透明热压氧化铝
Pub Date : 1979-04-01 DOI: 10.1016/0390-5519(79)90032-2
J.G.J. Peelen

The densification of alumina to nearly full density continuous hot pressing is described. The influence of the atmosphere on hot pressing is discussed as well as the influence of the process parameters temperature, pressure and transit rate. The microstructure of hot-pressed alumina is examined and compared with that of normally sintered alumina. X-ray diffraction is applied to investigate a possible crystallographic texture of the grains in hot-pressed alumina. The optical properties of the material are treated in a second paper.

叙述了氧化铝连续热压致密化至接近全密度的过程。讨论了气氛对热压的影响,以及工艺参数温度、压力和传递速率的影响。研究了热压氧化铝的微观结构,并与普通烧结氧化铝进行了比较。应用x射线衍射研究了热压氧化铝中晶粒可能的晶体结构。该材料的光学特性将在第二篇论文中讨论。
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引用次数: 9
Submicron TiO2ZrO2 powders produced by vapor phase reaction of TiCl4ZrCl4O2 system TiCl4气相反应制备亚微米TiO2ZrO2粉体ZrCl4O2体系
Pub Date : 1979-04-01 DOI: 10.1016/0390-5519(79)90034-6
Y. Suyama, M. Tanaka, A. Kato

Submicron TiO2ZrO2 powders were prepared by the vapor phase reaction of the TiCl4ZrCl4O2 system. The phases appeared were TiO2ss, ZrO2ss and ZrTiO4ss. The major crystal forms of TiO2 and ZrO2 were rutile and tetragonal system, respectively. Pure TiO2 was predominantly anatase and consisted of single crystalline particles with square and plate-like shape. As ZrCl4 concentration increased, the particle size decreased, the content and lattice constants of rutile increased and particles became polycrystalline. The compound ZrTiO4 was formed most abundantly as the ratio ZrCl4/TiCl4 approached 1 and the effective reaction temperature was raised. It was found that TiCl4 accelerates the oxidation of ZrCl4 and ZrCl4 retards that of TiCl4 in the vapor phase reaction of the TiCl4ZrCl4O2 system. It was concluded that the formation process of TiO2ZrO2 particles consists of the preferential nucleatoin of TiO2 and the growth by codeposition of TiO2 and ZrO2.

采用TiCl4ZrCl4O2体系气相反应制备了亚微米级TiO2ZrO2粉体。出现的相为TiO2ss、ZrO2ss和ZrTiO4ss。TiO2和ZrO2的主要晶型分别为金红石型和四方晶型。纯TiO2主要为锐钛矿,由方形和片状的单晶颗粒组成。随着ZrCl4浓度的增加,颗粒尺寸减小,金红石的含量和晶格常数增大,颗粒呈多晶状。当ZrCl4/TiCl4比接近1时,提高有效反应温度,化合物ZrTiO4生成量最大。在TiCl4ZrCl4O2体系气相反应中,TiCl4加速ZrCl4的氧化,ZrCl4延缓TiCl4的氧化。结果表明,TiO2ZrO2颗粒的形成过程是由TiO2优先成核和TiO2与ZrO2共沉积的生长过程组成的。
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引用次数: 3
期刊
Ceramurgia International
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