Synthesis and Sintering of Nanocrystalline Barium Titanate Powder under Non-Isothermal Conditions. Part 6. Structure,Grain Boundaries,and Dielectric Properties of Barium Titanate Obtained by Various Sintering Methods

The grain boundary structure of barium titanate obtained by controlled-rate sintering and high-pressure sintering (HPS), and the dependence of dielectric properties on grain size and consolidation method were studied. It was shown that sintering without the application of pressure leads to a diffusion-controlled formation of equilibrium grain boundaries with minimal impedance factor, which minimally decrease the dielectric constant of the ceramics. HPS results in the formation of non-equilibrium grain boundaries which have a large free volume, and which substantially decrease the dielectric constant. The Curie-Weiss constant was analyzed from the viewpoint of a matrix structural model, and a «brick-wall» model.     

纳米晶W-25Cu复合粉末烧结行为的研究

研究了机械合金化工艺制备纳米晶W-25Cu复合粉末的烧结致密化和晶粒长大行为,并考察了一种新型晶粒长大抑制剂对抑制W晶粒长大的作用,探讨了其作用机理。结果表明,烧结致密化和晶粒长大强烈依赖于烧结温度和时间。经1200℃烧结30min后,烧结相对密度和W晶粒尺寸为97.7%和310nm。新型晶粒长大抑制剂抑制W晶粒长大效果明显。     

Kinetics of Initial Coarsening During Sintering of Nanosized Powders

Grain growth during sintering is a critical issue for the manufacture of nanocrystalline bulk materials from nanosized powders. The grain growth process during sintering can be viewed as consisting of two parts: initial coarsening during early and intermediate stages of sintering and latter stage grain growth during the final stage of sintering. The latter stage grain growth is the normal grain growth that has been well studied and reported in the literature. The initial coarsening, which often inevitably causes a material to lose nanoscaled grain size characteristics, however, is not well studied at all. In this investigation, the initial coarsening during sintering of nanosized powders was studied by both nonisothermal and isothermal experimental techniques using tungsten as an example material. The results show that the initial coarsening during the heat-up process of a sintering cycle is sufficient to increase the grain size beyond the nanoscale. The kinetics of initial coarsening is found to be linear rather than polynomial, as predicted by the conventional power law of grain growth. The analysis of activation energies showed that surface diffusion is the primary mechanism for interparticle mass transport during the initial coarsening. The linear kinetic behavior could be attributed to the pinning of grain boundaries by surface grooves and high concentration of defects as the result of the synthesis of nanosized powders.     

Sintering of transparent Nd:YAG ceramics in oxygen atmosphere

Yttrium aluminum garnet (YAG) transparent ceramics were fabricated by sintering at oxygen atmosphere. Tetraethyl orthosilicate (TEOS) was added as the sintering additive to control the grain growth and densification. Pores were eliminated clearly at temperature lower than 1700oC, while grain size was around 3 μm. The in-line transmittance was 80% at 1064 nm when samples were sintered at 1710oC. The effect of TEOS was studied in oxygen atmosphere sintering for Nd:YAG transparent ceramics. At higher temperature like 1710oC, the grain growth mechanism was solute drag, while at 1630 and 1550 oC the grain growth was controlled by liquid phase sintering mechanism. And 0.5 wt.% TEOS was the best adding content for Nd:YAG sintered in oxygen atmosphere.     

Sintering kinetics of YAG ceramics

Solid state reactive （SSR） sintering kinetics was observed for YAG ceramics. There were two densification stages in sin- tering process due to its reaction. After the first stage, samples began to expand, then, the second densification stage began. At a heat- ing rate of 10 ℃/min, the sample warped down and warped back to straight. The apparent activation energy of the first densification process was about 522 kJ/mol for the initial shrinkage of A1203 and Y203 mixed powder green-body, which increased in the follow- ing process due to the solid state reaction. In the second densification stage, synthesis reaction of YAG still worked. Green-bodies processed with higher heating rate got more shrinkage at the same temperature than lower heating rate green bodies. And its kinetic field diagram was abnormal, compared with that of other reported ceramics, such as Al203. It was found that the reaction of YAG provided positive effect to the sintering driving force. The apparent activation energy for densification of SSR YAG sintered in ArH5 atmosphere was 855 kJ/mol at temperature holding sintering. And the apparent activation energy for grain growth was 1053 kJ/mol.     

硬质合金真空烧结炉电发热体的设计与计算

真空烧结在硬质合金生产中应用广泛,本文对真空烧结炉电发热体的功率、结构以及发热元件的设计与计算均作了较为详细的介绍,对工厂技术人员有一定的参考价值。     

Sintering Behavior of Porous Titanium Fiber Materials

The porous titanium fiber materials with open porosity were successfully prepared by the vacuum sintering technology. The morphology characteristics of sintering neck of porous titanium fiber materials were investigated by scanning electron microscopy （SEM）. The results show that the formation and growth of sintering neck of porous ti- tanium fiber material approximately follow the rule that the primary mechanism is grain boundary diffusion and sub- sidiary mechanisms are other diffusion mechanisms during the sintering process. The formation and growth of the sintering neck depend mainly on the sintering temperature and slightly on the soaking time. The sintering system of porous titanium fiber material was determined and the equation of the sintering neck＇s length was established.     

烧结曲线(MSC)在200nm WC-Co硬质合金晶粒长大模拟中的应用

利用Master Sintering Curve晶粒长大方程模拟了200 nm WC-Co硬质合金固相烧结和液相烧结过程中WC晶粒的长大曲线,并与实际烧结实验相比较.烧结实验选用的WC的粒度为200 nm,采用球磨混料,经过普通模压,压制压力为200 MPa,制备出直径为20 mm、厚度为3～5 mm的压坯.烧结实验在管式炉中进行,烧结气氛为高纯氢气,加热速率为10℃·min<'-1>,烧结时间为10 min.结果表明:Master SinteringCruve模型在WC-Co硬质合金烧结过程中具有很好的适用性.计算出的品粒长大随烧结温度的变化与实际烧结实验具有很好的一致性.经过固相烧结,200 nm的WC长大到254 nm,烧结激活能为450 kJ·mol<'-1>,但体积扩散和晶界扩散机制的区别不是很明显.经过液相烧结WC颗粒继续长大到287 nm,此时固液相的界面反应控制整个烧结过程,烧结激活能为474 kJ·mol<'-1>.压坯烧结激活能的增加,将显著抑制在烧结过程中WC晶粒的长大.     

江西锂云母—石灰石烧结工艺的改进研究

采用锂云母,石灰石,石灰为原料,ＬｉＯＨ结晶母液为添加剂,进行了提锂烧结工艺研究。初步结果表明,烧结温度为７５０－８５０℃时,Ｌｉ２Ｏ的溶出率可达９１％左右,与原有的锂云母－石灰石烧结工艺相比,烧结温度可降低１５０℃左右,Ｌｉ２Ｏ的溶出率可提高１１％左右。     

Nd-Fe-B磁体烧结致密化过程的研究

定量描述了Nd-Fe-B磁体的烧结致密化过程, 分析了有效稀土含量、合金粉末粒度与烧结致密化过程的关系, 讨论了Nd-Fe-B磁体烧结过程的致密化机制. Nd-Fe-B磁体烧结致密化过程可分为3个阶段, 即致密化过程迅速进行阶段、缓慢进行阶段、相对稳定阶段;随着烧结温度的上升, 第一阶段表现得更为突出, 第二阶段对应的烧结时间区段大大缩短. 有效稀土含量的提高、合金粉末粒度的减小显著促进Nd-Fe-B磁体烧结致密化过程. 主相颗粒重排以及主相颗粒长大与形状适位性变化是Nd-Fe-B磁体烧结过程的两类主要致密化机制, 而且后者对于Nd-Fe-B烧结磁体实现完全致密化起着决定性的作用.     

Formation and Sintering Behavior of Nanocrystalline Fe-Ni Powder by Mechanical Alloying

Thepotentialapplicationofnanostructuredma terialsusedasnovelstructuralorfunctionalengi neeringmaterialslargelydependsontheconsolida tionofpowdersbywhichthebulknanostructuredsolidsaremade .Theretentionofthemetastablemi crostructureintheconsolidationprocessismandato ryforpreservingthesuperiormechanical,electricalorcatalyticpropertiesofthematerial.Severalau thorsshowedthatthepressure assistedsinteringisadequateforbothreachingfulldensityandprevent inggraingrowth ,besidesthenanostructuredmateri als…     

WC-Co硬质合金烧结过程中的晶粒长大现象研究

在分析晶粒长大机理的基础上，指出在WC—Co硬质合金烧结过程中，WC晶粒的长大为正常长大和异常长大这两种方式并存，且在烧结早期WC晶粒就开始长大，并提出了可抑制WC晶粒长大的具体措施。     

Effects of Dysprosium Oxide Doping on Microstructure and Properties of Barium Titanate Ceramic

With the development of mixed integrated cir-cuits , mini mization of high voltage ceramic capacitorcomponents usedin high voltage outletsis required .Inthe past ,the breakdown voltage was raised mainly byincreasingthethickness of capacitors .Butthe most …     

粉末冶金铝合金烧结致密化过程

以纯Al粉为主要原料,添加Cu单质粉末以及Al-Mg、Al-Si中间合金粉,利用粉末冶金压制烧结方法制备出相对密度98%以上的Al-Mg-Si-Cu系铝合金.研究表明,烧结致密化过程主要分为3个阶段:初始阶段(室温~460℃),坯体内首先形成Al-Mg合金液相,液相中的Mg原子分别扩散至Al或Al-Si粉末中,与Al₂O₃反应并破除氧化膜,形成Al-Mg-O等化合物;同时,Al-Cu发生互扩散,形成Al₂Cu等金属间化合物.第二阶段(460~560℃),Al-Cu、Al-Si液相快速填充颗粒缝隙或孔洞,坯体相对密度显著提高;此阶段的致密化机制主要是毛细管力引起的颗粒重排,以及溶解析出导致的晶界平直化.第三阶段(560~600℃),随温度的升高,液相润湿性提高,晶粒快速长大,使得大尺寸孔洞填充,烧结体基本实现全致密,此阶段的致密化主要由填隙机制控制.在铝合金晶界处发现了MgAl₂O₄和MgAlCuO氧化物的存在,推测Al粉表面氧化膜的破除机制与合金成分有关.由于Al-Cu液相在Al表面的润湿速率远高于AlN的生长速率,因为在本体系中未发现AlN的存在.     

A Study of Grain Growth Kinetics in Sintered NdFeB Magnets

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Sintering High Tungsten Content W-Ni-Fe Heavy Alloys by Microwave Radiation

This paper presents a detailed study of microwave (MW) sintering of W-Ni-Fe heavy alloys (WHAs) with tungsten (W) content 90 to 98 mass pct (Ni and Fe mass ratio of 7 to 3) in comparison with conventional (CV) hydrogen sintering. Experimental results show that WHAs were MW sintered to fully dense (≥99 pct of theoretical) when heated to sintering temperatures at a heating rate of 50 K/min to 80 K/min (50 °C/min to 80 °C/min) and isothermally held for 2 to 10 minutes, with sintering cycle times of only 25 to 35 minutes (excluding the cooling time). The desired microstructures of finer W grains, more matrix phases, and lower W contiguity (in 95W and 98W) were produced compared to the counterparts by CV sintering. Such microstructural features offered the alloys excellent tensile properties: ultimate tensile strengths (UTS) 1080 to 1110 MPa and tensile elongation 22.1 to 26.8 pct in 90 to 95W, and UTS 920 MPa and elongation 11.2 pct in 98W. MW sintering appeared to be more effective in fabricating WHAs with W content ≥95 pct. It was observed that the superior UTS with MW-sintered alloys was mainly due to the fast heating and shortened isothermal holding times. Prolonged sintering led to substantial grain coarsening as a result of faster tungsten grain growth in MW sintering, and consequently deteriorated the tensile properties. The grain growth rate constant K achieved was calculated to be 5.1 μm³/s for MW sintering compared to 2.9 μm³/s for CV sintering. Fast heating and short isothermal holding times are thus suggested for the fabrication of WHAs by MW sintering.     

Microstructure of W - Ni - Sn Composites in Relation to Amount of Liquid Phase on Sintering

Microstructure transformation is examined for W - Ni - Sn composites made by liquid-phase sintering at 1200 °C for 1 h; the liquid phase was a eutectic containing 67.5 mass% Ni and 32.5 mass% Sn. There is a nonmonotone dependence of the tungsten grain size in the sintered composites on the volume proportion of liquid phase in the range 6.7–36.8%. The mean grain size in relation to volume proportion of liquid phase in liquid-phase sintering is calculated from rheological sintering theory. The form of the empirical function f(v) is quantitatively demonstrated, which determines the rate of tungsten grain growth on liquid-phase sintering and is dependent on the proportion of matrix in the composite and the size of the liquid phase layer. __________ Translated from Poroshkovaya Metallurgiya, Nos. 7–8(444), pp. 53–57, July–August, 2005.     

烧结温度对高钨重合金性能的影响

研究了烧结温度对高钨含量W—Ni—Fe重合金显微组织及力学性能的影响。结果表明：钨基重合金的显微组织和力学性能与烧结温度密切相关。合适的烧结温度可以使合金具有良好的显微组织和优良的力学性能，而烧结温度较低时，合金中的粘结相分布不均匀，烧结温度较高时，合金中的钨颗粒粗大，两者都会显著降低其力学性能。     

高Ni/Fe比W-Ni-Fe系重合金烧结行为

研究了钨质量分数为90%的高Ni/Fe比W-Ni-Fe系重合金在不同工艺参数(烧结温度、烧结时间等)下的烧结行为.研究结果表明:在相同烧结条件下,随粘结相中NiNe比增加钨合金烧结密度增加,致密化速率提高,同时烧结过程中W晶粒生长速率增大:当Ni/Fe比较低时,钨合金在循环烧结条件下难以实现完全致密化;但对高Ni/Fe比钨合金,循环烧结不仅可以获得比等温烧结更高的烧结密度,而且还可以有效地控制烧结过程中W晶粒的长大,获得细晶钨合金.