Comparative study of the fabrication of ultrafine Ti（C,N）-based cermets by spark plasma sintering and conventional vacuum sintering

Spark plasma sintering (SPS) and conventional vacuum sintering (VS) were employed to fabricate ultrafine Ti(C,N)-based cermets. The shrinkage behavior, microstructure, and porosity and mechanical properties of the samples fabricated by SPS were compared with those of the samples sintered by VS using optical microscopy, scanning electron microscopy, universal testing machine, and rockwell tester. The results are as follows: (1) The shrinkage process occurred mainly in the range of 1000-1300℃ during the VS process, and only a 0.2% linear shrinkage ratio appeared below 800℃；during the SPS process, a 60% dimensional change occurred below 800℃ as a result of pressure action. (2) By utilizing the SPS technique, it is difficult for obtaining fully dense Ti(C,N)-based cermets. Due to the much existence of pores and uncombined carbon, the mechanical properties of the sintered samples by SPS are inferior to sintered ones by VS. (3) grain size of the samples sintered by SPS is still below 0.5μm, but not by VS; because of low sintering temperature, there are no typical core/rim structures formed in the sintered samples by SPS1; the main microstrures of the sintered samples by SPS2 are a white core/grey shell sstructure, whereas by VS show a typical black core.grey shell structure.     

Phase Evolution during the Sintering of Submicron Ti(C,N)-Based Cermets

1 IntroductionTi(C,N)-based cermets consist Inainly ofhard carbonitride grains embedded in the toughbinder phase that is based on Co or Ni[l].MozC or WC in cermts imProves usually thewetting of carbonitride grains by the binder[2].Most of the carbonitride particles have core-rimstrUcture shown as figUre 1. The formationmechanism of this delicatC strUctUre is not yetclearly understood. Suzch et al.[3] prOPosedthe dissoluhon of Mo2C and TiC particles intoliquid Ni and the reprecipitatio…     

EFFECT OF Mo AND Mo2C ON THE MICROSTRUCTURE AND PROPERTIES OF THE CERMETS BASED ON Ti（C,N）

Effect of Mo and Mo2 C on the microstructure and properties of Ti（C,N）-based cermets was investigated in this article. The results have indicated that the weight percentage of Mo from 5 to 10 can reduce Ti（C,N） grain diameter and thickness of the rim, and Ti（C,N） grain can be wetted by Ni-Cu-Mo liquid so as to get small contiguity of Ti（C,N） grain. In that way, the transverse rupture strength of Ti（C,N）-based cermets has reached 1800-1900 MPa; the fracture toughness has been due to 16-18 MPa.m1/2. But 15 wt pct Mo was not more effective on Ti（C,N）-based cermets, because the thickness of the rim becomes larger. In the circumstance of Mo2 C, 5 wt pct Mo2 C was good for microstructure and properties of Ti（C,N）-based cermets, but 11 wt pct Mo2C has resulted in larger contiguity of Ti（C,N） grain and big Ti（C,N） grain diameter so as to reduce transverse rupture strength and fracture toughness. So that, the effect of Mo on Ti（C,N）-based cermets is better than Mo2C.     

Effect of Powder Particle Size on the Properties and Microstructure of Ti(C,N)-Based Cermet

1 IntroductionTo improve the durability of Ti(C, N)-basedcermet, many scholars have gained some measures, for example, using advanced sintering methods, Processing HIP blot isostatic pressing)trCdrieflt. Later in 1990's, there are a few reports on submicron cermets [1, 2].In this Study, we have characterized themicroS~ture of tWo cermets and interpretedthe difference between them. Moreover the effect of temper~ on phase transition and lattice-consuls of main Phases and the gradingsof main…     

Effect of sintering on microstructures and properties of sub-micron Ti （C, N）-based cermets

The influence of different sintering processes, including vacuum sintering, vacuum sintering followed by HIP and sintering-HIP, on the microstructure and properties of sub-micron Ti(C,N) cermets with various binder contents was studied. Image analysis based on back-scattered electrons image observations was used to determine the morphologic and structural characteristics. Transverse rupture strength(TRS), hardness, fracture toughness were measured and TRS data were treated by Weibull statistics further. It is shown that a very significant improvement in TRS can be obtained by HIP or sintering-HIP treatment for the alloys with lower and middle binder content at the controlled cooling rate, but the effect is not obvious for the alloys with higher binder content. HIP is also helpful for improving the hardness of sub-micron Ti(C,N) cermets, however, but can lower the fracture toughness. The varia-tion of these properties was interpreted in terms of the difference in morphologic and structural characteristics.     

Formation of carbonitride precipitates in hardfacing alloy with niobium addition

Niobium, as the most effective second-phase forming element, was added in the Fe-Cr13-C-N hard-facing alloy to get carbonitride precipitates. Morphology and composition of carbonitride in the hardfacing alloy were studied by optical microscopy, scanning electron microscopy, and electron probe microanalyzer. The ther-modynamics and the effect on the matrix of the formation of carbonitride were also discussed. It was found that niobium carbonitrides are complex Nb(C, N) precipitate distributed on grain boundary and matrix of the hardfacing alloy. Under as-welded condition, primary carbonitride particles were readily precipitated from the hardfacing alloy with large size and morphology as they were formed already during solidification. Under heat treatment condition, a large number of secondary carbonitrides can pre-cipitate out with very fine size and make a great secondary hardening effect on the matrix. As a result, addition of niobium in the hardfacing alloy can prevent the formation of chromium-rich phase on grain boundaries and inter-granular chromium depletion.     

Microstructure and mechanical properties of hot isostatically pressed cermets with TiN coatings

To increase the adhesion strength between the coating and the substrate, sintered Ti（C,N）-based cermets were selected and deposited with monolayer TiN using a multiarc ion-plating technique; subsequently, hot isostatic pressing （HIPhag） treatment was performed at 1000℃ using nitrogen pressure up to 110 MPa. The mechanical properties of cermets after a coating process and subsequent HIPing treatment have been evaluated with respect to the hardness, the residual stress, and the coating adhesion. The results show that atter the HIPing process, there was a higher increase ha critical load ha the TiN-coated cermets with lower surface roughness compared with those with higher surface roughness. In all cases, the residual stress was found to be compressive. The effects of substrate surface roughness and posttreatment on the adhesion strength of the coatings were thus investigated. It was also fotmd that the HIPing posttreatment process is well suited for hacreasing the adhesion strength between the coating and the substrate.     

Influence of preparation process on sintering behavior and mechanical properties of ultrafine grained Ti（C, N）-based cermets

The influences of forming and sintering processes on distortion, cracking as well as mechanical properties of sintered bodies of ultrafine grained Ti（C, N）-based cermets were investigated. The results show that lubricant is indispensable to fabrication of ultrafine Ti（C, N）-based cermets, however, with low binder content in powder mixture, the lubrication action of paraffin is attenuated. A appropriate level of 2% （mass fraction） paraffin is determined for a cermet with binder content of 36% （mass fraction）. It is also found that the influence of compaction pressure on distortion and cracking of sintered bodies presents a complex relationship. A relatively lower or higher compaction pressure, less than 100 MPa and more than 400 MPa respectively, favors uniform density distribution in green compact. The heating rate of sintering should be strictly controlled. Too fast heating rate results in enclosed pores to burst and forms large size pores in sintering body. A heating rate of 3 ℃/min is recommended.     

Characterization of phase transformation and microstructure of nano hard phase Ti（C,N）-based cermet by spark plasma sintering

By means of optical microscope (OM), scanning electron microscope (SEM) and transmission electron microscope (TEM), the process of densification, the characterization of phase transformation and the microstructure for spark plasma sintering (SPS) nano hard phase Ti(C, N)-based cermet were investigated. It is found that the spark plasma sintering (SPS) enables the nano hard phase Ti(C,N)-based cermet to densify rapidly, however, the full densification of the sintered samples can not be obtained. The rate of phase transformation is significantly quick.When being sintered at 1 200℃ for 8 min, Mo2C is completely dissolved, and TiN dissolves into TiC entirely and disappears. Above 1200℃, Ti(C,N) begins to decompose and the atoms of C and N separate from Ti(C,N) resul-ting in the generation of N2 and the graphite. Due to the denitrification and the graphitization, the density and the hardness of sintered samples are rather low. The distribution of grain size of the sample sintered at 1350℃ covers a wide range of 90-500 nm, and most of the grain size are about 200 nm. The hard phase is not of typical core-rim structure. Oxides on the surface of particles can not be fully removed and present in sample as titanium oxide TiO2.Graphite exists in band-like shape.     

Effects of molybdenum on the microstructure and mechanical properties of Ti（C,N）-based cermets with low Ni

The effects of Mo on the microstructure and mechanical properties of Ti（C,N）-based cermets with low Ni have been studied systematically. Different contents of Mo （4-12 wt.%） were added into Tl（C,N）-based cermets. Specimens were fabricated by conventional powder metallurgy and vacuum sintered at temperatures of 1440, 1450, and 1460℃ individually. The microstructure and fracture morphology were investigated by scanning electron microscope, and the mechanical properties such as transverse strength and hardness were measured. The results show that the microstructure is uniform and the thickness of rim phase is moderate when the content of Mo is 8 wt.%; the mechanical properties of the specimens sintered at 1450℃ are better than those sintered at 1440 and 1460℃. The integrated properties of transverse strength and hardness are the best when the content of Mo is 8 wt.% and the sintering temperature is 1450℃.     

高能球磨制备Ti(C,N)基金属陶瓷硬质相超微粉

对Ti(C,N)基金属陶瓷硬质相TiC、TiN、WC原料粉在不同球料比、不同球磨时间试验条件下进行高能球磨,探讨了TiC、TiN、WC粉体的高能球磨超细化机理和球磨行为特征。试验表明随球料比和球磨时间的增加,TiC、TiN、WC粉体得到细化,但达到一个极小值后细化趋于稳定。利用沉降法测试粉末粒度分布并在扫描电镜下观察粉末的形貌和粒度,发现在10∶1球料比下球磨96h后可以有效制备得颗粒粒度为0.20μm的金属陶瓷硬质相超微粉。     

Synthesis of titanium carbide by thermo-chemical methods with TiH2 and carbon black powders

A new synthesizing method for producing submicron TiC powders was studied by using TiH₂ and carbon black powders. It is well known that hydrogen absorption transforms titanium from metal (h.c.p.) to brittle hydride (f.c.c.) powders by ball-milling. This research focused on obtaining submicron-sized TiC powders from the ball-milled mixture of TiH₂ and carbon black by thermal treatment. The hydrogen, carbon, iron, and oxygen composition changes in the mixed powders were analyzed. Thereafter, a differential thermal analysis (DTA) test was performed to observe change of phase with ball-milling time. The TiC powders were obtained by heat treating the powders milled for 5h at various temperatures (600–1200°C). The phase microstructure was investigated via DTA, X-ray diffraction (XRD), and scanning electron microscope (SEM). The mixture milled for 2h had an f.c.t. structure containing 66.73 at. %H transformed to f.c.c. by milling for 4h. After 5h of ball-milling, submicron-sized particles of 273 nm were obtained. At the isothermal heat-treating temperature of 500°C, the Ti single phase was formed completely, and the TiC phase of lattice parameter 0.310 nm was completely formed over the temperature of 1000°C.     

Study,on Influence of Processes on the Dehydrogenation Performance of NaAlH4EI北大核心CSCD

In this paper, the effects of preparation process, ball-milling equipments, storing time and ball-milling time on the dehydrogenation performances were analyzed. All the samples were ball-milled by planetary ball mill except for sample 3 which was ball-milled by high-energy vibration ball mill. The results indicate that the above mentioned influence factors present obvious effect on the dehydrogenation performances of NaAlH4. The dehydrogenation amount of the samples turned up and down during ball milling increases by 50wt%. Compared to the samples prepared by planetary mill, the dehydrogenation amount of samples prepared by the high-energy vibration ball mill increases markedly. The results from studying on storing time and milling time show that the dehydrogenation amounts of the samples milled by planetary mill and laid aside for 24 h get an obvious increase. In addition, the amount of the hydrogen release of the samples milled for different time with planetary mill presents significantly difference. The amount of the hydrogen release of the sample milled for 80 min is higher than those milled for 100, 40 and 60 min. However, compared to other influence factors, the effect of ball-milling time on NaAlH4 is smaller.     

Study on Influence of Processes on the Dehydrogenation Performance of NaAlH4

分析了制备工艺过程、球磨设备、试样放置时间以及球磨时间对NaAlH4放氢性能的影响。其中除了试样3是采用高能球磨机外,其它所有试样均采用行星式球磨机。结果表明,这些因素对NaAlH4放氢性能的影响非常明显。试样在球磨过程中经过上下翻转后,其放氢量明显比不翻转高出了50%(质量分数)。不同球磨设备研究结果显示,试样3经过高能振动球磨机球磨后,其放氢量比行星式球磨机制备的试样的放氢量明显提高了。试样放置时间与试样球磨时间的研究结果显示,制备好的球磨试样经过24 h放置后,其放氢量明显提高。此外,试样经过不同时间球磨后,其放氢量也有明显的不同。经研究发现,球磨80 min试样的放氢量比球磨100 min和球磨40和60 min试样的放氢量要高,但和其它的影响因素相比,球磨时间对NaAlH4放氢性能的影响相对较小     

机械合金化对Cu—SiC粉末烧结性能的影响

本文主要讨论了Cu—SiC复合粉体经球磨后的烧结性能变化情况，通过对球磨后Cu—SiC复合粉体进行XRD、DSC分析，来了解球磨过程对Cu—SiC粉体以及烧结体性能的影响。X射线结果表明：随着球磨加工的进行，粉体的晶粒尺寸减小，Cu衍射峰消失。DSC分析的结果表明：在粉体中储存大量的能量，这些能量的储存降低了复合粉体的烧结温度，改善了烧结体的强度。烧结实验结果表明：在800℃的烧结温度下，经20h球磨后，粉体的抗折强度达到了15MPa以上。     

高能球磨制备Ni60-TiB2纳米金属基陶瓷结构喂料及其结构特性

以Ni60和TiB2粉为原料,在氩气保护下采用高能球磨技术制备Ni60-TiB2纳米金属基陶瓷结构喂料,并研究了其结构特性。用XRD、SEM、EDS和激光粒度分布仪等对粉末进行表征和分析,结果表明:Ni60-TiB2粉体在室温条件下,经20h球磨后其晶粒尺寸和微观应变分别为38nm和0.237%,显微组织为纳米级硬质相TiB2均匀弥散分布于粘结相NiCr上,粉末近似球状,流动性良好,稍加过筛后可直接用于HVOF喷涂。     

TiC粉末微晶化的正电子湮设研究

用正电子湮没方法研究了TiC粉末的微观结构缺陷。结果表明，TiC在球磨过程中，发生了非晶晶化反应，形成了微晶，同时缺陷向内表面聚集，并且球磨后平均粒径明显变小，使粉末的外表面增加，从而压制时更容易成型。     

Application of ball-milled powder mixture to intermetallics coating through reaction synthesis

The application of ball-milling for reactant powders to improve the intermetallic coating reaction was examined. Ni-50 at.% Al powder compacts milled at three different ball-to-powder weight ratios in a planetary mill were analyzed by differential scanning calorimetry (DSC) and coated onto mild steel through the reaction synthesis in a hot press. The effects of ball-milling on the coating reaction in the hot press were compared with those in the reaction synthesis in DSC. The experimental results show that the particle size of the elemental powders was decreased by ball-milling, and that the coating reaction in the hot press was enhanced by ball-milling for the reactant powders, unlike the reaction synthesis in DSC. This improvement was attributed to the increase in the density of the reactant compact by the load applied during the reaction.     

球磨法制备纳米TiC及其生成机理

采用高能球磨法制备纳米TiC颗粒,通过对不同球磨时间试样进行X射线衍射分析、扫描电镜及透射电镜进行形貌观察,得出球磨过程中TiC的生成机理。结果表明,球磨过程中,首先石墨和钛粉细化,石墨形成片状而钛粉形成细小颗粒;随着球磨时间的延长,片状石墨包裹钛粉;当磨球碰撞时达到Ti和C反应温度,Ti和C发生反应产生TiC,反应放出的热量维持反应的进行。制备的TiC粒度为10～100nm。     

高密度纯钨的低温活化烧结工艺及其致密化行为

采用溶胶喷雾干燥-煅烧-氢热还原法制备了BET粒径为0.21μm的超细纯钨粉末,并利用球磨处理进一步活化粉末。研究了超细纯钨粉末形貌及其性能随球磨时间的变化特征,探索了未球磨、球磨5h及球磨10h3种超细纯钨粉末烧结致密工艺,此外还详细研究了纯钨烧结体组织形貌、晶粒尺寸及显微硬度等性能随烧结温度及球磨时间的变化规律。结果表明,球磨处理对超细纯钨粉末的烧结起到了极大的活化作用,由球磨10h粉末制成的压块在1900℃下烧结2h其致密度即可达97.3%,比传统微米级纯钨粉末制成的压块达到相同烧结致密度的温度降低了600℃以上。同时,球磨处理可以大幅降低钨粉的起始烧结温度和再结晶温度,获得组织更加均匀细小、力学性能(硬度)更加优良的钨烧结体。