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Phase Composition of Samarium Niobate and Tantalate Thin Films Prepared by Sol-Gel Method 溶胶-凝胶法制备铌酸钐和钽酸盐薄膜的相组成
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0002
H. Brunckova, Ľ. Medvecký, E. Múdra, A. Kovalčíková, J. Ďurišin, M. Sebek, V. Girman
Abstract Samarium niobate SmNbO4 (SNO) and tantalate SmTaO4 (STO) thin films (~100 nm) were prepared by sol-gel/spin-coating process on alumina substrates with PZT interlayer and annealing at 1000°C. The precursors of films were synthesized using Nb or Ta tartrate complexes. The improvement of the crystallinity of monoclinic M′-SmTaO4 phase via heating was observed through the coexistence of small amounts of tetragonal T-SmTa7O19 phase in STO precursor at 1000°C. The XRD results of SNO and STO films confirmed monoclinic M-SmNbO4 and M′-SmTaO4 phases, respectively, with traces of orthorhombic O-SmNbO4 (in SNO). In STO film, the single monoclinic M′-SmTaO4 phase was revealed. The surface morphology and topography of thin films were investigated by SEM and AFM analysis. STO film was smoother with roughness 3.2 nm in comparison with SNO (6.3 nm). In the microstructure of SNO film, small spherical (~50 nm) and larger cuboidal particles (~100 nm) of the SmNbO4 phase were observed. In STO, compact clusters composed of fine spherical SmTaO4 particles (~20-50 nm) were found. Effect of samarium can contribute to the formation different polymorphs of these films for the application to environmental electrolytic thin film devices.
摘要采用溶胶-凝胶/旋涂法在具有PZT夹层的氧化铝衬底上制备了铌酸钐SmNbO4(SNO)和钽酸盐SmTaO4(STO)薄膜(~100nm)。使用Nb或Ta酒石酸盐配合物合成了薄膜的前体。通过在1000°C下STO前驱体中存在少量四方T-SmTa7O19相,观察到单斜M′-SmTaO4相的结晶度通过加热而提高。SNO和STO薄膜的XRD结果分别证实了单斜的M-SmNbO4和M′-SmTaO4相,以及微量的正交O-SmNbO4(在SNO中)。在STO薄膜中,发现了单斜的M′-SmTaO4相。用扫描电镜和原子力显微镜分析了薄膜的表面形貌。STO膜比SNO(6.3nm)更光滑,粗糙度为3.2nm。在SNO膜的微观结构中,观察到SmNbO4相的小球形(~50nm)和大立方体颗粒(~100nm)。在STO中,发现了由球形SmTaO4颗粒(~20-50nm)组成的致密团簇。钐的作用有助于形成这些膜的不同多晶型,用于环境电解薄膜器件。
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引用次数: 1
Microstructure, Mechanical Properties and Corrosion Behaviour of Iron - Manganese PM Materials Pressed and Sintered Once and Twice 一次和两次烧结铁锰永磁材料的组织、力学性能和腐蚀行为
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0012
M. Kupková, M. Hrubovčáková, M. Kabátová, M. Kupka
Abstract Elemental iron and manganese powders were blended to form mixtures containing 25, 30 and 35wt.% Mn. Mixtures were compressed into prismatic bars and sintered. Some of the bars were repressed and resintered. Compared to a bar pressed and sintered once, the bar pressed and sintered twice possessed a higher relative density, a higher bending stiffness, and a grid microindentation data set with a lower variance. Bars were immersed in Hank's solution for eight weeks. After this procedure, the bending stiffness were found reduced for all bars except for those pressed, sintered and only repressed, the bending stiffness of which remained unchanged. The repressing has most likely closed up throats connecting the clusters of pores with the free surface of a bar, reducing thus a surface area exposed to a corrosive attack. The resintering has opened up those throats, the electrolyte could fill accessible pores and corrosion weakened the near-surface material, reducing thus a bar's bending stiffness.
摘要将元素铁和锰粉末混合形成含有25、30和35wt%的混合物将混合物压缩成棱柱状棒并烧结。一些酒吧被压抑,并被重新安置。与压制和烧结一次的棒材相比,压制和烧结两次的棒材具有更高的相对密度、更高的弯曲刚度和更低方差的网格显微压痕数据集。酒吧在汉克的溶液中浸泡了八个星期。经过这一过程后,发现除压制、烧结和仅压制的钢筋外,所有钢筋的弯曲刚度都有所降低,其弯曲刚度保持不变。压制很可能封闭了连接孔隙簇和棒材自由表面的喉部,从而减少了暴露于腐蚀性侵蚀的表面积。重新烧结打开了这些喉部,电解质可以填充可接近的孔隙,腐蚀削弱了近表面材料,从而降低了棒材的弯曲刚度。
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引用次数: 0
The Effect of Powder Ball Milling on the Microstructure and Mechanical Properties of Sintered Fe-Cr-Mo-Mn-(Cu) Steel 粉末球磨对烧结Fe-Cr-Mo-Mn-(Cu)钢组织和力学性能的影响
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0009
P. Kulecki, E. Lichańska
Abstract The effect of ball milling powder mixtures of Höganäs pre-alloyed iron Astaloy CrM, low-carbon ferromanganese Elkem, elemental electrolytic Cu and C-UF graphite on the sintered structure and mechanical properties was evaluated. The mixing was conducted using Turbula mixer for 30 minutes and CDI-EM60 frequency inverter for 1 and 2 hours. Milling was performed on 150 g mixtures with (in weight %) CrM + 1% Mn, CrM + 2% Mn, CrM + 1% Mn + 1% Cu and CrM + 2% Mn + 1% Cu, all with 0.6%C. The green compacts were single pressed at 660 MPa according to PN-EN ISO 2740. Sintering was carried out in a laboratory horizontal furnace Carbolite STF 15/450 at 1250°C for 60 minutes in 5%H2 – 95%N2 atmosphere with a heating rate of 75°C/min, followed by sintering hardening at 60°C/min cooling rate. All the steels were characterized by martensitic structures. Mechanical testing revealed that steels based on milled powders have slightly higher mechanical properties compared to those only mixed and sintered. The best combination of mechanical properties, for ball milled CrM + 1% Mn + 1% Cu was UTS 1046 MPa, TRS 1336 MPa and A 1.94%.
研究了Höganäs预合金铁Astaloy CrM、低碳锰铁Elkem、元素电解Cu和C-UF石墨混合球磨粉对烧结组织和力学性能的影响。使用turbulermixer进行混音30分钟,使用CDI-EM60变频器进行混音1小时和2小时。在150 g(重量%)含0.6%C的CrM + 1% Mn、CrM + 2% Mn、CrM + 1% Mn + 1% Cu和CrM + 2% Mn + 1% Cu的混合物中进行铣削。根据PN-EN ISO 2740,绿色压片在660 MPa下进行单次压制。在实验室卧式炉STF 15/450中,在5%H2 - 95%N2气氛中,在1250℃下,以75℃/min的升温速率烧结60分钟,然后以60℃/min的冷却速率烧结硬化。所有钢均以马氏体组织为特征。力学测试表明,与混合和烧结的钢相比,以研磨粉末为基础的钢具有略高的力学性能。球磨后,CrM + 1% Mn + 1% Cu的最佳力学性能组合为UTS 1046 MPa, TRS 1336 MPa, A 1.94%。
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引用次数: 6
Effect of Alloying Type and Lean Sintering Atmosphere on the Performance of PM Components 合金化类型和贫烧结气氛对PM元件性能的影响
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0008
M. V. Sundaram, R. Shvab, S. Millot, E. Hryha, L. Nyborg
Abstract In order to be cost effective and to meet increasing performance demands, powder metallurgy steel components require continuous improvement in terms of materials and process development. This study demonstrates the feasibility of manufacturing structural components using two different alloys systems, i.e. lean Cr-prealloyed and diffusion bonded water atomised powders with different processing conditions. The components were sintered at two different temperatures, i.e. 1120 and 1250 °C for 30 minutes in three different atmospheres: vacuum, N2- 10%H2 atmosphere as well as lean N2-5%H2-0.5%CO-(0.1-0.4)%CH4 sintering atmosphere. Components after sintering were further processed by either low pressure carburizing, sinterhardening or case hardening. All trials were performed in the industrial furnaces to simulate the actual production of the components. Microstructure, fractography, apparent and micro hardness analyses were performed close to the surface and in the middle of the sample to characterize the degree of sintering (temperature and atmosphere) and the effect of heat treatment. In all cases, components possess mostly martensitic microstructure with a few bainitic regions. The fracture surface shows well developed sinter necks. Inter- and trans-granular ductile and cleavage fracture modes are dominant and their fraction is determined by the alloy and processing route.
摘要为了节约成本并满足日益增长的性能要求,粉末冶金钢构件需要在材料和工艺开发方面不断改进。本研究证明了使用两种不同合金体系制造结构部件的可行性,即不同加工条件下的贫铬预合金和扩散结合水雾化粉末。在两种不同的温度(即1120和1250°C)下,在三种不同的气氛中烧结部件30分钟:真空、N2-10%H2气氛以及贫N2-5%H2-0.5%CO-(0.1-0.4)%CH4烧结气氛。烧结后的部件通过低压渗碳、烧结硬化或表面硬化进行进一步处理。所有试验都是在工业炉中进行的,以模拟部件的实际生产。在样品表面附近和中间进行了微观结构、断口形貌、表观硬度和显微硬度分析,以表征烧结程度(温度和气氛)和热处理效果。在所有情况下,部件大多具有马氏体微观结构,并有少量贝氏体区域。断口显示烧结颈发育良好。晶粒间和穿晶韧性和解理断裂模式占主导地位,其分数由合金和加工路线决定。
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引用次数: 0
Properties of Powder Composite Polyhydroxybutyrate–Chitosan-Calcium Phosphate System 粉末复合聚羟基丁酸酯-壳聚糖-磷酸钙体系的性能
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0001
Ľ. Medvecký, R. Stulajterova, M. Giretová, M. Fáberová
Abstract Prepared powder polyhydroxybutyrate – chitosan - calcium phosphate composite system with 10 wt % of biopolymer component can be utilized as biocement which is characterized by the prolonged setting time and achieves wash out resistance after 5 minutes of setting. The origin powder tetracalcium phosphate/nanomonetite agglomerates were coated with the thin layer of biopolymer which decelerates both the transformation rate of calcium phosphates and hardening process of composites. The porosity of hardened composite was around 62% and the compressive strength (8 MPa) was close to trabecular bone. No cytotoxicity of composite resulted from live/dead staining of osteoblasts cultured on substrates.
摘要所制备的含有10wt%生物聚合物组分的粉末聚羟基丁酸酯-壳聚糖-磷酸钙复合体系可以用作生物水泥,其特征是凝固时间延长,凝固5分钟后达到耐冲刷性。在原始粉末磷酸四钙/纳米莫奈石团聚体上涂覆一层生物聚合物,这降低了磷酸钙的转化率和复合材料的硬化过程。硬化复合材料的孔隙率约为62%,抗压强度(8MPa)接近骨小梁。在基质上培养的成骨细胞的活/死染色没有导致复合物的细胞毒性。
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引用次数: 4
Density, Microstructure, Strength and Fractography of Spark Plasma and Conventionally Sintered Mn Steels 火花等离子体和常规烧结Mn钢的密度、组织、强度和断口形貌
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0010
M. Tenerowicz-Żaba, M. Kupková, M. Kabátová, E. Dudrová, M. Džupon, M. Sułowski
Abstract The aim of the study was to investigate Spark Plasma Sintering (SPS) of 1-3%Mn steels and compare the resultant microstructures, strengths and failure mechanisms with those of conventionally sintered materials. SPS was performed in a vacuum of 5 Pa at 1000°C for 15min under a uniaxial pressure of 20 MPa. The heating rate of 100°C/min was applied. For conventional processing, mixtures of powders were prepared in a Turbula mixer for 30 minutes. Samples were single pressed at 660 MPa, according to PN-EN ISO 2740 standard. Sintering of compacts was carried out in a laboratory tube furnace at 1120°C and 1250°C for 60 minutes in a mixture of 95%N2-5%H2. Heating and cooling rates were 75C°/min and 60°C/min, respectively. The density of SPS samples was higher (up to 7.37 g/cm3) than those after conventional sintering (up to 6.7 g/cm3). Yield strengths of SPS samples were in the range 920-1220 MPa, compared to the maximum of 602 MPa for conventionally sintered Fe-3%Mn-0.8%C. Transverse rupture strengths were the same for this alloy, 1234 MPa, but reached 1473 MPa for SPS 2Mn variant. Interfaces in SPS samples were significantly less contaminated with oxides, which is the result of a more favorable microclimate and pressure acting during SPS. These preliminary results indicate that further research on the SPS of Mn steels is warranted.
摘要研究了1-3%Mn钢的放电等离子烧结(SPS)工艺,并与常规烧结材料进行了显微组织、强度和失效机理的比较。SPS在1000°C, 5 Pa真空,20 MPa单轴压力下进行15min。加热速率为100℃/min。对于常规加工,粉末混合物在湍流混合器中制备30分钟。根据PN-EN ISO 2740标准,样品在660 MPa下单次加压。在实验室管式炉中,在1120℃和1250℃的温度下,在95%N2-5%H2的混合物中烧结60分钟。加热和冷却速度分别为75°C/min和60°C/min。SPS样品的密度(高达7.37 g/cm3)高于常规烧结后的密度(高达6.7 g/cm3)。SPS试样的屈服强度在920 ~ 1220 MPa之间,而Fe-3%Mn-0.8%C常规烧结试样的屈服强度最大值为602 MPa。该合金的横向断裂强度相同,为1234 MPa,而SPS 2Mn合金的横向断裂强度达到1473 MPa。SPS样品的界面氧化物污染明显减少,这是SPS过程中更有利的小气候和压力作用的结果。这些初步结果表明,对Mn钢SPS的进一步研究是有必要的。
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引用次数: 2
Plasticity Modelling in PM Steels PM钢的塑性建模
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0004
M. Andersson, V. Angelopoulos
Abstract Simulations are continuously becoming more and more important to predict the behaviour of materials, components and structures. Porous materials, such as PM, put special demands on the material models used. This paper investigates the application of the Gurson material model to PM steels. It is shown how the model can be calibrated to material data. The results are also applied to an indentation test, where it’s demonstrated that experimental results can be reproduced with some accuracy. Limitations of the model, and the potential to use more advanced material models are also discussed.
摘要模拟在预测材料、部件和结构的行为方面越来越重要。多孔材料,如PM,对所使用的材料模型提出了特殊要求。本文研究了Gurson材料模型在PM钢中的应用。展示了如何根据材料数据校准模型。该结果还应用于压痕试验,证明了实验结果可以以一定的精度再现。还讨论了该模型的局限性,以及使用更先进材料模型的潜力。
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引用次数: 0
The Effects of Post-Sintering Treatments on Microstructure and Mechanical Properties of Mn-Mo Steel 烧结后处理对Mn-Mo钢组织和力学性能的影响
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0011
C. Fiał
Abstract The effect of heat treatment on density, hardness, microstructure and tensile properties of Fe-0.85Mo-1.3Mn-0.6C sintered steel were investigated. Pre-alloyed Astaloy 85Mo, ferromanganese and UF4 graphite powders were mixed for 60 minutes in a Turbula mixer and then pressed in single-action die at 660MPa to produce green compacts (according to PN EN ISO 2740).The compacts were sintered in a specially designed semi-closed container at 1120 or 1250°C for 60 minutes in N2. The chemical composition of the sintering atmosphere was modified by adding getter and/or activator into the container. Two different types of heat treatment in nitrogen were carried out: sinteraustempering at 525°C for 60 minutes; and sinterhardening with additional tempering at 200°C for 60 minutes. The slightly better combination of strength and plasticity of steel for both sintering temperatures were achieved after sinterhardening+tempering variant. Average values of 0.2% offset yield stress, ultimate tensile strength and elongation after sintering in 1250°C, were 415MPa, 700MPa, and 2.0%, respectively.
摘要:研究热处理对Fe-0.85Mo-1.3Mn-0.6C烧结钢的密度、硬度、显微组织和拉伸性能的影响。预先合金的Astaloy 85Mo、锰铁和UF4石墨粉末在紊流混合器中混合60分钟,然后在660MPa的单作用模具中压制,以生产绿色压坯(根据PN EN ISO 2740)。在一个特殊设计的半封闭容器中,在1120或1250°C下,在N2中烧结60分钟。通过在容器中加入吸气剂和/或活化剂来改变烧结气氛的化学成分。在氮气中进行了两种不同的热处理:在525℃下烧结60分钟;在200°C下额外回火60分钟进行烧结硬化。在两种烧结温度下,钢的强度和塑性结合在烧结硬化+回火变体中均略好。1250℃烧结后,0.2%的偏置屈服应力、极限抗拉强度和伸长率的平均值分别为415MPa、700MPa和2.0%。
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引用次数: 0
Embrittling Components in Sintered Steels: Comparison of Phosphorus and Boron 烧结钢的脆化成分:磷和硼的比较
Q4 Materials Science Pub Date : 2017-12-01 DOI: 10.1515/pmp-2017-0006
H. Danninger, V. Vassileva, C. Gierl-Mayer
Abstract In ferrous powder metallurgy, both boron and phosphorus have been known to be sintering activators for a long time. However, the use has been widely different: while P is a standard additive to sintered iron and steels, boron has been frequently studied, but its use in practice is very limited. Both additives are also known to be potentially embrittling, though in a different way. In the present study the differences between the effects of both elements are shown: while P activates sintering up to a certain threshold, in part by stabilizing ferrite, in part by forming a transient liquid phase, boron is the classical additive enhancing persistent liquid phase, being virtually insoluble in the iron matrix. The consequence is that sintered steels can tolerate quite a proportion of phosphorus, depending on composition and sintering process; boron however is strongly embrittling in particular in combination with carbon, which requires establishing a precisely defined content that enhances sintering but is not yet embrittling. The fracture mode of embrittled materials is also different: while with Fe-P the classical intergranular fracture is observed, with boron a much more rugged fracture surface appears, indicating some failure through the eutectic interparticle network but mostly transgranular cleavage. If carbon is added, in both cases transgranular cleavage dominates even in the severely embrittled specimens, indicating that no more the grain boundaries and sintering necks are the weakest links in the systems.
在铁粉末冶金中,硼和磷长期以来都被认为是烧结助剂。然而,用途却大不相同:虽然P是烧结铁和钢的标准添加剂,但硼经常被研究,但它在实践中的应用非常有限。众所周知,这两种添加剂都有潜在的脆化作用,尽管方式不同。在目前的研究中,两种元素的作用之间的差异显示:虽然P激活烧结达到一定的阈值,部分是通过稳定铁氧体,部分是通过形成瞬态液相,硼是经典的添加剂,增强持久液相,几乎不溶于铁基体。结果是烧结钢可以承受相当比例的磷,这取决于成分和烧结工艺;然而,硼是强脆的,特别是与碳结合时,这需要建立一个精确定义的含量,以增强烧结,但还没有脆化。脆性材料的断裂模式也不同:Fe-P的断裂是典型的晶间断裂,而硼的断口则更为崎岖,表明一些破坏是通过共晶晶间网络进行的,但主要是穿晶解理。如果添加碳,在这两种情况下,即使在严重脆化的试样中,穿晶解理也占主导地位,这表明晶界和烧结颈不再是体系中最薄弱的环节。
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引用次数: 4
Reaction of Unalloyed and Cr-Mo Alloyed Steels with Nitrogen from the Sintering Atmosphere 非合金钢和Cr-Mo合金钢与烧结气氛中氮气的反应
Q4 Materials Science Pub Date : 2016-12-01 DOI: 10.1515/pmp-2016-0007
M. Dlapka, C. Gierl-Mayer, Raquel de Oro Calderon, H. Danninger, S. Bengtsson, E. Dudrová
Abstract Nitrogen is usually regarded as an inert sintering atmosphere for PM steels; however, this cannot be taken for granted in particular for steels alloyed with nitride forming elements. Among those elements, chromium has become more and more important as an alloying element in sintered low alloy structural steels in the last decade due to the moderate alloying cost and the excellent mechanical properties obtainable, in particular when sinter hardening is applied. The high affinity of Cr to oxygen and the possible ways to overcome related problems have been the subject of numerous studies, while the fact that chromium is also a fairly strong nitride forming element has largely been neglected at least for low alloy steel grades, although frequently used materials like steels from Cr and Cr-Mo prealloyed powders are commonly sintered in atmospheres consisting mainly of nitrogen. In the present study, nitrogen pickup during sintering at different temperatures and for varying times has been studied for Cr-Mo prealloyed steel grades as well as for unalloyed carbon steel. Also the effect of the cooling rate and its influence on the properties, of the microstructure and the composition have been investigated. It showed that the main nitrogen uptake occurs not during isothermal sintering but rather during cooling. It could be demonstrated that a critical temperature range exists within which the investigated CrM-based steel is particularly sensitive to nitrogen pickup.
氮气通常被认为是PM钢的惰性烧结气氛;然而,这不能被认为是理所当然的,特别是对于含氮化物形成元素的合金钢。在这些元素中,铬作为一种合金元素在近十年来在烧结低合金结构钢中变得越来越重要,因为它的合金化成本适中,而且可以获得优异的力学性能,特别是在烧结硬化时。铬对氧的高亲和力和克服相关问题的可能方法已经成为许多研究的主题,而铬也是一种相当强的氮化物形成元素的事实在很大程度上被忽视了,至少对于低合金钢等级,尽管常用的材料,如铬和Cr- mo预合金粉末的钢通常在主要由氮组成的气氛中烧结。在本研究中,研究了Cr-Mo预合金钢牌号和非合金钢在不同温度和不同时间烧结时的氮吸附。研究了冷却速度对合金性能、组织和成分的影响。结果表明,主要的氮吸收不是发生在等温烧结过程中,而是发生在冷却过程中。结果表明,在所研究的铬基钢对氮吸附特别敏感的临界温度范围内存在。
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引用次数: 2
期刊
Powder Metallurgy Progress
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