激光共聚焦扫描显微镜原位观察奥氏体不锈钢的敏化过程

使用配备红外线加热炉的激光共聚焦扫描显微镜(CLSM)对3种不同碳含量的奥氏体不锈钢AISI 302,AISI 304,AISI 316L的碳化物沉积以及敏化过程进行了原位观察,同时研究了碳含量、加热温度以及时间与碳化物沉积以及敏化带宽度之间的关系,绘制出了不锈钢出现晶界碳化物沉积和敏化带的时间-温度曲线。结果表明:AISI 302,AISI 304不锈钢在600~1 000℃加热时均会出现晶界碳化物沉积,发生敏化现象,且碳含量高的AISI 302不锈钢相比碳含量低的AISI304不锈钢其晶界上更容易先形成碳化物沉积和发生敏化现象;当加热温度升高至1 100℃时,两种不锈钢的晶界碳化物沉积溶解,敏化带消失;AISI 316L不锈钢由于碳含量低,试验时间内未观察到晶界碳化物沉积和敏化现象;敏化带宽度随加热温度和不锈钢碳含量的增加而增加,随加热时间的延长则先增大后减小。     

18Cr10NiNb耐热钢析出相的热力学计算和平衡相分析

将18Cr10NiNb耐热钢在650℃进行10,000h的时效试验,用扫描电镜和透射电镜分析了18Cr10NiNb奥氏体耐热钢的组织,通过热力学计算研究了500-1400℃碳、铌和氮含量的变化对平衡析出相的影响。结果表明:在18Cr10NiNb钢的时效过程中在晶内析出了富Nb的MX相,在晶界析出了富Cr的M_(23)C_6相。根据热力学计算,其平衡析出相为MX,M_(23)C_6和σ相。MX相和M_(23)C_6型碳化物的最高溶解温度分别约为1340℃和840℃。MX相的数量随C和Nb含量的提高而增加。σ相的数量随着C含量的提高而减少。添加0.2%的N元素后,MX相为含有N、Nb、Cr和少量C的复杂碳氮化物,且在其平衡组织中出现了Cr_2N相。     

激光表面重熔对高速钢显微组织的影响

采用CO_2连续波激光对W18Cr4V高速钢进行表面重熔处理。分析结果表明,经激光重熔后高速钢的显微组织明显细化,重熔层内的相构成为马氏体、奥氏体,过剩的δ铁素体和M_6C、M_(23)C_6型碳化物。枝晶内为孪晶马氏体和部分板条马氏体。枝晶间为富合金元素的奥氏体和M_6C碳化物,孪晶马氏体上沿孪晶面有M_(23)C_6碳化物共格析出。激光扫描速度增加、δ铁素体量增多,重熔层显微硬度下降。     

4Cr14Ni14W2Mo钢的奥氏体晶粒度和孪晶及碳化物

对锻造的4Cr14Ni14W2Mo钢经相应热处理后的奥氏体晶粒度、孪晶及碳化物类型进行了研究。认为固溶处理后的奥氏体晶粒度主要取决于固溶加热温度,与锻造温度关系不大。固溶加热过程实质是再结晶过程的继续,即二次再结晶。奥氏体晶粒的大小只能通过控制再结晶温度的高低和时间长短来实现。该钢热处理后,碳化物类型为M_(23)C_6和M_7C_3两种,而以M_(23)C_6居多。其中M_(23)C_6为(Cr、Fe、W、Mo)_(23)C_6和(Fe、Ni)_(23)C_6两种结构,而M_7C_3为(Cr、Fe)_7C_3。     

热轧态Inconel690合金中碳化物的溶解和析出

研究了热轧态690合金中碳化物的溶解和析出行为及其结构,结果表明:在热轧态合金中存在的碳化物多数沿晶界长条状分布,少量呈颗粒状分布于晶内,类型为M_(23)C_6.热轧态合金的晶界和晶内碳化物的完全固溶温度分别为1050℃、1080℃,在低固溶温度下未完全溶解的残余晶界碳化物直接导致后续TT处理晶界不再析出碳化物;将合金完全固溶处理后,在后续TT处理的晶界上会重新析出细小、半连续的碳化物.     

一种SCWR包壳管用9-12%Cr低活性F/M钢的组织及析出相研究

运用Thermo-Calc软件进行热力学计算,预测了一种新型9-12%Cr低活性F/M(铁素体/马氏体)实验钢的组织。对淬火回火热处理后的显微组织进行了观察,并对析出物进行电子衍射结构分析和EDS化学成分检测。结果表明,实验钢是典型的回火板条马氏体组织,位于各种晶界上的析出物均为富Cr的碳化物M_(23)C_6,其化学成分随碳化物的形貌变化而变化。对实验钢进行60%冷变形并随后在820℃退火10-300 min,M_(23)C_6在完全再结晶、奥氏体相变过程中进一步球化,Cr、W不断富集,Cr/Fe逐渐升高至2后成分趋于稳定,化学组成接近于(Cr_(15)Fe_6W_2)C_6。     

奥氏体钢晶间腐蚀机理电子理论研究

采用递归法计算了奥氏体钢的杂质掺入能、格位能、亲和能等电子结构参数,建立电子参数与奥氏体钢晶间腐蚀关系,探索晶间腐蚀机理。研究表明：奥氏体钢中S和P由晶内向晶界扩散,恶化晶界稳定性,且使电子从晶界流向晶内,造成晶界与晶内产生电位差,形成微电偶结构,发生晶间腐蚀。C和Cr具有较强亲和力,能在奥氏体钢晶界形成（Cr,Fe）23C6相。Ni提高C的格位能,降低C在奥氏体中的固溶度,促进（Cr,Fe）23C6的形成与长大,增加奥氏体钢的晶间腐蚀敏感性。Nb和Ti降低C的格位能,抑制（Cr,Fe）23C6的形成,提高奥氏体钢的抗晶间腐蚀能力。     

304奥氏体不锈钢晶间腐蚀敏感性的非线性超声表征

利用非线性超声检测技术并辅助于XRD与微观组织分析,探讨了在650℃经过2,6,10h敏化处理的304奥氏体不锈钢样品非线性超声特征参数的变化规律。结果表明:随着敏化时间的延长,归一化非线性系数单调增大;相比于固溶试样,经2,6,10h敏化处理后样品的归一化非线性系数分别增加28%,32%,43%,意味着以非线性系数表征304不锈钢的敏化度是可行的。分析认为:晶界析出碳化物(Cr23C6)与奥氏体基体产生的错配引发了局部应变场,干扰了超声波的传播;此外,随敏化时间延长,析出相的增加进一步加剧了超声波的畸变。     

稳定化处理对Super304H奥氏体耐热钢晶间腐蚀敏感性的影响

用光学显微镜(OM)、扫描电子显微镜(SEM)、电解萃取法、草酸电解实验、X射线衍射(XRD)和双环电化学动电位再活化法(DL-EPR)等方法,研究了固溶和稳定化处理工艺对Super304H钢的显微组织(包括晶粒度,析出相分布、数量和类型)及晶间腐蚀敏感性的影响。结果表明,经过1150℃×15 min固溶处理后Super304H钢的晶粒度维持在7-10级;经不同温度的稳定化处理后析出相的数量较固溶态明显增加,其中950℃仍为敏化温度,有大量M23C6(M=Fe,Cr)沿晶界析出;随着稳定化温度的升高Nb(C,N)的析出数量随之增加,抗晶间腐蚀性能不断提高;当温度达到1100℃时Nb(C,N)的析出量达到最多,其抗晶间腐蚀性能较固溶态有明显提高;1100℃处于Super304H钢的固溶温度范围,明显高于传统1Cr18Ni9Ti型不锈钢的稳定化温度900℃,说明Super304H钢供货态的固溶处理工艺实际上兼顾了固溶与稳定化的双重作用。     

Si元素对明弧堆焊奥氏体合金组织及耐磨性的影响

为获得以奥氏体为基体且韧性及耐磨性良好的明弧堆焊合金,采用药芯焊丝自保护明弧焊方法制备了以奥氏体为基体的Fe-C-Mn-Cr-Nb-V-Ti系多元耐磨合金,借助X射线衍射仪、扫描电镜及其附属能谱仪等测试手段,研究了Si含量对其组织和耐磨性的影响。结果表明:堆焊合金基体为γ-Fe,硬质相有(Fe,Cr,Mn,V)_(23)C_6,(Nb,Ti)C和(Fe,Cr)_3(C,B)等;当堆焊合金含1.5%Si(质量分数)时,出现了沿晶(Fe,Cr,Mn,V)_7C_3相;随着Si含量提高,沿晶界分布的(Fe,Cr,Mn,V)_(23)C_6型碳化物数量先增加然后减少,形态从树枝骨架状变为层片状离散孤立分布,胞状γ-Fe晶内原位析出的(Nb,Ti,V)C复合碳化物随之增大,堆焊合金耐磨性呈先提高后下降再提高的趋势;0.9%Si和1.5%Si堆焊合金试样的磨损质量损失低于一般高铬铸铁,具有良好的耐磨性和韧性,其磨损机制主要为磨粒的显微切削。     

Influence of grain boundary carbides on mechanical properties of high nitrogen austenitic stainless steel

Precipitation behavior of grain boundary carbides and its influence on mechanical properties and fracture mechanism of the high nitrogen austenitic stainless steel produced by different processing methods were studied. The simulation software Thermo-calc was applied to analyze the effects of element content on precipitation of carbides. The results show that hot-rolled plate has higher strength, but solution-treated one followed by water quenching has excellent combination of strength and ductility (toughness). M₂₃C₆ is the main precipitate and deteriorates the toughness of the steel obviously when it precipitates along grain boundaries. In this case, intergranular fracture is the predominant failure mechanism and the fracture surface is characterized by the shape of rock candy. The toughness at −40 °C is decreased by 53% when small amount of carbides precipitates during sand cooling process after solution treatment. The simulation results exhibit that with the decrease of C content, both the precipitation quantity and precipitation temperature of M₂₃C₆ decrease. Cr and N have no influence on precipitation quantity of M₂₃C₆, but the precipitation temperature will increase with the increase of Cr and the decrease of N.     

Grain boundary engineering of titanium-stabilized 321 austenitic stainless steel

Grain boundary engineering (GBE) primarily aims to prevent the initiation and propagation of intergranular degradation along grain boundaries by frequent introduction of coincidence site lattice (CSL) boundaries into the grain boundary networks in materials. It has been reported that GBE is effective to prevent intergranular corrosion due to sensitization in unstabilized 304 and 316 austenitic stainless steels, but the effect of GBE on intergranular corrosion in stabilized austenitic stainless steels has not been clarified. In this study, a twin-induced GBE utilizing optimized thermomechanical processing with small pre-strain and subsequent annealing was applied to introduce very high frequencies of CSL boundaries into a titanium-stabilized 321 austenitic stainless steel. The resulting steel showed much higher resistance to intergranular corrosion after sensitization subsequent to carbon re-dissolution heat treatment during the ferric sulfate–sulfuric acid test than the as-received one. The high CSL frequency resulted in a very low percolation probability of random boundary networks in the over-threshold region and remarkable suppression of intergranular corrosion during GBE.     

Influence of stabilization heat treatments on microstructure,hardness and intergranular corrosion resistance of the AISI 321 stainless steel

The AISI 321 is an austenitic stainless steel which contains Ti as stabilizing element. This material can be selected for high temperatures services due to its high creep and intergranular corrosion resistance. However, for services into the sensitization range of temperatures (450–850 °C), the steel must be previously heat treated at higher temperatures for TiC precipitation. In the present work the importance of this so-called stabilization treatment, and the best range of temperatures for its realization, were investigated by means of microscopy and electrochemical potendynamic reactivation tests. It was found that the higher temperature for stabilization must be 950 °C. Samples stabilized at 975 °C or 1000 °C and aged at 600 °C for 100 h showed the very begin of the sensitization process.     

低铬铁素体不锈钢晶间腐蚀敏感性的测试方法及性能

研究了爆炸复合板复层06Cr13R低铬铁素体不锈钢的晶间腐蚀敏感性测试方法及性能。结果表明：电化学动电位扫描法（双环EPR法）适合用于爆炸复合板复层06Cr13R低铬铁素体不锈钢晶间腐蚀敏感性的检测,其试验结果与草酸电解侵蚀法对应较好;06Cr13R低铬铁素体不锈钢的晶间腐蚀敏感性与铬-镍奥氏体不锈钢不同,其晶间腐蚀敏感性出现在910℃正火处理后,甚至强制吹风急冷条件下也无法避免,而经过800℃退火处理后,其晶间腐蚀敏感性可减轻。     

Weld decay-resistant austenitic stainless steel by grain boundary engineering

This paper presents an example of grain boundary engineering (GBE) for improving intergranular-corrosion and weld-decay resistance of austenitic stainless steel. Transmission and scanning electron microscope (TEM and SEM) observations demonstrated that coincidence site lattice (CSL) boundaries possess strong resistance to intergranular precipitation and corrosion in weld decay region of a type 304 austenitic stainless steel weldment. A thermomechanical treatment for GBE was tried for improvement of intergranular corrosion resistance of the 304 austenitic stainless steel. The grain boundary character distribution (GBCD) was examined by orientation imaging microscopy (OIM). The sensitivity to intergranular corrosion was reduced by the thermomechanical treatment and indicated a minimum at a small roll-reduction. The frequency of CSL boundaries indicated a maximum at the small roll-reduction. The corrosion rate was much smaller in the thermomechanical-treated specimen than in the base material for long time sensitization. The optimum thermomechanical treatment introduced a high frequency of CSL boundaries and the clear discontinuity of corrosive random boundary network in the material, and resulted in the high intergranular corrosion resistance arresting the propagation of intergranular corrosion from the surface. The optimized 304 stainless steel showed an excellent resistance to weld decay during arc welding.     

Elevated temperature failure of heat treatment furnace containers

Abstract

The present study characterises the failures that generally occur in heat treatment furnace containers, which are used for chromium deposition onto chain spindles. Containers are produced using austenitic stainless steel AISI 310S, with a wall thickness of 8 mm. When operating at temperatures of ～970°C, cracks appear on the external surface, through the container wall. This occurs after periods as short as 1000 h and produces a lack of tightness, which renders the container useless. A structural analysis of the container wall reveals heavy carbonitride precipitation in a 1 mm layer close to the internal surface of the wall, producing sensitisation and intergranular corrosion. Cracks formed on the external wall surface, growing through the grain boundaries and close to large chromium carbides, were responsible for container failure. External cracks are the result of interacting creep–fatigue mechanisms, exacerbated by the coarsening of carbides and austenitic grains, caused by long periods at 970°C. Plastic deformation caused by hammering during the cooling cycle can contribute to the collapse of the container.     

Influence of heat treatment on creep of a Mn–N stabilised austenitic stainless steel

Creep at 700 °C/196 MPa and 900 or 925 °C/27.4 MPa of 21Cr–4Ni–9Mn austenitic stainless steel is determined as a function of the heat treatment. The heat treatment variation involves altering the solution heat treatment cooling rate from water quenching to cooling at 6 or 4 °C/min causing: serrated grain boundaries versus planar grain boundaries, coarser intergranular carbides, and discontinuous precipitation of grain boundary reaction zones. Water quenching causes improved creep resistance. Creep fracture and cracking is intergranular. Coarse intergranular carbides and grain boundary reaction zones cause premature void formation and cracking, this damage leading to an accelerating creep rate and lowering creep resistance of the more slowly cooled conditions. During creep, grain boundary serrations, which may otherwise contribute to improved creep, are eliminated. Determining the individual influence of grain boundary serrations on creep requires a detailed investigation of various heat treatment parameters to prevent concurrent formation of grain boundary reaction zones and serrations.     

微观组织对0Cr17Ni4Cu4Nb马氏体不锈钢的耐点腐蚀性能的影响

采用化学浸泡法和模拟闭塞电池方法研究了固溶+时效和固溶+调整+时效处理的0Cr17Ni4Cu4Nb马氏体不锈钢的耐点腐蚀性能,并与18-8型奥氏体不锈钢(316L)耐点蚀性能进行了对比。结果表明,0Cr17Ni4Cu4Nb马氏体不锈钢组织内富Cu析出相促进了点蚀坑萌生,而点蚀坑发展则与组织形貌有关。固溶+调整+时效处理的0Cr17Ni4Cu4Nb马氏体不锈钢因组织内析出富Cu相多而大,其萌生的点蚀坑密度较高,但由于马氏体板条较细,其点蚀坑尺寸和深度较小;固溶+时效处理的0Cr17Ni4Cu4Nb马氏体不锈钢因组织内析出富Cu相少而小,萌生的点蚀坑密度较低,但粗大的板条马氏体组织导致点蚀坑尺寸和深度较大。与18-8型奥氏体不锈钢耐点蚀性能对比表明,通过对0Cr17Ni4Cu4Nb马氏体不锈钢进行合理的热处理,其耐点蚀性能可与18-8型奥氏体不锈钢相当。     

Failure cases related to material issues in wet-process phosphoric acid plant

The present paper describes three failure cases of metallic components handling wet-process phosphoric acid at ambient temperatures in a phosphate fertilizer plant. All the three cases of failure were related not directly to the corrosive environment rather to wrong selection or inferior quality of materials. In the first case, pipeline of stainless steel 316L failed due to inferior quality of material used in the elbow region. The elbow material was not a low carbon grade stainless steel and was also in heavily sensitized condition which led to intergranular corrosion and intergranular cracking. The other two cases were related to failures of pump sleeves made up of cast alloys equivalent to stainless steel 316 and Hastelloy C-276 respectively. SS 316 showed through-wall pitting and cracking while Hastelloy C-276 had undergone extensive corrosion along the interdendritic boundaries. Both the materials contained high carbon content which led to heavy precipitation of carbides (Cr-rich carbides in SS 316 and Mo-rich carbides in C-276) along inter-dendritic boundaries during solidification of the casting reducing their corrosion resistance. Recommendations to avoid such failures are also suggested.     

反复焊接对超低碳奥氏体不锈钢耐腐蚀性能的影响

通过对反复焊接1～5次的超低碳奥氏体不锈钢的晶间腐蚀试验及应力腐蚀试验，研究了反复焊接对超低碳奥氏体不锈钢的耐腐蚀性能的影响。试验结果显示，在同一部位反复焊接5次后，超低碳奥氏体不锈钢的晶间腐蚀倾向和应力腐蚀敏感性没有发生明显变化，表明超低碳奥氏体不锈钢在选择合适的焊接材料、焊接工艺和焊接方法的前提下，同一部位可反复焊接5次，而其耐腐蚀性能不会受到影响。