Ni-Cr-Fe合金高温氧化成膜特性及氧化/碳化临界条件下膜组织演变规律的研究
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摘要
Ni-Cr-Fe合金由于其表面可以形成一层均匀致密的Cr_2O_3保护膜,因此具有良好的耐氧化和抗渗碳性能,同时具有较好的高温蠕变强度,被广泛的应用于乙烯裂解炉的高温部件。随着乙烯裂解工艺的改进、裂解原材料的日渐复杂以及裂解深度的提高,裂解温度也随之有所提高,对乙烯裂解炉管材料的高温抗氧化/碳化性能也提出了更高的要求。Cr_2O_3保护膜在1000℃以下具有良好的稳定性和抗碳化性能,但当使用温度超过1000℃以后,Cr_2O_3容易分解为挥发性的CrO_3、CrO_2等氧化物,因此,单一的Cr_2O_3保护膜已经远远不能满足现代生产工艺的要求。通过合金化工艺加入其他合金元素,使合金表面形成一层稳定性更高的复合氧化膜成为当前抗碳化材料的研究热点之一。
本文以添加适量Si、Mn合金元素的铸态Ni-Cr-Fe合金为实验合金,系统的研究了预氧化工艺(温度、氧分压)及合金元素对合金表层氧化膜的物相组成、微观结构的影响;分析了MnO、Cr_2O_3及MnCr_2O_4尖晶石在碳化环境中的稳定性;并研究了预氧化合金表面复合氧化膜的热力学性能及抗碳化性能。采用X-射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)等多种测试方法对氧化膜的物相结构、表面形貌等进行了测试表征。
(1)通过改变预氧化温度及氧分压研究了预氧化工艺对氧化膜微观结构、成膜规律的影响。Ni-Cr-Fe合金在较低温度发生氧化时,共晶组织区域的相界可以为合金元素提供线状快速扩散通道,因此该区域形成的氧化膜较为发达主要以羽毛状为主;随着预氧化温度的提高,奥氏体的晶内扩散速率提高,该区域的合金元素主要通过表层Cr_2O_3氧化膜的缺陷向外扩散,逐渐有棒状Mn-Cr尖晶石生成,表层氧化膜趋向均匀。体系的氧分压对氧化膜的微观结构具有重要的影响,低氧分压时表层主要形成Cr_2O_3单一氧化膜,合金试样增重较大且氧化膜为多孔结构;随着氧分压的逐渐增大氧化膜也逐渐转变为致密的复合氧化膜,合金的氧化增重率降低。中等氧分压下复合氧化膜中Mn-Cr尖晶石含量最多。
(2)Ni-Cr-Fe合金氧化膜的生长动力学与合金基体的微观结构及其相应的Si含量密切相关。氧化过程中,Si含量较低的合金无法在合金基体与表层氧化膜界面处形成连续的SiO_2非晶层,因此氧化后所形成的氧化膜较厚且均匀;而Si含量较高的合金,奥氏体组织之上可以形成一层连续的SiO_2非晶层,阻碍了合金元素的扩散,导致表层氧化膜较薄,而在共晶组织区域形成不了连续的SiO_2非晶层,因此比较发达的脊状氧化物形成于共晶组织之上。合金元素Mn具有较大的扩散系数,致使Mn-Cr尖晶石在氧化膜的最外层生成。合金中Mn含量较低时,表层形成少量颗粒细小的Mn-Cr尖晶石;随着Mn含量的提高,表层Mn-Cr尖晶石形貌转变为板条状;如果合金中Si的含量较低而Mn的含量较高,则在合金表面形成星状的尖晶石相。
(3)通过对粉体MnO_2、Cr_2O_3及MnCr_2O_4尖晶石碳化性能的研究发现:MnO_2经高温烧结、碳化后转变为MnO,并在碳化过程中表现出较好的稳定性。Cr_2O_3在碳化初期表现出较好的稳定性,但随着碳化过程的进行Cr_2O_3转变为Cr_7C_3、Cr_(23)C_6和Cr_3C_2,表现为先失重后增重,组织结构也转变为多孔结构。MnCr_2O_4尖晶石在碳化过程中表现出极好的稳定性没有发生物相的转变。
(4)研究了不同成分合金预氧化处理后复合氧化膜的抗碳化性能。复合氧化膜中MnCr_2O_4尖晶石可以阻碍C向合金基体内部的扩散,延缓Cr_2O_3的碳化;计算了复合氧化膜生成热力学和扩散动力学,证实在合金表面生成的复合氧化膜由外到内依次为MnCr_2O_4、Cr_2O_3、SiO_2。
Ni-Cr-Fe based alloys were widely used as high temperature oxidation-resistantmaterials in ethylene cracking industry due to the fast formation of dense chromiumoxide layer on the surface in oxidation environment. With continuingimprovement ofthe ethylene crackingprocess, the growingcomplexityof raw materials and the depthof cracking, the ethylene cracking temperature were increased. Betteroxidation/carburization-resistant properties for ethylene cracking tube materials arerequired. The chromium oxide can protect alloys from oxidation and carburization attemperature below 1000℃. When the temperature excess 1000℃, chromium oxidecan be easily decomposed to volatile CrO_3, CrO_2 phases, which could loss theprotectiveproperty.AsingleCr_2O_3protectivefilm couldnot meet therequirements ofmodern industrial technology. When alloying elements were added, more stablecompositeoxidefilm canbeformedonthe alloysurface,whichis aresearchfocus onanti-carburizationmaterials.
In this paper, alloys were cast by adding Si and Mn elements to Ni-Cr-Febased alloys. The effects of alloy elements and the pre-oxidation conditions(temperature and oxygen partial pressure) on oxide film composition andmicrostructure were systematic studied. The stabilities of MnO、Cr_2O_3and MnCr_2O_4spinel were also analyzed in the carbonaceous environment. The thermodynamicproperties and carburization resistance of composite oxide film on the alloy surfacewere also studied. The oxide film structure and surface morphology werecharacterized using thin film X-ray diffraction (XRD), scanning electron microscopy(SEM),energyspectrumanalysis(EDS)andothermethods.
(1) The influence of pre-oxidation temperature and oxygen partial pressure onthe microstructure of the oxide film was studied. When oxidation of Ni-Cr-Fe based alloys occurat lowertemperature,moredeveloped oxides forms intheeutecticregion,mainly because of the laminar structure of eutectic areas. The phase boundaries canprovide fast diffusion channel for alloying elements, therefore, the surface oxidemainlybased on feather-like growth in this region. With the increase of pre-oxidationtemperature, diffusion of alloying elements within the austenite phase increased,mainly through the defect of Cr_2O_3 film in austenite areas, so some rod-like Mn-Crspinel were formed in this area. It was found that oxygen partial pressure of thesystem has an important effect on the microstructure of oxide film. At lower oxygenpartial pressure, a thick and porous structured oxide film was formed, and thedominant phase of oxide film was Cr_2O_3. With the increases of oxygen partialpressure, the dominant phase of oxide film gradually transformed to composite oxidefilm. The micro-structure of oxide film becomes dense and thinner. A maximumcontentofspinelphasewasobtainedinthemiddleoxygenpartialpressure.
(2) The growth kinetics of oxide film for Ni-Cr-Fe based alloy is closely relatedto the microstructure of the matrix and the corresponding Si content. During theoxidation process, a continuous amorphous layer of SiO_2 sub-layer in the low Sicontent alloys can not be formed, resulting in a thickand uniform oxide layer formedon the surface; while a continuous SiO_2 amorphous layer can be formed on thesub-surface in the higher Si content alloys, which can block the outside diffusion ofalloying elements from the substrate, resulting in a thinner outer oxide film. Moredeveloped oxide formed above this region due to a discontinuous of SiO_2sub-films.Higher diffusion coefficient of Mn ion is the reason of Mn-Cr spinel forms at theoutmost of the film. For lower Mn containing alloy, small particle Mn-Cr spinelwould to be formed. With increases of Mn content, the morphology of Mn-Cr spineltransforms tolath-shaped. LowerSi andhigherMn content ofthealloyresultedinthestellatemorphologyofMn-Crspinelonthealloysurface.
(3) Study of MnO_2, Cr_2O_3 and MnCr_2O_4 spinel powder sample in carbonaceousenvironment shows that MnO_2 would transfer to MnO after high temperaturecarburization, and MnO shows a good stabilityin carbonization process. Cr_2O_3 wouldtransfer to Cr_7C_3, Cr_(23)C_6 and Cr_3C_2 in the carburization process, which shows the weight loss first and weight gain later. The micro-structure was also porous structure.MnCr_2O_4 spinel shows excellent stability and no structure transformation during thewholecarburization process.
(4) The carburization resistance of composite oxide film for different alloysafter pro-oxidation were also studied. MnCr_2O_4 spinel in composite oxide filmcould hinder the diffusion of C to matrix, and delay the carburization of Cr_2O_3.Thermodynamics forming and diffusion dynamics of the composite oxide filmwere calculated, which confirm that the composite oxide film was in the order ofMnCr_2O_4, Cr_2O_3and SiO_2 from outmost to inner substrate.
本文以添加适量Si、Mn合金元素的铸态Ni-Cr-Fe合金为实验合金,系统的研究了预氧化工艺(温度、氧分压)及合金元素对合金表层氧化膜的物相组成、微观结构的影响;分析了MnO、Cr_2O_3及MnCr_2O_4尖晶石在碳化环境中的稳定性;并研究了预氧化合金表面复合氧化膜的热力学性能及抗碳化性能。采用X-射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)等多种测试方法对氧化膜的物相结构、表面形貌等进行了测试表征。
(1)通过改变预氧化温度及氧分压研究了预氧化工艺对氧化膜微观结构、成膜规律的影响。Ni-Cr-Fe合金在较低温度发生氧化时,共晶组织区域的相界可以为合金元素提供线状快速扩散通道,因此该区域形成的氧化膜较为发达主要以羽毛状为主;随着预氧化温度的提高,奥氏体的晶内扩散速率提高,该区域的合金元素主要通过表层Cr_2O_3氧化膜的缺陷向外扩散,逐渐有棒状Mn-Cr尖晶石生成,表层氧化膜趋向均匀。体系的氧分压对氧化膜的微观结构具有重要的影响,低氧分压时表层主要形成Cr_2O_3单一氧化膜,合金试样增重较大且氧化膜为多孔结构;随着氧分压的逐渐增大氧化膜也逐渐转变为致密的复合氧化膜,合金的氧化增重率降低。中等氧分压下复合氧化膜中Mn-Cr尖晶石含量最多。
(2)Ni-Cr-Fe合金氧化膜的生长动力学与合金基体的微观结构及其相应的Si含量密切相关。氧化过程中,Si含量较低的合金无法在合金基体与表层氧化膜界面处形成连续的SiO_2非晶层,因此氧化后所形成的氧化膜较厚且均匀;而Si含量较高的合金,奥氏体组织之上可以形成一层连续的SiO_2非晶层,阻碍了合金元素的扩散,导致表层氧化膜较薄,而在共晶组织区域形成不了连续的SiO_2非晶层,因此比较发达的脊状氧化物形成于共晶组织之上。合金元素Mn具有较大的扩散系数,致使Mn-Cr尖晶石在氧化膜的最外层生成。合金中Mn含量较低时,表层形成少量颗粒细小的Mn-Cr尖晶石;随着Mn含量的提高,表层Mn-Cr尖晶石形貌转变为板条状;如果合金中Si的含量较低而Mn的含量较高,则在合金表面形成星状的尖晶石相。
(3)通过对粉体MnO_2、Cr_2O_3及MnCr_2O_4尖晶石碳化性能的研究发现:MnO_2经高温烧结、碳化后转变为MnO,并在碳化过程中表现出较好的稳定性。Cr_2O_3在碳化初期表现出较好的稳定性,但随着碳化过程的进行Cr_2O_3转变为Cr_7C_3、Cr_(23)C_6和Cr_3C_2,表现为先失重后增重,组织结构也转变为多孔结构。MnCr_2O_4尖晶石在碳化过程中表现出极好的稳定性没有发生物相的转变。
(4)研究了不同成分合金预氧化处理后复合氧化膜的抗碳化性能。复合氧化膜中MnCr_2O_4尖晶石可以阻碍C向合金基体内部的扩散,延缓Cr_2O_3的碳化;计算了复合氧化膜生成热力学和扩散动力学,证实在合金表面生成的复合氧化膜由外到内依次为MnCr_2O_4、Cr_2O_3、SiO_2。
Ni-Cr-Fe based alloys were widely used as high temperature oxidation-resistantmaterials in ethylene cracking industry due to the fast formation of dense chromiumoxide layer on the surface in oxidation environment. With continuingimprovement ofthe ethylene crackingprocess, the growingcomplexityof raw materials and the depthof cracking, the ethylene cracking temperature were increased. Betteroxidation/carburization-resistant properties for ethylene cracking tube materials arerequired. The chromium oxide can protect alloys from oxidation and carburization attemperature below 1000℃. When the temperature excess 1000℃, chromium oxidecan be easily decomposed to volatile CrO_3, CrO_2 phases, which could loss theprotectiveproperty.AsingleCr_2O_3protectivefilm couldnot meet therequirements ofmodern industrial technology. When alloying elements were added, more stablecompositeoxidefilm canbeformedonthe alloysurface,whichis aresearchfocus onanti-carburizationmaterials.
In this paper, alloys were cast by adding Si and Mn elements to Ni-Cr-Febased alloys. The effects of alloy elements and the pre-oxidation conditions(temperature and oxygen partial pressure) on oxide film composition andmicrostructure were systematic studied. The stabilities of MnO、Cr_2O_3and MnCr_2O_4spinel were also analyzed in the carbonaceous environment. The thermodynamicproperties and carburization resistance of composite oxide film on the alloy surfacewere also studied. The oxide film structure and surface morphology werecharacterized using thin film X-ray diffraction (XRD), scanning electron microscopy(SEM),energyspectrumanalysis(EDS)andothermethods.
(1) The influence of pre-oxidation temperature and oxygen partial pressure onthe microstructure of the oxide film was studied. When oxidation of Ni-Cr-Fe based alloys occurat lowertemperature,moredeveloped oxides forms intheeutecticregion,mainly because of the laminar structure of eutectic areas. The phase boundaries canprovide fast diffusion channel for alloying elements, therefore, the surface oxidemainlybased on feather-like growth in this region. With the increase of pre-oxidationtemperature, diffusion of alloying elements within the austenite phase increased,mainly through the defect of Cr_2O_3 film in austenite areas, so some rod-like Mn-Crspinel were formed in this area. It was found that oxygen partial pressure of thesystem has an important effect on the microstructure of oxide film. At lower oxygenpartial pressure, a thick and porous structured oxide film was formed, and thedominant phase of oxide film was Cr_2O_3. With the increases of oxygen partialpressure, the dominant phase of oxide film gradually transformed to composite oxidefilm. The micro-structure of oxide film becomes dense and thinner. A maximumcontentofspinelphasewasobtainedinthemiddleoxygenpartialpressure.
(2) The growth kinetics of oxide film for Ni-Cr-Fe based alloy is closely relatedto the microstructure of the matrix and the corresponding Si content. During theoxidation process, a continuous amorphous layer of SiO_2 sub-layer in the low Sicontent alloys can not be formed, resulting in a thickand uniform oxide layer formedon the surface; while a continuous SiO_2 amorphous layer can be formed on thesub-surface in the higher Si content alloys, which can block the outside diffusion ofalloying elements from the substrate, resulting in a thinner outer oxide film. Moredeveloped oxide formed above this region due to a discontinuous of SiO_2sub-films.Higher diffusion coefficient of Mn ion is the reason of Mn-Cr spinel forms at theoutmost of the film. For lower Mn containing alloy, small particle Mn-Cr spinelwould to be formed. With increases of Mn content, the morphology of Mn-Cr spineltransforms tolath-shaped. LowerSi andhigherMn content ofthealloyresultedinthestellatemorphologyofMn-Crspinelonthealloysurface.
(3) Study of MnO_2, Cr_2O_3 and MnCr_2O_4 spinel powder sample in carbonaceousenvironment shows that MnO_2 would transfer to MnO after high temperaturecarburization, and MnO shows a good stabilityin carbonization process. Cr_2O_3 wouldtransfer to Cr_7C_3, Cr_(23)C_6 and Cr_3C_2 in the carburization process, which shows the weight loss first and weight gain later. The micro-structure was also porous structure.MnCr_2O_4 spinel shows excellent stability and no structure transformation during thewholecarburization process.
(4) The carburization resistance of composite oxide film for different alloysafter pro-oxidation were also studied. MnCr_2O_4 spinel in composite oxide filmcould hinder the diffusion of C to matrix, and delay the carburization of Cr_2O_3.Thermodynamics forming and diffusion dynamics of the composite oxide filmwere calculated, which confirm that the composite oxide film was in the order ofMnCr_2O_4, Cr_2O_3and SiO_2 from outmost to inner substrate.
引文
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