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研究生： 黃聖堯
Huang, Sheng-Yao
論文名稱： 鈮添加量對高合金不銹鋼高溫氧化行為之研究
Investigation of Oxidation Behavior in High-Alloy Austenitic Stainless Steel Containing Nb
指導教授： 郭瑞昭
Kuo, Jui-Chao
學位類別： 博士
Doctor
系所名稱： 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年： 2020
畢業學年度： 108
語文別： 英文
論文頁數： 191
中文關鍵詞： 高溫氧化 、沃斯田鐵系不銹鋼 、碳氮化鈮 、瘤狀氧化物 、EBSD
外文關鍵詞： oxidation, austenitic stainless steel, Nb(C, N), nodule, EBSD
相關次數： 點閱：110  下載：5 
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    • 本論文針對不同的鈮添加量(0, 0.29, 0.58 及 0.86 wt%)對於 22Cr25NiWCoCu 不銹 鋼之高溫氧化行為進行探討。
    首先，針對經 1300 oC、2 小時退火後不銹鋼進行顯微組織的分析。XRD 繞射的 結果顯示，基材為完全的沃斯田鐵相。隨著鈮含量的上升，平均晶粒尺寸由 426 μm 下降至 90 μm。藉由 EBSD 及 EDS 的分析可得知，未添加鈮的不銹鋼中之析出物僅 有 Cr23C6，而 Nb(C, N)為含鈮不銹鋼之主要析出物，Nb(C, N)的平均尺寸及體積分率 皆隨著鈮含量的上升而增加。
    接著探討鈮含量對此不銹鋼於 900 oC 乾空氣中的高溫氧化行為之影響。TGA 的 結果顯示，隨著鈮含量增加，材料的氧化速率提高。低掠角 XRD 分析指出，鈮的添 加有助於氧化初期 Cr2O3 的生成。橫截面顯微組織分析的結果顯示，Nb(C, N)的周圍 之氧化速率較高，鉻貧乏區生成於其下方，導致鐵氧化物優先於其周圍生成，最終形 成內層為(Cr, Fe, Mn)3O4、外層為 Fe2O3，厚度約 20 μm 的氧化層。
    在以氬氣攜帶 20 %水蒸氣的實驗中，四種材料在實驗開始的 1.5 小時內皆有劇 烈的質量變化，1.5 小時後則趨於平緩，整體的氧化行為接近對數線律。SEM 的結果 顯示，四種材料中，(1 0 0)晶面經長時間的氧化後傾向形成顆粒狀的氧化物。顆粒狀 氧化物亦可被觀察到在不含鈮及含 0.29 wt%鈮材料的(1 1 0)晶面中，而在含 0.58 及 0.86 wt%鈮的材料中，氧化物的形貌轉變為連續且平行。磊晶型態的氧化物可在(1 1 1)晶面中被觀察到，所有材料的(1 1 1)晶面均以外延式生長的方式形成單晶氧化層， 僅有少量的顆粒狀氧化物生成。藉由 FIB、EBSD 及 EDS 進行的橫截面分析可得知， Nb(C, N)週圍的氧化行為不受晶面方向影響，且具有較高的氧化速率。

    The effects of precipitation and oxidation behavior on 22Cr25NiWCoCu stainless steels with different concentrations of niobium (Nb) (0, 0.29, 0.58, and 0.86 wt%) were explored. The microstructure of the as-annealed specimens was firstly explored, and the changes in grain size, precipitation behavior, and microhardness were recorded. Subsequently, the oxidation behavior of the steels in both air and Ar-20 % H2O at 900 oC were analyzed. In addition, the effects of the Nb precipitates on the oxidation behavior on the samples were also investigated.
    For the investigation of the as-annealed materials, an X-ray diffraction analysis showed that the matrix of all of the studied steels was austenite. The average grain size decreased from 426 μm to 90 μm with increases in the Nb content. EBSD and EDS analyses showed that Cr23C6 was the main precipitate in the Nb-free steel, whereas Nb(C, N) were the main precipitates in the Nb-containing steels. The volume fraction and average particle size of the precipitates increased with increases in the Nb content.
    In the oxidation test in air, a TGA analysis showed the oxidation rate of the steel increased with increases in the Nb content. The GI-XRD results indicated that the addition of Nb promoted Cr2O3 formation. After 10-100 h of oxidation, Cr-depletion occurred at the region with Nb(C, N) precipitates due to its high Cr consumption rate, leading to Fe oxide generation. Finally, after 100 h of oxidation, the outer layer of Fe2O3 and the inner layer of (Cr, Fe, Mn)3O4 formed.
    In the oxidation in Ar-20 % H2O, all of the specimens exhibited significant changes in mass during first 1.5 h, after which their growth rate slowed. SEM observation showed that the oxides on the (1 0 0) plane of the four steels had a granular form. For the (1 1 0) planes, granular oxides could be found in the 0-Nb and 0.29-Nb steels, but in the 0.58-Nb and 0.86-Nb steels, continuous parallel oxides formed. In the case of the (1 1 1) grain of the four steels, the oxide exhibited epitaxial growth characteristics, where only a few granular oxides formed. In addition, nodules were also found in the Nb-containing steels. A faster oxidation rate was clearly found on these nodules as compared to in the nodule free sites. A cross- sectional analysis using FIB, EBSD, and EDS showed that the formation these nodules was also induced by the addition of Nb.

    1. Introduction..........................................1 1.1 Introduction.........................................1 1.2 Objectives...........................................6 2. Literature review.....................................8 2.1 Advance austenitic stainless steel - Sanicro® 25.....8 2.1.1 Alloy design......................................12 2.1.2 Precipitation behavior............................16 2.1.3 Oxidation behavior................................20 2.2 High temperature oxidation..........................25 2.2.1 Thermodynamics....................................25 2.2.2 Oxidation kinetic.................................28 2.2.3 Oxides in stainless steels........................31 2.2.4 Effect of grain size on chromia formation.........33 2.2.5 Effects of preferred orientation on oxidation rates in pure metals..........................................35 3. Experiments..........................................36 3.1 Production of the steels............................36 3.2 Analysis on the microstructure and precipitates.....37 3.3 Analysis on the high temperature oxidation behavior in dry air.................................................39 3.4 Analysis on the high temperature oxidation behavior in Ar - 20 % H2O...........................................41 4. Results..............................................45 4.1 Phase identification of the as-annealed specimens...45 4.1.1 Microstructural analyses..........................45 4.1.2 Precipitation behavior............................49 4.1.3 Microhardness.....................................62 4.2 High temperature oxidation behavior of 22Cr25NiWCoCu stainless steels with 0 % - 0.86 % Nb in dry air........63 4.2.1 Oxidation kinetics................................63 4.2.2 Phase characterization of top surface.............67 4.2.3 Surface microstructure............................68 4.2.4 Cross sectional microstructure....................75 4.3 High temperature oxidation behavior of 22Cr25NiWCoCu stainless steels with 0 % - 0.86 % Nb in Ar-20 % H2O at 900 oC..................................................83 4.3.1 Oxidation kinetics................................85 4.3.2 Phase characterization of top surface.............87 4.3.3 Surface microstructure............................97 4.3.4 Cross sectional microstructure...................151 5. Discussion..........................................154 5.1 Effects of niobium on microstructure and precipitation in As-annealed steels..................................154 5.2 Effects of Nb addition on the oxidation behavior of the as-annealed steels in Air..........................155 5.3 Effects of Nb addition on the oxidation behavior of the as-annealed steels in Ar - 20 % H2O................159 6. Conclusions.........................................165 7. References..........................................166 8. Appendix............................................176

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