CN115305446B - HK40耐热钢表面MgCr2O4镀层及其制备方法 - Google Patents
HK40耐热钢表面MgCr2O4镀层及其制备方法 Download PDFInfo
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Abstract
本发明涉及金属表面镀层制备技术领域，具体公开了一种HK40耐热钢表面MgCr2O4镀层及其制备方法。先对HK40耐热钢工件表面进行高温氧化处理，得到表面氧化改性的HK40耐热钢；再采用真空蒸发镀膜机在氧化改性的HK40耐热钢表面蒸镀上一层镁薄膜；然后将镁薄膜置于空气中转变为MgO薄膜，最后将表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，从而在HK40耐热钢表面反应形成具有MgCr2O4的镀层。所得到的镀层具有抗结焦性好、力学性能优异、易生产加工等特点。
Description
技术领域
本发明涉及金属表面镀层制备技术领域，具体涉及一种HK40耐热钢表面MgCr2O4镀层及其制备方法。
背景技术
炉管内表面状态是影响乙烯裂解炉管结焦特性的主要因素之一，HK40耐热钢是乙烯裂解炉管常用的材质，其具有抗氧化性强、耐硫化物腐蚀性好、耐热性能优良等特点。然而，炉管使用过程裂解过程中，外壁经受火焰加热，内壁则与碳源气体和载气接触，因此炉管不可避免的发生结焦，HK40耐热钢中的Fe、Ni等金属元素在渗碳气氛下具有强烈的催化活性，会催化结焦，进一步导致材料延伸率降低，脆化严重，很大程度上影响了炉管的使用寿命。
Cr2O3氧化层在1050℃以下具有良好的抗结焦性能。但是，当温度高于1050℃时，Cr2O3将会转变为疏松多孔的形态，严重影响其抗结焦性能。
发明内容
本发明的目的在于，提供一种HK40耐热钢表面MgCr2O4镀层及其制备方法。通过氧化在HK40耐热钢表面形成一层致密的Cr2O3，然后将镁蒸镀于Cr2O3表面，蒸镀结束后取出HK40耐热钢在空气中冷却并在表面获得一层致密的MgO(2Mg+O2＝2MgO)，最后通过真空扩散退火获得MgCr2O4镀层(MgO+Cr2O3＝MgCr2O4)，所获得镀层具有抗结焦性好、力学性能优异、易生产加工等特点。
同时，可以根据实际使用需求，通过控制蒸镀时间和真空扩散退火温度来控制镀层的厚度以及MgCr2O4的密度和粒径。因此，所述HK40耐热钢表面MgCr2O4镀层具有良好的可控性。
本发明提供的HK40耐热钢表面MgCr2O4镀层的制备方法，包括以下步骤：
(1)通过对HK40耐热钢工件表面进行高温氧化处理，得到表面氧化改性的HK40耐热钢。
氧化温度为800-900℃，氧化时间为5-10h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁单质进行蒸发。完成蒸镀后，得到表面蒸镀镁薄膜的氧化改性HK40耐热钢。
进行真空蒸镀过程时，控制蒸镀电压为1.0-1.6V，蒸镀电流为100-120A，蒸镀时间为5-20min，通过控制蒸镀时间来控制MgCr2O4的密度；
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却，HK40耐热钢表面蒸镀的镁薄膜转变为MgO薄膜。
冷却时间为10-30min，空气中镁薄膜转变为MgO薄膜的反应为2Mg+O2＝2MgO；
(4)将步骤(3)中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，得到所述的HK40耐热钢表面MgCr2O4镀层。
真空扩散退火时间为3-8h，退火温度为900-1200℃，通过控制退火温度来控制MgCr2O4的粒径，形成MgCr2O4的反应为MgO+Cr2O3＝MgCr2O4。
本发明提供了一种HK40耐热钢表面MgCr2O4镀层，在HK40耐热钢表面制备出抗碳化腐蚀性能优良的MgCr2O4镀层，MgCr2O4属于典型的尖晶石结构，具有极为优异的高温性能。MgCr2O4镀层可以阻碍碳与Fe、Ni及其氧化物的直接接触，有效解决HK40耐热钢催化结焦的问题，延长炉管的使用寿命，节约成本。对于促进HK40耐热钢在石油工业中的应用具有非常重要的意义。
附图说明：
图1为实施例中真空蒸发镀膜装置示意图；
图2为对比例1制得的HK40耐热钢表面Cr2O3氧化层的显微组织图；
图3为对比例2制得的HK40耐热钢表面MgO+Cr2O3氧化层的显微组织图；
图4为对比例3制得的HK40耐热钢表面MgO+Cr2O3氧化层的显微组织图；
图5为实施例1制得的HK40耐热钢表面MgCr2O4镀层的显微组织图；
图6为实施例2制得的HK40耐热钢表面MgCr2O4镀层的显微组织图；
图7为实施例3制得的HK40耐热钢表面MgCr2O4镀层的显微组织图；
图8为实施例4制得的HK40耐热钢表面MgCr2O4镀层的显微组织图；
图9为HK40耐热钢、对比例1、对比例2和实施例3样品的碳化腐蚀行为曲线图；
图10为HK40耐热钢、对比例1、对比例2和实施例3样品的拉伸性能曲线图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合附图对本发明作进一步详细描述。所描述的实施例仅是本申请一部分的实施例，这些实施例仅用于解释本发明而不用于限制本发明的范围。
对比例1
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将对比例1的样品选取7个进行结焦实验，同时制备7个无镀层的HK40耐热钢试样做结焦对比实验。每隔1小时取出一个试样测量结焦增重，得到的结焦增重曲线如图9所示。
(3)测量对比例1的抗拉强度和伸长率，同时测量无镀层的HK40耐热钢的抗拉强度和伸长率，得到的结果如图10所示。
对比例2
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，蒸镀电压为1.2V，蒸镀电流为120A，蒸镀时间为10min。
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却20min。
(4)将步骤(3)中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，退火时间为5h，退火温度为800℃。
(5)将对比例2的样品选取7个进行结焦实验，每隔1小时取出一个试样测量结焦增重，得到的结焦增重曲线如图9所示。
(6)测量对比例2的抗拉强度和伸长率，得到的结果如图10所示。
对比例3
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，蒸镀电压为1.2V，蒸镀电流为120A，蒸镀时间为20min。
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却20min。与对比例2相比，随着蒸镀时间的增加，MgO的密度增加。
实施例1
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，蒸镀电压为1.2V，蒸镀电流为120A，蒸镀时间为10min，蒸镀时间短，MgO的密度就比较低，后续形成的MgCr2O4比较少。
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却20min。
(4)将步骤(3)中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，退火时间为5h，退火温度为900℃，得到HK40耐热钢表面MgCr2O4镀层。
实施例2
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，蒸镀电压为1.2V，蒸镀电流为120A，蒸镀时间为20min。
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却20min。
(4)将步骤(3)中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，退火时间为5h，退火温度为900℃，得到HK40耐热钢表面MgCr2O4镀层。
实施例3
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，蒸镀电压为1.2V，蒸镀电流为120A，蒸镀时间为20min。
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却20min。
(4)将步骤(3)中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，退火时间为5h，退火温度为1100℃，得到HK40耐热钢表面MgCr2O4镀层。与实施例2相比，随着退火温度的升高，MgCr2O4的粒径变大。
(5)将实施例3的样品选取7个进行结焦实验，每隔1小时取出一个试样测量结焦增重，得到的结焦增重曲线如图9所示。
(6)测量实施例3的抗拉强度和伸长率，得到的结果如图10所示。
实施例4
(1)对HK40耐热钢工件表面进行高温氧化处理，氧化温度为850℃，时间为5h。
(2)将步骤(1)中制备的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，蒸镀电压为1.2V，蒸镀电流为120A，蒸镀时间为20min。
(3)将步骤(2)中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却20min。
(4)将步骤(3)中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，退火时间为5h，退火温度为1200℃，得到HK40耐热钢表面MgCr2O4镀层。
Claims (4)
1.一种HK40耐热钢表面MgCr2O4镀层的制备方法，其特征在于：所述制备方法步骤如下：
（1）对HK40耐热钢工件表面进行高温氧化处理，得到表面氧化改性的HK40耐热钢；
所述高温氧化温度为800-900℃，氧化时间为5-10h；
（2）将步骤（1）得到的表面氧化改性的HK40耐热钢放入真空蒸发镀膜机中，在真空环境中对镁进行蒸发，完成蒸镀后，得到表面蒸镀镁薄膜的氧化改性HK40耐热钢；
（3）将步骤（2）中表面蒸镀镁薄膜的氧化改性HK40耐热钢工件取出，在空气中冷却，HK40耐热钢表面蒸镀的镁薄膜转变为MgO薄膜；
（4）将步骤（3）中制备的表面附有MgO薄膜的氧化改性HK40耐热钢进行真空扩散退火处理，得到HK40耐热钢表面MgCr2O4镀层；
真空扩散退火时间为3-8h，退火温度为900-1200℃。
2.根据权利要求1所述的HK40耐热钢表面MgCr2O4镀层的制备方法，其特征在于，步骤（2）进行真空蒸镀过程时，控制蒸镀电压为1.0-1.6V，蒸镀电流为100-120A，蒸镀时间为5-20min。
3.根据权利要求1所述的HK40耐热钢表面MgCr2O4镀层的制备方法，其特征在于，步骤（3）冷却时间为10-30min。
4.根据权利要求1-3任一项所述方法制备的HK40耐热钢表面MgCr2O4镀层。
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| US4647547A (en) * | 1985-12-10 | 1987-03-03 | The United States Of America As Represented By The United States Department Of Energy | High temperature refractory of MgCr2 O4 matrix and unstabilized ZrO2 particles |
| JP2017203192A (ja) * | 2016-05-12 | 2017-11-16 | 日鉄住金鋼板株式会社 | 塗装めっき鋼板 |
| CN111304661A (zh) * | 2019-12-31 | 2020-06-19 | 上海大学 | 铝硅镁镀层及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4647547A (en) * | 1985-12-10 | 1987-03-03 | The United States Of America As Represented By The United States Department Of Energy | High temperature refractory of MgCr2 O4 matrix and unstabilized ZrO2 particles |
| JP2017203192A (ja) * | 2016-05-12 | 2017-11-16 | 日鉄住金鋼板株式会社 | 塗装めっき鋼板 |
| CN111304661A (zh) * | 2019-12-31 | 2020-06-19 | 上海大学 | 铝硅镁镀层及其制备方法 |
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