CN115044907B - 低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂及其使用方法 - Google Patents
低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂及其使用方法 Download PDFInfo
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Abstract
本发明公开了一种低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂,包括腐蚀溶液Ⅰ和腐蚀溶液Ⅱ,所述腐蚀溶液Ⅰ包括冰醋酸、草酸、氯化铁、十二烷基苯磺酸钠和水;所述腐蚀液Ⅱ为含硝酸的乙醇溶液;所述腐蚀剂的使用方法包括以下步骤:(1)将金相试样先奥氏体化,再水淬,最后磨抛;(2)将金相试样抛光面朝上浸入50~70℃的腐蚀液Ⅰ中,热腐蚀30~50秒,然后冲洗、干燥;(3)用腐蚀溶液Ⅱ轻轻擦拭金相试样的抛光面,直至表面呈银灰色,然后冲洗、干燥;(4)通过金相显微镜观察待检测样品的原奥氏体晶界的显示情况;该腐蚀剂不含有苦味酸,能清晰显示低碳压力容器用钢的原奥氏体晶界,操作简单、高效且具有较好的重现性。
Description
技术领域
本发明涉及一种钢材金相检验腐蚀剂,特别涉及一种低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂及其使用方法。
背景技术
低碳压力容器钢广泛应用于建造液化石油气(LPG)等低温储罐,除了要求较高的强度等级之外,还对-40℃~-60℃下的低温冲击韧性提出了严格的标准。钢的低温冲击韧性与其原奥氏体晶粒尺寸密切相关,两者总体上呈反比关系,因此,有效观察和测量低碳压力容器钢的原奥氏体晶粒尺寸对于其生产工艺调整和性能优化具有重要意义。
奥氏体晶界的显示方法主要有氧化法和化学试剂腐蚀法。氧化法利用奥氏体晶界处优先形成网络状的渗碳体和氧化亚铁等组成物来显示奥氏体晶界,适用于任何种类的结构钢和工具钢,但其工艺复杂,难以掌控。目前最常用的奥氏体晶界的显示方法是化学试剂腐蚀法,即将钢铁样品在高温奥氏体化后直接水淬获得马氏体,采用化学试剂腐蚀抛光后的样品,促使原奥氏体晶界的优先腐蚀而得到显示,其方法操作简单且效果明显。苦味酸水溶液是一种效果良好的腐蚀剂,但目前已被国家列为易制毒、易制爆管控制品而被禁用。
目前已有若干专利公开了可替代苦味酸溶液的腐蚀剂:公告号为CN105823671A的专利发明了一种中锰汽车用钢原奥氏体晶界的显示方法,其腐蚀剂组分及配方为:浸蚀剂1,蒸馏水:亚硫酸氢钠固体颗粒=(3~4):1;浸蚀剂2,按体积比,硝酸:无水乙醇=1:(9~24);先用浸蚀剂1腐蚀样品抛光面至雾面,然后用酒精冲洗,接着用浸蚀剂2腐蚀一定时间,但采用该专利对低碳压力容器用钢进行腐蚀,无法显示奥氏体晶界,说明该专利只适合特定钢种,局限性较强;公告号为CN112213171A的专利发明了一种S34MnV钢原始奥氏体晶界的腐蚀显示方法,其腐蚀剂组分及配方为:ET08-乙醇溶液(ET08购于浙江国检检测技术股份有限公司,ET08的质量分数为80%~90%),将抛光后的试样置于温度为70~75℃的腐蚀溶液中,热腐蚀40~50min至试样表面出现均匀分布的黄色斑点,最后取出试样并用清水冲洗即可,但具体配方保密未公布,且成本较高、腐蚀时间较长;公告号为CN102888608A的专利发明了一种显示细晶粒奥氏体不锈钢晶界的腐蚀剂及其制备方法,其腐蚀剂组分及配方为:80~150mL水,10~20mL质量分数为36%盐酸,15~25g氯化铁,10~15gCuCl2·2H2O,2.0~7.0mL冰醋酸,1-5滴新吉尔灭,均匀混合后进行腐蚀即可,但该腐蚀剂只适用于含有大量Cr、Ni等元素的不锈钢。因此,针对低碳压力容器钢,研发一种能有效替代苦味酸且能显示原奥氏体晶界的新型腐蚀剂及其显示方法已成为当前的迫切要求。
发明内容
发明目的:本发明旨在提供一种能清晰显示低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂,且不包含苦味酸水溶液;本发明的另一目的提供该腐蚀剂的使用方法。
技术方案:本发明的一种低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂,包括腐蚀溶液Ⅰ和腐蚀溶液Ⅱ,所述腐蚀溶液Ⅰ包括冰醋酸、草酸、氯化铁、十二烷基苯磺酸钠和水;所述腐蚀液Ⅱ为含硝酸的乙醇溶液。
所述腐蚀液Ⅰ中,冰醋酸和草酸均是弱酸,可腐蚀并显现奥氏体晶界而不腐蚀和显现马氏体板条群晶界。冰醋酸和草酸的共同作用还能有效溶解腐蚀产物并消除低碳压力容器用钢表面的钝化膜,使腐蚀过程能有效进行。氯化铁作为阴极去极化剂,可促进原奥氏体晶界区的电化学反应使晶界被腐蚀,产生凹陷,在显微镜下显现。十二烷基苯磺酸钠具有缓蚀作用,可以降低腐蚀速率,避免因速度过快而导致过腐蚀。腐蚀液Ⅰ使奥氏体晶界得到初步显示,而马氏体板条群晶界的腐蚀得到抑制。腐蚀液Ⅱ继续腐蚀来加深奥氏体晶界,使晶界的显示更为清晰。
优选的,所述腐蚀液Ⅰ中,每100mL溶液中含有4~6g冰醋酸,10~15g草酸,5~10g氯化铁,5~9g十二烷基苯磺酸钠,其余为水。
腐蚀液Ⅰ的配制:倒入少量去离子水于烧杯中,分别称量草酸、氯化铁和十二烷基苯磺酸钠,倒入烧杯中,并用玻璃棒不断搅拌使其能够充分溶解;然后称取冰醋酸倒入烧杯中,最后再往烧杯中加入去离子水定容即可。
优选的,所述腐蚀液Ⅱ中,硝酸的体积分数为4~6%,其余为乙醇;所述硝酸为质量分数为65~70%的硝酸,所述乙醇为无水乙醇。
腐蚀液Ⅱ的配制:烧杯中先倒入少量的无水乙醇,再量取硝酸于烧杯中,最后继续倒入无水乙醇定容即可。
本发明的腐蚀液的使用方法,包括以下步骤:
(1)将金相试样先奥氏体化,再水淬,最后磨抛;
(2)将金相试样抛光面朝上浸入50~70℃的腐蚀液Ⅰ中,热腐蚀30~50秒,然后冲洗、干燥;
(3)用腐蚀溶液Ⅱ轻轻擦拭金相试样的抛光面,直至表面呈银灰色,然后冲洗、干燥;
(4)通过金相显微镜观察的待检测样品的原奥氏体晶界的显示情况。
所述步骤(1)中,金相试样先奥氏体化,然后水淬获得马氏体,使试样保留原奥氏体晶界;优选的,金相试样在900~950℃保温30~60分钟进行奥氏体化。
所述金相试样为含C质量分数0.12~0.17%,Si质量分数0.20~0.36%,Mn质量分数1.3~1.6%,Cr质量分数0.045-0.180%,Ni质量分数0.042-0.310%,Mo质量分数0.005-0.120%的钢材。
所述步骤(2)使金相试样的奥氏体晶界得到初步显示,而马氏体板条群晶界的腐蚀得到抑制;步骤(3)采用擦拭的方式,好控制腐蚀情况,加深了奥氏体晶界,使晶界的显示更为清晰,但不会使马氏体板条群的晶界因腐蚀而显现。
发明机理:本发明的腐蚀剂包括腐蚀液Ⅰ和腐蚀液Ⅱ。在腐蚀溶液Ⅰ中,冰醋酸和草酸均是弱酸,其共同作用可腐蚀并显现奥氏体晶界而不腐蚀和显现马氏体板条群晶界;此外冰醋酸和草酸的共同作用还能有效溶解腐蚀产物并消除低碳压力容器用钢表面的钝化膜,使腐蚀过程能有效进行。氯化铁作为阴极去极化剂,可促进原奥氏体晶界区的电化学反应,有利于晶界产生腐蚀凹陷。十二烷基苯磺酸钠具有缓蚀作用,可降低腐蚀速率,避免因速度过快而导致过腐蚀。先将金相试样在腐蚀液Ⅰ中进行热腐蚀,使奥氏体晶界得到初步显示,而马氏体板条群晶界的腐蚀得到抑制。第二步采用腐蚀液Ⅱ继续腐蚀来加深奥氏体晶界,使晶界的显示更为清晰,采用擦拭的方式,好控制腐蚀情况,不会使马氏体板条群的晶界因腐蚀而显现。
有益效果:与现有技术相比,本发明具有如下显著优点:(1)该腐蚀剂不含有苦味酸,能清晰显示低碳压力容器用钢的原奥氏体晶界;(2)通过对腐蚀液Ⅰ中各组分配比的调整和设计,有效降低腐蚀剂的腐蚀速率和氧化能力,并能有效溶解腐蚀产物并消除钢表面的钝化膜,最终使奥氏体晶界优先显现出来,而马氏体板条群的晶界腐蚀得到有效抑制;(3)整个显示方法安全可靠,操作简单方便,整个操作流程时间短且能适用于一系列的低碳压力容器用钢原奥氏体晶界的腐蚀,适用范围较宽。
附图说明
图1是实施例1中金相试样腐蚀后的奥氏体晶粒的金相照片;
图2是实施例2中金相试样腐蚀后的奥氏体晶粒的金相照片;
图3是实施例3中金相试样腐蚀后的奥氏体晶粒的金相照片;
图4是对比例1中金相试样腐蚀后的金相照片;
图5是对比例2中金相试样腐蚀后的金相照片。
具体实施方式
下面结合实施例对本发明的技术方案作进一步说明。
实施例1
本发明的低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂,包括腐蚀溶液Ⅰ和腐蚀溶液Ⅱ,腐蚀溶液Ⅰ:100mL溶液中含有6g冰醋酸,12g草酸,5g氯化铁,7g十二烷基苯磺酸钠,其余为水;腐蚀溶液Ⅱ:硝酸的体积分数为6%,其中硝酸的质量分数为65%。
腐蚀溶液Ⅰ的配制:取40mL去离子水于烧杯中,称量12g草酸、5g氯化铁、7g十二烷基苯磺酸钠倒入烧杯中,并用玻璃棒不断搅拌使其能够充分溶解;然后称取6g冰醋酸倒入烧杯中,再加入去离子水定容到100mL,混合均匀。
腐蚀溶液Ⅱ的配制:向25mL无水乙醇中加入3mL质量分数65%硝酸于烧杯中混合均匀,继续加入无水乙醇定容到50mL,混合均匀。
本发明的低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂的使用方法,包括以下步骤:
(1)将金相试样加热至920℃保温30分钟进行奥氏体化,随后水淬至室温,然后对试样进行磨抛处理;其中金相试样的化学成分(wt%):C 0.12%,Si 0.36%,Mn 1.4%,P0.025%,S 0.010%,Cr 0.045%,Ni 0.310%,Mo 0.090%,Nb 0.012%,Ti 0.018%,V0.020%,余量为Fe;
(2)将金相试样抛光面朝上浸入60℃的腐蚀液Ⅰ中,热腐蚀45秒,用去离子水冲洗表面残留腐蚀剂,干燥;
(3)用脱脂棉蘸取腐蚀溶液Ⅱ,轻轻擦拭第(2)步腐蚀后待测试样的抛光面,直至表面呈银灰色,之后用酒精冲洗然后吹干;
(4)在金相显微镜下观察其奥氏体晶界,结果如图1所示。
由图1可以看出,在920℃保温30分钟的条件下,奥氏体晶粒比较细小,大小存在一定差异,但总体均匀;其中,奥氏体晶内的马氏体板条群晶界的腐蚀得到有效抑,而奥氏体晶界得到优先腐蚀,清晰可辨,这表明本实施例的腐蚀剂和腐蚀方法能清晰地显示该种低碳压力容器钢的奥氏体晶界。
实施例2
本发明的低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂,包括腐蚀溶液Ⅰ和腐蚀溶液Ⅱ,腐蚀溶液Ⅰ:100mL溶液中含有4g冰醋酸,15g草酸,7g氯化铁,9g十二烷基苯磺酸钠,其余为水;腐蚀溶液Ⅱ:硝酸的体积分数为4%,其中硝酸的质量分数为70%。
腐蚀溶液Ⅰ的配制:取40mL去离子水于烧杯中,称量15g草酸、7g氯化铁、9g十二烷基苯磺酸钠倒入烧杯中,并用玻璃棒不断搅拌使其能够充分溶解;然后称取4g冰醋酸倒入烧杯中,再加入去离子水定容到100mL,混合均匀。
腐蚀溶液Ⅱ的配制:向25mL无水乙醇中加入2mL质量分数70%硝酸于烧杯中混合均匀,继续加入无水乙醇定容到50mL,混合均匀。
本发明的低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂的使用方法,包括以下步骤:
(1)将金相试样加热至900℃保温45分钟进行奥氏体化,随后水淬至室温,然后对试样进行磨抛处理;其中金相试样的化学成分(wt%):C 0.14%;Si 0.30%,Mn 1.3%,P0.010%,S 0.010%,Cr 0.180%,Ni 0.042%,Mo 0.005%,Nb 0.038%,Ti 0.002%,V0.002%,余量为Fe;
(2)将金相试样抛光面朝上浸入50℃的腐蚀液Ⅰ中,热腐蚀50秒,用去离子水冲洗表面残留腐蚀剂,干燥;
(3)用脱脂棉蘸取腐蚀溶液Ⅱ,轻轻擦拭第(2)步腐蚀后待测试样的抛光面,直至表面呈银灰色,之后用酒精冲洗然后吹干;
(4)在金相显微镜下观察其奥氏体晶界,结果如图2所示。
由图2可以看出,在900℃保温45分钟的条件下,奥氏体晶界得到优先腐蚀,清晰可辨。由于奥氏体化温度较低,其晶粒尺寸较实施例1略为细小。这表明本实施例的腐蚀剂和腐蚀方法能清晰地显示该种低碳压力容器钢的奥氏体晶界。
实施例3
本发明的低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂,包括腐蚀溶液Ⅰ和腐蚀溶液Ⅱ,腐蚀溶液Ⅰ:100mL溶液中含有5g冰醋酸,10g草酸,10g氯化铁,5g十二烷基苯磺酸钠,其余为水;腐蚀溶液Ⅱ:硝酸的体积分数为5%,其中硝酸的质量分数为68%。
腐蚀溶液Ⅰ的配制:取40mL去离子水于烧杯中,称量10g草酸、10g氯化铁、5g十二烷基苯磺酸钠倒入烧杯中,并用玻璃棒不断搅拌使其能够充分溶解;然后称取5g冰醋酸倒入烧杯中,再加入去离子水定容到100mL,混合均匀。
腐蚀溶液Ⅱ的配制:向25mL无水乙醇中加入2.5mL质量分数68%硝酸于烧杯中混合均匀,继续加入无水乙醇定容到50mL,混合均匀。
本发明的低碳压力容器用钢的原奥氏体晶界显示的腐蚀剂的使用方法,包括以下步骤:
(1)将金相试样加热至950℃保温60分钟进行奥氏体化,随后水淬至室温,然后对试样进行磨抛处理;其中金相试样的化学成分(wt%):C 0.17%,Si 0.20%,Mn 1.6%,P0.022%,S 0.015%,Cr 0.120%,Ni 0.210%,Mo 0.120%,Nb 0.020%,Ti 0.010%,V0.040%,余量为Fe;
(2)将金相试样抛光面朝上浸入70℃的腐蚀液Ⅰ中,热腐蚀30秒,用去离子水冲洗表面残留腐蚀剂,干燥;
(3)用脱脂棉蘸取腐蚀溶液Ⅱ,轻轻擦拭第(2)步腐蚀后待测试样的抛光面,直至表面呈银灰色,之后用酒精冲洗然后吹干;
(4)在金相显微镜下观察其奥氏体晶界,结果如图3所示。
由图3可以看出,在950℃保温60分钟的条件下,由于奥氏体化温度较高且保温时间较长,奥氏体晶粒较实施例1和实施例2发生明显粗化,且混晶现象(粗大晶粒和细小晶粒混杂在一起)十分明显。这表明本实施例的腐蚀剂和腐蚀方法能清晰地显示该种低碳压力容器钢的奥氏体晶界。
对比例1
在实施例2的基础上,将冰醋酸替换为同等质量的草酸,其余腐蚀剂配方以及所采用的显示方法与实施例2完全相同。在金相显微镜下观察,结果如图4。
由图4可以看出,没有显示出奥氏体晶界,只能观察到马氏体组织,这表明,只有草酸的情况下,无法清晰地显示该种低碳压力容器钢的奥氏体晶界。这也说明了冰醋酸和草酸的共同作用对于优先腐蚀并显现该种低碳压力容器钢的奥氏体晶界十分重要。
对比例2
在实施例2的基础上,将草酸替换为同等质量的冰醋酸,其余腐蚀剂配方以及所采用的显示方法与实施例2完全相同。在金相显微镜下观察,结果如图5。
由图5可以看出,没有显示出奥氏体晶界,只能观察到马氏体组织,这表明,只有冰醋酸的情况下,无法清晰地显示该种低碳压力容器钢的奥氏体晶界。这也说明了冰醋酸和草酸的共同作用对于优先腐蚀并显现该种低碳压力容器钢的奥氏体晶界十分重要。
Claims (3)
1.一种低碳压力容器用钢的原奥氏体晶界的显示方法,其特征在于,包括以下步骤:
(1)将金相试样先奥氏体化,再水淬,最后磨抛;
(2)将金相试样抛光面朝上浸入50~70℃的腐蚀液Ⅰ中,热腐蚀30~50秒,然后冲洗、干燥;
(3)用腐蚀液Ⅱ轻轻擦拭金相试样的抛光面,直至表面呈银灰色,然后冲洗、干燥;
(4)通过金相显微镜观察待检测样品的原奥氏体晶界的显示情况;
所述腐蚀液Ⅰ中,每100 mL溶液中含有4~6g冰醋酸,10~15g草酸,5~10g氯化铁,5~9g十二烷基苯磺酸钠,其余为水;
所述腐蚀液Ⅱ中,硝酸的体积分数为4~6%,其余为乙醇;所述硝酸为质量分数为65~70%的硝酸,所述乙醇为无水乙醇。
2.根据权利要求1所述的显示方法,其特征在于,步骤(1)中,所述金相试样为含C质量分数0.12~0.17%,Si质量分数0.20~0.36%,Mn质量分数1.3~1.6%,Cr质量分数0.045~0.180%,Ni质量分数0.042~0.310%,Mo质量分数0.005~0.120%的钢材。
3.根据权利要求1所述的显示方法,其特征在于,步骤(1)中,金相试样奥氏体化为在900~950℃,保温30~60分钟。
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