CN105839041B - 一种制备成分渐变合金材料的热浸镀工艺方法及其设备 - Google Patents
一种制备成分渐变合金材料的热浸镀工艺方法及其设备 Download PDFInfo
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Abstract
本发明涉及一种制备成分渐变合金材料的热浸镀工艺方法及相关设备。该方法直接在基材表面得到合金材料,快速制备成分渐变的镀层合金或镁合金。该方法具体内容如下:(1)以钢(或镍、铜等高熔点材料)丝或带作为基体材料;(2)在坩埚中熔化合金;(3)基体材料经表面处理后,穿过液态合金进行热浸镀;(4)添加合金元素改变金属液成分;(5)得到延基体材料运动方向,成分渐变的合金材料。该方法可在短时间内制备某一成分范围内大量成分渐变的合金镀层,制备成品可作为高通量实验的样品。与其他高通量实验样品的制备方法相比,该方法效率高、成本低,且制备的材料可进行后续加工。
Description
技术领域
本发明属于合金制备技术领域,涉及一种成分渐变合金的制备方法和相关设备。
背景技术
热浸镀金属镀层常用于钢材的防腐处理,提高钢材的使用寿命。金属镀层钢材在建筑业、汽车、家用电器、造船业、电气业等多个领域得到广泛应用。为了提高镀层的耐蚀性、成品率和美观度,实际生产中还会向镀液中添加如镁、钛、钒、镍、铬、稀土等合金元素。但是,热浸镀工艺复杂,制备成本高,新型镀层的开发周期长。
镁合金作为低密度轻质材料,在航空、航天、汽车、机械制造、生物材料等领域广泛应用。并镁合金还具有良好的散热性,可以作为CPU、LED灯的散热器。但是镁合金耐蚀性很差,极大地限制了其在非惰性环境中的应用。开发高耐蚀镁合金已经成为社会迫切的需要。但传统半经验式的开发工艺效率低:合金样品制备周期长、元素范围筛选缓慢,最佳元素成分筛选难度大。
“材料高通量实验”是在短时间内完成大量样品的制备与表征测试。核心价值在于将高重复的制备与表征实验进行快速并行处理,以量变实现材料研究效率的质变。作为“材料基因组技术”的三大方法之一,“材料高通量实验”与“材料计算模拟”和“材料信息学/数据库”有机结合、互相补充,充分发挥其加速材料研发的效能。
借鉴传统连续热浸镀工艺,本发明设计了一种制备成分渐变合金材料的工艺方法。本方法可用于制备成分渐变的和合金镀层材料,筛选最佳元素含量;并且,该方法还可用于制备元素成分渐变的镁合金材料。
发明内容
本发明目的是开发一种制备成分渐变合金材料的热浸镀工艺方法,快速制备成分渐变的热浸镀镀层合金或镁合金,作为高通量实验的样品。
本发明的第一个方面是提供了一种制备成分渐变合金材料的热浸镀工艺方法,其特征在于有以下的工艺步骤:
a.用规格为长度为20m,直径为1mm丝或长宽厚为15m×0.10m×0.01 m的金属带作为基体材料,其中金属成分为钢或镍或铜,安装于浸镀设备上;
b.将镀液合金在锌锅中完全熔化,熔化温度为580℃-700℃;
c.将浸镀组件沉没辊和退火炉浸没于镀液中,并在退火炉内充入10%H2+90%N2混合的还原性气氛;
d.基体材料经过表面清洗和温度在600℃-850℃的退火还原后,穿过液态合金进行连续热浸镀;
e.当在基体材料表面能获得质量稳定的合金材料时,向锌锅内加入目标合金,使镀液内目标合金元素成分缓慢稳定改变;随着目标合金的缓慢溶解,得到延基体材料运动方向,特定成分渐变的合金材料。
本发明的第二个方面是提供了一种用于制备成分渐变合金材料的热浸镀设备。其特征部分在于以下部分:
a.参考工业化连续热浸镀工艺,提供了小型化连续热浸镀设备,主要包括用于基体材料清洁处理的碱洗酸洗池(或燃烧除油炉)、用于氢气还原的退火炉、进行浸镀金属镀液的锌锅、浸镀后镀层材料的退火炉、镀层平整用气刀、用于镀层冷却的水雾喷嘴;
b.增加了一组用于合金元素添加的辅助装置。
本发明提供的制备成分渐变合金材料的热浸镀工艺方法具有如下优点:
1.该方法可以在丝、带材表面获得成分连续变化的合金材料;
2.该方法较磁控溅射或3D打印技术,制备合金材料的效率高、成本低;
3.该方法得到的合金组织处于稳态或亚稳态,具有更广泛的适用性,可以进行后续深加工,从而可对合金材料的其他性能进行深入研究,研究意义更大。
附图说明
图1为用于制备成分渐变合金材料的热浸镀整体设备主视图, 图中标号:1.碱洗酸洗池(或燃烧除油炉);2.还原退火炉;3.锌锅;4.退火炉,炉内放置气刀;5.水雾冷却喷嘴;6.合金添加辅助装置。
图2 为热浸镀设备浸镀部分俯视图;
图3为含Ti 0.035%的Al–Zn–Si–Ti镀层SEM照片,深灰色为富Al相,浅灰色为富Zn相;
图4为Mg–4Nd–1Zn–0.5Zr合金SEM照片,深色为Mg集体,灰色为富Nd相。
具体实施方式
在一下实施例中具体列举了本发明优选的实施方式,但是应当理解,本发明的保护范围不仅限于此。以下实例中所使用的原材料均为商业购买,未经进一步处理直接使用。
实施例1
使用制备成分渐变合金材料的热浸镀设备进行实验如附图1,以长度为20 m,直径为1 mm的钢丝为基体材料,安装在浸镀设备上。将成分为55Al–43.4Zn–1.6Si的镀液合金在锌锅中完全融化并搅拌均匀,镀液合金融化温度为610 ℃。将浸镀组件沉没辊和退火炉浸没于镀液中,并在退火炉内持续充入氢压混合气(10%H2+90%N2)。用碱性溶液和酸性溶液对钢丝进行表面清洗,去除表面的油污和氧化皮,露出新鲜的Fe基体。清洗后的钢丝的递送速率为1.0 m/min的速度通过850 ℃的退火炉进行还原退火。钢丝退火后进入锌锅进行连续热浸镀。待钢丝表面形成质量均匀的合金镀层时,利用合金添加辅助装置向镀液中缓慢浸入Zn–1Ti合金块。Zn–1Ti合金经6 min完全浸入,8 min完全融化。同时每隔2min取一次镀液样品,并标记钢丝位置。随着Zn–1Ti合金的溶解及钢丝的递送,在钢丝表面制备了成分连续变化的镀层合金,其成分范围为55Al–43.4Zn–1.6Si到55Al–43.4Zn–1.6Si–0.1Ti,其中含Ti 0.035%的Al-Zn-Si-Ti镀层SEM照片如附图2所示。深灰色为富Al相,浅灰色为富Zn相。
实施例2
使用制备成分渐变合金材料的热浸镀设备进行实验如附图1,以长宽厚为15 m ×0.10 m ×0.01 m的钢带为基体材料,安装在浸镀设备上。将成分为55Al–43.4Zn–1.6Si的镀液合金在锌锅中完全融化并搅拌均匀,镀液合金融化温度为630 ℃。将浸镀组件沉没辊和退火炉浸没于镀液中,并在退火炉内持续充入氢氮混合气(10%H2+90%N2)。用碱性溶液和酸性溶液对钢带进行表面清洗,去除表面的油污和氧化皮,露出新鲜的Fe基体。清洗后的钢带的递送速率为0.6 m/min的速度通过750 ℃的退火炉进行还原退火。钢带退火后进入锌锅进行连续热浸镀。待钢带表面形成质量均匀的合金镀层时,利用合金添加辅助装置,向镀液中浸入纯Mg块。Mg块经10 min完全浸入,15min完全融化。同时每隔2min取一次镀液样品,并标记钢带位置。随着镁的溶解及钢带的递送,在整块钢带上镀上连续的镀层合金,其成分范围为55Al–43.4Zn–1.6Si到53Al–41.4Zn–1.6Si–4Mg。
实施例3
使用制备成分渐变合金材料的热浸镀设备进行实验如附图1,以长度为20 m,直径为1 mm的铜丝为基体材料,安装在浸镀设备上。将成分为99.5Mg–0.5Zr的合金液在坩锅中完全融化并搅拌均匀,合金融化温度为680 ℃,合金液表面用。将浸镀组件沉没辊和退火炉浸没于镀液中,并在退火炉内持续充入氢氮混合气(10%H2+90%N2)。用碱性溶液和酸性溶液对铜丝进行表面清洗,去除表面的油污和氧化皮,露出新鲜的Cu基体。清洗后的铜丝的递送速率为1.2 m/min的速度通过800 ℃的退火炉进行还原退火。铜丝退火后进入锌锅进行连续热浸镀。待铜丝表面形成质量均匀的合金镀层时,利用合金添加辅助装置,向镀液中缓慢浸入Zn–Ti合金块。Nd–20Zn合金经3 min完全浸入,15 min完全融化。同时每隔2min取一次合金液样品,并标记铜丝位置。随着Zn–Nd合金的溶解及铜丝的递送,在铜丝表面制备了成分连续变化的镀层合金,其成分范围为99.5Mg–0.5Zr到93.5Mg–5Nd–1Zn–0.5Zr,其中Mg–Nd–Zn–Zr镀层SEM照片如附图3所示。深色为Mg基体,灰色为富Nd相。
实施例4
使用制备成分渐变合金材料的热浸镀设备进行实验如附图1,以长宽厚为15 m ×0.15 m ×0.01 m的镍带为基体材料,安装在浸镀设备上。将成分为99.5Mg–0.5Zr的合金液在坩锅中完全融化并搅拌均匀,合金融化温度为690 ℃。将浸镀组件沉没辊和退火炉浸没于镀液中,并在退火炉内持续充入氢压混合气(10%H2+90%N2)。用碱性溶液和酸性溶液对镍带进行表面清洗,去除表面的油污和氧化皮,露出新鲜的Ni基体。清洗后的钢带的递送速率为0.8 m/min的速度通过750 ℃的退火炉进行还原退火。镍带退火后进入锌锅进行连续热浸镀。待镍带表面形成质量均匀的合金镀层时,利用合金添加辅助装置,向镀液中缓慢浸入Zn–Ti合金块。La–50Zn合金经3 min完全浸入,10 min完全融化。同时每隔2min取一次合金液样品,并标记镍带位置。随着镁的溶解及钢带的递送,在整块钢带上镀上连续的镀层合金,其成分范围为99.5Mg–0.5Zr到95.5Mg–2Nd–2Zn–0.5Zr。
Claims (2)
1.一种制备成分渐变合金材料的热浸镀工艺方法,其特征在于该方法具有以下的工艺步骤:
a.用规格为长度为20m,直径为1mm丝或长宽厚为15m×0.10m×0.01m的金属带作为基体材料,其中金属成分为钢或镍或铜,安装于浸镀设备上;
b.将镀液合金在锌锅中完全熔化,熔化温度为580℃-700℃;
c.将浸镀组件沉没辊和退火炉浸没于镀液中,并在退火炉内充入10%H2+90%N2混合的还原性气氛;
d.基体材料经过表面清洗和温度在600℃-850℃的退火还原后,穿过液态合金进行连续热浸镀;
e.当在基体材料表面能获得质量稳定的合金材料时,向锌锅内加入目标合金,使镀液内目标合金元素成分缓慢稳定改变;随着目标合金的缓慢溶解,得到延基体材料运动方向,成分渐变的合金材料。
2.一种实施权利要求1所述制备成分渐变合金材料的热浸镀工艺方法,用于制备成分渐变合金材料的热浸镀设备,其特征在于以下部分:
a.参考工业化连续热浸镀工艺,提供了小型化连续热浸镀设备,主要包括用于基体材料清洁处理的碱洗酸洗池、用于氢气还原的退火炉、进行浸镀金属镀液的锌锅、浸镀后镀层材料的退火炉、镀层平整用气刀、用于镀层冷却的水雾喷嘴;
b.增加了一组用于合金元素添加的辅助装置。
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