CN109020554A - 用于熔炼铝锂合金的不锈钢坩埚涂料及其制备方法 - Google Patents
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Abstract
一种用于熔炼铝锂合金的不锈钢坩埚涂料及其制备方法,涂料成分按重量百分比为:粘结剂组分30~40%,骨料60~70%;粘结剂组分按重量百分比含Al(OH)30.6~0.8%,MgO 0.5~0.8%,CrO30.5~0.6%,锌铬黄0.9~1.2%,铝粉19~25%,磷酸溶液31~48%,余量为水;骨料为粒度800~1000目的碳化硅粉;制备方法为:(1)将Al(OH)3和MgO混合后加入水和磷酸,在搅拌条件下加热到50~80℃;(2)加入铝粉、CrO3、锌铬黄和碳化硅粉,搅拌制成浆料;(3)球磨混合至少2h。本发明的涂料在涂覆后用于熔炼铝锂合金,涂层无开裂脱落等现象,所熔炼的铝锂合金铸锭没有碳化硅以及其他夹杂。
Description
技术领域
本发明属于材料加工技术领域,具体涉及一种用于熔炼铝锂合金的不锈钢坩埚涂料及其制备方法。
背景技术
铝锂合金由于其比强度高,比刚度高等特点,在航天、航空等领域得到大量应用,大工业生产使用的铝锂合金熔炼炉结构复杂,投资巨大;近年来,铝锂合金在无人机,自行车和轿车等领域开始应用,这些应用需要小截面的坯料,因此需要小容量的熔炼炉,而这些熔炼炉的坩埚大部分采用不锈钢制造;不锈钢在铝锂合金中溶蚀速度较快,使不锈钢坩埚中的Fe,Ni和Cr等元素溶解到铝锂合金熔体中,一方面使合金纯度降低,另一方面这些元素进入合金熔体中产生化合物,降低合金性能;同时坩埚的溶蚀使坩埚的使用寿命降低,同时也增加了坩埚“漏铝”的危险。
为了避免以上问题,简单、经济的方法是在坩埚内壁涂刷涂料;由于铝锂合金熔体的活度高,因此传统的铝合金熔炼坩埚的涂料都与铝锂合金液反应,反应后产生的渣,污染了合金,同时涂料的防护作用消失;现已查明在铝锂合金液中化学稳定(即与铝锂合金液不反应)的材料只有MgO和SiC。
已有研究在石墨坩埚上等离子喷涂Al2O3,然后涂MgO,再用于熔炼铝锂合金,该方法成本高,不易在不锈钢坩埚上实现,同时由于MgO附着力低,高温下易脱落,所以熔炼1~2炉就需再次喷涂;还有在不锈钢坩埚内壁先涂Al2O3涂层,然后涂MgO,再用于熔炼铝锂合金,MgO附着力更低,所以每次熔炼后,还需要刷涂料,不适合工业生产。
发明内容
针对现有不锈钢坩埚熔炼铝锂合金存在的上述问题,本发明提供一种用于熔炼铝锂合金的不锈钢坩埚涂料及其制备方法,利用SiC在铝锂合金液中的化学稳定性,采用耐高温、耐溶蚀的粘结剂,制成用于铝锂合金熔炼坩埚的耐用高效的涂料。
本发明的用于熔炼铝锂合金的不锈钢坩埚涂料的原料成分按重量百分比为:粘结剂组分30~40%,骨料60~70%;所述的粘结剂组分按重量百分比含Al(OH)3 0.6~0.8%,MgO 0.5~0.8%,CrO3 0.5~0.6%,锌铬黄0.9~1.2%,铝粉19~25%,重量浓度85%的磷酸溶液31~48%,余量为水;所述的骨料为粒度800~1000目的碳化硅粉。
上述的原料中,Al(OH)3的粒度为150~200目,MgO的粒度为200~300目,锌铬黄的粒度为200~300目,铝粉的粒度为300~500目。
本发明的用于熔炼铝锂合金的不锈钢坩埚涂料的制备方法按以下步骤进行:
1、将Al(OH)3和MgO混合均匀,然后加入水和磷酸,在搅拌条件下加热到50~80℃,制成混合溶液;
2、向混合溶液中加入铝粉、CrO3、锌铬黄和碳化硅粉,搅拌均匀制成浆料;
3、将浆料球磨混合至少2h,制成用于熔炼铝锂合金的不锈钢坩埚涂料。
本发明的用于熔炼铝锂合金的不锈钢坩埚涂料的使用方法为:
将不锈钢坩埚内表面打磨去除氧化层,然后将不锈钢坩埚加热到60~80℃;将用于熔炼铝锂合金的不锈钢坩埚涂料用喷枪喷涂到不锈钢坩埚的内表面,然后空气中风干0.5~1h;将喷涂后的不锈钢坩埚升温到750~800℃,保温至少1h,随炉冷却至常温,获得表面涂覆有涂层的用于熔炼铝锂合金的不锈钢坩埚。
上述使用方法中,涂层厚度50~80微米。
上述的使用方法中,升温到750~800℃时的升温速度为5~10℃/min。
本发明的涂料在不锈钢坩埚表面制成的涂层经反复加热至铝锂合金熔炼温度,再经冷却后,涂层没有开裂,脱落等现象;采用该坩埚进行铝锂合金熔炼,反复进行8次以上,涂层没有出现开裂,脱落等现象,并且所熔炼的铝锂合金铸锭没有碳化硅以及其他夹杂。
具体实施方式
本发明实施例中的不锈钢坩埚的材质选用321不锈钢。
本发明实施例中不锈钢坩埚的尺寸为直径Φ300mm,高度1200mm。
本发明实施例中物料混合时采用玻璃容器。
本发明实施例中采用的碳化硅粉为市购产品。
本发明实施例中采用的Al(OH)3、MgO、CrO3、锌铬黄和铝粉为市购分析纯试剂。
本发明实施例中采用的磷酸为市购分析纯试剂,重量浓度85%。
本发明实施例中采用的水为去离子水。
本发明实施例中涂层的主要成分为SiC和Al,其余为P2O5-Al2O3-Cr2O3复合物。
本发明实施例中2A97合金的成分按重量百分比含Li 1.3~1.5%,Cu 3.6~4.0%,Mg 0.5~0.8%,Zn 0.4~0.6%,Mn 0.4~0.5%,Zr 0.1~0.12%,余量为Al和不可避免杂质。
本发明实施例中5A90合金的成分按重量百分比含Li 1.8~2.0%,Mg 5.0~5.5%,Zr 0.1~0.12%,余量为Al和不可避免杂质。
本发明实施例中涂层厚度50~80微米。
本发明实施例中的原料CrO3为片状,制备涂料的过程中溶于水。
实施例1
用于熔炼铝锂合金的不锈钢坩埚涂料的原料成分按重量百分比为:粘结剂组分40%,骨料60%;所述的粘结剂组分按重量百分比含Al(OH)3 0.8%,MgO 0.6%,CrO30.6%,锌铬黄1.1%,铝粉22.5%,磷酸溶液37.9%,余量为水(36.5%);所述的骨料为粒度800~1000目的碳化硅粉;其中,Al(OH)3的粒度为150~200目,MgO的粒度为200~300目,锌铬黄的粒度为200~300目,铝粉的粒度为300~500目;
制备方法为:
将Al(OH)3和MgO混合均匀,然后加入水和磷酸,在搅拌条件下加热到50℃,制成混合溶液;
向混合溶液中加入铝粉、CrO3、锌铬黄和碳化硅粉,搅拌均匀制成浆料;
将浆料球磨混合2.5h,制成用于熔炼铝锂合金的不锈钢坩埚涂料;
使用方法为:
将不锈钢坩埚内表面打磨去除氧化层,然后将不锈钢坩埚加热到80℃;将用于熔炼铝锂合金的不锈钢坩埚涂料用喷枪喷涂到不锈钢坩埚的内表面,然后空气中风干1h;将喷涂后的不锈钢坩埚升温到750℃,升温速度为5℃/min,保温3h,随炉冷却至常温,获得表面涂覆有涂层的用于熔炼铝锂合金的不锈钢坩埚;
涂覆涂层后的不锈钢坩埚以20℃/min的加热速度加热到750℃,保温1小时,空冷到室温,重复加热冷却共10次,坩埚内的涂层没有开裂和脱落;
熔炼铝锂合金2A97,每炉80Kg;先将涂覆涂层后的不锈钢坩埚加热到500℃放入纯铝,纯铝熔化后继续加热至730℃,放入Cu,Al-Mn和Al-Zr中间合金至铝熔体中;中间合金熔化后,重新升温至730℃;加入金属Mg至合金熔体中,并加入覆盖剂LiF+LiCl,再加入纯锂至合金熔体中;在不破坏覆盖剂的条件下,轻微搅拌,然后静置20分钟出炉,通过DC铸造成Φ125mm的2A97合金圆锭;共进行8次熔炼,每次出炉后观察涂层,没有裂纹和脱落现象;获得的各批次圆锭进行断口检查,没有发现SiC类夹杂,经光谱分析,杂质元素含量没有增加;原料中全部的杂质含量按重量百分比为Fe 0.10%,Si 0.08%,Ni 0.005%,Cr 0.003%;获得的2A97合金的杂质含量按重量百分比为Fe 0.10%,Si 0.09%,Ni 0.005%,Cr0.003%。
实施例2
方法同实施例1,不同点在于:
(1)原料成分按重量百分比为:粘结剂组分35%,骨料65%;所述的粘结剂组分按重量百分比含Al(OH)3 0.6%,MgO 0.5%,CrO3 0.5%,锌铬黄0.9%,铝粉19.2%,磷酸溶液47.6%,余量为水;
(2)将Al(OH)3和MgO混合均匀,然后加入水和磷酸,在搅拌条件下加热到60℃;将浆料球磨混合3h;向混合溶液中加入铝粉、CrO3、锌铬黄和碳化硅粉,搅拌均匀制成浆料;
使用方法同实施例1,不同点在于:
(1)不锈钢坩埚加热到70℃;空气中风干0.8h;升温到780℃,升温速度为8℃/min,保温2h;
(2)涂覆涂层后的不锈钢坩埚以20℃/min的加热速度加热到750℃,保温1小时,空冷到室温,重复加热冷却共10次,坩埚内的涂层没有开裂和脱落;
熔炼铝锂合金5A90,先将涂覆涂层后的不锈钢坩埚加热到500℃放入纯铝,纯铝熔化后继续加热至720℃,放入Al-Zr中间合金至铝熔体中;中间合金熔化后,重新升温至720℃;加入金属Mg至合金熔体中,并加入覆盖剂LiF+LiCl,再加入纯锂至合金熔体中;在不破坏覆盖剂的条件下,轻微搅拌,然后静置20分钟出炉,通过DC铸造成Φ125mm的5A90合金圆锭;共进行6次熔炼,每次出炉后观察涂层,没有裂纹和脱落现象;获得的各批次圆锭进行断口检查,没有发现SiC类夹杂,经光谱分析,杂质元素含量没有增加;原料中全部的杂质含量按重量百分比为Fe 0.10%,Si 0.08%,Ni 0.005%,Cr 0.003%;获得的5A90合金的杂质含量按重量百分比为Fe 0.10%,Si 0.08%,Ni 0.004%,Cr 0.003%。
实施例3
方法同实施例1,不同点在于:
(1)原料成分按重量百分比为:粘结剂组分30%,骨料60%;所述的粘结剂组分按重量百分比含Al(OH)3 0.8%,MgO 0.8%,CrO3 0.6%,锌铬黄1.2%,铝粉24.2%,磷酸溶液31.1%,余量为水;
(2)将Al(OH)3和MgO混合均匀,然后加入水和磷酸,在搅拌条件下加热到80℃;将浆料球磨混合2h;向混合溶液中加入铝粉、CrO3、锌铬黄和碳化硅粉,搅拌均匀制成浆料;
使用方法同实施例1,不同点在于:
(1)不锈钢坩埚加热到60℃;空气中风干0.5h;升温到800℃,升温速度为10℃/min,保温1h;
(2)涂覆涂层后的不锈钢坩埚以20℃/min的加热速度加热到750℃,保温1小时,空冷到室温,重复加热冷却共10次,坩埚内的涂层没有开裂和脱落。
Claims (6)
1.一种用于熔炼铝锂合金的不锈钢坩埚涂料,其特征在于原料成分按重量百分比为:粘结剂组分30~40%,骨料60~70%;所述的粘结剂组分按重量百分比含Al(OH)3 0.6~0.8%,MgO0.5~0.8%,CrO3 0.5~0.6%,锌铬黄0.9~1.2%,铝粉19~25%,重量浓度80%磷酸溶液31~48%,余量为水;所述的骨料为粒度800~1000目的碳化硅粉。
2.根据权利要求1所述的一种用于熔炼铝锂合金的不锈钢坩埚涂料,其特征在于所述的Al(OH)3的粒度为150~200目,MgO的粒度为200~300目,锌铬黄的粒度为200~300目,铝粉的粒度为300~500目。
3.一种权利要求1所述的用于熔炼铝锂合金的不锈钢坩埚涂料的制备方法,其特征在于按以下步骤进行:
(1)将Al(OH)3和MgO混合均匀,然后加入水和磷酸,在搅拌条件下加热到50~80℃,制成混合溶液;
(2)向混合溶液中加入铝粉、CrO3、锌铬黄和碳化硅粉,搅拌均匀制成浆料;
(3)将浆料球磨混合至少2h,制成用于熔炼铝锂合金的不锈钢坩埚涂料。
4.一种权利要求1所述的用于熔炼铝锂合金的不锈钢坩埚涂料的使用方法,其特征在于:将不锈钢坩埚内表面打磨去除氧化层,然后将不锈钢坩埚加热到60~80℃;将用于熔炼铝锂合金的不锈钢坩埚涂料用喷枪喷涂到不锈钢坩埚的内表面,然后空气中风干0.5~1h;将喷涂后的不锈钢坩埚升温到750~800℃,保温至少1h,随炉冷却至常温,获得表面涂覆有涂层的用于熔炼铝锂合金的不锈钢坩埚。
5.根据权利要求4所述的用于熔炼铝锂合金的不锈钢坩埚涂料的使用方法,其特征在于所述的涂层厚度50~80微米。
6.根据权利要求4所述的用于熔炼铝锂合金的不锈钢坩埚涂料的使用方法,其特征在于所述的升温到750~800℃时的升温速度为5~10℃/min。
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CN111085658A (zh) * | 2020-01-10 | 2020-05-01 | 上海交通大学 | 用于铝锂合金砂型铸造的多层复合铸型涂料及其涂敷方法 |
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