镍基合金中非金属夹杂物及其去除技术的研究
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摘要
随着航空、航天、导弹和电子工业技术的飞速发展,对镍基合金的质量要求日益严格,尤其是对镍基合金中的线材,不仅要求其具有合格的化学成分和使用性能,而且还要求其具有合格的内在质量和表面质量。本文对某合金厂生产的4J43合金和Cr20Ni80合金线材出现的表面缺陷等质量问题进行了研究,发现与国内外同类产品相比,其合金成分较好,但合金中含有大量的脆性非金属夹杂物,这是导致产品出现表面裂纹、凹坑等质量问题的主要原因。针对目前镍基合金中非金属夹杂物的研究滞后,没有统一的鉴定和检测标准等问题,研究开发了新型的电解液,并采用金相检验与电解检验相结合的方法,对镍基合金线材中的非金属夹杂物进行了系统的研究,分析了合金中夹杂物的来源,并针对4J43合金和Cr20Ni80合金的生产工艺进行了优化。初步获得了较好的研究结果。
配制了以复合含氧酸盐、氯化钠、柠檬酸钠为电解质的电解液,该电解液不仅可以高效萃取出镍基合金中的非金属夹杂物,而且电解过程中电解液温度变化小、PH值恒定,絮状的阳极泥沉淀少,电解过程平稳,电解后半透膜中的夹杂物混杂的金属掉渣少,清洗分离容易,收得率高,萃取所得的夹杂物较好地保留了在合金中的原貌,提高了实验分析的准确性。
两种镍基合金中的夹杂物主要是熔炼过程生成的脱氧产物,因在浇注前未能完全上浮而滞留在合金中,属内生夹杂物。这些由Al、Si、Ca、Mn、Mg、Ti、Fe、Ni等元素组成的硅酸盐、铝酸盐及它们的复合夹杂物,在合金中因生成的时间、凝固的条件以及成分的不同而呈球状、小块状、条状及不规则形状。其中,大尺寸的脆性宏观夹杂物对合金的性能影响最大,尤其是4J43和Cr20Ni80合金中由Ti、Al、Fe组成的复合夹杂物,这类夹杂物主要是熔炼中钛脱氧产生的钛的氧化物或氮化物,多以锐角规则形貌出现,尺寸在20-300μm,变形率低、并具有较高的硬度。由于这种脆性夹杂物与合金基体之间在变形性方面存在着较大的差异,在加工变形过程中,合金基体的均匀连续性受到破坏,引起应力集中,导致合金基体与夹杂物交界处产生微裂纹,并且随着应力的增加,裂纹扩展并最终形成宏观缺口或断丝。
采用三元酸性渣系CaF_2-Al_2O_3-CaO对中频感应熔炼后的4J43合金进行电渣重熔,实验证实,在此渣系下电渣重熔工艺稳定,电渣重熔后的4J43合金中非金属夹杂物总量减少了近40%,大于50μm的夹杂物完全消除,夹杂物的粒径主要控制在0～20μm,由于电渣重熔前合金中的脆性夹杂物(以铝酸盐为主的复合夹杂物和附合了氧化铝和氧化铁的氧化钛、氮化钛夹杂物)在重熔过程中已完全去除,重熔后合金中的新生夹杂物主要是塑性的硅酸盐类夹杂,使得合金的抗拉强度和延伸率都有较大的提高,但重熔前后4J43合金膨胀性能无明显变化,均在国标规定范围内。下游用户质量反馈证实:新工艺生产的4J43合金其表面质量和后续加工的成材率都比以前有较大提高。
实验研究了钢包吹氩工艺参数对Cr20Ni80合金中夹杂物去除效果的影响,当吹氩量大于3.5L/min时,吹氩后夹杂物不但没有减少还有所增加,特别是大尺寸夹杂物,这主要是吹氩量大时氩气泡尺寸较大,引起钢液波动造成钢液卷渣和二次氧化;吹氩量选择在3L/min时,夹杂物去除效果最好,与未吹氩相比,合金中夹杂物可减少23%,特别是大尺寸夹杂物减少了12%,实验检测证实,在这种吹氩参数下生产的Cr20Ni80合金,其快速寿命和力学性能都有较大的提高,用户反馈得到了相同的结果。
With the rapid development of aviation,aerospace,missile and electronic industrial technology,the requirements for Ni-based alloys are stricter,especially for thin wires. Not only chemical constitution and service performance are limited,but also inner and surface qualities are required.The quality of 4J43 alloy and Cr20Ni80 alloy wires produced by one alloy company is examined and compared with the same products at home and abroad.It is found that all the alloy composition is coincident with standard requirement.But there are a lot of non-metallic inclusions in these two alloys and these nonmetallic inclusions may be the main cause of crack and break in products.Few people investigated on the behavior of non-metallic inclusions in the Ni-base alloy wire so far.In the paper new electrolyte used for electrolyzing Ni-based alloys is invented. Both metallographic examination and electrolytic assay are used to study nonmetal inclusions in Ni-based wires produced by normal process.The sources of inclusions in alloys are analyzed and process optimizing experiments for 4J43 alloy and Cr20Ni80 alloy are applied.Good test results are gained recently.
New neutral electrolyte is made up by mixing oxysalt,sodium chloride and citric acid, etc.New electrolyte can not only effectively extract nonmetal inclusions in Ni-based alloys but also can have other good characters,such as,temperature and PH value is invariable during electroanalysis,anode mud precipitation of garrulous shape is little, electroanalysis process is calm;garrulous precipitation mixed in inclusions in half transparent film is so little that can be easily cleaned & separated,and high harvest rate is acquired.The inclusions extracted keep their former morphologies well in alloy,thus improving the veracity of experiment.
The main inclusions existed in two Ni-based alloys are deoxidation results in melting process.These deoxidation results,which are detained in alloys owing to incomplete floating off before pouring,are endogenesis impurity.Silicate,aluminate and their composite inclusions are composed of elements such as Al,Si,Ca,Mn,Mg,Ti,Fe,Ni and so on.These inclusions exhibit many shapes such as sphericity、tablet、strip and abnormal shape because of different inborn time、solidified condition and component.In these kinds of Ni-based alloys,big brittle macroscopic inclusions have the huge impact on the properties of alloys,especially the composite inclusions composed of Ti、Al、Fe in 4J43 alloy and Cr20Ni80 alloy.This kind of impurity is mainly titanic oxides or nitrides generated by oxidizing of titanium in smelting which exhibits abnormal acute angle with size of 20-300μm and higher rigidity,belonging to brittle impurity with low strain rate.Because a rather large difference existed between fragile inclusions and alloy matrix in deformability,uniformity and continuity of alloy matrix were destroyed during the processing and deforming,causing stress concentration,inducing tiny cracks generated in the edge between alloy matrix and inclusions.With the increase of strain force,the crack extended and macroscopic gap or fracture formed.
4J43 alloy processed by medium frequency induction melting is treated by electroslag remelting used ternary acid residue system of CaF2-Al2O3-CaO in industrial experiment.The results show that the process of electroslag remelting is stable under acid residue system and thus can effectively decrease nonmetal inclusions in 4J43 alloy. The total amounts of nonmetal inclusions decrease about 40%than those of normal process withous remeltingand whose sizes are bigger than 50μm disappear.The sizes of inclusions are in the range of 0-20μm.Inclusions are mainly brittle inclusions such as composite impurity which is mainly composed by aluminate and titanium oxide (titanium nitride)with some alumina and femic oxide before remelting.But,inclusions are mainly plastic silicate after electroslag remelting.The reason is that nonmetal inclusions in 4J43 alloy have been wiped off and new inclusions are created during remelting process.Tensile strength and elongation improve greatly,but the expansion property varies very samall and all fit the requirement of the state standard.The following process show that the rate of finished products improve
The influence of bottom blowing argon of lidale on the effect of removing of inclusions for 2080 alloy is studied by industrial experiment.The results show that only proper blowing argon flux can gain good removing effect.When the argon flux is stronger than 3.5L/min,inclusions increase after blowing argon,especially big size inclusions.It is because that strong blowing flux conduce big air bubbles,arising big fluctuation and rolling residue of molten steel and farther oxidation also.When the argon flux is 3.5L/min,the removing effect is best,inclusions decreasing 23%, especially big size inclusions decreasing 12%,compared with normal process without blowing argon.The test results show that mechanical property and accelerated test lifetime improve greatly after bottom blowing argon and clients give the same results.
配制了以复合含氧酸盐、氯化钠、柠檬酸钠为电解质的电解液,该电解液不仅可以高效萃取出镍基合金中的非金属夹杂物,而且电解过程中电解液温度变化小、PH值恒定,絮状的阳极泥沉淀少,电解过程平稳,电解后半透膜中的夹杂物混杂的金属掉渣少,清洗分离容易,收得率高,萃取所得的夹杂物较好地保留了在合金中的原貌,提高了实验分析的准确性。
两种镍基合金中的夹杂物主要是熔炼过程生成的脱氧产物,因在浇注前未能完全上浮而滞留在合金中,属内生夹杂物。这些由Al、Si、Ca、Mn、Mg、Ti、Fe、Ni等元素组成的硅酸盐、铝酸盐及它们的复合夹杂物,在合金中因生成的时间、凝固的条件以及成分的不同而呈球状、小块状、条状及不规则形状。其中,大尺寸的脆性宏观夹杂物对合金的性能影响最大,尤其是4J43和Cr20Ni80合金中由Ti、Al、Fe组成的复合夹杂物,这类夹杂物主要是熔炼中钛脱氧产生的钛的氧化物或氮化物,多以锐角规则形貌出现,尺寸在20-300μm,变形率低、并具有较高的硬度。由于这种脆性夹杂物与合金基体之间在变形性方面存在着较大的差异,在加工变形过程中,合金基体的均匀连续性受到破坏,引起应力集中,导致合金基体与夹杂物交界处产生微裂纹,并且随着应力的增加,裂纹扩展并最终形成宏观缺口或断丝。
采用三元酸性渣系CaF_2-Al_2O_3-CaO对中频感应熔炼后的4J43合金进行电渣重熔,实验证实,在此渣系下电渣重熔工艺稳定,电渣重熔后的4J43合金中非金属夹杂物总量减少了近40%,大于50μm的夹杂物完全消除,夹杂物的粒径主要控制在0～20μm,由于电渣重熔前合金中的脆性夹杂物(以铝酸盐为主的复合夹杂物和附合了氧化铝和氧化铁的氧化钛、氮化钛夹杂物)在重熔过程中已完全去除,重熔后合金中的新生夹杂物主要是塑性的硅酸盐类夹杂,使得合金的抗拉强度和延伸率都有较大的提高,但重熔前后4J43合金膨胀性能无明显变化,均在国标规定范围内。下游用户质量反馈证实:新工艺生产的4J43合金其表面质量和后续加工的成材率都比以前有较大提高。
实验研究了钢包吹氩工艺参数对Cr20Ni80合金中夹杂物去除效果的影响,当吹氩量大于3.5L/min时,吹氩后夹杂物不但没有减少还有所增加,特别是大尺寸夹杂物,这主要是吹氩量大时氩气泡尺寸较大,引起钢液波动造成钢液卷渣和二次氧化;吹氩量选择在3L/min时,夹杂物去除效果最好,与未吹氩相比,合金中夹杂物可减少23%,特别是大尺寸夹杂物减少了12%,实验检测证实,在这种吹氩参数下生产的Cr20Ni80合金,其快速寿命和力学性能都有较大的提高,用户反馈得到了相同的结果。
With the rapid development of aviation,aerospace,missile and electronic industrial technology,the requirements for Ni-based alloys are stricter,especially for thin wires. Not only chemical constitution and service performance are limited,but also inner and surface qualities are required.The quality of 4J43 alloy and Cr20Ni80 alloy wires produced by one alloy company is examined and compared with the same products at home and abroad.It is found that all the alloy composition is coincident with standard requirement.But there are a lot of non-metallic inclusions in these two alloys and these nonmetallic inclusions may be the main cause of crack and break in products.Few people investigated on the behavior of non-metallic inclusions in the Ni-base alloy wire so far.In the paper new electrolyte used for electrolyzing Ni-based alloys is invented. Both metallographic examination and electrolytic assay are used to study nonmetal inclusions in Ni-based wires produced by normal process.The sources of inclusions in alloys are analyzed and process optimizing experiments for 4J43 alloy and Cr20Ni80 alloy are applied.Good test results are gained recently.
New neutral electrolyte is made up by mixing oxysalt,sodium chloride and citric acid, etc.New electrolyte can not only effectively extract nonmetal inclusions in Ni-based alloys but also can have other good characters,such as,temperature and PH value is invariable during electroanalysis,anode mud precipitation of garrulous shape is little, electroanalysis process is calm;garrulous precipitation mixed in inclusions in half transparent film is so little that can be easily cleaned & separated,and high harvest rate is acquired.The inclusions extracted keep their former morphologies well in alloy,thus improving the veracity of experiment.
The main inclusions existed in two Ni-based alloys are deoxidation results in melting process.These deoxidation results,which are detained in alloys owing to incomplete floating off before pouring,are endogenesis impurity.Silicate,aluminate and their composite inclusions are composed of elements such as Al,Si,Ca,Mn,Mg,Ti,Fe,Ni and so on.These inclusions exhibit many shapes such as sphericity、tablet、strip and abnormal shape because of different inborn time、solidified condition and component.In these kinds of Ni-based alloys,big brittle macroscopic inclusions have the huge impact on the properties of alloys,especially the composite inclusions composed of Ti、Al、Fe in 4J43 alloy and Cr20Ni80 alloy.This kind of impurity is mainly titanic oxides or nitrides generated by oxidizing of titanium in smelting which exhibits abnormal acute angle with size of 20-300μm and higher rigidity,belonging to brittle impurity with low strain rate.Because a rather large difference existed between fragile inclusions and alloy matrix in deformability,uniformity and continuity of alloy matrix were destroyed during the processing and deforming,causing stress concentration,inducing tiny cracks generated in the edge between alloy matrix and inclusions.With the increase of strain force,the crack extended and macroscopic gap or fracture formed.
4J43 alloy processed by medium frequency induction melting is treated by electroslag remelting used ternary acid residue system of CaF2-Al2O3-CaO in industrial experiment.The results show that the process of electroslag remelting is stable under acid residue system and thus can effectively decrease nonmetal inclusions in 4J43 alloy. The total amounts of nonmetal inclusions decrease about 40%than those of normal process withous remeltingand whose sizes are bigger than 50μm disappear.The sizes of inclusions are in the range of 0-20μm.Inclusions are mainly brittle inclusions such as composite impurity which is mainly composed by aluminate and titanium oxide (titanium nitride)with some alumina and femic oxide before remelting.But,inclusions are mainly plastic silicate after electroslag remelting.The reason is that nonmetal inclusions in 4J43 alloy have been wiped off and new inclusions are created during remelting process.Tensile strength and elongation improve greatly,but the expansion property varies very samall and all fit the requirement of the state standard.The following process show that the rate of finished products improve
The influence of bottom blowing argon of lidale on the effect of removing of inclusions for 2080 alloy is studied by industrial experiment.The results show that only proper blowing argon flux can gain good removing effect.When the argon flux is stronger than 3.5L/min,inclusions increase after blowing argon,especially big size inclusions.It is because that strong blowing flux conduce big air bubbles,arising big fluctuation and rolling residue of molten steel and farther oxidation also.When the argon flux is 3.5L/min,the removing effect is best,inclusions decreasing 23%, especially big size inclusions decreasing 12%,compared with normal process without blowing argon.The test results show that mechanical property and accelerated test lifetime improve greatly after bottom blowing argon and clients give the same results.
引文
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