CN113511907B - 一种钛铝合金熔炼用熵稳定耐火材料及其制备方法 - Google Patents
一种钛铝合金熔炼用熵稳定耐火材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种钛铝合金熔炼用熵稳定耐火材料及其制备方法。属于钛铝合金熔炼技术领域。包括以下原料:碳酸钙微粉、碳酸钡微粉、碳酸锶微粉、单斜氧化锆微粉、氧化铝微粉和结合剂。制备的钛铝合金熔炼用熵稳定耐火材料具有较高的熵值,高温化学稳定性好、抗热震性能好和抗钛铝合金熔体能力强。使用寿命大于20次;熔炼后钛铝合金的氧含量不超过0.08wt%。
Description
技术领域
本发明涉及钛铝合金熔炼技术领域,更具体的说是涉及一种钛铝合金熔炼用熵稳定耐火材料及其制备方法。
背景技术
钛铝合金密度低、比强度高、比刚度高、耐热性好、抗高温蠕变性能和抗氧化能力高,是超高音速飞行器和下一代先进航空发动机的首选材料。真空感应熔炼技术是制备钛铝合金的重要方法,耐火材料是真空感应熔炼过程中的“瓶颈”,熔炼全过程与合金熔体直接接触,其与合金的界面行为对合金最终品质有决定性影响。由于钛铝合金熔体高温下化学活性高,易与耐火材料发生反应,因此,开发性能优异的钛铝合金熔炼用耐火材料是制备高品质钛铝合金的关键前提。
真空感应熔炼用耐火材料通常要求具有优异的高温化学稳定性、抗钛铝合金侵蚀性能及热震稳定性能。常用的合金熔炼耐火材料包括ZrO2、Al2O3、CaO、Y2O3、CaZrO3和BaZrO3材料等。
现有技术中,ZrO2易与钛形成固溶体,导致合金中氧含量明显增加。Al2O3及CaO抗钛铝合金能力均与合金成分密切相关,Al2O3可以较好抵御高Al含量合金的侵蚀,但抗低Al含量合金侵蚀能力有待提升;CaO则随着钛铝合金中Al组分的增加,其与合金反应随之加剧。此外,纯CaO较难烧结,抗水化性较差。Y2O3抗热震性能差,使用寿命短。合成CaZrO3和BaZrO3耐火材料,在熔炼钛铝合金时,对合金的增氧作用有待进一步改善,且材料抗热震性能较差。
因此,如何提供一种钛铝合金熔炼用熵稳定耐火材料及其制备方法是本领域技术人员亟需解决的问题。
发明内容
有鉴于此,本发明提供了一种钛铝合金熔炼用熵稳定耐火材料及其制备方法。制备的钛铝合金熔炼用熵稳定耐火材料的高温化学稳定性好、抗热震性能好和抗钛铝合金熔体能力强。
为了实现上述目的,本发明采用如下技术方案:
一种钛铝合金熔炼用熵稳定耐火材料,按质量份包括以下原料:碳酸钙微粉8~15份、碳酸钡微粉20~30份、碳酸锶微粉15~25份、单斜氧化锆微粉40~55份、氧化铝微粉5~15份和结合剂0.5~5份。
优选的:碳酸钙微粉的碳酸钙含量≥90wt%,粒径D50为0.1~10μm。
优选的:碳酸钡微粉的碳酸钡含量≥90wt%,粒径D50为0.1~10μm。
优选的:碳酸锶微粉的碳酸锶含量≥90wt%,粒径D50为0.1~10μm。
优选的:单斜氧化锆微粉的ZrO2含量≥90wt%,粒径D50为0.3~8μm。
优选的:氧化铝微粉的Al2O3含量≥98wt%,氧化铝微粉的粒径D50为1~8μm。
有益效果在于:确保较易成型且具有较高的反应活性。
优选的:结合剂为聚乙烯醇、酚醛树脂和铝溶胶中的一种。
有益效果在于:促进原料成型。
一种钛铝合金熔炼用熵稳定耐火材料的制备方法,包括以下步骤:
(1)称取各原料混合后球磨处理,然后在100~200MPa条件下冷等静压成型,得到生坯;
(2)将生坯在110~200℃条件下干燥12~36小时,在1500~1800℃条件下保温1~8小时,制得钛铝合金熔炼用熵稳定耐火材料。
有益效果在于:确保原料充分反应并互相固溶。
优选的:步骤(1)球磨采用行星球磨机。
本发明还提供了上述的钛铝合金熔炼用熵稳定耐火材料在制备钛铝合金中的应用。
经由上述的技术方案可知,与现有技术相比,本发明公开提供了一种钛铝合金熔炼用熵稳定耐火材料及其制备方法,相较于现有技术本发明引入的碳酸钙、碳酸钡和碳酸锶微粉在热处理过程中发生分解反应,形成高活性的氧化钙、氧化钡和氧化锶粉体,能与单斜氧化锆微粉和氧化铝微粉迅速反应,生成锆酸盐和铝酸盐产物。由于钙、钡和锶原子结构相似,在热处理过程中会发生固溶,材料熵值大幅度提升,经物相分析测试,最终形成(Cax,Bay,Sr1-x-y)ZrO3-(Cax,Bay,Sr1-x-y)Al12O19熵稳定耐火材料。
熵稳定材料具有较高的熵值,高熵效应产生的相稳定性和结构稳定性使得材料具有较好的高温化学稳定性、抗热震性能和抗钛铝合金熔体能力。此外,(Cax,Bay,Sr1-x-y)ZrO3组分具有较优的抗钛组分侵蚀能力,而(Cax,Bay,Sr1-x-y)Al12O19具有较好的抗铝组分侵蚀的能力,因此,所制备的复相耐火材料具有优异的抗钛铝合金侵蚀能力;同时,(Cax,Bay,Sr1-x-y)Al12O19具有较低的热膨胀系数,也可以改善材料的抗热震性能。
本发明制备的钛铝合金熔炼用熵稳定耐火材料经检测:使用寿命大于20次;熔炼后钛铝合金的氧含量不超过0.08wt%。
因此,本发明所制备的钛铝合金熔炼用熵稳定耐火材料具有高温化学稳定性好、抗热震性能好和抗钛铝合金熔体能力强的特点。
具体实施方式
下面将结合本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明实施例公开了一种钛铝合金熔炼用熵稳定耐火材料及其制备方法。
实施例1
一种钛铝合金熔炼用熵稳定耐火材料,按质量份包括以下原料:
10份的碳酸钙微粉、24份的碳酸钡微粉、18份的碳酸锶微粉、45份的单斜氧化锆微粉、10份的氧化铝微粉和1份的结合剂。
为进一步优化技术方案:结合剂为聚乙烯醇。
所述碳酸钙微粉的碳酸钙含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸钡微粉的碳酸钡含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸锶微粉的碳酸锶含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:单斜氧化锆微粉的ZrO2含量≥90wt%,粒径D50为0.3~8μm。
为进一步优化技术方案:氧化铝微粉的Al2O3含量≥98wt%,氧化铝微粉的粒径D50为1~8μm。
制备方法:
(1)称取各原料混合后在行星球磨机中混合均匀,然后在200MPa条件下冷等静压成型,得到生坯;
(2)将生坯在110℃条件下干燥24小时,在1700℃条件下保温3小时,制得钛铝合金熔炼用熵稳定耐火材料。
本实施例制备的钛铝合金熔炼用熵稳定耐火材料经1600℃、0.06MPa氩气气氛条件下Ti48Al合金30分钟真空感应熔炼测试:使用寿命为23次;熔炼后钛铝合金的氧含量为0.07wt%。
实施例2
一种钛铝合金熔炼用熵稳定耐火材料,按质量份包括以下原料:
12份的碳酸钙微粉、30份的碳酸钡微粉、15份的碳酸锶微粉、50份的单斜氧化锆微粉、5份的氧化铝微粉和3份的结合剂。
为进一步优化技术方案:结合剂为酚醛树脂。
所述碳酸钙微粉的碳酸钙含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸钡微粉的碳酸钡含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸锶微粉的碳酸锶含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:单斜氧化锆微粉的ZrO2含量≥90wt%,粒径D50为0.3~8μm。
为进一步优化技术方案:氧化铝微粉的Al2O3含量≥98wt%,氧化铝微粉的粒径D50为1~8μm。
制备方法:
(1)称取各原料混合后在行星球磨机中混合均匀,然后在150MPa条件下冷等静压成型,得到生坯;
(2)将生坯在200℃条件下干燥36小时,在1600℃条件下保温8小时,制得钛铝合金熔炼用熵稳定耐火材料。
本实施例制备的钛铝合金熔炼用熵稳定耐火材料经1600℃、0.06MPa氩气气氛条件下Ti48Al合金30分钟真空感应熔炼测试:使用寿命为21次;熔炼后钛铝合金的氧含量为0.08wt%。
实施例3
一种钛铝合金熔炼用熵稳定耐火材料,按质量份包括以下原料:
15份的碳酸钙微粉、20份的碳酸钡微粉、15份的碳酸锶微粉、55份的单斜氧化锆微粉、15份的氧化铝微粉和5份的结合剂。
为进一步优化技术方案:结合剂为铝溶胶。
所述碳酸钙微粉的碳酸钙含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸钡微粉的碳酸钡含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸锶微粉的碳酸锶含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:单斜氧化锆微粉的ZrO2含量≥90wt%,粒径D50为0.3~8μm。
为进一步优化技术方案:氧化铝微粉的Al2O3含量≥98wt%,氧化铝微粉的粒径D50为1~8μm。
制备方法:
(1)称取各原料混合后在行星球磨机中混合均匀,然后在100MPa条件下冷等静压成型,得到生坯;
(2)将生坯在110℃条件下干燥12小时,在1500℃条件下保温8小时,制得钛铝合金熔炼用熵稳定耐火材料。
本实施例制备的钛铝合金熔炼用熵稳定耐火材料经1600℃、0.06MPa氩气气氛条件下Ti48Al合金30分钟真空感应熔炼测试:使用寿命为22次;熔炼后钛铝合金的氧含量为0.08wt%。
实施例4
一种钛铝合金熔炼用熵稳定耐火材料,按质量份包括以下原料:
8份的碳酸钙微粉、25份的碳酸钡微粉、25份的碳酸锶微粉、40份的单斜氧化锆微粉、10份的氧化铝微粉和1份的结合剂。
为进一步优化技术方案:结合剂为聚乙烯醇。
所述碳酸钙微粉的碳酸钙含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸钡微粉的碳酸钡含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:碳酸锶微粉的碳酸锶含量≥90wt%,粒径D50为0.1~10μm。
为进一步优化技术方案:单斜氧化锆微粉的ZrO2含量≥90wt%,粒径D50为0.3~8μm。
为进一步优化技术方案:氧化铝微粉的Al2O3含量≥98wt%,氧化铝微粉的粒径D50为1~8μm。
制备方法:
(1)称取各原料混合后在行星球磨机中混合均匀,然后在200MPa条件下冷等静压成型,得到生坯;
(2)将生坯在110℃条件下干燥24小时,在1800℃条件下保温1小时,制得钛铝合金熔炼用熵稳定耐火材料。
本实施例制备的钛铝合金熔炼用熵稳定耐火材料经1600℃、0.06MPa氩气气氛条件下Ti48Al合金30分钟真空感应熔炼测试:使用寿命为21次;熔炼后钛铝合金的氧含量为0.06wt%。
本说明书中各个实施例采用递进的方式描述,每个实施例重点说明的都是与其他实施例的不同之处,各个实施例之间相同相似部分互相参见即可。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (10)
1.一种钛铝合金熔炼用熵稳定耐火材料,其特征在于,按质量份由以下原料组成:碳酸钙微粉8~15份、碳酸钡微粉20~30份、碳酸锶微粉15~25份、单斜氧化锆微粉40~55份、氧化铝微粉5~15份和结合剂0.5~5份。
2.根据权利要求1所述的一种钛铝合金熔炼用熵稳定耐火材料,其特征在于所述碳酸钙微粉的碳酸钙含量≥90wt%,粒径D50为0.1~10μm。
3.根据权利要求1所述的一种钛铝合金熔炼用熵稳定耐火材料,其特征在于所述碳酸钡微粉的碳酸钡含量≥90wt%,粒径D50为0.1~10μm。
4.根据权利要求1所述的一种钛铝合金熔炼用熵稳定耐火材料,其特征在于所述碳酸锶微粉的碳酸锶含量≥90wt%,粒径D50为0.1~10μm。
5.根据权利要求1所述的一种钛铝合金熔炼用熵稳定耐火材料,其特征在于所述单斜氧化锆微粉的ZrO2含量≥90wt%,粒径D50为0.3~8μm。
6.根据权利要求1所述的一种钛铝合金熔炼用熵稳定耐火材料,其特征在于所述氧化铝微粉的Al2O3含量≥98wt%,氧化铝微粉的粒径D50为1~8μm。
7.根据权利要求1所述的钛铝合金熔炼用熵稳定耐火材料,其特征在于,所述结合剂为聚乙烯醇、酚醛树脂和铝溶胶中的一种。
8.一种权利要求1~7任一所述的钛铝合金熔炼用熵稳定耐火材料的制备方法,其特征在于,包括以下步骤:
(1)称取各原料混合后球磨处理,然后在100~200MPa条件下冷等静压成型,得到生坯;
(2)将所述生坯在110~200℃条件下干燥12~36小时,在1500~1800℃条件下保温1~8小时,制得钛铝合金熔炼用熵稳定耐火材料。
9.如权利要求8所述的一种钛铝合金熔炼用熵稳定耐火材料的制备方法,其特征在于,步骤(1)所述球磨采用行星球磨机。
10.权利要求1~7项中任一项所述的钛铝合金熔炼用熵稳定耐火材料在制备钛铝合金中的应用。
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