CN114836655B - 一种高铝Inconel 625合金及制备方法 - Google Patents
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- 239000000956 alloy Substances 0.000 title claims abstract description 38
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 37
- 229910001119 inconels 625 Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000003723 Smelting Methods 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- 230000006698 induction Effects 0.000 claims abstract description 11
- 239000010953 base metal Substances 0.000 claims abstract description 9
- 229910001092 metal group alloy Inorganic materials 0.000 claims abstract description 9
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 229910000838 Al alloy Inorganic materials 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
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- 238000012546 transfer Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
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- 210000001161 mammalian embryo Anatomy 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
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- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
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Abstract
一种高铝Inconel 625合金及制备方法，按质量百分比计，组分为：Cr 13~5，Fe 5，Nb 4.15，Mo 10，Al 5~9，余量为Ni。制备方法的步骤为：步骤（1）按预设比例称取反应物料，将反应物料置于行星球磨机中球磨；步骤（2）把球磨好的反应物料在压力机上压成直径为80 mm、高度约50 mm饼状坯；步骤（3）将饼状坯放入反应釜中，把引燃剂置于坯体上，充入保护气体洗气后，再充入保护气体保压，继续升温至体系发生自蔓延反应，得到母材合金；步骤（4）将母材合金进行真空感应二次熔炼，得到铸锭；步骤（5）将铸锭在1150℃进行30min固溶处理，水冷。
Description
技术领域
本发明涉及高铝Inconel 625合金的制备技术。
背景技术
熔盐光热发电(Concentrated solar power，CSP)技术不但可以有效地提供电力，而且可以在全球范围内大幅减少CO2排放，作为化石燃料最具竞争力的替代品之一，它受到越来越多的关注。氯化物熔盐以低成本、低熔点、沸点高、传热性能好等优点，已经被提议作为下一代CSP发电站中传热流体(Heat transfer fluids，HTF)和热能储存(Thermalenergy storage，TES)的候选介质材料。然而，氯化物熔盐对储热、传热系统管材有极强的腐蚀性，现有结构材料在高温下耐氯化物熔盐腐蚀性差。因此，开发在高温氯化物熔盐腐蚀环境下服役的新型合金意义重大。
镍基高温合金在高温下具有良好的强度、耐蚀性和抗氧化性能，在高温合金领域中应用广泛。其不但有良好的高温抗氧化和抗腐蚀能力，还有较高的蠕变强度和持久性能，已被看作下一代CSP的结构候选材料。相关研究指出，Al元素能很好的提高合金的抗高温熔盐腐蚀性能，主要是由于其形成的氧化铝薄膜有很好的致密性，在高温氯化物熔盐中不易脱落，而Cr元素在氯化物熔盐中优先溶解会降低抗腐蚀性。因此，本发明在Inconel 625合金标准成分的基础上提高Al含量，降低了Cr含量，制备了高铝Inconel 625合金。
发明内容
本发明的目的是提供一种高铝Inconel 625合金及制备方法。
本发明是一种高铝Inconel 625合金及制备方法，高铝Inconel 625合金，按质量百分比计，组分为：Cr 13~5，Fe 5，Nb 4.15，Mo 10，Al 5~9，余量为Ni。
上述高铝Inconel 625合金的制备方法，其步骤为：
步骤（1）按预设比例称取反应物料，将反应物料置于行星球磨机中球磨；
步骤（2）把球磨好的反应物料在压力机上压成直径为80 mm、高度约50 mm饼状坯；
步骤（3）将饼状坯放入反应釜中，把引燃剂置于坯体上，充入保护气体洗气后，再充入保护气体保压，继续升温至体系发生自蔓延反应，得到母材合金；
步骤（4）将母材合金进行真空感应二次熔炼，得到铸锭；
步骤（5）将铸锭在1150 ℃进行30 min固溶处理，水冷。
本发明的有益效果为：简化了生产设备，操作简单；与目前使用的VIM（真空感应熔炼）+VAR（真空自耗重熔）、VIM+ESR（电渣重熔）和VIM+PESR（保护气氛电渣重熔）等制备镍基合金工艺相比，工艺简单，能耗小且具备商业生产规模；本发明在Inconel 625合金标准成分的基础上通过加入过量的Al调控了Al含量，同时降低了合金的Cr含量。
附图说明
图1为实施例1、2、3的XRD图谱；图2为实施例4、5、6的XRD图谱；图3、图4、图5、图6、图7、图8分别为实施例1、2、3、4、5、6的金相组织图；图9、图10、图11、图12、图13、图14分别为实施例1、2、3、4、5、6的SEM组织形貌图。
具体实施方式
本发明是一种高铝Inconel 625合金及制备方法，高铝Inconel 625合金，按质量百分比计，组分为：Cr 13~5，Fe 5，Nb 4.15，Mo 10，Al 5~9，余量为Ni。
本发明的高铝Inconel 625合金制备方法，其步骤为：
步骤（1）按预设比例称取反应物料，将反应物料置于行星球磨机中球磨；
步骤（2）把球磨好的反应物料在压力机上压成直径为80 mm、高度约50 mm饼状坯；
步骤（3）将饼状坯放入反应釜中，把引燃剂置于坯体上，充入保护气体洗气后，再充入保护气体保压，继续升温至体系发生自蔓延反应，得到母材合金；
步骤（4）将母材合金进行真空感应二次熔炼，得到铸锭；
步骤（5）将铸锭在1150 ℃进行30min固溶处理，水冷。
以上所述的制备方法，步骤（1）所述球磨参数：时长8 h，选用氧化铝球磨珠，球料比为2:1，转速为80 r/min；压力机加压70 MPa。
以上所述的制备方法，步骤（2）所述反应物料中，采用的反应物原料为NiO、Cr、Fe、Mo、Nb2O5和Al粉末。
以上所述的制备方法，步骤（3）所述预热温度280~340 ℃，保护气氛为氩气，气压压力为4~6 Mpa。
以上所述的制备方法，步骤（4）所述预热时长60 min，真空度10-2 Pa，保持10 min合金化。
以上所述的制备方法，步骤（5）所述固溶处理以10 ℃/min的速度升温至1150 ℃保温30 min，水淬。
本发明在Inconel 625合金标准成分的基础上通过加入过量的Al调控了Al含量，同时降低了合金的Cr含量，先通过铝热法制备母材合金后用真空中频感应熔炼进行二次熔炼，消除铝热法制备的内部缺陷，得到了质量合格的块体合金材料。在提高耐高温腐蚀性能、高温抗蠕变性能的同时降低成本。制备过程简单、环境友好、成本低，适合大规模生产。
以下是本发明的具体实施例，并结合实施例对本发明的技术方案作进一步的描述，但本发明并不限于这些实施例：
实施例1：
铝热法制备初始铸坯，其制备步骤为：
表1 实施例1高铝Inconel 625合金反应物料配比(wt.%)
（1）配料：根据表1所示的反应物料配比称取好1kg反应原料，每种原料平均分成四份混合均匀；
（2）球磨：把混合均匀的反应物料放入QM-ISP4行星式球磨机球磨，转速为80 r/min，球磨时间8 h，注意的是每隔2 h改变球磨机转向防止结块，球磨珠材质为Al2O3，球料比1：2；
（3）铝热法制备：球磨结束后将反应物料放入模具中，用油压压力机施加70 MPa的压力，保压4 min后物料被压制成直径大约为80 mm厚度为50 mm左右的的圆饼状坯体。把压好的胚体放在铜坩埚中，胚体上方放2 g引燃剂薄片，将铜坩埚放入密闭的反应釜中洗气后，通入5 MPa氩气作为保护气体，通电加热后，当釜内温度升到280多度时引燃剂点燃，引发铝热反应，此时釜内压力和温度快速升高，反应开始后，关闭加热开关。等生成的产物在氩气气氛保护下随炉冷却至室温，打开反应釜，取出产物，合金上面被一层Al2O3层包裹，把包裹层敲碎后，得到块体合金。
真空中频感应熔炼二次熔炼，其制备步骤为：
（1）母材准备：将铝热法制备的高铝Inconel 625合金用线切割加工成宽度为10mm的长条并打磨掉表面的污渍，预防杂质引入；
（2）真空中频感应熔炼：在熔炼过程中先将中频感应炉扩散泵预热40~50 min后，把块体合金放入容积为3 kg的镁铝尖晶石坩埚中，并将刷了脱模剂提前预热到300度的金属梯形模具放入熔炼炉内，打开真空系统，确保真空度为10-2 Pa后打开熔炼系统，将加热功率以5 kw的梯度由0 kw开始依次调节，每次调节过后保持5 min确保加热均匀，当通过观察口观察到块体合金完全熔为液体后，再将加热功率调小至5 kw保温10 min确保成分均匀，随后翻转坩埚，将金属液倒入模具，等冷却后取出。
对其进行室温力学性能测试。硬度测试采用WILSON-VH1102型全自动显微硬度测试系统，载荷300 g，加载时间12 s，每个试样测量10个点取平均值，用维氏硬度HV0.3表示。拉伸测试在岛津AGS-X 300 kN电子万能试验机上进行，拉伸速率为0.5 mm/min，采用位移加载方式，每个成分试样进行3组平行实验。结果显示其硬度439.1 HV0.3，抗拉强度973.27MPa，延伸率4.50 %。
实施例2：
本例的反应物料如表2所示，其制备步骤同例1，室温力学性能测试结果：硬度445.0 HV0.3，抗拉强度1011.64 MPa，延伸率2.68 %。
表2 实施例2高铝Inconel 625合金反应物料配比(wt.%)
实施例3：
本例的反应物料如表3所示，其制备步骤同例1，室温力学性能测试结果：硬度468.5 HV0.3，抗拉强度984.04 MPa，延伸率2.32 %。
表3 实施例3高铝Inconel 625合金反应物料配比(wt.%)
实施例4：
将实施例1得到的高铝Inconel 625合金铸锭进行固溶处理，固溶处理步骤为：从实施例1合金铸锭上用线切割切下厚度为2.5 mm的板材，放入箱式炉中，用箱式炉以10 ℃/min的升温速度从室温加热到1150 ℃并保温30 min，做固溶处理，取出后水冷。
对其进行与实施例1相同的室温力学性能测试和800 ℃高温拉伸性能测试。800℃高温拉伸在AGS-X 300kN电子万能试验机上进行，拉伸速率为0.2 mm/min，采用位移加载方式，每个成分进行3组平行实验。其测试数据如表4所示：
表4 实施例4高铝Inconel 625合金固溶态力学性能
实施例5：
将实施例2得到的高铝Inconel 625合金进行固溶处理，其制备步骤同实施例4，其力学性能数据如表5所示。
表5 实施例5 高铝Inconel 625合金固溶态力学性能
实施例6：
将实施例3得到的高铝Inconel 625合金进行固溶处理，其制备步骤同实施例4，其力学性能数据如表6所示。
表6 实施例6 高铝Inconel 625合金固溶态力学性能
数据显示，本发明实现了高铝Inconel 625合金的制备。
以上所述，仅为本发明的具体实施例，但本发明的保护范围并不局限于此，任何熟悉本领域技术的技术人员在本发明公开的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。本发明的保护范围以权利要求书的保护范围为准。
Claims (1)
1.一种高铝Inconel 625合金的制备方法，其特征在于，按质量百分比计，组分为：Cr13～5，Fe 5，Nb 4.15，Mo 10，Al 5～9，余量为Ni；制备方法的步骤为：
步骤(1)按预设比例称取反应物料，将反应物料置于行星球磨机中球磨；
步骤(2)把球磨好的反应物料在压力机上压成直径为80mm、高度50mm饼状坯；压力机加压70MPa；
步骤(3)将饼状坯放入反应釜中，把引燃剂置于坯体上，充入保护气体洗气后，再充入保护气体保压，继续升温预热至体系发生自蔓延反应，得到母材合金；
步骤(4)将母材合金进行真空中频感应二次熔炼，得到铸锭；
步骤(5)将铸锭在1150℃进行30min固溶处理，水冷；
步骤(1)所述球磨参数：时长8h，选用氧化铝球磨珠，球料比为2:1，转速为80r/min；
步骤(1)所述反应物料中，采用的反应物原料为NiO、Cr、Fe、Mo、Nb2O5和Al粉末；
步骤(3)预热温度280～340℃，保护气体为氩气，气压压力为4～6MPa；
步骤(4)真空中频感应二次熔炼：在熔炼过程中先将中频感应炉扩散泵预热40～50min后，熔炼真空度10-2Pa，保持10min合金化；
步骤(5)所述固溶处理以10℃/min的速度升温至1150℃保温30min，水淬。
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