WO2022218444A1 - 超高n含量高温合金的vim炉冶炼方法 - Google Patents

超高n含量高温合金的vim炉冶炼方法 Download PDF

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WO2022218444A1
WO2022218444A1 PCT/CN2022/095043 CN2022095043W WO2022218444A1 WO 2022218444 A1 WO2022218444 A1 WO 2022218444A1 CN 2022095043 W CN2022095043 W CN 2022095043W WO 2022218444 A1 WO2022218444 A1 WO 2022218444A1
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content
nitrogen
smelting
vim furnace
vim
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French (fr)
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杨晓利
王立
雷应华
张志成
李林森
曹政
高首磊
张晓磊
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大冶特殊钢有限公司
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Priority to JP2023572990A priority Critical patent/JP7573126B2/ja
Priority to US18/563,262 priority patent/US20240271252A1/en
Publication of WO2022218444A1 publication Critical patent/WO2022218444A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/023—Alloys based on nickel
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C22C33/06—Making ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron

Definitions

  • the invention belongs to the field of vacuum smelting of superalloys in the metallurgical industry, and particularly relates to a VIM furnace smelting method for superalloys with ultra-high N content.
  • Ultra-high N content superalloy is a commonly used material in power plants, and is mostly used to manufacture forgings, rings and other products. Affected by the use environment and the special requirements for the purity of the alloy, the smelting of the alloy should be produced in a VIM furnace. In the process of smelting super high N content superalloy in VIM furnace, in high vacuum state, nitrogen element is easy to volatilize with the vacuum system, and the ideal target value cannot be obtained. In the high vacuum environment of VIM, it is usually impossible to effectively control the ultra-high content of N elements, so that the yield obtained by the traditional smelting process is very low.
  • one of the objects of the present invention is to provide a VIM furnace smelting method of a super high N content superalloy (also can be said to be: a kind of super high N content superalloy VIM furnace smelting process) Control method for precise control of N content).
  • the process method can ensure the target content of nitrogen and greatly improve the yield of the product.
  • a VIM furnace smelting method for a superalloy with an ultra-high N content includes a smelting step and a pouring step in a VIM furnace; in the later stage of the smelting, nitrogen-containing substances are added to the VIM furnace to adjust the N content.
  • the VIM furnace is a vacuum induction melting furnace.
  • the mass percentage of N in the superalloy with ultra-high N content is 1500-3000ppm, preferably 2000-3000ppm, more preferably 2700- 3000ppm; that is, after the casting step, the N content in the ultra-high N-content superalloy obtained is 1500-3000 ppm, preferably 2000-3000 ppm, more preferably 2700-3000 ppm.
  • the nitrogen-containing substance is a nitrogen-containing alloy with a nitrogen-containing mass percentage of 3% or more; at least one of manganese and aluminum nitride; preferably, the nitrogen-containing substance (such as ferrochromium nitride) is a nitrogen-containing substance after baking treatment; more preferably, the baking temperature is 750-1100 DEG C, the time is ⁇ 6 hours; compared with the usual non-baking of nitrogen-containing substances (such as ferrochromium nitride), the present invention innovatively performs the baking of nitrogen-containing substances (such as ferrochromium nitride) In order to remove the gas in the nitrogen-containing substances (mainly to remove H), reduce the temperature difference between the nitrogen-containing substances and the molten steel, and avoid causing a violent reaction to affect the yield of N.
  • the device for performing the roasting and the VIM furnace are located in the same workshop. Among them, if the temperature is lower than 750 °C, the effect of removing H is not good, and if the temperature exceeds 1100 °C, a part of the dissolved N in the ferrochromium nitride will be decomposed. Eventually, the yield of N will be affected; and the baking time is preferably more than 6 hours, so as to have the effect of removing H.
  • the inert gas is argon
  • the pressure of the argon in the VIM furnace is ⁇ 10000pa; the pressure of the argon is set to be as large as If the pressure is too small, the N content of the product alloy will not meet the requirements, and the N yield will decrease after the addition of nitrogen-containing substances (such as ferrochromium nitride), because the vacuum system of the vacuum induction furnace is a dynamic balance process.
  • Part of the N will be removed from the furnace with the vacuum system, so it needs to be supplemented by more nitrogen-containing substances (such as ferrochromium nitride), resulting in increased costs or unqualified final components. , it acts as a compressive stress on the molten steel surface, forcing the N brought into the molten steel by nitrogen-containing substances (such as ferrochromium nitride) into the molten steel to increase the resistance of the liquid surface, and the increased furnace pressure can also slow down the furnace.
  • the dynamic balance of the system is carried out; preferably, the introduction of the inert gas continues until the end of the pouring.
  • the smelting includes a melting stage and a refining stage, and the later stage of the smelting refers to the later stage of refining.
  • the time from adding the nitrogen-containing substance (such as ferrochromium nitride) to the start of pouring is no more than 15 minutes ; If the time between the addition of the nitrogen-containing species (such as ferrochromium nitride) to the start of pouring is too long, the yield of N in the alloy will be reduced.
  • the nitrogen-containing substance such as ferrochromium nitride
  • the amount of metallic chromium added is all the metal 80-85% of the total mass of the chromium raw material; the remaining 15-20% of the metal chromium is added according to the required amount before the inert gas is introduced in the later stage of smelting to adjust the composition.
  • the ultra-high N content superalloy of the present invention is a kind of metal material based on iron and nickel, which can work continuously at a high temperature above 600 ° C, preferably , a class of metal materials that work for a long time under stress.
  • the composition of the superalloy with ultra-high N content is as follows in terms of mass percentage: C: 0.02-0.10%; Cr: 23.00-27.00 %; Ni: 35.00-39.00%; W: ⁇ 0.50%; Mo: ⁇ 1.00%; P: ⁇ 0.04%; S: ⁇ 0.03%; Mn: ⁇ 1.50%; Si: ⁇ 1.00%; B: ⁇ 0.01% ; Nb: 0.40-0.90%; Co: ⁇ 3.00%; N: 0.15-0.30%; Al: ⁇ 0.40%; Ti: ⁇ 0.20%; Cu: ⁇ 0.50%;
  • An ultra-high N content superalloy is prepared by adopting the above-mentioned smelting method of the ultra-high N content superalloy in a VIM furnace.
  • the technical principle of obtaining the ideal target N content by VIM smelting in the present invention is that the fixed nitrogen content in ferrochromium nitride is much larger than that of other alloy raw materials, so ferrochromium nitride is used as the band of N element in the superalloy. into the medium.
  • VIM is smelted in a high vacuum state, N element will be excluded from the furnace in the form of free state with the vacuum system, and it is very difficult to effectively and accurately control the nitrogen content.
  • the present invention controls the addition timing of ferrochromium nitride (adding in the later stage of refining); controls the addition conditions (rushes into high-pressure inert gas before adding ferrochromium nitride to improve the yield of N element); controls the addition of ferrochromium nitride time to pour. In the case of ensuring the yield of N element, it is poured into an ingot. High-temperature alloy products with ideal target values are obtained.
  • the present invention has the following positive effects:
  • the method of the present invention is simple, easy and effective, and does not need to add special equipment and tooling.
  • the present invention improves the yield of N element in the smelting process of the VIM furnace by comprehensively improving the raw materials and the smelting process, and realizes the precise control of the N element content of the superalloy , so that the target content of nitrogen can be guaranteed and the ideal product can be obtained.
  • the present invention effectively solves the problem of the yield of N element in a high vacuum state, improves the yield of products such as rings, and reduces the production cost of manufacturing enterprises.
  • the present invention can ensure the yield of nitrogen elements by reasonably baking the ferrochromium nitride, and at the same time reduce the water in the ferrochromium nitride to bring H into the molten steel.
  • the present invention changes from the original high vacuum state to a high pressure state by filling the Ar gas of more than 10000Pa, so that the molten steel surface is in a dense compressive stress, which can enhance the solubility of the molten steel to N, thereby improving the yield.
  • the ferrochromium nitride of the present invention can be any brand of ferrochromium nitride with a nitrogen content of more than 3 wt%.
  • the ferrochromium nitride with the brand of FeNCr3-A is used as an example for illustration.
  • Embodiment 1 of the present invention utilizes a VIM furnace with a nominal capacity of 6 tons to smelt this ultra-high nitrogen content superalloy, comprising the following steps:
  • Step 1 Ferrochromium Nitride Baking: Ferrochromium nitride is baked in a high temperature annealing furnace in the workshop.
  • N content (the mass percentage of N in ferrochromium nitride) is 5.1%; baking (heating) temperature: 930° C.; baking time: 8.5 hours.
  • Step 2 Charging before smelting: Ni, Fe, Nb, Cr and other raw materials are successively loaded into the VIM furnace; 100% of ferrochromium nitride is reserved without adding; 20% of metal chromium is reserved without adding.
  • Step 3 smelting process: smelting the raw materials (including the melting period and the refining period, the mark of the completion of the melting period is that the monitoring full melting temperature is 1530°C, the temperature in the refining period is 1510°C, and the time is 130 minutes), and the refining period is added.
  • the required amount of metal chromium is used to adjust the composition.
  • the furnace is filled with argon gas to make the furnace pressure 10000pa argon gas, and then ferrochromium nitride is added to adjust the N content.
  • Step 4 pouring process: pour the molten steel obtained in the smelting process, wherein the time from the addition of ferrochromium nitride to the start of pouring (tapping) is 14 minutes.
  • Step 5 Inspection: inspect the casting composition content (wt%) according to the standard requirements, C: 0.061%; Cr: 25.40%; Ni: 37.03%; P: 0.006%; S: 0.002%; Mn: 0.74%; Si: 0.470 %; B: ⁇ 0.01%; Nb: 0.63%; N: 0.2857%; Al: 0.230%; Ti: 0.05%; Cu: 0.01%; H: 0.0001%.
  • the nitrogen yield ie nitrogen yield: the ratio of the nitrogen content in the obtained product to the content of nitrogen substituted in the raw materials used
  • the yield were 76.92% and 100%, respectively.
  • Embodiment 1 of the present invention utilizes a VIM furnace with a nominal capacity of 6 tons to smelt the superalloy with ultra-high nitrogen content. Include the following steps:
  • Step 1 Ferrochromium Nitride Baking: Ferrochromium nitride is baked in a high temperature annealing furnace in the workshop.
  • the parameters of the ferrochromium nitride baking are: the N content is 5.1%, the baking (heating) temperature: 930° C.; the baking time: 8.0 hours.
  • Step 2 Charging before smelting: Ni, Fe, Nb, Cr and other raw materials are successively loaded into the VIM furnace; 100% of ferrochromium nitride is reserved without adding; 20% of metal chromium is reserved without adding.
  • Step 3 smelting process: smelting the raw materials (including the melting period and the refining period, the completion of the melting period is marked as monitoring the full melting temperature of 1533 ° C, the temperature of the refining period is 1510 ° C, and the time is 120-130 minutes), wherein the melting process adds The required amount of metal chromium is used to adjust the composition.
  • argon gas with a pressure of 10,000pa is filled, and then ferrochromium nitride is added to adjust the N content.
  • Step 4 pouring process: pour the molten steel obtained in the smelting process, wherein the time from the addition of ferrochromium nitride to the start of pouring (tapping) is 15 minutes.
  • Step 5 Inspection: According to the standard requirements, inspect the casting composition content (wt%), C: 0.060%; Cr: 25.60%; Ni: 37.00%; P: 0.005%; S: 0.001%; Mn: 0.76%; Si: 0.440 %; Nb: 0.63%; N: 0.2893%; Al: 0.250%; Ti: 0.04%; Cu: 0.01%. H: 0.0001%.
  • the nitrogen yield and yield were 76.90% and 100%, respectively.
  • Step 5 Inspection: According to the standard requirements, inspect the casting composition content (wt%), C: 0.061%; Cr: 25.30%; Ni: 37.05%; P: 0.005%; S: 0.002%; Mn: 0.75%; Si: 0.500 %; B: ⁇ 0.01%; Nb: 0.65%; N: 0.2937%; Al: 0.250%; Ti: 0.05%; Cu: 0.01%; H: 0.00015%.
  • the nitrogen yield and yield were 76.70% and 100%, respectively.
  • Step 5 Inspection: Inspect the casting composition content (wt%) according to the standard requirements, C: 0.059%; Cr: 25.33%; Ni: 37.00%; P: 0.004%; S: 0.001%; Mn: 0.70%; Si: 0.480 %; B: ⁇ 0.01%; Nb: 0.62%; N: 0.2900%; Al: 0.250%; Ti: 0.04%; Cu: 0.01%; H: 0.00015%
  • the nitrogen yield and yield were 76.80% and 100%, respectively.
  • Step 5 Inspection: According to the standard requirements, inspect the casting composition content (wt%), C: 0.061%; Cr: 25.35%; Ni: 37.01%; P: 0.005%; S: 0.001%; Mn: 0.72%; Si: 0.500 %; B: ⁇ 0.01%; Nb: 0.65%; N: 0.2955%; Al: 0.250%; Ti: 0.05%; Cu: 0.01%; If it is too high, the durability and fatigue life during the user's use will be affected).
  • the nitrogen yield was 76.80%.
  • Step 5 Inspection: According to the standard requirements, inspect the casting composition content (wt%), C: 0.060%; Cr: 25.30%; Ni: 37.05%; P: 0.005%; S: 0.001%; Mn: 0.72%; Si: 0.460 %; B: ⁇ 0.01%; Nb: 0.60%; N: 0.2890%; Al: 0.250%; Ti: 0.05%; Cu: 0.01%; H: 0.00009%.
  • the nitrogen yield was 63.34%.
  • Step 5 Inspection: According to the standard requirements, inspect the casting composition content (wt%), C: 0.059%; Cr: 25.33%; Ni: 37.10%; P: 0.005%; S: 0.001%; Mn: 0.70%; Si: 0.510 %; B: ⁇ 0.01%; Nb: 0.66%; N: 0.2910%; Al: 0.260%; Ti: 0.06%; Cu: 0.01%; H: 0.0001%.
  • the nitrogen yield and yield were 74.38% and 100%, respectively.
  • the nitrogen yield and yield were 75.80% and 100%, respectively.
  • Example 1 the step (1) of Example 1, that is, the step of baking ferrochromium nitride, is omitted, and other steps are the same as those of Example 1.
  • Unbaked chromium nitride mainly causes a large amount of H element to be brought into the alloy by chromium nitride, resulting in excessive H element content and becoming waste.
  • the nitrogen yield and yield were 76.15% and 0.0%, respectively.
  • the casting composition content (wt%): C: 0.059%; Cr: 25.34%; Ni: 37.15%; P: 0.005%; S: 0.001%; Mn: 0.71%; Si: 0.520%; B: ⁇ 0.01%; Nb: 0.65%; N: 0.1010%; Al: 0.270%; Ti: 0.06%; Cu: 0.01%; H: 0.0001%

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Abstract

本发明公开了一种超高N含量高温合金的VIM炉冶炼方法及超高N含量高温合金，所述VIM炉冶炼方法包括在VIM炉中进行的熔炼步骤、和浇注步骤；在所述熔炼的后期，向所述VIM炉中加入含氮物质以调整N含量。本发明通过对原材料和熔炼工艺等的综合改善，提高了VIM炉熔炼过程N元素的收得率、实现该高温合金N元素含量的精准控制，从而可以保证氮元素的目标含量，得到理想的产品。

Description

超高N含量高温合金的VIM炉冶炼方法 技术领域
本发明属于冶金行业高温合金真空熔炼领域，具体涉及一种超高N含量高温合金的VIM炉冶炼方法。
背景技术
超高N含量高温合金是发电厂常用的一种材料，多用来制造锻件、环件等多种产品。受使用环境及对合金纯净度的特殊要求影响，该合金的冶炼要采用VIM炉生产。在VIM炉冶炼超高N含量高温合金过程中，在高真空状态下，氮元素容易随真空系统挥发，无法获得理想的目标值。在VIM的高真空环境下通常无法有效的实现超高含量N元素的控制，从而使得传统的冶炼工艺得到的良品率很低。
发明内容
针对现有技术存在的不足及缺陷，本发明的目的之一在于提供一种超高N含量高温合金的VIM炉冶炼方法(也可说是：一种超高N含量高温合金VIM炉熔炼过程中精准控制N含量的控制方法)。采用该工艺方法可以保证氮元素的目标含量、极大的提高产品的良品率。
本发明解决技术问题所采用的技术方案如下：
一种超高N含量高温合金的VIM炉冶炼方法包括在VIM炉中进行的熔炼步骤、和浇注步骤；在所述熔炼的后期，向所述VIM炉中加入含氮物质以调整N含量。其中，所述VIM炉为真空感应熔炼炉。
在上述超高N含量高温合金的VIM炉冶炼方法中，作为一种优选实施方式，所述超高N含量高温合金中N质量百分比为1500-3000ppm，优选为2000-3000ppm，更优选为2700-3000ppm；即所述浇注步骤之后，得到的超高N含量超高温合金中的N含量为1500-3000ppm，优选为2000-3000ppm，更优选为2700-3000ppm。
在上述超高N含量高温合金的VIM炉冶炼方法中，作为一种优选实施方式，所述含氮物质为含氮质量百分比为3％以上的含氮合金；进一步优选为氮化铬铁、氮化锰和氮化铝中的至少一种；优选地，所述含氮物质(比如氮化铬铁)为经过了烘烤处理之后的含氮物质；更优选地，所述烘烤的温度为750-1100℃，时间为≥6小时；相对于通常不对含氮物质(比如氮化铬铁)进行烘烤，本发明创新性地对含氮物质(比如氮化铬铁)进行所述烘烤以排除含氮物质中的气体(其中主要为去除H)、缩小含氮物质与钢液的温度差，避免引起反应剧烈影响N的收得。更优选地，进行所述烘烤的装置和VIM炉位于同一车间。其中，若温度低于750℃时，对去除H的效果不佳，若温度超过1100℃，氮化铬铁中溶解的N会有一部分分解出来。最终会影响N的收得率；且烘烤时间作为优选6小时以上，以可以起到去除H的效果。
在上述超高N含量高温合金的VIM炉冶炼方法中，作为一种优选实施方式，在所述熔炼的后期，加入所述含氮物质(比如氮化铬铁)之前，向所述VIM炉中通入惰性气体，优选地，所述惰性气体为氩气，所述VIM炉内氩气的压强≥10000pa；氩气的压强设置为在设备可承受力的范围内越大越好；若氩气的压强太小，会使得产物合金的N含量达不到要求、及导致含氮物质(比如氮化铬铁)加入后N收得率降低，因为真空感应炉的真空系统是一个动态平衡的过程，部分N会随着真空系统排除炉外，从而需要通过更多的含氮物质(比如氮化铬铁)来补充，造成成本提高或最终成分不合格判废；而充入较高压强的氩气，对钢液面是一个压应力的作用，迫使由含氮物质(比如氮化铬铁)带入钢液中的N排出液面的阻力增加，同时加大的炉内压强也可以减缓炉内系统的动态平衡的进行；优选地，所述惰性气体的通入持续到所述浇注结束。
优选地，所述熔炼包括熔化期和精炼期，所述熔炼的后期是指精炼后期。
在上述超高N含量高温合金在VIM炉中的冶炼方法中，作为一种优选实施方式，从加入所述含氮物质(比如氮化铬铁)到浇注开始之间的时间为不超过15分钟；若加入所述含氮物质(比如氮化铬铁)到浇注开始之间的时间太长会降低合金中N的收得率。
在上述超高N含量高温合金在VIM炉中的冶炼方法中，作为一种优选实施方式，在所述熔炼步骤中，在熔炼前向VIM炉中加入原料时，金属铬的 加入量为全部金属铬原料总质量的80-85％；剩余的15-20％所述金属铬根据需要量在熔炼后期通入所述惰性气体之前加入以调整成分。
在上述超高N含量高温合金的VIM炉冶炼方法，本发明所述超高N含量高温合金是以铁、镍为基，能在600℃以上的高温下持续工作的一类金属材料，优选地，在有应力作用下长期工作的一类金属材料。
在上述超高N含量高温合金的VIM炉冶炼方法，作为一种优选实施方式，按照质量百分比，所述超高N含量高温合金的成分组成如下：C：0.02-0.10％；Cr：23.00-27.00％；Ni：35.00-39.00％；W:≤0.50％；Mo：≤1.00％；P：≤0.04％；S：≤0.03％；Mn：≤1.50％；Si：≤1.00％；B：≤0.01％；Nb：0.40-0.90％；Co：≤3.00％；N：0.15-0.30％；Al：≤0.40％；Ti：≤0.20％；Cu：≤0.50％；Fe：余量。
一种超高N含量高温合金，所述超高N含量高温合金为采用上述超高N含量高温合金在VIM炉中的冶炼方法所制备得到。
本发明通过VIM熔炼在高真空状态下获得理想目标N含量的技术原理为：氮化铬铁中固定的氮含量远大于其他合金原料，所以采用氮化铬铁作为该高温合金中N元素的带入介质。但是由于VIM为高真空状态下冶炼，N元素会以自由态的形式随真空系统排除炉外，有效、精准的控制氮含量非常困难。所以本发明通过控制氮化铬铁的加入时机(在精炼后期加入)；控制加入条件(加入氮化铬铁之前冲入高压惰性气体，提升N元素的收得率)；控制加入氮化铬铁到浇注的时间。在保证N元素的收得率的情况下，浇注成锭。得到理想目标值的高温合金产品。
本发明与现有技术相比具有如下积极效果：
(1)本发明方法简单、易行、有效，无需增加专用装备和工装。
(2)本发明(高温合金，合金比例远高于钢铁)通过对原材料和熔炼工艺等的综合改善，提高了VIM炉熔炼过程N元素的收得率、实现该高温合金N元素含量的精准控制，从而可以保证氮元素的目标含量，得到理想的产品。
(3)本发明有效的解决了N元素在高真空状态下收得率的问题，提高环件等产品的良品率，降低了制造企业的生产成本。
(4)本发明通过对氮化铬铁进行合理的烘烤，可以保证氮元素的收得率，同时减少氮化铬铁中的水分带入H到钢液中。
(5)本发明通过充入10000Pa以上的Ar气，由原来的高真空状态变为高压强状态，使得钢液面处于密集的压应力，可以增强钢液对N的溶解度，进而提高收得。
(6)本发明充氩后，控制加入氮化铬铁到浇注的时间，也保证了N的收得和防止出现因氮化铬铁未全熔而出现异金属夹杂缺陷。
具体实施方式
为了突出表达本发明的目的、技术方案及优点，下面结合实施例对本发明进一步说明，示例通过本发明的解释方式表述而非限制本发明。本发明技术方案不局限于以下所列举的具体实施方式，还包括各具体实施方式之间的任意组合。
本发明的氮化铬铁可以是含氮量在3wt％以上的任何牌号的氮化铬铁，下面实施例中以牌号为FeNCr3-A的氮化铬铁为例进行说明。
实施例1
本发明实施例1利用公称容量6吨VIM炉冶炼该超高氮含量高温合金，包括以下步骤：
步骤1：氮化铬铁烘烤：在车间中的高温退火炉对氮化铬铁进行烘烤。
其中，所述氮化铬铁烘烤的参数为：N含量(N占氮化铬铁的质量百分比)为5.1％；烘烤(加热)温度：930℃；烘烤时间：8.5小时。
步骤2：熔炼前的装料：Ni、Fe、Nb、Cr等原材料陆续装入VIM炉中；氮化铬铁100％留料，不加；金属铬留料20％，不加。
步骤3：熔炼过程：对原料进行熔炼(包括熔化期和精炼期，熔化期完成的标志为监测全熔温度为1530℃，精炼期的温度为1510℃，时间为130分钟)，其中精炼后期加入所需要的金属铬量以调节成分，之后精炼后期向炉内充入氩气使炉内压强为10000pa的氩气，接着加入氮化铬铁，调整N含量。
步骤4：浇注过程：将熔炼过程得到的钢液进行浇注，其中从氮化铬铁加入至开始浇注(出钢)时间为14分钟。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.061％； Cr：25.40％；Ni：37.03％；P：0.006％；S：0.002％；Mn：0.74％；Si：0.470％；B：≤0.01％；Nb：0.63％；N：0.2857％；Al：0.230％；Ti：0.05％；Cu：0.01％；H：0.0001％。
氮收率(即氮收得率：所得产物中氮含量和所用原料中代入氮的含量之比)和良品率分别为76.92％和100％。
实施例2
本发明实施案例1利用公称容量6吨VIM炉冶炼该超高氮含量高温合金。包括以下步骤：
步骤1：氮化铬铁烘烤：在车间中的高温退火炉对氮化铬铁进行烘烤。
其中，所述氮化铬铁烘烤的参数为：N含量为5.1％，烘烤(加热)温度：930℃；所述烘烤时间：8.0小时。
步骤2：熔炼前的装料：Ni、Fe、Nb、Cr等原材料陆续装入VIM炉中；氮化铬铁100％留料，不加；金属铬留料20％，不加。
步骤3：熔炼过程：对原料进行熔炼(包括熔化期和精炼期，熔化期完成的标志为监测全熔温度为1533℃，精炼期的温度为1510℃，时间为120130分钟)，其中熔炼过程加入所需要的金属铬量以调节成分，之后精炼后期充入使压强为10000pa的氩气，接着加入氮化铬铁，调整N含量。
步骤4：浇筑过程：将熔炼过程得到的钢液进行浇注，其中，从氮化铬铁加入至开始浇注(出钢)时间为15分钟。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.060％；Cr：25.60％；Ni：37.00％；P：0.005％；S：0.001％；Mn：0.76％；Si：0.440％；Nb：0.63％；N：0.2893％；Al：0.250％；Ti：0.04％；Cu：0.01％。H：0.0001％。
氮收率和良品率分别为76.90％和100％。
实施例3
除了氮化铬铁的烘烤温度为800℃，其余皆与实施例1相同。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.061％；Cr：25.30％；Ni：37.05％；P：0.005％；S：0.002％；Mn：0.75％；Si：0.500％； B：≤0.01％；Nb：0.65％；N：0.2937％；Al：0.250％；Ti：0.05％；Cu：0.01％；H：0.00015％。
氮收率和良品率分别为76.70％和100％。
实施例4
除了氮化铬铁的烘烤温度为1050℃，其余皆与实施例1相同。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.059％；Cr：25.33％；Ni：37.00％；P：0.004％；S：0.001％；Mn：0.70％；Si：0.480％；B：≤0.01％；Nb：0.62％；N：0.2900％；Al：0.250％；Ti：0.04％；Cu：0.01％；H：0.00015％
氮收率和良品率分别为76.80％和100％。
对比例1
除了氮化铬铁的烘烤温度为650℃，其余皆与实施例1相同。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.061％；Cr：25.35％；Ni：37.01％；P：0.005％；S：0.001％；Mn：0.72％；Si：0.500％；B：≤0.01％；Nb：0.65％；N：0.2955％；Al：0.250％；Ti：0.05％；Cu：0.01％；H：0.00035％(合金使用过程中H含量越低越好，H过高后在用户使用过程中的持久和疲劳寿命会受到影响)。
氮收率为76.80％。
对比例2
除了氮化铬铁的烘烤温度为1200℃，其余皆与实施例1相同。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.060％；Cr：25.30％；Ni：37.05％；P：0.005％；S：0.001％；Mn：0.72％；Si：0.460％；B：≤0.01％；Nb：0.60％；N：0.2890％；Al：0.250％；Ti：0.05％；Cu：0.01％；H：0.00009％。
氮收率为63.34％。
对比例3
除了所通入氩气使炉内的压强为9000Pa，其余皆与实施例1相同。
步骤5：检验：按照标准要求检验铸件成分含量(wt％)，C：0.059％；Cr：25.33％；Ni：37.10％；P：0.005％；S：0.001％；Mn：0.70％；Si：0.510％；B：≤0.01％；Nb：0.66％；N：0.2910％；Al：0.260％；Ti：0.06％；Cu：0.01％；H：0.0001％。
氮收率和良品率分别为74.38％和100％。
对比例4
加入氮化铬铁到出钢之间的时间为17分钟，其余皆与实施例1相同。
按照标准要求检验铸件成分含量(wt％)，C：0.062％；Cr：25.28％；Ni：37.15％；P：0.005％；S：0.001％；Mn：0.60％；Si：0.500％；B：≤0.01％；Nb：0.67％；N：0.2913％；Al：0.250％；Ti：0.06％；Cu：0.01％；H：0.0001％。
氮收率和良品率分别为75.80％和100％。
对比例5
本对比例省略了实施例1的步骤(1)，即烘烤氮化铬铁的步骤，其他步骤与实施例1相同。
按照标准要求检验铸件成分含量(wt％)：C：0.059％；Cr：25.30％；Ni：37.20％；P：0.005％；S：0.001％；Mn：0.68％；Si：0.520％；B：≤0.01％；Nb：0.68％；N：0.2910％；Al：0.250％；Ti：0.06％；Cu：0.01％；H：0.0005％
未经烘烤的氮化铬主要造成大量的H元素由氮化铬带入合金中，造成H元素含量过高成为废品。
氮收率和良品率分别为76.15％和0.0％。
对比例6
本对比例省略了实施例1熔炼过程中向炉内通入氩气的工序，即精炼后期不通入氩气，其他步骤与实施例1相同。
按照标准要求检验铸件成分含量(wt％)：C：0.059％；Cr：25.34％；Ni：37.15％；P：0.005％；S：0.001％；Mn：0.71％；Si：0.520％；B：≤0.01％； Nb：0.65％；N：0.1010％；Al：0.270％；Ti：0.06％；Cu：0.01％；H：0.0001％
在未通入氩气的情况下，加入炉中的氮化铬铁熔化分解后，部分氮元素以游离态的N2在高真空状态下，由真空系统排除炉外。造成氮元素收得率很低，合金中氮元素不能满足标准要求最终成为废品。
氮收率和良品率分别为33.34％；良品率：0.0％。

Claims (10)

  1. 一种超高N含量高温合金的VIM炉冶炼方法，其特征在于，所述VIM炉冶炼方法包括在VIM炉中进行的熔炼步骤、和浇注步骤；在所述熔炼的后期，向所述VIM炉中加入含氮物质以调整N含量。
  2. 权利要求1所述的VIM炉冶炼方法，其特征在于，所述超高N含量高温合金中N的质量含量为1500-3000ppm，优选为2000-3000ppm，更优选为2700-3000ppm。
  3. 权利要求1所述的VIM炉冶炼方法，其特征在于，所述含氮物质为含氮质量百分比为3％以上的含氮合金；进一步优选为氮化铬铁、氮化锰和氮化铝中的至少一种；优选地，所述含氮物质为经过了烘烤处理之后的含氮物质；更优选地，所述烘烤的温度为750-1100℃，时间为≥6小时；更优选地，进行所述烘烤的装置和VIM炉位于同一车间。
  4. 权利要求1所述的VIM炉冶炼方法，其特征在于，在所述熔炼的后期，加入所述含氮物质之前，向所述VIM炉中通入惰性气体，优选地，所述惰性气体为氩气，所述VIM炉内氩气的压强≥10000pa；优选地，所述惰性气体的通入持续到所述浇注结束。
  5. 权利要求1所述的VIM炉冶炼方法，其特征在于，所述熔炼包括熔化期和精炼期，所述熔炼的后期是指精炼后期。
  6. 权利要求1所述的VIM炉冶炼方法，其特征在于，从加入所述含氮物质到浇注开始之间的时间为不超过15分钟。
  7. 权利要求1所述的VIM炉冶炼方法，其特征在于，在所述熔炼步骤中，在熔炼前向VIM炉中加入原料时，金属铬的加入量为全部金属铬原料总质量的80-85％；剩余的15-20％所述金属铬根据需要量在熔炼后期通入所述惰性 气体之前加入以调整成分。
  8. 权利要求1所述的VIM炉冶炼方法，其特征在于，所述超高N含量高温合金是以铁、镍为基，能在600℃以上的高温下持续工作的一类金属材料，优选地，在有应力作用下长期工作的一类金属材料。
  9. 权利要求1所述的VIM炉冶炼方法，其特征在于，按照质量百分比，所述超高N含量高温合金的成分组成如下：C：0.02-0.10％；Cr：23.00-27.00％；Ni：35.00-39.00％；W:≤0.50％；Mo：≤1.00％；P：≤0.04％；S：≤0.03％；Mn：≤1.50％；Si：≤1.00％；B：≤0.01％；Nb：0.40-0.90％；Co：≤3.00％；N：0.15-0.30％；Al：≤0.40％；Ti：≤0.20％；Cu：≤0.50％；Fe：余量。
  10. 一种超高N含量高温合金，其特征在于，所述超高N含量高温合金为采用权利要求1-9中任一项所述的VIM炉冶炼方法所制备得到的。
PCT/CN2022/095043 2021-05-24 2022-05-25 超高n含量高温合金的vim炉冶炼方法 WO2022218444A1 (zh)

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