CN115369304A - Preparation method of stainless steel material and stainless steel material - Google Patents

Preparation method of stainless steel material and stainless steel material Download PDF

Info

Publication number
CN115369304A
CN115369304A CN202210998502.2A CN202210998502A CN115369304A CN 115369304 A CN115369304 A CN 115369304A CN 202210998502 A CN202210998502 A CN 202210998502A CN 115369304 A CN115369304 A CN 115369304A
Authority
CN
China
Prior art keywords
stainless steel
steel material
temperature
forging
blank
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202210998502.2A
Other languages
Chinese (zh)
Other versions
CN115369304B (en
Inventor
曹艳飞
陈珍珍
刘宏伟
类承帅
赵志坡
李殿中
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Metal Research of CAS
Original Assignee
Institute of Metal Research of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Metal Research of CAS filed Critical Institute of Metal Research of CAS
Priority to CN202210998502.2A priority Critical patent/CN115369304B/en
Publication of CN115369304A publication Critical patent/CN115369304A/en
Application granted granted Critical
Publication of CN115369304B publication Critical patent/CN115369304B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D11/00Process control or regulation for heat treatments
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • C21D8/065Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires of ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04Refining by applying a vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • C22B9/20Arc remelting

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Forging (AREA)
  • Heat Treatment Of Steel (AREA)

Abstract

本申请提供一种不锈钢材料的制备方法和不锈钢材料,包括如下步骤:步骤(1):采用真空冶炼+真空自耗的双联工艺制备不锈钢坯料,并通过凝固参数控制减轻成分偏析;通过凝固参数控制减轻成分偏析包括:通过控制电流电压比,以控制自耗坯料糊状区最大熔池深度,进而减轻成分偏析,使得不锈钢坯料中的碳质量分数波动为±0.015%以内;步骤(2):对不锈钢坯料进行高温扩散均匀化处理,获得初级产品;步骤(3):对步骤(2)获得的初级产品进行锻造或轧制变形处理,获得不锈钢材料。本申请提供的不锈钢材料的制备方法和不锈钢材料,能够有效降低不锈钢的偏析程度,减少夹杂物的分布,细化晶粒,并有利于孔洞和高温铁素体等缺陷的控制。

Figure 202210998502

The application provides a preparation method of stainless steel material and stainless steel material, including the following steps: Step (1): Prepare stainless steel billet by adopting vacuum smelting + vacuum self-consumption double process, and reduce component segregation through solidification parameter control; through solidification parameter Controlling and mitigating composition segregation includes: controlling the maximum molten pool depth in the mushy zone of the self-consumable billet by controlling the current-voltage ratio, thereby reducing composition segregation so that the carbon mass fraction fluctuation in the stainless steel billet is within ±0.015%; step (2): Performing high-temperature diffusion and homogenization treatment on the stainless steel billet to obtain a primary product; step (3): performing forging or rolling deformation treatment on the primary product obtained in step (2) to obtain a stainless steel material. The preparation method of the stainless steel material and the stainless steel material provided by the application can effectively reduce the segregation degree of the stainless steel, reduce the distribution of inclusions, refine the crystal grains, and facilitate the control of defects such as holes and high-temperature ferrite.

Figure 202210998502

Description

不锈钢材料的制备方法和不锈钢材料Preparation method of stainless steel material and stainless steel material

技术领域technical field

本申请不锈钢材料技术领域,具体涉及一种不锈钢材料的制备方法和不锈钢材料。This application relates to the technical field of stainless steel materials, and specifically relates to a method for preparing stainless steel materials and stainless steel materials.

背景技术Background technique

目前,CSS-42L、Cronidur高温不锈钢由于具有更好的耐高温能力及耐腐蚀性,是新一代航空轴承钢的潜能材料。At present, CSS-42L and Cronidur high-temperature stainless steel are potential materials for the new generation of aerospace bearing steel due to their better high temperature resistance and corrosion resistance.

但是,由于这些钢种合金含量较高,在凝固过程中,往往由于严重的枝晶偏析导致成分的不均匀,这不仅使得凝固过程中容易产生难以去除的夹杂物,还经常出现雀斑等偏析型缺陷。而且由于这些钢中Cr元素含量较高,在后续的高温扩散及锻造工艺中容易形成脆性高温铁素体相,使得坯料在变形过程中易于开裂。而不合理的锻造工艺不仅会导致晶粒粗大和混晶现象,降低材料的强韧性,同时还容易造成流动失稳、微裂纹等缺陷,这些缺陷在后续的热处理过程中很难消除,会极大的缩短服役寿命,降低材料的安全性。However, due to the high alloy content of these steel types, during the solidification process, the composition is often uneven due to severe dendrite segregation. defect. Moreover, due to the high content of Cr in these steels, brittle high-temperature ferrite phases are easily formed in the subsequent high-temperature diffusion and forging processes, making the blanks easy to crack during deformation. An unreasonable forging process will not only lead to coarse grains and mixed crystals, which will reduce the strength and toughness of the material, but will also easily cause defects such as flow instability and microcracks. These defects are difficult to eliminate in the subsequent heat treatment process and will be extremely Greatly shorten the service life and reduce the safety of materials.

因此,如何提供一种能够有效降低不锈钢的偏析程度,减少夹杂物的分布的不锈钢材料的制备方法和不锈钢材料成为本领域技术人员急需解决的问题。Therefore, how to provide a method for preparing a stainless steel material and a stainless steel material that can effectively reduce the segregation degree of stainless steel and reduce the distribution of inclusions has become an urgent problem to be solved by those skilled in the art.

发明内容Contents of the invention

因此,本申请要解决的技术问题在于提供一种不锈钢材料的制备方法和不锈钢材料,能够有效降低不锈钢的偏析程度,减少夹杂物的分布。Therefore, the technical problem to be solved in this application is to provide a preparation method of stainless steel material and stainless steel material, which can effectively reduce the segregation degree of stainless steel and reduce the distribution of inclusions.

为了解决上述问题,本申请提出一种不锈钢材料的制备方法,包括如下步骤:In order to solve the above problems, the application proposes a preparation method of stainless steel material, comprising the following steps:

步骤(1):采用真空冶炼+真空自耗的双联工艺制备不锈钢坯料,并通过凝固参数控制减轻成分偏析;通过凝固参数控制减轻成分偏析包括:通过控制电流电压比,以控制自耗坯料糊状区最大熔池深度,进而减轻成分偏析,使得不锈钢坯料中的碳质量分数波动为±0.015%以内;Step (1): Prepare stainless steel blanks by vacuum smelting + vacuum self-consumption duplex process, and reduce composition segregation through solidification parameter control; reduce composition segregation through solidification parameter control includes: control the self-consumption billet paste by controlling the current-voltage ratio The maximum molten pool depth in the shape zone, thereby reducing composition segregation, makes the fluctuation of the carbon mass fraction in the stainless steel billet within ±0.015%;

步骤(2):对不锈钢坯料进行高温扩散均匀化处理,获得初级产品;Step (2): performing high-temperature diffusion and homogenization treatment on the stainless steel billet to obtain primary products;

步骤(3):对步骤(2)获得的初级产品进行锻造或轧制变形处理,获得不锈钢材料。Step (3): performing forging or rolling deformation treatment on the primary product obtained in step (2) to obtain a stainless steel material.

进一步地,通过控制电流电压比,以控制自耗坯料糊状区最大熔池深度包括如下步骤:Further, controlling the maximum molten pool depth in the mushy zone of the consumable billet by controlling the current-voltage ratio includes the following steps:

控制电流电压比在260-320A/V之间,使得自耗坯料糊状区最大熔池深度小于250mm,进而减轻成分偏析。The current-voltage ratio is controlled between 260-320A/V, so that the maximum molten pool depth in the mushy zone of the consumable billet is less than 250mm, thereby reducing composition segregation.

进一步地,在步骤(1)过程中,通入冷却氦气,冷却氦气的压强在0.2-1.5kpa之间。Further, in the process of step (1), cooling helium gas is introduced, and the pressure of the cooling helium gas is between 0.2-1.5kpa.

进一步地,对不锈钢坯料进行冒口切割和/或扒皮处理;对于长度为1-1.5m的钢锭,采用的坩埚直径为0.4-0.6m。在真空自耗结束后,对不锈钢坯料的冒口切割尺寸≥0.15m;和/或,对不锈钢坯料的扒皮厚度≥15mm;Further, the stainless steel billet is subjected to riser cutting and/or peeling treatment; for steel ingots with a length of 1-1.5m, the diameter of the crucible used is 0.4-0.6m. After the vacuum self-consumption ends, the cutting size of the riser of the stainless steel billet is ≥0.15m; and/or, the peeling thickness of the stainless steel billet is ≥15mm;

和/或,在所述步骤(1)过程中,采用真空冶炼+真空自耗的双联工艺制备不锈钢坯料包括如下步骤:在真空自耗过程中采用重量1t-3t的自耗坯;优选的,在真空自耗过程中采用1-1.5t的高温不锈钢自耗坯;And/or, in the process of step (1), adopting vacuum smelting+vacuum self-consumption dual process to prepare stainless steel billet includes the following steps: adopting a self-consumable billet with a weight of 1t-3t in the vacuum self-consumption process; preferably , 1-1.5t high-temperature stainless steel consumable blanks are used in the vacuum self-consumption process;

进一步地,初级产品为无高温铁素体的均匀组织;Further, the primary product is a uniform structure without high-temperature ferrite;

进一步地,步骤(2):对所述不锈钢坯料进行高温扩散均匀化处理,获得初级产品包括如下步骤:Further, step (2): performing high-temperature diffusion homogenization treatment on the stainless steel blank, and obtaining the primary product includes the following steps:

在高温扩散前增加预变形处理,所述预变形处理的温度≥1000℃,变形量≤30%;Add pre-deformation treatment before high-temperature diffusion, the temperature of the pre-deformation treatment is ≥1000°C, and the deformation amount is ≤30%;

和/或,将不锈钢坯料在≥1120℃进行高温保温,优选的,高温保温的温度为1120-1230℃;和/或,高温保温的时间为10-25h。And/or, the stainless steel billet is subjected to high temperature insulation at ≥1120°C, preferably, the temperature of high temperature insulation is 1120-1230°C; and/or, the time of high temperature insulation is 10-25h.

进一步地,不锈钢材料的晶粒的平均尺寸≤15μm,不锈钢材料的孔洞缺陷的尺寸≤10μm;不锈钢材料中的夹杂物最大尺寸≤5μm。Further, the average size of the grains of the stainless steel material is ≤15 μm, the size of the hole defect of the stainless steel material is ≤10 μm; the maximum size of the inclusions in the stainless steel material is ≤5 μm.

进一步地,步骤(3)中:对步骤(2)获得的初级产品进行锻造或轧制变形处理包括如下步骤:Further, in step (3): performing forging or rolling deformation treatment on the primary product obtained in step (2) includes the following steps:

对初级产品进行多火次锻造变形处理,多火次锻造变形处理中镦粗拔长交替进行;The primary product is subjected to multi-fire forging deformation treatment, and upsetting, drawing and elongation are alternately carried out in the multi-fire forging deformation treatment;

进一步地,在多火次锻造变形处理中,始锻的温度不低于1100℃,优选的,始锻的温度为1100-1200℃。Further, in the multi-fire forging deformation treatment, the initial forging temperature is not lower than 1100°C, preferably, the initial forging temperature is 1100-1200°C.

进一步地,在多火次锻造变形处理过程中,坯料总锻比≥7;和/或,最后一个火次的变形量≥50%;Further, during the multi-fire forging deformation treatment, the total forging ratio of the billet is ≥7; and/or, the deformation amount of the last fire time is ≥50%;

和/或,在多火次锻造变形处理过程中,终锻的温度不低于950℃;和/或,在多火次锻造变形处理过程中,应变速率不高于0.1s-1And/or, during the multiple-fire forging deformation process, the final forging temperature is not lower than 950°C; and/or, during the multiple-fire forging deformation process, the strain rate is not higher than 0.1s -1 .

进一步地,不锈钢材料制备方法还包括如下步骤:Further, the stainless steel material preparation method also includes the following steps:

步骤(4)后:将步骤(3)中获得的不锈钢材料加热到780-950℃保温2-5小时,然后空冷至室温。After step (4): heating the stainless steel material obtained in step (3) to 780-950° C. for 2-5 hours, and then air cooling to room temperature.

根据本申请的再一方面,提供了一种不锈钢材料,不锈钢材料由上述的不锈钢材料制备方法制得;不锈钢材料的碳质量分数波动在±0.015%以内,不锈钢材料的夹杂物最大尺寸≤5μm,不锈钢材料的1/2半径处晶粒的尺寸≤15μm,不锈钢材料的孔洞缺陷的尺寸≤10μm;所述不锈钢材料无高温铁素体。According to another aspect of the present application, a stainless steel material is provided, the stainless steel material is prepared by the above stainless steel material preparation method; the carbon mass fraction of the stainless steel material fluctuates within ±0.015%, and the maximum size of the inclusions of the stainless steel material is ≤5 μm, The grain size at 1/2 radius of the stainless steel material is ≤15 μm, and the size of the hole defect in the stainless steel material is ≤10 μm; the stainless steel material has no high-temperature ferrite.

进一步地,不锈钢材料中碳含量≤0.15wt%,铬元素含量>13wt%,总合金含量>30wt%。Further, the carbon content in the stainless steel material is ≤0.15wt%, the chromium element content is >13wt%, and the total alloy content is >30wt%.

本申请提供的不锈钢材料的制备方法和不锈钢材料,通过高均质自耗坯凝固、高温扩散均匀化、多火次交叉锻造等系列技术进行协同调控,在控制成分偏析,减少夹杂物的同时,保证了所得材料的晶粒细小均匀,并避免了高温铁素体和孔洞的出现。经过上述处理后,所得不锈钢材料的碳质量分数波动在±0.015%以内,夹杂物最大尺寸≤5μm,单位面积夹杂物个数不超过5/mm2,1/2半径处晶粒平均尺寸≤15μm,孔洞缺陷最大尺寸≤10μm,且组织中没有发现高温δ-铁素体。本申请能够有效降低不锈钢的偏析程度,减少夹杂物的分布,并有利于孔洞和高温铁素体等缺陷的控制。The preparation method of the stainless steel material and the stainless steel material provided by this application are coordinated and regulated through a series of technologies such as high-homogeneity self-consumable billet solidification, high-temperature diffusion homogenization, and multi-fire cross-forging. While controlling component segregation and reducing inclusions, It ensures that the crystal grains of the obtained material are fine and uniform, and avoids the appearance of high-temperature ferrite and holes. After the above treatment, the carbon mass fraction of the obtained stainless steel fluctuates within ±0.015%, the maximum size of inclusions is ≤5μm, the number of inclusions per unit area does not exceed 5/mm 2 , and the average grain size at 1/2 radius is ≤15μm , the maximum size of the hole defect is ≤10μm, and no high-temperature δ-ferrite is found in the structure. The application can effectively reduce the segregation degree of stainless steel, reduce the distribution of inclusions, and facilitate the control of defects such as holes and high-temperature ferrite.

附图说明Description of drawings

图1为实施例1的凝固前沿元素富集及夹杂物抛杂路径;Fig. 1 is the solidification front element enrichment and inclusion throwing path of embodiment 1;

图2为实施例1的高温扩散和锻造变形;Fig. 2 is the high temperature diffusion and forging deformation of embodiment 1;

图3为实施例1的Φ60mmCSS-42L钢棒材夹杂物统计图;Fig. 3 is the Φ 60mmCSS-42L steel rod inclusions statistical chart of embodiment 1;

图4为实施例1的Φ60mmCSS-42L钢棒材晶粒尺寸图;Fig. 4 is the Φ 60mmCSS-42L steel bar grain size figure of embodiment 1;

图5为实施例1的Φ60mmCSS-42L钢棒材的组织形貌图。FIG. 5 is a microstructure and morphology diagram of the Φ60mm CSS-42L steel bar in Example 1. FIG.

具体实施方式Detailed ways

结合参见图1-5所示,一种不锈钢材料的制备方法,包括如下步骤:Referring to Figures 1-5, a method for preparing a stainless steel material comprises the following steps:

步骤(1):采用真空冶炼+真空自耗的双联工艺制备不锈钢坯料,并通过凝固参数控制减轻成分偏析;通过凝固参数控制减轻成分偏析包括:通过控制电流电压比,以控制自耗坯料糊状区最大熔池深度,进而减轻成分偏析,使得不锈钢坯料中的碳质量分数波动为±0.015%以内;Step (1): Prepare stainless steel blanks by vacuum smelting + vacuum self-consumption duplex process, and reduce composition segregation through solidification parameter control; reduce composition segregation through solidification parameter control includes: control the self-consumption billet paste by controlling the current-voltage ratio The maximum molten pool depth in the shape zone, thereby reducing composition segregation, makes the fluctuation of the carbon mass fraction in the stainless steel billet within ±0.015%;

步骤(2):对不锈钢坯料进行高温扩散均匀化处理,获得初级产品;Step (2): performing high-temperature diffusion and homogenization treatment on the stainless steel billet to obtain primary products;

步骤(3):对步骤(2)获得的初级产品进行锻造或轧制变形处理,获得不锈钢材料。Step (3): performing forging or rolling deformation treatment on the primary product obtained in step (2) to obtain a stainless steel material.

本申请通过控制电流电压比进而控制最大熔池深度,适当的熔池深度和饱满的熔池形状有利于熔池中气体的排出,也有利于液体金属的补缩,而较小的糊状区则有利于减小钢的偏析程度。即,本申请能够通过控制电流电压比控制合金偏析程度。This application controls the maximum molten pool depth by controlling the current-voltage ratio. The appropriate molten pool depth and full molten pool shape are conducive to the discharge of gas in the molten pool and the feeding of liquid metal, while the smaller mushy zone It is beneficial to reduce the degree of segregation of steel. That is, the present application can control the degree of alloy segregation by controlling the current-voltage ratio.

本申请还公开了一些实施例,通过控制电流电压比,以控制自耗坯料糊状区最大熔池深度包括如下步骤:The present application also discloses some embodiments. Controlling the maximum molten pool depth in the mushy zone of the self-consumable billet by controlling the current-voltage ratio includes the following steps:

控制电流电压比在260-320A/V之间,使得自耗坯料糊状区最大熔池深度小于250mm,进而减轻成分偏析。The current-voltage ratio is controlled between 260-320A/V, so that the maximum molten pool depth in the mushy zone of the consumable billet is less than 250mm, thereby reducing composition segregation.

本申请采用电流电压比在260-320A/V之间,使得自耗坯料糊状区最大熔池深度小于250mm,能够有效减小钢的偏析程度,并有利于疏松、气孔等缺陷的控制,且能够在兼顾低偏析的同时,促进熔池中气体的排出和液体金属的补缩。经过步骤(1)处理后,碳质量分数波动在±0.015%以内。This application adopts the current-voltage ratio between 260-320A/V, so that the maximum molten pool depth in the mushy zone of the self-consumable billet is less than 250mm, which can effectively reduce the segregation degree of steel, and is beneficial to the control of defects such as porosity and pores, and It can promote the discharge of gas in the molten pool and the feeding of liquid metal while taking into account low segregation. After the treatment in step (1), the carbon mass fraction fluctuates within ±0.015%.

本申请还公开了一些实施例,在步骤(1)过程中,通入冷却氦气,其压强在0.2-1.5kpa之间。通入冷却氦气,可以减小枝晶臂和去除相对密度较高的夹杂物。具体地,通入冷却氦气可以减小一次和二次枝晶臂,通氦气后的一次枝晶臂间距最大为980μm,二次枝晶臂间距最大为145μm;同时,通入冷却气减轻了成分偏析和缩短了夹杂物长大的时间,有利于去除相对密度较高的夹杂物。本申请中通过通入冷却氦气达到细化枝晶的目的,且本申请还能够通过通入冷却氦气控制和减轻偏析,去除相对密度较高的夹杂物。The present application also discloses some embodiments. During the step (1), cooling helium gas is introduced with a pressure between 0.2-1.5kpa. Introducing cooling helium can reduce the dendrite arms and remove relatively high density inclusions. Specifically, feeding cooling helium can reduce the primary and secondary dendrite arms. After passing helium, the maximum spacing of primary dendrite arms is 980 μm, and the maximum spacing of secondary dendrite arms is 145 μm; at the same time, cooling gas reduces the The composition segregation is shortened and the growth time of inclusions is shortened, which is beneficial to the removal of inclusions with relatively high density. In this application, the purpose of refining dendrites is achieved by feeding cooling helium, and this application can also control and reduce segregation by feeding cooling helium, and remove inclusions with relatively high density.

本申请还公开了一些实施例,对不锈钢坯料进行冒口切割和/或扒皮处理;本申请通过冒口切割和扒皮处理可以保证成分的均匀性,避免锻造过程中开裂,并提高材料的利用率。扒皮处理能够去除铸锭柱状表面的轻质夹杂物,冒口切割能够去除铸锭浮于上表面的轻质夹杂物和铸锭靠近上表面偏析最大的位置。且经过上述处理后,所得不锈钢坯料的平均夹杂物尺寸为3μm,最大夹杂物尺寸不超过5μm,单位面积夹杂物个数不超过5/mm2The application also discloses some embodiments, which are to perform riser cutting and/or peeling treatment on the stainless steel billet; the application can ensure the uniformity of the composition through the riser cutting and skinning treatment, avoid cracking in the forging process, and improve the utilization rate of the material . Peeling treatment can remove the light inclusions on the columnar surface of the ingot, and riser cutting can remove the light inclusions floating on the upper surface of the ingot and the position where the segregation of the ingot is the largest near the upper surface. And after the above treatment, the average inclusion size of the obtained stainless steel billet is 3 μm, the largest inclusion size does not exceed 5 μm, and the number of inclusions per unit area does not exceed 5/mm 2 ;

本申请还公开了一些实施例,在步骤(1)过程中,对于长度为1-1.5m的钢锭,采用的坩埚直径为0.4-0.6m。在真空自耗结束后,对不锈钢坯料的冒口切割尺寸≥0.15m,和/或,扒皮厚度≥15mm,能够在保证材料均匀性的同时提高利用率。The present application also discloses some embodiments. During the step (1), for a steel ingot with a length of 1-1.5 m, the diameter of the crucible used is 0.4-0.6 m. After the vacuum self-consumption ends, the cutting size of the riser of the stainless steel billet is ≥0.15m, and/or the thickness of the skin is ≥15mm, which can improve the utilization rate while ensuring the uniformity of the material.

和/或,在步骤(1)过程中:采用真空冶炼+真空自耗的双联工艺制备不锈钢坯料包括如下步骤:在真空自耗过程中采用重量1t-3t的自耗坯;优选的,在真空自耗过程中采用1-1.5t的高温不锈钢自耗坯。自耗过程包括起弧、稳弧和熄弧三个阶段,通过对凝固参数的控制,包括对电流电压比,冷却强度及冒口切割和扒皮的控制,能够有效降低钢的偏析程度,减少夹杂物的分布,并有利于疏松、气孔等缺陷的控制。And/or, in the process of step (1): adopting vacuum smelting+vacuum self-consumption duplex process to prepare stainless steel billet comprises the following steps: adopting a weight 1t-3t self-consumable billet in the vacuum self-consumption process; preferably, in 1-1.5t high-temperature stainless steel consumable blanks are used in the vacuum self-consumption process. The self-consumption process includes three stages of arc starting, arc stabilization and arc extinguishing. Through the control of solidification parameters, including the control of current-voltage ratio, cooling intensity, riser cutting and peeling, it can effectively reduce the degree of segregation of steel and reduce inclusions. The distribution of matter, and is conducive to the control of defects such as porosity and pores.

综上所述,本申请中采用三个方面控制夹杂物和成分偏析,在凝固过程中通过控制电流电压比和加强冷却强度控制合金偏析程度;然后凝固结束后,再通过冒口切割直接切除偏析最大的位置并去除浮于表面的轻质夹杂物;最后扒皮,去除侧表面的轻质夹杂物。In summary, this application uses three aspects to control inclusions and composition segregation. During the solidification process, the degree of alloy segregation is controlled by controlling the current-voltage ratio and strengthening the cooling intensity; and then after the solidification is completed, the segregation is directly removed by cutting the riser The largest position and remove the light inclusions floating on the surface; finally peel off the skin and remove the light inclusions on the side surface.

本申请还公开了一些实施例,初级产品为无高温铁素体的均匀组织;上述步骤(1)中得到的初级产品为高温不锈钢低偏析双真空坯料,进一步结合预变形处理,增加元素的扩散通道,降低因为局部Cr元素富集而出现高温铁素体的概率。同时,通过精确控制高温扩散均匀化处理的温度和时间,避免热力学平衡状态下高温δ-铁素体的出现,降低在锻造中的开裂几率。The application also discloses some embodiments. The primary product is a uniform structure without high-temperature ferrite; the primary product obtained in the above step (1) is a high-temperature stainless steel low-segregation double-vacuum billet, which is further combined with pre-deformation treatment to increase the diffusion of elements channel, reducing the probability of high-temperature ferrite due to local Cr enrichment. At the same time, by precisely controlling the temperature and time of high-temperature diffusion homogenization treatment, the appearance of high-temperature δ-ferrite in a state of thermodynamic equilibrium is avoided, and the probability of cracking in forging is reduced.

本申请还公开了一些实施例,步骤(2):对不锈钢坯料进行高温扩散均匀化处理,获得初级产品还包括如下步骤:The application also discloses some embodiments, step (2): performing high-temperature diffusion homogenization treatment on the stainless steel billet, and obtaining the primary product also includes the following steps:

在高温扩散前增加预变形处理,预变形处理的温度≥1000℃,变形量≤30%;Add pre-deformation treatment before high-temperature diffusion, the temperature of pre-deformation treatment is ≥1000°C, and the deformation amount is ≤30%;

和/或,将不锈钢坯料在≥1120℃进行高温保温,以达到使枝晶间成分分布更加均匀的目的。And/or, the stainless steel billet is kept at high temperature at ≥ 1120° C., so as to achieve the purpose of making the distribution of interdendritic components more uniform.

优选的,高温保温的温度为1120-1230℃;避免温度过高而出现高温铁素体。Preferably, the temperature for high-temperature heat preservation is 1120-1230° C.; avoiding the occurrence of high-temperature ferrite due to excessive temperature.

和/或,高温保温的时间为10-25h。步骤(2)处理后所得坯料即初级产品无高温δ铁素体。And/or, the time for high temperature insulation is 10-25h. The billet obtained after the treatment in step (2) is the primary product without high temperature delta ferrite.

本申请还公开了一些实施例,不锈钢材料的晶粒的平均尺寸≤15μm,不锈钢材料无孔洞、裂纹等失稳缺陷;不锈钢材料中的夹杂物最大尺寸≤5μm。The application also discloses some embodiments, the average grain size of the stainless steel material is ≤15 μm, and the stainless steel material has no instability defects such as holes and cracks; the maximum size of inclusions in the stainless steel material is ≤5 μm.

本申请还公开了一些实施例,步骤(3)中:对步骤(2)获得的初级产品进行锻造或轧制变形处理包括如下步骤:The application also discloses some embodiments. In step (3): performing forging or rolling deformation treatment on the primary product obtained in step (2) includes the following steps:

对初级产品进行多火次交叉锻造变形处理;多火次锻造变形处理中镦粗拔长交替进行;多火次交叉锻造变形处理中,利用基于变形温度、应变速率和变形量的协同控制的热变形方式,得到晶粒细小均匀、无微裂纹等失稳缺陷的高温不锈钢材料,经过步骤(3)处理后的材料的晶粒平均尺寸≤15μm,无孔洞、微裂纹等失稳缺陷。The primary product is subjected to multi-fire cross-forging deformation treatment; in the multi-fire time forging deformation treatment, upsetting and elongation are alternately carried out; The deformation method is to obtain a high-temperature stainless steel material with fine and uniform grains and no instability defects such as microcracks. After the treatment in step (3), the average grain size of the material is ≤15 μm, and there is no instability defects such as holes and microcracks.

本申请还公开了一些实施例,在多火次交叉锻造变形处理中,始锻的温度不低于1100℃,优选的,始锻的温度为1100-1200℃。锻造温度不能过低,锻造温度太低容易形成微裂纹、流动失稳,动态再结晶也不能完全发生,易于形成混晶组织,对后续性能不利,但同时锻造温度也不能过高,锻造温度太高容易局部过热形成高温铁素体,高温铁素体易裂,对后续使用不利,同时锻造温度过高还会使得动态再结晶完成后的晶粒进一步长大,使得其强度和韧性降低。上述温度范围为最佳的锻造温度。The present application also discloses some embodiments. In the multi-fire cross forging deformation treatment, the initial forging temperature is not lower than 1100° C., preferably, the initial forging temperature is 1100-1200° C. The forging temperature should not be too low. If the forging temperature is too low, microcracks and flow instability will easily form, and dynamic recrystallization will not completely occur. It is easy to form a mixed crystal structure, which is not good for subsequent performance. High-temperature ferrite is easily formed by local overheating, and high-temperature ferrite is easy to crack, which is not good for subsequent use. At the same time, if the forging temperature is too high, the grains after dynamic recrystallization will grow further, reducing its strength and toughness. The above temperature range is the best forging temperature.

本申请还公开了一些实施例,在多火次交叉锻造变形处理过程中,坯料总锻比≥7,使得整个坯料各处变形均匀;和/或,最后一个火次的变形量≥50%;动态再结晶需要达到该临界变形量才能完全发生,不然易于形成混晶组织,对后续性能不利。和/或,在多火次交叉锻造变形处理过程中,终锻的温度不低于950℃;和/或,在多火次交叉锻造变形处理过程中,应变速率不高于0.1s-1The present application also discloses some embodiments. During the multi-fire cross forging deformation process, the total forging ratio of the billet is ≥7, so that the deformation of the entire billet is uniform; and/or, the deformation amount of the last fire time is ≥50%; Dynamic recrystallization needs to reach this critical deformation amount to fully occur, otherwise it is easy to form a mixed crystal structure, which is detrimental to subsequent performance. And/or, during the multi-fire cross forging deformation process, the final forging temperature is not lower than 950°C; and/or, during the multi-fire cross forging deformation process, the strain rate is not higher than 0.1s -1 .

本申请采用上述的终锻温度和应变速率能够防止终锻温度过低和应变速率过高导致的流动失稳和微裂纹。通过对多火次锻造过程中变形温度、应变速率和变形量三者的协同控制,能够在细化晶粒的同时,愈合孔洞型微缺陷,本申请所述孔洞型微缺陷消除,指的是制备所得的材料中,孔洞型微缺陷最大尺寸≤10μm。The application of the above-mentioned final forging temperature and strain rate can prevent flow instability and microcracks caused by too low final forging temperature and too high strain rate. Through the coordinated control of the deformation temperature, strain rate and deformation amount during the multi-fire forging process, the micro-defects of the micro-holes can be healed while the grains are refined. The elimination of the micro-defects of the holes in this application refers to In the prepared material, the maximum size of hole-type micro-defects is ≤10 μm.

经过上述步骤(3)处理后,所得锻材1/2半径处晶粒平均尺寸≤15μm,孔洞缺陷最大尺寸≤10μm。高温不锈钢的晶粒细小均匀且无微裂纹等失稳缺陷。After the above step (3), the average grain size at 1/2 radius of the obtained forged material is ≤15 μm, and the maximum size of hole defects is ≤10 μm. The high-temperature stainless steel has fine and uniform grains and no instability defects such as microcracks.

本申请还公开了一些实施例,不锈钢材料制备方法还包括如下步骤:The application also discloses some embodiments, the stainless steel material preparation method also includes the following steps:

步骤(4)后:将步骤(3)中获得的不锈钢材料加热到780-950℃保温2-5小时,然后冷却至室温。可以防止不锈钢沿晶界析出Cr23C6,增加晶间腐蚀倾向。冷却方式可以采用空冷。After step (4): heating the stainless steel material obtained in step (3) to 780-950° C. for 2-5 hours, and then cooling to room temperature. It can prevent the precipitation of Cr 23 C 6 along the grain boundary of stainless steel and increase the tendency of intergranular corrosion. The cooling method can be air cooling.

本申请提供了一些实施例,公开了一种不锈钢材料,不锈钢材料由上述的不锈钢材料制备方法制得;不锈钢材料的碳质量分数波动在±0.015%以内;不锈钢材料的夹杂物最大尺寸≤5μm,单位面积夹杂物个数不超过5个/mm2;不锈钢材料的1/2半径处晶粒的尺寸≤15μm;不锈钢材料的孔洞缺陷的尺寸≤10μm;且无高温铁素体及微裂纹等失稳缺陷。The present application provides some examples, disclosing a stainless steel material, which is prepared by the above-mentioned stainless steel material preparation method; the carbon mass fraction of the stainless steel material fluctuates within ±0.015%; the maximum size of the inclusions of the stainless steel material is ≤5 μm, The number of inclusions per unit area does not exceed 5/mm 2 ; the grain size at 1/2 radius of the stainless steel material is ≤15 μm; the size of the hole defect in the stainless steel material is ≤10 μm; and there is no high-temperature ferrite and microcracks, etc. stable defects.

1.本申请不锈钢材料为高温不锈钢,其碳含量≤0.15wt%,铬元素含量>13wt%,总合金含量>30wt%。这类钢由于存在超高的合金元素,导致钢液的粘度大,糊状区大,局部凝固时间长,枝晶发达,微观偏析严重,不仅使得凝固过程中容易产生难以去除的夹杂物,还经常出现雀斑等偏析型缺陷。高铬元素同时造成高温扩散过程中易于形成高温δ-铁素体,不利于后续均匀变形。为了解决这一共性问题,本申请通过高均质自耗坯凝固、高温扩散均匀化、多火次锻造变形等系列技术进行协同调控,以达到高温不锈钢材料的碳质量分数波动在±0.015%以内,夹杂物最大尺寸≤5μm,单位面积夹杂物个数不超过5/mm2,1/2半径处晶粒平均尺寸≤15μm,孔洞缺陷最大尺寸≤10μm,且组织中没有发现高温δ-铁素体,促进了高温不锈钢的洁净化和均质化。1. The stainless steel material of this application is a high-temperature stainless steel with a carbon content of ≤0.15wt%, a chromium content of >13wt%, and a total alloy content of >30wt%. Due to the existence of ultra-high alloying elements in this type of steel, the viscosity of molten steel is large, the mushy area is large, the local solidification time is long, the dendrites are developed, and the microscopic segregation is serious, which not only makes it easy to produce inclusions that are difficult to remove during the solidification process, but also Segregation-type defects such as freckles often appear. At the same time, the high chromium element makes it easy to form high-temperature δ-ferrite during the high-temperature diffusion process, which is not conducive to subsequent uniform deformation. In order to solve this common problem, this application uses a series of technologies such as solidification of high-homogeneous self-consumable billet, high-temperature diffusion homogenization, and multi-fire forging deformation to achieve the fluctuation of the carbon mass fraction of high-temperature stainless steel within ±0.015%. , the maximum size of inclusions ≤ 5 μm, the number of inclusions per unit area does not exceed 5/mm 2 , the average grain size at 1/2 radius ≤ 15 μm, the maximum size of hole defects ≤ 10 μm, and no high temperature δ-ferrite is found in the structure body, which promotes the cleanliness and homogenization of high-temperature stainless steel.

本申请通过控制电流电压比、加强冷却强度及合理的冒口切割和扒皮来控制减轻成分偏析,细化枝晶,减少夹杂物,一方面保证了铸坯质量,另一方面提高了材料利用率,降低了用料成本。This application controls the reduction of component segregation, refines dendrites, and reduces inclusions by controlling the current-voltage ratio, strengthening cooling intensity, and reasonable riser cutting and peeling. On the one hand, the quality of the billet is guaranteed, and on the other hand, the material utilization rate is improved. , reducing the cost of materials.

本申请通过控制铸坯高温扩散均匀化的参数,消除了脆性高温δ-铁素体相,降低了后续变形中的开裂几率。The present application eliminates the brittle high-temperature delta-ferrite phase by controlling the parameters of high-temperature diffusion and homogenization of the slab, and reduces the probability of cracking in subsequent deformation.

本申请通过基于变形温度、应变速率及变形量的协同控制的热变形方式,不仅保证了所得材料的晶粒细小均匀,同时还避免了流动失稳、微裂纹等缺陷。In this application, through the thermal deformation method based on the coordinated control of deformation temperature, strain rate and deformation amount, it not only ensures that the crystal grains of the obtained material are fine and uniform, but also avoids defects such as flow instability and microcracks.

2.本申请通过自耗铸坯低偏析化、高温扩散均匀化、多火次锻造变形处理,可有效减少微裂纹等失稳缺陷的产生,提高服役寿命和安全稳定性。其中,合理的高温均匀化参数可以改善凝固过程中导致的成分偏析,提高成分的均匀性。再经过多火次的锻造处理,会进一步愈合其在凝固过程中遗留的微缺陷,同时保证晶粒细小均匀。2. This application can effectively reduce the occurrence of instability defects such as microcracks and improve service life and safety and stability through low segregation of consumable billet, high temperature diffusion uniformity, and multi-fire forging deformation treatment. Among them, reasonable high-temperature homogenization parameters can improve the composition segregation caused by the solidification process and improve the uniformity of the composition. After multiple times of forging, the micro-defects left in the solidification process will be further healed, while ensuring that the grains are fine and uniform.

3.本申请适用于轴承钢、齿轮钢、模具钢等管材以及棒材的高品质制备。本申请提升高温不锈钢纯净度和均质化的方法,最终使轴承钢、齿轮钢、模具钢等棒材或管材能够满足高速、高温、腐蚀、大载荷苛刻工况条件以及高疲劳寿命服役性能要求。本申请为CSS-42L、Cronidur等高温不锈钢提供了一种提升内在质量的有效方法。3. This application is suitable for high-quality preparation of bearing steel, gear steel, mold steel and other pipes and bars. This application improves the purity and homogenization of high-temperature stainless steel, and finally enables the rods or pipes such as bearing steel, gear steel, and mold steel to meet the high-speed, high-temperature, corrosion, heavy-load harsh working conditions and high fatigue life service performance requirements . This application provides an effective method for improving the inner quality of CSS-42L, Cronidur and other high-temperature stainless steels.

经验证,本申请的方法得到的高温不锈钢基体致密,晶粒细小均匀,可用于航空、航天、工具、模具、齿轮等领域零部件的制造,具有服役寿命长、耐高温、可靠性高等优点。It has been verified that the high-temperature stainless steel obtained by the method of the present application has a dense matrix and fine and uniform grains, which can be used in the manufacture of parts in the fields of aviation, aerospace, tools, molds, gears, etc., and has the advantages of long service life, high temperature resistance, and high reliability.

实施例Example

实施例1Example 1

本实施例制备一种高温不锈钢棒材,具体制备步骤如下:This embodiment prepares a high-temperature stainless steel rod, and the specific preparation steps are as follows:

1)制备高温不锈钢低偏析双真空自耗坯料:采用双真空制备铸态坯料,钢锭材质为CSS-42L钢,自耗锭为1.5t,钢锭长度为1.5m,坩埚直径为0.4m,控制稳弧阶段电流电压比在320A/V并通入冷却氦气,其压强为0.2kpa,冒口切割0.25m,扒皮15mm,所得铸坯的平均夹杂物尺寸为3μm,最大夹杂物尺寸为5μm,碳质量分数波动在±0.008%以内。1) Preparation of high-temperature stainless steel low segregation double-vacuum self-consumption billets: double-vacuum preparation of cast billets, steel ingot material is CSS-42L steel, self-consumption ingot is 1.5t, steel ingot length is 1.5m, crucible diameter is 0.4m, and the control is stable. The current-voltage ratio in the arc phase is 320A/V and the cooling helium gas is introduced, the pressure is 0.2kpa, the riser is cut 0.25m, and the skin is peeled 15mm. The average inclusion size of the obtained slab is 3μm, and the maximum inclusion size is 5μm. Carbon The mass fraction fluctuates within ±0.008%.

2)坯料高温扩散均匀化处理:铸坯进行预变形,变形温度为1000℃,变形量为10%,随后在1120℃高温进行保温,保温时间为25h,使枝晶间成分分布更加均匀。2) Billet high-temperature diffusion and homogenization treatment: pre-deform the cast billet at a deformation temperature of 1000°C and a deformation amount of 10%, and then conduct heat preservation at a high temperature of 1120°C for 25 hours to make the interdendritic composition distribution more uniform.

3)多火次交叉锻造变形开坯处理:在锻造过程中,采用二镦二拔工艺实现交叉变形,始锻温度为1100℃,整个坯料锻比为7,其中最后一个火次锻比为2,终锻温度950℃,锻造应变速率为0.1s-1,将不锈钢材料加热到950℃保温2小时,然后空冷至室温。棒材1/2半径处晶粒平均尺寸为8μm,孔洞缺陷尺寸<10μm,无高温铁素体及微裂纹。3) Multi-firing cross-forging deformation billet opening treatment: In the forging process, the cross-deformation is realized by the two-upsetting and two-drawing process, the initial forging temperature is 1100°C, the forging ratio of the whole billet is 7, and the forging ratio of the last fire is 2 , the final forging temperature is 950°C, the forging strain rate is 0.1s -1 , the stainless steel material is heated to 950°C for 2 hours, and then air-cooled to room temperature. The average grain size at the 1/2 radius of the bar is 8 μm, the size of the hole defect is less than 10 μm, and there is no high-temperature ferrite and microcracks.

实施例2Example 2

本实施例制备一种高温不锈钢棒材,具体制备步骤如下:This embodiment prepares a high-temperature stainless steel rod, and the specific preparation steps are as follows:

1)制备高温不锈钢低偏析双真空自耗坯料:采用双真空制备铸态坯料,钢锭材质为CSS-42L钢,自耗锭为1.6t,钢锭长度为1m,坩埚直径为0.5m,控制稳弧阶段电流电压比在280A/V左右并通入冷却氦气,其压强为1.5kpa,冒口切割0.18m,扒皮18mm,所得铸坯的平均夹杂物尺寸为2μm,最大夹杂物尺寸为5μm,碳质量分数波动在±0.009%以内。1) Preparation of high-temperature stainless steel low-segregation double-vacuum consumable billet: double-vacuum is used to prepare the cast billet. The material of the ingot is CSS-42L steel, the consumable ingot is 1.6t, the length of the ingot is 1m, and the diameter of the crucible is 0.5m. The phase current-voltage ratio is about 280A/V and cooling helium is introduced, the pressure is 1.5kpa, the riser is cut 0.18m, and the skin is peeled 18mm. The average inclusion size of the obtained slab is 2μm, and the maximum inclusion size is 5μm. The mass fraction fluctuates within ±0.009%.

2)坯料高温扩散均匀化处理:铸坯进行预变形,变形温度为1000℃,变形量为10%,随后在1170℃高温进行保温,保温时间为16h,使枝晶间成分分布更加均匀。2) Billet high-temperature diffusion and homogenization treatment: pre-deform the cast billet at a deformation temperature of 1000°C and a deformation amount of 10%, and then heat-preserve at a high temperature of 1170°C for 16 hours to make the distribution of interdendritic components more uniform.

3)多火次交叉锻造变形开坯处理:在锻造过程中,采用二镦二拔工艺实现交叉变形,始锻温度为1150℃,整个坯料锻比为8,其中最后一个火次锻比为3,终锻温度950℃,锻造应变速率为0.1s-1,将不锈钢材料加热到780℃保温5小时,然后空冷至室温。棒材1/2半径处晶粒平均尺寸为12μm,孔洞缺陷尺寸小于10μm,无高温铁素体及微裂纹。3) Multi-firing cross-forging deformation billet opening treatment: In the forging process, two upsetting and two drawing processes are used to realize cross deformation, the initial forging temperature is 1150°C, the forging ratio of the whole billet is 8, and the forging ratio of the last fire is 3 , the final forging temperature is 950°C, the forging strain rate is 0.1s -1 , the stainless steel material is heated to 780°C for 5 hours, and then air-cooled to room temperature. The average grain size at the 1/2 radius of the bar is 12 μm, the size of the hole defect is less than 10 μm, and there is no high-temperature ferrite and microcracks.

实施例3Example 3

本实施例制备一种高温不锈钢棒材,具体制备步骤如下:This embodiment prepares a high-temperature stainless steel rod, and the specific preparation steps are as follows:

1)制备高温不锈钢低偏析双真空自耗坯料:采用双真空制备铸态坯料,钢锭材质为CSS-42L钢,自耗锭为1t,钢锭长度为1m,坩埚直径为0.4m,控制稳弧阶段电流电压比在260A/V左右并通入冷却氦气,其压强为1.33kpa。冒口切割0.15m,扒皮15mm,所得铸坯的平均夹杂物尺寸为2μm,最大夹杂物尺寸为4μm,碳质量分数波动在±0.012%以内。1) Preparation of high temperature stainless steel low segregation double vacuum self-consumption billet: adopt double vacuum to prepare cast billet, steel ingot material is CSS-42L steel, self-consumption ingot is 1t, steel ingot length is 1m, crucible diameter is 0.4m, controlled arc stabilization stage The current-voltage ratio is about 260A/V and the cooling helium gas is passed through, and its pressure is 1.33kpa. The riser was cut 0.15m, and the skin was peeled 15mm. The average inclusion size of the obtained slab was 2 μm, the maximum inclusion size was 4 μm, and the carbon mass fraction fluctuated within ±0.012%.

2)坯料高温扩散均匀化处理:铸坯进行预变形,变形温度为1000℃,变形量为8%,随后在1230℃高温进行保温,保温时间为10h,使枝晶间成分分布更加均匀。2) Billet high-temperature diffusion homogenization treatment: pre-deform the casting billet at a deformation temperature of 1000°C and a deformation amount of 8%, and then heat-preserve at a high temperature of 1230°C for 10 hours to make the distribution of interdendritic components more uniform.

3)多火次交叉锻造变形开坯处理:在锻造过程中,采用二镦二拔工艺实现交叉变形,始锻温度为1200℃,整个坯料锻比为9,其中最后一个火次锻比为4,终锻温度950℃,锻造应变速率为0.1s-1,将不锈钢材料加热到900℃保温3小时,然后空冷至室温。棒材1/2半径处晶粒平均尺寸为14μm,孔洞缺陷尺寸小于10μm,无高温铁素体及微裂纹。3) Multi-firing cross-forging deformation billet opening treatment: In the forging process, two upsetting and two drawing processes are used to realize cross deformation, the initial forging temperature is 1200°C, the forging ratio of the whole billet is 9, and the forging ratio of the last fire is 4 , the final forging temperature is 950°C, the forging strain rate is 0.1s -1 , the stainless steel material is heated to 900°C for 3 hours, and then air-cooled to room temperature. The average grain size at the 1/2 radius of the bar is 14 μm, the size of the hole defect is less than 10 μm, and there is no high-temperature ferrite and microcracks.

实施例4Example 4

本实施例制备一种高温不锈钢棒材,具体制备步骤如下:This embodiment prepares a high-temperature stainless steel rod, and the specific preparation steps are as follows:

1)制备高温不锈钢低偏析双真空自耗坯料:采用双真空制备铸态坯料,钢锭材质为CSS-42L钢,自耗锭为3t,钢锭长度为1.3m,坩埚直径为0.6m,控制稳弧阶段电流电压比在320A/V并通入冷却氦气,其压强为1.33kpa,冒口切割0.25m,扒皮21mm,所得铸坯的平均夹杂物尺寸为3μm,最大夹杂物尺寸为5μm,碳质量分数波动在±0.008%以内。1) Preparation of high-temperature stainless steel low segregation double-vacuum consumable billet: double-vacuum is used to prepare cast billet, the steel ingot is made of CSS-42L steel, the consumable ingot is 3t, the length of the steel ingot is 1.3m, the diameter of the crucible is 0.6m, and the arc is controlled and stabilized The current-voltage ratio of the stage is 320A/V and cooling helium is introduced, the pressure is 1.33kpa, the riser is cut 0.25m, and the skin is peeled 21mm. The average inclusion size of the obtained slab is 3μm, the maximum inclusion size is 5μm, and the carbon mass Score fluctuations are within ±0.008%.

2)坯料高温扩散均匀化处理:铸坯进行预变形,变形温度为1050℃,变形量为30%,随后在1150℃高温进行保温,保温时间为25h,使枝晶间成分分布更加均匀。2) Billet high-temperature diffusion homogenization treatment: pre-deform the cast billet at a deformation temperature of 1050°C and a deformation amount of 30%, and then heat-preserve at a high temperature of 1150°C for 25 hours to make the distribution of components between dendrites more uniform.

3)多火次交叉锻造变形开坯处理:在锻造过程中,采用二镦二拔工艺实现交叉变形,始锻温度为1100℃,整个坯料锻比为9,其中最后一个火次锻比为4,终锻温度980℃,锻造应变速率为0.05s-1,将不锈钢材料加热到800℃保温5小时,然后空冷至室温。棒材1/2半径处晶粒平均尺寸为8μm,孔洞缺陷尺寸<10μm,无高温铁素体及微裂纹。3) Multi-firing cross-forging deformation billet opening treatment: In the forging process, two upsetting and two drawing processes are used to realize cross deformation, the initial forging temperature is 1100°C, the forging ratio of the whole billet is 9, and the forging ratio of the last fire is 4 , the final forging temperature is 980°C, the forging strain rate is 0.05s -1 , the stainless steel material is heated to 800°C for 5 hours, and then air-cooled to room temperature. The average grain size at the 1/2 radius of the bar is 8 μm, the size of the hole defect is less than 10 μm, and there is no high-temperature ferrite and microcracks.

对比例1Comparative example 1

与实施例1制备方法基本相同,不同之处在于,稳弧阶段电流电压比在220A/V,最终轴承钢棒材经检测,测得碳含量波动超过了±0.025%,并发现了超过5μm的夹杂物,但棒材1/2半径处晶粒平均尺寸为13μm,孔洞缺陷尺寸小于10μm,并未发现高温铁素体及微裂纹。The preparation method is basically the same as in Example 1, except that the current-voltage ratio in the arc stabilization stage is 220A/V. After testing the final bearing steel bar, it is found that the fluctuation of carbon content exceeds ±0.025%, and it is found that the carbon content exceeds ±0.025%. Inclusions, but the average grain size at 1/2 radius of the bar is 13 μm, the size of hole defects is less than 10 μm, and no high-temperature ferrite and microcracks are found.

对比例2Comparative example 2

与实施例2制备方法基本相同,不同之处在于,铸坯锻前在1270℃高温进行保温,保温时间为16h,最终轴承钢棒材经检测,碳含量波动在±0.01%左右,平均夹杂物尺寸为2μm,最大夹杂物尺寸为5μm,但棒材1/2半径处晶粒平均尺寸为28μm,并发现了15μm微裂纹和高温铁素体。The preparation method is basically the same as in Example 2, the difference is that before forging, the slab is kept at a high temperature of 1270°C for 16 hours. After testing the final bearing steel bar, the carbon content fluctuates around ±0.01%, and the average inclusion The size is 2μm, the largest inclusion size is 5μm, but the average grain size at 1/2 radius of the bar is 28μm, and 15μm microcracks and high-temperature ferrite are found.

对比例3Comparative example 3

与实施例3制备方法基本相同,不同之处在于,终锻温度为850℃,最后一个火次锻造比为4,最终轴承钢棒材经检测,碳含量波动在±0.013%左右,平均夹杂物尺寸为3μm,最大夹杂物尺寸为5μm,且并未发现高温铁素体,棒材1/2半径处晶粒平均尺寸为15μm,但发现了20μm的微裂纹。The preparation method is basically the same as that of Example 3, except that the final forging temperature is 850°C, the last fire forging ratio is 4, the final bearing steel bar is tested, and the carbon content fluctuation is about ±0.013%, and the average inclusion The size is 3 μm, the largest inclusion size is 5 μm, and no high-temperature ferrite is found. The average grain size at 1/2 radius of the bar is 15 μm, but microcracks of 20 μm are found.

根据本申请的实施例,提供了一种不锈钢材料,不锈钢材料由上述的不锈钢材料制备方法制得。According to an embodiment of the present application, a stainless steel material is provided, and the stainless steel material is produced by the above-mentioned stainless steel material preparation method.

本领域的技术人员容易理解的是,在不冲突的前提下,上述各有利方式可以自由地组合、叠加。Those skilled in the art can easily understand that, on the premise of no conflict, the above-mentioned advantageous modes can be freely combined and superimposed.

以上仅为本申请的较佳实施例而已,并不用以限制本申请,凡在本申请的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本申请的保护范围之内。以上仅是本申请的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本申请技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本申请的保护范围。The above are only preferred embodiments of the application, and are not intended to limit the application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the application should be included in the protection scope of the application. Inside. The above are only the preferred embodiments of the present application. It should be pointed out that for those of ordinary skill in the art, some improvements and modifications can be made without departing from the technical principle of the application. These improvements and modifications should also be It is regarded as the scope of protection of this application.

Claims (10)

1. The preparation method of the stainless steel material is characterized by comprising the following steps:
step (1): preparing a stainless steel blank by adopting a duplex process of vacuum smelting and vacuum self-consumption, and reducing component segregation by controlling solidification parameters; the mitigating compositional segregation via solidification parameter control comprises: controlling the maximum molten pool depth of a pasty zone of the consumable blank by controlling a current-voltage ratio so as to further reduce component segregation, so that the fluctuation of the carbon content fraction in the stainless steel blank is within +/-0.015 percent;
step (2): carrying out high-temperature diffusion homogenization treatment on the stainless steel blank to obtain a primary product;
and (3): and (3) forging or rolling deformation treatment is carried out on the primary product obtained in the step (2) to obtain the stainless steel material.
2. A method of manufacturing a stainless steel material according to claim 1, wherein said controlling a current to voltage ratio to control a consumable billet mush zone maximum weld puddle depth comprises the steps of:
the current-voltage ratio is controlled between 260-320A/V, so that the maximum molten pool depth of the consumable blank mushy zone is less than 250mm.
3. The method for preparing a stainless steel material according to claim 1, wherein during step (1), cooling helium gas is fed, and the pressure of the cooling helium gas is between 0.2 and 1.5 kpa.
4. The method for preparing a stainless steel material according to claim 1, wherein the stainless steel blank is subjected to riser cutting and/or skinning;
further, in the step (1), for the steel ingot with the length of 1-1.5m, the diameter of the crucible is 0.4-0.6m; after the vacuum self-consumption is finished, cutting a dead head of the stainless steel blank to a size of more than or equal to 0.15m; and/or the peeling thickness of the stainless steel blank is more than or equal to 15mm;
and/or, a consumable blank with the weight of 1t-3t is adopted in the vacuum consumable process; preferably, 1-1.5t of high-temperature stainless steel consumable blank is adopted in the vacuum consumable process.
5. A method of manufacturing a stainless steel material according to claim 1, wherein the primary product is a homogeneous structure without high temperature ferrite;
and/or, the step (2): the method comprises the following steps of carrying out high-temperature diffusion homogenization treatment on the stainless steel blank to obtain a primary product:
adding pre-deformation treatment before high-temperature diffusion, wherein the temperature of the pre-deformation treatment is more than or equal to 1000 ℃, and the deformation is less than or equal to 30%;
and/or, carrying out high-temperature heat preservation on the stainless steel blank at the temperature of more than or equal to 1120 ℃, preferably, the high-temperature heat preservation temperature is 1120-1230 ℃; and/or the high-temperature heat preservation time is 10-25h.
6. A method of producing a stainless steel material according to claim 1, characterized in that the average size of the grains of the stainless steel material is ≤ 15 μ ι η; the size of the holes of the stainless steel material is less than or equal to 10 mu m; the maximum size of inclusions in the stainless steel material is less than or equal to 5 mu m.
7. The method for preparing a stainless steel material according to claim 1, wherein in the step (3): the forging or rolling deformation treatment of the primary product obtained in the step (2) comprises the following steps:
performing multiple-fire forging deformation treatment on the primary product, wherein upsetting and lengthening are performed alternately in the multiple-fire forging deformation treatment;
further, in the multiple-fire forging deformation treatment, the initial forging temperature is not lower than 1100 ℃, and preferably, the initial forging temperature is 1100-1200 ℃.
8. The method for preparing a stainless steel material according to claim 7, wherein during the multiple-fire forging deformation treatment, the total forging ratio of the blank is not less than 7; and/or the deformation of the last fire is more than or equal to 50 percent;
and/or in the process of the multiple-fire forging deformation treatment, the temperature of finish forging is not lower than 950 ℃; and/or, during the multiple-fire forging deformation treatment, the strain rate is not higher than 0.1s -1
9. The method for preparing a stainless steel material according to claim 1, further comprising the steps of:
after the step (4): heating the stainless steel material obtained in the step (3) to 780-950 ℃, preserving heat for 2-5 hours, and then air-cooling to room temperature.
10. A stainless steel material, characterized in that it is produced by the method of manufacturing a stainless steel material according to any one of claims 1-8; the fluctuation of the carbon content fraction of the stainless steel material is within +/-0.015 percent, the maximum size of inclusions in the stainless steel material is less than or equal to 5 mu m, the size of crystal grains at the 1/2 radius part of the stainless steel material is less than or equal to 15 mu m, and the size of hole defects of the stainless steel material is less than or equal to 10 mu m; the stainless steel material is free of high-temperature ferrite;
and/or the stainless steel material contains less than or equal to 0.15wt% of carbon, more than 13wt% of chromium element and more than 30wt% of total alloy.
CN202210998502.2A 2022-08-19 2022-08-19 Preparation method of stainless steel material and stainless steel material Active CN115369304B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210998502.2A CN115369304B (en) 2022-08-19 2022-08-19 Preparation method of stainless steel material and stainless steel material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210998502.2A CN115369304B (en) 2022-08-19 2022-08-19 Preparation method of stainless steel material and stainless steel material

Publications (2)

Publication Number Publication Date
CN115369304A true CN115369304A (en) 2022-11-22
CN115369304B CN115369304B (en) 2024-02-06

Family

ID=84066112

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210998502.2A Active CN115369304B (en) 2022-08-19 2022-08-19 Preparation method of stainless steel material and stainless steel material

Country Status (1)

Country Link
CN (1) CN115369304B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103526038A (en) * 2013-10-22 2014-01-22 北京科技大学 Electroslag remelting production method of high-strength high-plasticity TWIP (Twinning Induced Plasticity) steel
CN105088094A (en) * 2015-08-11 2015-11-25 宝钢特钢有限公司 Manufacturing method of nitrogen-controlled austenitic stainless steel large forging piece
CN106756081A (en) * 2016-12-27 2017-05-31 钢铁研究总院 The preparation method of big specification Ti Al Nb series alloy fines crystalline substance ingot casting
CN112359218A (en) * 2021-01-13 2021-02-12 北京科技大学 Method for refining carbide in large-size GH4738 cast ingot
CN114231825A (en) * 2021-12-22 2022-03-25 中国科学院金属研究所 High-carbon high-alloy steel product and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103526038A (en) * 2013-10-22 2014-01-22 北京科技大学 Electroslag remelting production method of high-strength high-plasticity TWIP (Twinning Induced Plasticity) steel
CN105088094A (en) * 2015-08-11 2015-11-25 宝钢特钢有限公司 Manufacturing method of nitrogen-controlled austenitic stainless steel large forging piece
CN106756081A (en) * 2016-12-27 2017-05-31 钢铁研究总院 The preparation method of big specification Ti Al Nb series alloy fines crystalline substance ingot casting
CN112359218A (en) * 2021-01-13 2021-02-12 北京科技大学 Method for refining carbide in large-size GH4738 cast ingot
CN114231825A (en) * 2021-12-22 2022-03-25 中国科学院金属研究所 High-carbon high-alloy steel product and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
杨绍利: "《钛铁矿熔炼钛渣与生铁技术》", 北京:冶金工业出版社, pages: 338 *

Also Published As

Publication number Publication date
CN115369304B (en) 2024-02-06

Similar Documents

Publication Publication Date Title
WO2021018203A1 (en) Copper-iron alloy slab non-vacuum down-drawing continuous casting production process
CN104805319A (en) Manufacturing method for 2xxx series ultra-large-dimension aluminum alloy round ingot
CN111394590B (en) A vacuum self-consumption remelting method of deformed superalloy GH4169
CN110468361B (en) Preparation method of deformed high-temperature alloy fine-grain bar
CN103074557B (en) Method for improving weld structure and performance of magnesium alloy
CN108787750B (en) One-step large-deformation rolling method for β solidified TiAl alloy plate
CN103498075B (en) Preparation method of deformation-resistant high-temperature alloy and deformation-resistant high-temperature alloy part
CN112430767A (en) Large-size hollow ingot casting and ingot casting method
CN110484775A (en) Reduce the process of GH4169 nickel-base alloy ingot metallurgy defect
CN110343908A (en) The hip moulding and heat treatment process of IN718 alloy powder and its alloy
CN118048589A (en) A method for preparing large-size and high-uniformity Ti650 high-temperature titanium alloy slab
CN114231825B (en) High-carbon high-alloy steel product and preparation method thereof
CN105803257B (en) Method for improving liquid-state fluidity of TiAl-Nb alloy
CN115369304B (en) Preparation method of stainless steel material and stainless steel material
CN108660320A (en) Electroslag remelting process of a low-aluminum and high-titanium superalloy
CN108015255A (en) A kind of preparation method of high-speed tool steel
CN102517476B (en) High strength aluminum alloy capable of reducing porosity and dispersed shrinkage and preparation method thereof
CN114905010A (en) Nickel-based alloy wire and preparation method thereof
CN113073217B (en) Grain refiner and application thereof
CN109434319A (en) TIG (tungsten inert gas) welding wire for aluminum alloy and preparation method thereof
CN110468292B (en) Manufacturing method of GH4169 nickel-based alloy ingot with low metallurgical defects
CN115323186A (en) A process for controlling the height of superalloy vacuum arc remelting ingot crown
RU2829982C1 (en) Method of manufacturing turbine disk integrated with shaft
CN112453337B (en) Preparation method of high-aluminum-titanium-content powder high-temperature alloy electrode bar
CN101613808A (en) Non-vacuum Production Method of CuCrZr Alloy Wire Rod

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant