CN112981263A - 顺磁性硬质不锈钢及其制造方法 - Google Patents
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Abstract
本发明涉及顺磁性不锈钢,其化学组成包含按重量计:‑26≤Cr≤40%,‑5≤Ni≤20%,‑0≤Mn≤5%,‑0≤Al≤5%,‑0≤Mo≤3%,‑0≤Cu≤2%,‑0≤Si≤5%,‑0≤Ti≤1%,‑0≤Nb≤1%,‑0≤C≤0.1%,‑0≤N≤0.1%,‑0≤S≤0.5%,‑0≤P≤0.1%,余量由铁和任何杂质组成,各杂质具有小于或等于0.5%的含量,所述钢具有500至900的硬度HV10。其还涉及由这种钢制成的部件,特别是钟表组件,和制造所述部件的方法。
Description
技术领域
本发明涉及具有500至900 HV的硬度的顺磁性不锈钢和由这种钢制成的部件,特别是钟表组件。其还涉及制造这种不锈钢部件的方法。
背景技术
硬质和非铁磁性金属合金可用于许多领域,尤其用于经受高机械和/或摩擦应力并需要保持对磁场不敏感的组件。这特别是许多钟表组件的情况,例如在机芯层面的轮、轮齿、轴或甚至游丝。对于外部部件,对获得高硬度也感兴趣,例如对于表壳中心(middle)、外圈、底盖(back)或甚至表冠(crown)。确实,高硬度通常使得可以获得对优质美学外观而言极好的可抛光性,以及优异的耐划伤和耐磨损性,和因此暴露于外部环境的这些组件的良好耐用性。
在冶金学中,根据合金的化学组成及其热机械史,利用各种机制硬化合金。因此,固溶硬化、结构硬化、冷加工、钢中的马氏体转变、亚稳态分解(spinodal decomposition)或甚至通过晶粒细化硬化(Hall Petch)是已知的。在最出色的合金中,同时使用这些硬化机制的几种。但是,硬度大于500 HV的非铁磁性合金是稀有的。此外,为了达到这样的硬度水平,结晶非铁磁性合金在旨在通过第二相淀析获得最大硬度的任选热处理之前通常需要高度冷加工。这是例如只适合通过冷加工硬化的奥氏体不锈钢或甚至一些适合通过冷加工和随后淀析热处理硬化的奥氏体高温合金(superalloys)的情况。在实践中,由在冷加工状态下的这些合金制造组件是困难的。首先,在通过锻造成型的情况下,获得正确的冷加工程度以获得所需硬度并不简单,尤其是对具有复杂几何形状的部件而言。作为替代,可在具有限定和均匀的冷加工程度的半成品中进行机械加工,但并不总是容易获得具有所需冷加工程度的正确材料形式。此外,任何机械加工操作都是非常困难和昂贵的,因为合金已至少部分为硬化状态。最后,如果所用方法不涉及塑性变形,如某些粉末冶金或增材制造法,根本不可能硬化这些合金。作为替代,可以制造固有地具有大于500 HV的硬度的合金,例如某些高熵合金或某些金属间合金,但由于它们的极高硬度和极低延性,它们也很难机械加工并几乎不可能变形。因此理解寻找适合通过热处理硬化而不需要预先冷加工,同时在硬化状态下为非铁磁性的合金的益处。因此在柔软和延性状态下进行成型,并且一旦完成部件后进行硬化热处理。这特别解释了碳钢和马氏体不锈钢的巨大成功,但后者遗憾地是铁磁性的。
为了在非铁磁性合金中获得大于500 HV的硬度,现在广泛使用其它解决方案。在形成部件后特别对例如奥氏体不锈钢或钛合金应用各种表面硬化方法。但是,硬化层的厚度通常极小,约为几十微米,并且该处理通常改变表面外观。对于钟表组件,因此必须在硬化后重新加工部件以获得干净的和通常抛光的表面。但是,这些精加工操作除去所有或一部分硬化层,因此这种解决方案在实践中很少使用,尤其因为表面硬化处理通常昂贵。
也理解了寻找适合通过热处理硬化的具有500-900 HV的非铁磁性合金的需要,在该硬度范围内通常存在在硬化和回火状态下的碳钢、马氏体不锈钢、某些显著硬化的不锈钢或一些冷加工和热处理的奥氏体高温合金。
发明内容
本发明涉及在制造过程中不需要预先冷加工的借助热处理获得顺磁行为和500至900 HV10的硬度的优化不锈钢组合物。
根据本发明的组合物按重量计如下:
- 26 ≤ Cr ≤ 40%,
- 5 ≤ Ni ≤ 20%,
- 0 ≤ Mn ≤ 5%,
- 0 ≤ Al ≤ 5%,
- 0 ≤ Mo ≤ 3%,
- 0 ≤ Cu ≤ 2%,
- 0 ≤ Si ≤ 5%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.1%,
- 0 ≤ N ≤ 0.1%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%,
余量由铁和任何杂质组成,各杂质具有小于或等于0.5%的含量。
根据本发明,制造不锈钢部件的方法包括对具有上文列举的在铁素体或铁素体-奥氏体范围内的组成的基础材料进行第一热处理或热机械处理(thermomechanicaltreatment)和随后硬化该材料以在环境温度下保持铁素体或铁素体-奥氏体结构。这种铁素体或铁素体-奥氏体微结构是柔软和因此延性的,这使得容易成型。然后,在任选成型后,进行硬化处理以将铁素体转变成奥氏体相和转变成富铬的金属间σ相。
本发明的新颖性特别源于使用σ相作为硬化源,因为这种相在不锈钢中一直被认为有害并因此不受欢迎。确实,由于σ相富铬并通常在晶粒边界处形成,其通过降低合金中存在的其它相的铬浓度而极大降低耐腐蚀性。随后,其甚至在极少量下也非常迅速和显著地使不锈钢变弱。确实,这种相具有复杂的四方结构,其固有地非常脆并且其在晶粒边界处的存在为裂纹扩展创造有利的路径。其因此从未用于不锈钢,尽管它有两个特别有利的性质——在900至1100 HV10之间的硬度和顺磁性质。
根据本发明,优化不锈钢的组成和方法以获得σ相和奥氏体相的精细分布,没有偏向于在晶粒边界处形成σ相。由两种非铁磁性相组成的这种特定微结构能够获得硬度和韧度之间的极好折衷、良好的耐腐蚀性以及优异的可抛光性。
在参考下列附图阅读下列详述时将显现本发明的其它特征和优点。
附图说明
图1和2分别代表根据本发明的Fe-35%Cr-9%Ni(重量%)钢在硬化处理之前和之后的衍射图。
图3代表通过光学显微镜获得的根据本发明的Fe-32%Cr-9%Ni(重量%)钢的图像。
图4代表相同合金的磁滞曲线。
具体实施方式
本发明涉及具有500至900 HV10的硬度的顺磁性不锈钢以及制造由这些钢制成的部件的方法。HV10硬度是指根据标准ISO 6507-1:2018测得的Vickers硬度。本发明还涉及用这种钢制成的部件,更尤其是钟表组件。其可由选自下列非穷举列表的外部部件组成:表壳中心、底盖、外圈、表冠、按钮(push-piece)、表带连接(wristlet link)、表带、舌扣、表盘、指针和表盘刻度(dial index)。其也可由选自下列非穷举列表的机芯组件组成:齿轮、轴、轮齿(pinion)、游丝、夹板(bridge)、主夹板(plate)、螺丝和摆轮。
根据本发明的不锈钢具有按重量计的下列组成:
- 26 ≤ Cr ≤ 40%,
- 5 ≤ Ni ≤ 20%,
- 0 ≤ Mn ≤ 5%,
- 0 ≤ Al ≤ 5%,
- 0 ≤ Mo ≤ 3%,
- 0 ≤ Cu ≤ 2%,
- 0 ≤ Si ≤ 5%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.1%,
- 0 ≤ N ≤ 0.1%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%,
余量由铁和任何杂质组成,各杂质具有小于或等于0.5%的含量。
优选地,它们具有按重量计的下列组成:
- 28 ≤ Cr ≤ 38%,
- 5 ≤ Ni ≤ 15%,
- 0 ≤ Mn ≤ 3%,
- 0 ≤ Al ≤ 3%,
- 0 ≤ Mo ≤ 3%,
- 0 ≤ Cu ≤ 2%,
- 0 ≤ Si ≤ 5%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.05%,
- 0 ≤ N ≤ 0.05%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%,
余量同样由铁和任何杂质组成,各杂质具有小于或等于0.5%的含量。
更优选地,它们具有按重量计的下列组成:
- 30 ≤ Cr ≤ 36%,
- 5 ≤ Ni ≤ 10%,
- 0 ≤ Mn ≤ 3%,
- 0 ≤ Al ≤ 1%,
- 0 ≤ Mo ≤ 1%,
- 0 ≤ Cu ≤ 1%,
- 0 ≤ Si ≤ 3%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.05%,
- 0 ≤ N ≤ 0.05%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%,
余量同样由铁和任何杂质组成。
根据本发明,制造不锈钢部件的方法包括步骤a):提供或制造具有落在上文列举的范围内的组成的坯料。这种坯料具有主要铁素体结构或优选100%铁素体结构。由经受在950℃-1450℃的温度下的热处理或热机械处理和随后硬化的基础材料获得该坯料。基础材料可以是粉末或固结材料的形式。其可通过铸造、通过压制、通过金属注射成型(MIM)、通过增材制造,更广义地说,通过粉末冶金制成。可以考虑在单个步骤中制造基础材料和进行热处理,例如借助选择性激光熔化(SLM)技术。这些不同的技术使得可以用基础材料制造尺寸与要生产的部件基本相等的坯料,在这种情况下不需要后续成型步骤。
优化基础材料的组成以在950℃至1450℃的温度下保持1分钟至24小时的时间时获得主要或完全铁素体结构。选择温度以获得小于或等于40%的奥氏体质量分数和大于或等于60%的铁素体质量分数。奥氏体的存在使得可以获得最低硬度和最大延性以便容易成型,例如通过锻造、通过冲切或通过机械加工。
在950℃-1450℃范围内的热处理或热机械处理可用于对通过铸造获得的基础材料进行均化、重结晶或应力松弛处理或对粉末形式的基础材料进行烧结。在铁素体或铁素体-奥氏体范围内的处理可在单个周期中进行或包括几个热处理或热机械处理周期。在其之前或之后也可具有其它热处理或热机械处理。
在铁素体或铁素体-奥氏体范围内停留后,对坯料施以快速冷却(也称为硬化)到小于500℃的温度以防止在冷却过程中形成新相。因此,在环境温度下保持铁素体或铁素体-奥氏体结构。由于根据本发明的组合物,铁素体结构足够稳定以在快速冷却后在环境温度下得以保留,但足够亚稳定以在650℃至900℃的中等温度下的后续热处理过程中容易并快速转变成σ相和转变成奥氏体。
在步骤a)之后,该合金具有低硬度和高延性,以便在适用的情况下容易成型,例如通过锻造、通过冲切或通过机械加工。
在步骤a)之后,该方法包括任选步骤b):通过机械加工、冲切或通过涉及变形的任何操作,如锻造将坯料成型。这一步骤可在几个工序中进行。如果来自步骤a)的坯料已具有要制造的部件的最终形状,则不需要这一步骤。
除成型外,塑性变形操作可用于在将铁素体转变成奥氏体和σ相的后续步骤的过程中特别提高铁素体转变速率。此外,由于通过冷加工实现的硬化对铁素体结构而言很低并且根据本发明的合金在通过硬化处理前主要或完全是铁素体,这一塑性变形步骤不会引发对通过机械加工或冲切进行的任选成型而言成问题的硬化。在一个或多个工序中的这种塑性变形可在小于650℃的温度下进行。
在任选成型后,该方法包括步骤c):坯料在650℃至900℃之间的硬化热处理以获得最终性质。设定在650℃至900℃之间的热处理的持续时间以确保铁素体的完全转变和因此获得由σ相和奥氏体相形成的微结构。
如上文提到,铁素体转变成奥氏体 + σ相的速率特别取决于合金的组成及其热机械史。一般而言,该处理的持续时间在30分钟至24小时之间。在硬化处理后,钢具有40%至80%的σ相质量分数和20%至60%的奥氏体质量分数,百分比取决于化学组成和进行的热处理。由于该硬化热处理,所得部件具有500至900 HV10的高硬度。对于所有不锈钢,也可少量存在任选的非金属夹杂物而不影响机械和磁性性质。此外,在该合金中也可少量存在用于增强机械加工性的夹杂物,例如硫化锰。
在这种硬化热处理步骤后可接着任选的表面精加工步骤d),如抛光。
此外,在步骤a)中的具有奥氏体 + 铁素体结构的坯料存在下,该制造方法可包括在硬化热处理前在950℃-1450℃温度范围内的附加步骤b’),以将奥氏体 + 铁素体结构转变成100%铁素体结构。
总体而言,在高温(950℃-1450℃)热处理和随后硬化后,钢特别具有下列性质:
·150至400 HV10的硬度。
·良好延性,在环境温度下在大于50%压缩下塑性变形而不开裂。
·由于存在铁素体,铁磁行为。
在硬化热处理后,根据本发明的钢特别具有下列性质:
·500至900 HV10的硬度。
·顺磁行为。
·由于非常精细的微结构,优异的可抛光性。
·良好的耐磨损性。
·良好的耐腐蚀性。
关于耐腐蚀性,由于高铬浓度,根据本发明的钢特别有效。因此这些钢对于外部部件是特别有利的。
最后,使用下文实施例举例说明本发明。
实施例
在第一个实施例中,命名为Fe35Cr9Ni的钢含有按质量百分比计56%铁、35%铬和9%镍。其通过由高纯度元素(> 99.9%)电弧熔炼制造,在环境温度下通过压缩变形以使厚度减小为1/2,并在氩气气氛中在1300℃下经受在铁素体范围内的均化热处理2小时,随后气体硬化(大约200K/min)。在这种均化热处理后,该合金Fe35Cr9Ni具有单相铁素体微结构,具有350 HV10的Vickers硬度。通过如图1中所示的X-射线衍射(XRD)分析证实完全铁素体结构(空间群Im3m)。在均化后,在800℃下进行硬化热处理6小时。获得包含奥氏体相和σ相的精细、均匀和两相的微结构。图2中所示的X-射线衍射分析证实存在奥氏体(空间群Fm3m)和对应于σ相的四方结构(空间群 P42/mnm)。
在这种冶金态下,合金Fe35Cr9Ni具有670 HV10的Vickers硬度。使用根据ISO9227标准的盐雾试验评估其耐腐蚀性。在该试验后,该合金没有表现出腐蚀迹象,证实其在含盐环境中的优异耐腐蚀性。由于σ相的存在(即使小比例)始终引发不锈钢的耐腐蚀性的大幅降低,这更加引人注目。
在第二个实施例中,命名为Fe32Cr9Ni的钢含有按质量百分比计59%铁、32%铬和9%镍。其也通过由高纯度元素(> 99.9%)电弧熔炼制造,在氩气中在1300℃下经受均化热处理2小时,随后气体硬化,在环境温度下通过压缩变形以使厚度减小为1/2,在空气中在1200℃下经受重结晶热处理1分钟,随后水淬硬化。在这种重结晶热处理后,该合金Fe32Cr9Ni具有单相铁素体微结构,具有220 HV10的Vickers硬度。然后在真空中使其达到700℃,持续6小时。在偏振光中的光学显微镜中观察到的微结构显示在图3中。观察到两个相的精细分布,凸起的是奥氏体相,在基质中的是σ相。在这种冶金态下,合金Fe32Cr9Ni具有635 HV10的Vickers硬度。关于这种钢的磁性质,用振动样品磁力计在环境温度下测量磁滞曲线(磁化强度M vs 外加场H)。尽管具有相对较高的体积磁化率,但这种钢具有顺磁行为特有的线性行为(图4)。
Claims (16)
1.顺磁性不锈钢,其化学组成包含按重量计:
- 26 ≤ Cr ≤ 40%,
- 5 ≤ Ni ≤ 20%,
- 0 ≤ Mn ≤ 5%,
- 0 ≤ Al ≤ 5%,
- 0 ≤ Mo ≤ 3%,
- 0 ≤ Cu ≤ 2%,
- 0 ≤ Si ≤ 5%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.1%,
- 0 ≤ N ≤ 0.1%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%,
余量由铁和任何杂质组成,各杂质具有小于或等于0.5%的含量,
所述钢具有500至900的硬度HV10,
所述钢具有由40%至80%质量百分比的σ相和20%至60%质量百分比的奥氏体相形成的微结构,奥氏体相源自具有包含100%铁素体的结构的合金的转变。
2.根据权利要求1的钢,其化学组成包含按重量计:
- 28 ≤ Cr ≤ 38%,
- 5 ≤ Ni ≤ 15%,
- 0 ≤ Mn ≤ 3%,
- 0 ≤ Al ≤ 3%,
- 0 ≤ Mo ≤ 3%,
- 0 ≤ Cu ≤ 2%,
- 0 ≤ Si ≤ 5%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.05%,
- 0 ≤ N ≤ 0.05%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%。
3.根据权利要求1或2的钢,其化学组成包含按重量计:
- 30 ≤ Cr ≤ 36%,
- 5 ≤ Ni ≤ 10%,
- 0 ≤ Mn ≤ 3%,
- 0 ≤ Al ≤ 1%,
- 0 ≤ Mo ≤ 1%,
- 0 ≤ Cu ≤ 1%,
- 0 ≤ Si ≤ 3%,
- 0 ≤ Ti ≤ 1%,
- 0 ≤ Nb ≤ 1%,
- 0 ≤ C ≤ 0.05%,
- 0 ≤ N ≤ 0.05%,
- 0 ≤ S ≤ 0.5%,
- 0 ≤ P ≤ 0.1%。
4.由根据前述权利要求之一的顺磁性不锈钢制成的部件。
5.根据权利要求4的部件,其特征在于其由外部部件或机芯的钟表组件组成。
6.包括根据权利要求5的钟表组件的表。
7.制造顺磁性不锈钢部件的方法,其特征在于其包括下列相继步骤:
a) 提供或制造基本具有要制造的部件的形状或具有不同形状的坯料,所述坯料具有根据权利要求1至3之一的化学组成并具有包含100%铁素体的结构,
b) 如果步骤a)中的所述坯料具有与要制造的部件不同的形状,将所述坯料成型,
c) 所述坯料的热处理或硬化处理以获得部件,所述硬化处理在650至900℃的温度下进行30分钟至24小时的时间以将所述结构的铁素体转变成奥氏体相和金属间σ相,在所述硬化处理后接着冷却到环境温度。
8.根据权利要求7的制造方法,其特征在于已通过在950至1450℃的温度下对基础材料进行热处理或热机械处理1分钟至24小时的时间产生步骤a)中的坯料的主要或完全铁素体结构,在所述热处理或热机械处理之后接着硬化到小于500℃的温度以在环境温度下保持铁素体结构。
9.根据前一权利要求的制造方法,其特征在于所述基础材料是粉末或固结材料的形式。
10.根据权利要求8的制造方法,其特征在于所述基础材料已通过铸造、通过压制、通过金属注射成型、通过增材制造或通过粉末冶金获得。
11.根据权利要求7的制造方法,其特征在于通过选择性激光熔化制成步骤a)中的坯料。
12.根据权利要求7至11之一的制造方法,其特征在于在步骤a)之后,所述坯料具有150至400 HV10的硬度。
13.根据权利要求7至11之一的制造方法,其特征在于所述成型步骤b)包括一个或多个在小于650℃的温度下的塑性变形工序。
14.根据权利要求7至11之一的制造方法,其特征在于所述成型步骤b)通过锻造、冲切或机械加工进行。
15.根据权利要求8的制造方法,其特征在于所述热处理或热机械处理在几个周期中进行。
16.根据权利要求7至11之一的制造方法,其特征在于当所述结构包含奥氏体时,所述方法包括,在步骤c)之前,在950至1450℃的温度下对所述坯料进行热处理或热机械处理步骤b’) 1分钟至24小时的时间以获得完全铁素体结构,在所述热处理或热机械处理之后接着硬化到小于500℃的温度以在环境温度下保持完全铁素体结构。
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