CN114182178A - 一种高氮无镍奥氏体不锈钢及其制备方法和应用 - Google Patents

一种高氮无镍奥氏体不锈钢及其制备方法和应用 Download PDF

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CN114182178A
CN114182178A CN202111500275.8A CN202111500275A CN114182178A CN 114182178 A CN114182178 A CN 114182178A CN 202111500275 A CN202111500275 A CN 202111500275A CN 114182178 A CN114182178 A CN 114182178A
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stainless steel
austenitic stainless
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nitrogen nickel
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CN114182178B (zh
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饶钦盛
甄飞麟
黄明帅
倪释凌
戴芬
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Guangzhou Golden South Magnetic Material Co ltd
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Abstract

一种高氮无镍奥氏体不锈钢，按照质量百分比，包括以下组分，0.7％～1.2％N、15％～20％Cr、9％～12％Mn、2.5％～3.5％Mo、≤0.8％Si、≤0.007％C、≤0.005％S、≤0.013％P，余量为Fe。一种高氮无镍奥氏体不锈钢的制备方法，包括如下步骤：混料、生坯压制、热脱脂、烧结渗氮和固溶处理。上述高氮无镍奥氏体不锈钢的制造成本低，耐腐蚀性能好，生物相容性良好，在生物医学上具有广阔的应用前景，属于医用不锈钢领域。

Description

一种高氮无镍奥氏体不锈钢及其制备方法和应用
技术领域
本发明涉及医用不锈钢领域，具体涉及一种高氮无镍奥氏体不锈钢及其制备方法和应用。
背景技术
医用不锈钢是生物医用金属中应用最多，最广的一类材料。最常用的316L和317L等奥氏体不锈钢植入材料和医疗工具中的镍元素会与汗水、唾液等体液发生副反应，导致皮肤出现肿胀、发红、瘙痒等症状，对人体有潜在的致癌危害。自上世纪90年代中期开始，一些发达国家已率先立法，限制使用含镍不锈钢作为人体植入材料和各种与人体直接接触的器械。另外，对于医用不锈钢来说，化学稳定性和生物相容性至关重要。据报道，少量氮元素的加入能大幅促进奥氏体的稳定性，并扩大奥氏体相区。CN101368252A公开了一种无镍含氮奥氏体不锈钢，其成分及质量百分比为：0.05～0.25％N、≤0.10％C、24.0～30.0％Mn、12.0～14.0％Cr、≤1.0％Si、0.35～1.00Mo、≤0.05％S、≤0.05％P、余Fe。该种不锈钢随具有较好的力学性能和耐腐蚀性，但未呈现出较好的生物相容性。
发明内容
针对现有技术中存在的技术问题，本发明的目的是：提供一种低成本、综合力学性能良好、具有优良耐腐蚀性和生物相容性的高氮无镍奥氏体不锈钢及其制备方法和应用。
为了达到上述目的，本发明采用如下技术方案：一种高氮无镍奥氏体不锈钢，按照质量百分比，包括以下组分，0.7％～1.2％N、15％～20％Cr、9％～12％Mn、2.5％～3.5％Mo、≤0.8％Si、≤0.007％C、≤0.005％S、≤0.013％P，余量为Fe。
一种高氮无镍奥氏体不锈钢的制备方法，包括如下步骤：混料、生坯压制、热脱脂、烧结渗氮和固溶处理。
作为一种优选，混料时，将粘结剂和预合金粉混合，粘结剂和预合金粉的重量占比分别为5～10％和90～95％，各粘结剂组分的质量占比为：聚酰胺1～2％、聚乙烯蜡1～2％、棕榈蜡1～2％、微晶蜡1～2％。
作为一种优选，生坯压制过程中，将混料后得到的混合粉料放入模具中，采用液压装置进行压制。
作为一种优选，压制温度为130～170℃，保温时间为5～10min。
作为一种优选，热脱脂过程中，热脱脂温度为400～600℃，保温时间为0.5～2h。
作为一种优选，烧结渗氮过程中，烧结气氛为氮气，烧结温度为1100～1300℃，烧结时间为1～3h。
作为一种优选，固溶处理的气氛为氮气，固溶处理温度为1100～1200℃，固溶处理时间为1～2h。
一种上述的高氮无镍奥氏体不锈钢的应用，用于人体植入材料或家具灯饰行业。
上述高氮无镍奥氏体不锈钢主要应用于生物医学领域，从而替代传统的医用镍铬不锈钢，同时由于其良好的综合力学性能和耐腐蚀性，也可用于国防，能源，化工，铁路，造船，航空等工业领域。
总的说来，本发明具有如下优点：
1、成本低。本发明制备的高氮无镍奥氏体不锈钢的不需添加贵重合金元素，成本低，且利用温压成型工艺脱脂后的孔隙可以缩短渗氮时间，增大渗氮距离，不仅具有很好的经济效益同时可以提高氮的均匀性。
2、综合力学性能优越。本不锈钢为单相奥氏体较高的氮含量可以更好地促进间隙固溶强化和沉淀强化作用，提高不锈钢的力学性能。
3、优良的耐腐蚀性。氮可以改善金属/Cr2O3膜界面钝化膜的稳定性，阻滞Cr的溶解，使膜内的Cr富集程度增加，提高钝化膜的致密度，从而有效调高不锈钢的耐腐蚀性。
4、良好的生物相容性。本发明制备的不锈钢不含镍元素，对细胞无毒性。且具有较高的氮含量，氮含量的提高可以使不锈钢拥有更高的表面能，有利于细胞粘着。但是过高的氮含量会导致不锈钢集基体析出氮化物CrN及Cr2N，降低不锈钢的韧性和耐腐蚀性，所以氮含量应不高于1.2％。本发明制备的不锈钢在提高其生物相容性的同时，不降低其韧性和耐腐蚀性。
附图说明
图1为MC3T3-E1细胞在空白组样品上培养7天后用罗丹明缀合的鬼笔环肽和DAPI染色后的免疫荧光图。
图2为MC3T3-E1细胞在316L不锈钢样品上培养7天后用罗丹明缀合的鬼笔环肽和DAPI染色后的免疫荧光图。
图3为MC3T3-E1细胞在高氮无镍奥氏体不锈钢样品上培养7天后用罗丹明缀合的鬼笔环肽和DAPI染色后的免疫荧光图。
具体实施方式
下面将结合附图和具体实施方式来对本发明做进一步详细的说明。
实施例一
一种高氮无镍奥氏体不锈钢，按照质量百分比，包括以下组分，0.7％～1.2％N、15％～20％Cr、9％～12％Mn、2.5％～3.5％Mo、≤0.8％Si、≤0.007％C、≤0.005％S、≤0.013％P，余量为Fe。
使用温压成型工艺(WC)制备高氮无镍奥氏体不锈钢。
第一步，混料：将粉末状的粘结剂和粉末状的预合金粉混合，粘结剂和预合金粉的占比分别为6wt.％和94wt.％。预合金粉的成分(wt.％)为0.4％N、17％Cr、11.5％Mn、3.5％Mo、0.8％Si、0.007％C、0.005％S、0.013％P、余量为Fe。其中各粘结剂组份所占的配比为：1.5wt.％聚酰胺+1.5wt.％聚乙烯蜡+1.5wt.％棕榈蜡+1.5wt.％微晶蜡，合共6wt.％。将上述粉末与溶剂混合，形成混合粉料。粉末质量(g)和溶剂体积(ml)的最佳比例为100：25，溶剂为酒精。
第二步，生坯压制：将混合粉料放入模具中，163℃保温5min，用手动小型液压机将其压制成直径为15mm和厚度大约为5mm的温压生坯。
第三步，热脱脂：热脱脂温度为500℃，保温时间为1h。
第四步，烧结渗氮：烧结气氛为氮气，烧结温度为1250℃，烧结时间为2h。
第五步，固溶处理：固溶处理的气氛为氮气，固溶处理温度为1150℃，固溶处理时间为1.5h。
一种上述的高氮无镍奥氏体不锈钢的应用，用于人体植入材料或家具灯饰行业。其用于人体植入材料时，可用于制作口腔种牙和心血管支架等。
如表1所示为上述高氮无镍奥氏体不锈钢与316L不锈钢的性能对照数据，高氮无镍奥氏体不锈钢其硬度和压缩屈服强度明分别为282.4HV和468.3MPa，均远高于316L不锈钢的179.7HV和244.5MPa，且高氮无镍奥氏体不锈钢在压缩力达到21kN时试样未发生断裂。
表1
Figure BDA0003401317220000041
在0.6mol/L的NaCl溶液中，该种高氮无镍奥氏体不锈钢的腐蚀电流密度为0.038±0.002uA cm2，316L不锈钢为0.014±0.002μA cm2，两者的腐蚀电流密度相近，均远远低于1mA/cm2。
图1～图3为MC3T3-E1细胞在不同样品上培养7天后用罗丹明缀合的鬼笔环肽和DAPI染色后的免疫荧光图。316L不锈钢样品表面细胞饱满，以多边形和纺锤形细胞为主；温压成型的高氮无镍奥氏体不锈钢样品表面细胞长而细的树突状结构数量进一步增加，细胞呈现出星状形态并长出更长的伪足，伪足相互交织，形态进一步分化，呈现出良好的生物相容性。
上述实施例为发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (9)

1.一种高氮无镍奥氏体不锈钢，其特征在于：按照质量百分比，包括以下组分，0.7％～1.2％N、15％～20％Cr、9％～12％Mn、2.5％～3.5％Mo、≤0.8％Si、≤0.007％C、≤0.005％S、≤0.013％P，余量为Fe。
2.一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：包括如下步骤：混料、生坯压制、热脱脂、烧结渗氮和固溶处理。
3.按照权利要求2所述的一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：混料时，将粘结剂和预合金粉混合，粘结剂和预合金粉的重量占比分别为5～10％和90～95％，各粘结剂组分的质量占比为：聚酰胺1～2％、聚乙烯蜡1～2％、棕榈蜡1～2％、微晶蜡1～2％。
4.按照权利要求2所述的一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：生坯压制过程中，将混料后得到的混合粉料放入模具中，采用液压装置进行压制。
5.按照权利要求4所述的一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：压制温度为130～170℃，保温时间为5～10min。
6.按照权利要2所述的一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：热脱脂过程中，热脱脂温度为400～600℃，保温时间为0.5～2h。
7.按照权利要求2所述的一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：烧结渗氮过程中，烧结气氛为氮气，烧结温度为1100～1300℃，烧结时间为1～3h。
8.按照权利要求2所述的一种高氮无镍奥氏体不锈钢的制备方法，其特征在于：固溶处理的气氛为氮气，固溶处理温度为1100～1200℃，固溶处理时间为1～2h。
9.一种权利要求1所述的高氮无镍奥氏体不锈钢的应用，其特征在于：用于人体植入材料或家具灯饰行业。
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