CN112079645A - 一种织构化碳化硅晶须增韧的氧化铝基陶瓷及其制备方法和应用 - Google Patents

一种织构化碳化硅晶须增韧的氧化铝基陶瓷及其制备方法和应用 Download PDF

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CN112079645A
CN112079645A CN202010838576.0A CN202010838576A CN112079645A CN 112079645 A CN112079645 A CN 112079645A CN 202010838576 A CN202010838576 A CN 202010838576A CN 112079645 A CN112079645 A CN 112079645A
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alumina
silicon carbide
based ceramic
textured
casting
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CN112079645B (zh
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周宇章
谭大旺
郭伟明
林华泰
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Guangdong University of Technology
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Abstract

本发明属于复合梯度陶瓷领域，公开一种织构化碳化硅晶须增韧的氧化铝基陶瓷及其制备方法和应用。该氧化铝基陶瓷是以氧化铝、碳化硅晶须和烧结助剂MgO或Y2O3为原料，以石蜡为结构辅助剂，先将原料混合得到混合粉体，将混合粉体分散于液态热石蜡中，经铸造冷却后得到铸件，在常温下挤压铸件实现织构化，高温去除石蜡后得到生坯，生坯经轴向加压为20～50MPa，升温至1500～1800℃烧结制得。本发明方法实现了碳化硅晶须径向定向排列的织构化氧化铝基陶瓷的制备，在摩擦面上具有高耐磨性与热导率，在高速加工耐热合金，高硬度金属材料时有利于降低切削温度，具有更高的稳定性，与市场上常见的陶瓷刀具相比具有明显的应用优势。

Description

一种织构化碳化硅晶须增韧的氧化铝基陶瓷及其制备方法和 应用
技术领域
本发明属于复合梯度陶瓷材料技术领域，更具体地，涉及一种织构化碳化硅晶须增韧的氧化铝基陶瓷及其制备方法和应用。
背景技术
现代切削技术的发展必然是向着高速化、精密化的与自动化迈进，这对切削用的刀具性能提出更高的要求。发展陶瓷刀具可以减少稀有资源的使用，同时提高加工效率，实现高速高效绿色加工。
目前，主流的陶瓷刀具体系可以分为氧化铝基与氮化硅基两大类，其中氧化铝基的陶瓷刀具研究最早，相关理论较为成熟，且原料在自然界中含量丰富。经过多代的改良，在力学性能与切削性能方面，氧化铝基的复合陶瓷刀具已经得到很大的提升，在切削铁系金属时，其切削速度比硬质合金刀具高几倍。特别在加工一些切削热大，切削温度高的金属材料如镍基高温合金等材料时，氧化铝基陶瓷刀具在耐摩擦与耐高温方面具有更明显的优势。
同样地，氧化铝基陶瓷刀具也有脆性大，抗冲击性能差的特点，需要进行增韧处理。目前市面上已有的处理方法是加入碳化硅晶须、石墨烯薄片等物质进行强化。其中晶须增韧刀具已经得到广泛应用，但由于氧化铝刀具热导率低，用于增韧的晶须在烧结体内随机排布时不能有效地增加热导率，而高速切削的温度很高，从而限制了其高速切削性能。
为解决这一问题，通过晶须在陶瓷内的定向排布，实现晶须的内部织构化，从而实现高到导热性，提高其切削性能。而径向定向排列的结构可以最大化实现多个切削刃垂直于晶须方向，实现最大化的切削效果。
本发明综合了材料内部织构化的材料设计制备方法与陶瓷增韧技术增韧，发明一种增韧晶须径向定向排列的织构化碳化硅晶须增韧氧化铝基陶瓷切削刀具材料，以其为材料制备的转位刀片与整体刀具与传统的晶须增韧陶瓷刀具相比具有更优异的切削性能。
发明内容
为了解决上述现有技术存在的不足和缺点，提供一种织构化碳化硅晶须增韧的氧化铝基陶瓷。该陶瓷为碳化硅晶须径向定向排列的织构化氧化铝基陶瓷。
本发明的另一目的在于提供上述织构化碳化硅晶须增韧的氧化铝基陶瓷的制备方法。该方法以氧化铝、碳化硅晶须和烧结助剂为原料，以石蜡为结构辅助剂，先将原料混合得到混合粉体，将混合粉体分散于液态热石蜡中，经铸造冷却后得到铸件，在常温下挤压铸件实现织构化，高温去除石蜡后得到生坯，生坯经高温加压烧结得到烧结体，烧结体经机械加工后得到成品刀具，实现碳化硅晶须径向定向排列的织构化氧化铝基陶瓷的制备。
本发明的再一目的在于提供上述织构化碳化硅晶须增韧的氧化铝基陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种织构化碳化硅晶须增韧的氧化铝基陶瓷，所述氧化铝基陶瓷是将氧化铝粉、碳化硅晶须、烧结助剂MgO或Y2O3，加入溶剂和球磨介质，进行球磨混合后干燥，得到混合粉体；再将混合粉体分散于热石蜡中，并趁热倒入模具中，铸造成所需形状的铸件；常温下对上述铸件施加轴向的压力为10～100MPa，铸件在高压下沿中心变形，形成晶须径向排列的织构化挤压件；然后常压下在100～250℃对织构化挤压件进行排胶，将石蜡完全挥发，得到生坯；将生坯装入石墨模具中，并置于热压烧结炉或放电等离子烧结炉中，在氩气气氛保护下，轴向加压为20～50MPa，升温至1500～1800℃保温，此后降温至500～600℃，并随炉冷却至室温制得。
优选地，所述的氧化铝基陶瓷的相对密度为98％以上，所述氧化铝基陶瓷在垂直于加压方向的面上的维氏硬度为18～23GPa，在弦切面中心处的维氏硬度为17～21GPa。
优选地，所述溶剂为乙醇、丙酮或去离子水；所述球磨介质为氧化铝球或碳化硅球；所述球磨的转速为100～300r/min，所述球磨的时间为4～24h。
优选地，所述的氧化铝粉的粒径为1～3μm，纯度为98～100wt.％；所述MgO或Y2O3粉的纯度为99～99.9wt.％，所述MgO或Y2O3粉的粒径为0.2～1μm。
优选地，所述碳化硅晶须和氧化铝粉的体积比为(4.5～55)：(54.5～94.5)；
优选地，所述烧结助剂占粉体总质量的0.3～1.5％。
优选地，所述生坯的外径为10～100mm，高度为3～80mm，外径与内径的比值为1.25～2。
优选地，所述升温的速率为10～150℃/min，所述保温的时间为20～120min，所述降温的速率为10～150℃/min。
一种织构化碳化硅晶须增韧的氧化铝基陶瓷的制备方法，包括如下具体步骤：
S1.将氧化铝粉、碳化硅晶须、烧结助剂MgO或Y2O3，加入溶剂和球磨介质，进行球磨混合后干燥，得到混合粉体；
S2.将混合粉体分散于热石蜡中，并趁热倒入模具中，铸造成所需形状的铸件；
S3.在常温下对上述铸件施加轴向的压力为10～100MPa，铸件在高压下沿中心变形，形成晶须径向排列的织构化挤压件；
S4.常压下在100～250℃对织构化挤压件进行排胶，将石蜡完全挥发，得到生坯；
S5.将生坯装入石墨模具中，并置于热压烧结炉或放电等离子烧结炉中，在氩气气氛保护下，轴向加压为20～50MPa，升温至1500～1800℃保温，此后降温至500～600℃，并随炉冷却至室温，制得织构化碳化硅晶须增韧的氧化铝基陶瓷，该陶瓷为碳化硅晶须径向定向排列的织构化氧化铝基陶瓷。
所述的织构化碳化硅晶须增韧的氧化铝基陶瓷在切削刀具领域中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明的氧化铝基陶瓷的晶粒径向定向织构化结构具有径向，轴向的物理机械性能差异性，垂直径向方向的表面具有高耐磨性，沿径向方向具有高热导率。
2.本发明的织构化氧化铝基陶瓷在摩擦面上具有高耐磨性与热导率，在高速加工耐热合金，高硬度金属材料时有利于降低切削温度，具有更高的稳定性。
3.本发明的的氧化铝基陶瓷晶粒径向定向排列工艺采用常温的轴向加压处理，相比于一般的流延成型工序更少，大大提高了生产效率；同时可灵活改变挤压坯体的模具尺寸、施压的力度大小，从而实现对刀具形状、尺寸、织构化程度的控制，满足各种生产需求。
4.本发明织构化碳化硅晶须增韧的氧化铝基陶瓷在垂直径向方向的表面具有高耐磨高导热性，其加工工序少，生产效率高，在高速加工耐热合金，高硬度金属材料时有利于降低切削温度，具有更高的稳定性，与市场上常见的陶瓷刀具相比具有明显的应用优势。
附图说明
图1为实施例1制得碳化硅晶须径向定向排列的织构化氧化铝基陶瓷在垂直于加压方向的形貌；
图2为对比例1制备的碳化硅晶须增韧氧化铝基陶瓷在垂直于加压方向的面上形貌。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.制备
(1)将体积比为60：55：5的氧化铝粉(纯度99.99％)、碳化硅晶须、烧结助剂Y2O3(纯度99.99％)进行配料，以乙醇为溶剂，以氧化铝球为球磨介质，转速为200r/min，进行辊式球磨混合10h，经过干燥，得到混合粉体；
(2)将混合粉体分散于热石蜡中，并趁热倒入模具中(外径80mm，高75mm，外径与内径之比为1.6)，铸造成筒形铸件；
(3)在常温下对铸件施加90MPa轴向的压力，铸件在高压下沿中心变形，形成晶须径向排列的织构化挤压件。
(4)常压下在250℃对织构化挤压件进行排胶，将石蜡完全挥发，得到生坯；
(5)将生坯装入石墨模具中，并置于热压烧结炉或放电等离子烧结炉中，在氩气气氛保护下，轴向加压40MPa下，以50℃/min升温至1700℃烧结，保温100min，此后以50℃/min降温至500℃，并随炉冷却至室温，制得碳化硅晶须径向定向排列的织构化氧化铝基陶瓷。
2.性能测试：本实施例所得的氧化铝陶瓷的显微形貌显示在垂直于步骤(5)中加压方向的面上晶须基本上沿径向排列，相对密度为99.8％，所述氧化铝陶瓷在垂直于加压方向的面上的维氏硬度为22GPa，在弦切面中心处的维氏硬度为21.5GPa。
图1为实施例1制得碳化硅晶须径向定向排列的织构化氧化铝基陶瓷在垂直于加压方向的形貌；从图1中可知：在截面上有80％以上的长棒状碳化硅晶须的长轴方向与截面外接圆中心线之间的夹角小于30°，整体上实现了定向织构化。
对比例1
1.制备
(1)将体积比为60：55：5的氧化铝粉(纯度99.99％)、碳化硅晶须、烧结助剂Y2O3(纯度99.99％)进行配料，以乙醇为溶剂，以氧化铝球为球磨介质，转速为200r/min，进行球磨混合10h，经过干燥，得到混合粉体；
(2)将混合粉体直接装入石墨模具中，在氩气气氛保护下，轴向加压40MPa下，以50℃/min升温至1700℃，保温100min，此后以50℃/min降温至500℃，并随炉冷却至室温，制得碳化硅晶须增韧氧化铝基陶瓷；
将氧化铝基陶瓷进行机械开刃加工，获得碳化硅晶须增韧氧化铝基陶瓷切削刀具。
2.性能测试：本对比例所得的氧化铝陶瓷的显微形貌显示在垂直于步骤(2)中加压方向的面上晶须方向随机分布，所述氧化铝陶瓷在垂直于加压方向的面上的维氏硬度为21.6GPa，在弦切面中心处的维氏硬度为21.5GPa。
图2为对比例1制备的碳化硅晶须增韧氧化铝基陶瓷在垂直于加压方向的面上形貌。从图2中可知，对比例陶瓷的截面上晶须排布散乱，未表现出定向织构化现象。
实施例2
与实施例1不同的在于：步骤(5)中所述轴向加压为20MPa，
本实施例所得的氧化铝陶瓷显微形貌显示在垂直于加压方向的面上晶须基本上沿径向排列，相对密度为98.5％，所述氧化铝陶瓷在垂直于加压方向的面上的维氏硬度为20GPa，在弦切面中心处的维氏硬度为19GPa。
实施例3
与实施例1不同的在于：步骤(5)中所述轴向加压为50MPa，所述烧结温度为1500℃；保温时间为50min。
本实施例所得的氧化铝陶瓷显微形貌显示在垂直于加压方向的面上晶须基本上沿径向排列，相对密度为98％，所述氧化铝陶瓷的维氏硬度在垂直于加压方向的面上的维氏硬度为21GPa，在弦切面中心处的维氏硬度为20GPa。
实施例4
与实施例1不同的在于：步骤(2)中所述模具的外径为20mm，高为75mm，外径与内径之比为1.6；
本实施例所得的氧化铝陶瓷显微形貌显示在垂直于加压方向的面上晶须基本上沿径向排列，相对密度为99.7％，所述氧化铝陶瓷在垂直于加压方向的面上的维氏硬度为21.6GPa，在弦切面中心处的维氏硬度为20GPa。
实施例5
与实施例1不同的在于：步骤(2)中所述模具的外径为20mm，高为5mm，外径与内径之比为1.6；
本实施例所得的氧化铝陶瓷显微形貌显示在垂直于加压方向的面上晶须基本上沿径向排列，相对密度为99.6％，所述氧化铝陶瓷在垂直于加压方向的面上的维氏硬度为21.8GPa，在弦切面中心处的维氏硬度为20.2GPa。
本发明的氧化铝陶瓷的相对密度为98％以上，所述氧化铝陶瓷在垂直于加压方向的面上的维氏硬度为18～23GPa，在弦切面中心处的维氏硬度为17～21GPa。将该织构化氧化铝基陶瓷进行机械开刃加工，获得碳化硅晶须径向定向排列的织构化氧化铝基陶瓷切削刀具。
上述实施例为本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、组合和简化，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 (10)

1.一种织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述氧化铝基陶瓷是将氧化铝粉、碳化硅晶须、烧结助剂MgO或Y2O3，加入溶剂和球磨介质，进行球磨混合后干燥，得到混合粉体；再将混合粉体分散于热石蜡中，并趁热倒入模具中，铸造成所需形状的铸件；常温下对上述铸件施加轴向的压力为10～100MPa，铸件在高压下沿中心变形，形成晶须径向排列的织构化挤压件；然后常压下在100～250℃对织构化挤压件进行排胶，将石蜡完全挥发，得到生坯；将生坯装入石墨模具中，并置于热压烧结炉或放电等离子烧结炉中，在氩气气氛保护下，轴向加压为20～50MPa，升温至1500～1800℃保温，此后降温至500～600℃，并随炉冷却至室温制得。
2.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述的氧化铝基陶瓷的相对密度为98％以上，所述氧化铝基陶瓷在垂直于加压方向的面上的维氏硬度为18～23GPa，在弦切面中心处的维氏硬度为17～21GPa。
3.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述溶剂为乙醇、丙酮或去离子水；所述球磨介质为氧化铝球或碳化硅球；所述球磨的转速为100～300r/min，所述球磨的时间为4～24h。
4.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述的氧化铝粉的粒径为1～3μm，纯度为98～100wt.％；所述MgO或Y2O3粉的纯度为99～99.9wt.％，所述MgO或Y2O3粉的粒径为0.2～1μm。
5.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述碳化硅晶须和氧化铝粉的体积比为(4.5～55)：(54.5～94.5)。
6.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述烧结助剂占粉体总质量的0.3～1.5％。
7.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述生坯的外径为10～100mm，高度为3～80mm，外径与内径的比值为1.25～2。
8.根据权利要求1所述的织构化碳化硅晶须增韧的氧化铝基陶瓷，其特征在于，所述升温的速率为10～150℃/min，所述保温的时间为20～120min，所述降温的速率为10～150℃/min。
9.根据权利要求1-8任一项所述的织构化碳化硅晶须增韧的氧化铝基陶瓷的制备方法，其特征在于，包括如下具体步骤：
S1.将氧化铝粉、碳化硅晶须、烧结助剂MgO或Y2O3，加入溶剂和球磨介质，进行球磨混合后干燥，得到混合粉体；
S2.将混合粉体分散于热石蜡中，并趁热倒入模具中，铸造成所需形状的铸件；
S3.常温下对上述铸件施加轴向的压力为10～100MPa，铸件在高压下沿中心变形，形成晶须径向排列的织构化挤压件；
S4.常压下在100～250℃对织构化挤压件进行排胶，将石蜡完全挥发，得到生坯；
S5.将生坯装入石墨模具中，并置于热压烧结炉或放电等离子烧结炉中，在氩气气氛保护下，轴向加压为20～50MPa，升温至1500～1800℃保温，此后降温至500～600℃，并随炉冷却至室温，制得织构化碳化硅晶须增韧的氧化铝基陶瓷。
10.权利要求1-8任一项所述的织构化碳化硅晶须增韧的氧化铝基陶瓷在切削刀具领域中的应用。
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