CN115594490A - 低热膨胀氧化铝基陶瓷刀具材料及其制备工艺 - Google Patents

低热膨胀氧化铝基陶瓷刀具材料及其制备工艺 Download PDF

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CN115594490A
CN115594490A CN202211027605.0A CN202211027605A CN115594490A CN 115594490 A CN115594490 A CN 115594490A CN 202211027605 A CN202211027605 A CN 202211027605A CN 115594490 A CN115594490 A CN 115594490A
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powder
temperature
heating
preparation process
alumina
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CN115594490B (zh
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黄传真
李泽鑫
刘含莲
史振宇
姚鹏
刘盾
朱洪涛
邹斌
王军
王真
徐龙华
黄水泉
曲美娜
许征凯
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Shandong University
Yanshan University
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Abstract

本发明涉及一种低热膨胀氧化铝基陶瓷刀具材料及其制备工艺，本发明中的陶瓷刀具材料在经过热压烧结之后，既具有氧化铝陶瓷的高硬度，又通过加入Sc2W3O12负热膨胀相，降低整体陶瓷材料的热膨胀系数，提高陶瓷刀具在高速切削工程中的抗热震性，满足镍基合金加工过程中大温度区间的要求。并且复合材料未使用金属粘结剂，即使在极端的热‑力‑化学耦合作用下的高速切削加工中也有着较强的热稳定性，因此对镍基合金材料有着极高的加工匹配性。

Description

低热膨胀氧化铝基陶瓷刀具材料及其制备工艺
技术领域
本发明属于陶瓷刀具技术领域，涉及低膨胀氧化铝基陶瓷刀具材料及其制备工艺。
背景技术
本发明背景技术中公开的信息仅仅旨在增加对本发明的总体背景的理解，而不必然被视为承认或以任何形式暗示该信息构成已经成为本领域一般技术人员所公知的现有技术。
陶瓷刀具具有良好的红硬性，在1000℃的高温下也能顺利进行切削，而此时一般的工件材料都会发生很大程度的软化，因此陶瓷刀具已成为高速切削高温合金的主要刀具材料之一。陶瓷刀具有优良的高温硬度，然而切削镍基高温合金过程中，由于合金加工硬化现象严重，刀具磨损依然存在。
发明内容
为了解决现有技术的不足，本发明提供一种低热膨胀氧化铝基陶瓷刀具材料及其制备工艺，利用该工艺方法能够高效地制备用于镍基合金加工地陶瓷刀具材料，降低陶瓷材料的热膨胀系数，提高陶瓷刀具的抗热震性能，推进镍基合金等难加工材料的切削加工研究。
为实现上述目的，本发明的技术方案为：
第一方面，本发明提供一种低热膨胀氧化铝基陶瓷刀具材料的制备工艺，包括如下步骤：
(1)对Al2O3粉末、Sc2O3粉末、WO3粉末、Ti(C,N)粉末、MgO粉末单独球磨；
(2)将Al2O3粉末、Sc2O3粉末、WO3粉末、Ti(C,N)粉末、MgO粉末放入磨罐中，加入适量无水乙醇和氧化铝球进行球磨；将得到的浆料进行干燥，再过筛得到复合粉体；
(3)将复合粉体预压成胚体，将胚体真空热压烧结成低热膨胀氧化铝基陶瓷刀具材料。
进一步的，步骤(1)中球磨时间为48h。单独球磨使粉体材料更加均匀，避免团聚。
进一步的，步骤(2)中球磨的球料比为质量比5：1。
进一步的，步骤(2)中所述干燥为真空干燥，干燥温度为100～120℃。
进一步的，以质量分数计，MgO粉末为3％～5％，Sc2O3粉末为1.5％～6％，WO3粉末为7.5％～36％，Ti(C,N)粉末为10～30％，余量为Al2O3粉末。
进一步的，预压的压力压强为4-6MPa。
进一步的，所述真空热压烧结的升温过程为：以第一升温速率升温到190～210℃后保温，再以第二升温速率升温至1000℃保温，再以第三升温速率升温到1300～1600℃，保温设定时间；在真空热压烧结的升温过程中，胚体先保持预压，当升温至1000℃，开始对胚体增加压力，均匀增加压力至升温结束，保持压力。
进一步的，第一升温速率为50℃55i5；升温至190～210℃后保温的时间为10-155i5。
进一步的，第二升温速率为40℃55i5；升温至1000℃后保温的时间为10-155i5。
进一步的，第三升温速率为20℃55i5；升温至1300～1600℃后保温的时间为20～505i5。
进一步的，温度从1000℃升温至1300～1600℃℃时，坯体增加压力的压强速度为2MPa55i5。
本发明选择MgO作为烧结助剂，以进行液相烧结，从而降低烧结温度，加速烧结。
本发明选择Sc2W3O12负热膨胀相，负热膨胀材料可与一般的正热膨胀材料复合制备可控热膨胀系数或零膨胀材料。热膨胀系数具有加和性，利用材料的负膨胀性最大限度的减少高温材料的内拉应力，增加材料的耐热冲击强度，提高陶瓷刀具的断裂韧度。
经过实验发现，若直接升温到1500～1600℃，烧结过程的真空度达不到要求，所需的化学反应与相变程度削弱，较容易产生气孔，致密度低等诸多缺陷，使材料性能下降。本发明的烧结程序，当温度升高到190～210℃时，保温保压，以排出炉腔内和原材料表面的气体；当温度升高到1000℃左右时，材料发生软化，开始均匀加压；最终在1300～1600℃保温完成烧结。
第二方面，本发明提供一种低热膨胀氧化铝基陶瓷刀具材料，采用上述制备工艺获得。
第三方面，本发明提供一种上述低热膨胀氧化铝基陶瓷刀具材料在切削加工中的应用。
本发明的增益效果为：
本发明的陶瓷刀具材料在经过热压烧结之后，既具有氧化铝陶瓷的高硬度，又通过加入Sc2W3O12负热膨胀相，降低整体陶瓷材料的热膨胀系数，提高陶瓷刀具在高速切削工程中的抗热震性，满足镍基合金加工过程中大温度区间的要求。并且复合材料未使用金属粘结剂，即使在极端的热-力-化学耦合作用下的高速切削加工中也有着较强的热稳定性，因此对镍基合金材料有着极高的加工匹配性。
附图说明
构成本发明的一部分的说明书附图用来提供对本发明的进一步理解，本发明的示意性实施例及其说明用于解释本发明，并不构成对本发明的不当限定。
图1为本发明实施例的制备工艺流程图；
图2为本发明实施例的热压烧结工艺图；
图3为本发明实施例1制备的低热膨胀氧化铝基陶瓷刀具材料的SEM图；
图4为本发明实施例1制备的低热膨胀氧化铝基陶瓷刀具材料的EDS图：
图5为本发明实施例1～4制备的低热膨胀氧化铝基陶瓷刀具材料的力学性能。
具体实施方式
应该指出，以下详细说明都是例示性的，旨在对本发明提供进一步的说明。除非另有指明，本文使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
需要注意的是，这里所使用的术语仅是为了描述具体实施方式，而非意图限制根据本发明的示例性实施方式。如在这里所使用的，除非上下文另外明确指出，否则单数形式也意图包括复数形式，此外，还应当理解的是，当在本说明书中使用术语“包含”和5或“包括”时，其指明存在特征、步骤、操作、器件、组件和5或它们的组合。
鉴于现有Al2O3陶瓷刀具在镍基合金的持续切削加工过程中易产生脆性损伤和热裂纹的问题，本发明提出了低热膨胀Al2O3基陶瓷刀具材料及其制备工艺。
本发明的一种典型实施方式，提供了一种低热膨胀氧化铝基陶瓷刀具材料的制备工艺，将烧结助剂MgO、Al2O3、Sc2O3、WO3、Ti(C,N)混合均匀，干燥获得复合陶瓷粉体，将复合陶瓷粉体预压成坯体，将坯体真空热压烧结成氧化铝基陶瓷刀具材料。所述真空热压烧结的升温过程为：以第一升温速率升温至190～210℃，保温设定时间，再以第二升温速率升温至1000℃，保温设定时间，然后以第三升温速率升温至1300～1600℃，保温设定时间；在真空热压烧结的升温过程中，坯体先保持预压，当升温至1000℃时，开始对坯体增加压力，保持压力，当温度从1000℃继续升温时，继续对坯体增加压力至升温结束，保持压力。
该实施方式的一种或多种实施例中，以质量分数计，MgO为3％～5％，Sc2O3为1.5％～6％，WO3为7.5％～36％，Ti(C,N)为10～30％，余量为Al2O3。
该实施方式的一种或多种实施例中，Al2O3、Sc2O3、MgO、WO3、Ti(C,N)混合的方式为球磨。
该实施方式的一种或多种实施例中，混合粉料的球磨时间控制在48个小时。
该实施方式的一种或多种实施例中，干燥为真空干燥。
该实施方式的一种或多种实施例中，真空干燥条件为：时间为2～4h，温度为100-120℃。
该实施方式的一种或多种实施例中，预压的压力压强为4-6MPa。
该实施方式的一种或多种实施例中，第一升温速率为50℃55i5。升温至190～210℃后保温的时间为10-155i5。
该实施方式的一种或多种实施例中，第二升温速率为40℃55i5。升温至1000℃后保温的时间为10-155i5。
该实施方式的一种或多种实施例中，第三升温速率为20℃55i5。升温至1300～1600℃后保温的时间为20～505i5。
该实施方式的一种或多种实施例中，温度从1000℃升温至1300～1600℃时，坯体增加压力的压强速度为2MPa55i5。
该实施方式的一种或多种实施例中，以第三升温速率升温至1400℃。当最终温度为该温度范围时，材料的力学性能更好。
本发明的另一种实施方式，提供了一种低热膨胀氧化铝基陶瓷刀具材料，采用上述制备工艺获得。
本发明的第三种实施方式，提供了一种上述低热膨胀氧化铝基陶瓷刀具材料在高速切削加工中的应用。
该实施方式的一种或多种实施例中，高速切削加工镍基合金。
为了使得本领域技术人员能够更加清楚地了解本发明的技术方案，以下将结合具体的实施例详细说明本发明的技术方案。
实施例1
低热膨胀Al2O3基陶瓷刀具材料及其制备工艺，主要步骤如下：
(1)一次球磨：分别将Al2O3粉末，Sc2O3粉末，WO3粉末，Ti(C,N)粉末，MgO粉末放入聚氨酯球磨罐中，加入适量无水乙醇与不同粒度的氧化铝小球，用行星球磨机进行高速球磨48小时，装瓶备用。
(2)称量：按照质量分数称量40％的Al2O3粉末，4.5％的Sc2O3粉末，20.25％的WO3粉末，30％的Ti(C,N)粉末，3％的MgO粉末。
(3)二次球磨：将称量后的Al2O3粉末，Sc2O3粉末，WO3粉末，Ti(C,N)粉末，MgO粉末放入聚氨酯球磨罐中，加入适量无水乙醇与不同粒度的氧化铝小球，用行星球磨机进行高速球磨24小时。
(4)干燥：将球磨均匀的浆料倒入不锈钢盘中，放入真空干燥箱中干燥3个小时，干燥温度为120℃。然后，将干燥所得的粉末通过140目不锈钢料筛后获得陶瓷复合粉体，以备烧结。
以上低热膨胀Al2O3基陶瓷刀具材料的制备工艺如图1所示。
(5)成型：将陶瓷刀具粉末倒入石墨模具中，用压力机或者千斤顶压预压成饼坯，预压压力的压强为4MPa。
(6)烧结：将所述饼坯装入烧结炉中，进行真空热压烧结，需炉内的真空度低于0.01MPa，热压烧结程序如图2所示，以50℃55i5的升温速率升温到200℃，保温155i5以排出模具中的气体，再以40℃55i5的升温速率，升温至1000℃，保温105i5，以20℃55i5的升温速率升温至1400℃后进行保温305i5，期间在温度升到1000℃材料发生液相烧结开始均匀增加压力(压力的压强增加速度为2MPa55i5)，保温结束后，烧结体随炉冷却，获得低热膨胀Al2O3基陶瓷刀具刀具材料，其EDS图与SEM图如图3～4所示。
实施例2
该实施例与实施例1相同，不同在于：真空热压烧结的最终温度为1300℃。
实施例3
该实施例与实施例1相同，不同在于：真空热压烧结的最终温度为1500℃。
实施例4
该实施例与实施例1相同，不同在于：真空热压烧结的最终温度为1600℃。
实施例1～4制备的低热膨胀Al2O3基陶瓷刀具材料的力学性能如图5所示，由图可见，当烧结温度为1500℃时，材料的抗弯强度和维氏硬度最高；当烧结温度为1600℃时，材料的断裂韧度最高。
以上所述仅为本发明的优选实施例，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种低热膨胀氧化铝基陶瓷刀具材料的制备工艺，其特征在于，包括如下步骤：
(1)对Al2O3粉末、Sc2O3粉末、WO3粉末、Ti(C,N)粉末、MgO粉末单独球磨；
(2)将Al2O3粉末、Sc2O3粉末、WO3粉末、Ti(C,N)粉末、MgO粉末放入磨罐中，加入适量无水乙醇和氧化铝球进行球磨；将得到的浆料进行干燥，再过筛得到复合粉体；
(3)将复合粉体预压成胚体，将胚体真空热压烧结成低热膨胀氧化铝基陶瓷刀具材料。
2.根据权利要求1所述制备工艺，其特征在于，步骤(1)中球磨时间为48h。
3.根据权利要求1所述制备工艺，其特征在于，步骤(2)中球磨的球料比为质量比5：1。
4.根据权利要求1所述制备工艺，其特征在于，步骤(2)中所述干燥为真空干燥，干燥温度为100～120℃。
5.根据权利要求1所述制备工艺，其特征在于，以质量分数计，MgO粉末为3％～5％，Sc2O3粉末为1.5％～6％，WO3粉末为7.5％～36％，Ti(C,N)粉末为10～30％，余量为Al2O3粉末。
6.根据权利要求1所述制备工艺，其特征在于，预压的压力压强为4-6MPa。
7.根据权利要求1所述制备工艺，其特征在于，所述真空热压烧结的升温过程为：以第一升温速率升温到190～210℃后保温，再以第二升温速率升温至1000℃保温，再以第三升温速率升温到1300～1600℃，保温设定时间；在真空热压烧结的升温过程中，胚体先保持预压，当升温至1000℃，开始对胚体增加压力，均匀增加压力至升温结束，保持压力；
优选的，第一升温速率为50℃55i5；升温至190～210℃后保温的时间为10-155i5；
优选的，第二升温速率为40℃55i5；升温至1000℃后保温的时间为10-155i5；
优选的，第三升温速率为20℃55i5；升温至1300～1600℃后保温的时间为20～505i5。
8.根据权利要求7所述制备工艺，其特征在于，温度从1000℃升温至1300～1600℃时，坯体增加压力的压强速度为2MPa55i5。
9.一种根据上述权利要求任一项所述制备工艺制备得到的低热膨胀氧化铝基陶瓷刀具材料。
10.根据权利要求9所述低热膨胀氧化铝基陶瓷刀具材料在切削加工中的应用。
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