CN113650168A - 一种陶瓷的锻造方法 - Google Patents

一种陶瓷的锻造方法 Download PDF

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CN113650168A
CN113650168A CN202111070081.9A CN202111070081A CN113650168A CN 113650168 A CN113650168 A CN 113650168A CN 202111070081 A CN202111070081 A CN 202111070081A CN 113650168 A CN113650168 A CN 113650168A
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樊磊
安立楠
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Zhengzhou University of Aeronautics
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Abstract

本发明涉及一种陶瓷的锻造方法，属于陶瓷制备技术领域。本发明的陶瓷的锻造方法，包括以下步骤：将待锻造陶瓷在锻造温度下施加振荡压力进行锻造。本发明的陶瓷的锻造方法，通过振荡压力下改变陶瓷材料高温下的变形机制，提升陶瓷材料变形能力和变形速率，使陶瓷材料内部微观疲劳的产生和材料变形历程的大幅提升，进而使陶瓷材料能够在更低的温度和压力下达到更高的变形速率并达到更大的变形量，从而使得陶瓷锻造得以实现并大幅降低成本。此外，利用振荡压力锻造所产生的变形过程可以实现陶瓷材料相对密度的提升和性能的强化，也可以实现一定形状和尺寸陶瓷构件的锻造成形。

Description

一种陶瓷的锻造方法
技术领域
本发明涉及一种陶瓷的锻造方法，属于陶瓷制备技术领域。
背景技术
锻造是通过压力使材料产生塑性变形从而获得一定形状、尺寸和性能的方法。锻造常用于金属材料的加工成型，对于陶瓷材料由于其滑移困难，塑性差因此很难进行锻造加工。常用的高性能陶瓷构件的制备方法主要为热压烧结，相较于热压烧结，锻造过程在材料内部产生更大的剪切应力，使材料产生更大的变形，不仅可以极大的消除材料内部的孔隙结构，还可以产生织构组织和加工硬化从而大幅提高材料性能。
陶瓷材料多以离子键和共价键结合，这使得陶瓷材料位错产生和运动很困难。虽然高温下随着原子活动能力的提高，产生变形所需要的应力会逐渐降低，但要实现陶瓷锻造仍需要较高的温度和压力。在现有的静态压力条件下，陶瓷材料的高温蠕变机制主要以Coble和Naborro-Herring扩散机制为主，应变量小且应变速率低，若要将其变形机制提升至滑移或位错控制的幂律变形机制以达到提高应变量和应变速率的效果，则需要很高的温度和非常高的静态压力，往往超过设备和高温模具如石墨模具的承受范围。这使得陶瓷锻造难以实现或需要极高的成本。
发明内容
本发明的目的是提供一种陶瓷的锻造方法，能够降低陶瓷锻造成本。
为了实现以上目的，本发明所采用的技术方案是：
一种陶瓷的锻造方法，包括以下步骤：将待锻造陶瓷在锻造温度下施加振荡压力进行锻造。
本发明的陶瓷的锻造方法，通过振荡压力改变陶瓷材料在高温下的变形机制，提升陶瓷材料变形能力和变形速率，使陶瓷材料内部微观疲劳的产生和材料变形历程的大幅提升，进而使陶瓷材料的高温变形机制能够在更低的温度和压力达到更高的变形速率并达到更大的变形量，从而使得陶瓷锻造得以实现并大幅降低成本。此外，利用振荡压力锻造所产生的变形过程可以实现陶瓷材料相对密度的提升和性能的强化，也可以实现一定形状和尺寸陶瓷构件的锻造成形。
优选的，所述振荡压力和锻造温度应当满足以下条件：所述待锻造陶瓷在所述振荡压力的中值压力和所述锻造温度下进行变形时的压力指数≥2。压力指数≥2时，所述变形的机制为晶界滑移或位错蠕变控制的幂律变形。所述锻造温度在待锻造陶瓷的蠕变温度以上。
振荡压力的中值压力的选取是与锻造温度配合选取。优选的，所述振荡压力的振幅为振荡压力的中值压力的8-100％，例如为12.5％、14.2％或20％。
优选的，所述振荡压力的压力中值为40-120MPa，例如为50MPa、70MPa、80MPa或100MPa。
优选的，所述振荡压力的频率为1-20Hz，例如可以为5Hz或10Hz。
优选的，所述振荡压力的波形为正弦波或余弦波。
优选的，所述待锻造陶瓷的相对密度为60-100％。本发明的陶瓷锻造方法对于相对密度99％以下的待锻造陶瓷采用本发明的锻造方法锻造后，可实现进一步地致密化从而实现相对密度的提升；对于致密(相对密度≥99％)或非致密(相对密度<99％)的待锻造陶瓷，锻造后陶瓷的强度和硬度得以提升。
优选的，所述锻造的时间为0.5-2h，例如为1h。
优选的，所述待锻造陶瓷为液相烧结陶瓷或固相烧结陶瓷。所述液相烧结陶瓷为含有晶间玻璃相或非晶相的陶瓷材料。例如，所述液相烧结陶瓷为液相烧结氮化硅陶瓷或液相烧结氮化铝陶瓷。所述固相烧结陶瓷为晶间无玻璃相或晶间非晶相的陶瓷。优选的，所述固相烧结陶瓷为碳化硼陶瓷或氧化铝陶瓷。所述待锻造陶瓷可以为制备时添加烧结助剂的陶瓷，也可以为烧结时不使用助剂的陶瓷。
待锻造陶瓷为碳化硼陶瓷时，锻造的温度优选为1800-2000℃，振荡压力的压力中值为50-70MPa。
待锻造陶瓷为氮化硅陶瓷时，锻造的温度优选为1600-1800℃，振荡压力的压力中值为40-70MPa。
待锻造陶瓷为氧化铝陶瓷时，锻造的温度优选为1500-1800℃，振荡压力的压力中值为70-120MPa。
所述待锻造陶瓷在施加振荡压力进行锻造前，已经进行了烧结并产生了烧结结合。该烧结结合的待锻造陶瓷既可以是在锻造之前先进行烧结，冷却后取出的陶瓷材料，也可以是在施加振荡压力前，在加热时产生的烧结。所述烧结即可以为加压烧结也可以为无压烧结。同时烧结既可有烧结助剂，也可以无烧结助剂。优选的，通过加压或无压烧结得到待锻造陶瓷，然后将待锻造陶瓷加热至锻造温度，并在锻造温度下施加振荡压力进行锻造。
附图说明
图1为实施例1中待锻造陶瓷和锻造后的陶瓷的形貌图。
具体实施方式
以下结合具体实施方式对本发明的技术方案作进一步的说明。
实施例1
本实施例的陶瓷的锻造方法，以无烧结助剂加入的热压烧结碳化硼陶瓷(形状为直径30mm，高4.61mm的圆柱体，相对密度为98％)作为待锻造陶瓷，包括以下步骤：
将待锻造陶瓷放入直径40mm的石墨模具，将装入待锻造陶瓷的石墨模具放入高温炉中，真空条件下加热至锻造温度1900℃并保温1h，在保温阶段加载振荡压力，振荡压力波形为正弦波，频率为5Hz，压力中值为70MPa，振幅为10MPa，振荡锻造1小时后，得到直径40mm，高2.78mm的碳化硼锻造件；待锻造陶瓷在1900℃、70MPa的变形时的应力指数n＝3.38。
所得待锻造陶瓷和锻造后锻造件如图1所示，所得碳化硼陶瓷锻造件相对密度为99.5％，维氏硬度由待锻造陶瓷的28GPa提升到锻造件的36GPa，抗弯强度由待锻造陶瓷的270MPa提升到锻造件的620MPa。
实施例2
本实施例的陶瓷的锻造方法，以无烧结助剂加入的热压烧结碳化硼陶瓷(形状为直30mm，高5mm的圆柱体，相对密度为99.7％)作为待锻造陶瓷，包括以下步骤：
将待锻造陶瓷放入直径40mm的石墨模具，将装入待锻造陶瓷的石墨模具放入高温炉中，真空条件下加热至锻造温度2000℃并保温1h，在保温阶段加载振荡压力，振荡压力波形为正弦波，频率为20Hz，压力中值为50MPa，振幅为10MPa，振荡锻造1小时后，得到直径40mm的碳化硼锻造件；待锻造陶瓷在2000℃、50MPa的变形时的应力指数n＝3.63。
所得碳化硼陶瓷锻造件相对密度为99.7％，维氏硬度由待锻造陶瓷的30GPa提升到锻造件的36GPa，抗弯强度由待锻造陶瓷的315MPa提升到锻造件的670MPa。
实施例3
本实施例的陶瓷的锻造方法，以采用加入质量比10％Y2O3为烧结助剂的氮化硅陶瓷(液相烧结氮化硅陶瓷，相对密度为80％)作为待锻造陶瓷，包括以下步骤：
将待锻造陶瓷放入石墨磨具中，在氮气气氛下，加热至1800℃保温，加载振荡压力，振荡压力的振荡波形为正弦波，频率为5Hz，振荡压力中值为70MPa，振幅为10MPa，振荡锻造1小时后，得到变形后的氮化硅陶瓷锻件；待锻造陶瓷在1800℃、70MPa下的应力指数n＝2.2。
所得氮化硅陶瓷锻造件相对密度为98％，维氏硬度由原来的9GPa提升至14GPa,抗弯强度由320MPa提升至710MPa。
实施例4
本实施例的陶瓷的锻造方法，以采用加入质量比2％Li2O和10％Y2O3为烧结助剂，1500℃无压烧结的氮化硅陶瓷(液相烧结氮化硅陶瓷，相对密度为72％)作为待锻造陶瓷，包括以下步骤：
将待锻造陶瓷放入石墨磨具中，在氮气气氛下，加热至1600℃保温，加载振荡压力，振荡压力的振荡波形为正弦波，频率为5Hz，振荡压力中值为40MPa，振幅为30MPa，振荡锻造1小时后，得到变形后的氮化硅陶瓷锻件；待锻造陶瓷在1600℃、40MPa下的应力指数n＝2.1。
所得氮化硅陶瓷锻造件相对密度为96％，维氏硬度由原来的6GPa提升至12GPa,抗弯强度由230MPa提升至640MPa。
实施例5
本实施例的陶瓷的锻造方法，以无烧结助剂加入的固相烧结氧化铝陶瓷(相对密度为99.4％)为待锻造陶瓷，包括以下步骤：
将待锻造陶瓷放入石墨模具中，加热至1600℃保温，加载振荡压力，振荡压力的振荡波形为正弦波，频率为1Hz，振荡压力中值为120MPa，振幅为10MPa，振荡锻造1小时后，得到变形后的氧化铝陶瓷锻件；待锻造陶瓷在1600℃、120MPa下的变形时的应力指数n＝3.12。
所得氧化铝陶瓷锻造件相对密度为99.8％，维氏硬度由原来的14GPa提升到16GPa，抗弯强度由330GPa提升至400GPa。

Claims (10)

1.一种陶瓷的锻造方法，其特征在于：包括以下步骤：将待锻造陶瓷在锻造温度下施加振荡压力进行锻造。
2.根据权利要求1所述的陶瓷的锻造方法，其特征在于：所述振荡压力和锻造温度应当满足以下条件：所述待锻造陶瓷在所述振荡压力的中值压力和所述锻造温度下进行变形时的压力指数≥2。
3.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述振荡压力的振幅为振荡压力的中值压力的8-100％。
4.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述振荡压力的压力中值为40-120MPa。
5.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述振荡压力的频率为1-20Hz。
6.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于，所述振荡压力的波形为正弦波或余弦波。
7.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述待锻造陶瓷的相对密度为60-100％。
8.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述锻造的时间为0.5-2h。
9.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述待锻造陶瓷为液相烧结陶瓷或固相烧结陶瓷。
10.根据权利要求1或2所述的陶瓷的锻造方法，其特征在于：所述待锻造陶瓷为碳化硼陶瓷时，锻造的温度为1800-2000℃，振荡压力的压力中值为50-70MPa；所述待锻造陶瓷为氮化硅陶瓷时，锻造的温度为1600-1800℃，振荡压力的压力中值为40-70MPa；所述待锻造陶瓷为氧化铝陶瓷时，锻造的温度为1500-1800℃，振荡压力的压力中值为70-120MPa。
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