CN114538931B - 一种高性能AlON透明陶瓷及其低温快速制备方法 - Google Patents

一种高性能AlON透明陶瓷及其低温快速制备方法 Download PDF

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CN114538931B
CN114538931B CN202210235813.3A CN202210235813A CN114538931B CN 114538931 B CN114538931 B CN 114538931B CN 202210235813 A CN202210235813 A CN 202210235813A CN 114538931 B CN114538931 B CN 114538931B
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transparent ceramic
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alon
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张朝晖
贾晓彤
程兴旺
徐天豪
刘罗锦
李先雨
贾兆虎
刘娅
冯向向
王强
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Beijing Institute of Technology BIT
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Abstract

本发明涉及一种高性能AlON透明陶瓷及其低温快速制备方法，将γ‑Al2O3、AlN、三相烧结助剂(Y2O3、MgO、La2O3)进行球磨混合；将干燥后的粉体装入石墨模具中；将石墨模具置于放电等离子烧结炉中进行真空烧结，最后在N2气氛下对样品进行除碳处理。该方法采用新型Y2O3、MgO、La2O3三相烧结助剂并利用放电等离子烧结技术通过固相反应一步制得AlON透明陶瓷，不仅简化了AlON透明陶瓷的制备工艺，且大幅降低了AlON透明陶瓷的烧结温度，缩短烧结时间，同时提高了AlON透明陶瓷的致密度，在保证AlON陶瓷透过率的前提下极大地提高AlON透明陶瓷的综合力学性能。

Description

一种高性能AlON透明陶瓷及其低温快速制备方法
技术领域
本发明涉及一种高性能AlON透明陶瓷及其低温快速制备方法，属于透明陶瓷材料制备领域。
背景技术
尖晶石型氮氧化铝(γ-AlON)是Al2O3-AlN体系中一类重要的单相、稳定的固溶体陶瓷，具有光学各向同性的立方结构。AlON透明陶瓷具有优异的光学透明性、高强度、高硬度以及极佳的耐磨和抗划伤性，抗化学腐蚀性等特点，是制备透明装甲的理想材料。
目前，AlON透明陶瓷烧结主要采用无压烧结，该方法需先高温合成AlON粉体，再对粉体进行预成型，最后高温烧结使其致密化。该烧结方法存在成本高、工艺过程复杂、烧结温度高、保温时间长、产品致密度低等缺点，从而导致陶瓷样品的力学性能较差，难以满足装甲材料的性能需求。
中国专利200710013606.9公开了一种透明AlON陶瓷的制备工艺，将重量比为80～95％的Al2O3与5～20％的AlN混合，并加入质量分数为0.1～9％的Y2O3和CaF2作为烧结助剂，先对粉体进行预成型后在800～1200℃下，保温0.5～3h进行素烧，降温后在1800～1900℃下，保温0.5～8h进行二次无压烧结。该方法烧结温度高、烧结时间长，且得到的AlON透明陶瓷的致密度仅为99％，其近红外区透过率仅为50％左右。
中国专利202110440670.5公开了一种溶液燃烧合成法制备高纯高透光性的AlON陶瓷的方法。该方法利用水溶性铝盐、水溶性有机物、有机燃料、氧化剂、金属硝酸盐或者无机酸等燃烧反应得到Al2O3和C的混合物。该混合物在1300～1800℃氮气气氛下反应0.1～10h得到AlON粉体，随后对粉体进行除碳。将预成型的生坯置于氮气气氛中，1800～2000℃保温1～20h。该方法得到的AlON透明陶瓷样品的晶粒尺寸在100～250μm之间，其维氏硬度仅为15～17GPa。
放电等离子烧结(SPS)是一种新型粉末冶金烧结技术，与传统的无压烧结方法相比，放电等离子烧结技术的主要特点是通过脉冲电流加热对陶瓷进行快速致密化烧结，其具有升温速度快、烧结时间短、烧结温度低、加热均匀、生产效率高等优点，可以在低温、短时间内使陶瓷粉末致密化，在一定程度上能够抑制晶粒长大，使其保持原始颗粒的微观结构，从本质上提高烧结体的综合性能。另外，放电等离子烧结技术能够使Al2O3和AlN通过直接固相反应一步生成AlON透明陶瓷，极大地简化了制备工艺，节约了制备时间和制备成本。
为降低烧结温度、缩短保温时间、提高致密度、降低气孔率，获得高质量的AlON透明陶瓷，一般需要加入烧结助剂。烧结助剂的种类和用量对AlON透明陶瓷的透过率极其敏感，烧结助剂的种类和含量不同，AlON陶瓷透明性会有很大差异。烧结助剂用量过少，则烧结温度较高，样品致密化困难，气孔难以排出，从而导致AlON透明陶瓷的透过率和力学性能下降；烧结助剂用量过多，则过量的烧结助剂在晶体内部生长第二相，引起光的散射，同样导致AlON透明陶瓷透过率下降。因此找到合适的烧结助剂种类和含量，使AlON透明陶瓷在保证透过率的情况下具有优异的力学性能，成为制备高性能AlON透明陶瓷的关键。
发明内容
本发明目的在于提供一种高性能AlON透明陶瓷及其低温快速制备方法，克服现有AlON透明陶瓷制备技术的缺点，通过新型烧结助剂组合使用以及新型放电等离子烧结方法，在保证AlON陶瓷透过率的情况下极大地提高其力学性能。
本发明中高性能AlON透明陶瓷的低温快速制备方法，主要包括以下步骤：
步骤1)粉体混合：以摩尔比为(55～70mol％)：(45～30mol％)的γ-Al2O3粉、AlN粉为原料，并加入Y2O3、MgO、La2O3三相烧结助剂，其中Y2O3质量分数为0.05～0.4wt％，MgO质量分数为0.05～0.6wt％，La2O3质量分数为0.01～0.3wt％，且三相烧结助剂的总质量分数不超过1wt％。将原料粉体、烧结助剂和无水乙醇共同放入尼龙球磨罐中，采用进口高纯Al2O3磨球、球料比3：1～5：1，利用全方位行星式球磨机对粉体进行混匀、分散，球磨转速为100～450r/min，球磨时间为2～30h。
步骤2)粉体干燥：利用旋转蒸发仪干燥粉体，将干燥后的粉体进行研磨并过200目筛，最终得到均匀分散的混合粉体。
步骤3)装模：将干燥后的混合粉体装入石墨模具中。为更好的脱模，粉体与石墨模具间需垫1到2层石墨纸；为防止烧结过程中热量散失，需在石墨模具外表面裹1到2层石墨毡。
步骤4)放电等离子烧结：将装好的模具放入放电等离子烧结炉炉腔中，待真空度小于20Pa后开始烧结，以20～400℃/min的升温速率升至1450～1700℃，保温1～40min后随炉冷却，烧结过程中压力为10～100MPa。其中，升温速率优选50～200℃/min，烧结温度优选1550～1650℃，保温时间优选5-15min，烧结压力优选40-70MPa。
步骤5)除碳：将放电等离子烧结后的样品进行N2条件下高温除碳处理，温度为1650～1900℃，时间为1～6h。
步骤6)磨平抛光：将除碳后的AlON透明陶瓷样品进行磨平、抛光，最终得到高透过率的AlON透明陶瓷。
所述的高性能AlON透明陶瓷的低温快速制备方法中，γ-Al2O3、AlN、Y2O3、MgO、La2O3粉体的纯度均大于99.9％，粒径0.01～1μm。
所述的高性能AlON透明陶瓷的低温快速制备方法中，为保证固相反应有足够的驱动力，需在其固相反应温度前加完所有压力，最终得到AlON透明陶瓷样品。
根据所述的高性能AlON透明陶瓷的低温快速制备方法制备出的AlON透明陶瓷的硬度为17～25GPa；弯曲强度为300～600MPa；断裂韧性为3～6MPa·m1/2。
本发明的有益效果包括：
1)本发明采用全方位行星式球磨机对粉体进行匀化、分散，在不添加任何分散剂的情况下即可实现烧结助剂在原料粉体中的均匀分散，解决了由于烧结助剂局部分散不均匀而导致样品显微结构不均匀的问题，有效提高了样品的综合力学性能。
2)本发明采用先进的放电等离子烧结技术通过一步固相反应烧结得到AlON透明陶瓷，与传统的无压烧结相比，大幅降低了烧结温度，缩短了烧结时间，能够有效抑制烧结过程中的晶粒长大现象，同时极大地简化了工艺流程，提高了工作效率，节约了成本。
3)本发明采用新型Y2O3、MgO、La2O3三相烧结助剂，进一步降低AlON透明陶瓷的烧结温度，缩短烧结时间，提高AlON透明陶瓷的致密度，降低其气孔率，同时在保证AlON陶瓷透过率的前提下极大地提高了其综合力学性能。
4)本发明中，烧结压力在固相反应前全部加完，从而保证反应发生时有足够的驱动力，确保固相反应完全进行，最终得到高性能的AlON透明陶瓷。
5)本发明采用N2条件下高温除碳的方法，有效解决了放电等离子烧结过程中不可避免的模具污染问题。
附图说明
图1(a)为实施例1中样品的XRD图；
图1(b)为实施例2中样品的XRD图；
图1(c)为实施例3中样品的XRD图；
图2(a)为实施例1中样品的断面SEM图；
图2(b)为实施例2中样品的断面SEM图；
图2(c)为实施例3中样品的断面SEM图；
图3(a)为实施例1中样品的透过率曲线；
图3(b)为实施例2中样品的透过率曲线；
图3(c)为实施例3中样品的透过率曲线。
具体实施方式
下面结合附图和具体实施例进一步说明本发明，但不作为对本发明的限制。
实施例1
步骤1)粉体混合
将摩尔比为60mol％：40mol％的γ-Al2O3粉(纯度99.99％，粒径50nm)和AlN粉(纯度99.99％，粒径50nm)、烧结助剂(0.08wt％Y2O3+0.2wt％MgO+0.08wt％La2O3)，以3mm、8mm、10mm的高纯Al2O3球为球磨介质，球料比3：1，并加入无水乙醇作为分散介质，共同放入尼龙罐中，利用全方位行星式球磨机以100r/min的转速球磨30h。
步骤2)粉体干燥
利用旋转蒸发仪干燥粉体，将干燥后的粉体进行研磨并过200目筛，最终得到均匀分散的混合粉体。
步骤3)装模：将干燥后的混合粉体装入石墨模具中。为更好的脱模，粉体与石墨模具间需垫1到2层石墨纸；为防止烧结过程中热量散失，需在石墨模具外表面裹1到2层石墨毡。
步骤4)放电等离子烧结：将装好的模具放入放电等离子烧结炉炉腔中，待真空度小于20Pa后开始烧结，以100℃/min的升温速率升至1600℃，保温5min后随炉冷却，烧结过程中压力为40MPa。
步骤5)除碳：将烧结好的样品置于N2气氛下进行1800℃，保温3h的除碳处理。
步骤6)磨平抛光：将除碳后的AlON透明陶瓷样品进行磨平、抛光，最终得到高透过率的AlON透明陶瓷。
对本实施例制得的AlON透明陶瓷进行测试，结果如下：
(1)本实施例中样品的XRD图如图1(a)所示，样品为AlON纯相，无其他杂相。
(2)本实施例中AlON透明陶瓷的致密度为99.8％，其断面微观结构如图2(a)所示，从图中可以看出，AlON透明陶瓷呈现典型的脆性断裂特征，其微观结构致密、无明显气孔。
(3)本实施例中AlON透明陶瓷在可见光波段的最大透过率为68％，其透过率曲线如图3(a)所示。
(4)本实施例中AlON透明陶瓷的硬度为18.82GPa、弯曲强度为500.07MPa、断裂韧性为5.04MPa·m1/2。
实施例2
步骤1)粉体混合：
将摩尔比为64.3mol％：35.7mol％的γ-Al2O3粉(纯度99.99％，粒径20nm)和AlN粉(纯度99.99％，粒径50nm)、烧结助剂(0.12wt％Y2O3+0.3wt％MgO+0.04wt％La2O3)以3mm、8mm、10mm的高纯Al2O3球为球磨介质，球料比4：1，并加入无水乙醇作为分散介质，共同放入尼龙罐中，利用全方位行星式球磨机以150r/min的转速球磨20h。
步骤2)与实施例1相同
步骤3)与实施例1相同。
步骤4)放电等离子烧结：
将装好的模具放入放电等离子烧结炉炉腔中，待真空度小于20Pa后开始烧结，以150℃/min的升温速率升至1580℃，保温10min后随炉冷却，烧结过程中压力为50MPa。
步骤5)除碳：将烧结好的样品置于N2气氛下进行1700℃，保温3h的除碳处理。
步骤6)与实施例1相同。
对本实施例制得的AlON透明陶瓷进行测试，结果如下：
(1)本实施例中样品的XRD图如图1(b)所示，样品为AlON纯相，无其他杂相。
(2)本实施例中AlON透明陶瓷的致密度为99.9％，其断面微观结构如图2(b)所示，从图中可以看出，AlON透明陶瓷呈现典型的脆性断裂特征，其微观结构致密、无明显气孔。
(3)本实施例中AlON透明陶瓷在可见光波段的最大透过率为71％，其透过率曲线如图3(b)所示。
(4)本实施例中AlON透明陶瓷的硬度为19.01GPa、弯曲强度为490.60MPa、断裂韧性为4.66MPa·m1/2。
实施例3
步骤1)粉体混合：
将摩尔比为64.3mol％：35.7mol％的γ-Al2O3粉(纯度99.99％，粒径20nm)和AlN粉(纯度99.99％，粒径50nm)、烧结助剂(0.16wt％Y2O3+0.4wt％MgO+0.08wt％La2O3)以3mm、8mm、10mm的高纯Al2O3球为球磨介质，球料比5：1，并加入无水乙醇作为分散介质，共同放入尼龙罐中，利用全方位行星式球磨机以200r/min的转速球磨10h。
步骤2)与实施例1相同
步骤3)与实施例1相同。
步骤4)放电等离子烧结：
将装好的模具放入放电等离子烧结炉腔中，抽真空到真空度小于20Pa后开始烧结，以200℃/min的升温速率升至1600℃，保温5min后随炉冷却，烧结过程中压力为60MPa。
步骤5)除碳：将烧结好的样品置于N2气氛下进行1800℃，保温2h的除碳处理。
步骤6)与实施例1相同。
对本实施例制得的AlON透明陶瓷进行测试，结果如下：
(1)本实施例中样品的XRD图如图1(c)所示，样品为AlON纯相，无其他杂相。
(2)本实施例中AlON透明陶瓷的致密度为99.9％，其断面微观结构如图2(c)所示，从图中可以看出，AlON透明陶瓷呈现典型的脆性断裂特征，其微观结构致密、无明显气孔。
(3)本实施例中AlON透明陶瓷在可见光波段的最大透过率为75％，其透过率曲线如图3(c)所示。
(4)本实施例中AlON透明陶瓷的硬度为19.28GPa、弯曲强度为569.49MPa、断裂韧性为5.25MPa·m1/2。
上述内容对本发明实施例结合附图进行了说明，但本发明包括但不限于上述实施例，凡是在本发明精神的原则之下进行的任何修改、补充、等同替换或局部改进，都将视为在本发明的保护范围之内。

Claims (7)

1.一种高性能AlON透明陶瓷的低温快速制备方法，其特征在于，该方法包括以下工艺步骤：
1)粉体混合：以γ-Al2O3粉、AlN粉为原料，加入烧结助剂，进行球磨混合；
烧结助剂为Y2O3、MgO、La2O3三相混合，其中Y2O3质量分数为0.05～0.4wt％，MgO质量分数为0.05～0.6wt％，La2O3质量分数为0.01～0.3wt％，且三相烧结助剂的总质量分数不超过1wt％；
2)粉体干燥：对粉体进行干燥，取干燥后的粉体过筛，得到均匀分散的混合粉体；
3)装模：将干燥后的混合粉体放置于石墨模具中；
4)放电等离子烧结：将模具放入放电等离子烧结炉中，抽真空，待炉内真空度小于20Pa后进行烧结，得到AlON陶瓷样品；
5)除碳：将放电等离子烧结后的样品置于N2条件下进行高温除碳处理；
6)磨平抛光：将除碳后的AlON陶瓷样品进行磨平、抛光，最终得到高透过率的AlON透明陶瓷。
2.根据权利要求1所述的高性能AlON透明陶瓷的低温快速制备方法，其特征在于，所述步骤1)中：γ-Al2O3粉、AlN粉的摩尔比为55～70mol％：45～30mol％。
3.根据权利要求1所述的高性能AlON透明陶瓷的低温快速制备方法，其特征在于，利用全方位行星式球磨机对粉体进行充分混合、匀化和分散，具体为：采用尼龙球磨罐，高纯Al2O3磨球，球料比3：1～5：1，无水乙醇为球磨介质，转速100～450r/min，球磨2～30h；
直径3mm、8mm、10mm的高纯Al2O3磨球质量比1：1：1；
γ-Al2O3、AlN、Y2O3、MgO、La2O3粉体纯度均大于99.9％，粒径0.01～1μm。
4.根据权利要求1所述的高性能AlON透明陶瓷的低温快速制备方法，其特征在于，所述步骤3)中，为防止粘连，粉体与石墨模具间需垫1到2层石墨纸；为保温，需在石墨模具外表面裹1到2层石墨毡。
5.根据权利要求1所述的高性能AlON透明陶瓷的低温快速制备方法，其特征在于，所述步骤4)中烧结条件为：以50～300℃/min的升温速率升至1450～1700℃，保温1～40min后随炉冷却，烧结过程中压力为10～100MPa；
在固相反应温度前加完所有压力，使固相反应有足够的驱动力，同时提高AlON透明陶瓷的力学性能。
6.根据权利要求1所述的高性能AlON透明陶瓷的低温快速制备方法，其特征在于，所述步骤5)中高温除碳条件为：温度1600～1900℃，保温时间1～6h。
7.一种高性能AlON透明陶瓷，其特征在于，根据权利要求1到6任一项所述的制备方法所得。
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