CN106518075A - 一种片层状BN(C)晶粒增韧的Si‑B‑C‑N陶瓷的制备方法 - Google Patents

一种片层状BN(C)晶粒增韧的Si‑B‑C‑N陶瓷的制备方法 Download PDF

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CN106518075A
CN106518075A CN201611030272.1A CN201611030272A CN106518075A CN 106518075 A CN106518075 A CN 106518075A CN 201611030272 A CN201611030272 A CN 201611030272A CN 106518075 A CN106518075 A CN 106518075A
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贾德昌
梁斌
杨治华
王胜金
何培刚
段小明
周玉
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Harbin Institute of Technology
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Abstract

本发明提供了一种片层状BN(C)晶粒增韧的Si‑B‑C‑N陶瓷的制备方法，属于Si‑B‑C‑N陶瓷制备方法技术领域。步骤一、按照摩尔比和质量比称取立方硅粉、六方氮化硼粉、石墨粉和六硼化镧粉作为原料备用；步骤二、将步骤一称取的原料装入球磨罐中，在氩气气氛保护下进行高能球磨即获得含有LaB6的Si‑B‑C‑N陶瓷复合粉末；其中球料质量比为10～90:1，磨球直径为5～9mm，球磨时间为10～60h；步骤三、将步骤二获得的陶瓷复合粉末进行放电等离子烧结即可获得片层状BN(C)晶粒增韧的Si‑B‑C‑N陶瓷材料。本发明制备方法得到的硅硼碳氮陶瓷材料具有较高的断裂韧性，降低了陶瓷发生“灾难性”断裂的可能性；添加的稀土化合物LaB6促成了片层状BN(C)晶粒的原位生长。

Description

一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法
技术领域
本发明涉及一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，属于Si-B-C-N陶瓷的制备方法技术领域。
背景技术
硅硼碳氮(Si-B-C-N)陶瓷材料具有密度低、强度高、模量低、抗氧化性好、抗蠕变性好、热膨胀系数低的特点，成为新型的高温结构材料，在航天飞机鼻锥、机翼前缘、舵面、盖板以及发动机喷管等极具应用潜力。但是，其本身的固有脆性严重限制了大规模的工业应用。为改善硅硼碳氮陶瓷的断裂韧性，颗粒(如Al、ZrO2等)、短纤维(如碳纤维、碳化硅纤维等)等“第二相”已经被引入硅硼碳氮陶瓷基体。这些“第二相”均不同程度地改善了硅硼碳氮陶瓷的脆性(梁斌等，科学通报,2015,60:236-245.)。片层状或者板状晶粒可以有效改善陶瓷的脆性，但是目前尚没有文章或者专利报道原位生长的片层状晶粒增韧硅硼碳氮陶瓷的制备方法。
发明内容
本发明的目的是为了解决上述现有技术存在的问题，进而提供一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法。
本发明的目的是通过以下技术方案实现的：
一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，
步骤一、按照摩尔比和质量比称取立方硅粉、六方氮化硼粉、石墨粉和六硼化镧粉作为原料备用；
步骤二、将步骤一称取的原料装入球磨罐中，在氩气气氛保护下进行高能球磨即获得含有LaB6的Si-B-C-N陶瓷复合粉末；其中球料质量比为10～90:1，磨球直径为5～9mm，球磨时间为10～60h；
步骤三、将步骤二获得的陶瓷复合粉末进行放电等离子烧结即可获得片层状BN(C)晶粒增韧的Si-B-C-N陶瓷材料。
所述步骤一中，Si:B:C:N的摩尔比为2:1:3:1，LaB6的添加量为原料总质量的2～20wt％。
所述步骤一中，立方硅粉的纯度为99％～99.9％，立方硅粉的粒径为1～20μm；石墨粉的纯度为99％～99.9％，石墨粉的粒径为1～20μm；六方氮化硼粉的纯度为99％～99.9％，六方氮化硼粉的粒径为1～20μm；六硼化镧粉的纯度为99％～99.9％，六硼化镧粉的粒径为10～50μm。
所述步骤二中，球料质量比为20～80:1，磨球直径为6～8mm，球磨时间为15～45h。
所述步骤三中，烧结温度为1600～2200℃，压力为30～80MPa，保温时间为2～20min。
本发明制备方法得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料经分析测试可知，硅硼碳氮陶瓷材料具有较高的断裂韧性，断裂韧性为7.50～8.10MPa·m-1/2，降低了陶瓷发生“灾难性”断裂的可能性；本发明制备方法中添加的稀土化合物LaB6促成了片层状BN(C)晶粒的原位生长。
附图说明
图1是实施例1制备得到的添加LaB6的硅硼碳氮陶瓷粉末的XRD图谱.
图2是实施例1制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的XRD图谱。
图3是实施例2制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的断口扫描照片。
图4是实施例2制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的维氏压痕扫描照片。
具体实施方式
下面将对本发明做进一步的详细说明：本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式，但本发明的保护范围不限于下述实施例。
实施例1
本实施例所涉及的一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，具体按照以下步骤进行：一、按照Si:B:C:N摩尔比为2:1:3:1的比例称取立方硅粉、六方氮化硼粉和石墨粉；再称取原料总重量8wt％的LaB6粉体；其中立方硅粉纯度为99％～99.9％，粒径为1～20μm；石墨粉纯度为99％～99.9％，粒径为1～20μm；六方氮化硼纯度为99％～99.9％，粒径为1～20μm；六硼化镧纯度为99％～99.9％，粒径为10～50μm；二、将称取的原料装入球磨罐中，在氩气气氛保护下进行高能球磨即可获得含有LaB6的Si-B-C-N陶瓷复合粉末；其中球料质量比为30:1，磨球直径为8mm，球磨时间为40h；三、将步骤二中获得的陶瓷复合粉末进行放电等离子烧结即可获得片层状BN(C)晶粒增韧的Si-B-C-N陶瓷材料；其中烧结温度为1800℃，压力为50MPa，保温时间为10min。
图1是本实施例制备得到的添加LaB6的硅硼碳氮陶瓷粉末的XRD图谱(■表示LaB6晶相)，通过图1可观察到一个馒头峰和几个尖锐的衍射峰，说明高能球磨后硅粉、氮化硼粉、石墨粉的特征衍射峰均已消失，LaB6仍保持原有的结晶态，也就是说，本实施例制备得到的添加LaB6的硅硼碳氮陶瓷复合粉末大部分具有非晶态的结构。图2是本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的XRD图谱(■表示α-SiC晶相，●BN(C)晶相，★表示La的硼/碳/氮化合物)，通过图2可知本实施例中高温烧结后获得的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料主要由α-SiC和BN(C)晶相构成，此外还含有少量La的化合物。
对本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料经分析测试可知，本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的断裂韧性为7.40MPa·m-1/2。
实施例2
本实施例所涉及的一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，具体按照以下步骤进行：一、按照Si:B:C:N摩尔比为2:1:3:1的比例称取立方硅粉、六方氮化硼粉和石墨粉；再称取所用原料总重量12wt％的LaB6粉体；其中立方硅粉纯度为99％～99.9％，粒径为1～20μm；石墨粉纯度为99％～99.9％，粒径为1～20μm；六方氮化硼粉纯度为99％～99.9％，粒径为1～20μm；六硼化镧纯度为99％～99.9％，粒径为10～50μm；二、将称取的所有原料装入球磨罐中，在氩气气氛保护下进行高能球磨即可获得含有LaB6的Si-B-C-N陶瓷粉末；其中球料质量比为40:1，磨球直径为8mm，球磨时间为30h；三、将步骤二中获得的复合粉体进行放电等离子烧结即可获得片层状BN(C)晶粒增韧的Si-B-C-N陶瓷材料；其中烧结温度为1900℃，压力为50MPa，保温时间为5min。
图3是本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的断口扫描照片，通过图3可观察到片层状的晶粒，经过进一步分析可知该晶粒主要成分为BN(C)，也就是说本实施例中高压烧结后获得的硅硼碳氮陶瓷材料中BN(C)晶粒发育良好，具有明显的片层状结构。图4是本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的维氏压痕扫描照片，通过图4可观察到本实施例制备的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料在维氏压头作用下产生了微裂纹，裂纹扩展路径曲折，并有晶粒拔出、裂纹桥联现象，说明片层状BN(C)晶粒的形成有利于硅硼碳氮陶瓷材料的断裂韧性。
对本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料经分析测试可知，本实施例制备得到的片层状BN(C)晶粒增韧的硅硼碳氮陶瓷材料的断裂韧性为7.90MPa·m-1/2。
以上所述，仅为本发明较佳的具体实施方式，这些具体实施方式都是基于本发明整体构思下的不同实现方式，而且本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。

Claims (5)

1.一种片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，其特征在于，
步骤一、按照摩尔比和质量比称取立方硅粉、六方氮化硼粉、石墨粉和六硼化镧粉作为原料备用；
步骤二、将步骤一称取的原料装入球磨罐中，在氩气气氛保护下进行高能球磨即获得含有LaB6的Si-B-C-N陶瓷复合粉末；其中球料质量比为10～90:1，磨球直径为5～9mm，球磨时间为10～60h；
步骤三、将步骤二获得的陶瓷复合粉末进行放电等离子烧结即可获得片层状BN(C)晶粒增韧的Si-B-C-N陶瓷材料。
2.根据权利要求1所述的片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，其特征在于，所述步骤一中，Si:B:C:N的摩尔比为2:1:3:1，LaB6的添加量为原料总质量的2～20wt％。
3.根据权利要求1所述的片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，其特征在于，所述步骤一中，立方硅粉的纯度为99％～99.9％，立方硅粉的粒径为1～20μm；石墨粉的纯度为99％～99.9％，石墨粉的粒径为1～20μm；六方氮化硼粉的纯度为99％～99.9％，六方氮化硼粉的粒径为1～20μm；六硼化镧粉的纯度为99％～99.9％，六硼化镧粉的粒径为10～50μm。
4.根据权利要求1所述的片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，其特征在于，所述步骤二中，球料质量比为20～80:1，磨球直径为6～8mm，球磨时间为15～45h。
5.根据权利要求1所述的片层状BN(C)晶粒增韧的Si-B-C-N陶瓷的制备方法，其特征在于，所述步骤三中，烧结温度为1600～2200℃，压力为30～80MPa，保温时间为2～20min。
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